Salicylic Acid

PRODUCTION OF SALICYLIC ACID BY
KOLB SCHMITT PROCESS
Session 2011-2015
Group Members:
Suleman Nasrullah UW-11-Ch.E-BSc-002
Khesro Dawood UW-11-Ch.E-BSc-016
Iftikhar Ali UW-11-Ch.E-BSc-055
Ikram Ullah UW-11-Ch.E-BSc-061
DEPARTMENT OF CHEMICAL ENGINEERING

WAH ENGINEERING COLLEGEUNIVERSITY OF WAH, WAH CANTT PAKISTAN
PRODUCTION OF SALICYLIC ACID BY
KOLB SCHMITT PROCESS
This report is submitted to Department of Chemical Engineering, Wah

Engineering College, University of Wah for the partial fulfillment of
the requirements for the Bachelors Degree in Chemical Engineering.
Internal Examiner External Examiner
DEPARTMENT OF CHEMICAL ENGINEERING

WAH ENGINEERING COLLEGEUNIVERSITY OF WAH, WAH CANTT PAKISTAN
DEDICATED TO
Our
Beloved Parents,
Respected Teachers
And
Sincere Friends
i
ACKNOWLEDGEMENT
All praises to ALMIGHTY ALLAH, who provided us with the strength to
accomplish the final year project. All respects are for His HOLY PROPHET (PBUH),
whose teachings are true source of knowledge & guidance for whole mankind.
Before anybody else we thank our Parents who have always been a source of
moral support and driving force behind whatever we do. We are indebted to our project
advisor Mr.Kashif Iqbal and Mr.Ahmad Farooqi for his worthy discussions, encouragement,
inspiring guidance, remarkable suggestions, keen interest, constructive criticism &
friendly discussions which enabled us to complete this report. He spared a lot of his precious
time in advising & helping us in writing this report. Without his painstaking tuition, kind
patronization, sincere coaching and continuous consultation, we would not have been
able to complete this arduous task successfully.
We are also grateful to the Head of department Prof. Dr. A.K. Salariya, Prof .Dr. G.M
Mamoor, Madam Adila Anbreen, and Mr.Waqas Ahmad for their profound gratitude and
superb guidance in connection with the project.
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PREFACE
O-Hydroxy Benzoic acid is mainly in the manufacturing of aspirin. Other uses are
in the manufacture of phenolic resins, rubber retarders, dyestuffs, and also its salts and esters
for a variety of applications. This project report deals with design calculations of 35 tons/day
of the O-Hydroxy Benzoic Acid production rate, along with their relevant aspects such as
material of construction, instrumentation and control, economic viability and environmental
aspects. O-Hydroxy Benzoic Acid also finds its application in Pakistan for variety of
purposes.
Keeping these points in mind we urged to work & we are feeling great to present
our work on Production of Salicylic Acid by Kolbe Schmitt process. This report is divided
in different sections. First of all the introduction of Salicylic Acid is given, which highlights
its importance. Next are detailed description of Production of Salicylic Acid by Kolbe Schmitt
process of. Afterwards material and energy balance is presented.
In preceding chapters introduction to different equipments of plant along with their
designing procedure and specification sheets is presented. Instrumentation & Control,
HAZOP Study, and Cost Estimation for this plant are also included in this report
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LIST OF TABLES
Table-1.1: Physical Properties of Hydroxybenzoic acid ........................................................... 2

Table-1.2 : Solubilitys of the Hydroxybenzoic Acids in Water, Wt % .................................... 3
Table-3.1.1: Material balance around CSTR (R-1) ................................................................. 18
Table 3.1.2: Material balance around flash tank (FT-1) .......................................................... 20
Table-3.1.3: Material balance around autoclave(R-2) ............................................................. 22
Table-3.1.4 : Material balance around distillation column (DC-1) ......................................... 24
Table-3.1.5 : Material balance around dilution tank (M-1) ..................................................... 25
Table-3.1.6: Material balance around Acidification tank(R-3) ............................................... 26
Table-3.1.7: Material balance around centrifuge (FF-1) ......................................................... 27
Table-3.1.8 :Material balance around dryer (DE-1) ................................................................ 28
Table-3.1-9: Material balance around sublimation tank (SB-1) .............................................. 29
Table-3.1.10: Material balance around Crystallizer (C-1)....................................................... 30
Table-4.1.1(a): Calculations at the inlet of reactor .................................................................. 32
Table-4.1.1(b): Calculations at the outlet of reactor................................................................ 33
Table-4.1.4(a): Energy balance calculation at inlet ................................................................. 37
Table-4.1.4(b): Energy balance calculation at outlet............................................................... 38
Table-4.1.7(a): Energy balance calculation at inlet ................................................................. 42
Table-4.1.7(b): Energy balance calculation at outlet............................................................... 43
Table-5.4: Vessel diameter against minimum thickness ......................................................... 56
Table-5.5: Different type of head comparison ......................................................................... 57
Table-5.4.1: Comparison of the different tray ......................................................................... 83
Table -5.8.3: Size of the vacuum rotary dryers ..................................................................... 126
Table-7.1: HAZOP Guide Words and Meanings .................................................................. 152
Table 9.1: Marshall and Swift Equipment Cost Index .......................................................... 159
Table 9-2: Equipment cost ..................................................................................................... 163
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LIST OF FIGURES
Figure-5.1: Reynolds number against Power number ............................................................. 59

Figure-5.2: Jacketed vessels,(a)Spirally baffled jacket (b) Dimple jacket (c) Half-pipe 61
Figure-5.3: Reynold number verses J factor ........................................................................... 62
Figure-5.4: Design velocity factor vs kv ................................................................................. 69
Figure-5.5: Different types of blades....................................................................................... 77
Figure -5.6: Relation b/w downcomer area and weir length ................................................... 87
Figure-5.7: Fl,v vs fractional entrainment ................................................................................ 96
Figure-5.5.1: Basic Impeller types (a) Turbine impeller (b) Pitch bladed turbine ............... 100
Figure-5.5.2: Chemical process equipment selection and design) by Stanly M.Walas ........ 103
Figure-5.8.1: Classification of Dryers based on Method of Operation ................................. 117
Figure-5.8.2: Classification of dryer based on physical form of feed ................................... 118
Figure-5.8.3: Classification of dryers on scale of production ............................................... 119
Figure-5.8.4 :Classification of Dryer based on Nature of feed.............................................. 120
Figure-5.8.5: Vacuum Rotary Dryer ..................................................................................... 122
Figure-5.9.1: True and pseudo sublimation cycle. ................................................................ 130
Figure -5.10.1: Capacity against Pump efficiency ................................................................ 138
Figure-6.1 : Control loop of CSTR Scheme ..................................................................... 148
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TABLE OF CONTENTS
1. Introduction
1.1 Introduction ........................................................................................................................ 1
1.2 Properties of Salicylic Acid ......................................................................................... 2
1.2.1 Physical Properties ............................................................................................... 2
1.2.2 Chemical Properties ............................................................................................. 3
1.3 Uses of Salicylic Acid ....................................................................................................... 9
2. Process Selection
2.1 Synthesis of Salicylic Acid ........................................................................................ 10
2.1.1 First Synthesis .................................................................................................... 10
2.1.2 KOLB Process .................................................................................................... 10
2.1.3 SCHMITT Modification ..................................................................................... 10
2.1.3 More, et al ........................................................................................................... 11
2.1.4 Stopp,et al ........................................................................................................... 11
2.1.4 Barkley et al ........................................................................................................ 11
2.1.5 Jenson, et at ........................................................................................................ 11
2.2 Process Flow Sheet Description ................................................................................ 13
2.2.1 Preparation of Sodium Phenolate ....................................................................... 13
2.2.2 Preparation of Sodium salicylate ........................................................................ 13
2.2.3 Acidification tank ............................................................................................... 13
2.2.4 Purification from water (removal of water) ........................................................ 14
2.2.5 Sublimation and crystallization .......................................................................... 14
3. Material Balance
3.1 Material Balance 15
3.1.1 Material balance around CSTR (R-1): .................................................................. 17
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3.1.2 Material balance around flash tank (FT-1) ............................................................ 19
3.1.3 Material balance around autoclave(R-2) ............................................................... 21
3.1.4 Material balance around distillation column (DC-1) ............................................ 23
3.1.5 Material balance around dilution tank (M-1) ........................................................ 24
3.1.6 Material balance around Acidification tank(R-3) ................................................. 25
3.1.7 Material balance around centrifuge (FF-1) ........................................................... 27
3.1.8 Material balance around dryer (DE-1) .................................................................. 28
3.1.9 Material balance around sublimation tank (SB-1) ................................................ 29
3.1.10 Material balance around Crystallizer (C-1) .......................................................... 30
3.1.11 Overall material balance....................................................................................... 31
4. Energy Balance
4.1 Energy Balance .................................................................................................................. 32
4.1.1 Energy balance around CSTR (R-1) ..................................................................... 32
4.1.2 Energy balance around flash tank (FT-1) .............................................................. 34
4.1.3 Energy balance around Compressor (JC) .............................................................. 35
4.1.4 Energy balance around autoclave (R-2) ................................................................ 37
4.1.5 Energy balance on Distillation column (DC-1)..................................................... 39
4.2.6 Energy balance on dilution tank (M-1) ................................................................. 41
4.1.7 Energy balance around Acidification tank (R-3) .................................................. 42
4.1.8 Energy balance around Dryer (DE-1) .................................................................... 44
3.1.9 Energy balance around Sublimation unit (SB-1) .................................................. 46
5. Design of Equipment
5.1 Design of chemical reactor .............................................................................................. 47
5.1.1 Design of CSTR (Continuous Stirred-Tank Reactor) ............................................ 52
5.2 Design of Flash tank .................................................................................................. 65
5.2.1 Design calculation steps ......................................................................................... 67
5.3 Design of Autoclve Reactor (R-2) .................................................................................... 74
5.3.1 Design Calculations................................................................................................ 75
5.4 Design of distillation column ........................................................................................... 81
5.4.2 Designing steps of Distillation column .................................................................. 83
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5.5 Design of dilution tank ..................................................................................................... 99
5.5.1 Dilution Tank ......................................................................................................... 99
5.6 Design of Acidification tank ......................................................................................... 105
5.6.1 Design of Acidification Tank ........................................................................... 105
5.7 Design of Centrifuge ..................................................................................................... 110
5.7.1 Design of Centrifuge ........................................................................................ 110
5.7.2 Design calculation ............................................................................................ 111
5.8 Design of Dryer ............................................................................................................. 117
5.8.1 Drying Operation .............................................................................................. 117
5.8.2 Design steps for Dryer:..................................................................................... 122
5.9 Design of Sublimation tank ........................................................................................... 129
5.9.1 Sublimation tank ............................................................................................... 129
6.Instrumentation &Control
6.1 Instruments ..................................................................................................................... 143
6.2 Instrumentation and Control Objective ......................................................................... 143
6.3 Components of Control System..................................................................................... 144
6.5 Modes of Control ............................................................................................................ 145
6.6 Alarms and Safety Trips and Interlocks ......................................................................... 145
6.7 Different types of Controller .......................................................................................... 146
6.8 Control Scheme of CSTR ............................................................................................... 147
7.HAZOP Study
7.1 Introduction ................................................................................................................... 146
7.2 P&IDS 147
7.3 Responsibility of HAZOP team Member 147
8 Potential Health Effect

8.1 Emergency Overview ..................................................................................................... 156
8.2 First Aid Measures ......................................................................................................... 156
8.3 Fire Fighting Measures ................................................................................................... 157
8.4 Accidental Release Measures ......................................................................................... 157
8.5 Exposure Control and Personal Protection ..................................................................... 157
viii
8.6 Disposal and Considerations .......................................................................................... 158
8.7 Toxicological Information ............................................................................................... 158
9. Cost Estimation
9.1 Purchase Equipment Cost ................................................................................................. 159
9.2 Fixed Capital Investment ................................................................................................ 163
9.3 Total Capital Investment ................................................................................................ 163
9.4 Annual Production Costs ................................................................................................ 164
9.5 Rate Of Return 165
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NOMENCLATURE
A Heat transfer area (m2)
Aa Active area (m2)
Ah Area of hole
AT Tower area (m2)
B Baffle spacing (m)
Cp Specific heat (Btu/lb-F)
ho Outside fluid film coefficient (Kwatt/m2-C)
hi Inside fluid film coefficient (Kwatt/m2-C)
k Thermal conductivity (Kwatt/h-m-C)
L Liquid flow rate (kg-mol/h)
LMTD Log mean temperature difference (C)
Pl Liquid density (kg/m3)
U Overall heat transfer coefficient (kwatt/h-m-C)
Latent heat (kJ/Kg)
Cs Stress concentration factor for torispherical heads
RC Crown radius
Rk Knuckle radius
Di Internal diameter of tank = 1.148 m

Do External diameter of tank
x
Chapter # 01 Introduction
CHAPTER
1
Introduction
1.1 Introduction
Salicylic acid is also called 2-hydroxybenzoic acid or o-hydroxybenzoic acid, and is
widely distributed in the plant kingdom in the form of esters.
Where the hydroxy is ortho, meta,or para are commonly known as the
monohydroxybenzoic acids. Of the three acids, the ortho isomer, salicylic acid, is by far the
most important. The main importance of salicylic acid and its derivatives lies in their
antipyretic and analgesic actions (see Analgesics, antipyretics, and anti-inflammatory agents).
Natural salicylic acid, which exists mainly as the glucosides of methyl salicylate and salicyl
alcohol , is widely distributed in the roots, bark, leaves, and fruits of various plants and trees.
As such, their use as preparations for ancient remedies is probably as old as herbal therapy.
Hippocrates recommended the juice of poplar trees as treatment for eye diseases. Salicyl
alcohol glucosides (salicin) occur in Populous halsamifera (poplar) and Snlix helix (willow)
trees. Methyl salicylate glucosides occur in Betula (birch) and Togas (beech) trees.
Free salicylic acid occurs in nature only in very small amounts. It baa been isolated
from the roots, plants, blossoms, and fruit of Spirctea ulmaria, from which its original name,
aecidium spiricum, was derived. Salicylic acid as well as salicylates occur in tulips, hyacinths,
and violets, and in common fruits, eg, oranges, apples, plums, and grapes, which explains the
presence of salicylic acid in most wines.
Some 2400 years ago Hippocrates prescribed decoctions of willow leaves as a

treatment for fever and pain. The active principle in willow leaves is salicylic acid, whose
biosynthesis is based on the deamination of phenylalanine to trans- cinnamic acid which,
when hydrolyzed and oxidized at the - carbon atom, gives salicylic acid.
Salicylate esters are found in several plant genera, the principal ones being Salix,
Spiraea, and Gaultheria. For example, methyl salicylate is present in large quantity in the form
of a glucoside in birch bark, various spiraeas (meadowsweet or Spiraea ulmaria), and
wintergreen leaves.Salicylic acid was first obtained in 1838 by R.Piria, an Italian chemist at
the Instituteof Pisa, by melting salicylaldehyde, obtained from meadowsweet, with caustic
potash. In 1844 the French chemist
1
Cahours obtained salicylic acid by hydrolysis of methyl salicylate. The final step namely
preparation from a natural source, was accomplished in 1874 by the German chemist
H.Kolbe, who synthesized the acid by carboxylation of sodium peroxide, a process still in use.
1.2 Properties of Salicylic Acid

1.2.1 Physical Properties
Salicylic acid is obtained as white crystals, fine needles, or fluffy white crystalline
powder. It is stable in air and may discolour gradually in sunlight. The synthetic form is white
and odourless. When prepared from natural methyl salicylate, it may have a lightly yellow or
pink tint and a faint, wintergreen like odor. Hydroxybenzoic acid crystallizes from water in
the form of white needles and from alcohol as platelets or rhombic prisms. P-Hydroxybenzoic
acid crystallizes in the form of monoclinic prisms. Various physical properties of
hydroxybenzoic acids are listed in
Table-1.1 Physical Properties of Hydroxybenzoic acid
Value (Isomer)
Property
Ortho Meta Para
Molecular weight 138.12 138.12 138.12
Melting point, oC 159 20L5-203 214.5 215.6
Boiling point, oC 211 swub
Density 1.44333
4
1.473 22
29 1.497 29
20
Flash point (Tag closed-cup), oC 1.57
Ka (acid dissociation) at 25oC 1.05 8.310-5 2.610-5
Heat of combustion, mJ/molo 3.026 3.038 3.035
Heat of sublimation, kJ/molo 95.14 116.1
2
Table-1.2 Solubilitys of the Hydroxybenzoic Acids in Water, Wt %

Temperature, oC Isomer
Ortho Meta Para
0 0.12 0.35 0.25
10 0.14 0.55 0.50
20 0.20 0.85 0.81
30 0.30 1.35 0.81
40 0.42 2.0 1.23
50 0.64 3.0 2.3
60 0.90 4.3 4.2
70 1.37 7.0 7.0
80 2.21 11.0 12.0
1.2.2 Chemical Properties

The hydroxybenzoic acids have both the hydroxyl and the carboxyl moieties and,
as such, participate in chemical reactions characteristic of each. In addition, they can undergo
electrophilic ring substitution. Reactions characteristic of the carboxyl group include
decarboxylation; reduction to alcohols; and the formation of salts, acyl halides, amides, and
esters. Reactions characteristic of the phenolic hydroxyl group include the formation of salts,
esters, and ethers. Reactions involving form sodium salicylate. However, if salicylic acid
dissolves in the presence of alkali metals or caustic alkalies, e.g., excess sodium hydroxide,
the disodium salt forms. The hydroxybenzoic acids have both the hydroxyl and the carboxyl
moieties and, as such, participate in chemical reactions characteristic of each. In addition, they
can undergo electrophilic ring substitution. Reactions characteristic of the carboxyl group
include decarboxylation; reduction to alcohols; and the formation of salts, acyl halides,
amides, and esters. Reactions characteristic of the phenolic hydroxyl group include the
formation of salts, esters, and ethers. Reactions involving form sodium salicylate. However, if
salicylic acid dissolves in the presence of alkali metals or caustic alkalies, e.g., excess sodium
hydroxide, the disodium salt forms.
3
Reactions of the carboxyl group of salicylic acid
Salicylic acid can be converted to salicyloyl chloride by reaction with thionyl chloride in
boiling benzene. However, the formation of acyl halides can be complicated by the presence
of the phenolic hydroxyl. For example, the reaction with phosphorus to arid pent chlorides is
not restricted to the formation of the acid chloride. Further interaction of the phosphorus
halide and the phenolic hydroxyl results in the formation of the phosphoric or phosphorous
esters.The formation of amides can be accomplished by the dehydration of the ammonium salt
of salicylic acid. The more common method for amides is the reaction of the ester, acylhalide,
or anhydride with an amine or ammonia. Each step is fast .Esterification is frequently carried
out by direct reaction of the carboxylic acid with an alcohol in the presence of a small amount
of mineral acid, usually concentrated sulphuric or hydrochloric acid. The ester of commercial
importance is methyl salicylate. Direct esterification has the advantage of being a single-step
synthesis; its disadvantage is the reversibility of the reaction. The equilibrium can be shifted
to the right if either raw material is used in large excess, or by selective removal of one of the
products. One less frequently employed technique is the transformation of the acid to the acid
chloride followed by alcoholises; each step is essentially irreversible. Another method is the
reaction of the alkali salt, eg, sodium salicylate, with an alkyl or an aryl alkyl halide.
4
Table-1.3 Solubilities of the Hydroxybenzoic Acids in Non-aqueous Solvents, Wt %

Isomer
Solvent Ortho Meta Para
Acetone at 23oC 396 327 285
Benzene at 25 oC 0.775 0.010 0.0035
1-butanol 28.838c C 20.7 36.5c C 19.5 22.5c C
Ethanol (99 wt %) 40.6 41c C 3.9.6 65c C 38.7567c C
n-heptane 2.0992.2c C 2.0197c C 1.5197c C
Methanol at 15 oC 39.87 40.38 36.22
Carbon tetrachloride at 25 oC 0.262
Chloroform (satd in H2O) at 1.84

25 oC
Carboxyl. Typical decarboxylation by simple heating of a free acid occurs with only a few
types of acids. However, decarboxylation of salicylic acid takes place readily because of the
presence of the hydroxyl group, which is electron donating . Upon slow heating, salicylic acid
decomposes to phenol and carbon dioxide; when heated rapidly, it sublimes.
Generally, the carboxyl group is not readily reduced. Lithium aluminum hydride is one of the
few reagents that can reduce an acid to an alcohol. The scheme involves the formation of an
alkoxide, which is hydrolyzed to the alcohol. Commercially, the alternative to direct reduction
involves esterification of the acid followed by reduction of the ester.
Salicylic acid dissolves in aqueous sodium carbonate or bicarbonate to serve. However,
phenolate ions are ambident , as such and under certain conditions, as with the use of alkyl
halides, the problem of C- versus O-alkylation can occur. Either reaction can be made
essentially exclusive by the proper choice of reaction conditions. For example, polar solvents
favor formation of the ether, whereas nonpolar solvents favor ring substitution (see
Alkylation). Esters of the phenolic hydroxyl are obtained easily by the Schotten-Baumann
reaction. The reaction in many cases involves an acid chloride as the acylating agent.
However, acylation can also be achieved by reaction with an acid anhydride. The single most
important commercial reaction of this type is the acetylation of salicylic acid with acetic
anhydride to yield acetylsalicylic acid (aspirin).
5
Reactions of the hydroxyl group of salicylic acid.

