5.

DISTILLATION
18 January 2023 10:53

LINKS : Distillation of Crude Oil & Oil Products - ÜRET Brülör (uret.com.tr)
Tray Distillation Columns - The Engineer's Perspective (theengineersperspectives.com)

---------- Table of Content ----------

 OVERVIEW (Interview purpose)
 Relative Volatility ( 𝛂 𝐀𝐁 )
 Boiling Point Diagrams
 P - T Diagram
 T - x - y Diagram
○ Effect of Pressure on Boiling Point Diagram of Pressure on boiling point diagram
 Analytical method
 Types of Distillation
 Fractional Distillation
○ Rectifying / Enriching Section
 Operating line equation for Rectifying / Enriching Section
 Reflux Ratio(R)
□ Total reflux
□ Operating line equation of enriching section in tearm of Reflux ratio
 Graphical Approach
○ Striping Section
 Operating line equation for Striping Section
 Graphical Approach
 Boiling up Ratio ( 𝐑 𝛎 )
□ Operating line equation of stripping section in tearm of Boiling up ratio
○ Concept of the Minimum Reflux Ratio( 𝐑 𝐦 )/Optimum reflux ratio
 ○ About plates/trays in unit or column
○ Feed Line Equation
□ Method 1
□ Method 2
 Graphical representation of equation of feed
 Variation in reflux ratio with the type of feed
 Feed Quality (q)
 Equation of Feed line
 Batch distillation / Differential distillation / Rayleigh distillation :
 Fenske's Equation
 Efficiency of the column
 Designing Of Distillation Column
 Calculation of diameter of column
 Section 1 : Graphical Determination of Distillation column designing
 Case Study
 (1) Determine process operation variable :
 (2) Determine the minimum reflux ratio 𝐑 𝐦𝐢𝐧 :
 (3) To calculate actual reflux ratio 𝐑 𝐀𝐜𝐭𝐮𝐚𝐥 :
 (3) To calculate Actual/minimum number of trays 𝐍 𝐀𝐜𝐭𝐮𝐚𝐥
 (4) Principle dimension of the column (diameter/height)
○ Calculation of diameter of column : (IIT Kanpur 2023)
○ Pressure drop between two plates
 Tray Tower Operating Problems
 (1) Entrainment
 (2) Flooding
 (3) Weeping
 (4) Dumping
○ How to avoid operating problems
---------------------------------------------------------------------------------------------------------------

OVERVIEW (Interview purpose)

---------
 Distillation :
" Distillation is the separation techaniques of more volatile component from the mixture
of less and more volatile components by partial vaporization of the original solution followed by
condensation."

 Mechanism : difference in boiling point / Relative volatility.

 Applications :
- Organic industries :
○ Ethanol water separation.
○ Aniline and Nitrobenzene separation in the process Aniline production.
- Most common in Petroleum refinery.

- Rajasthan is the largest producer of petroleum in India followed by Gujarat and Assam. Rajasthan has a
share of about 23.29% in crude oil production in the country. In India, oil is found in Assam, Gujarat,
Mumbai High and in the river basins of Godavari and Krishna.

- Venezuela has the largest oil reserves of any country in the world, with more than 300 billion barrels of
proven reserves.
- That is a 17.5% share of the entire global resource, and in 2011 the country surpassed Saudi Arabia to
top worldwide list.
 Distillation unit is divided into the two unit :
- Atmospheric Distillation Unit(ADU)
- Vacuum Distillation Unit (VDU)

- From above picture;

- First we preheat the crude oil to remove impurities such as salt and then sent to the distillation unit.
- In reality, in industries preheat the crude oil and converted into the saturated vapour and then send to
the distillation unit.
- Due to that the energy requirement in distillation unit is less and because of no or less heating the purity
of product will be maintain.

 Why we remove salt or Desalting ?

- Because salt is corrosive in nature.
- Desalting is done by adding hot water and oil together, the salt is soluble in water and oil is insoluble in
nature, oil is float on water.

- In picture there is arrows are called cuts where we get nephtha, kerosene, etc.
- Nephtha, kerosene or all other components are not get easily there will be so many units(mechanism)
are present in arrow.

- In column from top to bottom the boiling point is increases.

- FCC (Fluid Catalytic Cracking) is always connect to the VDU.
- FCC is the heart of refining.

 How to select Crude oil ? ---------

- It is based on TAN(Total Acid Number).
" TAN value is the milligram of KOH required for neutralization of 1 gm of oil sample."

 It is measure with the help of two methods;

(1) potentiometric titration
(2) chromatographic titration
- Second method is not use because the crude is fully black therefore there we will not see and colour
change.
- But cuts (products) are transparent(see colour change) so there we will use chromatographic titration.
- But in reality in refinary mostly method one is use in both cases.
  Low TAN means.....
- Cost ↑
- TAN value < 0.5
- Density ↓
- API(American Petroleum Institute) gravity ↑

 High TAN means.....

- Cost ↓
- TAN value > 1
- Density ↑ (high density means there is wex and sulphur content present in high amount)
- API gravity ↓

- We should purchase crude oil of less than 1 TAN value.

- If oil is heavier then the extrection of products (cuts) such as nephtha, kerosene, etc. Is so difficult.

- Generally PSU's purchase less than 1 TAN value crude oil.

- HPCL purchase 0.5 TAN value crude oil. (means invest cost on raw material)
- Reliance purchase 1.5 TAN value crude oil. (means invest cost on separation units)

 Why we calculate TAN value in cuts(naphthalene, etc.) ?

- In crude oil naphthenic acid is present which boiling point is 220 𝐶 and vapour of this acide is highly
corossive and it will damage units.
- TAN value just give roughly idea about presence of naphthenic acid in cuts.
- In refinary most of the fixed capital is invested(use stainless steel) in units connected just after
distillation unit to separate products like naphthalene, kerosene, etc.

-----------------------------------------------------------------------------------------------------------------

 Relative Volatility (𝛂𝐀𝐁) ---------

- It just signify ease of separation.
- It is also called separation factor for distillation.

- αAB ------> A is More volatile coponent & B is low volatile component

- αBA ------> B is More volatile coponent & A is low volatile component
 In general 𝛂(𝐌𝐕𝐂)(𝐋𝐕𝐂)

 More Volatile Component(MVC) ------> low boiling point ------> High vapour pressure ------> lighter
in nature.
 Less Volatile Component(LVC) ------> high boiling point ------> low vapour pressure -------> heavier
in nature.

- Boiling point of benzene 80.10 C & Tolune 110.60 C at STP.

"It is a ratio of more volatile component(MVC) to less volatile component(LVC) in the

vapour phase to the that in liquid phase."
OR
"It is the ratio of MVC to LVC in different - different phases."

𝐲𝐀

𝛂𝐀𝐁 =
𝐲𝐁
𝐱𝐀
𝐱𝐁

- More volatile component is A & Less volatile component is B.

- yA + yB = 1 -------> yB = 1 - yA & xA + xB = 1 -------> xB = 1 - xA

𝐲𝐀
𝟏 - 𝐲𝐀 𝛂 𝐱
𝛂𝐀𝐁 = 𝐱𝐀 ------OR----> 𝐲𝐀 = 𝟏+(𝛂𝐀𝐁 −𝟏)𝐱
𝐀

𝟏 - 𝐱𝐀 𝐀𝐁 𝐀

 If we take ideal mixture;

- Then Raoul's law : PT yA = xA PA sat & PT yB = xB PB sat

xA PA sat xB PB sat
- From here yA = & yB =
PT PT

yA
yB
- Put value of yA and yB in to αAB = xA
xB

xA PA sat
PT
xB PB sat
PT PA sat 𝐏𝐀 𝐬𝐚𝐭
- αAB = xA = ----------------------> 𝛂𝐀𝐁 =
PB sat 𝐏𝐁 𝐬𝐚𝐭
xB

"Relative volatility is the ratio of the saturation(Sat.) pressure of MVC to the Sat. Pressure of LCV.
 B
- Antoine equation : ln PA sat = A -
T+C

- Form Antoine equation 𝛂𝐀𝐁 is the function of temperatue. (condition is ideal mixture)
- 𝛂𝐀𝐁 is indirectly depend on pressure.

 Partial pressure : pressure exerted by individual composition in mixture.

 Saturation pressure : Pressure at which vapour is in thermodynamic equilibrium with its condensed sate.
Or the pressure of a vapour which is in equilibrium with its liquid (as steam with water).

 NOTE : ---------
 𝛂𝐀𝐁 >> 1 ------> separation is easy
- Here component A outlet from top of the Distillation column and B outlet is bottom of Distillation
column.

 𝛂𝐀𝐁 = 1 -------> there is no separation (both coponents have closest boiling point )

 𝛂𝐀𝐁 << 1 -------> separation is possible

- Here component B outlet from top of the Distillation column and A outlet is bottom of Distillation
column.

 Equilibrium curve :

 Boiling Point Diagrams ---------

 NOTE : In Heat Transfer

- Boiling point elevation(BPE) = B.P. Of solution - B.P. Of water
- If BPE is ↑ then the capacity of evaporator is ↓.
- This both B.P. Is according to pressure into the evaporator.
 - We are represent boiling point elevation with the help of Duhring's plot.

