Chemical Engineering

Laboratory 2

Pre-lab
Experimental number : 4th experiment
 [Experiment 4] 1. Title : Distillation Column

2. Objective

In this experiment by using bench-scale distillation column apparatus, we will try to separate a

mixture of two miscible liquids(distilled water, methanol). Our ultimate goal of this experiment is

understanding the principle of distillation, McCabe-Thiele method and estimate theoretical number of

stages, efficiency, and optimal reflux ratio.

3. Theory

1) Distillation

Distillation is a physical process separating a mixture by preferentially boiling the more volatile

components out of the mixture. When the mixture is heated, the vapor that comes off will be more

volatile material than the liquid phase substances. The resulting vapor will pass into condenser and the

less volatile material will become liquid and collected in a receiver flask. The liquid boils when the

applied pressure equals to the vapor pressure of the liquid. Therefore from the difference of liquid’s

boiling point, we can estimate its volatility. Successful distillation requires several factors : the

difference in vapor pressure of the mixture components, the size of the sample, and the distillation

apparatus. If we repeat distillation process several times, it can give us more purity separation.

However, because of low thermodynamic efficiency, we need to calculate theoretical number of trays

by using McCabe-Thiele method.

(1) Types of Distillation column

‘Simple Distillation’ is used to separate some components which have widely different boiling point.

For simple distillation only single distillation cycle is needed to separate the mixture. Example of

simple distillation is separating water and salt from sea water. Unlike simple distillation ‘Fractional

Distillation’ is used to separate some components which have similar boiling point. For fractional

distillation ‘fractionating columns’ are needed. It provide a large surface area in which the distillate

can repeat condensation and evaporation. Thanks to the fractionating columns, separation can be

improved. Example of fractional distillation is crude oil separation. According to the way how they
operate we can also divide distillation columns as ‘Batch Columns’ and ‘Continuous Columns’.

‘Batch Columns’ is a batch-wise distillation column which is charged with a batch. ‘Continuous

Columns’ processes a continuous feed stream so, it can handle high throughputs.

2) Raoult’s law

Raoult’s law provide a relation between the vapor pressure of a substance and its mole fraction(Eq.1)

in a mixture. If we assume ideal solution mixture of A and B, each substances ratio of partial vapor

pressure to its vapor pressure as a pure liquid is approximately equal to the mole fraction(Eq.2).

d ln p ∆vap H
Moreover by using Clausius-Clapeyron equation (Eq.3 : = 2 ), we can also calculate
dT RT

vapor pressure with temperature.

nA nB
(Eq. 1) x A= , xB= , x + x =1 (n A ,n B: number of A,B moles)
n A +n B n A +n B A B

(Eq. 2) P A =x A∗P A , PB =x B∗PB , PT =P A + P B ( P A , PB : pure A, B vapor pressure)

o o o o

3) McCabe-Thiele method

McCabe-Thiele method is used to calculate ideal number of trays for separation of binary mixture in

the distillation column. There are two basic assumption for this method : Latent heat of vaporization

for each components are equal, Other thermodynamics effects are negligible. From this assumption

we can set the flow rate of liquid and vapor as equal at each trays(Eq.4).

(Eq. 4) : V n−1 ≈V n ≈ V n +1 (Flow rate of vapor), Ln−1 ≈ Ln ≈ Ln+1 (Flow rate of liquid)

(1) Equilibrium Curve

If we assume a binary mixture composed of and , we can

i k
(Equilibrium Curve)

plot equilibrium curve by calculating ‘Relative volatility’. The

relative volatility is expressed as α ik (Eq.7). i means more

<Fig 5. Equilibrium relation curve

for methanol and water>
volatile components and k means less volatile components. From (Eq.9) we can plot equilibrium

curve which is used to calculate for ideal number of trays.

y i /x i y i /x i
(Eq. 6) x i+ x k =1 , y i + y k =1, (Eq. 7) α ik = = (Relative volatility)
y k /x k (1− y ¿¿ i)/(1−x i)¿

α ik xi
(Eq. 8) α ik (1− y ¿¿ i) x i= y i ¿ (1−x i ¿, (Eq. 9) y i= (Equilibrium Curve)
1+(α ik −1)x i

( x i means mole fraction of i in liquid phase, y i means mole fraction of i in vapor phase)

(2) Rectifying section and Stripping section

Rectifying section located at the top of the distillation column where reflux occurs. In this section

there is a condenser and the flow rate of vapor is faster than liquid. If we calculate material balance

and total balance of<Fig.3(left)>, we can get (Eq.10) and (Eq.11). Stripping section, on the other

hand, located at the bottom of distillation column. In this section there is reboiler and the flow rate of

liquid is faster than vapor. If we calculate material balance and total balance of <Fig.5(left)>, we can

get (Eq.12) and (Eq.13).

