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CHE441

Lecture 8: Separation Design

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Layers in the Process Design
Design for overall utility systems
including the plant site
UTILITY SYSTEM
Heat exchanger networking to
HEAT RECOVERY minimize energy consumption
SEPARATION R&D on separation & purification
for product quality, recovery,
REACTION
cost , etc.
CHEMISTRY
R&D on the chemistry for
optimum: conditions,
topologies, type, etc.
BUSINESS
R&D + Economic decision into
which chemical route
A corporate decision into what
business area to FOCUS 2
Separation Design

Purpose of separation
Separate unreacted reactants, byproducts, inert from products
Purify products to meet specification
Recovery toxic or polluted materials
Separation design
Identify the separation requirements
Select separation methods
Size separation units

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Separation Methods Distillation

Distillation is a process of separating the component or substances


from a liquid mixture by selective evaporation and condensation.

Mechanism: different volatility

Operation: heat transfer

Most commonly used in chemical engineering separation

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Separation Methods Gas Absorption

Gas absorption (also known as scrubbing) is an operation a


component is removed from a gas by contacting the gas with
a solvent that dissolves the component selectively. The
solvent is then regenerated in a stripping process and
recycled to the absorber.

Mechanism: different volatility

Operation: mass transfer

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Separation Methods Stripping

Stripping is a physical separation process where one or more


components are removed from a liquid stream by a vapor
stream.

Mechanism: different volatility

Operation: mass transfer

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Separation Methods Liquid-Liquid
Extraction
Liquidliquid extraction also known as solvent extraction and
partitioning, is a method to separate compounds based on
their relative solubilities in two different immiscible liquids,
usually water and an organic solvent. It is an extraction of a
substance from one liquid into another liquid phase.

Mechanism: different solubility

Operation: mass transfer

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Separation Methods Adsorption

Adsorption is the adhesion of atoms, ions, or molecules from


a gas, liquid, or dissolved solid to a surface. This process
creates a film of the adsorbate on the surface of the
adsorbent.

Mechanism: adsorbability

Operation: mass transfer

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Separation Methods Membrane

Membrane separationis a technology which selectively


separates (fractionates) materials via pores and/or minute
gaps in the molecular arrangement of a continuous structure.

Mechanism: Permeability

Operation: mass transfer

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Separation Methods Crystallization

Crystallizationis also a chemical solidliquid separation


technique, in which mass transfer of a solute from the liquid
solution to a pure solid crystalline phase occurs.

Mechanism: Solubility or melting point

Operation: heat transfer

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Example: Select the separation method

Separation requirement Separation method

Preparation of high-purity industrial gases Adsorption (PSA) or Membrane


such as oxygen, nitrogen, hydrogen, etc.

Remove acid gas (CO2, H2S) from flue gas Absorption (amine) (with stripping)

Purify inorganic salts Crystallization

Remove salts from crude oil Liquid-liquid separation

Separate propylene from propane Distillation

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Distillation Column Design

Distillation column operation animation


Separation requirements:
Components
Recovery ratio or composition
Design two factors
Height related to number of trays (2 ft between trays)
Diameter vapor and liquid flow rate

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Basic Understandings Phase Diagram

The Figure on right shows a constant pressure phase


diagram for an ideal solution (one that obey
Raoult's Law)
Note: usually the mole fraction of the more volatile
component is plotted on the horizontal axis,
whereby x is the mole fraction in the liquid phase
and y is the mole fraction in the vapour phase.
1. Temperature range from tA to tB for phase change
2. Different curves for dew point and bubble point
3. Vapor-liquid Equilibrium during phase change and
gives different compositions on vapor and liquid
phase.

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Phase Diagram Example

Benzene-Toluene mixer phase diagram


Could we identify the pure benzene boiling point
and pure toluene boiling point?

Benzene boiling point: 80.1 C


Toluene boiling point: 110.6 C

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Basic Understandings Tray Operation

An ideal plate is one where the vapor leaving the plate is


in equilibrium with the liquid leaving the same plate (see
the equilibrium diagram : xn and yn are in equilibrium).