Ring Substitution. In the introduction of a third group into a disnbstituted benzene, the
position the group takes depends on the groups present. In the case of salicylic acid the
hvdroxyl directs ortho and pan and the carboxyl directs meta substitution. It is generally
accepted that if both an ortho-para and a meta director are competing for the orientation of a
third group, the ortho-para director prevails since, unlike the meta director, it activates the
ring. Specifically, the hydroxyl group is electron-donating which, on the basis of resonance
considerations, increases the Electron density in the S and 5 positions. The electron-
withdrawal nature of the car-boxyl group decreases the electron density around the 4 and C
positions, which further enhances the electron density of the 3 and 5 positions. As a rule,
direct substitution occurs more easily in the less sterically hindered 5 position, but most often
small amounts of the 3 substituted and 3,5-disubstituted product also form. High yields of the
3-substituted salicylic acid usually can only be prepared indirectly.
Ring-substitution reactions of salicylic acid. X = halogen.
6
Direct halogenation of salicylic acid is generally carried out in glacial acetic acid. As
expected, the main product is the 5-halo-salicylic acid with small quantities of the 3-halo- and
3, 5-dihalosalicylic acids
Reaction with cold nitric acid results primarily in the formation of 5-nitrosalicylic acid .
However, reaction with fuming nitric acid results in decarboxylation as well as the formation
of 2, 4, C-trinitrophenol (picric acid). Sulfonation with chlorosulfonic acid at 16OoC yields 5-
sulfosalicylic acid . At higher temperatures (1800 oC) and with an excess of chlorosulfonic
acid, 3,5-disulfosalicylic acid forms. Sulfonation with liquid sulfur trioxide in
tetrachloroethylene leads to a nearly quantitative yield of 5-sulfosalicylic acid.
Because salicylic acid contains the deactivating meta-directing carboxyl group, Friedel-Crafts
reactions (qv) are generally inhibited. This effect is somewhat offset by the presence of the
activating hydroxyl group. Salicylic acid also reacts with isobutyl or t-butyl alcohol in 80%
sulfuric acid at 750C to yield 5-t-butylsalicylic acid. In the case of isobutyl alcohol, the
intermediate carbonium ion rearranges to (CH3)3C+.
The Reimer-Tiemann reaction of salicylic acid with chloroform and alkali results in the 3- and
5-formyl derivatives.
If the reaction is carried out with carbon tetrachloride, the corresponding dicarboxylic acids
form. Alkylation involving formaldehyde in the presence of hydrogen chloride is known as
chloromethylation. The reagent may be a mixture of formalin and hydrochloric acid,
paraformaldehyde and hydrochloric acid, a chloromethyl ether, or a formal. Zinc chloride is
commonly employed as a catalyst, although many others can be used. Chloromethylation of
salicylic acid yields primarily the 5-ubstituted product.
The reaction of salicylic acid with formaldehyde with catalytic amounts of acid results in the
condensation product methylene-5, 5-disalicylic acid.
7
Salicylic acid, upon reaction with amyl alcohol and sodium, reduces to a ring-opened aliphatic
dicarboxylic acid, ie, pimelic acid. The reaction proceeds through the intermediate
cyclohexanone-2-carboxylic acid.
During certain substitution reactions, the carboxyl group is often replaced by the entering
group. Au example is fuming nitric acid, which results in the formation of trinitrophenol.
Another is the bromination of salicylic acid in aqueous solution to yield the tribromophenol
derivative
Salicylic acid couples with diazonium salts in the expected manner. With diazotized aniline,
i.e, benzenediazonium chloride, the primary product is 5-phenylazosalicylic acid .
The close proximity of the carboxyl and the hydroxyl groups can be used for beterocyclic
synthesis, as in the preparation of hydroxyxanthones
8
1.3 Uses of Salicylic Acid

Approximately 60% of the salicylic acid produced in the United States is consumed
in the manufacture of aspirin: this statistic has remained relatively constant for at least the last
ten years. Approximately 10% of the salicylic acid produced is consumed in various
applications, eg, foundry and phenolic resins, rubber retarders, dyestuffs, and other
miscellaneous uses. The remaining 30% is used in the manufacture of its salts and esters for a
variety of applications.
There are many foundry-resin systems in use. Salicylic acid is a small component
only in the Shell process. It is used as a cross-linking agent in the phenol fornrnldehyde resin
used as a sand core and mold binder and imparts higher tensile strength. More recent
developments have demonstrated that higher concentrations of salicylic acid than previously
used further improve cold and hot tensile strength and reduce cure and machine processing
time.
The continuing interest in energy and environmental considerations has led to the
low energy processes, which typically do not use salicylic acid. Their growth has been
somewhat limited because of the large capital expenditures required; however, the economics
is expected to shift as the cost of energy increases. Therefore, a zero or small negative growth
for salicylic acid is predicted in foundry-resin applications. Salicylic acid has also been used
in other phenolic resin applications, ie, binders for grinding wheels, fiber glass, and brake
linings.
Salicylic acid is used mainly in the synthesis of acetylsalicylic acid, the most
commonly dispensed pharmaceutical product. In the form of esters, amides, and salicylic acid
salts it serves as a starting material for other pharmaceutical products. Technical-grade
salicylic acid is used primarily as an intermediate in the production of agrochemical products,
dyes, and colorants, as well as in the rubber industry and in the manufacture of phenolic
resins.
Salicylic acid itself offers therapeutic benefits in the treatment of rheumatic
disorders, for which purpose it is usually administered in the form of the readily soluble
sodium salt. On account of its keratolytic action the acid is also widely used for cleaning the
skin.
9
Chapter # 02 Process Selection
CHAPTER
2
Process Selection
2.1 Synthesis of Salicylic Acid

2.1.1 First Synthesis
Salicylic acid was first prepared by R.Piria by the fusion of salicyaldehide with the
potassium hydroxide. In 1859, a synthesis method of preparing salicylic acid was discovered
by treating the phenol with carbon dioxide in presence of metallic sodium. However the only
commercial method of manufacturing salicylic acid until 1874 was the saponification of the
methyl salicylate obtained from the leaves of the winter green or Bark of the birch.
2.1.2 KOLB Process

The first technically suitable process was introduced in 1874 by Kolb. It involves the
reaction of the dry sodium phenolate with carbon dioxide under pressure and high temperature
(180-200) 0C. The drawback of the process was that the yield was not more than 50% and the
separation of by products which were in large quantity was difficult. Salicylic acid is
manufactured by the reaction of phenol with caustic soda and the subsequent treatment of the
sodium phenolate formed with carbon dioxide and acidifying the resultant product with the
sulfuric acid .Phenol and caustic soda are charged in equal molar proportions to a mixer. The
resulting solution is heated to a temperature of 1300C and further evaporated to dryness in a
stirred autoclave or a heated ball mill. Dry carbon dioxide gas is absorbed and the crude
product from the autoclave is dissolved in the equal amount of water and filtered. The filtrate
is precipitated and dried. To obtain pure product, the crude sodium salicylate solution
decolorized with the activated carbon containing the zinc dust and filtered. The clarified
filtrate is acidified with the excess of sulfuric acid to precipitate the salicylic acid which is
centrifuged and dried to give the high grade salicylic acid.
2.1.3 SCHMITT Modification

Schmitt introduced the new lower temperature ranges from 120-1400C which
significantly increased the yield of the process. The reaction of the carbon dioxide on the
phenol forms an intermediate phenyl carbonate which rearranges itself to give o-sodium
salicylate. The Kolb-Schmitt synthesis method is still the only industrial process in use in
different modifications.
10
2.1.3 More, et al
More introduced a new step process for the carbonation of dry sodium phenolate. The
reaction is carried out in a stirred reactor. Carbon dioxide is passed at a temperature of 1300C
until 25% of the stoichiometric amount of the carbon dioxide is absorbed. In step 11 the
temperature of the raised to 2100C and the remaining carbon dioxide is introduced into the
reactor for 5 hr. the yield of the process was 80 to 82% and for time duration the yield was
76%.
2.1.4 Stopp,et al
The carbonation of the sodium salicylate is carried out in a fluidized bed reactor at
0
140 C and pressure of 6bar until half of the phenolate is converted to salicylate. The resulting
reaction mixture can be further carbonated in a subsequent stage at a temperature of 2100Cand
a pressure of 10 bars. The subsequent stage may be fluidized bed reactor or stirred vessel. The
yield was 85%.
2.1.4 Barkley et al
The sodium phenolate was cooled to 900C. The carbon dioxide was passed into the
autoclave; the temperature was maintained at 1200C until the carbon dioxide adsorption was
come to an end. The temperature was raised to induced rearrangement of the intermediate
product. The temperature was kept 160-1700Cunder a carbon dioxide pressure 5 bar.
2.1.5 Jenson, et at
An improved method for the production of salicylic acid from phenol with high degree
of conversion and with a significant reduction in the by-products was modified by Jenson and
his colleagues. The process comprises of reaction of sodium phenolate with the carbon
dioxide indirect single step at a temperature above 1650C.In the Kolb carboxylation, the
reaction between sodium phenolate with carbon dioxide could advantageously takes place in
single step well the temperature at which sodium phenyl carbonate is ordinarily converted to
sodium salicylate. More particularly instead of introducing carbon dioxide below 150 0C to
produce sodium phenyl carbonate which is then in second step is converted to sodium
salicylate being held above 1650C
11
TT-1 NaOH Phenol TT-2 E-1
Water Water
20
1 2
R-1
Waste water
100 C 4 23
125 C J-5
1atm 3
DC-1
FT-1 22
9 ER-1
21
M-1
95 C
5 TT-6
70 C J-4
JC-1 6 4.93atm 125 C

10
11
TT-3
Sulphuric acid
TT-5 R-2 1 atm Water
TT-5 7 CO2
J-1
4.93atm
R-3
Carbon Dioxide Pure Water
100 C TT-4
18
DE-1 12 20 C
CO2
16 FF-1
C-1 SB-1
70 C
14 J-3
20 C
13
15
17 Sodium Sulphate
19 Salicylic Acid
20 C Waste water treatment
TT-1 NaOH Storage tank TT-2 Phenol storage tank R-1 CSTR FT-1 Flash tank M-1,2 Dilution tank R-3 Acidification tank
FF-1 Centrifuge DE-1 Dryer SB-1 Sublimation tan C-1 Crystallizer DC distillation TT-3 H2SO4 storage tank
TT-4 Water storage tank JC-1 Compressor J-1,2,3,4,5 Pumps R-2 Autoclave E-1,2 Condenser
Figure-2.1 Process Flow sheet of the Production of salicylic Acid
12
2.2 Process Flow Sheet Description

The reactions involve in the process
C6H5OH + NaOH C6H5ONa + H20
C6H5ONa + CO2 C6H4 (OH) (COONa)
C6H4 (OH) (COONa) + 1/2H2SO4 C6H4 (OH) (COOH) + 1/2Na2S04
2.2.1 Preparation of Sodium Phenolate

Phenol is approximately 60% is reacted with 50%caustic soda in a CSTR. The
reaction temperature is 1000C. The reaction is exothermic; heat evolved from the reaction is
absorbed by cooling jacket to make the process isothermal. Slightly excess amount of phenol
is fed into the reactor instead of caustic soda because of material of construction is greatly
influenced by the strong alkali. The reaction temperature is so high that lump formation of
sodium phenolate is not take place.
2.2.2 Preparation of Sodium salicylate

The product of the first reactor is fed into the flash tank where separation of water is
carries out. Phase separation is carried out in flash tank under low pressure and high
temperature. Then for any batch valve is opened and autoclave is charged and valve of the
carbon dioxide is opened at the pressure of 2 bars for the time of 5-6hrs. The reaction
temperature is raised to about 1250C. Autoclave is our second reactor of the process.
Almost 70% conversion is achieved; carbon dioxide released is recycled back and then
utilized. This mixture is vaporized leaving the thick slurry of sodium salicylate. The
evaporated material is condensed and sent into the continuous distillation column where
separation of phenol and sodium phenate is carried out. The product of reaction take from the
bottom and sent to the acidification tank.
2.2.3 Acidification tank

This is our third reactor of the process. The product of the autoclave is thick slurry and
it is diluted with the water in the dilution tank. The solution, so obtained is charged into the
acidification tank where 40% sulfuric acid is reacted that comes from the storage tank of
sulfuric acid. In the acidification tank solid salicylic acid as well as sodium sulfate is formed.
The reaction temperature should be 20C as it gives the maximum conversion. Reaction is
exothermic while temperature is controlled by cooling jacket.
13
2.2.4 Purification from water (removal of water)

Removal of water is carried in two steps: in first step centrifuge removes the large
amount of water i.e. from 16 to 66 % water content. The waste water is sent to the waste
water treatment plant. The solid product that contains salicylic acid and sodium sulfate is sent
to the dryer where almost all water content is removed. Water in some traces amount might be
present in our desired product.
2.2.5 Sublimation and crystallization

The solid product is charged into the sublimation tank where steam is used as heating
medium and vacuum is created with the help of vacuum pump At reduced pressure the
sublimation of salicylic acid is carried out at 1000C. The vapors coming from the sublimation
tank are injected into crystallizer where condensation of vapors takes place resulting more
than 99% pure product.
14
Chapter # 03 Material Balance
CHAPTER
3
Material Balance
3.1 Material Balance

Assumptions
1. One Hour Operation i.e. 35 tons per hour Salicylic acid.

2. Conversion in the Reactor is 99%
Reactions involves in the process
1. C6H5OH+NaOH C6H5ONa+H2O
2. C6H5ONa +CO2 C6H4 (OH) (COONa)
3. C6H4 (OH) (COONa) +1/2H2SO4 C6H4 (OH) (COOH) +1/2Na2SO4
From reaction-3
1443 kg C6H4 (OH) (COOH) 1 kg mole C6H4 (OH) (COONa)
138 kg C6H4 (OH) (COOH)
10.47kg mole 0.99
=10.357kgmole C6H4 (OH) (COONa)

or
=1429.321kg/hC6H4 (OH) (COONa)
1429kg C6H4 (OH) (COOH) 0.5kgmole H2SO4 98kg H2SO4
1kgC6H4 (OH) (COOH) 1kg mole H2SO4
=507.505kg/h H2SO4
1429 kg C6H4 (OH) (COOH) 0.5kg mole Na2SO4 142kg Na2SO4

1kg C6H4 (OH) (COOH) 142kg mole Na2SO4
=735.37kg/h Na2SO4
15
From reaction-2
10.357kgmole C6H4 (OH) (COONa) 116kg C6H5ONa
1kgmole C6H4 (OH) (COONa) 0.7
=1716.35kg/h C6H5ONa
or
=14.79kgmole C6H5ONa
10.357kgmole C6H4 (OH) (COONa) 44kg CO2
1kgmole C6H4 (OH) (COONa) 0.7
=657.68kg/hrCO2
From reaction-1
14.79kgmole C6H5ONa 40kg NaOH
1kgmole C6H5ONa 0.99
=597.82kg/hr NaOH
10.357kgmole C6H5ONa 94kg C6H5OH
1kgmole C6H5ONa
=1685.87kg/hr C6H5OH
16
3.1.1 Material balance around CSTR (R-1)
R-1
3
1
C6H5OH+NaOH C6H5ONa+H2O
Steam description
Steam 1 = Raw material
Steam 2 = Raw material
Steam 3 = Product
Apply the material balance equation;
Input - Output + Generation - Consumption = Accumulation (1)
Steady state, accumulation = 0
Then
Input - Output = Generation Consumption... (2)
17
Limiting reactant is NaOH.
14.95kgmole of NaOH 0.995*40=597.84kg of NaOH is in execs
So 14.94-14.87=2.99 kg of NaOH is going out at stream 3
Phenol added 1685.87kg, which is 60%, and also 40% water added which is 1123.98 kg
stream 2.
Consumption of phenol=1685.87 0.995= 1397.8kg of phenol is consume in the reaction.
Generation of water = 597.87*0.99+1123.98+597.87=1989.48kg, at stream 3.
Putting all valves in the Eq-2.we get
4026.3kg=4026.3kg
Table-3.1.1 Material balance around CSTR (R-1)

Input Output
Components 1(kg/h) 2(kg/h) 3(kg/h)
C6H5OH - 1685.87 287.99
NaOH 597.8 - 2.99
H2O 597.8 1123.98 1989.48
C6H5ONa - - 1745.95
Total 4026.3 4026.3
18
3.1.2 Material balance around flash tank (FT-1)
FT-1
5
Steam description
Steam 3 = vapor liquid mixture, Feed
Steam 4 = Vapor product
Steam 5 = liquid product
By using raoults law equation:
p
k= (1)
p

xi = v (2)
1 + (k i 1)
f
yi = k i xi (3)
Where P=25kpa,
(P*) C6H5OH =3.51
(P*) H2O= 101.33
(P*) C6H5ONa= 2.07
19
(K) C6H5OH = 0.1404
(K) H2O = 4.053
(K) C6H5ONa=0.0828
Lets start with assume, v/f=0.1, putting valves in the below equation to get
( 1)
=0 (4)
(1 + ( 1)

So we assume the valve of V/F, must be b/w 0 and 1.so at V/F=0.01, the equation-4 is
satisfied.
x C6H5OH = 0.98 and also Y C6H5OH = 0.02
x H2O = 0.02 Y H2O = 0.98
Top product =1954.65 kg, and
Bottom product = 2070.95 kg
Input - Output + Generation - Consumption = Accumulation
The reduced to;
Input = Output
Feed = Top product +bottom product
4026.41 = 1954.65 + 2070.95
4026.41 kg = 4026.41 kg
Table 3.1.2 Material balance around flash tank (FT-1)

Components Input Output
3(kg) 4(kg) 5(kg)
C6H5OH 287.98 5.75 282.22
NaOH 2.99 - 2.99
H2O 1989.48 1949.69 39.78
C6H5ONa 1745.95 - 1745.95
Total 4026.41 4026.41
20
3.1.3 Material balance around autoclave(R-2)
22 8
R-2
5
23
C6H5ONa +CO2 C6H4 (OH) (COONa)
70% Conversion
Steam description:
Steam 5 = Feed
Steam 6 = carbon dioxide addition
Steam 7 = Product
Steam 8 = vapor mixture
Steam 22 =Recycle From distillation column
Steam 23 = Carbon dioxide remove
The process stream from the flash tank is entering to autoclave. While the side stream 6
containing CO2 is also fed. 70% of CO2 is removed as a side stream and 30% is reacted with
C6H5ONa to form C7H5NaO3.
0.7 1745.95=1223.16kg
1223.16-657.60=564.56kg.
Input - Output + Generation - Consumption = Accumulation-------Eq-1
21
Then
Input - Output = Generation Consumption
2728.57= 2728.57 kg
Table-3.1.3 Material balance around autoclave(R-2)

5(kg) 6(kg) 22(kg) 7(kg) 8(kg) 23(kg)
C6H5OH 282.22 - 17.64 17.64 282.22 -
C7H5NaO3 - - - 1692.78 - -
CO2 - 657.60 - - - 455.72
NaOH 2.98 - - 2.98 - -
H2O 39.78 - - 39.78 - -
C6H5ONa 1745.95 - 513.30 523.78 523.78 -
2070.91 657.6 530.94 2541.54
Total 2728.57 2728.57
22
3.1.4 Material balance around distillation column (DC-1)
20
DC-1
Stream description
Steam 8 = Feed 22
Steam 20 =Top product
Steam 22 =Bottom Product
Top product
C2H5OH = 98%
H2O = 2%
Bottom product
C2H5OH = 3%
C6H5ONa = 97%
Overall material balance
F= D+W
C6H5OH balance
0.35 (1406.01) = 0.98 D + 0.02 (W)
Distillate product =875.06 kg
Bottom product = 530.9 kg
23
Table-3.1.4 Material balance around distillation column (DC-1)

8(kg) 20(kg) 22(kg)
C6H5OH 882.22 864.58 17.64
C6H5ONa 523.78 10.47 513.31
875.05 530.9
Total 1406.01 1406.01
3.1.5 Material balance around dilution tank (M-1)
M-1
Steam description
10
Steam 7 = Feed
Steam 9 = Addition of water
Steam 10 = product
For the dilution we added, we added water double of the feed.
2 1763.64=3527.29kg
3527.29 kg of water
24
Table-3.1.5 Material balance around dilution tank (M-1)

