Distillation Column

Figure 1. P&ID for Distillation

Separation process is done inside the distillation unit. The main goal of this process is
separating the levulinic acid, the main product, from other side products and impurities so the
higher purified percentage of levulinic acid will be obtained. The side products, which are formic
acid and furfural, are also separated in a two different distillation columns. Walas (1988) stated
several rules of thumb for selecting and designing appropiate column control:
Distillation usually is the most economical method of separating liquids, superior to
extraction, adsorption, crystallization, or others.
For ideal mixtures, relative volatility is the ratio of vapor pressures
12
= P
2
/P
1
.
Tower operating pressure is determined most often by the temperature of the
available condensing medium, 100-120F if cooling water; or by the maximum
allowable reboiler temperature, 150psig steam, 366F.
Sequencing of columns for separating multicomponent mix- tures: (a) perform the
easiest separation first, that is, the one least demanding of trays and reflux, and leave
the most difficult to the last; (b) when neither relative volatility nor feed
concentration vary widely, remove the components one by one as overhead products;
(c) when the adjacent ordered components in the feed vary widely in relative
volatility, sequence the splits in the order of decreasing volatility; (d) when the
concentrations in the feed vary widely but the relative volatilities do not, remove the
components in the order of decreasing concentration in the feed.
Economically optimum reflux ratio is about 1.2 times the minimum reflux ratio R
m
.
The economically optimum number of trays is near twice the minimum value N
m
.
The minimum number of trays is found with the Fenske-Underwood equation:
N
m
= log[

Minimum reflux for binary or pseudobinary mixtures is given by the following when
separation is esentially complete (x
D
1) and D / F is the ratio of overhead product
and feed rates:

when feed is at the bubblepoint,

when feed is at the dewpoint.

A safety factor of 10% of the number of trays calculated by the best means is
advisable.
Reflux pumps are made at least 25% oversize.
For reasons of accessibility, tray spacings are made 20-24 in.
Peak efficiency of trays is at values of the vapor factor

in the range 1,0-

1,2 (ft/sec) vacuum.
The optimum value of the Kremser-Brown absorption factor A = K(V/L)is in the
range 1.25-2.0.
Pressure drop per tray is of the order of 3 in. of water or 0.1 psi.
Tray efficiencies for distillation of light hydrocarbons and aqueous solutions are 60-
90%; for gas absorption and stripping, 10-20%.
Sieve trays have holes 0.25-0.50 in. dia, hole area being 10% of the active cross
section.
Valve trays have holes 1.5in. diaeach provided with a liftable cap, 12-14 caps/sqft of
active cross section. Valve trays usually are cheaper than sieve trays.
Bubblecap trays are used only when a liquid level must be maintained at low
turndown ratio; they can be designed for lower pressure drop than either sieve or
valve trays.
Weir heights are 2in., weir lengths about 75% of tray diameter, liquid rate a
maximum of about 8gpm/in. of weir; multipass arrangements are used at high liquid
rates.
Packings of random and structured character are suited especially to towers under 3
ft dia and where low-pressure drop is desirable. With proper initial distribution and
periodic redistribulion, volumetric efficienciescan be made greater than those of tiray
towers. Packed internals are used as replacements for achieving greater throughput or
separation inexisting tower shells.
For gas rates of 500 cfm, use 1 in. packing; for gas rates of 2000 cfm or more, use 2
in.
The ratio of diameters of tower and packing should be at least 15.
Because of deformability, plastic packing is limited to a 10-15 ft depth unsupported,
metal to 20-25 ft.
Liquid redistributors are needed every 5-10 tower diameters with pall rings but at
least every 20ft. The number of liquid streams should be 3-5/sqft in towers larger
than 3 ft dia (some experts say 9-12/sqft), and more numerous in smaller towers.
Height equivalent to a theoretical plate (HETP) for vapor-liquid conlacting is 1.3-
1.8ft for 1in. pall rings, 2.5-3.0 f:for 2 in. pall rings.
Packed towers should operate near 70% of the flooding rate given by the correlation
of Sherwood, Lobo, et al.
Reflux drums usually are horizontal, with a liquid holdup of 5 min half full. A
takeoff pot for a second liquid phase, such as water in hydrocarbon systems, is slzed
for a linear velocity of that phase of 0.5 ft/sec. minimum diameter of 16in.
For towers about 3ft dia, add 4ft at the top for vapor disengagement and 6 f t at the
bottom for liquid level and reboiler return.
Limit the tower height to about 175ft max because of wind load and foundation
considerations. An additional criterion is that L/D be less than 30.
The first distillation column will separate formic acid from the levulinic acid and other by
products. Both furfural and formic acid form an azeotrope with water. In this case formic acid
acts as an entrainer to make the separation feasible. Levulinic acid, formic acid, and water leave
the column at the bottom while formic acid with high recovery percentage leaves at the top. The
column is operated at 1,01 bar because there is no need for a high pressure and the second
column also operates at 1,01 bar so no compressors or expanders are needed. The second (C02)
and third (C03) column separates furfural and levulinic acid from its mixture. The disadvantage
of these separation methods is the presence of an entrainer in the mixture, which has to be
removed to obtain pure levulinic acid without any impurities, including water.
Formic acid and water form maximum boiling containing 77.5% acid at 101.3 kPa and
83.2 % acid at 2.4 MPa. At the 101.3 kPa, the azeotropic mixture boils at 380.3 K, and at 2.4
MPa it boils at 407.8 K. This dependence upon pressure makes it possible to produce
concentrated formic acid using pressure shift distillation. The feed liquor is pumped to a column
operated at 300 kPa producing nearly pure water as distillate. The bottom product is fed to a
vacuum (20 kPa) column producing nearly pure formic acid as distillate. The bottom product
from the vacuum column is circulated to the pressurized column. The temperatures of all feeds
entering the column are at the bubble point temperature of the feed. This results in an optimal
separation. (Girisuta, 2006)
A. Column Material Selection
It is allowed to use metal material for non-food products, but it is essential to select a
material that is non-corrosive because the distillation process will happen in high temperature,
thus evaporating water content from the mixture. The material chosen is carbon steel (CS)
because of the total pressure drop allowance in column. This criterion is based on ASME B31.4
and the rules of thumb that has been explained before.

