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0 INTRODUCTION / PURPOSE 3
1 SCOPE 3
2 FIELD OF APPLICATION 5
3 DEFINITIONS 5
4 PRODUCT STRATEGY 5
4.1 General 5
4.2 Market for the Product 6
4.3 Production Costs 7
4.4 Process Technology 7
7 RECYCLE 11
10 REVIEW 24
APPENDICES
TABLES
1 CLASSIFICATION OF MATERIALS 11
FIGURES
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8 HEAT EFFECTS 17
9 EQUILIBRIUM EFFECTS 19
10 KINETIC EFFECTS 21
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
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The starting point can range from a gleam in the eye to a well defined problem,
but always involved is the exploitation of technology to make products via a
combination of chemical or biochemical transformations, physical transformations
and separation processes carried out in appropriate hardware. Unfortunately,
while the scientific principles are fixed and immutable, there is an infinite range of
process steps and conditions that can be devised for each proposed
plant.
The material in this guide draws from the evolutionary procedure developed by
Prof. JM Douglas (University of Massachusetts). An iterative framework of this
kind is essential for rapid screening of potential processes in order to identify
quickly those suitable for more detailed investigation.
GBHE has an impressive record of innovation but it can be improved still further.
The information required to put together a process to make small quantities of a
novel product, or radically improve at large scale manufacture of a well
established product, is best obtained by the collaboration of a number of
disciplines. The different language, style, culture and motivations of the
individuals in these disciplines are powerful if combined in balanced cooperation
and the cooperation is then more likely to maximize the economic potential of the
opportunity.
1 SCOPE
This Guide, one of the series on Reactor Engineering, is intended to help the
multidisciplinary teams at the Research, Development, Engineering and
Marketing interfaces to devise, evaluate and select appropriate process
technologies for a product at any stage in its life cycle.
This Guide does not deal with the selection of raw materials.
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An attempt is made here to list the points of information required at each stage
and briefly indicate their relevance. The list is not exhaustive, comprehensive or
infallible, but a guide to rational evolution and a stimulant to lateral thinking.
The order of the stages may differ from the preference of the reader. This
illustrates not so much the idiosyncrasies of the authors (which are admitted) but
the highly iterative nature of the design procedure. At each stage it is likely that
several process options will exist for further evaluation or later consideration.
Note: No case studies are included. There are many alternative methods
for using this guide. Each team involved in process conception will
probably find that it helps them in different ways to develop their own
insights.
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An attractive process satisfies the criteria set for safety, environment, control,
economics, etc.
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3 DEFINITIONS
For the purposes of this Process Engineering Guide, the following definitions
apply:
Conversion - Moles of a key reactant which have reacted divided by the total
number of moles of the key reactant fed to the reactor.
Yield - Moles of a key reactant transformed into a desired product divided by the
total number of moles of the key reactant which have reacted.
With the exception of proper nouns, terms with initial capital letters which appear
in this document and are not defined above are defined in the Glossary of
Engineering Terms.
4 PRODUCT STRATEGY
4.1 General
New process development should fit into the business strategy for the product.
This requires a shared understanding of the business and technical factors.
GBHE can provide guidance on developing this understanding which enables the
different business interests - R&T, Marketing, Production, and Engineering - to
review the major areas likely to influence the overall scope of a prospective
investment.
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(a) Commercial.
(b) Technology.
(c) Manufacture.
(d) Strategic fit.
The method then develops a series of questions that help the team to increase
their understanding, share information and identify areas of concern.
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There is a need for customers who want to buy the product and they usually
determine the product properties. "Market pull" stems from customers' product
needs, identifying areas of opportunity that can frequently be profitably explored
in conjunction with customers. Answers to the following questions should be
sought.
(1) now;
(2) in 5 years;
(3) in 10 years.
(f) How is the market influenced by different product properties that can be
achieved by varying process conditions?
(g) Price/volume/product property relationship?
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At the process conception stage, the location of a production plant may not be
known. The integration with existing site facilities, e.g. cooling towers, boiler
house, waste treatment plants, may therefore have to be deferred.
