3.4 & 3.5 Material Balances & Flow Sheet

3.
3 CHEMISTRY &
SEPARATION
PART I
2012 G.P. Towler / UOP. For educational use in conjunction with

Towler & Sinnott Chemical Engineering Design only. Do not copy
Separation Processes
Separation processes are needed for feed pretreatment,
product recovery and waste processing
Most separations are based on moving a component
from one phase to another and then segregating the
two phases
Driven by activity gradient as phases try to reach equilibrium
Affected by rates of mass transfer and heat transfer
G.P. Towler / UOP. For educational use in conjunction with 2012

Separation Specifications
P, yA, yB
Product enriched in A
F, zA, zB
R, xA, xB
Recovery: How much of the desired component

made it to the stream it was supposed to be in:
P yA
P yA
Recovery of A
F z A P yA R xA

Separation Specifications
P, yA, yB
Product enriched in A
F, zA, zB
R, xA, xB
Purity: The concentration of desired component in
the stream it was supposed to be in:
Purity of A in product = yA

Cost
Impact of Separation
Specifications
Tighter specifications
lead to higher cost:
90
99
99.9
99.99
)%(purity
Purity orspecifications
Recovery
Final product must meet
Set by ASTM, USP, etc.
Recycles sometimes have purity specifications

e.g. to protect catalyst from contaminants or poisons
Product that is not recovered is lost profit and also increased

waste cost: separation recovery factors into plant yield

Vapor-Vapor Separations
Membrane
Based on differences in relative
permeability of gases
,Used for H2/CH4, CO2 removal
air separation
Adsorption
Adsorb components selectively on a solid
Regenerate sorbent by temperature swing
(TSA) or pressure swing (PSA)
Used for air separation, H2/CH4, most
separations involving low concentrations
Absorption
Using a liquid solvent
in an absorberstripper loop
Used for acid gases,
drying, water wash
Adsorption
One component from vapor phase preferentially adsorbs
onto the surface of a solid adsorbent
Two types of adsorption:
Reversible:
Usually physisorption
Adsorbed component can be released by decreasing pressure or
increasing temperature
Sorbent can be regenerated and used in multiple cycles, hence
temperature-swing adsorption (TSA) and pressure-swing adsorption (PSA)
Irreversible:
Usually chemisorption
Adsorbed component usually reacts irreversibly with solid
Low concentrations can be achieved, but solid is difficult to regenerate
Used for contaminant removal guard beds

Membrane Separation
Thin membranes of polymer or metal can be used to
separate gases:
Different species diffuse through a thin membrane at different rates:
Different gases have different solubility in metal or polymer
Permeate passes through the membrane and becomes

enriched in faster or more soluble species
Retentate does not pass through membrane and becomes
enriched in slower or less soluble species
Membranes have relatively low cost, but cannot obtain high
purity or recovery
Membranes are therefore widely used for bulk separation of
gases

Asymmetric Membrane
Dense
layer
to 1.0 m 0.1
Porous
support
to 1.0 0.1
mm
(not to scale)
Polymer membranes are usually cast as asymmetric membranes

Thin, dense, active layer is supported on a thicker stronger porous layer
Backing cloth is used in some cases as support for active layer

Hollow Fiber Membranes

Feed
One hollow fiber (of

thousands)
Permeate
Potting
Retentate
Membrane cross
section
Membranes are cast as long thin fibers

A bundle of fibers is set into a resin (potting) that effectively forms a
tubesheet
Feed is fed shell-side and permeate withdrawn from inside the fibers

Flat Sheet (Spiral Wound)

Membranes
Membranes are cast as sheets

Sheets are glued back-to-back along edges to form an
envelope and attached to a perforated tube
The assembly is then rolled up into a spiral-wound module
Gas Separation Membranes

SEM, TEM, STEM can be used
for microscopic analysis
Note asymmetric structure
Thin selective skin
Porous support layer

12-UOP 5565M
Membrane Modules
UOP Separex
modules for rejecting CO2 from natural gas

Vapor-Liquid Separations
Flash
Single stage thermal
phase eqbm&
Evaporation
Single stage removal of
volatile solute or solvent
Distillation
Multiple stage separation
between identified light key
heavy key components&
Fractionation
Separation of
multicomponent
mixture into fractions by
boiling ranges (e.g. in oil
refining)

Absorption
Removal of vapor
component using
non-volatile solvent
Stripping
Multi-stage removal
of volatile solute
from solvent
Multi-stage: see next lecture
See heat exchange lectures
Vapor-Liquid Flash Drums