 P - T Diagram :

 Here we can boil feed (F) in 2 ways :

(1) P = Constant and increases the T.
(2) T = Constant and decreases the P.

 T - x - y Diagram : ---------

- yA = More Volatile Component in vapour phase

- xA = More Volatile Component in liquid phase

- Both components(A+B) have different boiling points therefore composition of A & B in liquid phase &
vapour phase is different while heating is apply.

 Calculation of boiling points :

- Given : PT , Antonie constant A, B and C.

B
- ln PA sat = A − and Raoult's law : PT = xA PA sat + (1 − xA )PB sat
T+C

- For pure component A : (xA = 1) -----> PT = PA sat and same for PT = PB sat

- Now we have PT put it in to Antonie equation and find TA & TB .

 Costant pressure Equilibria : ---------

 Why point A is start below and point B is start from top?
- Because point A has MVC so boiling point is low and at point B has LVC so boiling point is higher that A.

 Here initially we know the data of mole fraction of A and B in liquid phase.

- Let take case 1 : At mole fraction of A = 60 & B = 40 we found first bubble in liquid at temperature T1 .

- Now, in case 2 : At mole fraction of A = 80 & B = 20 we found first bubble in liquid at temperature(T2 ),
which is less than T1 .

 From Above 2 cases why boiling point is decreases?

- Because as we increase quantity of MVC the boiling point of mixtur is decreases.

- Now as we increases the quantity of B(LVC) in mixture then the boiling point is increases from right(TA ) to
left side(TB ) in diagram.

"Locus(set of points) of all temperature at which first bubble is formed is called bubble point curve
(T vs x)."

"Temperature at which the first bubble of vapour is formed is called bubble point temperature."

"Temperature at which the last drop of liquid is vaporised is called Due point temperature."
 "Locus of temperature at which last drop of liquid vaporised is called Due point curve (T vs y)."

Space between due point curve and bubble point curve the phase is (Liquid + vapour).

 Tie line : ---------

- It gives the idea about MVC in the vapour phase and MVC in the liquid phase.
- It also gives idea about how much percentage of feed in liquid and vapour.
- It shows at any given temperature the composition of liquid(xA ) and vapour(yA ).
- Every tie line temperature is costant throughout the tie line.
- Number of tie line = number of plates in column
- Tie lines represents the equilibrium composition.

 In diagram at Zf composition the perpendicular line is pass through first tie line and second tie line.
- Here we observe the composition of A in liquid phase xA & vapour phase yA decreases. Why?
- Because if we increases the temperature the MVC is started to vaporise and the xA is decreases in liquid
phase.
- But yA also decreases in vapour phase because we increases the temperature the LVC(B) is also started to
vaporise and the yB is increases in vapour phase therefore the yA is decreases.

 At high pressure condition the curve is shrink(સંકોચવું).

 Objective : To plot the x-y diagram from T-x-y diagram.

- We get equilibrium curve by 3 ways :
(1) Experimentally
(2) Thermodynamic relations (Analytic method)
(3) Published resources.
 - zf = mole fraction of MVC in feed
- Here no. Of tie lines = no. Of points
- This points shows temperature of plates.
- From graph as we move bottom to top "temperature" is decreases.
- Here T4 > T3 > T2 > T1 .
- In x-y diagram gape between curve and diagonal is increases the separation is easy.
- Above diagram is for equimolar[50% A and 50% B] composition.

 Here x-y curve is called equilibrium curve. Why?

- At tie line composition of vapour and liquid are in equilibrium (means at fix temp. And pressure) till you do
not change temp.(T1 ) And pressure.
- As temp. and pressure change your equilibrium get disturbed, now you reach temp.(T2 ) here you will find
another equilibrium(tie line).
- At different-different temp. and pressure you will find different equilibriums.
- By the help of this equilibrium(tie line) we will creat x-y curve therefore it is called equilibrium curve.

 When compositions are not equimolar then the curves : ---------

 Que ask in GATE :

- At Boiling point curve : point A : 𝐙𝐟 = 𝐱 𝐀

- (L+V) region : point B : 𝐲𝐀 > 𝐙𝐟 > 𝐱 𝐀
- At Due point curve : point C : 𝐙𝐟 = 𝐲𝐀

 Effect of Pressure on Boiling Point Diagram of Pressure on Boiling Point Diagram :

Pressure ↑ -------> length of tie line ↓ -------> curve shrink -------> driving force ↓ -------> separation
difficult -------> number of tray ↑ -------> Relative volatility(𝛂) ↓ ------->energy required ↑ ------->
operating cost ↑.

- Therefore we work in low operating pressure.

- Increase in pressure is undesirable condition for distillation.
- At high pressure formation of Azeotropes is starts.
- If we work at same temperature and increase pressure then the driving force is decreases, for same driving
force temperature is also increase along with pressure which increase the duty of reboiler and at the end the
cost of operation is increases.
 - This is the vapour-liquid equilibria at increased pressure.

 Effect of pressure on x-y diagram : ---------

- Equilibrium curve where we get max yA (MVC) in our case yA thta equilibrium curve we will follow and we
1
operate to set that curve's temerature and presuure.
 𝐏 𝟏 < 𝐏 𝟐 < 𝐏 𝟑 < 𝐏 𝟒 < 𝐏 𝟓 | 𝛂𝟏 > 𝛂𝟐 > 𝛂𝟑 > 𝛂𝟒 > 𝛂𝟓

 NOTE : in absorption to get maximum xA the slop of equilibrium curve is minimum.

 Point to be noted :
- Degree of freedom(DOF) = compositions(C) - phases(P) + 2
- For binary mixture : c = 2
- Vapour and liquid phase exist : P = 2
- Then DOF = 2 - 2 + 2 = 2

- Variable present is : Temperature, pressure, liquid composition(x) and vapour composition(y)

- To operate any system you must be done DOF = 0.

- To fix any two variable then DOF will be 0.
- Generally in distillation we fix temperature and pressure (intensive variables) then automatically your x and y
get fixed.
- That's why we does not varying Temperature and pressure both simultaneously.
---------------------------------------------------------------------------------------------------------------
 Analytical method : ---------
QUE : Construct a T-x-y diagram for a mixture of benzene and toluene at 200 kPa. Benzene and toluene
B
mixtures may be considered as ideal. Data : Vapour pressure, Psat , data : ln Psat = A - , where Psat is in
(T+C)
kPa and T is in K.
compound A B C
Benzene (1) 14.1603 2948.78 −44.5633
Toluene (2) 12.2515 3242.38 −47.1806
 Solution :
𝐁
 Step 1 : 𝐥𝐧 𝐏 𝐬𝐚𝐭 = A -
(𝐓 𝐂)

- As we know for ideal mixtures PT = PA sat & PT = PB sat [benzene = A & Toluene = B ]
B
- ln PA sat = A -
(TA +C)

B 2948.78
- TA = -C= - (-44.5633) = 377.3083 K
A − ln PA sat 14.1603 − ln 200

B 3242.38
- TB = -C= - (-47.1806) = 513.4966 K
A − ln PB sat 12.2515 − ln 200
 - Here we get range of boiling point temperature : 377.3083 K to 513.4966 K

B B
 Step 2 : ln PA sat = A - | ln PA sat = A -
(TA +C) (TA +C)

2948.78
- ln PA sat = 14.1603 -
(TA +(−44.5633))

2948.78
∴ ln PA sat = 14.1603 - = 5.3694
(380+(−44.5633))

∴ 𝐥𝐧 𝐏𝐀 𝐬𝐚𝐭 = 214. 734 kPa

3242.38
- ln PB sat = 12.2515 -
(TA +(−47.1806))

3242.38
∴ ln PB sat = 12.2515 - = 2.50934
(380+(−47.1806))

∴ 𝐏𝐁 𝐬𝐚𝐭 = 12.2968 kPa

- As we know Dalton's law : 𝐏𝐓 = ∑ 𝐏𝐢

PT = PA + PB
∴ 𝐏𝐓 = 𝐱 𝐀 𝐏𝐀 𝐬𝐚𝐭 + 𝐱 𝐁 𝐏𝐁 𝐬𝐚𝐭 [Raoult's law]
∴ PT = xA PA sat + (1 − xA )PB sat

PT − PB sat 200 − 12.2968

- xA = = = 0.9272
PA sat − PB sat 214.734 − 12.2968

○ Raoult's law : Pi = Pi saturated xi | Dalton law : Pi = yi PTotal combine to gether

- 𝐏𝐓 𝐲𝐀 = 𝐱 𝐀 𝐏𝐀 𝐬𝐚𝐭

xA PA sat 0.9272 ×214.734

∴ yA = PT
== 200
= 0.99551

- Same way find for other temperatures and put all the values in below table.

 Step 3 : construct the table

sat
Temperature ln PA ln PB sat xA yA

380 214.734 12.2968 0.9272 0.9955

 400 352.1650 21.3613 0.5400 0.9508
420 547.8674 34.9732 0.3218 0.8815
440 815.0736 54.4551 0.1913 0.7796
460 1167.097526 81.2285 0.1094 0.6384
480 1616.9450 116.7693 0.05548 0.4485
500 2176.9477 162.5643 0.01858 0.2022

 Step 4 : Graph

-----------------------------------------------------------------------------------------------------------------

Types of Distillation
---------
(1) Fractional Distillation
(2) Flash Distillation
(3) Batch Distillation
(4) Steam Distillation
(5) Vaccume Distillation
(6) Azeotropic Distilation.