The technique implied by this Process Engineering Guide can help in those
market entry studies where a choice of process routes are required to bypass
patents, reduce production costs, use different raw materials, etc.
When the opportunity identified is for a material with particular properties, then in
order to identify candidate products a sequence of manual and database
searches of open, patent and trade literature and property banks is followed by
laboratory research.
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On the basis of the "GBHE", the "input-output structure" of the process (Prof. JM
Douglas) should be set down. See Figure 3.
(a) What are the likely stoichiometric equations and reaction steps?
These will include not only the relationships between feed and desired
products, but also side reactions. Reaction synthesis software will clearly
play a part in future. Fundamental chemical judgment will be needed to sift
the probable from the Possible
.
(b) What is the availability, specification and cost of raw materials?
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(h) Does the process look technically feasible? Are there any novel/unusual
processing steps or equipment that need additional development, and
hence development lead time?
Using this data to estimate a preliminary total production cost, either manually or
preferably using the structured approach of "COMPARE", the dominant
contributions to this cost should now be clear. If this looks potentially acceptable
and the process technology is capable of being developed, proceed through the
iteration. Most processes can be initially ranked at this stage.
The next objective is to decide whether the process will be batch or continuous.
The decision tree (see Figure!4) will help in making a decision when information
has been obtained in the following further areas:
(f) Is there a catalyst? If so, in what form; does it decay? How is spent
catalyst disposal effected safely?
(g) Are there competing reactions and what happens to the unwanted
products?
(h) Is the reaction limited by chemical equilibrium? If so, how can the
limitation be removed?
Now we have to make a preliminary decision about whether the desired reactions
can take place under one set of physical and chemical conditions. There are
obvious capital advantages in minimizing the number of reaction vessels but
there may be operating or production cost benefits in separating reactor systems.
For example, if desirable products can be removed after intermediate stages, or
if a number of desired sequential reactions require very different process
conditions.
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We can now explore the "recycle structure" shown in Figure 5. The objective is to
identify what materials are present in the recycle(s), whether there are any
constraints and to make a first estimate of the recycle rate and composition. In
many cases significant improvements in operational yield can be achieved by
operating at less than maximum conversion per pass and recycling excess feed
material.
For multiple reaction systems there may be several recycle structure options, e.g.
in a two reactor scheme should unconverted material ex-Reactor 2 be recycled to
the inlet of Reactor 1 or Reactor 2?
Listing the components in terms of their normal boiling points gives an immediate
appreciation of the separation problem.
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(a) Is it feasible to isolate the product from the rest of the material? If so,
continue. If not, is the product quality acceptable, or is further
separation/purification required?
(4) If there are different reaction stages, can the same solvent be used in
all of them?
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The first estimate of conversion and yield relationship should be based either on
patent literature or on the Chemist's experiments and preferably based on a
preliminary reaction scheme. The minimum data required is a product yield
spectrum at one conversion. As a very crude first approximation, the conversion-
yield relationship for the desired product could be obtained by joining this point
with 100% yield at zero conversion using a straight line on a log-log plot of
(1-conversion) vs yield. The byproduct yield takes up the balance in the ratios at
the spectrum point.
At this point an initial mass balance of the overall recycle flows for a particular
conversion can be calculated.
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A preliminary structure into which our reactor(s) can be fitted has been defined in
Clause 7. In order to decide on the most appropriate type of reactor configuration
and operating conditions it is important that some understanding is developed of
how the reactions which form products and byproducts are interrelated. At a
preliminary stage an identification of trends, rather than definitive set of reaction
mechanisms is required, in order to gain an insight into the conversion-yield
relationship and the variables that affect it. Laboratory experimentation should
therefore be approached with the aim of answering the question; HOW IS THE
PRODUCT DISTRIBUTION AFFECTED BY:
(c) Pressure.
(f) Heat and mass transfer effects between various phases in the reactor or
across the reactor boundary.
(g) Catalysts/solvents.
When preliminary definition of the process flowsheet has been achieved, very
detailed experiments can be conducted in the likely region of operation, to
provide relevant design data and have accurate descriptions of the performance
of the reaction scheme.