7(kg) 9(kg) 10(kg)
C6H5OH 17.64 - 17.64
C7H5NaO3 1692.78 - 1692.78
NaOH 2.98 - 2.98
H2O 39.78 3527.29 3567.0
C6H5ONa 523.78 - 523.78
2541.54 3527.29
Total 5290 5290
3.1.6 Material balance around Acidification tank(R-3)
11
R-3
10
12
1 99% 1
C6 H4 (OH)(COONa) + H2 SO4 C6 H4 (OH)(COOH) + Na2 SO4
2 2
Reaction Conversion 99.9%
Steam description
Steam 10 = Feed
Steam 11 = raw material added
Steam 12 = Product
25
For the preparation of salicylic acid added, 40% sulfuric acid through stream 11 to
acidification tank and 60% water to the acidification tank at steam 11.
Salicylic acid produced = 1443.75 kg
Sulfuric acid added= 507.50 kg
Water added =761.25 kg
Sodium sulfate produced = 751.15 kg
Input - Output + Generation - Consumption = Accumulation-------Eq-1
Input - Output = Generation Consumption-----------------------Eq-2
6557.76 kg = 6557.76 kg
Table-3.1.6 Material balance around Acidification tank(R-3)

10(kg) 11(kg) 12(kg)
C6H5OH 17.64 - 17.64
C7H5NaO3 1692.78 - -
NaOH 2.98 - -
H2O 3567.0 760.26 4328.35
C6H5ONa 523.78 - 10.47
H2SO4 - 507.5 -
Na2SO4 - - 751.15
Salicylic acid - - 1443.75
5290 1267.76
Total 6557.76 6551.36
26
3.1.7 Material balance around centrifuge (FF-1)
FF-1
12 13
Steam description
Steam 12 = Feed
14
Steam 13 = waste remove
Steam 14 = Desire product
At this unit we remove, 60% of water as a waste steam at steam 13.
Water remove = 0.60*4382 kg =2856.7 Kg
Phenol remove =0.98*17.64 =17.29 Kg
Sodium phenolate remove = 0.98*10.47=10.26 Kg
Table-3.1.7 Material balance around centrifuge (FF-1)

12(kg) 13(kg) 14(kg)
C6H5OH 17.64 0.35 17.29
C7H5NaO3 - - -
NaOH - - -
H2O 4328.35 1471.63 2856.71
C6H5ONa 10.47 0.21 10.26
H2SO4 - -
Na2SO4 751.15 751.15 -
Salicylic acid 1443.75 1443.75 -
3667.09 2884.26
Total
6551.36 6551.35
27
3.1.8 Material balance around dryer (DE-1)
DE-1
14 15
Steam description
16
Steam 1 = Feed
Steam 2 =remove as waste
Steam 2 = product
Water removed = 0.98*1471.63 =1442.20 kg
Phenol removed = 0.02*0.335 =0.07 kg
Sodium phenolate removed =0.02*736.15 =15.013 kg
Table-3.1.8 Material balance around dryer (DE-1)

14(kg) 15(kg) 16(kg)
C6H5OH 0.2 0.07 0.28
C7H5NaO3 - - -
NaOH - - -
H2O 1471.01 1442.2 29.43
C6H5ONa 0.3 0.04 0.16
H2SO4 - - -
Na2SO4 751.95 15.02 736.13
Salicylic acid 1443.75 1443.75
1457.33 2209.75
Total 3667.08 3667.08
28
3.1.9 Material balance around sublimation tank (SB-1)
SB-1
16 17
Steam description
18
Steam 16 = Feed
Steam 17 = waste remove
Steam 18 = Pure product salicylic acid 99.9%
The slurry type mixture is then feed to the sublimation unit through stream 16.In which most
of the Na2SO4 is removed and only in small amount water is remained. The product from
sublimation tank is fed to the crystallizer through stream 18 to purify the salicylic acid up to
99%.In the crystallizer the small amount of water is also removed. The final product from
crystallizer is a crystals form salicylic acid.
Table-3.1-9 Material balance around sublimation tank (SB-1)

16(kg) 17(kg) 18(kg)
C6H5OH 0.28 0.07 -
C7H5NaO3 - - -
NaOH - - -
H2O 29.43 28.61 1.17
C6H5ONa 0.16 0.02 -
H2SO4 - - -
Na2SO4 736.13 736.13 -
Salicylic acid 1443.75 - 1443.75
764.83 1444.92
Total 2209.75 2209.75
29
3.1.10 Material balance around Crystallizer (C-1)
C-1
18 19
Steam description
Steam 18 = Feed
20
Steam 19 = waste
Steam 20 = Product, 99% pure salicylic acid
Table-3.1.10 Material balance around Crystallizer (C-1)

18(kg) 19(kg) 20(kg)
Salicylic acid 1443.75 1443.75 -
H2O 1.17 - 1.17
1443.75 1.17
Total 1444.92 1444.92
30
3.1.11 Overall material balance
Input Out put

NaOH (kg/h) =597.83
Salicylic Acid (kg/h) =1443.75
Phenol (kg/h) =1685.87
Water (kg/h) =6773.99
Water (kg/h) =6010.29 Overall Material Balance
Carbon Dioxide (kg/h) =455.72
Carbon Dioxide (kg/h) =607.57
Sodium Sulphate (kg/h) =736.13
Sulphuric Acid (kg/h) =507.50
597.83
Total input = Total output
9409.06 kg/ h=9409.06 kg/h
31
Chapter # 04 Energy Balance
CHAPTER
4
Energy Balance
4.1 Energy Balance
4.1.1 Energy balance around CSTR (R-1) 100 C

3
Operating Temperature =100C
100 C 100 C
R-1
1 3
Table-4.1.1(a) Calculations at the inlet of reactor

Standard heat = ( + )
Components Molar flow of formation at Cp at 100C
C T
Kj/kgmol.
kgmol KJ/kmol C
C KJ
C6H5OH 17.93 -165 181.3 75 208453.83
NaOH 14.95 -426 78.08 75 69335.09
H2O 95.65 -285 77.4 75 449175.41
Total 726964.68
32
Table-4.1.1(b) Calculations at the outlet of reactor

Mole Out
Components Standard heat of
Cp at 95C T = ( + )
out formation
kgmol KJ/kmol Kj/kgmol. C C kj

C6H5OH 3.6 -165 181.3 75 2268.99
NaOH 0.074 -426 309.1 75 -2.64
H2O 110.52 -285 77.4 75 11235.37
C6H5ONa 14.79 -326 242.3 75 13096.52

Total 30598.238
So the energy balance equation becomes:
Q = Hr = H i Hi
out in
Q = Hr = 696366.7 KJ
33
4.1.2 Energy balance around flash tank (FT-1)

95 C
4
100 C
FT-1
3
95 C
5
Calculation at outlet
Q = latent heat + sensible heat
Q = mh + mCp t
Heat of vaporization of H2O=2551.6 kj/kgmol
Heat of vaporization of C6H5OH=45700 kj/kgmol
Qv = (mh)H2O + (mh)C6H5OH
= (108.31 2551.6) + (0.06 45700)
Hv = 279105.795kj
Energy balance
Hf + Q = Hv + Hl ----------------Eqtn (1)
t
Hl = m Cp
t.ref
Hl = 280915.09kj
Q = 533423.09kj, heat is required for the separation water.
34
4.1.3 Energy balance around Compressor (JC)
Pressure = 1 atm JC-1 Pressure = 4.9 atm

Temperature = 25 C Temperature = 38 C
Inlet volumetric flow rate
Inlet flow rate 14.94 kmol/hr = 0.00398 kmol/s
2
2 = 1 ( )
1
Where
n = 0.0039 kmol/sec
R = 0.0821 m3atm/ kmol K
P = 1atm
T = 298.15 K
V = 0.095 m3/s
Outlet temperature
2
2 = 1 ( )
1
1 = 25
2 = 4.95 atm
1 = 1
1
= ( ) = 0.278
2 = 39
35
Work per kmole

1

W = Z1T1R(1) [((2 ) 1)]
3
By putting values
W= 6106.35 KJ/kg mol
The power required by an adiabatic compressor is calculated from the following equation.
1
0.371 1
=
(1)
[( ) 1]
Ta= 25C
= 1.31
q= 332.12 kg/hr
= 0.85
Pb= 4.95 atm
Pa= 1atm
P=7045.58 Pascal
P=7.045 Kpa
36
4.1.4 Energy balance around autoclave (R-2)
2 8
2
30 C
R-2
5
23
125 C
6
Table-4.1.4(a) Energy balance calculation at inlet

Standard
heat of
Components T
Molar flow formation at Cp at 90C = ( + )
out
C
kgmol Kj/kgmol Kj/kgmol. C C kj

C6H5OH 2.99 -165 181.3 65 34742.3
NaOH 0.07 -426.06 78.08 65 325.43
H2O 2.21 -241.07 77.4 65 10585.73
C6H5ONa 14.8 -326 243.06 65 228998.92
CO2 15.8 -393 39.5 5 -3167.9
Total 25.34 282575.19
37
Table-4.1.4(b) Energy balance calculation at outlet

Standard
heat of
Components Molar flow formation Cp at 125C T = ( + )
out at

C
kgmol Kj/kgmol Kj/kgmol. C C kj

C6H5OH 2.99 -165 183.3 35 18688
NaOH 0.07 -426.06 78.08 35 161.47
H2O 2.21 -241.07 77.4 35 5454.12
C6H5ONa 4.8 - 245.06 35 39605.28
CO2 4.7 -393 38.08 35 4417.06
10.57 -1561.5 257.09 35 111610.21
Total 25.34 179936.14
So the general energy balance equation becomes:
Q = Hr = H i Hi
out in
Q = Hr = 102639.05 KJ
38
4.1.5 Energy balance on Distillation column (DC-1)
183 C
20
125 C
DC-1
198 C
Inlet temperature=125 C
22
Phenol Cp at 125 C =135.6kj/kgmole.C
Sodium phenol Cp at 125 C =280.9kj/kgmole. C
Calculation at inlet
Cp of feed = (0.62 135.6) + (0.37 280.9)
=187.633 kj/kgmol. C
Qf = (mcp T) + (mcp T)
Qf = 2419.5 kj
Cp phenol at outlet (bottom) = 150.9kj/kgmole. C
Cp of Na-phenol=290kj/kgmole.C
Cp of top product =155kj/kgmole.C
QT = (mcp T) + (mcp T)
QT = 2159.51 kj
Cp of Na-phenol = 299kj/kgmole.C
QB = (mcp T) + (mcp T)
39
QB = 2174.02kj
The energy balance,
QF + Steam enthalpy = QT + QB + condensor heat (1)
Steam enthalpy = S 766 kj (2)
condensor heat = mL = (mcp T) (3)
Heat of vapor = 35m (4)
mL
= (5)
cp T
mL
= = 6386.45kg
cp T
The equation become,
QF + S 766 = QT + QB + 2088.45 35
Steam required = 454 kg
40
4.1.6 Energy balance on dilution tank (M-1)
25 C
125 C
M-1
7
T=?
10
Heat balance
1 + 2 = 3
t ref = 25 C
[198.5 77.4 (T-25) + 0.08 243 (100) + 10.5 357.7 (100) + 2.2 (77.03) (100)] =
[(198.17 77.03) + (0.18 18.23) + (0.08 243) + (10.57 257.3) + (0.074 308)] (T-25)
Toutlet = 70 C
41
4.1.7 Energy balance around Acidification tank (R-3)
25 C
11
70 C
R-3
10
20 C
12
1 99% 1
C6 H4 (OH)(COONa) + H2 SO4 6 4 ()() + 2 4
2 2
Table-4.1.7(a) Energy balance calculation at inlet
Standard
heat of
Components Molar flow formation Cp at 125C T = ( + )
outlet at

C
kgmol Kj/kgmol Kj/kgmol. C C

C6H5OH 0.187 - 183.3 45 1511.61
NaOH 0.074 - 78.08 45 228.47
H2O 240.46 - 77.4 45 779554.48
C6H5ONa 0.08 - 245.06 45 856.13
CO2 0 - 38.08 45 0
C6H4 (OH) 10.57 -1561.5 257.09 45 137345.55
(COONa)
H2SO4 5.178 -811.56 137.06 45 27734.09
Total 256.55 947230.33
42
Table-4.1.7(b) Energy balance calculation at outlet

Standard
heat of
Componentsout Molar formation at Cp at T = ( + )

flow C 125C
Kj/kgmol.
kgmol Kj/kgmol C
C
C6H5OH 0.18 - 183.3 50 1649.7
NaOH 0 - 78.08 50 0
H2O 240.46 - 77.4 50 930580.2
C6H5ONa 0.08 - 245.06 50 980.24
CO2 0 - 38.08 50 0
C6H4 (OH) 0.090 -1561.5 257.09 50 1016.37
(COONa)
Na2SO4 5.28 -1384.67 137.29 50 28933.50
C6H4 (OH) 10.46 -589.06 160.9 50 77989.13
(COOH)
Total 256.55 1041148.47
So the general energy balance equation becomes:
Q = Hr = H i Hi
out in
Q = Hr = 93918.08 KJ
43
4.1.8 Energy balance around Dryer (DE-1)
70 C
20 C
DE-1
14 15
70 C
16
Steam is fed through jacket to the dryer at temperature of 145 C
Moisture content in product=0.013
Product temperature=70 C
Specific heat of components at temperature of 70 C
kj
Cp,water = 75
kgmole. C
kj
Cp,S.acid = 160
kgmole. C
kj
Cp,Soduim sulphat 137.29
kgmole. C
kj
Cp,phenol = 150
kgmole. C
kj
Cp,Na phenol = 261
kgmole. C
Q Inlet calculations.
44
H1 = (mcpt) H2O + (mcpt) phenol + (mcpt) Na-phenol + (mcpt) S.acid + (mcpt) Na-sulphate
H1=42708.81kj
Outlet calculations.
H3 = (mcpt) H2O + (mcpt) phenol + (mcpt) Na-phenol\
H3=308873.64kj
H4 = (mcpt) H2O + (mcpt) phenol + (mcpt) Na-phenol + (mcpt) Na-sulphat + (mcpt) S.acid
H4=126113.72kj
Heat balance
H1=H3+H4
42708.81=434987.36
Q=H out H in
Q=392278.55kj
Inlet calculations.
H1 = (mcpt) H2O + (mcpt) phenol + (mcpt) Na-phenol + (mcpt) S.acid + (mcpt) Na-sulphate
H1=42708.81kj
Outlet calculations.
H3 = (mcpt) H2O + (mcpt) phenol + (mcpt) Na-phenol\
H3=308873.64kj
H4 = (mcpt) H2O + (mcpt) phenol + (mcpt) Na-phenol + (mcpt) Na-sulphat + (mcpt) S.acid
H4=126113.72kj
Heat balance
H1=H3+H4
42708.81=434987.36
Q=H out H in
Q=392278.55kj (It is the heat required feed to the dryer as a steam).
45
4.1.9 Energy balance around Sublimation unit (SB-1)
SB-1
17
16
Inlet calculations
H1=126113.72kj
18
H2=10.53 38 100
=39330kj
Hin=165443kj
Outlet calculations
H4 = (mCp t)Na2SO + (mCp t)H2O + (mCp t)C6H5OH + (mCp t)C6H5ONa
H4 = 54087.95kj
H3 = 109722.38kj
Hout = 163810.38kj
Q= 1632.67kj
46
Chapter # 05 Design of Equipment
CHAPTER
5
Design of Equipment
5.1 DESIGN OF CHEMICAL REACTOR (CSTR)
Reactor Selection
Reactor is the heart of a chemical plant. Chemical reactors are the vessels that are
designed for a chemical reaction to occur inside them. The design of a chemical reactor deals
with multiple aspects of chemical engineering. It is the job of a chemical engineer to ensure
that the reaction proceeds with the highest efficiency towards the desired output product,
producing the highest yield of product while requiring the least amount of money to purchase
and operate.
Normal operating expenses include energy input, energy removal, raw material costs,
etc. energy changes can come in the form of heating or cooling, pumping to increase
pressure, frictional pressure loss. However, in searching for the optimum it is not just the cost
of the reactor that must be minimized. Rather, the economics of the overall process must be
considered. With the variety of reactors available, some engineers believe that reactor
classification is not possible. No matter how incomplete a classification may be,
however, the designer needs some guidance, even though there may be some reactor types
that do not fit into any classification. Accordingly, we will classify reactors using the
following criteria:
1. Phases in contact
2. Catalytic or non-catalytic
3. Batch or continuous
Phases in Contact
The first consideration is classifying the reactors according to the phases in contact.
These are:
1. gas-liquid
2. liquid-liquid
3. gas-solid
4. liquid-solid
5. gas-liquid-solid
47
After specifying the phases in contact, the next task is to decide whether to conduct the
reaction in a batch or continuous mode. In the batch mode, the reactants are charged to a
stirred-tank reactor (STR) and allowed to react for a specified time. After completing the
reaction, the reactor is emptied to obtain the products. This operating mode is unsteady
state. Other unsteady-state reactors are:
1. Continuous addition of one or more of the reactants with no product withdrawal, and
2. All the reactants added at the beginning with continuous withdrawal of Product.
At steady-state, reactants flow into and products flow out continuously without a
change in concentration and temperature in the reactor.
Our system is liquid-liquid. So for liquid continuous flow we can use tank Reactor or tubular
counter current reactor. Now we have to select either CSTR or PFR.There are two ideal
models for developing reactor-sizing relationships: the plug flow and the perfectly stirred-tank
models. In the plug-flow model, the reactants flowing through the reactor are continuously
converted into products. During reaction there is no radial variation of concentration, back
mixing or forward mixing. In a perfect STR, the reactants are thoroughly mixed so that
the concentration of all species and temperature are uniform throughout the reactor and
equal to that leaving the reactor.
Table-5.1 Comparison of different reactor
48
CSTR (Continuous Stirred-Tank Reactor)
In a CSTR, one or more fluid reagents are introduced into a tank reactor equipped
with an impeller while the reactor effluent is removed continuously. The impeller stirs
the reagents to ensure proper mixing. The contents of the reactors are completely mixed
so that the complete contents of the reactors are at the same concentration and
temperature as the product stream. Since the reactor is designed for steady state, the flow
rates of the inlet and outlet streams, as well as the reactors conditions, remain
unchanged with time. Simply dividing the volume of the tank by the average volumetric
flow rate through the tank gives the residence time, or the average amount of time a
discrete quantity of reagent spends inside the tank.
In short CSTR has following properties.
1. Mixing of reactants
2. Good temperature control
3. High heat and mass transfer efficiencies
4. Useful for slow reactions requiring large hold up time
5. Uniform composition though out the reactor
Choice of CSTR
A CSTR is proffered usually under the following circumstances:
1. Liquid phase reaction.