 Fractional Distillation :
 - Investment in fractional distillation column is high but get better quality of product.
- It work at high temperature so we do not use temperature sensitive material.

 Condenser is a heat exchanger which is used to condense gaseous substance into liquid by the process of
cooling.
- Here we are use condenser which have two types :
(1) Partial Condenser (2) Total condenser

Partial Condenser Total Condenser

• Cooling water requirement (Duty) is less in this • Cooling water requirement (Duty) is higest in this
case. case.
• As Duty is less, operating cost is also less. • As Duty is very high, operating cost is also very
high.
• It acts as an ideal stage. • It does not act as an ideal stage.
• In this case, product obtained is in vapour form • In this case, product obtained is in liquid form
which is very difficult to transport, handle and which is easy to transport, handle and store.
store.
 Out of partial condenser & total condenser we use the one which fulfil our requirement in the optimum cost.
- Case 1 : If cost of condensation > cost of transportation then we use partial condenser because in this case
we have to condense only partially which decreases the requirement of cooling water.

- Case 2 : If cost of condensation < cost of transportation then we use total condenser because here we have
to transport liquid & liquid transportation is much easy and cheaper than vapour transportation.

- Partial condenser act as stage where inlet concentration and outlet concentration are not same, means
separation happen. Were as in total condenser inlet concentration and outlet concentration are same, so
there is no separation happen.

- Partial condenser product is (Liquid + Vapour) mixture, therefor the space required for storage of vapour is
large, where as in Total condenser product is pure liquid, so space required is less than the vapour.

- In 99% of cases we use total condenser.

- As we discuss partial condenser act as stage, during calculation we include that stage means Nm+2 not Nm+1 .
- Here in Nm+1 ---> 1 is show partial reboiler and Nm+2 ---> 2 is shows (partial reboiler + partial condenser).

 Notations : ---------
- F = feed flowrate
- D = Distillate flowrate
- W = Bottom flowrate
- xf = Mole fraction of MCV in the feed
- xD = Mole fraction of MCV in the distillate
- xw = Mole fraction of MCV in the bottom
- (1 − xf ) = Mole fraction of LCV in the feed
- (1 − xD ) = Mole fraction of LCV in the distillate
- (1 − xw ) = Mole fraction of LCV in the bottom

 According to Mc-CABE AND THIELE Method :

- L = Liquid flowrate in Rectifying/Enriching section
- V = Vapour flowrate in Rectifying/Enriching section
- L = Liquid flowrate in Stripping section
- V = Vapour flowrate in Stripping section
 To calculate number of trays analytically there are two methods are used :
(1) Mc-CABE AND THIELE Method -------> Easy method but less efficient compart to method2
(2) PONCHON AND SAVARIT Method -------> hard method but efficient the method 1.

 We do Calculation According to Mc-CABE AND THIELE Method :

○ Assumptions :
(i) Enthalpy is constant -----> do not require enthalpy data.
(ii) The molal heat of vaporization of the two components are equal (When one mole of the heavier
component is vaporised, one mole of the lighter component is condensed).
(iii) For every mole of liquid vaporized, a mole of vapour is condensed.
(iv) Other thermodynamics effects are negligible, e.g. Heat effects such as heats of solution, heat of
dissolution and heat transfer to and from the distillation column are negligible.
(V) The mixture is binary i.e. there are only two components.

- 100% tray efficiency. Trays calculated using the McCabe-Thiele method are called "theoretical trays". In
practice fluids do not reach equilibrium on each tray, and so the "tray efficiency" is used to determine the
number of actual trays required to make a given separation.

 Overall Balance : F = D + W
 Component Balance : F.xf = D.xD + W.xW

- If our feed is (L+V) the it enter from middle of section.

- If our feed is (L) the it enter from top of section.
- If our feed is (V) the it enter from bottom of section.

 Rectifying / Enriching Section : ---------

 Operating line equation for Rectifying / Enriching Section :
 NOTE : Plate always count from top of the section.
- In the section transfer of solute occurs but flowrate will not be change.

th
 Calculation for nth & (n + 1) plate :
- Overall Balance : Vn (vapour coming from top) = L(back to column) + D (distillate)
- Component Balance : Vn+1 . yn+1 = Ln . xn + D. xD

- Apply assumption : L1 = L2 = Ln = L | V1 = V2 = Vn+1 = V

∴ V. yn+1 = L. xn + D. xD

𝐲𝐧+𝟏 = 𝐕𝐋 . 𝐱𝐧 + 𝐃𝐕 . 𝐱𝐃 it is operating line equation of Enriching section.

- Compare with Y = MX + C

𝐃 𝐋
C (intercept) = . 𝐱 𝐃 | Slope :
𝐕 𝐕

---------------------------------------------------------------------------------------------------------------
QUE : A binary distillation column is designed by Mc-Cabe Thile method to get a distillate mole fraction of
0.9. the enriching section operating line has an intercept with y-axis at 0.3 mole fraction. The ratio of liquid
to vapour molar flowrate in the enriching section is __________ (rounded off to third decimal place).
[GATE : 2018 IIT Guwahati]
 Solution :
D D 1
- Given : (intercept) = . xD = 0.3 & xD = 0.9 ---------> =
V V 3

- Overall Balance : V = L + D
L D
∴1 = +
V V
 𝐋 𝟐
∴ = = 0.67
𝐕 𝟑
---------------------------------------------------------------------------------------------------------------
▪ Reflux Ratio(R) : ---------
- It is just showing return upon withdraw.

𝐑𝐞𝐭𝐮𝐫𝐧 (𝐋)
R=
𝐰𝐢𝐭𝐡𝐝𝐫𝐚𝐰 (𝐃)

Case 1 : Total reflux (D=0, F=0, W=0) -----> R⟶ ∞

Case 2 : Minimum Reflux (L⟶ 𝟎) -----> R⟶ 𝟎

 Why ? Total Reflux : To increase the product quality, concentration of product.

 Explanation of case 1 : F = D + W
- If D = 0 then F = W which means whatever you feed all take-out from bottom without any separation, that's
why we must be close Feed (F=0) therefor the W is automatically 0.
- [F = 0, D = 0, W = 0] this condition is used during the start up of the column so that the maximum
enrichment condition(equilibrium) can be achieved by the column in less time.

 Case : As reflux ratio is increases

- Slope of the operating line of rectifying section increases. Graphically, the line moves away from the
equilibrium curve, towards the diagonal line.
- Reflux rate(L) is increases.
- Liquid collected at the bottom(𝐿) is also increased means feed to reboiler increases.
- Duty of the reboiler also increases.
- Required Size of the reboiler also increases.
- Boil up rate (𝑉 ) also increases means boil up ration increases.
- Slope of the operating line of stripping section decreases. Graphically stripping line moves away from the
equilibrium curve, towards the diagonal line.
- As vapour rate increases, load on the column also increases and to accommodate this increased load, we
need to increase the diameter of the column.
- As diameter of the try or column increases, area available for mass transfer also increases, rate of mass
transfer also increases, tray performance and tray efficiency also increases.
- Number of ideal stage required for desired separation also decreases.
- Feed(V) to condenser also increases.
- Duty of condenser also increases.
- Size of condenser also increases.
 NOTE : Reflux rate(L) is always saturated liquid & Boil up rate(𝑉 ) is always saturated vapour.
If we get extra cooling to the reflux and convert in to cold liquid then it is same condition as we increases
the reflux rate, in both cases we do not get any benefit in both cases load is increases in column. These
conditions are not used in industries.
Increases in reflux ratio over cold liquid reflux as it involves the calculations based on amount of
reflux(mass) while in making reflux cold, we need to make change in the energy(thermal potential).

 Total reflux : ---------

- Slope of the operating line of rectifying section and stripping section is unity. Hence both lines are merge
with the diagonal line.
- Reflux rate(L) is maximum.
- Liquid collected at the bottom(𝐿) is also increased means feed to reboiler maximum.
- Duty of the reboiler also maximum.
- Required Size of the reboiler also maximum.
- Boil up rate (𝑉 ) also maximum means boil up ration maximum.
- As vapour rate maximum, load on the column also maximum and to accommodate this maximum load, we
need to maximise the diameter of the column.
- As diameter of the try or column maximum, area available for mass transfer also maximum, rate of mass
transfer also maximum, tray performance and tray efficiency also maximum.
- Number of ideal stage required for desired separation also minimum.
- Feed(V) to condenser also maximum.
- Duty of condenser also maximum.
- Size of condenser also maximum.

 Operating line equation of enriching section in tearm of Reflux ratio :

L D
- operating line equation : yn+1 = . xn + . xD
V V

- Overall balance : V = L + D put in to operating line equation

L D
∴ yn+1 = . xn + . xD
L+D L+D

L
1
∴ yn+1 = L D . xn + L . xD
+1 +1
D D

𝐲𝐧+𝟏 = 𝐑+𝟏
𝐑
. 𝐱𝐧 + 𝐑+𝟏
𝟏
. 𝐱𝐃 Operating line equation in tearm of Reflux ration.
 - Compere with Y = MX + C

𝐑 𝟏
Slope : | intercepts : . 𝐱𝐃
𝐑 𝟏 𝐑 𝟏

 NOTE :
𝐋 𝐑
- Slope : or < 1
𝐕 𝐑 𝟏

- If R = 0 ; slope of operating line in enriching section = 0.