L D L
(Eq. 10) : V n +1 y n +1=Ln x n + D x D  y n +1= x n+ x D ( <1 ) (Eq. 11) : V =L+ D
V V V
L B L
(Eq. 12) : Lm x m=V m +1 y m +1+ B x B  y m +1= x − x ( >1) (Eq. 13) : L=V + B
V n V B V

<Fig. 3 Rectifying section schematic diagram(left), <Fig. 4 Stripping section schematic diagram(left),
and operating line(right)> and operating line(right)>

(3) Feed Section

At feeding section q means liquid fraction of the feed(Eq.13). By subtracting (Eq.10) and (Eq.12) we

can calculate (Eq.14). Then from (Eq.13) and (Eq.14) we can calculate feed line equation(Eq.15). At

feeding section according to the feed’s state there is 5 cases of feeding section flow. Subcooled
liquid<Fig.9(a)>, saturated liquid<Fig.9(b)>, mixture of saturated liquid and vapor<Fig.9(c)>,

subcooled liquid<Fig.9(d)> and superheated vapor<Fig.9(e)>.

−q xF
<Eq. 13> : LF =qF , V F= (1−q ) F , V +V F=V , L+ LF =L <Eq. 15> : y= x+
1−q 1−q

( D x D +B x B ) LF
V y i=L xi + D x D ( ROL ) −V y i =L x i−B x B ( SOL)  <Eq. 14> : y i= − x
VF VF i

<Fig. 8 Feed line plot> <Fig. 9 Feeding flow change according to feed’s states>
*How to calculate Theoretical number of trays : From ROL, SOL, and feed line equation we can get

theoretical number of trays. (1)On <Fig.5> place point x F , x B , x D (feed, bottom, distillation liquid

phase mole fraction) on x line. (2)Draw ROL passing (x D , y D ) and then draw q-line passing (x F , y F )

. (3)Draw SOL passing (x ¿ ¿ B , y B)¿ and intersection point of ROL and q-line. (4)Starting from

(x D , y D ) draw horizontal line to equilibrium curve and then draw vertical line to x=y line. Repeat this

until meet (x ¿ ¿ B , x B )¿. (5)The number of triangle made by (4) is theoretical number of trays.

(4) Reflux ratio

Reflux is used to separate more purity overhead product. It just condense distilled vapor and return a

portion of condensed liquid to the top of the distillation system. By doing reflux, number of

distillation trays can be reduced and the efficiency can be improved. Therefore setting proper Reflux

Theoretical stage number

ratio is very important. (Stage efficiency : × 100 %)
Real stage number

L
(Eq. 16) : RR ( Reflux ratio ) = (V =L+ D at rectifying section ¿
D

4. Apparatus & Reagent

1) Apparatus

(1) Distillation column (2) Measuring cylinder

<Fig.9 Exp 4 Apparatus distillation column>

100 mL 1ea (3) Triangular flask 100 mL 6ea (4) Specific gravity flask 25 mL(for measuring specific

gravity of materials) (5) Stopwatch (6) Scientific calculator 1ea (7) 20 cm long Ruler

Since I explained about distillation column at ‘Theory’ part, I will briefly explain about the distillation

apparatus<Fig.9>. At ‘Rectifying section’(top) there is a condenser to make vapor to liquid. It is total

condenser so, it is not counted as equilibrium stage. The liquid will be collected in top product vessel

and to save time we will just collect top product from top product vessel not from top product tank.

On the other hand, at ‘Stripping section’(bottom) there is reboiler to make liquid to vapor. It is in

vapor/liquid equilibrium state. Liquid at stripping section will be collected in the bottom product tank.

Also there is feeding section on the middle of this apparatus, and total number of stage is 8.

