Lecture-V Reaction and Separation System

Download as pdf or txt
Download as pdf or txt
You are on page 1of 54

Bahir Dar Institute Faculty of

of Technology Chemical and Food Engineering

Lecture - V
Integrated Process Design: Reaction and Separation
system synthesis

2014 E.C Nigus Gabbiye Habtu (PhD)


Objectives
• Be able to apply heuristics in selecting separation processes to
separate liquids, vapors, and vapor-liquid mixtures.

• Understand how distillation columns are sequenced and how to


apply heuristics to narrow the search for a near-optimal sequence.

• Understand the importance of selecting reaction paths that do not


involve toxic or hazardous chemicals

• Be able to distribute the chemicals in a process flowsheet, to


account for the presence of inert species, to purge species that
would otherwise build up to unacceptable concentrations, to
achieve a high selectivity to the desired products.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 2


Reaction and Separation system synthesis: Introduction
1. Almost all chemical processes require the separation of chemical species (components), to:
▪ Purify a reactor feed

▪ Recover unreacted species for recycle to a reactor

▪ Separate and purify the products from a reactor

2. Frequently, the major investment and operating costs of a process will be those costs associated
with the separation equipment

❑ Less efficient
Reactor
▪ Less reactor cost
▪ High undesired
❑ High efficient Reactor product formed
▪ High reactor cost ▪ High separation
▪ Less undesired product formed cost
▪ Low separation cost

3. For a binary mixture, it may be possible to select a separation method that can accomplish the
separation task in just one piece of equipment. However, more commonly, the feed mixture
involves more than two components, involving more complex separation systems

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 3


Reaction and Separation system synthesis: General structure of the
separation system
▪ To determine the general structure of the separation system, the phase of the
reactor effluent has to be determined----From the onion mode (R & S)

1. If the reactor effluent is a liquid, we only need a liquid separation system.


This system might include distillation columns, extractions units, azeotropic
distillalion,
Ref: Douglas (1988)

Select from distillation,


enhanced distillation,
stripping towers, liquid-
liquid extraction, etc.

25/03/2022 Lecture on Integrated Process Design by Nigus Gabbiye(PhD) 4


Reaction and Separation system synthesis: General structure of
the separation system
2. If the reactor mixture is a two-phase mixture, we can use the reactor as a phase splitter (or
put a flash drum after the reactor). We send the liquids to a liquid separation system If
the reactor is operating above cooling-water temperature, we usually cool the reactor
vapor stream and phase-spill this stream

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 5


Reaction and Separation system synthesis: General structure of
the separation system
3. If the reactor effluent is all vapor. we cool the stream (cooling-water temperature)
and we attempt to achieve a phase split) or to completely condense this stream.
The condensed liquid is sent to a liquid recovery system. and the vapor is sent to a
vapor recovery system.
Ref: Douglas (1988)

Select from partial


condensation, cryogenic
distillation, absorption,
adsorption, membrane
separation, etc.

Select from
distillation,
enhanced
distillation, stripping
Attempt to cool
towers, liquid-liquid
reactor
extraction, etc.
products using
cooling water

Reactor exit is vapor

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 6


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
• Preliminary Process Synthesis
– The process design involves the synthesis of configurations
that produce chemicals in a reliable, safe and economical
manner, and at high yield with little or no waste.

• Synthesis of chemical processes involves:


– Selection of processing mode: continuous or batch (the
scale of the process is a primary consideration)
– Fixing the chemical state of raw materials, products,
and by-products
– Process operations (unit operations) - flowsheet
building blocks
– Synthesis steps to eliminate the differences – Heuristics

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 7


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

• Process operation in process synthesis

(design and integration)


– Chemical reaction (to eliminate differences in molecular type)

– Mixing and recycle (to distribute the chemicals)

– Separation (to eliminate differences in composition)

– Temperature, pressure and phase change

– Task integration (to combine tasks into unit operations)

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 8


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

• Recall Approaches to chemical process design and integration

– Building an irreducible structure: Mainly Heuristic approach

– Creating and optimizing a superstructure

• Heuristic
– Heuristic rules that expedite the selection and positioning of
processing operations as flowsheets are assembled.