- Intercept on y-axis is ZERO means operating line lays on diagonal line(y=x) and there is no separation
occurs.

 Graphical Approach : ---------

- Form assumption : yn+1 = y & xn = x | y=x from graph

R 1
- yn+1 = .x + .x
R+1 n R+1 D

R 1
∴y= .x + . xD
R+1 R+1

R 1
∴y= .y + . xD [y=x]
R+1 R+1

R+1−R 1
∴y = .x
R+1 R+1 D
 ∴y = xD & From y=x -----> x = xD

- Point (𝐱 𝐃 , 𝐱 𝐃 )

○ If we increases the value of R then the operating line will be towards the equilibrium curve or away from the
equilibrium curve?
 Ans : Away from the equilibrium curve.

 Quiz : what is the order of R?

 ANS : R1 < R2 < R3 < R4

 Striping Section : ---------

 Operating line equation for Striping Section :

th
 Calculation for mth & (m + 1) plate :
 Overall Balance : Lm (Liquid coming from bottom) = V(vapour generate by reboiler) + W (bottom product)
 Component Balance : Vm+1 . ym+1 = Lm . xm − W. xW
 - Apply assumption : L1 = L2 = Ln = L | V1 = V2 = Vn+1 = V
∴ V. ym+1 = L. xm − W. xW

̅
𝐲𝐦+𝟏 = 𝐋 . 𝐱𝐦 − 𝐖 . 𝐱𝐖 it is operating line equation of Striping section.
𝐕 𝐕

- Compare with Y = MX + C

𝐖 𝐋̅
C (intercept) = − . 𝐱 𝐖 | Slope :
𝐕 𝐕
- Where :
V = Vapour flowrate in striping section
L = liquid flowrate in striping section
W = Bottom flowrate
xW = Mole fraction of MVC in bottom

 NOTE :
𝐋̅ 𝐋̅
- Slope : or > 1 ; here W is never grater than L.
𝐕 𝐋̅ −𝐖

 Graphical Approach : ---------

- Form assumption : ym+1 = y & xm = x | y=x from graph

L W
- ym+1 = . xm − . xW
V V

L W
∴ y = .y − . xW [y=x]
V V
 L W
∴y 1 − = − . xW
V V

V−L W
∴y V
= − V . xW

∴y( L − V) = W. xW

- Overall Balance : L = V + W ---------> W = L - V

∴y = xW & From y=x -----> x = xW

- Point (𝐱 𝐖 , 𝐱 𝐖 )
----------------------------------------------------------------------------------------------------------------
QUE : Find out the operating line equation of stripping section. Given data : (i) The intercept of the
operating line = -0.15, (ii) The mole fraction of LVC in bottom is 0.85.
 Solution :
W
- Given : .x = - 0.15 & (1 - xw ) = 0.85 --------> xw = 0.15
V W

L W L
- V = L - W ------> 1 = - -------> = 1+1 = 2
V V V

L W
- ym+1 = . xm − . xW
V V

∴ 𝐲𝐦+𝟏 = 𝟐. 𝐱 𝐦 − 𝟎. 𝟏𝟓

QUE : from above question find vapour composition of MVC at plate 6. Given : x6 = 0.4 & x6 = 0.3
 Solution :
- ym+1 = 2. xm − 0.15

∴ y5+1 = 2 × 0.3 − 0.15

∴ 𝐲𝟔 = 0.45
-----------------------------------------------------------------------------------------------------------------
▪ Boiling up Ratio (𝐑 𝛎 ): ---------
𝐑𝐞𝐭𝐮𝐫𝐧 𝐕
𝐑𝛎 = =
𝐰𝐢𝐭𝐡𝐝𝐫𝐚𝐰 𝐖

 Operating line equation of stripping section in tearm of Boiling up ratio :

 - operating line equation : y = .x − .x

- Overall balance : Lm = V + W put in to operating line equation

V+W
∴ ym+1 = . xm + . xW

W W
+
∴ ym+1 = W W
. xm + W
. xW
W W

𝐑𝛎 𝟏 𝟏
𝐲𝐦 𝟏 = . 𝐱𝐦 + . 𝐱𝐖 Operating line equation in tearm of Boiling up ratio.
𝐑𝛎 𝐑𝛎

- Compere with Y = MX + C

𝐑𝛎 𝟏 𝟏
Slope : | intercepts : . 𝐱𝐖
𝐑𝛎 𝐑𝛎

 Concept of the Minimum Reflux Ratio(𝐑 𝐦 ) :

"Both lines (operating line of stripping section & operating line of the enriching section) intersect at a
point on equilibrium curve at that point the reflux ratio is called minimum reflux ratio."

Rm
 Slope =
Rm +1

xD −y′ Rm
∴ =
xD −x′ Rm +1
 xD −y′
- Assume that =x
xD −x′

∴xRm + x = Rm

x
∴ Rm =
1−x

- Now put the value of x;

xD −y′
xD −x′
∴ Rm =
x −y′
1− D ′
xD −x

𝐱 𝐃 −𝐲 ′
∴ 𝐑𝐦 =
𝐲 ′ −𝐱 ′

○ About plates/trays in unit or column : ---------

- In general standerd book Ropt = 1.2 to 1.4 Rmin

- Minimum Reflux ratio is the minimum reflux ration at which required number of plates or trays are infinite.

𝐑 𝐦𝐢𝐧 ys.
𝐑 𝐦𝐚𝐱 ys.

- As we increases reflux ratio from minimum to maximum, number of stages decreases abruptly in the
beginning and then slowly. Such that at total reflux ratio, number of stages become minimum.
- As we increases reflux ratio from minimum, diameter of column increases slowly in the beginning and then
rapidly till at total reflux, it become maximum.

- Optimum reflux ratio is the point at which total cost is minimum. This point is reached near the minimum
reflux ratio as decrease in number of stages is significant and increase in diameter of column is negligible.
----------------------------------------------------------------------------------------------------------------
QUE : A binary distillation column is to be designed using McCabe Thiele method. The distillation contains
90 mole% of the more volatile component. The point of intersection of the q-line with the equilibrium curve
is (0.5, 0.7). The minimum reflux ratio (rounded off to the first decimal place) for this operation is ______
[GATE : 2016 IISc Bangalore]
Solution :

xD −y′ Rm 0.9−0.7
- = = = 0.5
xD −x′ Rm +1 0.9−0.5

∴ Rm = 0.5 Rm + 0.5

∴ 𝐑𝐦 = 1
----------------------------------------------------------------------------------------------------------------

 Feed Line Equation : ---------

 - Pinch point at where driving force will be ZERO.
- Reflux ration along with pinch point is Minimum Reflux Ratio.
- Feed line always passes through intersection point of both operating lines(operating line of stripping section
& operating line of the enriching section).
- This intersection point will be sift any where between diagonal line and equilibrium curve but maximum at
equilibrium curve not beyond that.
----------------------------------------------------------------------------------------------------------------
QUE : Find out the reflux ratio if More volatile component is 0.95.

 Solution : here the section is rectifying section and in this section value of xn never larger than the yn+1 .

QUE : Find out the reflux ratio if More volatile component is 0.95.

 Solution :
R 1
yn+1 = . xn + . xD
R+1 R+1

R 1
∴0.70 = × 0.56 + × 0.95
R+1 R+1
 ∴0.70 R + 0.70 = 0.56 R + 0.95

∴R = 1.7857

Graphical Approach :

----------------------------------------------------------------------------------------------------------------

 Equation of Feed line : ---------

 Method 1 :
 Operating line of rectifying section :
Vyn+1 = L.xn + D.xD

∴V.y = L.x + D.xD ------------(1) [where yn+1 = y & xn = x]

 Operating line of striping section :

Vym+1 = L.xm - W.xW

∴ V.y = L.x + W.xW ------------(2) [where ym+1 = y & xm = x]

- Equation (2) - (1);

y(V - V) = x(L - L) - [W. xW + D. xD ]

(F = D + W and xf . f = xD . D + xW . W)

∴y(V - V) = x(L - L) - xf . f

 NOTE : ---------
- For liquid :
 q.f -------> amount if liquid
∴ q.f = L - L
𝐋̅ 𝐋
∴𝐪
𝐟

- For vapour :
(1 - q).f -------> amount if vapour
∴ (1 - q).f = V - V
𝐕 𝐕 𝐕 𝐕
∴
𝐟 𝐟

- Now ;
∴y(V - V) = x(L - L) - xf . f

∴y(1 - q).f = q.f - xf . f

𝐪 𝐱𝐟
𝐪 𝟏 𝐪 𝟏

- Compare with Y = MX + C

𝐪 𝐱𝐟
𝐪 𝟏 𝐪 𝟏

 Method 2 :
- If two lines intersects at a point with coordinates (xq ,xq ).

 Operating line of rectifying section :

Vn yq = Ln .xq + D.xD

 Operating line of striping section :

Vm yq = Lm .xq − W.xW
 Subtract the Equations;
yq (Vm - Vn ) = xq (Lm - Ln ) - [W. xW + D. xD ]

(F = D + W and xf . f = xD . D + xW . W)

∴ yq (Vm - Vn ) = xq (Lm - Ln ) - xf . f --------------------------- (P)

- Feed is liquid at a temperature Tf which is less than the boling point.

