BINARY

DISTILLATION
Separation Process Engineering
Chemical Engineering
Universitas Pertamina
2019

Ayu Dahliyanti, M.Eng.

 OUTLINE OBJECTIVES
▪ Key Components ▪ To apply the McCabe-Thiele method
for determining minimum reflux
▪ Distillation Basic Principles ratio, minimum equilibrium stages,
▪ Equipment & Design Specifications number of trays at various operating
conditions.
▪ Design of distillation column: ▪ To estimate overall stage efficiency
McCabe-Thiele Graphical Method
▪ To determine the height and
▪ Estimation of stage efficiency diameter of a trayed tower
▪ Distillation Column Sizing: Tray & ▪ To determine packed height and
Packed Columnh Distillation diameter of a packed column.
• Chapter 7: Seader, Henley and Roper, “Separation Process Principles”,
MAIN 3rd Edition, John Wiley and Sons, Inc., 2011
REFERENCES • Chapter 4: Wankat, "Separation Process Engineering Includes Mass
Transfer Analysis", 3rd Ed., Prentice Hall, 2011
KEY COMPONENTS

 Key Components: The components which

Distillate/
fractional recoveries are specified (the target Overhead
products) at distillate and bottom products.
 The most volatile of the keys is called the Light
Key (LK) and the least volatile is called the Distillation
Heavy Key (HK). Feed Column
 The other components are called non-
keys(NK)
 Determination of key components is important
before proceeding with the calculation Bottom
DETERMINATION OF
KEY COMPONENTS

Column Column Column

1 2 3
LK iC5 C3 iC4

HK nC4 iC4 nC4

DETERMINE
THE KEY
COMPONENTS
OF EACH
COLUMN!
DISTILLATION BASIC PRINCIPLES

 Goals: to produce distillate rich in light key (more

volatile) and bottoms product rich in heavy key (less
volatile) by exploiting their relative volatility (α≠1)
 Dates back to 1st century A.D
 Most common (90%-95%) separation technique in
chemical process industry.
 Very energy intensive
 In the US alone, ~40,000 distillation columns were in
use, accounting for 40% energy consumption by
chemical process industry (Humphrey & Keller, 1997)
 Schematic of 5 stage separators (countercurrent cascade) &
distillation column with T1<T2<T3<T4<T5

DISTILLATION
CASCADE

Distillation column is
basically a cascade
(combination/
arrangement) of multiple
flash separators which
operate at different
temperatures in order
to achieve higher degree
of separation.
DISTILLATION EQUIPMENT

Process at each stage/tray/plate

SELECTION OF COLUMN INTERNALS
COMMERCIAL
BINARY
DISTILLATION
OPERATIONS
BINARY DISTILLATION • RECTIFYING SECTION OPERATING LINE

COLUM DESIGN WITH • STRIPPING SECTION OPERATING LINE

• FEED LINE
MCCABE-THIELE
METHOD
  Specified Variables

DESIGN SPECIFICATIONS

(above feed line)

(below feed line)

Results
(Calculated)
 RECTIFYING SECTION OPERATING LINE
Assumptions: Total Mass Balance:
• The two components have V= L + D
equal & constant latent Component Mass Balance:
heat of vaporization.
• Sensible enthalphy changes
(Cp.dT) and heat of mixing
is negligible compared to
latent heat changes. Since R=L/D and molar flow is constant:
• Insulated column
(adiabatic).
• Column pressure is
Operating line equation:
uniform (no pressure
drop)
RECTIFYING SECTION OPERATING LINE
STRIPPING SECTION OPERATING LINE

Total Mass Balance:

Component Mass Balance:

Since boilup ratio 𝑉𝐵 = 𝑉ഥΤ𝐵 and molar flow is constant:

Operating line equation:

STRIPPING SECTION OPERATING LINE
FEED LINE
(q line)

▪ Rectifying and Stripping

operating line will intersect
at one point.
▪ The intersection if
connected to feed
composition (x=y=z) will
form another operating line
(feed line / q line)
 q → ratio of the increase in molar reflux rate across the feed stage
FEED LINE to the molar feed rate
(q line)
or
Feed conditions
For subcooled liquid & superheated vapor:
consideration
FEED LINE Component Mass Balance Rectifying:

(q line)
Component Mass Balance Stripping:
Using q-line equation to
find intersection of Combine both equations to give:
rectifying & stripping line
Since:
Column overall mass balance:

