Flowsheet Separation Train

Separation Train Structure

• To determine the general structure of the

separation train, determine the phase of reactor
effluent.
• For vapor-liquid systems, there are three possible
scenarios
• Assume…
• phase splits are cheapest method of separation
• some type of distillation separation is possible
 Separation Train Structure

• Reactor effluent is liquid

• assume that we only need a liquid separation system,
which may include distillation columns, extraction units,
azeotropic distillation, etc.

liquid liquid
reactor
feeds separation products
system
system

liquid recycle
 Separation Train Structure

• Reactor effluent is 2-phase

• Use the reactor as a phase splitter (or put a flash drum
right after the reactor to separate at a pressure different
from the reaction).

vapor

reactor
feeds liquid
system
 Separation Train Structure

• Reactor effluent is 2-phase

• Send liquid to a liquid separation system.

vapor

liquid liquid
reactor
feeds separation products
system
system

liquid recycle
 Separation Train Structure

• Reactor effluent is 2-phase

• If operating above cooling-water temperature, cool
reactor vapor to 100°F and phase-split.

phase
vapor
split
vapor
liquid

liquid liquid
reactor
feeds separation products
system
system

liquid recycle
 Separation Train Structure

• Reactor effluent is 2-phase

• If the low-temperature flash liquid contains mostly
reactants (an no product components formed as
intermediates in a consecutive reaction), recycle.
phase
vapor
split
vapor liquid

liquid liquid
reactor
feeds separation products
system
system

liquid recycle
 Separation Train Structure

• Reactor effluent is 2-phase

• If the low-temperature flash liquid contains mostly
products, send to liquid separation system.

phase
vapor
split
vapor
liquid

liquid liquid
reactor
feeds separation products
system
system

liquid recycle
 Separation Train Structure

• Reactor effluent is gas

• Cool to cooling water temperature (100°F) and phase split
or completely condense.

vapor

vapor phase
reactor
feeds split
system

liquid
 Separation Train Structure

• Reactor effluent is gas

• Cool to cooling water temperature (100°F) and phase split
or completely condense.

gas recovery
purge
system

vapor

vapor phase
reactor liquid
feeds split
system

liquid

liq sep
system products
liquid recycle
 Separation Train Structure

• Reactor effluent is gas

• Send condensed liquid to liquid recovery system, vapor to
gas recovery system.

gas recovery
purge
system

vapor

vapor phase
reactor liquid
feeds split
system

liquid

liq sep
system products
liquid recycle
 Separation Train Structure

• Reactor effluent is gas

If no phase split is obtained under cooling water,
• can reactor system be pressurized to induce a split
without effecting product distribution?
• If not, consider use of high pressure and a refrigerated
partial condenser.
• If not, consider sending reactor effluent directly to vapor
recovery system.
 Vapor Recovery System Decisions

• What is the best location?

• What is the cheapest type of vapor recovery system?

• Location choices: gas recycle purge

• Purge stream
• Gas-recycle stream
• Flash vapor stream
• none prevent recycle
of certain
prevent loss of
valuable or
components undesirable
material

vapor from
phase split
 Vapor Recovery Systems

• The best location for the VRS is…

• the purge stream if significant amounts of valuable materials are
being lost in the purge
• the gas-recycle stream if materials that are deleterious to the reactor
operation are present
• The flash vapor if both items are important

gas recycle purge

prevent recycle prevent loss of

of certain valuable or
components undesirable
material
vapor from
phase split
 Vapor Recovery Systems

• The types of VRSs available are…

• Condensation (high pressure, low temperature, both)
• Absorption (into liquid-phase)
• Adsorption (onto solid adsorbent, i.e., carbon, zeolite, etc.)
• Membranes (pervaporation, ceramics)
• Reactors (chemical nature of vapor is changed)
 Vapor Recovery Systems

• VRS Strategy
• Design VRS before LRS because each of the VRS processes typically
generates a liquid stream that must be further purified
• Combine the VRS and LRS and feed the reactor effluent directly to
the LRS when
• A partial condenser and flash drum are being considered to phase-split
the reactor effluent and only a small amount of the liquid components
are leaving with the flash vapor
• And the first LRS unit is chosen to be distillation
• Increases distillation column diameter, but increased cost may be less
than costs associated with using a VRS
• No heuristic is available, so this must be considered as a process
alternative
 Liquid Recovery System Desicions

• How should light ends be removed if they contaminate

the product?
• What should be the destination of light ends?
• Should components forming azeotropes with the
reactants be recycled, or should azeotrope be broken?
• What separations can be made by distillation?
• What sequence of columns should be used?
• How should separations be accomplished if distillation
is not feasible?
 LRS - Light Ends

• Alternatives for light-ends disposal

• Drop pressure or increase temperature of a stream, and remove the light
ends in a phase splitter (flash drum).
• Use a partial condenser on the product column.
• Use a stripper (pasteurization) section on the product column or a stripper
(stabilizer column) before the product column.

• Destination light ends

• Vent to flare
• low value
• environmental
• Send to fuel
• Flammable w/ fuel value
• Recycle to VRS
• Valuable
light product
• Introduces another recycle
arrangement of pasteurization section
 LRS – Azeotropes with Reactants

• Recycle azeotropic mixture

• Requires all equipment in the recycle loop be oversized to
handle incremental flow of the extra components

• Break the azeotrope

• Usually requires two columns, one operating at non-
atmospheric pressure
 Applicability of Distillation

• In general, distillation is the least expensive means of

separating mixtures of liquids.
• If the relative volatilities of two components with
neighboring boiling points is less than about 1.1,
distillation becomes very expensive due to:
• Large reflux ratios, corresponding to large vapor rates and Large
column diameters.
• Large condensers/reboilers, corresponding to large utility demands.
• Group such close a neighboring boilers, and treat as a
single component, and develop the best distillation
strategy for this group.
 Column Sequencing

• Alternatives for a ternary mixture

A B
A

A
B
C

C CB
Column Sequencing

As number of components increase, so

do the alternate sequences available to
the designer.