- Hf = Enthalpy per mole of feed
- HL = Enthalpy of one mole of feed at its boiling point temperature (Tb ) = F(HL − Hf )
F(HL Hf )
- Number of moles of vapour to be condensed to provide this heat to feed liquid =
λV
- λV = molar latent heat of vapour = HV − HL

 Material balance of feed plate(rectifying and stripping sections are merge at feed plate);
F + Ln +Vm = Lm + Vn

- Where ;
F = feed,
L = liquid flowrate in rectifying section
L = liquid flowrate in stripping section
V = vapour flowrate in rectifying section
V = vapour flowrate in stripping section

∴ Vm − Vn = Lm − Ln − F ------------(1)

 Lm = Ln + F + (Vm − Vn )

F(HL − Hf )
∴ Lm = Ln + F +
λV

λV + (HL − Hf )
∴ Lm = Ln + F --------------- (2)
λV

HV − HL + (HL − Hf )
∴ Lm = Ln + F
HV − HL

HV − Hf
∴ Lm = Ln + F
HV − HL

∴ Lm = Ln + F.q ---------------------(A)
 𝐇𝐕 − 𝐇𝐟
- Where; q =
𝐇𝐕 − 𝐇𝐋

 From equation (1);

∴ Vm − Vn = Lm − Ln − F
∴ Vm − Vn = Ln + F.q − Ln − F
∴ Vm − Vn = F.q − F
∴ Vm − Vn = F(q − 1) ---------------------- (B)

 Put results (A) & (B) in equation (P);

∴ yq (Vm - Vn ) = xq (Lm - Ln ) - xf . f

∴ yq × F(q − 1) = xq (Ln + F.q - Ln ) - xf . f

∴ yq × F(q − 1) = xq (F.q) - xf . f

𝐪 𝐱𝐟
∴ 𝐲𝐪 = 𝐱𝐪 − -------> q-line equation
𝐪 𝟏 𝐪 𝟏

 This equation is commonly known as the equation of the q-line. If xq = xf , then yq = xf .

𝐪
- Thus, the point of intersection of the two operating lines lies on the straight line of slope passing
𝐪 𝟏
through the point (xf , xf ).

 Now from equation (2);

λV + (HL − Hf )
Lm = Ln + F
λV

λV + (HL − Hf )
∴q =
λV

- HL = nCp (Tb − To ) | Hf = nCp (Tf − To ) | (HL − Hf ) = Cp (Tb − Tf ) -----> n = 1mole

- Where; To = reference temperature | Tb = boiling point temperature | Tf = feed temperature

λV + Cp (Tb − Tf )
∴q =
λV

𝐂𝐩 (𝐓𝐛 𝐓𝐟 ) + 𝛌𝐕
Q=
𝛌𝐕
 Feed Quality (q) : ---------
- It is the % of liquid present in the feed when feed is mixture of liquid and vapor.

"Amount of the heat required to vaporized 1 mole of the feed (at feed condition) to saturated vapor
with respect to latent heat of vaporization."

𝐇𝐕 − 𝐇𝐟 𝐂𝐩 (𝐓𝐛 −𝐓𝐟 )+ 𝛌𝐕
q= =
𝐇𝐕 − 𝐇𝐋 𝛌𝐕

- λV = Latent heat of vaporization

- Tb = Boiling point temperature
- Tf = Feed temperature
- Cp = average heat capacity which is constant.
- HV = Enthalpy of saturated vapor
- Hf = Enthalpy of feed
- HL = Enthalpy of saturated liquid

○ Case 1 : feed is Subcooled liquid (q > 1 with positive)

- In this condition Subcooled liquid temperature (Tf ) < boiling temperature (Tb ) means Cp (Tb − Tf ) tearm is
positive and λV is always positive.

Cp (Tb −Tf )+ λV Cp (Tb −Tf ) positive

- So that; q = = + 1 ---------> q = +1
λV λV positive
- Therefore the value of q is always grater than 1.

○ Case 2 : feed is saturated liquid (q = 1)

- Meaning of saturated liquid : Liquid that at its bubble/ boiling point temperature.
- In this condition Saturated liquid temperature (Tf ) = boiling temperature (Tb )

Cp (Tb −Tf )+ λV 0+ λV
- q= = -------------> q = 1
λV λV

 NOTE : 1000 is the bubble point of H2 O at 1 atm.

○ Case 3 : feed is liquid + vapour mixture (0 < q < 1)

HV − Hf
- q= [HV < Hf < HL ]
HV − HL
 NOTE : most widely feed used in distillation column.

○ Case 4 : feed is Saturated vapor (q = 0)

- In this case we do not provide any type of sensible heat and latent heat because our feed is already in
saturated vapor.

- Feed enthalpy (Hf ) = vapor enthalpy (HV )

HV − Hf HV − HV
- q= = = 0
HV − HL HV − HL

○ Case 5 : feed is Saturated Vapor (q < 0)

- In this case enthalpy of feed (Hf ) > enthalpy of Vapor (HV )

HV − Hf
- q= = negative
HV − HL

 Graphical representation of equation of feed : ---------

(i) Subcooled liquid (q > 1 with positive)
(ii) Saturated liquid (q = 1)
(iii) (liquid + vapour) mixture (0 < q < 1)
(iv) Saturated vapor (q = 0)
(v) Superheated Vapor (q < 0)
 - x′ & y′ is point on equilibrium curve where rectifying, stripping and feed line intersects.
- If feed is saturated -----> xf = x′ | If feed is sapurheated -----> xf = y′ .
- (Liquid + vapour) mixture : 0 < slope < ∞ | Superheated vapour : 0 < slope < 1

○ Variation in reflux ratio with the type of feed : ---------

𝐑 𝐂𝐨𝐥𝐝 𝐥𝐢𝐪𝐮𝐢𝐝 < 𝐑 𝐒𝐚𝐭𝐮𝐫𝐚𝐭𝐞𝐝 𝐥𝐢𝐪𝐮𝐢𝐝 < 𝐑 𝐂𝐨𝐥𝐝 𝐥𝐢𝐪𝐮𝐢𝐝 < 𝐑 𝐩𝐚𝐫𝐭𝐢𝐚𝐥 𝐯𝐚𝐩𝐨𝐮𝐫 < 𝐑 𝐒𝐚𝐭𝐮𝐫𝐚𝐭𝐞𝐝 𝐯𝐚𝐩𝐨𝐮𝐫 < 𝐑 𝐒𝐮𝐩𝐞𝐫𝐡𝐞𝐚𝐭𝐞𝐝 𝐯𝐚𝐩𝐨𝐮𝐫

- If our feed is cold liquid then to reach saturated liquid(to decrease the cold liquid potential) we need to
decreases the reflux rate or increase the vapour potential, therefore here the reflux ratio is minimum than
others.
- In saturated liquid case we decrease the liquid potential therefore we need to increase the reflux rate than
cold liquid to maintain balance. Because here liquid is easily get vaporized then cold liquid.
- Similarly for other.
- In case of superheated vapour feed the vapour potential is increases(increases because feed and stripping
section both contain vapour) then the reflux rate(L) is maximum than others but not total reflux.
-----------------------------------------------------------------------------------------------------------------
QUE : In the Mc-Cabe-Thiele diagram, if the X-coordinate of the point of intersection of the q-line and the
vapour-liquid equilibrium curve is grater than the X-coordinate of the feed point, then the quality of the
feed is _________ [GATE : 2012 IIT Delhi]
(A) Superheated vapour
(B) Liquid below bubble point
(C) Saturated vapour
(D) Saturated liquid
 Solution :

QUE : If we change q1 = 0.25 to q2 = 0.75 then how slope of the feed line changes = ?
 Solution :
q2 q1 0.75 0.25
- Final slope − initial slope = − = − = −𝟐. 𝟔𝟕
q2 − 1 q1 − 1 0.75 − 1 0.25 − 1
 - If in question they ask change then write answer with minus sign.
- If in question they ask %increment or % decrement then do not write with sign.

QUE : Consider the equilibrium data for methanol-water system at 1 bar given in the figure below.