– These rules are based on experience and hold in general, but


should be tested (e.g., by simulation) to ensure that they apply in
the specific application.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 9


Reaction and Separation system synthesis: Heuristics for
Raw actions reaction process synthesis
Raw Materials and Chemical Reactions
Heuristic 1: Select raw materials and chemical reactions to avoid, or reduce,
the handling and storage of hazardous and toxic chemicals.

Example: Manufacture of Ethylene Glycol (EG).

O
1
C2H4 + -2 O2 → CH2 - CH2 (R.1)

O OH OH
(R.2)
CH2 - CH2 + H2O → CH2 - CH2

➢ Since both reactions are highly exothermic, they need to be controlled carefully. But
a water spill into an ethylene-oxide storage tank could lead to an accident similar to
the Bhopal incident. Often such processes are designed with two reaction steps,
with storage of the intermediate, to enable continuous production, even when
maintenance problems shut down the first reaction operation.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 10


Reaction and Separation system synthesis: Heuristics for reaction
process synthesis:
❑ Alternatives to the two-step EG process
• Eliminate the storage tanks(s)
• Use chlorine and caustic in a single reaction step, to avoid
the intermediate

R-3

• As ethylene-oxide is formed, react it with carbon dioxide to


form ethylene-carbonate, a much less active intermediate
that can be stored safely and hydrolyzed, to form the
ethylene-glycol product, as needed:

R-4

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 11


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Distribution of Chemicals
Use an excess of one chemical reactant in a reaction operation to
Heuristic 2: completely consume a second valuable, toxic, or hazardous chemical
reactant.
Example: Consider using excess ethylene in DCE
production

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 12


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Distribution of Chemicals
Heuristic 3: ▪ When nearly pure products are required, eliminate inert
species before the reaction operations, when the separations
are easily accomplished, or when the catalyst is adversely
affected by the inert
▪ Do not do this when a large exothermic heat of reaction
must be removed.

Example:

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 13


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Distribution of Chemicals (Cont’d)

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 14


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

Distribution of Chemicals (Cont’d)

Heuristic 4: ▪ Introduce liquid or vapor purge streams to provide exits


for species that
─ enter the process as impurities in the feed
─ produced by irreversible side-reactions
▪ when these species are in trace quantities and/or are
difficult to separate from the other chemicals.
Example: NH3 Synthesis Loop.

▪ Note: Purge flow rate selection


depends on economics!

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 15


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

Do not purge valuable species or species that are toxic and


Heuristic 5:
hazardous, even in small concentrations.
– Add separators to recover valuable species.

– Add reactors to eliminate toxic and hazardous species.

Example: Catalytic converter in car exhaust system.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 16


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

Heuristic 6: By-products that are produced in reversible reactions, in small


quantities, are usually not recovered in separators or purged.
Instead, they are usually recycled to extinction.

▪ Often small quantities of chemicals are produced in side-reactions.


When the reaction proceeds irreversibly, small quantities of by-
products must be purged, otherwise they will buildup in the process
continuously until the process must be shut down.

▪ When, however, the reaction proceeds reversibly, it becomes


possible to achieve an equilibrium conversion at steady state by
recycling product species without removing them from the process.
In so doing, it is often said that undesired byproducts are recycled to
extinction.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 17


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

Heuristic 7: For competing series or parallel reactions, adjust the temperature,


pressure, and catalyst to obtain high yields of the desired
products. In the initial distribution of chemicals, assume that
these conditions can be satisfied - obtain kinetics data and check
this assumption before developing a base-case design.

Example: Manufacture of allyl-chloride.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 18


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

▪ What range of operating


temperatures favor
production of Allyl Chloride
?

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 19


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
MeOAc Manufacture using Reactive Distillation

Heuristic 8: For reversible reactions, especially, consider conducting them in


a separation device capable of removing the products, and
hence, driving the reactions to the right. Such reaction-
separation operations lead to very different distributions of
chemicals. MeOAc Manufacture using Reactive
Distillation
Example: Manufacture of Ethyl-acetate using MeOAc
reactive distillation.

HOAc

MeOH + HOAc MeOAc + H2O, Reaction
 zone
MeOH
Conventionally, this would call for reaction:
followed by separation of products using a H 2O
sequence of separation towers. MeOH + HOAc
→ MeOAc + H O
 2

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 20


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

Separations!!!