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As far as the process as a whole is concerned, a major decision is how the heat
of reaction is to be handled. If the exotherm / endotherm is significant, there are
three ways of dealing with the situation.
(b) The temperature change can be confined by providing heat capacity in the
process stream.
or
In many cases operation is at some point between the above cases. Figure 8
shows the logic diagram for the key questions to be addressed.
If capacity is provided in the form of a heat carrier then that component has to be
separated and recycled. Choices of a heat carrier include:
(4) An inert material. The amount is minimized if this and reaction conditions
can be chosen such that a latent heat of phase change can be involved.
Modifications of the flows calculated in Clause 7 are also likely from the
consideration of reactor type and operating conditions described in 8.1.
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NOTES:
(3) Localized hot spots within a heat transfer reactor can also approach
equilibrium.
(5) Laboratory reactors may be at low pressure; plant can be high. If the
reaction involves a volume increase, check equilibrium will not limit at the
plant pressures.
Figure 9 shows the logic diagram for the key questions to ask with respect to
equilibrium effects.
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There are five characteristic time scales for a reactor which are relevant; the
reaction half life, the reactor residence time, the interphase mass transfer time,
the heat transfer time and the single phase mixing time. Clearly, the reactor
residence time should equal or exceed the reaction half life, but only if significant
product degradation occurs at longer residence times will the residence time
have to closely match the reaction half life.
The characteristic heat transfer time is usually less than the mass transfer
and can normally be neglected except for highly exothermic reactions. These will
generally require heat transfer within the reactor.
The single phase mixing time <1 second is only important for reaction half life of
this order. Note that for stirred tank reactors the internal recycle time lies
between the mixing and residence time and is often near the reaction half life.
This can affect scale up where in the laboratory:
and an identical reactor system has scaled up from a stirred tank device to a plug
flow with recycle device.
When the interphase mass transfer time is about the reaction half life - and this is
common for gas-liquid reactor systems - then the diffusional and reactive
processes interact strongly and a full analysis of the reaction dynamics is likely to
be required.
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Figure 10 shows the logic diagram for the key questions to ask with respect to
kinetic effects.
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Further background information on the main factors that affect reactor system
design for particular types of reaction mechanism is given in Appendix A.
9 SEPARATION SYSTEM
The selection of the best type of separation for a given duty is a topic which still
requires considerable research. A hierarchy has been proposed subdividing the
separation task into 3 categories, which are likely to be of increasing cost, viz:
For example, Type 1 Separations (filtration, simple vapor-liquid flash) are likely to
be cheapest for chemical, but not necessarily for biochemical, systems. On their
own they may not provide sufficient separation to meet the required specification.
(c) Density.
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In his experiments the Chemist will probably have tried several forms of
separation for extracting the desired product and this also might provide a useful
guide to the means by which full scale separation can best be achieved, through
knowledge of some of the properties that can be exploited.
In the bulk chemical industry large use is made of Distillation (for liquid-liquid
systems) and Filtration/Centrifuging/Drying (for liquid-solid systems). As data are
more readily available for these types of separation they provide useful initial
estimates for the cost of separation.
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A preliminary flowsheet has now been obtained for the process together with
some information on:
After revising the "input data" given in Clauses 4 and 5, Clauses 6-9 should be
repeated using the more detailed information now available.
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11.3 Reactors
11.4 Separation
Fluid Separation.
"A Guide to Capital Cost Estimating", 3rd edition (1988). Institution of Chemical
Engineers.
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There are many books written on chemical reactor design which cover in great
detail the various facets of this subject. At this preliminary stage of process
evaluation we are more concerned with the effect of the reactor system on the
total flowsheet rather than the detailed reactor design. Hence, it is satisfactory to
consider ideal reactors for initial investigation of the process options. This Clause
sets out briefly the main aspects of Reactor System Design.
Where x, y are some indices, not necessarily equal to the stoichiometric ratios.
However, some free radical reactions and most catalytic reactions have rate
equations of the form:-
The term "k1" (reaction rate constant) is given by the Arrhenius equation:-
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A.2 EQUILIBRIUM
And
The above equation immediately shows how, under equilibrium conditions, the
product formation can be increased by changing the relative concentrations in
the reactive medium.