Flash or knockout drums are widely used in chemical
plants:
Downstream of condensers and coolers
Upstream of compressors and between compressor stages
As reflux drums on columns
In relief systems
Design function is to separate liquid drops from vapor and

prevent vapor blowing out into liquid-filled lines by
maintaining liquid level control
There will usually be ~1 to 2% liquid entrainment in the
vapor from a knockout drum unless a demister is used.
Vertical Flash Drum
Vessel diameter is chosen to

give vapor velocity that is less
than terminal velocity of drops
ut 0.07[)L v(/v]1/2
Use 0.15 ut if there is no

demister
Allow 1 diameter above feed
and at least 0.6 diameters
below feed for settling, also
allow 0.4 diameters for
demister
Height of liquid depends on
level control
Liquid Level Control Bands

Level control needs to allow for some natural
variation in liquid level due to splashing, etc.
Alarms must not be set too close to normal operating
level or they will be a nuisance (& will be ignored)
Operators need time to respond to alarms before
shutdown
A typical assumption is about

2 minutes between alarm
and trip, so allow 10 minutes
of liquid residence time
below feed
But note: midpoint of normal
operating band should be >
Dv/2 below feed point, so if 5
mins of liquid holdup gives
height < Dv/2, use half a
diameter
to
the
midpoint
Towler & Sinnott
Chemical
Engineering
Design only. Doand
not copy
LAHH shutdown trip

LAH alarm
Normal operating band
LAL alarm
LALL shutdown trip
min of 5
liquid or
Dv/2
min 5
of
liquid
Horizontal Flash Drum
Bigger area for settling + more space for liquid holdup

Trade-off is higher plot space and stronger foundations needed to
support vessel
Often used when process control demands some liquid inventory,
e.g. reflux drums
Design is more complex than vertical drum see Ch16
Liquid-Liquid Separations
Decanting
Single stage thermal
phase eqbm&
Extraction
Multi-stage
contacting of two
liquid phases

Mixer-Settler
Single theoretical stage
extraction process
Often 2 or 3 stages are still
cheaper than a column
Membrane
Based on differences in relative
permeability of components
Membrane can be used to keep
two solvents from mixing
Horizontal Decanter
Light
liquid
Vent
Heavy
liquid
Feed
Dispersion
band
Drain
Design is similar to knockout drum: allow droplets to settle and

provide adequate holdup for level control see Chapter 16
Siphon take-off can control level without instruments if densities
are constant
Multistage Extraction:
Sulfolane Process
Used for L/L extraction of

benzene and toluene from
gasoline using sulfolane solvent
3.4 UNIT RATIO MATERIAL

BALANCE
3.5 DETAILED FLOW
SHEET
Process
Classification
Chemical processes can be classified as batch,
continuous or semi-batch and as either
transient or steady state
Batch process is one in which the feed is
charged into the system at the beginning of the
process, and the products are removed all at
once some time later
Continuous process is when the inputs and
outputs flow continuously across the boundaries
throughout the duration of the process.
23
Semi-batch process is a process in which its

inputs are nearly instantaneous but the
outputs are continuous or vice versa
If the values of all process variables in a
process do not change with time, the
process is said to be operating at steady
state. If any changes with time, transient
or unsteady state operation exists
24
One of the main responsibilities of

chemical engineers is to create/construct/
analyse chemical processes (or, at least, to
understand the existing processes)
The layout of a chemical process is called
process flow sheet (PFS) or process
flow diagram (PFD) PFS or PFD can be for
just a single process unit or for the whole
process, either simple or complicated process.
25
Examples of PFS or PFD
PFD for a water-softening by ion-exchange process

26
PFD for Ammonia Synthesis Plant

27
Normally, a PFS or a PFD comprises:

All major process equipments/units
Lines entering or leaving the process/unit and/or
lines connecting two or more process
equipments/units (these lines are called
streams)
Flow rate of each stream
Composition of each stream
operating conditions of each stream and/or
unit/equipment (e.g., T, P)
Energy/heat needed to be added to and/or
removed from any particular part of the process
or the entire process
28
Some important symbols of process

equipments
29
Material Balance
Equation
Material balance are based on :

Law of Conservation of Mass
The law states that mass can neither be
created nor destroyed
Material balance equations are the
manifestation of the law
TOTAL MASS INPUT = TOTAL MASS OUTPUT
The design of a new process or analysis
of existing one is not complete until it is
established that the inputs and outputs
of the process satisfy the material
balance equation.
31
Material Balance
Equation
Suppose methane, is a component of both

input and output of a process
qin(kg CH4/h)
Process
unit
qout(kg CH4/h)
If the flow rates of input and output are found

to be different. Possible explanations are .
1.
2.
3.
4.
methane is leaking
methane is consumed or generated in a reaction
methane is accumulating in the process vessel
wrong measurement
32
General Material Balance