Heuristic 9: Separate liquid mixtures using distillation and stripping


towers, and liquid-liquid extractors, among similar
operations.

Ref: Douglas (1988)

Select from distillation,


enhanced distillation,
stripping towers,
liquid-liquid extraction,
etc.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 21


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Separations(Cont’d)
• Attempt to condense or partially condense vapor
Heuristic 10
mixtures with cooling water. then, use Heuristic 14

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 22


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Separations(Cont’d)
Separate vapor mixtures using partial condensers,
Heuristic 11: cryogenic distillation, absorption towers, adsorbers, and/or
membrane devices.
Ref: Douglas (1988)

Combination of the
previous two flowsheets

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 23


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Separations Involving Solid Particles

• Using multiple evaporators (called effects) in


Heuristic 12: series, the latent heat of evaporation of water is
recovered and reused. With a single evaporator,
the ratio of the amount of water evaporated to
the amount of external steam supplied to cause
the evaporation is typically 0.8. For two effects,
the ratio becomes 1.6; for three effects 2.4, and
so. The magnitude of the boiling-point elevation
(often in the range of 3 to 10 oF) caused by the
dissolved inorganic compounds is a controlling
factor in selecting the optimal number of effects.
When the BPE is small, minimum evaporation cost
is obtained with 8 to 10 effects. When the BPE is
appreciable, the optimal number of effects is
small, 6 or less

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 24


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Separations Involving Solid Particles (Cont’d)

Heuristic 13 • When employing multiple effects, the liquid and


vapor flows may be in the same or different
directions. Use forward feed, where both liquid
and vapor flow in the same direction, for a small
number of effects, particularly when the liquid
feed is hot. Use backward feed, where liquid
flows in a direction opposite to vapor flows, for
cold feeds and/or a large number of effects.
With forward feed, intermediate liquid pumps are
not necessary, whereas they are for backward
feed

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 25


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Heat Transfer in Reactors
▪ Although heat transfer in reactors is better discussed in the context of heat and
power integration, it is treated here because many methods dealing with heat
transfer in reactors also affect the distribution of chemicals. Treated first are
exothermic reactors.

Heuristic 14: To remove a highly-exothermic heat of reaction, consider the


use of excess reactant, an inert diluent, and cold shots.
These affect the distribution of chemicals and should be
inserted early in process synthesis.
excess reactant

an inert diluent

cold shots.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 26


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Heuristic 15: For less exothermic heats of reaction, circulate reactor fluid to an
external cooler, or use a jacketed vessel or cooling coils. Also,
consider the use of intercoolers.

Endothermic reactors are treated similarly:


To control temperature for a highly-endothermic heat of reaction,
Heuristic 16 consider the use of excess reactant an inert diluent, and hot
shots. These affect the distribution of chemicals and should be
inserted early in process synthesis.

For less endothermic heats of reaction, circulate reactor fluid to


Heuristic 17: an external heater, or use a jacketed vessel or heating coils.
Also, consider the use of interheaters.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 27


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis

Heat Exchangers and Furnaces


❑ The usual methods of heat exchange are:
1. Heat exchange between two process fluids using a double-
pipe, shell-and-tube, or compact heat exchanger
2. Heat exchange between a process fluid and a utility, such
as cooling water or steam, using a double-pipe, shell-and-
tube, air-cooled, or compact heat exchanger.
3. High-temperature heating of a process fluid using heat
from the products of combustion in a furnace
4. Heat exchange within a reactor or separator, rather than
in an external heat-exchange device.
5. Direct heat exchange by mixing the two streams that are
exchanging heat. 6. Heat exchange involving solid particles

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 28


Reaction and Separation system synthesis: Heuristics for
reaction process synthesis
Heat Exchangers and Furnaces (Cont’d)

Heuristic 18: • Unless required as part of the


design of the separator or reactor,
provide necessary heat exchange
for heating or cooling process fluid
streams, with or without utilities, in
an external shell-and-tube heat
exchanger using countercurrent
flow. However, if a process stream
requires heating above 750°F, use a
furnace unless the process fluid is
subject to chemical decomposition.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 29


Reaction and Separation system synthesis: General structure of
the separation system