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McCabe-Thiele Method - Equilibrium
Curve
The Figure (right) showed a typical equilibrium curve for a
binary mixture on x-y plot. It contains less information than the
phase diagram (i.e. temperature is not included), but it is most
commonly used. It is useful for graphical design in determining
the number of theoretical stages required for a distillation
column.
Expressed by relative volatility

For a liquid mixture of two components (called a binary


mixture) at a given temperature and pressure, the relative
volatility is defined as
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Example:

A binary mixer has equilibrium curve as: y = 2.08x / (1+1.08x), whats the
relative volatility? In saturated liquid, if the light component takes 40 mol%,
whats the light component mol% in the saturated vapor at the same T, P?
What are the mol% of the corresponding heavy component in sat. liquid and
vapor?

a = 2.08, Y = 2.08*40% / (1+1.08*40%) = 0.5810. Heavy x


= 60%, Heavy y = 1-0.5810 = 0.419.
a = 0.581/0.4 / (0.419/0.6) = 2.08

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McCabe-Thiele Method - Rectifying
Section Operating Line (ROL)
Overall Mass Balance (Right figure): Vn+1 = Ln + D
Component Balance: Vn+1 yn+1 = Ln xn + D xD
(Ln + D) yn+1 = Ln xn + D xD
Assume
L1 = L2 = .......... Ln-1 = Ln = Ln+1 = L = constant
V1 = V2 = .......... Vn-1 = Vn = Vn+1 = V = constant
Introducing Reflux Ratio R = L / D,

This is the Operating Line Equation for the rectifying section,


or ROL in short.
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McCabe-Thiele Method ROL Slope and
Intercept

(xD, xD) to (0, xD/(R+1))


Slope R/(R+1)
Intercept xD/(R+1)
Draw it with equilibrium curve

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McCabe-Thiele Method Staircase for
theoretical stages
By plotting the operating line on the equilibrium curve, we
can graphically construct using the "staircase" construction
to determine the number of theoretical stages required for
the separation in the rectifying section.

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McCabe-Thiele Method Stripping
Section Operating Line (SOL)
Example: figure out the SOL equation

Overall Mass Balance (Right figure): L = V + B


Component Balance: V ym+1 = L xm + B xB

The stripping operating line (SOL) is straight line


with slope ( L' / L' - B) and intercept ( B xB / L' - B )

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McCabe-Thiele Method Feed Line (q-
line)
Overall material balance: L' = L + q F, V = V' + (1-q) F
Rectifying section : V y = L x + D xD
Stripping section : V' y = L' x - B xB
At the feed point where the two lines operating lines intersect:
( V - V' ) y = ( L - L' ) x + D xD + B xB
V - V' = ( 1 - q ) F
L - L' = - q F
In addition, from component balance around the entire column:
F xF = D xD + B xB
Thus, ( 1 - q ) F y = - q F x + F xF

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McCabe-Thiele Method Feed Line (q-
line)
For a given feed condition, xF and q are fixed,
therefore the q-line is a straight line with slope
-q / (1-q) and intercept xF / (1-q).
If x = xF , then y = xF. i.e. the q-line passes
through the point (xF, xF) on the 45o diagonal.

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McCabe-Thiele Method Three Lines and
Theoretical Stages
The number of theoretical stages is then the
number of triangles that can be drawn between
these operating lines and the equilibrium curve.
The last triangle on the diagram represents the
reboiler.
http://www.separationprocesses.com/Distillation/
DT_Animation/McCabeThiele.html

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McCabe-Thiele Method Examples

How to reach minimal number of theoretical stages?


How to reach minimal reflux ratio?
A binary mixer has equilibrium curve as: y = 2.08x /
(1+1.08x), The feed is saturated liquid, where the
light component takes 40 mol%. If we want the top
product has 99mol% light component, can we
identify the minimal reflux ratio? Draw the lines to
indicate.

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Reflux Ratio vs. Number of Theoretical Trays

Typically the optimum reflux ratio is approximately


1.2 to 1.5 times Rmin
Simulation via software (Aspen plus, Hysys, ProII)
1. Set separation specifications
2. Set theoretical tray number
3. Run the simulation to find reflux ratio
4. Record the tray number and reflux ratio
5. Repeat step 2.
6. Identify reflux ratio from the figure

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Overall Efficiency and Plate Efficiency

Overall column efficiency

A function of viscosity and relative volatility

Murphree plate efficiency

where ye is the composition of the vapor that would be in equilibrium with the
liquid leaving the plate.
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Tray Types

Sieve Plate (Perforated Plate)


Bubble-cap Plates
Valve Plates (Floating-cap Plates)

Cost: Sieve < Valve < Bubble-cap


Turn-down ratio: Sieve < Valve < Bubble-cap

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Plate Liquid Flow Pattern
& Active Area
Liquid flow patterns on cross-flow trays: (a) single
pass; (b) reverse flow; (c) double pass.
An approximate criterion for selecting the liquid flow
pattern is the liquid volumetric flow rate per unit
weir length, which should ideally be in the range 5 to
8 litres/s per m (2 to 3 gpm/in).
Active area (bubbling area): liquid vapor contact
with valve/bubble-cap/hole
For single pass, active area = A 2Ad