Equation
A balance on a material in a process system
may be written as:
Input + generation - output - consumption =

accumulation
The equation may be written for any material

that enters or leaves any process system
It can be applied to the total mass or total
moles of this material or to any atomic
species involved in the process
33
EXAMPLE: The General Balance Equation

Each year 50,000 people move into a city, 75,000
people move out, 22,000 are born, and 19,000
die.
Write a balance on the population of the city.
SOLUTION Let P denotes people:
Input + generation - output - consumption =
accumulation
Each year the city's population decreases by 22,000

people.
34
Two types of balances may be written for

any system;
differential balances and
integral balances
Differential balances indicate what is

happening in a system at an instant of time.
Each term is a rate and has a unit of
quantity unit per time
Integral balances describe what happens
between two instant of time. Each term of
the equation is an amount of the quantity
with a corresponding unit
35
Balances on Steady- State

Processes
The process is said to be operating at steadystate when all process variables do not change
with time.
The accumulation term in a balance must equal
to zero to ensure that the amount/mass of
material in the process do not change with time
STEADY STATE means ACCUMULATION = 0
Input + generation - output - consumption = 0

Input + generation = output + consumption
36
The generation and consumption

terms
are
applied
only
when
chemical reaction is involved
if there is no reaction,
Input =output
37
Balances on Steady- State Continuous

Processes (Continuous Distillation
Process)
One thousand kilograms per hour of a mixture of benzene
(B)
and toluene (T) containing 50% benzene by mass is separated
by distillation into two fractions. The mass flow rate of benzene
in the top stream is 450 kg B/h and that of toluene in the
bottom stream is 475 kg T/h. The operation is at steady state.
Write balances on benzene and toluene to calculate the
unknown component flow rates in the output streams.
450 kg B/hr
q1 (kg T/hr)
500 kg B/hr
500 kg T/hr
Distillation
475 kg T/hr
q2 (kg B/hr)
38
,no reaction
rate of input = rate of output
450 kg B/hr
q1 (kg T/hr)
500 kg B/hr
500 kg T/hr
Distillation
475 kg T/hr
q2 (kg B/hr)
39
EXAMPLE: Balances on a Batch Mixing

Process
Two methanol-water mixture are contained in separate

flasks. The first mixture contains 40 wt % methanol,
and the second contains 70% methanol. If 200 g of the
first mixture are combined with 150 g of the second,
what are the mass and composition of the product.
40
Flowchart
Draw a flowchart of the process, using boxes
or other symbols to represent process units
(reactors, mixers, separation units, etc.) and lines
with arrows to represent inputs and outputs.
100 mols/hr
C2H6
2100
2000
mols/hr Air
mols/hr
0.0476
mol C2H6/ mol
0.21 mol O2/
mol
0.200
mol O2/
mol
0.79 mol N2/
mol
0.752
mol N2/
mol
41
The chart must be fully labeled with values

of known variables at the locations of the
streams
For example a stream containg 21 mole %

O2 and 79%N2 at 320C and 1.4 atm flowing
at a rate 400 mol/h might be labeled.
42
the total amount or flow rate of the stream and the fractions of each component,
Or directly as the amount or flow rate of each component.
43
Assign algebraic symbols to unknown streams [such as

(kg solution/min), x (lbm N2/lbm), and n (kmol C3H8)]
and write their associated units on the chart
44
When labeling component mass or mole fractions of

a stream the last one must be 1 minus the sum
of the others.
If you are given that the mass of stream 1 is half that
of stream 2, label the masses of these streams m
and 2m rather than ml and m2;
if you know that there is three times as much
nitrogen (by mass) in a stream as oxygen, label the
mass fractions of O2 and N2 y(g O2/g) and 3y(g
N2/g) rather than yl and y2.
If a volumetric flow rate of a stream is

given, convert to mass or molar flow rate
since balances are not normally written in
volumetric quantities
45
Degree of Freedom
Draw and label flow chart
Analysis
Count the unknown variables on
the flow chart,
nunknowns
Count the independent equations relating them,
nindep eqns
ndf = nunknowns - nindep eqns
If ndf = 0, the problem is solvable
If ndf>0, the problem is underspecified, need to
provide more information/equations.
If ndf0, the problem is overspecified, more
equations than unknowns, redundant and
possibly inconsistent information.
46
An experiment on the growth rate of certain organisms

requires an environment of humid air enriched in oxygen.
Three input streams are fed into an evaporation chamber
to produce an output stream with the desired composition.
A: Liquid water, fed at a rate of 20.0 cm 3/min
B: Air (21 mole% O2, the balance N2)
C: Pure oxygen, with a molar flow rate one-fifth of
the molar flow rate of stream B. The output gas is
analyzed and is found to contain 1.5 mole % water. Draw
and label a flowchart of the process, and calculate all
unknown stream variables.
47
48
Flowchart Scaling
Calculation
and
Basis
of
The procedure of changing