A distillation column operating at 1.0 bar is required to produce 92mol% methanol. The
. It is an equimolar mixture of methanol and water. The minimum reflux ratio is
(A) 0.33 (B) 0.50 (C) 0.54 (D) 1.17 [GATE : 2020 IIT Delhi]
 Solution :

Rm 0.92 −0.78
- Slope of enriching line in term of minimum reflux ratio : = --------> 𝐑 𝐦 = 0.5
Rm +1 0.92 −0.5

Rm 0.92 −0.75
- If they asking for feed is saturated vapour then : = --------> 𝐑 𝐦 = 0.5385
Rm +1 0.92 −0.14

QUE : A binary feed consisting of 25 mol% liquid and 75 mol% vapour is separated in a staged distillation
 column. The mole fraction of the more volatile component in the distillate product is 0.95. The molar flow
rate of distillate is 50% of the feed flow rate and the McCabe-Thiele method can be used to analyse the
column. The q-line intersects the operating line of the enriching section at (0.35, 0.5) on the x-y diagram.
The slope of the stripping section operating line (up to one decimal place) is___________.
[GATE : 2015 IIT Roorkee]
 Solution :
L
- Given : D = 0.5 f & q = 0.2 then = ?
V

- Take a basis : f = 100 mol/hr then D = 0.5 × 100 = 50 mol/hr

Rm 0.95 −0.5
- = = 3
Rm +1 0.95 − 0.35

Rm L L
- As we know = = = 3 ----------> L = 150 mol/hr
Rm +1 D 50

- We know; q . f = L − L ------> 0.25 × 100 = L − 150 -------> L = 175 mol/hr

- Now material balance at top : V = L + D = 150 + 50 = 200 mol/hr

- We know ; f(q - 1) = V - V --------> 100(1 - 0.25) = 200 - V -------> V = 125 mol/hr

L 175
- Now slope = = 1.4
V 125
-----------------------------------------------------------------------------------------------------------------

 Batch distillation / Differential distillation / Rayleigh

distillation : ---------
 - If small difference in boiling point then we use fractional distillation.
- If large difference in boiling point then we use batch distillation.

 Mathematical interpretation :
- Assume that any time during the course of the distillation there are
- L mol of liquid in the still of composition x mole fraction A and that an
- Amount dD mol of distillate is vaporised of mole fraction y* in equilibrium with the liquid.

○ Material balance :
Total material Component A
Moles in 0 0
Moles out dD y*dD
Moles accumulated dL d(Lx) = Ldx + xdL
In - out = accumulation 0 - dD = dL 0 - y*dD = d(Lx)

- Moles in is ZERO because there is not continue entering feed, this is batch process.
- Moles out : y*dD because vapour and liquid composition of component A in equilibrium.
- dL for total material if we multiply that by mole fraction of component A which is x then we get d(Lx).

- Overall balance : (-dL) = dD

- Component balance : 0 - y*dD = d(Lx)
- y*dD = Ldx + xdL
 - Form overall balance : y*dL = Ldx + xdL
∴(y* - x)dL = L dx
w dL x dx
∴ ∫f = ∫x w
L f (y* - x)

𝐟 𝐱𝐟 𝐝𝐱
𝐥𝐧 𝐰
= ∫𝐱𝐰 (𝐲* - 𝐱)
Reyleigh Equation

- Where
f = mole of charge of composition xf
W = mole of residual liquid of composition xw .

- In GATE exam : they will give straight line equation for 𝐲* = MX + C.

𝛂.𝐱
- In college exam : they will give 𝐲* = .
𝟏+(𝛂−𝟏)𝐱

𝐟.𝐱 𝐟 𝐟(𝟏−𝐱 𝐟 )
- For college exam equation : 𝐥𝐧 = 𝛂 ln
𝐰.𝐱 𝐰 𝐰(𝟏−𝐱 𝐰 )

○ Differential condensation : ---------

𝐟 𝐲 𝐝𝐲
𝐥𝐧 = ∫𝐲 𝐃
𝐃 𝐟 (𝐲 - 𝐱*)

- Where
f = mole of feed vapour of composition yf
D = vaporous residue of composition yD .
----------------------------------------------------------------------------------------------------------------
QUE : Consider a batch distillation process for an equimolar mixture of benzene and toluene at atmospheric
pressure. The mole fraction of benzene in the distillate collected after 10 minutes is 0.6. the process in
further continued for additional 10 minutes. The mole fraction of benzene in the total distillate collected
after 20 minutes of operation is ________ [GATE : 2020 IIT Delhi]
(A) Less than 0.6
(B) Exactly equal to 0.7
(C) Grater than 0.7
(D) Exactly equal to 0.6
 Solution :
- As time increases -------> Low volatile component is started to vaporized -------> concentration of more
volatile component decreases in distillate. If at starting concentration of MVC is 0.6 then after 20 minute it
will be less than 0.6.
 QUE : The vapour-liquid equilibrium curve of a binary mixture A-B may be approximated by a linear equation
over a narrow range of liquid mole fraction (0.2 < xA < 0.3) as follows

yA = 1.325 xA + 0.121

Here is the mole fraction of A in the vapour. 100 moles of a feed (xAf = 0.28) is batch distillate to a final
residue (xAw = 0.2). Using the Rayleigh equation the number of moles of the residue left behind in the
distillation unit, up to 2 digits after the decimal point, is [GATE : 2013 IIT Bombay]
(A) 60.3 moles (B) 63.2 moles (C) 65.6 moles (D) 66.85 moles
 Solution :
f x dx
ln = ∫x f
w w (y* - x)

100 0.28 dxA

∴ ln = ∫0.2
w (1.325 xA + 0.121 - xA )

100 0.28 dxA

∴ ln = ∫0.2
w (0.325 xA + 0.121)

100 1
∴ ln = ln(0.325 xA + 0.121) from 0.2 to 0.28
w 0.325

100 1
∴ ln = [ln(0.325 × 0.2 + 0.121) − ln(0.325 × 0.28 + 0.121)]
w 0.325

100 1 (0.325 ×0.28 + 0.121)

∴ ln w
= 0.325 ln (0.325 ×0.2 + 0.121)

100 1 0.212
∴ ln = ln
w 0.325 0.186

100 1
∴ ln = [0.1308 ] = 0.40258
w 0.325

100
∴ = e0.40258
w

100
∴ = 1.4957
w

∴W = 66.858 moles
----------------------------------------------------------------------------------------------------------------

 Fenske's Equation : ---------

 - It is used to calculation of minimum number of plates.

 Conditions :
L
(1) Total reflux : R ⟶ ∞ when R = where D ⟶ 0
D
(2) F = 0, D = 0, W = 0
R R R
(3) R ⟶ ∞, slope of reflux / enreaching line : | limR ⟶ ∞ = limR ⟶ ∞ = 1
1
R+1 R+1 R 1+
R

L L
(4) R ⟶ ∞, slope of stripping line : = where W = 0 then slope = 1.
V L−W

○ Minimum number of trays from graphical method :

- Number of tie lines = number of plates/trays.

- This total reflux condition is done when column is in starting phase so that we get more enrichment in top
section.

○ Analytical method to find number of plates/trays : ---------

𝐱 (𝟏−𝐱 𝐰 )
𝐥𝐧 𝐃
𝐱 𝐰 (𝟏−𝐱 𝐃 )
𝐍𝐦 + 𝟏 =
𝐥𝐧 𝛂𝐚𝐯𝐠

- If you have α1 and α2 then 𝛂𝐚𝐯𝐠 = √𝛂𝟏 . 𝛂𝟐

 Nm = minimum number of plates/ trays in column with or without total reboiler / total condenser.
Nm = minimum number of plates/ trays in column excluding partial reboiler / partial condenser.
 Nm + 1 = minimum number of plates/ trays in column including(+) partial reboiler(1).
Nm + 1 = minimum number of plates/ trays in column including(+) partial condenser(1).

 NOTE : partial reboiler or partial condenser both are acts as stage / plate/ tray.

- Example : Nm + 1 = 4.6 Or Nm = 3.6 ; write answer : 5 or 4.

 Nm + 1 + 1 = Nm + 2 = minimum number of plates/ trays in column including(+) partial condenser(1)

including(+) partial reboiler(1).

 Example :
- Minimum number of plates/ trays in column including partial condenser including total reboiler.
Nm + 1 = 5

- Minimum number of plates/ trays in column including partial condenser including partial reboiler.
Nm + 2 = 5

- Conclusion from this example is that the left side changes but right side of the formula remain same.

𝐱 (𝟏−𝐱 𝐰 ) 𝐱 (𝟏−𝐱 𝐰 ) 𝐱 (𝟏−𝐱 𝐰 )

𝐥𝐧 𝐃 𝐥𝐧 𝐃 𝐥𝐧 𝐃
𝐱 𝐰 (𝟏−𝐱 𝐃 ) 𝐱 𝐰 (𝟏−𝐱 𝐃 ) 𝐱 𝐰 (𝟏−𝐱 𝐃 )
𝐍𝐦 = | Nm + 1 = | Nm + 2 =
𝐥𝐧 𝛂𝐚𝐯𝐠 𝐥𝐧 𝛂𝐚𝐯𝐠 𝐥𝐧 𝛂𝐚𝐯𝐠

----------------------------------------------------------------------------------------------------------------
QUE : A distillation column handling a binary mixture of A and B is operating at total reflux. It has two ideal
stages including the reboiler. The mole fraction of the more volatile components in the residue is 0.1. the
average relative volatility αavg is 4. the mole fraction of A in the distillate (xD ) is _______ [GATE : 2021
IIT Bombay]
 Solution :

- Nm + 1 = 2, xw = 0.1, xD = ? , αavg = 4

x (1−xw )
ln D
xw (1−xD )
- Nm + 1 =
ln αavg

x (1−0.1)
ln D
0.1(1−xD )
∴2=
ln 4
 xD (1−0.1)
∴ ln = 2.7726
0.1(1−xD )

xD (0.9)
∴ = e2.7726
0.1 − 0.1xD

∴ xD (0.9) = 16 (0.1 − 0.1xD )

∴ 𝐱 𝐃 = 0.64
---------------------------------------------------------------------------------------------------------------

 Efficiency of the column : ---------

- There are three type of efficiency we have seem in the column :
(i) Overall efficiency
(ii) Murphree efficiency
(iii) Point efficiency

(i) Overall efficiency (𝛈𝐨 ):

𝐭𝐡𝐞𝐨𝐫𝐢𝐭𝐢𝐜𝐚𝐥 𝐨𝐫 𝐢𝐝𝐞𝐚𝐥 𝐧𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐩𝐥𝐚𝐭𝐞𝐬 𝐨𝐫 𝐭𝐫𝐚𝐲𝐬 (𝐍𝐭𝐡 )

𝛈𝐨 =
𝐀𝐜𝐭𝐮𝐚𝐥 𝐧𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐩𝐥𝐚𝐭𝐞𝐬 𝐨𝐫 𝐭𝐫𝐚𝐲𝐬 (𝐍𝐚𝐜𝐭 )

- This is less efficient method.