➢ Common Industrial Separation Methods


Separation Phase of the Separating Developed or Separation
Method feed agent(s) added phase principle
Flash L and/or V Pressure reduction V or L difference in
or heat transfer
volatility
Distillation L and/or V Heat transfer or V or L difference in
shaft work
(ordinary) volatility
Gas V Liquid absorbent L Solibilty
absorption
Stripping L Vapor stripping V difference in
agent
volatility
Extractive L and/or V Liquid solvent and V and L difference in
heat transfer
distillation volatility
Azeotropic L and/or V Liquid entrainer V and L difference in
and heat transfer
distillation volatility

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 30


Reaction and Separation system synthesis: General structure of
the separation system
Common Industrial Separation Methods (Cont’d)
Separation Phase of the Separation agent Developed or Separation principle
Method feed added phase

Liquid-liquid L Liquid solvent Second liquid Difference in solubility


extraction
Crystalli-zation L Heat transfer Solid Difference in solubility or
m.p.

Gas adsorption V Solid adsorbent Solid difference in adsorbabililty

Liquid adsorption L Solid adsorbent Solid difference in adsorbabililty

Membrane L or V Membrane Membrane difference in permeability


and/or solubility

Supercritical L or V Supercritical Supercritical Difference in solubility


extraction solvent fluid
Leaching S Liquid solvent L Difference in solubility

Drying S and L Heat transfer V Difference in volatility

Desublimation V Heat transfer S Difference in volatility

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 31


Reaction and Separation system synthesis: General structure of
the separation system
Separation is Energy Intensive

1. Unlike the spontaneous mixing of chemical species, the separation of a mixture of


chemicals requires an expenditure of some form of energy

2. Separation of a feed mixture into streams of differing chemical composition is


achieved by forcing the different species into different spatial locations, by one or a

combination of four common industrial techniques:

▪ the creation by heat transfer, shaft work, or pressure reduction of a second phase
that is immiscible with the feed phase (ESA – energy separating agent)

▪ the introduction into the system of a second fluid phase (MSA – mass separating
agent). This must be subsequently removed.

▪ the addition of a solid phase upon which adsorption can occur (MSA – mass
separating agent)

▪ the placement of a membrane barrier (ESA – energy separating agent)

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 32


Reaction and Separation system synthesis: General structure of
the separation system
Selecting Separation Method (1)
❑ The development of a separation process requires the selection of:
▪ Separation methods

▪ ESAs and/or MSAs

▪ Separation equipment

▪ Optimal arrangement or sequencing of the equipment

▪ Optimal operating temperature and pressure for the equipment

❑ Selection of separation method depends on feed condition :


▪ Vapor: partial condensation, cryogenic distillation , absorption, adsorption, gas permeation
(membranes), desublimation

▪ Liquid: partial vaporization, distillation, stripping, extractive distillation, azeo-distillation,


LL extraction, crystallization , adsorption, membrane separation (dialysis, reverse osmosis,
ultrafiltration and pervaporation), supercritical extraction

▪ Solid: if slurry →filtration, if wet → drying, if dry →leaching

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 33


Reaction and Separation system synthesis: General structure of
the separation system
Selecting Separation Method (2)
▪ The separation factor, SF, defines the degree of separation achievable between
two key components of the feed. This factor, for the separation of component 1
from component 2 between phases I and II, for a single stage of contacting, is
defined as:

C 1I / C 2I C = composition variable, I, II =
SF =
C 1II / C 2II phases rich in components 1 and 2.

▪ SF is generally limited by thermodynamic equilibrium. For


example, in the case of distillation, using mole fractions as the
composition variable and letting phase I be the vapor and phase
II be the liquid, the limiting value of SF is given in terms of
vapor-liquid equilibrium ratios (K-values) as:

 s 
y1 / x1 K1 P1
SF = = = 1,2  = s for ideal L and V 
y2 / x2 K2  P2 

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 34


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns

❑ Distillation sequencing using simple columns:


These simple columns employ:
– One feed split into two products phase;

– Key components adjacent in volatility, or any components

that exist in small quantities between the keys will become

impurities in the products;

– A reboiler and a condenser.

How do we arrange the distillation is a design factor?