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or, occasionally,
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The proportion of desired product formed in the reaction can often be increased
by improved choice of:
(a) Temperature.
(b) Concentration (including pressure and mass transfer effects and reactor
type/configuration).
If the activation energies (E) of the various reactions are different then changes
in temperature will affect the yields at a given conversion. Increasing temperature
will normally increase reaction rates, hence reduce reaction volume. Sometimes
compromise is necessary.
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Provided the unreacted raw materials can be effectively separated from products
downstream of the reactor the opportunity exists to increase yield by operating at
partial conversion and recycling the unreacted feeds.
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Chemist:
In the pure state all these glycols are solids; NPG melts at 60C and
DCNPG at 75C. Both are soluble in acetic acid, so I ran the reaction in an
acetic acid-water solution at ambient pressure at 80C. This was most
convenient in the laboratory and the reaction went all right.
Engineer:
Why was the acetic acid-water solution used? Is it essential for the
reaction?
Chemist:
I needed to dissolve the solids in something, since it is inconvenient to
blow chlorine through a beaker of solids. I had acetic acid on the lab
bench, and it was used as a solvent by other researchers working with
similar compounds.
Engineer:
Can the reaction be run without a solvent?
Chemist:
I think we need an acid solvent. In fact, the solution needs to be dilute. In
one run using concentrated acid, solids precipitated and fouled up the
reactor.
Engineer:
What would happen if I melted NPG and bubbled Cl2 through the liquid?
Chemist:
It might work, but I prefer the acetic acid.
Engineer:
What would happen if I ran my reaction under pressure?
Chemist:
I don't know because I ran my reactions either under vacuum or at
atmospheric pressure.
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Chemist:
There was a tar-like residue occasionally. But, I was careful to select high
purity reagent grade chemicals to avoid this
Engineer:
Here is a list of materials that might appear in the reactants under process
conditions. What would happen to these? Air? Iron? Closely related
chemicals found in impure feed stock?
Chemist:
Oxygen would have no effect if present at, say, less than l per cent.
Nitrogen have no effect at all. Iron would cause a very bad colour and
should be kept out.
The only close relative to the main reactant that might be in cheaper feed
stock is
(7) What yields were obtained of the product and main byproducts?
How many compounds have been identified in the product, by what
methods, and at what concentrations? How long was the reaction
run? What if the reaction was run for a longer or shorter period?
Chemist:
I got a 60 per cent yield of DCNPG and the remainder was mainly
MCNPG. From past experience I know that 4 to 6 hours is the best
run time. I ran one sample through a gas liquid chromatograph and
found NPG, acetic acid, H20, Cl2, HCl, MCNPG, DCNPG,TCNPG,
four unknowns, plus some tars. The lowest concentration
detectable was 500 ppm.
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Chemist:
The MCNPG would react to the desired product, and not much
would happen to TCNPG, except it might form some residue. I will
try a batch and see what happens.
(8) What are the physical, chemical, safety, and toxic properties of all
the materials involved, including intermediate species that may
occur during reaction?
Chemist:
HCl and Cl2 are dangerous gases, and H2O-HCl mixtures can be
quite corrosive. NPG and DCNPG in dust or powder form would
irritate the lungs. I don't know how toxic the other compounds are.
None are explosive or burn readily.
Engineer:
We will need to know the melting points, boiling points, solubilities
in a variety of solvents, densities, vapor pressure, and so forth of all
compounds, including trace materials. This is critical for
engineering design. What color is the desired product?
Chemist:
It could be white. The least bit of iron colors it brown, and if the
reactors run too long the product has little black particles in it.
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Engineer:
Why recrystallize in acetic acid and why use the ethanol wash? How much
heat is given off? Do you need to use the steam jacket all the time? Would
it be dangerous to bubble in the chlorine gas too fast? What would happen
if liquid chlorine were dumped in with the reactants?
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Engineer:
Could you easily make a run without the acetic acid?