the values of all stream
amounts or flow rates by a
proportional amount while
leaving
the
stream
compositions unchanged is
referred to as scaling the
flow chart.
Scaling up: if the final

stream quantities are larger
than the original quantities,
Scaling down: if they are
smaller.
49
Suppose you have balanced a process

and the amount or flow rate of one of
the process streams is n1.
You can scale the flowchart to make
the amount or flow rate of this stream n2
by multiplying all stream amounts
or flow rates by the ratio n2/n1.
50
It is desired to achieve the same separation with a continuous

feed of 1250 lb-moles/h. Scale the flowchart accordingly.
The scale factor is:
51
Before scaling
After scaling
52
Material balance on single

unit process
General Procedure
Calculations
for
Material
Balance
1. Choose as a basis of calculations an amount or flow rate

of one of the process streams
2. Draw a flowchart of the process. Include all the given
variables on the chart and label the unknown stream
variables on the chart
3. Write the expressions for the quantities requested in
problem statement
4. Convert all mass and molar unit quantities to one basis
5. Do the degree of freedom analysis.
For any given
information that has not been used in labeling the
flowchart, translate it into equations in terms of the
unknown variables
6. If nDF = 0, write material balance equations in an order
such that those involve the fewest unknowns are written
first
7. Solve the equations and calculate the additional
quantities requested in the problem statement
8. Scale the quantities accordingly
54
Example :An aqueous solution of NaOH contains

20% NaOH by mass. It is desired to produce an
8% NaOH solution by diluting a stream of 20%
solution with a stream of pure water.
Calculate the ratios (liters H2O/kg feed solution) and
(kg product solution/kg feed solution).
55
NaOH balance (input = output).
mass balance (input = output).
Ratios requested in problem statement.
56

3.4 &amp; 3.5 Material Balances &amp; Flow Sheet

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3.

2012 G.P. Towler / UOP. For educational use in conjunction with

G.P. Towler / UOP. For educational use in conjunction with 2012

Recovery: How much of the desired component

G.P. Towler / UOP. For educational use in conjunction with 2012

G.P. Towler / UOP. For educational use in conjunction with 2012

Set by ASTM, USP, etc.

Recycles sometimes have purity specifications

Product that is not recovered is lost profit and also increased

G.P. Towler / UOP. For educational use in conjunction with 2012

G.P. Towler / UOP. For educational use in conjunction with 2012

Permeate passes through the membrane and becomes

G.P. Towler / UOP. For educational use in conjunction with 2012

Polymer membranes are usually cast as asymmetric membranes

G.P. Towler / UOP. For educational use in conjunction with 2012

Hollow Fiber Membranes

One hollow fiber (of

Membranes are cast as long thin fibers

G.P. Towler / UOP. For educational use in conjunction with 2012

Flat Sheet (Spiral Wound)

Membranes are cast as sheets

Gas Separation Membranes

G.P. Towler / UOP. For educational use in conjunction with 2012

modules for rejecting CO2 from natural gas

G.P. Towler / UOP. For educational use in conjunction with 2012

G.P. Towler / UOP. For educational use in conjunction with 2012

Multi-stage: see next lecture

See heat exchange lectures

Vapor-Liquid Flash Drums

Design function is to separate liquid drops from vapor and

Vertical Flash Drum

Vessel diameter is chosen to

Use 0.15 ut if there is no

Liquid Level Control Bands

A typical assumption is about

LAHH shutdown trip

Horizontal Flash Drum

Bigger area for settling + more space for liquid holdup

G.P. Towler / UOP. For educational use in conjunction with 2012

Design is similar to knockout drum: allow droplets to settle and

Used for L/L extraction of

3.4 UNIT RATIO MATERIAL

Semi-batch process is a process in which its

One of the main responsibilities of

Examples of PFS or PFD

PFD for a water-softening by ion-exchange process

PFD for Ammonia Synthesis Plant

Normally, a PFS or a PFD comprises:

Some important symbols of process

Material balance are based on :

Suppose methane, is a component of both

If the flow rates of input and output are found

General Material Balance

Input + generation - output - consumption =

The equation may be written for any material

EXAMPLE: The General Balance Equation

Each year the city's population decreases by 22,000

Two types of balances may be written for

Differential balances indicate what is

Balances on Steady- State

Input + generation - output - consumption = 0

The generation and consumption

Balances on Steady- State Continuous

EXAMPLE: Balances on a Batch Mixing

3.4 & 3.5 Material Balances & Flow Sheet

3.4 & 3.5 Material Balances & Flow Sheet