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 35


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
• For sharp splits of a three-component mixture (with no azeotropes) we
can either recover the lighted component first or the heaviest component
first, and then we split the remaining two components. Only we have
two option to decide the best!

▪ The lightest component ▪ The heaviest component


What is the criterion to
is taken overhead in taken as bottom product in
each column select among the two??? each column.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 36


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
• Use a sequence of ordinary distillation (OD) columns to separate a
multicomponent mixture provided:
▪  in each column is > 1.05.

▪ The reboiler duty is not excessive.

▪ The tower pressure does not cause the mixture to approach the TC of the
mixture.

▪ Column pressure drop is tolerable, particularly if operation is under vacuum.

▪ The overhead vapor can be at least partially condensed at the column pressure to
provide reflux without excessive refrigeration requirements.

▪ The bottoms temperature for the tower pressure is not so high that chemical
decomposition occurs.

▪ Azeotropes do not prevent the desired separation.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 37


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Pressure/Condenser Determination

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 38


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Number of Sequences for Ordinary Distillation
• A simple distillation column is defined as a column with a single feed, equipped
with a condenser and a reboiler.

• When the process involves the separation of a n-component mixture, there are
different possibilities in the component separation order, each possibility
corresponds to a different column sequence. The number of simple column
sequences(NS,) can be predicted by the formula of (Thompson and King, 1972 )

➢ This is valid for sharp split


▪ A sharp split can be realized when each
[2(P − 1)]! stream is enriched in one component while the
Ns = concentration of the other ones is
P ! (P − 1)! kept below an acceptable limit. In this case, from
a n-component mixture, if n products are
obtained, it is necessary to connect n simple
columns
▪ Reliable design methods, together with trustworthy control systems, made
simple columns sequences the preferred choice in the process industrial practice

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 39


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Number of Sequences for Ordinary Distillation
➢ Number of sequence(NS,) for P − 1 ordinary distillation (OD) columns, NS,
to produce P products:

Component - # of Ns
P Separators
2 1 1
➢ When the number of
3 2 2
components increases, the
4 3 5
number of alternatives
5 4 14
increases very rapidly
6 5 42
7 6 132
8 7 429

1. There may be significant differences in the capital and operating costs between
different distillation sequences
2. Heat integration may have a significant effect on operating costs.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 40


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Example 1: 4 Components: Alternative sequences for the separation of
a four-product mixture. We have five possible sequences

2 4−1 ! 6×5×4×3×2×1
𝑁𝑆 = = =5
4! 4 − 1 ! 4×3×2×1×3×2×1

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 41


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Practical constraints restricting options
1. Safety considerations might dictate that a particularly hazardous component be removed
from the sequence as early as possible to minimize the inventory of that material.

2. Reactive and heat-sensitive components must be removed early to avoid problems of


product degradation.

3. Corrosion problems often dictate that a particularly corrosive component be removed


early to minimize the use of expensive materials of construction.

4. If thermal decomposition in the reboilers contaminates the product, then this dictates that
finished products cannot be taken from the bottoms of columns.

5. Some compounds tend to polymerize when distilled unless chemicals are added to
inhibit polymerization.

6. There might be components in the feed to a distillation sequence that are difficult to
condense.

What are the Heuristics???

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 42


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Best Sequence using Heuristics: The following guidelines are often used
to reduce the number of OD sequences that need to be studied in detail
Heuristic 1. Sequence separation points in the order of decreasing relative volatility
so that the most difficult splits are made in the absence of other components. In
other words, do the most difficult separation last

Heuristic 2. Sequences that remove the lightest components alone one by one in
column overheads should be favored. In other words, favor the direct sequence.

Heuristic 3. A component composing a large fraction of the feed should be removed


first. Sequence separation points that favor near equimolar amounts of distillate
and bottoms in each column. The reboiler duty should not be excessive: In other
words, favor the indirect sequence.

Heuristic 4. Favor splits in which the molar flow between top and bottom products in
individual columns is as near equal as possible.
Heuristic 5. Remove thermally unstable, corrosive, or chemically reactive
components early in the sequence.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 43


Reaction and Separation system synthesis: General structure of
the separation system
• Example 2: Sequencing and distillation process selection

Reaction
product mixture

Feed

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 44


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns

Example 3: Self test Exercise

Question:

Design a sequence of
ordinary distillation
columns to meet the
given specifications.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 45


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Exercise – Possible Solution

➢ Using Heuristic 4, the first


column in position to separate
the key components with the
greatest separation factor (SF).