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Column Sizing
Plate spacing: 24 or 2 as rule of
thumb.
Column diameter: a function of vapor Plate spacing
flowrate (and liquid flowrate)
Small diameter high vapor flow
prevent liquid flow flooding
Large diameter low vapor flow
liquid drop from holes weeping
Downcomer: area, length, height Downcomer
clearance
Weir height
Weir height

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An Example of Tray Column Design:

Acetone is to be recovered from an aqueous waste stream by continuous


distillation. The feed will contain 10 wt% acetone at 20oC. Acetone of at least 98 wt
% purity is wanted, and the aqueous effluent must not contain more than 50 ppm
(maximum feed 100,000 lb/hr), design the valve tray.
Data:
Latent heat of water = 41,360 J/mol, latent heat of acetone = 28,410 J/mol
Mean specific heats: Cpw = 75.3 J/mol/C, Cpa = 128 J/mol/C

Sinnot, R.K. Coulson & Richardsons, Chemical Engineering. Boston: Butterworth


and Heinemann, 1999

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General Procedure

Known: F, xF, qF, xD, xB.


Step 1: Solve D and B using materials balance.
Step 2: Solve Rmin based on operating curves and equilibrium curves.
Step 3: Determine R and number of theoretical stages.
Step 4: Determine column efficiency and actual number of stages. Estimate
pressure drop across column.
Step 5: Based on L and V as well as physical properties on each stage,
determine column diameter.
Step 6: Determine downcomer area, weir length, height, tray/downcomer
capacity and pressure drop based on valve type.

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Determine D and B

D+B = F
DxD+BxB = FxF

Mole fraction: xF = 0.033, xD = 0.94, xB = 15.5e-6


F = 100,000 lb/hr

D = 10,200 lb/hr
B = 89,800 lb/hr
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Determine Rmin
(x1, y1)

(x1, y1)


(x1, y1) is the pinch point.

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Determine R and number of theoretical
stages
R = 3 Rmin in this case (typically R is only 1.2-1.5 Rmin)
Draw steps to determine Nth
Calculate Eo
Eo = 0.52782 0.27511log10() + 0.044923[log10()]2
= 0.324

Calculate Nr = (Nth-1)/Eo = 46

Pc = 46x0.090x1000x9.81 = 40.6 kPa (90 mm water per tray)


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System factor and try spacing factor

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Preliminary sizing of
Column Diameter
ACFS (actual cubic feet per second = 101
GPM = 228.2
TS = 24
SF = 1
TSF = 1

=3

= 228

Read the Chart to determine the minimum


Column Diameter
Pay attention to the liquid flow passes per
tray

D = 4 ID, SF (single flow) 37


Detailed Sizing

Minimum downcomer area is sized based on

GPM 24 1
Ad = 1.31
175 TS SF

Read Chart D to get chord Height

H = 8

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Detailed Sizing
Read Chart E to get chord Length
Lweir = 3

Bubbling area
Ab = At-Adt-Adb-Ae
At-2Ad = 9.95 sqrt

If tray capacity is less than 85%, the


downcomer area should be increased
until tray capacity downcomer
capacity. This constitutes a balanced
design. 39
Calculate Pressure drop
w e ir h e ig h t
Weir height = 3
Downcomer clearance = 2.5

d o w n c o m e r c le a r a n c e


CFM (air equivalent)
=
= 5078

# of valves per tray = 10x9.95 = 100


40

CFM per valve = 51


Calculate Pressure drop

P due to valve:
Type A: 4.2 in H2O
Type To: 2.0 in H2O

P due to liquid on
tray:
GPM/Lweir=76 GPM/ft
P 2 in liquid
= 2x59.3/62.4
= 1.9 inch H2O

Total P per tray using


type To valve:
P = 3.9 inch H2O
= 99 mm H2O 41
Another Example

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Packed Column for Absorption and
Stripping
Which is absorption? Which is stripping?

Vapor L iq u id Vapor L iq u id
A y A
i
x i
yi

xi yi
xi
y
x
M a s s t r a n s fe r f r o m t h e liq u id M a s s tr a n s fe r fro m th e g a s
to th e g a s p h a s e to t h e liq u id p h a s e

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y out x in y
Absorption Sizing yin O p e r a tin g lin e
y x y out

Absorption driving force: yA yA* G L y A- y A*


yout E q u ilib r iu m c u r v e
Equilibrium curve: y*=mx (linear)
z y in
1
aK y is the total resistance to mass transfer
y in x out x x
based on the gas phase
Given yin, yout, xin, xout, G, L, aKy, m, size the
total height of the tower.
Height of tower = NOGHOG
nOG is the number of overall gas transfer unit
The height of an overall gas transfer unit,
HOG, is defined as

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Example

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