Mass balance around the feed stage:

Thus, q-line equation becomes:

FEED LINE
(q line)
Feed conditions
consideration
Complete McCabe- • Optimal number of total equilibrium stages (N)
• Optimal feed stage location
Thiele Method • Compositions at each stage Stage ≈ Tray

Rectifying line

Feed/ q-line
No. of stages = 5
(4 + 1partial
reboiler)
Stripping line
LIMITING CASES: Minimum reflux
(Rmin=Lmin/D)
Reflux Ratio (R=L/D)
• N=

Total reflux (L/V=1)

• No product
• F=0
• y=x is the operating line
• N = N min
Total Reflux Minimum Reflux
REVIEW DISTILLATION COLUMN

 Stream and composition

 Operating line
 Total vs minimum reflux
Solution: (a)

a) N min at total reflux

operating line y = x
N min = 6.7
Solution: (b)
b) For partially vaporized feed, q=

q =1 – D/F

Total Mass Balance:

L= D + B
450 = D+B ...(i)
Light Key Mass Balance:
zf.F = xd.D + xb.B
0.6(450) = (0.95)D+(0.05)B ...(ii)
So that:
D = 275 lbmol/h; B =175 lbmol/h; and D/F = 0.611
Solution: (b)
Draw q-line equation:

Slope: 0.637
Intercept :
Point 1 → y=x=zf =0.6
Point 2 → ?
When R=Rmin, q line will intersect equilibrium curve
(x= 0.465, y=0.684)
Find rectifying line equation:

Point 1 (x= 0.465, y=0.684)

Point 2 (x=y=xd=0.95)
Slope: 0.55
Rmin = 1.22
Solution (c)
Since R/Rmin = 1.3
Operating Reflux Ratio = 1.59

Rectifying section operating line:

N = 13.2 (12.2 + 1 partial reboiler)

Optimal feed location : stage 7
REVIEW

 Distillation equipment & nomenclature

 Reflux Ratio
 Boilup Ratio
 Operating Line (how many, how to draw)
 Feed stage location
 Total reflux
 Minimum reflux
 CONDENSER TYPE
• Use coolingTYPE
CONDENSER water or coolant/refrigerant to condense vapor

Total condenser Partial condenser Mixed condenser

• Only liquid distillate • Vapor distillate & liquid • Vapor & liquid distillate
• For reflux drum reflux at equilibrium
pressure up to 215 • Provides extra stage
psia • For reflux drum pressure
215-365 psia
DETERMINATION
OF THE NUMBER
OF STAGES
When using partial
condenser

N = 13.2
(11.2 + 1 partial reboiler + 1 partial
condenser
REBOILER TYPE

Kettle Type (partial reboiler)

• Bottom products in equilibrium with
returning vapor
• Equivalent to 1 equilibrium stage
Kettle type

Vertical thermosyphon type, favored

when:
• Bottom product contain thermally
sensitive compounds
• Bottom pressure is high
• Only small ∆T is available for heat transfer
• Heavy fouling occurs
• Type (B) equal to 1 equilibrium stage

Vertical thermosyphon (A) Vertical thermosyphon (B)

 Qc
CONDENSER HEAT DUTIES
Energy balance around the condenser:

𝑄𝑐 = (𝐷 + 𝐿)∆𝐻

Using McCabe-Thiele assumptions of equal heat of vaporization and

reflux ratio relation (R=L/D):

For total condenser:

For partial condenser

QR
(vapor distillate)
 Qc
REBOILER HEAT DUTIES
Energy balance around the reboiler:

𝑄𝑅 = (𝑉 + 𝐵)∆𝐻

Using McCabe-Thiele assumptions of equal heat of vaporization and

boilup ratio relation (VB=V/B):

For partial reboiler

(liquid bottom product)

QR
EXERCISE
Calculate condenser heat duty and rate of cooling water (T=25oC) needed to
support distillation process in the previous example (total condenser, R = 1.59).
Assume cooling water is heated up to its saturation temperature. Give some
comments regarding the result. Cp water → 4.2 kJ/kg.K
∆H (latent heat) vaporization → Benzene: 394 kJ/kg; Toluene : 351 kJ/kg
DISTILLATION COLUMN SIZING
TRAY COLUMN
PACKED COLUMN
STAGE/TRAY EFFICIENCY (Eo)