 Sequence separation points in the


order of decreasing relative volatility
so that the most difficult splits are
made in the absence of other
components.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 46


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
Exercise – Possible Solution
 = 1.5

 = 3.6  = 2.8

 = 1.35

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 47


Reaction and Separation system synthesis: General structure of
the separation system
Distillation sequencing using columns with more Than two
products
N:B:- Single-column sidestream arrangements can be attractive when the middle
product is in excess and one of the other components is present in only minor
quantities. Thus, the sidestream column only applies to special circumstances for
the feed composition.

(a) More than 50% middle component (b) More than 50% middle component
and less than 5% heaviest component. and less than 5% lightest component.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 48


Reaction and Separation system synthesis: General structure of
the separation system
• In case where the lightest and heaviest components are chosen to be the key separation
in the first column. Two further columns are required to produce pure products and the
arrangement is known as distributed distillation or sloppy distillation.

▪ More cost-effective against ▪ If the 2nd and 3rd


utilities, or heat integration column in (a )are
if operated at different operated at same
pressure pressure, it is
prefractionator
▪ Give more degree of
freedom during design

a) Distributed distillation or sloppy distillation b) Prefractionator arrangement


separates nonadjacent key components.

➢ Comparing with a simple column arrangements, the distributed and prefractionator arrangements
typically require 20 to 30% less energy than conventional arrangements for the same separation duty.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 49


Reaction and Separation system synthesis: General
structure of the separation system
• Sharp versus Sloppy Separation

Figure: (a, b) Sharp split sequences,

(c) sloppy split sequence (d) Three component sloppy sequence with a
reduced number of columns

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 50


Reaction and Separation system synthesis: Column
Sequencing- Simple Columns
• In some cases, complex rather than simple distillation columns
should be considered when developing a separation sequence
• .

Ref: Tedder and Rudd (1978)


Distillation sequencing Using thermal
coupling

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 51


Reaction and Separation system synthesis: General structure of
the separation system
• When simple distillation is not practical for all separators in a multicomponent
mixture separation system, other types of separators must be employed and
the order of volatility or other separation index may be different for each
type.

• If they are all two-product separators and if T equals the number of different
types, then the number of possible sequences is now given by:

T P −1
Ns =T Ns

• For example, if P = 3, and ordinary distillation, extractive distillation with


either solvent I or solvent II, and LL extraction with solvent III are to be
considered, T = 4, and applying the above gives 32 possible sequences (for
ordinary distillation alone, NS = 2).

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 52


Reaction and Separation system synthesis: General structure of
the separation system
Distillation Sequencing for Azeotropic Distillation: Three way to
affect azeotropic distillation
1. Change in pressure. The first option to consider when separating a mixture that
forms an azeotrope is exploiting change in azeotropic composition with pressure.
If the composition of the azeotrope is sensitive to pressure and it is possible to
operate the distillation over a range of pressures without any material
decomposition occurring, then this property can be used to carry out a separation.
▪ A change in azeotropic composition of at least 5% with a change in pressure
is usually required.
2. Add an entrainer to the distillation. A mass separation agent, known as an
entrainer, can be added to the distillation. The separation becomes possible
because the entrainer interacts more strongly with one of the azeotrope-forming
components than the other. This can in turn alter in a favorable way the relative
volatility between the key components.

3. Use a membrane. If a semipermeable membrane is placed between the vapor and


liquid phases, it can alter the vapor–liquid equilibrium and allow the separation to
be achieved.

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 53


Reaction and Separation system synthesis: General structure of
the separation system
A. Problem to solved using heuristics

Text Book
Group Chemical Process Design and Conceptual Design of
Integration(Robin Smith)— Chemical Process(James
Chapter 11 M. Douglas) -Chapter 7
I #2 ///
II #6 ///
III #3 ///
IV /// #7.6-4
V #5 ///

25/03/2022 Lecture on Integrated process Design by Nigus Gabbiyev(PhD) 54

You might also like