B. Calculation Methods (Fenske-Underwood-Gilliand Method)
The first step in the design of distillation equipment is specification of the required
distribution of light and heavy key components. Then the specific operating conditions and
equipment size are established, ultimately on the basis of an economic balance or simply by
exercise of judgment derived from experience. The design parameters that need to be determined
include intermediate ones such as limiting reflux and trays that are needed for establishing a
working design. These design parameters are the following:
Minimum number of theoretical trays
Distribution of nonkeys between the overhead and bottoms products
Minimum reflux
Operating reflux
Number of theoretical trays
Location of the feed tray
Tray efficiencies.

B.1. Distillation Column I (C-101)
1. Stream Composition
Basis = 1 hour, feed = 13890,254 kg/hour
Table 1.Feed, distillate, and bottoms composition
Component Feed (%) Distillate (%) Bottoms (%)
Cellulose
0,02
0,00
0,02
Formic Acid
1,01
99,99
0,02
Furfural
1,14
0,01
1,13
Glucose 0,04 0,00 0,04
Hemicellulose 0,09 0,00 0,10
HMF 0,29 0,00 0,29
Levulinic Acid 3,62 0,00 3,65
Lignin 1,18 0,00 1,19
Sodium Hydroxid 0,00 0,00 0,00
Water 90,76 0,00 91,69
Xylose 1,86 0,00 1,88
100 100 100

2. Temperatures
Dew point of the distillate
Table 2. Dew point of the distillate
Component P m Y X
Formic Acid (LK) 101,50 1,00 0,99 1,00
Furfural (HK) 2,39 0,02 0,01 0,00
1,00 1,00
Distillate dew point is 100,40
o
C
Where:

Bubble point of the bottom
Table 3. Bubble point of the bottom
Component P (kPa) m Y X
Cellulose 2,47 0,02 0,00 0,00
Formic Acid 2,43 0,02 0,00 0,00
Furfural 2,47 0,02 0,00 0,01
Glucose 0,00 0,00 0,00 0,00
Hemicellulose 2,47 0,02 0,00 0,00
HMF 0,19 0,00 0,00 0,00
Levulinic Acid 0,19 0,00 0,00 0,04
Lignin 2,47 0,02 0,00 0,01
Sodium Hydroxid 0,00 0,00 0,00 0,00
Water 110,11 1,09 1,00 0,92
Xylose 2,47 0,02 0,00 0,02
1,00 1,00
Bottom bubble point is 102,78
o
C.
where,

, so that

101,55
o
C.