(ii) Murphree efficiency (𝐄𝐦 ) :

𝐀𝐜𝐭𝐮𝐚𝐥 𝐬𝐞𝐩𝐚𝐫𝐚𝐭𝐢𝐨𝐧 𝐲𝐧 − 𝐲𝐧+𝟏

𝐄𝐦 = =
𝐦𝐚𝐱𝐢𝐦𝐮𝐦 𝐬𝐞𝐩𝐚𝐫𝐚𝐭𝐢𝐨𝐧 𝐲𝐧 ∗ − 𝐲𝐧+𝟏

αxn
- yn ∗ =
1+(α−1)xn
 - This efficiency is associated with whole plate not column.
- When yn is equilibrium with xn there we get yn ∗ .
- Here all composition are average because we are consider whole plate not a particular point.
- This efficiency (Em ) can be grater than 1 or grater than 100%.
- Murphree efficiency can be equal to the point efficiency in that condition when column diameter is very
small.

(iii) Point efficiency (𝛈𝐩 ): ---------

𝐲𝐧 𝐩 − 𝐲𝐧+𝟏 𝐩
𝛈𝐩 =
𝐲𝐧 𝐩 ∗ − 𝐲𝐧+𝟏 𝐩

- This efficiency is associated with particular point on plate or tray not for whole plate.
- Point efficiency can not be grate than 1.
---------------------------------------------------------------------------------------------------------------
QUE : The composition of vapour entering a tray in a distillation column is 0.47. the average composition of
the vapour leaving the tray is 0.53. the equilibrium composition of the vapour corresponding to the liquid
leaving this tray is 0.52. all the compositions are expressed in mole fraction of the more volatile component.
The Murphree efficiency based on the vapour phase, rounded to the nearest integer, is ____________
(in%). [GATE : 2017 IIT Roorkee]
 Solution :

yn − yn+1 0.53 − 0.47

- Em = = = 1.2 × 100 = 120 %
yn ∗ − yn+1 0.52 − 0.47

kmol
QUE : A binary saturated liquid with 50% A and 50% B enters the fractionating column at a rate of 50 .
min
 The composition of volatile component A in distillate and bottom are 90% and 1% respectively. Calculate
the reflux ratio, if operating line for stripping section is y = 1.5x − 0.005. [GATE : 2022 IIT Kharagpur]
Solution :
kmol
- Given : F = 50 , xf = 0.5, xD = 0.90, xw = 0.01
min

- From matrial balance;

F = D + W ------> 50 = D + W ----> W = 50 - D

- Component balance ;
F.xf = D.xD + W.xw
∴50 × 0.5 = D × 0.90 + W × 0.01
∴25 = D × 0.90 + (50 - D) × 0.01
D = 27.5 kmol/min
W = 50 - D ----------> W = 22.47 kmol/min

- From standard equation,

Rν +1 1
ym+1 = . xm + .x compare with from queation : y = 1.5x − 0.005
Rν Rν W

Rν +1
= 1.5 -------------> Rν =2
Rν

V
- From defination of Rν (boiling up ratio) =
W

V = Rν .W = 2 × 22.47 = 44.94 kmol/min

- From question : binary saturated liquid means the value of q = 1.

V-V V −V
(1 - q) = OR (q - 1) =
f f

44.94 −V
∴(1 - 1) = 50
------> V = 44.94 kmol/min

- Material balance around condenser ;

V=L+D
∴L = 44.94 - 27.53
∴L = 17.416 kmol/min

L 17.416
- Reflux ratio = = = 0.63
D 27.53
 --------------------------------------------------------------------------------------------------------------

Designing Of Distillation Column

---------

 Calculation of diameter of column :

𝛑
- 𝐀𝐓 = 𝐀𝐍 + 𝐀𝐝 & 𝐀𝐓 = 𝐃𝐜 𝟐 [in question you nedd to find 𝐃𝐜 ]
𝟒

 NOTE : column diameter decided by the vapour flowrate because [𝐀 𝐍 >> 𝐀 𝐝 ].

○ Concept of the calculation of Net area (𝐀𝐍 ) :

kg m
- Mass flowrate (Ṁ ) = ρ × A × v = 3 × m2 ×
m s

𝐌̇𝐯 = 𝛒𝐯 × 𝐀 𝐍 × 𝐯𝐨𝐩

- ρv = density of vapour
- AN = Net area which is associated with vapour
- vop = Operational velocity

 vop is already given in to question as; vop = 30-50% vf

- vf = flooding velocity(it is high vapour flowrate) (given)

○ Concept of calculation of downcomer area(𝐀𝐝 ):

 - Ad is given in the quastion as; Ad = 10-20% AT
----------------------------------------------------------------------------------------------------------------
QUE : Two packed towers are designed for the same mass velocity of the gas. The first has liquid and gas
flow rates of 30 kg/s and 1.2 kg/s, respectively, while the corresponding flow rates in the second tower are
67.5 kg/s and 1.8 kg/s. The ratio of the diameter of the wider tower to that of the narrower tower is
___________. [GATE : 2018 IIT Guwahati]
(A) 2 (B) 1.8 (C) 1.5 (D) 1.225
 Solution :
- Given :
For wider column : Ṁ v = 1.8 kg/sec | Ṁ L = 67.5 kg/sec
For narrower column : Ṁ v = 1.2 kg/sec | Ṁ L = 30 kg/sec
Dw
DN
=? & Same mass velocity of the gas.

Ṁ
- Mass velocity =ρ×v
A

Ṁ w Ṁ N
- =
Aw AN

Ṁ w Ṁ N Dw Ṁ w 1.8
∴π 2 =π 2 ------------> = =
D D DN Ṁ N 1.2
4 w 4 w

𝐃𝐰
∴ = 1.225 m
𝐃𝐍

QUE : A separation column for vapour-liquid contact process 200 kmol/h of vapour. The flooding velocity is
3 m/s. If the column operates at 85% of flooding velocity and the down comer area is 10% of the total
cross-sectional area, what is the diameter of the column? Average density of vapour = 2 kg/m3 and its
molecular weight = 44. [GATE : 2005 IIT Bombay]
(A) 0.82 m (B) 0.72 m (C) 0.78 m (D) 1 m
 Solution :
200 ×44
Ṁ v = 200 kmol/h = kg/s , vf = 3 m/s, ρv = 2 kg/m3 , AD = 0.10 AT ,
3600
vop = 0.85 vf = 0.85 × 3 = 2.55 m/s

- Ṁ v = ρv × AN × vop

200 ×44
∴ = 2 × AN × 2.55
3600

∴ AN = 0.479 m2
 - AT = AN + Ad

∴ AT = 0.479 + 0.10 AT

∴ AT = 0.532 m2

π
∴ 4 Dc 2 = 0.532

∴ 𝐃𝐜 = 0.823 m
----------------------------------------------------------------------------------------------------------------

 Section 1 : Graphical Determination of Distillation column designing ---------

(Step : 1) Determine process operation variable.
(Step : 2) Determine the minimum reflux ratio
(Step : 3) Choose actual reflux ratio
(Step : 4) Determine the minimum number of trays
(Step : 5) Principle dimension of the column (diameter/height)

 Step 1 : Determine process operation variable.

- Assume feed rate, composition, purity of distillate and bottom and the quality of the feed are known.
- Perform overall material and component balance to determine the compositions of the distillate and
bottoms.
- Overall balance : F = D + W
- Component balance : F.𝑧 = D.𝑥 . W.𝑥
- This material balance is for More Volatile Component(MVC).

- If you define flowrates first then you can find compositions or vice-versa.

 Step : 2 Determine the Minimum Reflux Ratio

- This graphical approach is determined using the Mc-Cabe Thiele Method for binary mixtures. The ratio of
reflux flow to distillate flow is called the reflux ratio.

(A) Assumptions : Mc-Cabe Thiele Method

(i) Constant Molal or Molar Overflow : The molar flowrates of the vapour and liquid are nearly constant in
each section of the column. This also measures the operating lines are straight lines.
 (ii) Heat Effects are negligible : For example, heat losses to and from the column are small and neglected.

(iii) For every mole of vapour condensed, another mole of liquid is vaporised.

(iv) The liquid and vapour leaving the tray is in equilibrium with the vapour and liquid entering the tray.

○ Draw the equilibrium curve : ---------

 (Method 1 & 2) Form this topic : T - x - y Diagram
α.x
 Method 3 : by using formula : y =
1+(α−1)x
- Put he value of x and get the value of y and construct the x-y diagram.