2. Low Pressure system.
3. Intense agitation is required.
4. Large residence time.
5. Better To control required.
6. Easy cleaning.
7. Selective considerations may also dictate the use of stirred tank reactor they are
preferred if undesirable side reaction predominate and are useful when one desires to
skip certain concentration and temperature ranges where by product formation may
be excessive.
8. There is a rapid response at the reactor outlet to changes in the reactor feed stream
.This characteristics facilities automation control of the reactor.
9. Because of simplicity of their contraction CSTRS, s cost much less than per unit
volume than tubular reactors.
49
Why I Chose CSTR
Based on the following reasons I preferred CSTR for this process
1. Mixing of the two immiscible liquid reactants phases is necessary for the reaction.
2. High mass and hear transfer efficiency.
3. Reactants are liquid and it is homogenous reaction.
Agitation
Agitation is a mean whereby mixing of phases can be accomplished and by
which mass and heat transfer can be enhanced between phases or with external
surfaces. In its most general sense, the process of mixing is concerned with all
combinations of phases of which the most frequently occurring ones are.
1. Gases with gases
2. Gases with liquids
3. Gases with granular solids
4. Liquids into gases
5. Liquids with granular solids
6. Pastes with each other
7. Solids with solids
The dimensions of the liquid content of a vessel and the dimensions and arrangement
of impellers, baffles and other internals are factors that influence the amount of energy
required for achieving the required amount of agitation or quality of mixing. The internal
arrangements depend on the objectives of the operation: whether it is to maintain the
homogeneity of reacting mixture or to keep a solid suspended or a gas dispersed or to
enhance heat or mass transfer.
The Vessel
A dished bottom requires less power than a flat one. When a single impeller is to be
used, a liquid level equal to the diameter is optimum, with the impeller located at the center
for all liquid systems. Economic and manufacturing consid erations, however often dictate
higher ratios of depth to diameter.
Baffles
Except at very high Reynolds numbers, baffles are needed to prevent vortexing and
rotation of the liquid mass as a whole. A baffle width one-twelfth the tank diameter,
W=D/12; a length extending from one half the impeller diameter, d/2, from the tangent line at
the bottom to the liquid level, but sometimes terminated just above the level of the eye of the
uppermost impeller. When solids are present or when heat transfer jacket is used, the
baffles are offset from the wall a distance equal to one sixth, W/6 the baffles width.
Four radial baffles at equal spacing are standard; six are only slightly more effective, and
three appreciably less so.
50
Draft Tubes
A draft tube is a cylindrical housing around and slightly larger in diameter than the
impeller. Its height may be little more than the diameter of the impeller or it may extend the
full depth of the liquid, depending on the flow pattern that is required. Usually draft tubes are
used with axial impellers to direct suction and discharge Streams. An impeller-draft tube
system behaves as an axial flow pump of somewhat low efficiency. Its top to bottom
circulation behaviour is of particular value in deep tanks for suspension of solids.
Impeller Types
The typical impellers used in transitional and turbulent mixing are listed in
Table 5-2. These have been divided into different general classes, based on flow
patterns, applications, and special geometries. The classifications also define application
types for which these impellers are used. For example, axial flow impellers are efficient for
liquid blending and solids suspension, while radial flow impellers are best used for gas
dispersion. Up/down impellers can be disks and plates, are considered low-shear
impellers, and are commonly used in extraction columns. The pitched blade turbine,
although classified as an axial flow impeller, is sometimes referred to as a mixed flow
impeller, due to the flow generated in both axial and radial directions. Above a D/T ratio of
0.55, pitched blade turbines become radial flow impellers.
Table-5.2 Flow pattern vs. Impellers

Flow Pattern Impeller
Axial Flow Propeller, Pitched Blade Turbine, Hydrofoils
Radial Flow Flat-blade Impeller, Disc Turbine (Rushton), Hollow-blade Turbine
High Shear Cowles, Disc, Bar, Pointed blade Impeller
Specialty Retreat Curve Impeller, Sweptback Impeller, Spring Impeller
Up/Down Disks, Plate, Circles
Selection Criteria of Impeller

We are selected the pitched blade turbine,450 because
The weighted of the reaction mixture is calculated to be up to 11.391 cP which lies

in the range of impeller.
Efficient turbulence flow impeller for blending immiscible liquids.
Combine axial and radial flows are achieved.
Especially effective for heat exchange with vessel walls and internal coils
It can operate at reasonable speed.
Low cast.
Wide application range.
51
5.1.1Design of CSTR (Continuous Stirred-Tank Reactor)

Volume is calculated with the help of;
Rate of reaction
Residence time
Then power consumed is calculated.
Mechanical design
Thickness of Shell
Impeller Design
Diameter of Impeller
Material of Construction
Procedure:
Space time of reaction

Collect physical data required for the design.
Identify pre dominant rate controlling mechanism.
Choose a suitable reactor type.
Make an initial selection of reactor condition to give desired conversion and yield.
Size he reactor.
Select suitable material of construction.
Make a preliminary design for the reactor.
Table-5.3 Feed Specification:

1(Kg/h) 2(kg/h) Density (kg/m3)
C6H5OH - 1685.87 1072
NaOH 597.8 - 1023.56
H2O 597.8 1123.98 999
C6H5ONa - -
Total 4026.3
52
Volume of reactor
1685.87 597.8 1720
Volumetric flow of the Mixture = + +
1071 1023.56 999
3
Volume of the Mixture = 0.096 m /mint
Space time =10 mint
= V/Vo
V = 0.961 m3
If capacity<1.89m3
Allowable head space is taken 15%
If capacity >1.89m3
Allowable head space is taken 10%
Allowable head Space is Taken 15%
Volume of the Reactor = 1.057 m3
Dimensions of the Reactor
Length and Diameter Calculation
V= (D2/4) x L
L/D = 1.5
So
L = 1.723m
D = 1.148m
53
Mechanical Design
Diameter of shell = Di = 1.148 m
Working or operating pressure = 101.325 KPa
Design pressure = 140.237KPa
Working or operating temperature = 100 oC
Design pressure = 1.2 * 100 = 109 oC
Materials Selection
For Reactor: Carbon steel Type 310
Its composition is:
Cr = 24-26% Ni =19-22.90 % C =0.25%
High strength and resistant to scaling at high temperatures.

This alloy shows increased resistance to high temperature corrosion.
Jacketed high-temperature, high-pressure reactors, oil refining& ill tubes.
For Blades: Carbon steel Type 410

Its composition is:
Cr = 11.50-13.50% C = 0.15%
Lowest cost general purpose stainless steel.

Wide use where corrosion is not severe.
Bubble-tower parts for petroleum refining, pump rods and valves, machine parts,
turbine blades.
For Baffles: Carbon steel Type 405
Its composition is:
Cr =11.50-14.50 % C =0.08 % Al = 0.1-0.3%
Version of Type 410 with limited hardenability but improved weldability.

Good weld ability and cladding properties.
54
Wall Thickness
For the calculation of wall thickness we have to calculate the total pressure which is
the sum of static pressure and operating pressure. The thickness of wall depends on the
pressure and temperature of vessel.
P Hydrostatic = gh
Ps = 101.1 9.8 2.53
Ps =26.46 kpa
Total Pressure at base = Ps + P
Total design pressure =26.46+101.325
Maximum allowable internal pressure = 127.571.1 =140.327kpa
For cylindrical Shells thickness of wall can be found as
PDi
tw = + Cc
2SEj 1.2P
OR
Pri
tw = + Cc
SEj 0.6P
tw = minimum wall thickness, m
P = maximum allowable internal pressure, kPa
ri = inside radius of shell before corrosion allowance is added, m
S = maximum allowable working stress, kPa
Cc = corrosion allowance and its value is taken 3 mm
Ej = efficiency of joints expressed as a friction and its value is 0.85
Putting the values of all ,we get
101.325 1.104/2
tw = + 0.03
160000 0.85 0.6 101.325
t w = 7.24mm
55
Table-5.4 Vessel diameter against minimum thickness

Vessel Diameter (m) Minimum thickness (mm)
1 5
1-2 7
2-2.5 9
2.5-3 10
3-3.5 12
Standard thickness = 7mm
Outside Diameter
Outside Diameter D0 = Di + 2t = 1.148 + 2(0.00072) = 1.1497 m
Shell thickness
Pri
X= + Cc
SEi 0.6P
2.53
101.325 2
X= + Cc
160000 0.85 0.6 101.325
X=6.99mm
Selection of Reactor Head
Factors affecting selection of Head
Process temperature and pressure

Nature of the materials to be handled
Position of the vessel(Horizontal or vertical)
Nature of the support
Economy
56
Table-5.5 Different type of head comparison

Head Type Characteristics
Flat High discontinuity stresses , high

material cost
Ellipsoidal Suitable for pressure above 1.5MN/m2
Hemispherical Suitable for heavy duty high pressure

vessels, most expensive
Conical Suitable for removal of solids from

process vessels, commonly used ads
reducers
Torispherical Suitable for low pressure vertical

vessels
Ellipsoidal head is used for pressure greater than 150 psi and for less than that pressure we use
Torispherical head. That is why we have selected a Torispherical head.
Torispherical Head thickness
Pi RCCS
th
2 Jf Pi (CS 0.2)
CS 1/4[3 ( RC/R k)^2]
Where
Cs = Stress concentration factor for torispherical heads
RC = Crown radius = diameter of the shell = 1.148m
Rk = Knuckle radius = 0.06 RC
Cs = 2.09
57
140.32 1.1483 2.09

=
2 16000 0.85 + 140.32(2.09 0.02)
Heat thickness = 5.72 mm
Agitator Design
For turbine agitator
Impeller diameter Da = DT /3 = 0.63m
Width of Baffles J = DT /12 = 0.1625m
Impeller Width W = Da /5 = 0.65m
Length of Impeller blades La =Da /4 = 0.13m
Impeller Height above vessel E =DT /3 = 0.1625m
No. of baffles = 4
For liquid-liquid mixture and reaction with heat transfer:
Tip Velocity = 10 15 ft/sec
Tip Velocity = 5 m/sec
Tip Velocity = x Da x N
Form this equation we can fine speed of Impeller as
5
N=
3.15 1.77
Speed of Impeller N = 58.88 RPM
Power Calculation
Power required by the impeller is given by following equation
P = Npo (Nr)3 (Da )5 p = k t (Nr)3 (Da )5
Where
P = Power, watts
Np = Dimensionless power number
P = average density, Kg/m
58
N = no. of revolutions per min of impeller, RPM
D = diameter of the impeller, m
Power number is related with the Reynolds number of the impeller
REYNOLDS NUMBER
Reynolds no. of impeller is given by following equation
(Da )2 Npo p
Re =

(1.1407)2 58.8 1031.12

Re =
0.298
Re= 642069.02
For such a high Reynolds number, which is greater than 10^5 we use the relation for power
requirement as
P = K T N3 D5
KT from literature for six blade disc turbine = 1.63
Putting these values in above equation we get:
P = 4 (58.88)^3 (0.65)^5 1031.3
Power P =2.08 hp
Figure-5.1 Reynolds number against Power number
59
Selection of Cooling Jacket
Following are the cooling arrangements for continuous stirred tank reactor:
1. Jackets
2. Internal coils
3. External coils
Jacketing provides the optimum method of heating and cooling process vessels in terms of
control, efficiency and product quality.
It has many advantages which are given below:
1. All liquids can be used and velocity of heat transfer media can be accurately
controlled.
2. Jacket is fabricated from less expensive metal than the reactor itself.
3. Contamination, cleaning and maintenance problems are eliminated.
4. Maximum efficiency, economy and flexibility is achieved. \
Now there are three types of jackets available which are

1. Spiral baffle jacket
2. Half pipe coil jacket
3. Dimple jacket
Circulation baffles are usually installed in the annular space to increase the velocity of the
liquid flowing through the jacket and improve the heat transfer coefficient, see figure5.2 (a).
The same effect can be obtained by introducing the fluid through a series of nozzles spaced
down the jacket. The momentum of the jets issuing from the nozzles sets up a swirling motion
in the jacket liquid; Figure 5.2 (d). The spacing between the jacket and vessel wall will
depend on the size of the vessel, but will typically range from 50 mm for small vessels to 300
mm for large vessels. Half-pipe jackets are formed by welding sections of pipe, cut in half
along the longitudinal axis, to the vessel wall. The pipe is usually wound round the vessel in a
helix; Figure 5.2 (c).
The pitch of the coils and the area covered can be selected to provide the heat transfer area
required. Standard pipe sizes are used; ranging from 60 to 120 mm outside diameter. The half-
pipe construction makes a strong jacket capable of withstanding pressure better than the
conventional jacket design. Dimpled jackets are similar to the conventional jackets but are
constructed of thinner plates. The jacket is strengthened by a regular pattern of hemispherical
dimples pressed into the plate and welded to the vessel wall, Figure 2 (b).
60
Figure-5.2 Jacketed vessels, (a) Spirally baffled jacket (b) Dimple jacket (c) Half-pipe
jacket (d) Agitation nozzle
Jacket selection:
Factors to consider when selecting the type of jacket to use are listed below:
1. Cost: in terms of cost the designs can be ranked, from cheapest to most expensive,
As:
simple, no baffles
agitation nozzles
spiral baffle
dimple jacket
half-pipe jacket
2. Heat transfer rate required: select a spirally baffled or half-pipe jacket if high rates are
required.
3. Pressure: as a rough guide, the pressure rating of the designs can be taken as:
jackets, up to 10 bar
dimpled jackets, up to 20 bar
Half-pipe, up to 70 bar.
So, half-pipe jackets would be used for high pressure. Spiral baffle jacket is less expensive
and give low pressure drop than dimple and half pipe coil jacket. So the selected jacket is
spirally baffle jacket.
61
Calculations for cooling water flow rate:
Nr = RPM of impeller = 58.08 rpm = 0.98 rps

= Density of mixture = 1031.216 Kg/m3
= Viscosity of mixture = 1.1391 * 10-2 Pa.sec
k = 0.121542 W/m.K
Cp = Heat capacity of mixture = 253.6 kJ/Kg.oC
Di = Internal diameter of tank = 1.148 m
Do = External diameter of tank = 1.149321 m
Da = Impellers diameter = 0.63 m
Temperature of mixture = 100 oC
Temperature of water at inlet = Ti = 25 oC
Temperature of water at outlet = To = 40 oC
Log mean temperature difference:

LMTD = [To Ti]/ln (To/Ti)
LMTD = [40-25] / ln (40/25)
LMTD = 32 oC
Impellers Reynolds Number:

Re = ( Da2 Nr )/
Re = (0.6332 * 0.98 * 1031.716)/1.1391 * 10-2
Re = 45433.6
Now using a graph between j and Re taken from Process heat transfer by D.Q.Kern,
which is given below in figure 5.2
It comes out to be j = 430
Figure-5.3 Reynold number verses J factor
62
Now calculations for film coefficient on reactor side (hi)

hi = (j*k/ Di) * (Cp /k)1/3 *(/ w)0.14
Where (/ w)0.14 is taken as unity. So
For water as coolant
hj = 500 W/m2. oC
For carbon steel Type 310
kw = 37.92 W/m. oC
Overall heat transfer coefficient based on outer surface is given as:
1/Uo = + 1/ho +1/hj + x/k
Uo =370.13 W/m2.oC
As the heat load is given by Q = -696369.7 KJ/h
And temperature difference =T = 100 32 = 68 oC
Now the area of reactor available for heat transfer is;
A = Q / (Uo T)
A = 696369.7 / (111.13 * 68)
A = 9.098 m2
Total surface area of reactor is
A = Di + (/4) Di2
A = (3.141 * 1.149 ) + [(3.141/4) * 1.1442]
A = 15.09 m2
Cooling water flow rates:

Temperature of water at inlet = Ti = 25 oC
Temperature of water at outlet = To = 40 oC
Temperature difference = T = 40 25 = 15K = 15 oC
Cooling water flow rate = m = Q/ Cp T
m = 696369.7/ (4.18* 15)
m = 1113.37kg/h
63
5.1.3 Specification Sheet for CSTR
Identification
Item Reactor
Item Number R-1
Number of Item 1
Operation Continuous
Type Agitator cylindrical vessel
Function Formation of Sodium Phenolate from Carbolic acid and Caustic soda.
Design Data
Volume 0.9613
Design Volume 1.05763
Temperature (Process temperature) 100C
Design Temperature 109C
Working Pressure 1 atm
Design Pressure 1.4023 atm
Dia of Vessel 1.148m
Height of vessel 1.723m
Height to dia ratio 1.5
Type of head Torispherical
Thickness of cylindrical protion 7mm
Thickness of head 5.72mm
No. of baffle 4
64
5.2 DESIGN OF FLASH TANK
Flash Tank
The name originate from the fact that a liquid at a pressure equal to or greater than its bubble
point pressure flashes or vaporizes, when the pressure is reduced below its bubble point
pressure producing two phase system of liquid and vapour in equilibrium.
Basic equations used in flash calculation are

L+V=1
Yi
Ki =
Xi
Where Ki equilibrium constant
Yi = vapor phase composition
Xi = liquid phase composition
From Raults and Henry Law

Yi i P = Xi ri PiSat
where
I = 1 for low to moderate pressure
i = 1 assumption as no data is available in literature
Zi K I
Yi =
1 + V(K I 1)
For the flash calculation necessary condition
Pdew < P < Pbubble
Very important equation used in flash calculation
Pbubble = XI PIsat + X2 P2sat = 1
65
Jet Ejector
The two most common ejectors are operated by water or steam. The liquid ejectors are
used for creating a modest vacuum or for mixing liquids. The steam ejectors is important in
creating and holding a vacuum in a system. Ejectors have no moving parts and operated by
the action of one high pressure steam entraining and other vapors (or liquids) at low pressure
into a moving stream and thereby a removing them from the process system at an intermediate
pressure
Feature
Ejectors have the following features which make them good choice for continuously
producing economical vacuum condition.
1. They handle wet, dry or corrosive vapour mixtures

2. They develop any reasonable vacuum needed for industrial operation.
3. All sizes are available to match any small or large capacity requirement.
4. Their efficiencies are reasonable to good.
5. Have no moving parts, hence maintenance low, operation fairly constants when
corrosion is not a factor.
6. Quiet operation.
7. Stable operation within design range
8. Installation cost relatively low when compare to mechanical vacuum pumps.
9. Space requirement is small
10. Simple operation.
Types
Ejectors may be single or multi-stage. The extra stages, with or without inter stage
condensing of steam; allow the system to operate at lower absolute pressure than a single
stage unit. Various combinations of series of jets with no inter-condensing can be connected
to jets with inter-condensers or after condensers to obtain various types of the operation and
steam economy.
Types of flash tank
There are two types of vapor-liquid separator.
1. Vertical vapor-liquid separator

2. Horizontal vapor-liquid separator
Since the vertical and horizontal vapor-liquid separators have the same design equations and
have similar design calculations, therefore the only parameter on which one can be selected
for our required separation is the value of L/D ratio.
66
5.2.1Design calculation steps

Determine the bubble and dew pint
Vapor Velocity Factor
Maximum Vapor Velocity
Cross Sectional Area
Calculating Diameter
Holdup Volume
Surge Volume
HLLL
Height from Normal to High Liquid Level
Height From HH to Centerline of Inlet Nozzle
Calculate Disengagement & Total Height
L/D Ratio
Table-5.6 Feed Specification:
Components Kg/hr Molecular Mol/hr Mol fraction
weight
C6H5OH 287.98 94 3.09 0.024
NaOH 2.99 98 0.038 0.000029
H2O 1989.48 18 110.5 0.859
15.05 0.11
C6H5ONa 1745.95 116
Total 4026.41 128.6 1
Bubble point equation for multiple components under Raoult's Law
Pbubble = (Zi )
Pbubble = (0.859 101.33 + 3.51 0.024 + 2.07 0.11)
Pbubble = 87.35 kpa
Dew Point Equation for Multiple Components under Raoult's Law

1 ZA
=
Pdew PA
0.859 0.024 0.11

Pdew = + +
101.33 3.51 2.07
Pdew = 13.9kpa
67
Table-5.7 Flash calculation of flash tank

Component K-values L/V Yi Xi
0.859 4.053 0.01 0.9886 0.1128531

H2O
0.024 0.1404 0.01 0.02 0.1461549
C6H5OH
0.11 0.0828 0.01 0.0001361 0.73099
C6H5ONa
The following design parameters are to be used in the design of vapor-liquid separator
Vapor density, v = 994.94 kg/m3

Liquid density, L = 1170.943 kg/m3
Volumetric flow rate of vapor, Qv = 1.967 m3/hr

Volumetric flow rate of liquid, Ql = 1.76 m3/hr
Vapor velocity factor
First we calculate liquid vapor separation factor:
W
0.5
v

Vapor velocity factor =

l

Wv
l
Wl = 2070.95 kg/hr
Wv = 1954.65 kg/hr
l = 0.73*1258+0.1461*1023+0.1128*994 = 1170.94 kg/m^3
v = 0.00014*1258+0.02*1023+0.98*994 = 994.94 kg/m^3
2070.95 994.95
Separation factor = ( )( ) ^0.5
1954.65 1170.94
68
Separation factor = 0.96
Figure-5.4 design velocity factor vs kv

From graph the value of Kv come to be
Kv= 0.15 ft/sec
1170.94 994.94 0.5

= 0.15 ( )
944.94
So vapor velocity factor come to be Vv= 0.063ft2/sec
=0.071 m2/sec
Vapor flow rate:
Density of vapors = 994.94 Kg/m3
Lv = 1954.65 kg/hr
1954.65
VV =
994.94
Vv = 1.96 m3/hr
Cross sectional Area of the Vapour:
vapor flow rateAv

=
vapor velocity
Vapor flow rate = 1.96 m3/hr
Vapor velocity = 0.019m/s or 68.4 m/hr
1.96
=
68.4
Av = 0.0933 m2
69
The Total Cross sectional area
The minimum fraction area for vapor is 20-25%
Let us assume it to be 20%