3. Relative Volatilities
Relative Volatility of each component is defined base to T
av
= 101,55
o
C.and
HK
as the
base .
Table 4. Relative volatilities of the distillate
Component P m
Formic Acid (LK) 1,00 1,00 1,80
Furfural (HK) 0,02 0,02 0,76
Where,

4. log[

= log [

From Figure 4.1, we can define N
M
.


Figure 2. Fenske equation for minimum plates expressed in graph form (Source: Gulf, 2002)
From this figure, we can get log N
M
= 1,28 ; so that, N
M
= 19,05 trays 19 trays
5. Defining Nopt/N
M
from Figure 4.2, for finding Nopt.

Figure 3. Relation between optimum-to-minimum ratio and Fenske separation factor (Source: Gulf, 2002)

From this figure, we can get Nopt/NM = 1,84, so that Nopt = 1,84 x 19,05 = 35,052 35.By
assuming the tray efficiency is about 85%, we can calculate Nactual as (Nopt/Tray Efficiency), so
that we get Nactual = 41 trays.

6. log[

= log [


After getting this value, we can define Ropt/R
M
from figure 4.3.

Figure 4. Optimum-minimum reflux ratio relationship to the columns feed, distillate, and bottoms
composition (Source: Gulf, 2002)

Based on this figure, if we have log[

] = 2,20 and

, the value R
opt
/R
M
= 1,35.

7. Defining the value of by using Figure 4.4
The calculated value of

and

= = 0,87, then
= 1,58

Figure 5. Underwoods vs key ratios in feed (Source: Gulf, 2002)

By using Figure 4.5-4.7, the value of(i.xi
D
)/(i-) will be obtained as:

Figure 6. Underwoods vs parameter for in range 1,01 to 1,11 (Source: Gulf, 2002)


Figure 7. Underwoods vs parameter for in range 1,05 to 3,00 (Source: Gulf, 2002)


Figure 8. Underwoods vs parameter for heavy key and heavier components(Source: Gulf, 2002)

RM + 1 = (i.xi
D
)/(i-) = -6,21
RM = -6,21 1 = -7,21

9. R
opt
= (-7,21) x (1.35) = -9,73.

10. Tray Spacing = 0.5 m (Heuristic: Stage spacing range 20 24 inch).

11. Height of Tower

20,71 m
(Heuristic: Maximum column height allowed is 175 ft or 53,025 m, so the result is meeting the
requirements.)

12. Column Diameter

Where

= Maximum allowable vapour velocity, m/s

= Plate spacing

= Maximum vapor rate, kg/s

2,04 m.
13. Plate Design
Column Diameter (D
c
) = 2,04 m
Column Area (A
c
) = D
c
2
/4 = 3,27m
2

Downcomer Area (A
d
) = 0.12 x A
c
= 0,12 x 3,27m
2
= 0,39 m
2

Net Area (A
n
) = (A
c
A
d
) = 2,88 m
2

Active Area (A
a
) = (A
c
2A
d
) = [2,66 (2 x 0,32)] m
2
= 2,49 m
2

Hole Area (A
h
) = 0.1A
a
(10% estimated from active area) = 0,1 2,49= 0,25 m
2
Weir Length is define from Figure 11.31 of Coulson and Richardson Book.
(A
d
/A
c
) x 100% = 12 %
Lw/Dc = 0,76
Lw = 1,55 m.

Figure 9. Relation between downcomer and weir length (Source: Coulson and Richardson, 2002)

Hole Diameter = 0,005 m
Plate Thickness = 0,005 m
Number of Holes = 2,04/(1.965 x 10
-5
) = 103816,79 holes.