Chemist:
To run without the acetic acid solvent would probably ruin my reactor. I
have grown to like the acetic acid, and anyway it possibly might help
reduce tar formation. If you don't allow acetic acid, how can I recrystallize
the product? What are you going to do, distil the product? Sublime it?
Crystallize it from its melt? These are all difficult to do in my
lab
(10) Do you know of any other reaction paths to the products? Can the
overreacted material be reacted back?
Engineer:
I would really like to see if there is some useful reaction in which I can use
the HCl molecules formed. If not, we have as much waste HCl to dispose
of as we have useful product formed.
DEBRIEFING SESSION
Engineer:
I have looked over the questionnaire and am now considering several
alternatives. If I duplicate your lab procedure at 10,000 pounds per day
production, I would have a mess handling all the dirty acetic acid,
hydrogen chloride, excess chlorine fumes, and dirty ethanol. Quite a bit of
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Now when materials come out of the reactor, they will be NPG, MCNPG,
DCNPG, and TCNPG, and perhaps I will run the reactor at conditions that
give only a small yield of DCNPG and therefore even less TCNPG and
higher residues. I would like to split off the NPG and MCNPG so that they
can be recycled to the reactor, and the TCNPG and higher residues so
that they can be disposed of.Somehow the Cl2 and HCl have to be
separated to recycle the Cl2. What can be done with the HCl? Could we
use that anywhere else in the company?
Can you think of five or six different ways that the NPG-MCNPG mixture
could be removed from the NPG-MCNPG-DCNPG-TCNPG-residue
mixture, and then the DCNPG from the remaining DCNPG-TCNPG-
residue mixture? Maybe the TCNPG-residue mixture should be removed
first?
Should the pure chlorine reactant be too harsh, perhaps nitrogen could be
used as a diluent, since it should be inert. Maybe the HCl byproduct could
be the diluent? It would be nice if the heat of reaction could be used to
melt the solids during recrystallisation. Can't use ordinary equipment since
iron is not allowed anywhere. Maybe I can run the reaction at such high
pressures that the chlorine is a liquid and the HCl is still a gas; then I
would let only the gas out of the reactor, thereby eliminating the HCl-Cl2
separation problem at the source.....
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C.2.1 Introduction
The objective here is to propose a framework for the generation of options for
resolving process mixtures into the desired components and to identify the role of
physical properties and heuristics in identification and evaluation of these
options.
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In general, the introduction of either type of additional material into the separation
process may be made at any stage. The examples 2 and 3 illustrate the ilemma.
Example 2:
(a) Filter, redissolve filter cake in water (either before or after removing residual
EDB).
(b) Add water to the two-phase mixture to dissolve up Reglone and then separate
the resulting two liquid phases.
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The dye stuff will generally be partially soluble. Four options for separation
present themselves:
(1) Add salt to 'salt out' more dye stuffs before filtration and drying.
(2) Filter, add salt to the filtrates to precipitate more material, filter and dry
combined filtered materials.
(3) Concentrate the mixture to precipitate more dye stuff before filtration and
drying.
The first two options are physiochemically identical (without getting into fine
detail) and clearly the second option would introduce unnecessary complexity.
The third and fourth options are not so easy to dismiss on thermodynamic
grounds. "Received wisdom" would dismiss them for other very good reasons.
Option!(4) would be dismissed since plant designed to handle aqueous acidic
solutions is not compatible with organic solvent processing. Drying from solvents
(although thermally more attractive than from water) requires contained plant.
Selective extraction of dye stuff from the byproduct organics is likely to be
adversely affected. Option!(3) would involve evaporative, ultrafiltration/membrane
processes, which whilst theoretically attractive, generate grave operational
difficulties.
These discussions illustrate the need for some strategy in the selection of
processing steps if the combinational explosion is to be contained.
(1) If our physical property assessments tell us that the mixture is resolvable
by mechanical or thermal methods, the way is clear to complete the
separation process.
(2) Some phase distribution processes can generate the required product
states directly (e.g. distillation) but the majority of such operations will, in
general, require subsequent operations to complete the resolution (e.g.
liquid extraction, absorptive processes, crystallization).
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