0.093
Thus = =0.186 m2
0.25
Diameter
Dvd 4Qv

Uv
Where
Vv = 0.0106 m/sec
Qv =1.967m3/sec
Dvd =0.313 m
If there is a mist eliminator add 0.0762 to 0.1524 m to Dvd to accommodate a support ring and
to round up to the next 6 in. increment to obtain Diameter.
D = Dvd + 0.1524 m
D = 0.465m
Holdup Volume
Let us assume the hold-up time to be =5min
VH (Th)(QL)
Th =5 min.
QL =0.2274610 m3/sec
VH =0.146m3
Surge Volume
Vs (Ts)(QL)
Ts 2 min.
QL 0.146 m3/sec
Vs =0.0586 m3
70
HLLL & Height from Low to Normal Liquid Level
HLLL 6 inch
HLLL = 0.15 m
VH
HH
(/4DV 2
Where
VH =0.146 m3
Dv =0.313 m
HH =0.892m
Height from Normal to High Liquid Level
VS
HS
( / 4) DV
2
Vs =0.058 m3
Dv =0.313 m
Hs =0.133 m
Height From HH to Centerline of Inlet Nozzle
HLIN 12 dN
4Qm
dN
( 60) /

m
Qm QL QV
m L V (1 )
QL
QL QV
= 0.5277
Qm = 0.000960m3/sec
m = 1.03Kg/m3
71
dn = 0.0000283m
HLIN = 0.303m
Calculate Disengagement & Total Height
1
HD 24 dN
2
HD =0.60 m
HT HLLL HH HS HLIN HD
HT = 2.056 m
L/D Ratio
L/D ratio = 4.53 < 5
Therefore selection of vertical vapor/liquid separator is made
72
5.2.2 Specification Sheet for flash tank
Identification
Item Number FT-1
Number of Item 1
Operation Continuous
Type Vertical flash tank
Function Separation of water
Design data
Temperature 95C
Pressure 50 Kpa
Design Pressure 101.325 Kpa
Dia of Vessel 0.465m
Height of vessel 2.056m
Vapor velocity 0.071 m/s
Cross-sectional area 0.13 m2
73
5.3 DESIGN OF AUTOCLAVE REACTOR (R-2)
Introduction
Autoclaves have been used in industry for many decades. As technology has
progressed so has autoclave design, initially from basic riveted steam heated vessels to vessels
fabricated utilizing the latest welding techniques with highly sophisticated computerized
control systems. The industries that make use of autoclaves have also evolved over the years.
Initially used in the textile, timber, food, sterilizing and rubber industries, autoclaves are now
essential items in the advanced composites and Investment casting industries
For use in the production of advanced composite materials, a hot atmosphere autoclave
has to achieve the following criteria:
Safety systems
Achieve the required internal environment (i.e. heat and pressure)
Programmable temperature control and uniform temperature distribution
Programmable pressure control
Computerized process control, monitoring and data logging
Two particular types of autoclaves have been selected as covering the most important
ranges of high pressure work. These are
1. High pressure autoclaves

2. Low pressure autoclaves
Autoclaves can be made of Iron, steel, copper bronze or tin but some kind of the steel is
by the far the most common material used in their manufacture on account of its great
strength. Modern practice supports use of nickel steel and nickel chrome steel for those
autoclaves designed to withstand very high pressure. Autoclaves are made of very large size
from small apparatus of few hundered cubic centimeters capacity to huge pans capable of
holding a charge of twenty thousand gallons. Autoclaves are generally cylindrical in shape,
height being from 2-3 times the diameter. Bottom may be ellipsoidal. 10% design allowance
in volume must be given for safety point of view. Many of the different materials are used for
packing of the joints. The commonest packing is lead, copper, alluminium and asbestos. Not
only does the choice of material used on type of autoclave, but also depend on pressure. It is
more common one type to fix one or more safety valves of the ordinary steam boiler type to
an autoclave .But these were constantly getting chocked with material either distilled or
splashed into the valve.
74
Factors affecting Autoclave size:
In a recent paper on design of autoclaves for pressure leaching of nickel literates (King,
1996), the following have been listed as the determining factors in the pressure autoclave size:
solids throughput and size distribution
1. Selected autoclave circuit

2. Slurry density
3. Retention time
4. Design Temperature
5. Design Pressure
5.3.1 Design Calculations:
Carboxylation of the process is done in autoclave. Carbon dioxide at the pressure of 2

bar reacted with sodium phenolate to give intermediate product sodium salicylate.
Table-5.3.1 Feed specification
Component Mass in Density Fraction F
NaOH 2.98 1023.56 0.001 1.02356

Water 39.78 996 0.014 13.944
Phenol 282.22 1072 0.103 110.416
Na.Phenolate 1745.955 895 0.6398 572.621
CO2 657.6 770 1 770
Total 2728.535 1468.005
Density 1468 kg/m3
Mass in 2728.53 kg/h
V 1.85 m3/h
The time required to complete the reaction is one hour from literature. As the reactor is
operated batch wise, so we take one hour residence time to calculate the volume of the
reactor.
Residence time = volume of reactor/volumetric flow rate
V= 1.85 m3
10% design allowance
V=2.03 m3
H/D=2.3
75
VTotal=Vcylinder shell + Vellipsoidal head
2.03 = D 2 H D3
4 24
= D 2 (2.3D) D 3
4 24
D = 1.01 m
H = 2.3 D
= 2.33 m
Calculation for Agitator
Type: Turbine Pitched Blade
Operates at low speed and are much larger than propellers. Turbine has an excellent feature
in designing the flow patter where a change in design can divert the flow pattern of fluid by
radial flow or axial flow in the reactor vessel. Based on the configuration of the impeller
blades these flow patterns can be achieved. Radial design make the fluid to flow at high
velocity in radial direction whereas axial impellers use pitched blades, make the fluid to
flow parallel to shaft in downward direction and then push the fluid towards the wall of
the agitator vessel. Axial turbine impeller is used for chemical reactions, suspension solid
and miscible liquid mixing.
Why we use turbine pitch blade agitator?
Following are the advantages for using turbine pitch agitator in this operation.
Excellent for dispersion operations

Creates good radial flow
Only for less viscous liquid below 15 to 20 Ns/m2
Good temperature control
Creates axial flow
The diameter of the propellers depends on the rotational speed and diameter of
the agitator vessel. Depending on the agitator vessel size and the fluid viscosity the power
consumption of the turbine pitch agitator may exceed more than 50kW.
76
Figure-5.5 Different types of blades

1.01
i. Diameter of impeller Da = = = 0.33 m
3 3

ii. Height of impeller from bottom Ha = = 1 = 0.33 m

Dt 1.01
iii. Impeller blade width = 15 = 0.06 m
15
Dt 1.01
iv. Four vertical baffles width = = 0.10 m
10 10
Power Consumption:
The power consumed by an agitator at various rotational speed and physical properties e.g
viscosity and density for a systems geometry can be determined from the power number
correlation. The procedure involves:
Calculating the Reynolds number NRE for mixing.

Reading the Power number NP from the appropriate curve, and calculating the power
P given by
P = NpN3Da5
Where
P= Power Consumption
Np= Power Number
= Density of fluid
N= Impeller rotational speed
77
Da= Impeller diameter
Calculation of Reynolds number for mixing is:
Re = NDa2/
= 1468 kg/m-3
Da= 0.33 m
N= rev/min=?
= 0.298 Pa.s
For N we have the formula:
Ts = DaN
Where Ts= rotational tip speed
The International recommendation on the maximum tip speed are as follows:
dirty water - 130 ft/min
medium slurries up to 25% solids and 200 micron solids - 1150 ft/min
higher slurry concentrations and moderate solids - 1000 ft/min
pumps with elastomer impeller - 850 ft/min
Tip speeds that are higher than recommended are likely to cause excessive erosion. Elastomer
impellers are often used in the mining industry for the transfer of tailings which is a highly
abrasive slurry.
According to international standards we take 100ft/s rotational speed:
1000 = 3.14 0.76 3.28 N
N = 2.12 r/sec
Re = NDa2/
= 6032
At this Reynolds Number the value of Power Number is 1.65
So
P = NpN3Da5
= 1.65 1468 2.123 0.335
= 5.851 KW
Efficiency of the motor 85% so

5.851
Power required = = 6.88 KW
0.85
Power= 6.88 1.35 = 9.28 Hp
78
Cooling Jacket:
As the reaction is exothermic, and we maintain the outlet temperature up to 125C so we use
cooling jacket to control the temperature of the reactor.
Heat of reaction from energy balance -102639 KJ
Heat required to increase the temperature from 95C to 125C
t = 30C
m = 314 kgmol/h
Cp (mixture) = 181.85 KJ/kgmolC
Q = mCpt = 14208.5 KJ
Net heat Q = heat absorbed by jacket
= 88430 KJ
Now we find the mass flow rate of water in jacket required to absorb this heat, t should not
exceeded 20C. We take it 15C.
Q = mCpt
88430 = m*4.18*15
m = 1410.37 kg/h
79
5.3.3 Specification Sheet for Autoclave reactor
Identification
Item Number R-02
Number of Item 1
Operation Batch
Type Agitated Cylindrical Pressure Vessel
Function Formation of Sodium Salicylate from Sodium Phenolate and Carbon dioxide.
Design
Temperature 125C
Pressure 1.98atm
Design Pressure 2.17atm
volume 2.03m3
Height 2.33m
Diameter 1.01m
Height to diameter ratio 2.3
80
5.4 DESIGN OF DISTILLATION COLUMN
5.4.1 Distillation column
A process in which liquid and vapor mixture of two or more substances is separated
into its component fractions of desired purity, by the application and removal of heat.
Distillation is based on the fact that the vapor of a boiling mixture will be richer in the
components that have lower boiling points. Therefore, when this vapor is cooled and
condensed, the condensate will contain more volatile components. At the same time, the
original mixture will contain more of the less volatile material. All distillation involve two
processes: vaporization followed by condensation. In a distillation a liquid mixture is heated
until it is boiled, then the vapor above the boiling liquid is removed, condensed and collected
as a liquid distillate. The molecules in a liquid are in constant motion and have a tendency to
escape from the liquids surface and enter the gaseous phase. The pressure exerted by these
gaseous molecules is called the vapor pressure of the liquid. The temperature at which the
liquids vapor pressure is equal to external pressure over the liquid is called the boiling point
of a liquid.
The choice between plate and packed column

Vapor liquid mass transfer operation may be carried either in plate column or packed
column. These two types of operations are quite different. A selection scheme considering the
factors under four headings.
Factors that depend on the system i.e. Scale, foaming, fouling factors, corrosive systems, heat
evolution, pressure drop, liquid holdup.
Factors that depend on the fluid flow moment.
Factors that depends upon the physical characteristics of the column and its internals
i.e. Maintenance, weight, side stream, size and cost.
Factors that depend upon mode of operation i.e. Batch distillation, continuous distillation,
turndown, intermittent distillation.
The relative merits of plate over packed column are as follows:
Plate column are designed to handle wide range of liquid flow rates without flooding.
If a system contains solid contents, it will be handled in plate column, because solid
will accumulate in the voids and coating the packing materials and making it
ineffective.
Dispersion difficulties are handled in plate column when flow rate of liquid are low as
compared to gases.
81
For large column heights, weight of the packed column is more than plate column.
If periodic cleaning is required, main holes will be provided for cleaning. In packed
columns packing must be removed before cleaning.
For non-foaming systems the plate column are preferred.
For particular process, phenol and sodium phenolate system, we have selected plate column
due to:
Cleaning is easy
Favourable when operating pressure is more than atmospheric pressure
High liquid High liquid
Temperature variations dont effect plate performance
Suitable for variable liquid or vapor loads
Classification of trays
Classification of trays is based on:
Type of plate used in the contacting area
Type and number of down comers making up the down comer area
Direction and path of the liquid flowing across the contacting area of the tray
Vapor (gas) flow direction through the (orifices in) the plate
Presence of baffles, packing or other additions to the contacting area to improve the
separation performance of the tray.
Choice of plate types
There are four main tray types, the bubble cap, sieve tray, ballast or valve trays and the
counter flow trays. I have selected sieve tray because:
I decided sieve tray because of the following reasons
Manufacturing cost is low

Operating cost is low
Simple to construct
Minimum entrainment as compare to bubble cap and valve tray
less pressure drop as compare to other
82
Table-5.4.1- Comparison of the different tray
5.4.2Designing steps of distillation column

Calculation of Minimum Reflux Ratio Rm.
Calculation of optimum reflux ratio.
Calculation of theoretical number of stages.
Calculation of actual number of stages.
Calculation of diameter of the column.
Calculation of weeping point.
Calculation of pressure drop.
Calculation of thickness of the shell.
Calculation of the height of the column.
83
Preliminary calculations:
Feed = 1406.01kgmol
xF = 0.75
MD (Average molecular weight of distillate)
MD = (94 0.98) + (116 0.02)
MD=94.44kgmol
MB (Average molecular weight of bottom)
MB=(116 0.98) + (94 0.02)
MB=115.56kgmol
Basis: 1 Hour Operation
From graph
Rm=2
Reflux ratio=1.5 2
Reflux ratio=3
Number of Ideal Trays=13
Number of Ideal trays in Enriching Section = 6
Number of Ideal trays in Stripping Section = 7

Reflux ratio = (1)

R = L =
R = 3.15 9259.52
R = 29167.4gmol
L=Flow rate on the top tray = 29167.4gmol
From material balance

=+

= ( + 1)
84
= (3.15+1) 9259.52
= 38427.008
= Gas flow rate in Enriching Section
Feed in liquid entering at bubble point
Hv Hf
= =1
Hv Hf
Slope
q
=0
q1
Again from material balance
= +
= 13264.6 + 4594.5
= 17859.1
Liquid flow in stripping section
From material balance
= [( 1) ] +
= [(1 1) ] +
= 38427.008
Design Specification
1. Tray Spacing, (ts):
Let ts = 457mm (18in).
2. Hole Diameter, (dh):
Let dh = 5 mm.
3. Hole Pitch (lp):
Lp between 2.5 to 4 diameter
85
Let lp = 3 dh
lp = 35 = 15 mm.
4. Tray thickness (tT):
Let tT = 0.6 dh
tT = 0.65 = 3 mm.
Ratio of hole area to perforated area (Ah/Ap)

2
1/2( 4 )
=
3/4 2
3.14 2
1/2( 4 5 )
=
3/4 52
= 0.100
Plate diameter (Dc)
Flooding velocity

= 1

530.95 2.52
=
874.47 1023
= 0.029
1 = 0.052
10232.52
Uf = 0.052 2.52
Uf = 1.04 msec
Un = Actual velocity = 0.8 1.04
86
Un = 0.832 m/sec
Volumetric flow rate of vapour

=

38427.008 94.44
=
2.52 3600 1000
= 0.4003 /
Net area = column cross sectional area Down comer area
=

=

0.400
=
0.832
= 0.4802
2
=
4
LW
= 0.75
DC
Figure -5.6 Relation b/w downcomer area and weir length
87
LW
QC = 2 sin1 ( )
DC
QC = 97.18
Q LW DC COSQc
Ad = (4 Dc 2 3600
C
)( )
2 2 2
Ad = 0.099Dc 2
An = Ac Ad
0.480 = 0.785 2 0.099 2
=0.836 m
=0.630.836
= 0.526
Ad= 0.099 0.8362
= 0.069 2

= 0.8362
4
= 0.548 2
= 0.548 0.069
= 0.479 2
Perforated plate area (Ap)
Active area (Aa)
= (2 )
= 0.548 (2 0.069)
= 0.41 2
0.526
= = 0.629
0.836
= (2 )
= 0.548 (2 0.069)
= 0.41 0.1 = 0.2412
88
Total hole area (Ah)
= 0.1
= 0.1
= 0.1 0.241 = 0.0241 2
4
= =

4 0.0241
=
3.14 0.005
= 1007
Number of holes=1007
Head loss through dry hole

= 1 + 2( )(2 )

Uh = gas velocity
K1 and K2 constant
K1=0
2 = 50.8 2
Cv = discharge coefficient
Cv = 0.730
50.8
2 = = 95.32
0.730
50.8
= = 0.058
0.730
3
= = 0.60
5
Volumetric flow rate of vapor at the top of enriching section
3
= = 0.400
2.52
= 0 + 95.32( )(2 )
1023
Velocity through holes area at the top
89

=

0.400
= = 16.59
0.0241
2.52
= 0 + 95.32 ( ) (16.592 )
1023
= 64.56 2
Head loss due to bubble formation
409
=

= Surface tension mN/m (dyne/cm)
dh = hole diameter, mm
kg
l = Average density of liquid ( m3 )
409 17.45
= = 1.39
1023 5
Height of liquid crest over weir
0.704
=

Volumetric flow rate of liquid

=

4594.5 116 3
= = 1.44 104
1023 3600 1000
1.44 104 0.704

= ( ) 1.025
0.526
= 18.33
Down comer flooding
hhg
hds = hw + how +
2
Where hw = weir height, mm
hds = static slot seal (weir height minus height of top of slot above plate floor, height
90
Equivalent clear liquid, mm)
how = height of crest over weir, equivalent clear liquid, mm
hhg = hydraulic gradient across the plate, height of equivalent clear liquid, mm.
0
hds = 45 + 18.33 + 2
= 63.33
Design value
+ = 64.56 + 1.39 = 65.95
+ = 45 + 18.23 = 63.23
0.0241
= = 0.058
0.41
Theoretical value of ( + )=16 mm
Calculating how at bottom condition of the section

3
= 1.44 104

= 1.371
1.371
( 2.5
)=( )
0.5262.5

( ) = 6.83
2.5
1.44 104 2.3
= 1.030 ( )
0.526
= 18.33
Therefore hds = 45+18.33 = 63.33 mm
= . 0.5

= ( )

38427.008
= ( 2.52 )
0.41 3600
91

= 5.07
= 5.07 (2.520.5 )
= 2.45
Aeration factor = =0.6
Relative Froth density = t =0.20
= 0.6 64.56 = 38.73

=

38.73
= = 193.65
0.20
Head loss over down comer apron

= 165.2()2
Take clearance
1
= = 12.5
2
=
= 64.56 12.5 = 52.06
= 0.526 52.06 = 27.38

1.44104 2
= 165.2( )
27.38
= 11
= +
= 64.56 + 11 = 75.56
92
Down comer backup
= + + + +
= 75.56 + 45 + 18.33 + 11 + 0
= 149.89
149.89
= = 299.78
0.5
Efficiency method
{0.776 + (0.00457 hw)} (0.238 Ua g 0.5 ) + (104.6 W)

=
(Nsc. g 0.5 )
Ua = gas velocity through active area
Averaga vapour flow rate

Ua =
3600 Average vapour density Active area
38427.008 116
Ua = 1000 = 1.19 msec
3600 2.52 0.41
Lw + Dc
Df =
2
0.526 + 0.836
Df = = 0.681 m
2
W= Liquid flow rate
q 1.44 104 2
W= = = 2.11 104 m sec
Df 0.681
Nsc. g = Schmidt number = g(g Dg) = 0.66
Number of gas phase transfer
0.776 + (0.0045 ) (0.238 0.5 ) + (104.6 )

=
(. 0.5 )
0.776 + (0.0045 45) (0.238 1.19 2.520.5

= = 0.68
(0.660.5 )
93
1
1 = ( )
1000
38.73 0.41
1 =
1000 5.71 104
1 = 27.79
DL= Liquid phase diffusion coefficient
K1 a = (38.75 108 8.08 109 )0.5 [(0.40 1.19 2.520.5 ) + 0.17]
1 = 1.69
Slope of equilibrium curve
= 0.4375
= 0.84
= 1.2
t= mt Gm/Lm
= 0.4375 1.2 = 0.525

=
= 0.84 1.2 = 1.002
= 0.76
1
=
1 1
+ 1
1
= = 0.67
1 0.76
0.68 + 46.96
= 1 1.037 = 0.67
Point efficiency=Eog=0.67
Murphree plate Efficiency (Emv)
Pelect number=Npe
94
Npe = Z12 (DE Q1)
Z1= Length of liquid travel in 1 m
DE= eddy diffusion coefficient
DE = (6.675 103 1.191.44 ) + (0.922 104 hl) 0.0056
DE = (6.675 103 1.191.44 ) + (0.922 104 38.73) 0.0056

2
DE = 8.56 m sec
Qc
Z1 = Dc cos ( 2 )
97.18
Z1 = 0.836 COS ( ) = 0.55 m
2
Z12
Npe =
DE Q1
0.552
Npe =
8.56 27.79
Npe = 5.1
Eog = 0.76 0.67 = 0.502
Emv
= 1.28
Emg
Emv=1.280.67=0.81
Overall efficiency (EOC)
L g0.5
= = 0.039
G l
95
Figure-5.7 Fl,v vs fractional entrainment

= fractional entrainment gross down flow = 0.076
1
= [ ]

1 + (1 )
1
= 0.81 [ ] = 0.773
0.076
1 + 0.81 (1 0.076)
Overall efficiency
log[1 + ( 1)]
=

log[1 + 0.773(0.76 1)]

= = 0.726
0.76
Actual trays
NT=Theoretical plates
Nact= Actual trays

=

13
= = 17
0.726
96
Actual trays in rectifying section=9
Actual trays in stripping section= 8
Total Height of Distillation column
Z=N*Tray spacing+0.9+Ls+0.25D
0.9m=Height given above top tray.
Ls=0.06N+2
Ls= 3.02
Tray spacing=0.6m and N=17
Height of column (Z) =15 m
97
5.4.3 Specification Sheet for distillation column
Identification
Item Distillation Column
No. required 1
Sieve tray
Tray Type
Function
Separation of phenol and Sodium phenolate from water
Operation Continuous No. of holes 1007
Operating Pressure 1 atm Hole diameter 0.005 m
Number of Trays 17 Weir height 45 mm
Reflux Ratio 3 Weir length 0.526 m
Tray thickness 3 mm Active area 0.41 m2
Height of column 15 m % flooding 80
Diameter of column 0.835 m Pressure drop per tray 0.47 Psi
98
5.5 DESIGN OF DILUTION TANK
5.5.1 Dilution Tank

The preparation of mixtures of solids, liquids and gases is an essential part of most
production processes in the chemical and allied industries; covering all processing stages,
from the preparation of reagents through to the final blending of products. The equipment
used depends on the nature of the materials and the degree of mixing required. Mixing is often
associated with other operations, such as reaction and heat transfer. Liquid and solids mixing
operations are frequently carried out as batch processes.
Mixing
Term mixing involves the subdivision and blending of separate fluids so that microscopic
diffusion or shear will lead to more complete homogeneity.
Selection of Mixer
The following factors must be taken into account when choosing equipment for mixing
Liquids:
Batch of continuous operation
Nature of the process: miscible liquids, preparation of solutions, or dispersion of
Immiscible liquids.
Degree of mixing required.
Physical properties of the liquids, particularly the viscosity.
Whether the mixing is associated with other operations: reaction, heat transfer.
The term mixing is applied to operations which tend to reduce non uniformities or gradients in
composition, properties, or temperature of material in bulk. Such mixing is accomplished by
movement of material between various parts of the whole mass. For fluids the movement
occurs by a combination of these mechanisms: bulk flow in both laminar and turbulent
regimes and both eddy and molecular diffusion.
Objective of Mixing
A very common and important mixing operation is bringing different molecular

species together to obtain a chemical reaction
The movement or transfer of materials to or from surfaces of particles or phases.
99
Figure-5.5.1 Basic Impeller types (a) Turbine impeller (b) Pitch bladed turbine (c)
Marine propeller
Selection of Impeller
The following table gives general criterion for selecting an impeller for particular
applications:
Table-5.5.1 Selection of impeller

Type of impeller (Agitator) Allowable limit of Viscosity of fluid (cp)
Propeller Below 3000
Turbine At 3000-50,000
Paddle At 50,000-90,000
Modified Paddle At 90,000-1,000,000
100
Selection of impeller is based on the viscosity of the fluid in the dilution tank. The feed from
the autoclave has a temperature of 125 C .
Viscosity measurement
B
log10 = A + + CT + DT 2
T
Reference. (Transport properties of chemical and hydrocarbon by Carl L.Yaws)
The weight average viscosity of the fluid is about of 35 poise.
= 36.778poise
= 3678 centipoise
From the above criteria of selection, the best suited is turbine.
Mass flow rate to the tank = 5290.94 kg/h
Density of the Mixture = 1080.1 kg/m3

3
= 4.899 m hr
5290.94
The volumetric flow rate to the mixer = 1080
There are some other types of turbines from which we select 45 o pitched four blade turbine
because of the following reasons:
Viscosity is too high.