14. Plate Pressure Drop
Dry Plate Pressure Drop
Maximum vapor velocity through holes:
U
h(max)
= V
m
/A
h

= 8,20m/s
(A
h
/A
a
)*100 = (0,25/2,49)*100
= 10,04
From Figure 11.34, 6th Ed. Coulson and Richardsons if the (A
h
/A
a
)*100 = 10,04, when plate
thickness to plate diameter is 1, then C
o
= 0.83
h
d
= 51 (U
h
/C
o
)
2
(d
v
/d
l
)
= 51 (8,20/0.83)
2
(1,00/1134,31)
= 4,39 mm liquid
Residual Drop
h
r
= 12.5*1000/d
l

= 12.5*1000/1134,31
=11,02 mm liquid
h
w
+ h
ow
= 50 + 4,39
= 54,39 mm liquid
Total Plate Pressure Drop
h
t
= h
d
+ h
r
+ (h
w
+ h
ow
)
= 4,39 + 11,02 + 54,39
= 69,80 mm liquid
Pt = 9,81*10
-3
*h
t
*d
l

= 776,71 Pa
=0,77 kPa = 0,12 psi
P
top
= 14,5 psi
P
bottom
= 14,5+ (19*0,12) = 16,78 psi

15. Shell Calculations
Minimum Shell Thickness

in
Therefore, 3/16 in thickness can be used
Selection of Head and Head Thickness Calculation
Torispherical Head

Diameter
OD + (OD/24) + 2 sf + 2/3 icr
= 40,16 + 1,67 + (2*3) + (2/3*4)
= 50,50 in
Weight of Head

= 328,70 lb
Calculation of Axial Stress in Shell

16. Specifications and Operation Condition
Table 5. Specifications and operation condition of distillation column I
1. Type Distillation Column
2. Material Carbon Steel
3. Temperature 102,78
o
C
4. P
top
14,5 psi
5. P
bottom
16,78 psi
5. Light Key Formic Acid
6. Heavy Key Furfural
7. Space between Tray 0,5 m
8. Column Height 20,71 m
9. Column Diameter 2,04 m
10. Column Thickness 0,18 in
11. Plate Thickness 0,005 m
12. Plate Pressure Drop 0,12 psi
13. Hole Valve Tray Size 0,005 m
14. Number Hole Valve Tray 103816,79
15. Hole Area 0,25 m
2

16. Weir Length 1,55 m
17. Column Area 3,27 m
2

18. Net Area 2,88 m
2

19. Active Area 2,49 m
2

20. Price $ 65000










B.2. Distillation Column II (C-102)
1. Stream Composition
Basis = 1 hour, feed = 13749,505 kg/hour
Table 6.Feed, distillate, and bottoms composition
Component Feed (%) Distillate (%) Bottoms (%)
Cellulose 0,02 0,00 0,02
Formic Acid 0,00 0,00 0,00
Furfural 1,15 99,97 0,00
Glucose 0,04 0,00 0,04
Hemicellulose 0,10 0,00 0,10
HMF 0,29 0,00 0,29
Levulinic Acid 3,65 0,03 3,70
Lignin 1,19 0,00 1,20
Sodium Hydroxid 0,00 0,00 0,00
Water 91,69 0,00 92,75
Xylose 1,88 0,00 1,90
100 100 100

2. Temperatures
Dew point of the distillate
Table 7. Dew point of the distillate
Component P m Y X
Furfural (LK) 150,02 1,00 0,99 1,00
Levulinic Acid (HK) 73,00 4,93 0,01 0,00
1,00 1,00
Distillate dew point is 103,45
o
C
Where:

Bubble point of the bottom
Table 8. Bubble point of the bottom
Component P (kPa) m Y X
Cellulose 2,48 0,02 0,00 0,00
Formic Acid 2,43 0,02 0,00 0,00
Furfural 0,06 0,00 0,00 0,00
Glucose 0,00 0,00 0,00 0,00
Hemicellulose 2,48 0,02 0,00 0,00
HMF 0,19 0,00 0,00 0,00
Levulinic Acid 0,19 0,00 0,00 0,04
Lignin 2,48 0,02 0,00 0,01
Sodium Hydroxid 0,00 0,00 0,00 0,00
Water 110,41 1,09 1,01 0,93
Xylose 2,48 0,02 0,00 0,02
1,01 1,00
Bottom bubble point is 170
o
C.
where,

, so that

136,73
o
C.