Number of theoretical stages

Number of actual stages

Drickamer-Bradford correlation

μ : Feed molar average viscosity at tower

average temperature

𝜇𝑎𝑣𝑒𝑟𝑎𝑔𝑒 = 𝑥𝑖 𝜇𝑖 + 𝑥𝑗 𝜇𝑗
 Relative Volatility (α):
STAGE/TRAY EFFICIENCY (Eo)
O’Connell correlation
μ : Feed molar average viscosity at
tower average temperature

𝜇𝑎𝑣𝑒𝑟𝑎𝑔𝑒 = 𝑥𝑖 𝜇𝑖 + 𝑥𝑗 𝜇𝑗
ASSIGNMENT
Calculate stage efficiency & the
actual number of stages for the
previous example (7.1) using both
methods! Cite all the source you use
to get the data necessary for this
calculation.
DISTILLATION EQUIPMENT

Process at each stage/tray/plate

 Normal operation Downcomer Flooding
Column Height Design Limit
DOWNCOMER FLOODING
• Liquid backflow caused by inadequate downcomer
area
• Rarely occurs when downflow area is at least 10%
of the total area and tray spacing at least 24-in
• 24-in spacing is commonly used & easily maintained.
Smaller spacing is desirable for smaller-diameter
column
Column Height = 4ft above top tray (entrainment removal) +
(Ncolumn x tray spacing) + 10 ft below
bottom tray (bottom surge capacity)

• If height > 250 ft → two or more column arranged

in series is more preferable
• Tallest column: 338 ft (Shell, Texas)
EXERCISE
Calculate distillation column height
from the previous example (7.1),
assume column efficiency is 72%!
 Column Diameter Design Limit
ENTRAINMENT
ENTRAINMENT FLOODING
FLOODING

• Occurs when froth/vapor level

reaches the tray above, then
recycled back to the tray below
• Due to very high vapor rate
and inadequate cross sectional
area
• Reduce separation efficiency
 TRAY COLUMN Obtained from the relation between vapor flow rate, flooding velocity, &
DIAMETER cross sectional area in top & bottom stage

Flooding
1. Calculation of Capacity Parameter (C) in ft/s
capacity (CF)

FHA and CF are obtained by calculating FLV

(kinetic energy ratio)
FHA
 TRAY COLUMN Obtained from the relation between vapor flow rate, flooding velocity, & cross
DIAMETER sectional area in top & bottom stage

1. Calculation of Capacity Parameter (C) in ft/s

• Column diameter is calculated

For simplification, C is sometimes assumed to be equal to CF at both the top & bottom
2. Calculation of superficial velocity (Uf) in ft/s stage condition
• The larger one is used, unless
the difference is significant.

3. Calculation of column diameter (DT) in ft

EXERCISE
Calculate the distillation column diameter from the previous example (benzene-toluene distillation, total
condenser, partial reboiler, R = 1.59). Use top stage data.

Benzene & Toluene density = 49.5 lb/ft3

Step 1: Calculation of Liquid & Vapor density
Liquid Vapor

T=T drum
Average molecular weight of Liquid or Vapor

Specific volume (volume/mol)

 REFLUX DRUM SIZING Using the data of liquid and vapor stream leaving the flash drum

1. Calculation of Capacity Parameter (C) in ft/s Flooding

capacity (CF)
Assume C=CF (use Fig. 6.24)

2. Calculation of flooding velocity (Uf) in ft/s

3. Calculation of drum diameter (DT) in ft

4. Calculation of drum volume (VV) in ft3 4. Check drum height (H) to diameter (DT) ratio

t : residence time (hour); if H > 4DT ;then

Should be at least 5 minutes
PACKED COLUMN INTERNALS Trays are substituted by packing with certain heights

Random packing materials Structured packing materials

 PACKED COLUMN HEIGHTS HETP: Height Equivalent to the Theoretical Plate

HETP METHOD,
from McCabe-Thiele diagram
1) Calculate slope ratio

2) Calculate HOG (height of overall gas transfer unit)

HG = height of gas transfer unit
HL = height of liquid transfer unit
[value depends on packing type;
2) Calculate HETP see Seader Ch. 6.7-6.8]
Example: Calculate packing height from the HETP: Height Equivalent to the Theoretical Plate
previous example of benzene-toluene distillation
END