45o pitched blades gives axial as well as radial mixing of ingredients.
It consumes less power as compared to flat blade turbine for same duty.
Volume calculations
Residence time = 40 minutes
Residence time=0.6hr
Volume of the tank = volumetric flow rate
Volume = 4.8990.6 = 2.9343
Taking 10 % allowance we have
Volume = 3.234 3
101
Dimension of Tank
For a blended tank rule of thumb is, L/D=2
For finding diameter the formula is
2
=
4
Putting the value of V we get the diameter of the tank.
D=1.272m
Length of the tank = 2D = 2.544 m
Size of Impeller
Specifications for Standard Pitched Blade Turbine
Da/Dt = 1/3
H/ Dt = 1
J/ Dt = 1/ 12
E/ Dt = 1/ 3
W/Da = 1/ 5
L/ Da =
Where
Da = Diameter of Impeller
Dt = Diameter of Tank
H = Height of liquid in the tank
J = Width of Baffles
W = Width of impeller
E = Height of impeller above Baffle
L = Length of impeller
If
V = Volume of Mixer = 5m3
102
V1 = Volume of Mixing fluid = 4.4m3

Volume = = 4 2 .
If H = Dt

Then = 3
4
By substituting the equations we get all the values.
Dt = 1.6m
H = 1.6m
Ht = 1.8m
Da = 0.53m
E = 0.26m
J = 0.13m
W = 0.106m
L = 0.132m
Power calculations
For four blades turbine with four baffles (from figure)
Figure-5.5.2 Chemical process equipment selection and design) by Stanly M.Walas

Flow number = Nq =0.6 0.87
Power number = Np = 1.30 -1.40
Taking Nq = 0.6 and D/T = 0.25
From the figure 10.7 Re = 350
103
Figure-5.5.3 (Chemical process equipment selection and design) by Stanly M.Walas)
D2 N Density
Re =

From equation getting the N = 172.35 re/min
Power calculations:
Re=350
From figure 10.6 the Np=2

Np = 3 5
P=1183.95 W
P= 11.83KW
104
5.6 DESIGN OF ACIDIFICATION TANK
5.6.1 Design of Acidification Tank

When the reaction in autoclave is completed the outcome stream is at Temperature of

125 C and it needs to be cooled to approach the acidification temperature requirement. So this
stream is passed through dilution tank where along with lowering of temperature to 70C, the
dilution of feed for reactor is carried out to get maximum conversion. Then this stream
containing reactant sodium salicylate enters into the Acidification tank and also another
stream of 40% sulphuric acid is added into the reactor. The reaction is carried out at 20C
because this temperature gives maximum conversion at these conditions of temperature and
pressure. As for as the nature of reaction is concerned, it is an Exothermic reaction. So the
released amount of energy is simultaneously absorbed by the circulating cooling water in the
jacket surrounding the reactor and maintain the reactor temperature 20C.
5.6.2 Design calculations
Density 1670.26kg/m3
Mass flow rate 8860.95kg/h

volumetric flow rate 5.10 m3/h
Total volume covered by the fluid in the reactor
V= 5.10m3
10% design allowance

Volume of the reactor = 5.61m3
According to design consideration diameter of the tank is:
Diameter of tank = Height of liquid in tank
We know the formula for the volume of reactor,

= ( 2 1 )
4
(As Hl=DT)
Therefore DT = 1.69m
105
The bottom of reactor (with reference liquid mixing and processing by Holland and
chapman) is taken as Hemispherical. So the total volume now will be contributed by this part
of reactor also.
To find the volume of hemispherical part. We have,
2
v = 3 r 3
As
Dt = 2 r
VB = 1.26m3
Now the total volume of reactor
Total volume = Cylindrical + Hemispherical
Vt = 5.61 + 1.26 = 6.87m3
Length to diameter ratio:

From literature considering length to diameter ratio, L/D = 1.5
So putting in formula,

= 2
4
3.14
6.87 = 1.692
4
L = 3.06m
According to the literature (with reference liquid mixing and processing)
DT = Diameter of the tank = 1.69 m
Dimpeller = DT/3 = 0.56 m
HI = Impeller height from bottom = Di = 0.56 m
Wi = Impeller Blade width = Di / 5 = 0.11 m
r = Impeller blade length = Di / 4 = 0.14 m
Length of impeller blade mounted on shaft = r/2 = 0.07 m
Liquid height = Diameter of tank = 1.69 m
No. of baffles (According to literature) = 4
106
Baffle width = Wb = DT /10 = 0.16 m
Power Calculations:
3 5
= { }

Where
P = Power
Np = Power Number n = rev/sec
Di = Diameter of the impeller = density of fluid
NFR = Froud Number gc= force of gravity
2
=

For n we have n value:
n= 2.38 rev/sec
Re = 20520
Then looking at the graph b/w Reynolds number and power no.
NPR = 5
2
= ( )

n = rev / sec = 2.38 rev/sec, Di = impeller dia. = 1.86 ft , gc = 32
So we get from here:
NFR = 0.4
Calculating exponent term: m

log
= ( )

a = 1, NRE = 20520, b = 40 (values of a and b are from literature and graph)
107
Therefore the value of Froud no.s exponent m is given as

m = -0.106
3 5
= { }

n ( rev/sec) = 2.38 rev/sec, m = -0.106, NPR = 5, = 104.27 lb/ft3, NFR = 0.4, Di= 1.86 ft
So the power calculated is given by,
P =1 4.775 kw
Cooling Jacket
As the reaction is exothermic, and we maintain the outlet temperature up to 20C so we use
cooling jacket to control the temperature of the reactor.
Heat of reaction from energy balance -93918 KJ
Heat that must be removed to maintain the outlet temperature at 20C
t = 50C
m = 160 kgmol/h
Cp (mixture) = 135.23 KJ/kgmolC
Q = mCpt= 108186 KJ
Net heat + Q = heat absorbed by jacket
Q= 202104 KJ
Now we find the mass flow rate of water in jacket required to absorb this heat, t should not
exceeded 20C. We take it 15C.
Q = mCpt
202104 = m*4.18*15
m = 3223.34 kg/h
108
5.6.3 Specification Sheet for Acidification tank
Identification
Item Number R-03
Number of Item 1
Operation Batch
Type Agitated Cylindrical Vessel
Function Formation of product, salicylic acid from reaction of sulfuric acid with
Sodium salicylate.
Design
Temperature 20C
Pressure 1 atm
Design Pressure 1.27 atm
volume 6.87 m3
Length 3.06 m
Diameter 1.67 m
length to diameter ratio 1/5
109
5.7 DESIGN OF CENTRIFUGE
5.7.1 Design of Centrifuge

A mechanical device that uses centrifugal or rotational forces to separates substances
of different densities, such as solids from liquids or liquids from other liquid. Denser material
tends to move to the bottom of the tube, displacing lighter particles to the top. A centrifuge is
most often used for the separation of particles from solutions according to their size; shape,
density, viscosity of the medium and rotor speed. These machines utilize the natural
separation realities present in a high-speed circular G-force environment. Like a high-
powered clothes dryer, these exceedingly fast machines spin in order to separate materials
from one another. The denser materials separate from the less dense during the centrifugation
process. The term centrifuge encompasses a wide variety of process equipment used for
many different applications in the chemical process industries. Although these units may look
different and play key roles in much unrelated processes.
Centrifuges are classified into two main categories that are
1. Filtering Centrifuges
2. Sedimentation centrifuges
Classification of centrifuge
These two categories can be further split into subcategories, depending on whether the
centrifuge runs on a continuous or batch basis.
Filtering centrifuges
Filtering centrifuges effect a separation by using a medium such as screen or cloth, to separate
the solids from liquid. The solids are retained on the medium, while the liquid passes through
both the solids and the medium.
There are following subcategories of filtering centrifuges
Batch Filtering centrifuges

Vertical Basket Centrifuges
Horizontal Peeler
Inverting Bag Centrifuge
Continuous Filtering Centrifuges
Screen Bowl Centrifuge
Scroll Screen centrifuge
Pusher Centrifuge
110
Sedimentation Centrifuges
These centrifuges effect a separation by having a heavier solid, that is a solid with higher
specific gravity than the liquid in which it is suspended, will settle in or from a lighter liquid,
which has lower specific gravity than the solid.
There are following classifications of sedimentation centrifuges
Batch sedimentation Centrifuges

Imperforated Basket Centrifuges
Tubular Centrifuges
Continuous Sedimentation centrifuges
Solid Bowl or Decanting Centrifuges
Disc Centrifuges
Vertical basket Centrifuges

Vertical Basket Used for slow/medium filtering slurries. Even distribution of cake
across vertical face is ideal and is the result in slow and medium filtering.
Prone to high process vibration.
Three types
Vertical basket manual discharge cake discharge is manual.
Vertical basket peeler automatic flow used to discharge cake to avoid safety risks for
toxic cakes.
Vertical basket designed for sanitary operation and have a clean in place system
5.7.2 Design calculation

Calculations of Volume of Centrifuge
5
Volume of centrifuge = 1.22
4
V= 1.525 m3
Calculations of Diameter & height

V= 4 2
H/D = 0.625
1.525 4
D3=
3.14 0.625
D=1.46 m
111
H=0.9125 m
Thickness of Cake
R= 1.46 =0.73 m
2
msolid=1041.67 + 556.47 = 1598.14
solid=2059.3 kg/m3
Vsolid= 1598.14 = 0.78 m3

2059.3
Vsolid= ( 2 )
0.78=3.14 0.9125 (0.732 IRC2)
0.78=1.53 2.86 IRC2
1.53 0.78
IRC =
2.86
IRC = 0.52 m
Thickness of cake=
R=0.73 0.52
R=0.21 m
R=21 cm
Calculation of Inner Radius of Slurry (IRS)

Volume of slurry= ( 2 )
(3.14 0.9125 0.732 ) 1.22

IRS=
3.14 0.9125
IRS=0.33 m
IRS=33 cm
Relative Centrifugal Force (RCF)
112
RCF=0.000142 n2D
=0.000142 (1000)2 4.79
=680.18 g
Centrifugal Pressure
1
Pc=2 2 ( 2 2 )
= 1 1293.5 (104.67) 2 (0.732 0.332 )

2
=3.004 106 N.m2
Wall Thickness

f= ( + 2 )
1.41 108 S=0.73 (3.004106+8037.8650.73104.672)
2.41 108 S=2.19 106 + 0.64 108 s
(2.41 0.64)108 S=2.19 106
2.19 10 6
S= =0.1237 10-3 m
1.77 10 8
S=12.37 mm
S=13 mm
Self and total Stresses
SS= 2 2
Ss=(104.67)2 (0.73)2 (8037.86)
Ss=4.69 107 N/m2
Ss=2 4.69 107 N/m2
ST =2 4.69 107 N/m2
= 9.38 107 N/m2
113
Allowable stresses are=2.41 108 N/m2
(ST < f)=(Justified)
No. of Holes in Wall of Basket
Diameter of hole=5 mm = 0.19685
Area for one hole=(0.7874)2
=0.0004 m2
Total Area available=
=3.14 1.46 0.9125
=4.18 m2
No. of holes= 4.18 = 10450 holes

0.0004
No. of holes/m2=2500
Power Calculations
1
Moment of inertia of feed = IF = ( 2 + 12 )
2
Where R=Radius of Basket
R1=R e (e is thickness of liquid)
R1=0.73 0.115 (0.73)
R1=0.64 m
So, IF = 1572.89 (0.732 0.64 2 )

2
IF=96.97 kg.m2
Moment of inertia of basket = Ib = 2 2
Where m2=Mass of Basket
m2=
m2=3.14 1.46 0.9125 0.01237 8037.86
m2=415.9 kg
114
Ib=415.9 0.732 = 221.63
I=IF + Ib = 96.97 + 221.63
I=318.6 Kg m2

=
=318.6 104.67 = 111.16 N-m

5 60
p=
P=111.16 104.67
P=11635.12 Watts
P=11.63 Kw
P=15.59 H.P.
P=16. H.P.
115
5.7.3 Specification Sheet for centrifuge
Equipment Centrifuge
Type Vertical basket centrifuge
Method of operation Batch wise
No. Required one
To separate Salicylic Acid crystals from

Function mother liquor.
Basket Diameter 1.46 m
Speed 1000 rpm
Maximum centrifugal force 680.18 g.
Typical motor size 16 H.P.
Material of construction of basket Stainless steel 316
No. of holes per sq. meter 2500
116
5.8 DESIGN OF DRYER
5.8.1 Drying Operation

Drying of solids means the removal of relatively small amounts of water or other
liquid from the solid material to reduce the content of residual liquid to an acceptably low
value. Drying is usually the final step in a series of operation and the product from a dryer is
often ready for final packaging.
Classification of Dryer Types
A wide variety of dryers are used in the process industries. However following criteria is
employed to classify dryers:
Method of Operation
The first subdivision is by method of heat transfer.
Conduction Heating.
Convection Heating.
Figure-5.8.1 Classification of Dryers based on Method of Operation
117
Physical Form of Feed
It must first be emphasized that purely mechanical means should be used to decrease the
moisture content of the wet feed to as low a figure as possible, because with few exceptions,
processes such as evaporation, filtration and centrifuging are cheaper and faster than
equivalent processes in drying plant.
Figure-5.8.2 Classification of dryer based on physical form of feed
118
Operation Scale
It will be seen that the number of types for continuous large scale drying is much more limited
than for medium scale outputs. What quantity of product is desired? For larger production a
spray or rotary dryer should be considered. Rotary and spray dryers handle most large
production demands, but in small production plants other dryers are often more economical.
The figure shows below showing the scale of operation.
Figure-5.8.3 Classification of dryers on scale of production
119
Feed Nature
We then come to classification in terms of overriding features such as toxic or heat sensitive
materials, special form of dry product. The best solution to the feed problem is to try the
material in a pilot unit.
Figure-5.8.4 Classification of Dryer based on Nature of feed

Selection of Dryer
When selecting a dryer there are a lot of things to be considered, such as;
Type of feed
Type of production
Capital cost
Method of operation
Reliability of unit
Availability of data
Quality of product
Maintenance cost
120
Why to select Vacuum Rotary Dryer
Type of feed: Our feed is in form of slurry & rotary dryer best handles the slurries.
Type of production: Our plant is based on continues operation & rotary dryer is
considered to be the best dryer as a continues unit.
Capital cost: Rotary dryer has a low capital cost per unit of output.
Method of operation: Convection is the method of operation & rotary dryer is best
suitable for this method.
Availability of data: Either data is available for designing or not? Rotary dryer can be
scaled up with sufficient success from data given in the literature.
Quality of product: A dryer needs to balance a quality against cost of production. &
rotary dryer fulfills this need.
Maintenance cost: Maintenance costs are often a major consideration. Past history
shows rotary dryers have relatively low maintenance cost.
Heat transfer: Because the material coming from centrifuge is sticky, so in order to
make an effective heat transfer, surface renewal is needed. Because materials sticks to
the surface of dryer so an agitator is required for surface renewal and to make an
effective heat transfer.
Vacuum cause: Salicylic acid has tendency to disintegrate into benzoic acid and
phenol at its boiling point, therefore vacuum is employed in order to lower the boiling
point of water.
Operation of Vacuum Rotary Dryer
A rotary dryer consist of a revolving cylindrical shell, slightly inclined to the outlet. Wet feed
enters one end of cylinder, dry material discharges from the other. As the shell rotates internal
flights lift the solids and shower them down through the interior of shell. Rotary dryers are
heated by direct contact of heated gas with solids by hot gas passing through an external
jacket or by stream condensing in a set of longitudinal tube mounted on the inner surface of
shell. The last of these types is called a steam tube rotary dryer. In a direct, indirect rotary
dryer hot gas first passes through jacket and then through shell where it comes in contact with
solids
The centrifugalize undried product salicylic acid is weighed, then by means of the hoist, lifted
to the hopper of the cylindrical vacuum drier, at the same time. The stirrer inside the drier is
started up.
After loading, 0.4 MPa & 145oC saturated steam is used in the jacket for heating. The vacuum
pump is started up, the system is at vacuum state, vacuity 0.08 MPa, the material
temperature should not exceed 70oC during the drying process. The drying time is usually 3 ~
4 hours. After drying samples are taken and analyzed.
121
When the moisture is 0.5%, the product will be qualified and ready for discharge. The
obtained product is coarse salicylic acid, weighed, then transported to the sublimation
refinement.
Figure-5.8.5 Vacuum Rotary Dryer
5.8.2 Design steps for Dryer:

Heat Duty calculations:
Feed =73400 kg/day
Moisture contents=16 %
Feed temperature =20 C (293 K)
Moisture contents in final product=0.19 %
Product temperature = 70 C (343 K)
Thermal Data for Moisture and solids
Evaporation enthalpy = 2370 KJ/kg
Water enthalpy at 54oC (327k) (B.pt.) at 15 KPa (vacuum) = 225.622 KJ/kg
Water vapor enthalpy, Average (54k 14k) = 2669.78 KJ/kg

(327K 418K)
Solids temp. in constant rate during period = 327K
Product Moisture at start of falling- rate period, Xc = 8%
122
Dry Solids = m s d = ms (1 X1)
= 74000 (1 0.16)
= 61656 kg/day
61656
Product, m s p = = 10.0019
(12 )
=61773.3 kg/day
53280.200.8
Moisture at change to falling rate = = = 5361.3 kg/day
12 10.20
Moisture contents in final product = 61656 0.0019 = 375.585 kg/day
Evaporation
Total evaporation =
Total evaporation = 73400 - 61773
Total evaporation = 11627 kg/day
Evaporation up to falling rate = 5361.3 117.14
Evaporation up to falling rate = 5244.16 kg/day
Up to Constant rate = 11625 5244.16
6380.84 kg/day
Table-5.8.1 Feed Specification
Feed temperature Constant rate temperature Falling rate temperature
Steam
temperature 418 418 418 418 418 418
Solids
temperature 293 327 327 327 327 343
123
T1 T2
LMTD =
T
ln(T1 )
2
At feed LMTD =107.10 K
At constant rate LMTD=91 K
At falling rate LMTD =82.74 K
Solid Heat load
At feed point
() 287.8(327293)61.74
= =24873.8 kj/h
24 24
At falling rate point
282.32(343327)61.74
= 11847.31 kj/h
24
Liquid Heat load
At feed point
419.89(327 293)4.191
24
= 2493.52 Kj/h
At falling rate point
4.63(343327)4.191
24
= 12.94 Kj/h
Evaporation heat load
At constant rate
4321 2370
= = 426731.76 Kj/h
24
124
At falling rate
3356 (2669.78225.62)
=3426295.44 kj/h
24
Table-5.8.2 Total heat loads

Feed zone(kj/h) Constant zone(kj/h) Falling zone(kj/h)
Heat load 27366.8 426731.76 343713
Surface area
Q
Surface area=
LMTDheat transfer rate Loading%
For feed zone
27366.8
= 2.53m2
107.1021011
For constant zone
426731
=10.02m2
915850.80
For falling zone
343713
=23.75m2
82.743000.60
Total surface area=36.3m2
Total heat load= 797810 kj/hr.