3. Relative Volatilities
Relative Volatility of each component is defined base to T
av
= 136,73
o
Cand
HK
as the
base .
Table 9. Relative volatilities of the distillate
Component P m
Furfural (LK) 1,00 1,00 1,80
Levulinic Acid (HK) 0,56 0,02 3,62
Where,

4. log[

= log [

From Figure 4.1, we can define N
M
.

Figure 10. Fenske equation for minimum plates expressed in graph form (Source: Gulf, 2002)

From this figure, we can get log N
M
= 1,19 ; so that, N
M
= 15,38 trays 15 trays
5. Defining Nopt/N
M
from Figure 4.2, for finding Nopt.

Figure 11. Relation between optimum-to-minimum ratio and Fenske separation factor (Source: Gulf, 2002)

From this figure, we can get Nopt/N
M
= 1,81, so that Nopt = 1,81 x 15,38 = 27,84 28.By assuming
the tray efficiency is about 85%, we can calculate Nactual as (Nopt/Tray Efficiency), so that we get
Nactual = 33 trays.

6. log[

= log [(

) (

) (

)


After getting this value, we can define Ropt/R
M
from figure 4.3.

Figure 12. Optimum-minimum reflux ratio relationship to the columns feed, distillate, and bottoms
composition (Source: Gulf, 2002)

Based on this figure, if we have log[

] = 5,81 and

, the value R
opt
/R
M
= 1,47.

7. Defining the value of by using Figure 12
The calculated value of

and

= 0,31, then = 1,94

Figure 13. Underwoods vs key ratios in feed (Source: Gulf, 2002)

By using Figure 4.5-4.7, the value of(i.xi
D
)/(i-) will be obtained as:

Figure 14. Underwoods vs parameter for in range 1,01 to 1,11 (Source: Gulf, 2002)


Figure 15. Underwoods vs parameter for in range 1,05 to 3,00 (Source: Gulf, 2002)

Figure 16.Underwoods vs parameter for heavy key and heavier components(Source: Gulf, 2002)

RM + 1 = (i.xi
D
)/(i-) = 7,59
RM = 7,59 1 = 6,59

9. R
opt
= (6,59) x (1,47) = 9,69.

10. Tray Spacing = 0.5 m (Heuristic: Stage spacing range 20 24 inch).

11. Height of Tower

16,66 m
(Heuristic: Maximum column height allowed is 175 ft or 53,025 m, so the result is meeting the
requirements.)

12. Column Diameter

Where

= Maximum allowable vapour velocity, m/s

= Plate spacing

= Maximum vapor rate, kg/s

2,12 m.
13. Plate Design
Column Diameter (D
c
) = 2,12 m
Column Area (A
c
) = D
c
2
/4 = 3,53m
2

Downcomer Area (A
d
) = 0.12 x A
c
= 0,12 x 3,53m
2
= 0,42 m
2

Net Area (A
n
) = (A
c
A
d
) = 3,11 m
2

Active Area (A
a
) = (A
c
2A
d
) = [2,66 (2 x 0,32)] m
2
= 2,69 m
2

Hole Area (A
h
) = 0.1A
a
(10% estimated from active area) = 0,1 2,49= 0,27 m
2
Weir Length is define from Figure 11.31 of Coulson and Richardson Book.
(A
d
/A
c
) x 100% = 12 %
Lw/Dc = 0,76
Lw = 1,61 m.

Figure 17. Relation between downcomer and weir length (Source: Coulson and Richardson, 2002)

Hole Diameter = 0,005 m
Plate Thickness = 0,005 m
Number of Holes = 2,12/(1.965 x 10
-5
) = 107888,00 holes.