Components 2 3 4 5 6

Sequences 1 2 5 14 42
Column Sequencing

column 1 column 2 column 3 column 4

possible 1 A/BCDE B/CDE C/DE D/E
sequences 2 A/BCDE B/CDE CD/E C/D
for a
3 A/BCDE BC/DE B/C D/E
5-component
separation 4 A/BCDE BCD/E B/CD C/D
5 A/BCDE BCDE BC/D B/C
6 AB/CDE A/B C/DE D/E
7 AB/CDE A/B CD/E C/D
8 ABC/DE D/E A/BC B/C
9 ABC/DE D/E AB/C A/B
10 ABCD/E A/BCD B/CD C/D
11 ABCD/E A/BCD BC/D B/C
12 ABCD/E AB/CD A/B C/D
13 ABCD/E ABC/D A/BC B/C
14 ABCD/E ABC/D AB/C A/B
Column Sequencing

column 1 column 2 column 3 column 4

20 1 A/BCDE B/CDE C/DE D/E
possible 2 A/BCDE B/CDE CD/E C/D
column
3 A/BCDE BC/DE B/C D/E
designs
4 A/BCDE BCD/E B/CD C/D
5 A/BCDE BCD/E BC/D B/C
6 AB/CDE A/B C/DE D/E
7 AB/CDE A/B CD/E C/D
8 ABC/DE D/E A/BC B/C
9 ABC/DE D/E AB/C A/B
10 ABCD/E A/BCD B/CD C/D
11 ABCD/E A/BCD BC/D B/C
12 ABCD/E AB/CD A/B C/D
13 ABCD/E ABC/D A/BC B/C
14 ABCD/E ABC/D AB/C A/B
 Column Sequencing Heuristics

• Remove corrosives as soon as possible.

• Remove reactive components or monomers as soon as
possible.
• Remove products as distillates.
• Remove recycle streams as distillates, particularly if they are
recycled to a packed bed reactor.
 Separation System/Process Interactions

• Selecting the best separation sequence cannnot always be

isolated from the design of the remainder of the process.

• Thus, select the sequence that minimizes the number of

columns in a recycle loop.
 Complex Column Heuristics

• Ease of separation index (ESI)

K A K C a AB
ESI = =
K B K B a BC
• If ESI < 1, A/B split is harder than B/C split
• If ESI > 1, A/B split is easier than B/C split
Column Sequencing

column 1 column 2 column 3 column 4

ESI < 1.6: 1 A/BCDE B/CDE C/DE D/E
2 A/BCDE B/CDE CD/E C/D
40-80%
3 A/BCDE BC/DE B/C D/E
middle
4 A/BCDE BCD/E B/CD C/D
product
5 A/BCDE BCD/E BC/D B/C
6 AB/CDE A/B C/DE D/E
&
7 AB/CDE A/B CD/E C/D
8 ABC/DE D/E A/BC B/C
nearly equal
9 ABC/DE D/E AB/C A/B
amounts of
10 ABCD/E A/BCD B/CD C/D
overhead and
11 ABCD/E A/BCD BC/D B/C
bottom
12 ABCD/E AB/CD A/B C/D
present
13 ABCD/E ABC/D A/BC B/C
14 ABCD/E ABC/D AB/C A/B
 Complex Column Heuristics

• Use the direct sequence if

x AF a AB − 1

x AF + x CF a AC − 1 A B

A
B
C

C
 Complex Column Heuristics

• Use the indirect sequence if

x AF a AB − 1

x AF + x CF a AC − 1 A

A
B
C

C B
 Complex Column Heuristics

• consider a sidestream
• when < 30% of the feed is intermediate
• when xAF and/or xCF < 0.1
• intermediate is recycled, high purity not required
• volatiles are not evenly distributed
• above the feed when the intermediate is more difficult to separate
from the heavy than from the light. Otherwise, consider a
sidestream below the feed.
A
A

B A
A
B
B
C
C
B
sidestream sidestream
rectifier C stripper C
 Other Types of Separations

• If distillation is too expensive, alternatives are commonly

considered;
• Extraction
• Extractive distillation
• Azeotropic distillation
• Reactive distillation
• Crystallization
• Adsorption
• reaction
 Extraction

• Solvent S is added to B/C mixture.

B

C (+B)
B
C

C,S C
 Extractive Distillation

• A heavy component (S) is added to change the VLE. The

heavy component is recycled in the system.
B C

B Example:
C
B = HNO3
C = H2O
S = H2SO4
C,S
 Azeotropic Distillation

• Azeotropes can be broken by

• With 3 columns by addition of a third component
• With 2 columns by changing operating pressure

BCS ternary
Example:
hetrogeneous azeotrope B,C Azeotrope
B = ethanol
C = water
S = benzene

B
C

B B,C C
 Reactive Distillation

• Addition of an entrainer can often react with one of the

components in the mixture that is difficult to separate. The
reaction is then reversed in a second column.

B S
Example:
B & C= xylenes
aBC = 1.03
S = organometallic
B
C aB/CS = 30

C+S C