2) Reagent

5. Experimental Procedures

1) Continuous Distillation Column

(1)Close all valves. (2)Make sure that all switches are turned OFF. (3)Turn on the main power switch

and check all gauges. (4)Charge the Feed-tank with 50 mol% MeOH 10ℓ and open the feed-tank

M w ,MeOH M w , water
valve. (50mol% MeOH 10L mole fraction(1:1) x mole  ×x+ × x= 10L  x
ρMeOH ρwater

=170.7mol, ∴ we need 5.47kg of MeOH) (5)Fill the Reboiler with 10 mol% MeOH 2ℓ. (50mol%

MeOH 10L mole fraction of water and methanol(1: 9) x : 9x mole 

M w ,MeOH M w , water
×x+ × 9 x= 2L  x =9.88mol, ∴ we need 0.316kg of MeOH) (Before fill the tank
ρMeOH ρwater

we have to check if under valve is closed and upper valve is opened) (6)Check the tubes and pipes of

the cooling water supply system (especially leakage) and turn on the system. (7)Activate the reboiler
with the power of 500~600 mA. (8)Control the preheater to set the temperature at 50 mol%-

73.1℃(40 mol%-75.3℃). (9)After the boiling starts, turn on the feed pump. At that time, record the

concentration of the supply liquid. (Before turn on the feed pump and reboiler we have to fill the tank

with solution),(Check the feed flow rate with mass cylinder and stopwatch),(We can control feed flow

rate by controlling feed pump, set feed flow rate as 20mL/min) (10)Reflux all the top product until the

system gets stabilized (about 30 min).(while waiting stabiliztion measure specific gravity of MeOH

and water(by using pycnometer), (1.weigh empty pycnometer, 2.Fill pycnometer with liquid to

overflow, 3.insert stopper, 4.wipe overflowed liquid) (11)Check the surface temperature of condenser

and keep the cooling water to a sufficient level. (12)After 30 min, check each flow meter and when

they are changed, adjust them again. (13)Check whether the liquid is collected in the condensation

tray. At the same time, measure the flow rate for a minute using the stopwatch and the mass cylinder.

(14)Start the reflux pump and set the reflux ratio to 1 using the control knob attached to the pump

(reflux ratio 1 means the amount of flow entered in top production tank are one while amount of

reflux flow which returned in column are 1) (measure reflux flow rate). (15)Check each flow every 30

minutes and adjust them again if they are changed. Every time you do that, take the top and bottom

product samples to measure the concentration. (By using pycnometer) Record the temperature of

rectifying section and stripping section. (16)After the feed pump has started, the experiment will take

almost 3 h (±30 min). (17)After the experiment is over, controls and all knobs should be set to zero,

and all switches turned off. Stop the cooling water supply and throw all the tank liquid. Be careful

when you dump the reboiler liquid because of the high temperature. (Turn off feed pump  reboiler

 reflux pump  wait until liquid is top collected at top product part  turn off equipment power 

drain remaining liquid of all tanks(feed, reboiler, top tank, bottom tank)

** Cautions 1) Liquids in reboiler is very hot so be careful to handle it, 2) Be careful when using
methanol, no skin contact and inhaling are strongly recommended. Should be followed safety rule.

6.Reference

1) McCabe-Thiele. Cho, Jungho. "Continuous Distillation Column Design." Continuous Distillation

Column Design. doi:10.1002/9781118543702.ch8.
2) Distillation. Kister, H. Z. (1992). Distillation design (Vol. 1, p. 340). New York: McGraw-Hill.

3) McCabe-Thiele. "The Separation of a Binary Water/Ethanol Solution via a Continuous Feed

Distillation Column as a Function of Feed Stage Location and Reflux Ratio." International Journal of
Science and Research (IJSR) 4, no. 12 (2015): 807-12. Accessed September 27, 2021.
doi:10.21275/v4i12.nov152084.

4) McCabe-Thiele . 박창호, 김우식, and 정인식. 물질전달 및 분리공정. 1999 (p.55~p.91)

5) Methanol. MSDS 성균관대-연구실안전관리시스템. Accessed September 26, 2021.

https://safety.skku.edu/UserHome/Index?LabNo=0.

6) Water. MSDS. 성균관대-연구실안전관리시스템. Accessed September 26, 2021.

https://safety.skku.edu/UserHome/Index?LabNo=0.

7) Chemical Engineering Laboratory II 2020. Sungkyunkwan University School of Chemical

Engineering, Experiment 4, P.35-41

8) Reflux. Gillespie, Claire. "What Is the Difference Between Reflux & Distillation?" Sciencing.
March 02, 2019. Accessed September 26, 2021. https://sciencing.com/difference-between-reflux-
distillation-5953384.html.