14. Plate Pressure Drop
Dry Plate Pressure Drop
Maximum vapor velocity through holes:
U
h(max)
= V
m
/A
h

= 7,59m/s
(A
h
/A
a
)*100 = (0,27/2,69)*100
= 10,04
From Figure 11.34, 6th Ed. Coulson and Richardsons if the (A
h
/A
a
)*100 = 10,04, when plate
thickness to plate diameter is 1, then C
o
= 0.83
h
d
= 51 (U
h
/C
o
)
2
(d
v
/d
l
)
= 51 (7,59/0.83)
2
(1,00/971,05)
= 4,40 mm liquid
Residual Drop
h
r
= 12.5*1000/d
l

= 12.5*1000/971,05
=12,87 mm liquid
h
w
+ h
ow
= 50 + 4,40
= 54,40 mm liquid
Total Plate Pressure Drop
h
t
= h
d
+ h
r
+ (h
w
+ h
ow
)
= 4,40 + 12,87 + 54,40
= 71,67 mm liquid
Pt = 9,81*10
-3
*h
t
*d
l

= 682,73 Pa
=0,68 kPa = 0,10 psi
P
top
= 14,5 psi
P
bottom
= 14,5+ (19*0,10) = 16,50 psi
15. Shell Calculations
Minimum Shell Thickness

in
Therefore, 3/16 in thickness can be used
Selection of Head and Head Thickness Calculation
Torispherical Head

Diameter
OD + (OD/24) + 2 sf + 2/3 icr
= 41,73 + 1,74 + (2*3) + (2/3*4)
= 52,14 in
Weight of Head

= 584,11 lb
Calculation of Axial Stress in Shell

16. Specifications and Operation Condition

Table 10. Specifications and operation condition of distillation column II
1. Type Distillation Column
2. Material Carbon Steel
3. Temperature 170
o
C
4. P
top
14,5 psi
5. P
bottom
16,50 psi
5. Light Key Furfural
6. Heavy Key Levulinic Acid
7. Space between Tray 0,5 m
8. Column Height 16,66 m
9. Column Diameter 2,12 m
10. Column Thickness 0,18 in
11. Plate Thickness 0,005 m
12. Plate Pressure Drop 0,10 psi
13. Hole Valve Tray Size 0,005 m
14. Number Hole Valve Tray 107888,00
15. Hole Area 0,27 m
2

16. Weir Length 1,61 m
17. Column Area 3,53 m
2

18. Net Area 3,11 m
2

19. Active Area 2,69 m
2

20. Price $ 65000














B.3. Distillation Column III (C-103)
1. Stream Composition
Basis = 1 hour, feed = 13749,505 kg/hour
Table 11.Feed, distillate, and bottoms composition
Component Feed (%) Distillate (%) Bottoms (%)
Cellulose 0,02 0,00 0,02
Formic Acid 0,00 0,00 0,00
Furfural 0,00 0,00 0,00
Glucose 0,04 0,00 0,04
Hemicellulose 0,10 0,00 0,10
HMF 0,29 0,00 0,30
Levulinic Acid 3,70 99,75 0,00
Lignin 1,20 0,00 1,25
Sodium Hydroxid 0,00 0,00 0,00
Water 92,75 0,25 96,31
Xylose 1,90 0,00 1,98
100 100 100

2. Temperatures
Dew point of the distillate
Table 12. Dew point of the distillate
Component P m Y X
Levulinic Acid (LK) 1,52 0,00 0,01 0,00
Water (HK) 2308,59 1,00 0,99 1,00
1,00 1,00
Distillate dew point is 104,39
o
C
Where:

Bubble point of the bottom
Table 13. Bubble point of the bottom
Component P (kPa) m Y X
Cellulose 2.42 0,02 0,00 0,00
Formic Acid 2.39 0,02 0,00 0,00
Furfural 0.06 0,00 0,00 0,00
Glucose 0.00 0,00 0,01 0,00
Hemicellulose 2.42 0,02 0,00 0,00
HMF 0.18 0,00 0,00 0,00
Levulinic Acid 0.18 0,00 0,00 0,00
Lignin 2.42 0,02 0,01 0,00
Sodium Hydroxid 0.00 0,00 0,00 0,00
Water 105.15 1,04 0,96 1,00
Xylose 2.42 0,02 0,02 0,00
1,00 1,00
Bottom bubble point is 220,00
o
C.
where,

, so that

162,20
o
C.