797810
Steam flow rate = = = 291.27 kg/h
2739
125
Table -5.8.3 Size of the vacuum rotary dryers
For heating surface of 36.3 m2, 390.5 ft2
Total capacity of dryer, V=14.73m3
Let L/D=6

Volume of cylindrical dryer, V= D2L
4
14.73= (D2) (6D)

4
3.12=D3
D=1.46 m
L=6D = 6 1.46 = 8.77 m
( )
v=
Rate of drying, m

v =Rate of drying (kg/h)

m
T=temperature of steam
Ti=Temperature at interface
A=Drying area
i=Latent heat at temperature, Ti
hy=Heat transfer co-efficient, KJ/hr.m2.K
126
v =585(418383)36.3
m
2229.94
v =334.1 kg/h
m

tT= [(1 ) + ln ( )]
2
11627
= [(0.16 0.08) + 0.08 (0.08/0.0019)]
334.31
tT=13.19 h
For total drying time the # of batches are calculated as:
24
No. of batches=
tT
24
No. of batches= 13.19 = 1.82 ~ 2
127
5.8.3 Specification Sheet for dryer
Identification
Item Number DE-1
Number of Item 1
Operation Batch wise
Type Vacuum Rotary Dryer
Function Removal of water from the slurry
Design Data
Surface Area 36.3m2
Design Volume 14.73m3
Working Pressure 15 KPa
Width of Dryer 1.82m
Height of Dryer 2.43m
Length to diameter ratio 6
Feed inlet temperature 20 C
Feed outlet temperature 70 C
Steam inlet temperature 125 C
Steam outlet temperature 70 C
Moisture contents in feed

40%
Moisture contents in product 1.34%
128
5.9 DESIGN OF SUBLIMATION TANK
5.9.1 Sublimation tank:
Sublimation is a process in which a solid is vaporized without going into liquid state
and then are condensed back into solid state.
Whereas:
Quasi-sublimation
In this process a molten solid is vaporized and then condensed directly back to solid
state. Normally a substance processed by sublimation, is a solid at or near ambient
temperature and pressure and has a reasonably high vapors pressure at operating temperatures,
typically a minimum of 5 m.Hg absolute.
Sublimation is used to separate volatile solids and to purify the substances. One should
consider using sublimation when performing the following steps:
Removing the volatile product from a non-volatile material or mixture of materials or

removing the volatile materials from a non-volatile product.
Separating more volatile from less volatile components in a mixture of volatile
materials.
Separating a product from its impurities when either is unstable or heat sensitive at
temperatures close to the melting point.
Preparing a required type or size of crystalline product.
Purifying a wet feedstock in which drying and purification can take place in a single
sublimation step.
129
Some commercial sublimation processes are given in following table:
Table-5.9.1 Variety of Substance can be sublimed

ALUMINIUM CHLORIDE MOLYBDENUM TRIOXIDE
ANTHRACINE NAPHTHLENE
ANTHRANILIC ACID b-NAPHTHOL
ANTHRAQUINONE PHTHALIC ANHYDRIDE
BENZANTHRONE O-PHTHALIMIDE
BENZOIC ACID PYROGALLOL
CALCIUM SALICYLIC ACID
CAMPHOR SULFURE
CHROMIUM CHLORIDE TEREPHTHALIC ACID
FERRIC CHLORIDE TITANIUM CHLORIDE
ICE THYMOL
IODINE URANIUMHEXAFLUORIDE
MAGNESIUM ZIRCONIUM TETRACHLORIDE
Principles of operation
The mechanism of a sublimation process can be described with reference to the

Pressure Temperature phase diagram in the given figure. The significance of the P-T
diagram applied to one component system. The phase diagram is divided into three regions,
Solid, Liquid and vapor, by the sublimation, vaporization and fusion curves.
Fig-5.9.1 True and pseudo sublimation cycle.
These three curves intersect at a unit point called Triple point. The position of the triple
point in the diagram is of utmost importance
130
If it occurs at a pressure above atmospheric, the solid cannot melt under normal
atmospheric conditions, and process is called as True Sublimation :( Direct from
solid to vapour).
If it occurs at a pressure less than atmospheric, however, certain precaution are
necessary, The phase changes Solid to vapor or vapor to solid must be controlled,
because it may involve the liquid state.
In industrial applications it is not uncommon for liquification to be allowed in vaporization
stage, to facilitate better heat transfer, but this must never be allowed in the Desublimation
or Crystallization step. The condensation equipment therefore must operate well below the
triple point. If liquification is employed before vaporization, the operation is often called
Pseudo-Sublimation.
Both true and Pseudo-sublimation are depicted in the fig. For the case of a substance with a
triple point at a pressure greater than atmospheric, TRUE SUBLIMATION occurs. The
complete cycle is given by the path ABCDE, the original solid A is heated to some
temperature represented by B. The increase in the vapor pressure pressure of the substance is
traced along the sublimation curve from A to B. The condensation side of the process is
represented by the broken line BCDE. As the vapor passes out of the vaporizer into the
condenser, it may cool slightly and it may become diluted as it mixes with some inert gas
such as air. Point C, therefore representing a temperature and partial pressure slightly lowers
than point B.
The condensation side of the process is represented by the broken line BCDE. As the
vapors pass out of the vaporizer into the condenser, it may cool slightly, and it may become
diluted as it mixes with some inert gas such as Air. POINT C, therefore representing a
temperature and partial pressure slightly lower than point B, can be taken as condition at the
inlet to the condenser. After entering the condenser the vapor mixes with more inert gas and
partial pressure of the substance and temperature will drop to some point D. Thereafter the
vapor cools essentially at a constant pressure to the conditions represented by point E, the
temperature of the condenser.
When the Triple point of the substance occurs at a pressure less than atmospheric, the heating
of the solid may easily result in its temperature and vapor pressure exceeding the Triple point
conditions. The solid will then melt in the vaporizer through path A to B in the fig. represents
such a process. However great care must be taken in the condensation stage. The partial
pressure of the substance in the vapor stream entering the condenser must be reduced below
the Triple point pressure to prevent initial condensation to a liquid.
The required partial pressure reduction can be brought about by diluting the vapors with an
inert gas, but the fractional pressure drop in the vapor lines is generally sufficient in itself.
Point C represents the conditions at the point of entry into the condenser and the condensation
path is represented by CDE.
131
Process and equipment
On commercial scale, it is difficult to vaporize and condense a solid as well as to

control these steps. Heat transfer is typically low and removing condensed solids from a
surface is not possible. A proposed sublimation process can become commercial if
economical solutions to such problems can be found.
Sublimation techniques can be classified conveniently into three basic types:
Simple sublimation
Vacuum sublimation
Entrainer sublimation
Simple sublimation
In this type of sublimation the solid material is heated and vaporized, and then vapor
diffuses to condenser. The driving force for diffusion is the partial pressure difference
between the vaporizing and condensing surfaces. The vapor path between the vaporizer and
the condenser should be as short as possible to reduce the resistance to flow. Simple
sublimation has been practiced for the, Ammonium chloride, iodine and for the flowers of
sulfur also.
Vacuum sublimation
Its a natural follow on from simple sublimation. The transfer of Vapor from vaporizer
to the condenser is enhanced by reducing the pressure in the condenser, which thus increases
the partial pressure driving force. Iodine, pyrogellol and many metals have been purified by
this type of sublimation. The exit gases from the condenser usually pass through a cyclone or
a scrubber to protect the vacuum-raising equipment and to minimize the loss of product.
Entrainer Sublimation
In this type of sublimation an inert gas is blown into the vaporization chamber of a
sublimer to increase the rate of flow of vapors to the condensing equipment and thus increase
the yield. Such a process is known as
132
Entrainer sublimation
The use of entrainer in process has many desirable features:
It enhances the vapor flow from sublimer to the condenser

It also provides the heat needed for sublimation
Providing an efficient mean to control the temperature
Providing enough contact time to saturate air with vapor
The purification of Salicylic acid provides a good application of the use industrially of
entrainer sublimation. Air may be used as the carrier gas: But as salicylic acid can be
decarboxylated in hot air, a mixture of air and carbon dioxide is often preferred. A 5 to 10%
of carbon dioxide is recycled through the plant, passing over heater coils before over the
containers, e.g. Bin or trays, holding the impure salicylic acid in the vaporizer. The vapors are
then passed through the series of air cooled chambers, where sublimed salicylic acid is
deposited. A trap removes any entrained sublimate before the gas stream is returned to the
heaters. Make up CO2 and air are introduced into the system as required, and the process
continues until the containers are emptied of all volatile matter.
The impure material is pulverized in a mill, and hot air or any suitable gas mixture blows the
fine particles, which readily volatilize, into a series of separator, e.g. cyclones, where non-
volatile solid impurities are removed: A filter may also be fitted in the vapor lines to remove
final traces of impurities. The vapors are then passed to the series of condensers. The gases
can be recycled or passed to atmosphere through a cyclone or scrubber.
Product yield
The yield from an entrainer sublimation process can be estimated as follows. The inert gas
flow rate G and mass rate of sublimation S are related by
G g Pg
=
S s Ps
Pt = Ps + PG
s Ps
S = G( )( )
g P Ps
The equation become in term of molecular weight

=( )( )

133
Vaporization stage
P=1.015barr
Ps=0.0144barr
G=14094.93kg/sec
138 0.0144
Sv = 14094.93 ( )( )
29 1.015 0.0144
Sv = 1442kg/hr
Condensation stage
P=1barr
Ps=0.000023barr
138 0.000023
Sc = 14094.93 ( )( )
29 1 0.0144
Sc = 0.54kg/hr
To obtain the max yield of the product the air should be saturated with the vapors of salicylic
acid at 150 0C and saturation will only be approached if the air and salicylic acid are contacted
for a sufficient period of time at the required temperature. A fluidized bed vaporizer may
allow these optimum conditions to be approached; but if air is simply blown over bins or trays
is containing the solid, saturation will not be achieved and the actual rate of sublimation will
be less than that calculated. In some cases the degree of saturation may be as low as 10 % of
the possible value. The calculated loss of product in the condenser exit gases is only a value.
134
Chapter # 05 Selection of Pumps
5.10 PUMPS SPECIFICATIONS
Introduction:
Pump is a device that imparts momentum and mechanical energy to the process fluid. Pumps
are used to transfer fluid from one location to other.
Main Types of Pumps:
Reciprocating pump
Centrifugal pump
Reciprocating Pump:
Reciprocating pumps delivered energy to a flowing fluid by means of a piston acting through
a cylinder. Although steam is often employed as a source of power for this type of pumps, the
piston can be activated by other means, such as o rotating crankshaft operated by an electric
motor. Thus reciprocating piston pumps can be classified as
Steam pumps
Power pumps
They can also be classified as single acting or double acting depending on weather energy is
delivered to the fluid on both the forward and backward strokes of the piston. Reciprocating
pumps, in general, have an advantage of being able to deliver fluids against high pressure and
operate with good efficiency over a wide range of operating conditions. A major disadvantage
of piston and plunger pumps is that they cannot be used with fluids, which contain abrasive
solids. Reciprocating diagram pumps, however, are satisfactory for handling fluids with large
amount of suspended solids at low heads.
Centrifugal Pumps:
The centrifugal pumps are most commonly used type in the chemical industry. It can
be constructed in a wide range of corrosion resistance materials or lighted with rubber or
plastic. It is in fact, used for almost all pumping operations other than those where a large
head or a positive displacement is required
In centrifugal pumps, the mechanical energy of the liquid is increased by centrifugal action.
The liquid enters through a suction connection concentric with the excess of a high
speed rotary element, called the impeller. The impellers carried radial vanes integrally
case in it. Liquids flow outwards in the space between the vanes and leave the impeller, at a
considerable greater velocity with respect to the ground than at the entrance to the impeller.
In properly functioning pump, the space between the vanes is completely filled with a
135
liquid flowing without cavitation. The liquid leaving the outer periphery of the
impeller is collected in a spiral casing, called the volute and leaves the pumps
through a tangential discharge connection. In the volute, the velocity head of the liquid
from the impeller is converted into pressure head. Centrifugal pumps may be single stage or
multi stage, propeller, mixed flow and peripheral.
Selection Criteria:
Many different factors can influence the final choice of the pump for a particular operation.
The following list indicates the major factors that govern the pump selection:
The amount of liquid that must be pumped out.

The properties of the fluid
The increase in pressure of the fluid due to work input of the pump
Types of the flow distributions
Types of the power supply
Cost and mechanical efficiency of the pump.
We have selected centrifugal pumps for a process because of the following
outstanding advantages:
They are simple in operation and cheep

Fluid is delivered at uniform pressure without shocks or pulsation
They are no valves involved in pump operation
They operate at high speed(up to 4000 rpm) therefore they can be coupled directly to
an electric motor
The discharge line may be partly shut off or completely closed off without changing
the pump
Maintenance costs are lower than other types of pumps.
136
Selection of Pump (J-1)
45.85 psi
14.7 psi
Mass flow rate of feed = 1195.65 kg/h
Density of mixture = (density of NaOH composition of NaOH) + (density of water

composition of water)

Density of mixture = 1565 3 (97.5 3 )
mass flow rate

q0 =
density of mixture
3
Volumetric flow rate = 0.76

Pressure difference = P =4485.6 2

Head developed =
Head developed = 46.06 ft. (14.02 m)
From graph on page 509 timmerhaus
For a capacity of 0.7 m3/h and for head of 14.02 m single Stage centrifugal pump is best.
137
Figure -5.10.1 Capacity against pump efficiency

From using Figure 12.17 of Plant Design and Economics for Chemical Engineers,
fifth edition at capacity efficiency of centrifugal pump this
= 0.65
.
Power required =

The head developed can be calculated by P =
P = 1565 9.8 14.06
P = 215.116 kpa
Power required = 6 watt
138
5.10.1 Specification sheet of pump (J-1)

Pump Type Single stage centrifugal pump
Fluid Handle Mixture of NaOH and Water
Density of fluid 1565kg/m3
Efficiency 65%
Capacity 0.7 m3/h.
Pressure Developed 31.15 psi
Inlet Pressure 14.7 psi
Outlet Pressure 45.85 psi
Power Required 6 watt
139
Selection of Pump, J-2
72.01 psi
14.7 psi
Mass flow rate of feed = 3527.29 kg/h
Density of water = (density of water composition of water)

Density of mixture = 1000 3 (62.34 )
3

Volumetric flow rate =
3
= 3.527
Pressure difference = outlet - inlet

P = 8252.64
2

Head developed =

Head developed = 32.38 ft. (40.36 m)
From graph on page 509 Plant Design and Economics for Chemical Engineers, fifth edition
by Timmerhaus
For a capacity of 3.527 m3/h and for head of 14.02 m single Stage centrifugal pump is best.
From using Figure 12.17 of at capacity efficiency of centrifugal pump this
= 0.70
.
Power required =

The head developed can be calculated by P =
140
P = 1000 9.8 40.36
= 395.529 kpa
Power required = 19.92 kilowatt
141
5.10.2 Specification sheet of pump (J-3)
Pump Type Single stage centrifugal pump
Fluid Handle Water
Density of fluid 1000kg/m3
Efficiency 70%
Capacity 3.527 m3/h.
Pressure Developed 57.31 psi
Inlet Pressure 14.7 psi
Outlet Pressure 72.01 psi
Power Required 19.92 kilowatt
142
Chapter # 06 Instrumentation &Control
CHAPTER
6
Instrumentation &Control
6.1 Instruments
Instruments are provided to monitor the key process variables during plant
Operation. They may be incorporated in automatic control loops or used for the
manual Monitoring of the process operation. They may also be part of an automatic
computer Data logging system Instruments monitoring critical process variables will
be fitted with automatic alarms to alert the operators to critical and hazardous
situations. It is desirable that the process variable to be measured directly. Often,
however this is impractical and some dependent variable that is easier to measure and
monitored in its place. For example, in the control of distillation columns the
continuous on-line analysis of the over-head product is desirable but it is difficult and
expensive to achieve reliably so temperature is often monitored as an indication of
composition.
6.2 Instrumentation and Control Objective

The primary objective of the designer when specifying instrumentation and
Control schemes are:
1. Safer Plant Operation

To keep the process variables within known safe operating limits.
To detect dangerous situations as they develop and to provide alarms
and automatic shut-down systems.
To provide inter locks and alarms to prevent dangerous operating procedures.
2. Production Rate
To achieve the design product output.
3. Product Quality
To maintain the product composition within the specified quality standards
4. Cost
To operate at the lowest production cost, commensurate with the other
Objectives.
143
These are not separate objectives and must be considered together. The order in which they
are listed is not meant to imply the precedence of any objective over another, other than that
of putting safety first. Product quality, production rate and the cost of production will be
dependent on sales requirements. For example, it may be a better strategy to produce a better
quality product at a higher cost. In a typical chemical processing plant these objectives are
achieved by a Combination of automatic control, manual monitoring and laboratory analysis.
6.3 Components of Control System

Process
Any operation or series of operations that produces a desired final result is a process. In this
discussion the process is the Salicylic acid production.
Measuring Means
All the parts of the control system the measuring element is perhaps the most
important. If measurements are not made properly the remainder of the system cannot operate
satisfactorily. The measured available is dozen to represent the desired condition in the
process.
Analysis of measurement variable to be measured
1. Measured
Pressure measurements
Temperature measurements
Flow Rate measurements
Level measurements
2. Variables to be recorded
Indicated temperature, composition, pressure, etc.
3. Controller
The controller is the mechanism that responds to any error indicated by
the error detecting mechanism. The output of the controller is some
predetermined function of the error. In the controller there is also an error-
detecting mechanism which compares the measured variables with the desired
value of the measured variable, the difference being the error.
4. Final Control Element
The final control element. Receives the signal from the controller and by
some predetermined relationships changes the energy input to the process.
144
6.4 Classification of Controller
In general the process controllers can be classified as:
Pneumatic controllers
Electronic controllers
Hydraulic controllers
In the salicylic acid manufacturing the controller and the final control element may be
pneumatically operated due to these following reasons:
The pneumatic controller is vary rugged and almost free of maintenance. The
maintenance men have not had sufficient training and background in electronics,
so basically pneumatic equipment is simple.
The pneumatic controller appears to be safer in a potentially explosive atmosphere
which is often present in the petro chemical industry.
Transmission distances are short. Pneumatic and electronic transmission systems are
generally equal up to about 250 to 300 feet. Above this distance, electronic systems
begin to offer savings.
6.5 Modes of Control

The various type of control are called "modes" and they determine the type of response
obtained. In other words these describe the action of the controller that is the relationship of
output signal to the input or error signal. It must be noted that it is error that actuates the
controller. The four basic modes of control are:
1. Integral Control
2. Proportional Control
3. Rate or Derivative Control
In industry purely integral, proportional or derivative modes seldom occur alone in the control
system. The On-off controller is the controller with very high gain. In this case the error
signal at once off the valve or any other parameter upon which it sits or completely
sets the system.
6.6 Alarms and Safety Trips and Interlocks

Alarms are used to alert operators of serious and potentially hazardous, deviations in process
conditions. Key instruments are fitted with switches and relays to operate audible and visual
alarms on the control panels.
145
The basic components of an automatic trip systems are:
A link to transfer the signal to the actuator usually consisting of a system of pneumatic
or electric relays.
An actuator to carry out the required action; close or open a valve, switch off a motor.
A safety trip can be incorporated in control loop. In this system the high temperature alarm
operates a solenoid valve, releasing the air on the pneumatic activator closing the valve on
high temperature.
Interlocks
Where it is necessary to follow the fixed sequence of operations for example, during a plant
start-up and shut-down, or in batch operations-inter-locks are included to prevent operators
departed from the required sequence. They may be incorporated in the control system design,
as pneumatic and electric relays or may be mechanical interlocks.
6.7 Different types of Controller

Flow Controllers
These are used to control feed rate into a process unit. Orifice plates are by far the most
common type of flow rate sensor. Normally, orifice plates are designed to give pressure drops
in the range of 20 to 200 inch of water. Venturitubes and turbine meters are also used.
Temperature Controller
Thermocouples are the most commonly used temperature sensing devices. The two
dissimilar wires produce a millivolt emf that varies with the "hot -junction"
temperature. Iron constrict ant thermocouples are commonly used over the 0 to 1300F
temperature range.
Pressure Controller
Bourdon tubes, bellows and diaphragms are used to sense pressure and differential
pressure. For example, in a mechanical system the process pressure force A sensor to monitor
the control variable and provide an output signal when a preset valve is exceeded (the
instrument).is balanced by the movement of a spring. The spring position can be related to
process pressure.
Level Controller
Liquid levels are detected in a variety of ways. The three most common are:
Following the position of a float, that is lighter them the fluid.