3. Relative Volatilities
Relative Volatility of each component is defined base to T
av
= 162,20
o
Cand
HK
as the
base .
Table 14. Relative volatilities of the distillate
Component P m
Levulinic Acid (LK) 1,00 1,00 2,86
Water (HK) 0,56 0,02 1,02
Where,

4. log[

= log [

From Figure 4.1, we can define N
M
.

Figure 18. Fenske equation for minimum plates expressed in graph form (Source: Gulf, 2002)

From this figure, we can get log N
M
= 1,31 ; so that, N
M
= 20,42 trays 20 trays
5. Defining Nopt/N
M
from Figure 4.2, for finding Nopt.

Figure 19. Relation between optimum-to-minimum ratio and Fenske separation factor (Source: Gulf, 2002)

From this figure, we can get Nopt/N
M
= 1,68, so that Nopt = 1,68 x 20,42 = 34,31 34.By assuming
the tray efficiency is about 85%, we can calculate Nactual as (Nopt/Tray Efficiency), so that we get
Nactual = 40 trays.

6. log[

= log [(

) (

) (

)


After getting this value, we can define Ropt/R
M
from figure 4.3.

Figure 20. Optimum-minimum reflux ratio relationship to the columns feed, distillate, and bottoms
composition (Source: Gulf, 2002)

Based on this figure, if we have log[

] = 5,88 and

, the value R
opt
/R
M
= 1,25.

7. Defining the value of by using Figure 4.4
The calculated value of

and

= 0,04, then = 1,79

Figure 21. Underwoods vs key ratios in feed (Source: Gulf, 2002)

By using Figure 4.5-4.7, the value of(i.xi
D
)/(i-) will be obtained as:

Figure 22. Underwoods vs parameter for in range 1,01 to 1,11 (Source: Gulf, 2002)


Figure 23. Underwoods vs parameter for in range 1,05 to 3,00 (Source: Gulf, 2002)

Figure 24. Underwoods vs parameter for heavy key and heavier components(Source: Gulf, 2002)

RM + 1 = (i.xi
D
)/(i-) = 0,49
RM = 0,49 1 = -0,51

9. R
opt
= (-0,51) x (1,25) = -0,6375

10. Tray Spacing = 0.5 m (Heuristic: Stage spacing range 20 24 inch).

11. Height of Tower

20,20 m
(Heuristic: Maximum column height allowed is 175 ft or 53,025 m, so the result is meeting the
requirements.)

12. Column Diameter

Where

= Maximum allowable vapour velocity, m/s

= Plate spacing

= Maximum vapor rate, kg/s

2,05 m.
13. Plate Design
Column Diameter (D
c
) = 2,05 m
Column Area (A
c
) = D
c
2
/4 = 3,31m
2

Downcomer Area (A
d
) = 0.12 x A
c
= 0,12 x 3,53 m
2
= 0,40 m
2

Net Area (A
n
) = (A
c
A
d
) = 2,91 m
2

Active Area (A
a
) = (A
c
2A
d
) = [2,66 (2 x 0,40)] m
2
= 1,86 m
2

Hole Area (A
h
) = 0.1A
a
(10% estimated from active area) = 0,1 1,86= 0,19 m
2
Weir Length is define from Figure 11.31 of Coulson and Richardson Book.
(A
d
/A
c
) x 100% = 12 %
Lw/Dc = 0,76
Lw = 1,56 m.

Figure 25. Relation between downcomer and weir length (Source: Coulson and Richardson, 2002)

Hole Diameter = 0,005 m
Plate Thickness = 0,005 m
Number of Holes = 2,05/(1.965 x 10
-5
) = 104326,00 holes.

14. Plate Pressure Drop
Dry Plate Pressure Drop
Maximum vapor velocity through holes:
U
h(max)
= V
m
/A
h

= 10,79m/s
(A
h
/A
a
)*100 = (0,19/1,86)*100
= 10,22
From Figure 11.34, 6th Ed. Coulson and Richardsons if the (A
h
/A
a
)*100 = 10,22, when plate
thickness to plate diameter is 1, then C
o
= 0.82
h
d
= 51 (U
h
/C
o
)
2
(d
v
/d
l
)
= 51 (10,79/0.82)
2
(1,00/1087,48)
= 8,12 mm liquid
Residual Drop
h
r
= 12.5*1000/d
l

= 12.5*1000/1087,48
=11,49 mm liquid
h
w
+ h
ow
= 50 + 8,12
= 58,12 mm liquid
Total Plate Pressure Drop
h
t
= h
d
+ h
r
+ (h
w
+ h
ow
)
= 8,12 + 11,49 + 58,12
= 77,73 mm liquid
Pt = 9,81*10
-3
*h
t
*d
l

= 829,24 Pa
= 0,83 kPa = 0,12 psi
P
top
= 14,5 psi
P
bottom
= 14,5+ (19*0,12) = 16,78 psi
15. Shell Calculations
Minimum Shell Thickness

in
Therefore, 3/16 in thickness can be used
Selection of Head and Head Thickness Calculation
Torispherical Head

Diameter
OD + (OD/24) + 2 sf + 2/3 icr
= 40,35 + 1,68 + (2*3) + (2/3*4)
= 50,70 in
Weight of Head

= 611,75 lb
Calculation of Axial Stress in Shell

16. Specification and Operation Condition
Table 10. Specifications and operation condition of distillation column III
1. Type Distillation Column
2. Material Carbon Steel
3. Temperature 220
o
C
4. P
top
14,5 psi
5. P
bottom
16,78 psi
5. Light Key Levulinic Acid
6. Heavy Key Water
7. Space between Tray 0,5 m
8. Column Height 20,20 m
9. Column Diameter 2,05 m
10. Column Thickness 0,18 in
11. Plate Thickness 0,005 m
12. Plate Pressure Drop 0,12 psi
13. Hole Valve Tray Size 0,005 m
14. Number Hole Valve Tray 104326,00
15. Hole Area 0,19 m
2

16. Weir Length 1,56 m
17. Column Area 3,31 m
2

18. Net Area 2,91 m
2

19. Active Area 1,86 m
2

20. Price $ 65000



Main Variables in Designing Distillation Column
1. Temperature
Temperature is the variable that is prone to change in the distillation column. Reaction
process in the distillation column temperature must be guarded in order to achieve maximum
process. To keep the temperature in the distillation column then used steam. Temperature sensor
is a thermocouple. Controlled variable is the temperature in the distillation column. Control
parameter is steam flow rate. Temperature is controlled at inlet temperature, bottom temperature,
and distillate temperature.
The literature of optimum sequencing of columns is referenced by King (1980, pp. 711-
720) and Henley and Seader (1981, pp. 527-555). For preliminary selection of near optimal
sequences, several rules can be stated as guides, although some conflicts may arise between
recommendations based on the individual rules. Any recommended cases then may need
economic evaluations.
Perform the easiest separation first, that is, the one least demanding of trays and
reflux, and leave the most difficult to the last.
When neither relative volatility nor concentration in the feed varies widely, remove
the components one-by-one as overhead products.
When the adjacent ordered components in the process feed vary widely in relative
volatility, sequence the splits in the order of decreasing relative volatility.
When the concentrations in the feed vary widely but the relative volatilities do not,
sequence the splits to remove components in the order of decreasing concentration in
the feed.


2. Pressure
Pressure is one of the most important variables in the distillation column. Pressure in the
distillation column is meant to be kept as same as or slightly above atmospheric pressure.
Pressure changes can occur due to input a continuous distillation column and the reaction in the
distillation column. Excessive pressure can affect the quality of the product and can also be
dangerous if the distillation column exploded due to excess pressure. This to prevent excess
pressure distillation column equipped with a relief valve to release the pressure on the
environment. Controlled variable is the pressure in distillation column. When the pressure
exceeds the set point, then the relief valve on the reactor will open thereby releasing the pressure
of the distillation column. Pressure is controlled at top pressure and bottom pressure.
3. Flow Rate
Flow rate in is one of the most important variables to be controlled in a distillation
column. Flow rate in into the distillation column can affect the composition in the distillation
column which will also affect the yield. Besides this flow rate can also affect the height of the
liquid in the distillation column. Sensors are used to measure the flow rate is orificemeter. Then
the flow rate in is controlled by the controller based on set point. Control the flow rate by the
flow control valve (FCV).