Measuring the apparent weight of a heavy cylinder as it buoyed up more or
less by the liquid (these are called displacement meters).
146
Measuring the difference between static pressure of two fixed elevation, one on
the vapor which is above the liquid and the other under the liquid surface. The
differential pressure between the two level taps is directly related to the liquid level in
the vessel.
Transmitter
The transmitter is the interface between the process and its control system. The job of the
transmitter, is to convert the sensor signal (millivolts, mechanical movement, pressure
differential, etc.) into a control signal 3 to 15 psig air-pressure signal, 1 to 5 or 10 to 50
milli ampere electrical signal, etc.
Control Valves
The interface with the process at the other end of the control loop is made by the final
control element is an automatic control valve which throttles the flow of a stem that
opens or closes an orifice opening as the stem is raised or lowered. The stem is
attached to a diaphragm that is driven by changing air-pressure above the
diaphragm. The force of the air pressure is opposed by a spring.
6.8 Control Scheme of CSTR

Temperature Control
The simplest method of cooling a CSTR is shown in figure (6.1). Here we measure the reactor
temperature and manipulated the flow of cooling water to the jacket. Using a jacket for
cooling has two advantages. First, it minimizes the risk of leaks and thereby cross
contamination between the cooling system and the process. Second, there are no internals to
obstruct an agitator from providing effective mixing.
A temperature sensor measure the inside reactor temperature and transfer signal to
temperature transducer, transducer convert these signals in other form and the output of
transducer is accepted by controller and controller transfer its signal to final control element.
Final control element takes step to overcome these disturbances.
Flow Control
Ratio control is special type of feed forward control where two disturbances (loads) are
measured and held in a constant ratio to each other. It is mostly used to control the ratio of
flow rates of two streams. Both flow rates are measured but only one can be controlled. The
stream whose flow rate is not under control is usually referred to as wild stream.
Figure (6.1) show ratio control configurations for two streams. Phenol stream is wild stream
while NaOH stream is controllable stream.
147
In figure (6.1) we measure both flow rates and take their ratio. This ratio is compared to the
desired ratio (set point) and the deviation (error) between the measured and desired ratios
constitutes the actuating signal for the ratio control.
Set point
TIC
TT
CW
Phenol Wild stream
FT
Divider RC
Error
HW
FT
Product
CSTR
NaOH Controllable stream
Figure-6.1-Control loop of CSTR Scheme
148
Chapter # 07 HAZOP Study
CHAPTER
7
HAZOP Study
7.1 Introduction
AHAZOP study identifies hazards and operability problems. The concept involves
investigating how the plant might deviate from the design intent. If in the process of
identifying problems during a HAZOP study, a solution becomes apparent, it is recorded as
part of the HAZOP result; however, care must be taken to avoid trying to find solutions
which are not apparent, because the prime objective for HAZOP is problem
identification.
The objectives of a HAZOP study can be summarized as follows:
To identify (areas of the design that may possess a significant hazard potential.
To identify and study features of the design that influence the probability of a
hazardous incident occurring.
To familiarize the study team with the design information available.
To ensure that a systematic study is made of the areas of significant hazard

potential.
To identify pertinent design information not currently available to the team.
To provide a mechanism for feedback to the client of the study teams detailed
comments.
A HAZOP study is conducted in the following steps:
1. Specify the purpose, objective, and scope of the study. The purpose may have the
analysis of a yet to be built plant or a review of the risk of unexacting unit. Given the
purpose and the circumstances of the study, the objectives listed above can he made
more specific. The scope of the study is the boundaries of the physical unit, and also
the range of events and variables considered. For example, at one time HAZOP's were
mainly focused on fire and explosion endpoints, while now the scope usually includes
toxic release, offensive odor, and environmental end-points. The initial establishment
of purpose, objectives, and scope is very important and should be precisely set down
so that it will be clear, now and in the future, what was and was not included in the
149
study. These decisions need to be made by an appropriate level of responsible

management.
2. Select the HAZOP study team. The team leader should be skilled in HAZOP and in
interpersonal techniques to facilitate successful group interaction. As many other
experts should be included in the team to cover all aspects of design, operation,
process chemistry, and safety. The team leader should instruct the team in the HAZOP
procedure and should emphasize that the end objective of a HAZOP survey is hazard
identification; solutions to problems are a separate effort.
3. Collect data. For HAZOP analysis.
Process description
Process flow sheets
Data on the chemical, physical and toxicological properties of all raw materials,
intermediates, and products.
Piping and instrument diagrams (P&IDs)
Equipment, piping, and instrument specifications
Process control logic diagrams
Layout drawings
Operating procedures
Maintenance procedures
Emergency response procedures
Safety and training manuals
150
151
Table-7.1 HAZOP Guide Words and Meanings

Guide Words Meaning
No Negation of design intent
Less Quantitative decrease
More Quantitative increase
Part of Qualitative decrease
As well as Qualitative Increase
Reverse Logical opposite of the intent
Other than Complete substitution
4 Conduct the study. Using the information collected, the unit is divided into study
"nodes" and the sequence diagrammed in Figure, is followed for each node. Nodes are
points in the process where process parameters (pressure, temperature, composition,
etc.) have known and intended values. These values change between nodes as a result
of the operation of various pieces of equipment' such as distillation columns, heat
exchanges, or pumps. Various forms and work sheets have been developed to help
organize the node process parameters and control logic information.
5 Write the report. As much detail about events and their consequence as is uncovered
by the study should be recorded. Obviously, if the HAZOP identifies a not improbable
sequence of events that would result in a disaster, appropriate follow-up action is
needed. Thus, although risk reduction action is not a part of the HAZOP, the HAZOP
may trigger the need for such action.
6 The HAZOP studies are time consuming and expensive. Just getting the P & ID's up to
date on an older plant may be a major engineering effort. Still, for processes with
significant risk, they are cost effective when balanced against the potential loss of life,
property, business, and even the future of the enterprise that may result from a major
release.
152
7.2 P & IDS must have
A P&ID should include: (Basically every mechanical aspect of the plant with some
exceptions)
Instrumentation and designations
Mechanical equipment with names and numbers
All valves and their identifications
Process piping, sizes and identification
Miscellaneous - vents, drains, special fittings, sampling lines, reducers, increasers
and swaggers
Permanent start-up and flush lines
Flow directions
Interconnections reference
Control inputs and outputs, interlocks
Interfaces for class changes
Seismic category
Quality level
Annunciation inputs
Computer control system input
Vendor and contractor interfaces
Identification of components and subsystems delivered by others
Intended physical sequence of the equipment
153
7.3 Responsibility of HAZOP team Member
HAZOP leader
Plan sessions and timetable

Control discussion
Limit discussion
Encourage team to draw conclusion
Ensure secretary has time for taking note
Keep team in focus
Encourage imagination of team members
Motivate members
Discourage recriminations
Judge importance issues
HAZOP Secretary
Take adequate notes

Record documentations
Inform leader if more time required in taking notes
If unclear, check wording before writing
Produce interim lists of recommendations
Produce draft report of study
Check progress of chase action
Produce final report
Process Engineer
Provide a simple description of process.

Provide design intention for each process unit.
Provide information on process conditions and design conditions
Mechanical Design Engineer
Provide specification details

Provide vendor package details
Provide equipment and piping layout information
Instrument Engineer
Provide details of control philosophy

Provide interlock and alarm details
154
Plant Engineer or Manager
Provide information on compatibility with any existing adjacent plant

Provide details of site utilities and services
Provide (for study on existing plant) any update on maintenance access and
modifications
Shift Operating Engineer or Supervisor
Provide guidance on control instrumentation integrity from an operating

experience view point
Provide (for study on existing plant) information on plant stability at the
specified control parameters
Provide information on experienced operability deviations of hazard potential
Chemist
Provide details of process chemistry

Provide details of process hazards (polymerizations, byproducts, corrosion etc.)
Project Engineer
Provide details of cost and time estimation and also budget constraints.
Ensure rapid approval if require
155
Chapter # 08 Potential Health Effect
CHAPTER
8
Potential Health Effect

8.1 Emergency Overview
Harmful if swallowed.
Irritating to respiratory systems and skin.
Risk of serious damage to eyes.
May cause irritation to the respiratory tract.
Symptoms may include coughing, sore throat, labored breathing, and chest pain.
8.2 First Aid Measures

General
In all cases of doubt or when symptoms persists, always seek medical attention.
Inhalation
Inhalation move affected person from the exposure. If recovery not rapid or complete seek
medical attention.
Ingestion
Do not induce vomiting. In case of spontaneous vomiting, be sure the vomit can freely drain
because of danger of suffocation. Only when conscious, rinse mouth with plenty of water and
give plenty of water to drink. Keep patient at rest and obtain medical attention.
Skin
Remove contaminated clothing. Wash affected area with plenty of soap and water. If irritation
persists, seek medical attention. Launder clothing before reuse.
Eyes
Rinse immediately with plenty of water for at least 5 minutes while lifting the eyes lids. Seek
medical attention. Continue to rinse.
156
8.3 Fire Fighting Measures:
Extinguishing Media
Foam, dry chemical, sand, dolomite etc.
Explosion Hazards
Finely divided material can cause dust explosion.
Combustion Products
Burning may release oxides of carbon and other hazardous gases or vapors.
Protective Measures
Fire fighters should wear self-contained breathing apparatus.
8.4 Accidental Release Measures:

Personal Precaution in Spill
Avoid breathing dust. Avoid direct contact skin, eyes and clothing.
Precautions To Protect Environment
Prevent contaminated of soil, drains and surface water.
Spill Clean Up Methods
Cover spillage with damp inert material, take-up or collect and place into a suitable closable
labeled container for disposal. Wash the area clean with water and detergent.
8.5 Exposure Control and Personal Protection

Ventilation
Provide adequate general and local exhaust ventilation.
Respirators
If unable to control dust emissions below OES limits, an approved dust protection to P2 level
of protection is recommended.
Gloves Use protective gloves.
Eyes Use eye protection. All contacts concentrate irritation effect.
157
Other Equipment
Wear personal protective equipment appropriate to quantity of material handled
8.6 Disposal and Considerations

Disposal Methods
This material or its container must be disposed of as hazardous waste according to Special
Waste Regulations 1996, in compliance with Duty of Care Regulations and Special Waste
regulations.
8.7 Toxicological Information

LD50. Oral. Rat. 891 mg/kg
Toxicological Information
Ingestion of large doses may cause central nervous system effects.
Health Hazards, General
Dust will severely irritate membranes of nose, thorrat, lungs and eyes.
Inhalation
Irritating to the respiratory system.
Ingestion
Ingestion will cause gastric irritation and vomiting. May cause severe systemic effects.
Skin
May be absorbed though skin.
Eyes
Dust may cause mechanical irritation to eyes.
Other Health Effects
Evidence of mutagenic effects.
Medical Consideration
Some individuals may exhibit salicylate hypersensitivity, characterised by urticarial, rhinitis

and dyspboea.
158
Chapter # 09 Cost Estimation
CHAPTER
9
Cost Estimation
9.1 Purchase Equipment Cost:
Table 9.1 Marshall and Swift Equipment Cost Index
Year Cost index
2006 499.6
2007 525.4
2008 575.4
2009 521.9
2010 550.8
2011 585.7
2012 584.8
2013 587.3
2014 580.2
Cost index in year A

Cost in year A = cost in year B
Cost index in year B
Reactor (CSTR)
Agitated cylindrical jacketed vessel

Diameter = 1.92
Height = 2.53
Design pressure = 1.27
Capacity of water in jacket = 223
Vessel cost = 12,000 1 1= $ 12,00
Agitator jacketed vessel cost = 15,000 220.40 = $ 51,648
Equipment cost = $ 63,649
159
Flash tank
Pressure vessel
Diameter = 0.43
Height = 2.39
Equipment cost = 6,000 1 1 = $ 6,000
Autoclave

Diameter = 1.01
Height = 2.33
Design pressure = 5
Capacity = 1.6333
Vessel cost = 30,000 1 1.1 = $ 33,000
Agitator jacketed vessel cost = 15,000 1.60.40 = $ 18,250
Distillation column
Sieve tray
Diameter = 0.835
Height = 15
Number of plates = 17
Operating pressure 1 1.27
Vessel cost = 13,000 1 1 = $ 13,000
Cost of plate = 300 1 = $ 300
Cost of 17 plates = $ 5,100
Dilution tank
Four blade turbine agitator

Diameter = 1.47
Height = 0.835
Power of agitator = 11.83
Vessel cost = 9000 1 1 = $ 9,000
Agitator cost = 3,000 11.830.50 = $ 9,837

160
Acidification tank

Diameter = 1.67
Height = 3.06
Design pressure = 1.27
Capacity = 3.2233
Vessel cost = 18,000 1 1 = $ 18,000
Agitator jacketed vessel cost = 15,000 3.220.40 = $ 17,613
Centrifuge
Carbon steel
Diameter = 1.46
Equipment cost = 58,000 1.460.45 = $ 84,680
Dryer
Rotary dryer
Area = 35.3
Equipment cost = 35,000 35.30.40 = $ 174,006
Sublimation tank
Diameter = 1.34
Height = 2.01
Equipment cost = 8,000 1 1 = $ 8,000
Crystallizer
Diameter = 1.65
Height = 2.45
Equipment cost = 8,000 1 1 = $ 8,000
Compressor
Centrifugal
Power = 7
Equipment cost = 1,920 70.80 = $ 122,326
161
Storage tanks
Cone roof stainless

Assumption capacity of tank = 503
Number of tanks =4
Tank cost = 2,300 500.55 2 = $ 39,554
Tanks cost (4) = $158,216
Pumps 1
Head = 1.33
Mass flow rate = 0.332 1
Power = 0.008
Cost = $ 1060
Pump 2
Head = 16.21
Power = 0.0194
Cost = $ 1330
Pump 3
Head = 10.94
Power = 0.008
Cost = $1060
162
Table 9-2 Equipment cost

Equipment Number Cost
CSTR R-101 $ 58,640
Flash Tank FT-101 $ 6000
Autoclave R-102 $ 23,250
Distillation Column DC-101 $17100
Dilution tank M-101 $ 18870
Acidification tank R-103 $ 35613
Centrifuge FF-101 $ 84680
Dryer DE-101 $174006
Sublimation Tank SB-101 $ 8000
Crystallizer C-101 $ 8000
Compressor JC-101 $ 17348
Pump P-101 $ 1060
Pump P-102 $ 1330
Pump P-103 $ 1060
Storage Tank TT-101 $ 39554
Total plant equipment cost $611,973
9.2 Fixed Capital Investment
Total physical plant cost = (1 + 1 + 2 + . +9)

= $751,163 3.14
= $ 2,358,651
Fixed capital investment = (1 + 10 + 11 + 12)
= 2,358651 1.45
= $ 3,420,045
9.3 Total Capital Investment

We have calculated the fixed capital cost of the plant according to cost index of 2004
and data available in Plant Design and Economics. The present cost of plant can be calculated
from recent cost index using formula.
PPC = $ 611,973 x 3.40 = $ 2080708

Fixed capital = $ 2197019 x 1.45 = $ 3185677 (2004)
Fixed capital = $ 4162905 (2014)
Working capital = 0.15 x 4162905
Working capital = $ 624436 (2014)
Total investment required = F.C + W.C
163
Total investment required = $ 4787840 (2014)
9.4 Annual Production Costs

Variable costs
Raw Material
Phenol 2.53 $/kg
Sodium hydroxide 0.56 $/kg
Carbon dioxide 0.11 $/kg
Sulphuric acid 1.59 $/kg
Raw Material cost $ 5,294,0917 (2014)
Miscellaneous $ 409,21
Utilities $ 208,145
Sub-total A = $ 53,189,983
Fixed costs
Maintenance $ 409218
Operating labor $ 21379
Laboratory costs $ 49106
Supervision $ 49106
Plant overheads $ 122765
Capital charges $ 409218
Insurance $ 40922
Local taxes $ 81844
Royalties $ 40922
Sub-total B = $ 1224480
Direct production cost = Subtotal A + Subtotal B
Direct production cost = $ 54414463

Sub-total C = Sales Expense + General Overheads
Sales expense = $ 10886094
General overheads = $ 122765
Sub-total C = $ 11008859
Annual Production Cost = $ 65,423,322
Production cost ($/Kg) = Annual Production Cost/Annual Production Rate
Production cost ($/Kg) = $5.72
Selling Price of Salicylic Acid per kg = $6.62
164
Total Income = Selling price Quantity of product manufactured
Total Income = 6.62 11434500

Total Income = 75,696,390 $
Gross income = Total Income Total Product Cost
Gross Income = $ 10,273,068
Let the Tax rate be 35% (common)

Net Profit = Gross income - Taxes
Net Profit = $ 72,100,816
( )
Return on investment =
9.5 Rate Of Return
0.379159244 = 37.91%
9.6 Payback Period
Payback Period = Reciprocal of rate of return
2.67 Year
165
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Salicylic Acid

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PRODUCTION OF SALICYLIC ACID BY

KOLB SCHMITT PROCESS

Khesro Dawood UW-11-Ch.E-BSc-016

Iftikhar Ali UW-11-Ch.E-BSc-055

Ikram Ullah UW-11-Ch.E-BSc-061

DEPARTMENT OF CHEMICAL ENGINEERING

This report is submitted to Department of Chemical Engineering, Wah

Internal Examiner External Examiner

DEPARTMENT OF CHEMICAL ENGINEERING

Table-1.1: Physical Properties of Hydroxybenzoic acid ........................................................... 2

Figure-5.1: Reynolds number against Power number ............................................................. 59

3.1.1 Material balance around CSTR (R-1): .................................................................. 17

7.3 Responsibility of HAZOP team Member 147

8 Potential Health Effect

A Heat transfer area (m2)

Aa Active area (m2)

AT Tower area (m2)

B Baffle spacing (m)

Cp Specific heat (Btu/lb-F)

ho Outside fluid film coefficient (Kwatt/m2-C)

hi Inside fluid film coefficient (Kwatt/m2-C)

k Thermal conductivity (Kwatt/h-m-C)

L Liquid flow rate (kg-mol/h)

LMTD Log mean temperature difference (C)

Pl Liquid density (kg/m3)

U Overall heat transfer coefficient (kwatt/h-m-C)

Latent heat (kJ/Kg)

Cs Stress concentration factor for torispherical heads

Di Internal diameter of tank = 1.148 m

Some 2400 years ago Hippocrates prescribed decoctions of willow leaves as a

1.2 Properties of Salicylic Acid

Molecular weight 138.12 138.12 138.12

Melting point, oC 159 20L5-203 214.5 215.6

Boiling point, oC 211 swub

Flash point (Tag closed-cup), oC 1.57

Ka (acid dissociation) at 25oC 1.05 8.310-5 2.610-5

Heat of combustion, mJ/molo 3.026 3.038 3.035

Heat of sublimation, kJ/molo 95.14 116.1

Table-1.2 Solubilitys of the Hydroxybenzoic Acids in Water, Wt %

Ortho Meta Para

0 0.12 0.35 0.25

10 0.14 0.55 0.50

20 0.20 0.85 0.81

30 0.30 1.35 0.81

40 0.42 2.0 1.23

50 0.64 3.0 2.3

60 0.90 4.3 4.2

70 1.37 7.0 7.0

80 2.21 11.0 12.0

1.2.2 Chemical Properties

Reactions of the carboxyl group of salicylic acid

Table-1.3 Solubilities of the Hydroxybenzoic Acids in Non-aqueous Solvents, Wt %

Chloroform (satd in H2O) at 1.84

Reactions of the hydroxyl group of salicylic acid.

Ring-substitution reactions of salicylic acid. X = halogen.

1.3 Uses of Salicylic Acid

2.1 Synthesis of Salicylic Acid

2.1.2 KOLB Process

2.1.3 SCHMITT Modification

JC-1 6 4.93atm 125 C

Figure-2.1 Process Flow sheet of the Production of salicylic Acid

2.2 Process Flow Sheet Description