(B) Draw the feed line (q - line) :

- The feed line can be constructed by locating the point on the 450 line that corresponds to the feed
composition.
- This point can be extended with a slope of where q is the feed quality.
- The feed line can be directly plotted through the following equation : y = x− which is in the form
of Y = MX + C.

(C) Upper Operating Line (Rectifying line/ Enriching line) :

- Draw the operating line for the enriching section.
- First find the desired top product composition (on the x-axis) and locate the corresponding point on the 450
line.
- Connect this point to the point where the equilibrium curve and the feed line intersect.
- This is the upper operating line.
 x
- The y intercept of this line is equal to D .
(R+1)
xD
- The following equation can be used to determine the minimum reflux : Rmin = - 1.
yintercept

 Graphical representation : ---------

 Step 3 : Choose Actual Reflux Ratio

- As the reflux ration increases, the number of trays and thus the capital cost of the column decreases.
- However, as a trade-off, on increasing in reflux ratio will also increase the vapour rate within the tower, thus
increases expenses such as condenser and reboilers.
- Most columns are designed to operate between 1.3 and 1.5 times the minimum reflux ratio because this is
approximately the region of minimum operating cost.
- Therefore, based on first estimates, the operating reflux ration is equated so that Ractual = 1.2 × Rmin
 Step 4 : Determine the Theoritical Numbers of Trays
(1) Upper/ lower operating line using the actual reflux ratio.
xD
- Plot the point and draw the line to the xD .
(R+1)

R 1 L D
- The equation of the upper operating line is : yn+1 = . xn + . xD OR yn+1 = . xn + . xD
R+1 R+1 V V

(2) Starting from composition of the distillate, a horizontal line is drawn to the equilibrium curve. This line
demonstrate the first tray.

(3) From the privious intersection, drop vertically until the upper operating line is obtained. Follow step two
to determine next tray.

 Step 5 : Determine Actual Number of Trays ---------

- This is determine by taking the quotient of the number of theoritical trays to the tray efficiency.
- Typical values for tray efficiency range from 0.5 to 0.7.
- These values depend on the type of trays being used, as well as the internal liquid and vapour flow rates.

𝐍𝐭𝐡𝐞𝐨𝐫𝐢𝐭𝐢𝐜𝐚𝐥
𝐍𝐚𝐜𝐭𝐮𝐚𝐥 = 𝐄𝐟𝐟𝐢𝐜𝐢𝐞𝐧𝐜𝐲

Case Study
 (1) Determine process operation variable :
- Feed stream, Acetone / Acetic Acid; F = 100 mole/hr
- Light - Key mole fraction; Zf or xf = 0.30
- Percentage of light in Distillate; xD =0.90
- Percentage of light in bottoms; xW = 0.10
- Quality of Feed; Q = 1

 Material balance :
- Overall material balance : F = D + W -----> 100 = D + W ------> D = 100 - W

- Component balance : F.Zf = D.xD + B.xw ------> 100 × 0.3 = 30.0 (100 − W) × 0.9 + W × (0.1)
∴ W = 75 mole/hr
- D = 25 mole/hr

 Graphical Method :
(2) Determine the minimum reflux ratio 𝐑 𝐦𝐢𝐧 :
- First draw the equilibrium curve.
- Second feed line draw. (for that q value is given in que)
- Here in our case saturated liquid means q = 1.
q 1
- Slope of feed line = =∞
q−1 1−1
- Third draw enriching line which is passes through a point (x′ , y′ ).
 xD
- Form graph we get intercept yintercept = of enriching line.
Rmin +1
- Form graph yintercept = 0.605
- From intercept we can find Rmin .
yintercept 0.9
- Rmin = −1= − 1 = 0.5
xD 0.605

○ There is second method to find Rmin :

- From graph we can find slope(θ) of enriching line by the help of protector.
xD −y′ Rm xD −y′
- Slope(θ) = = ------> Rm =
xD −x′ Rm +1 y′ −x′

(3) To calculate actual reflux ratio 𝐑 𝐀𝐜𝐭𝐮𝐚𝐥 : ---------

- In question the relationship between RActual & Rmin is given.

- Here we take RActual = 1.2 × Rmin = 1.2 × 0.5 = 0.6

(3) To calculate Actual/minimum number of trays 𝐍𝐀𝐜𝐭𝐮𝐚𝐥 :

RActual
- For actual condition the slope of enriching line is =
RActual + 1

RActual 0.6
- Slope = = = 0.375
RActual + 1 0.6 + 1

xD 0.9
- And intercept on graph for RActual : yintercept = = = 0.5625
RActual +1 0.6+1

- Now draw the graph again;

 - From graph we can note that the actual trays required is 5.

(4) Principle dimension of the column (diameter/height) : ---------

 Height of column :
- The tower height can be related to the number of trays in the column. The following formula assume that a
spacing of two feet between trays will be sufficient including additional five to ten feet at both ends of the
tower.

𝐇𝐭𝐨𝐰𝐞𝐫 = 2.3 𝐍𝐚𝐜𝐭𝐮𝐚𝐥

○ Design Guideline :
- Height of the column should not be higher than 175 feet.
- Height to diameter ratio should be less than 20 to 30.
- If the tower is higher than 190 feet, then a design with smaller tray spacing should be considered.

○ Vapour Velocity :
 - Before we can determine the tower diameter, we need to determine the vapour velocity. The vapour velocity
can be derived from the flooding velocity. To limit our column from flooding, we chose a velocity 60 to 85
percent of flooding.

 Calculation of diameter of column : (IIT Kanpur 2023 : 2M) ---------

𝛑
- 𝐀𝐓 = 𝐀𝐍 + 𝐀𝐝 & 𝐀𝐓 = 𝐃𝐜 𝟐 [in question you nedd to find 𝐃𝐜 ]
𝟒

 NOTE : column diameter decided by the vapour flowrate because [𝐀 𝐍 >> 𝐀 𝐝 ].

○ Concept of the calculation of Net area (𝐀𝐍 ) :

kg m
- Mass flowrate (Ṁ ) = ρ × A × v = × m2 ×
m3 s

𝐌̇𝐯 = 𝛒𝐯 × 𝐀 𝐍 × 𝐯𝐨𝐩

- ρv = density of vapour
- AN = Net area which is associated with vapour
- vop = Operational velocity

 vop is already given in to question as; vop = 30-50% vf

- vf = flooding velocity(it is high vapour flowrate) (given)

○ Concept of calculation of downcomer area(𝐀𝐝 ) :

- Ad is given in the quastion as; Ad = 10-20% AT

 We can find flooding velocity from chart : ---------

 𝛒𝐟 𝛒𝐯
𝐯𝐟 = 𝐂𝐟
𝛒𝐯

Cf = Coefficient of flooding (at low pressure it is constant)

At high pressure the value of 𝐂𝐟 is decreases and at low pressure it is increases.

○ Pressure drop between two plates :

- Here pressure 𝐏𝟏 (P = ρ. g. h) is because of liquid on that plate + vapour pressure

- Pressure 𝐏𝟐 is because of oressure of liquid on that plate + pressure of vapour on that liquid.
- Here h = space between two tray/plate.
∆P = 𝐏𝟐 − 𝐏𝟏

Tray Tower Operating Problems

---------
- Common problem faced in Distillation Column :
 Entrainment
Flooding
Weeping
Dumping
- These problems are not in packed bed column.

(1) Entrainment :
- When Liquid Carried by vapours up to the tray above is known as Entrainment.
- It is cause by
- This problem occur when we can not calculate diameter of column appropriate to operation.

- If you choose the small diameter then operation parameter need then the vapoure flowrate in column is
increases and if you choose bigger diameter then vapour flow rate is decreases.

 Entrainment showing in the figure :

(2) Flooding :
- When the , in comparison with liquid flowrate the liquid fills the downcomer
as well as an entire tray space and eventually the entire column.
- this phenomenon is called 'flooding'.
- Excessive entrainment can cause of flooding. (worst condition of Entrainment)
- Efficiency will decreases of the tray.

- In flooding the forth (height) of liquid on tray increases and fill entire space between two tray, therefore
there is no vapour present and that's why the efficiency of the column is decreases.

 Flooding showing in the figure : ---------

 The point at which this effect occures the velocities of vapour in column is operated is called is called as
flooding velocities.

- Here liquid occupy the whole space between two plates therefore pressure drop between two plate
increases.
- Pressure drop between two plate because of liquid therefore it is called hydraulic pressure drop.
- Pressure drop gape between caps and plate is dry tray pressure drop.(no vapour present gape between cap
and plate).
- Gape id also called perforation.

(3) Weeping :
- If a very small fraction of the liquid flows from a tray to lower one through perforation or openings of the
trays, the phenomenon is called 'weeping'.
- Weeping occurs at .

 Weeping showing in the figure :

 (4) Dumping : ---------
- When the , in comparison to liquid flowrate, liquid flows from a tray opening
without entering into downcomer. This phenomenon is called 'dumping'.

○ diagram of problems related to tray tower :

 How to avoid operating problems :

(1) Reboiler act as a pressure filter in the case of weeping we can increase the heat duty so as to avoid the
condition of weeping.

(2) In case of flooding we can decrease the heat duty to avoid the condition of flooding.

------------------------------------------------ END ---------------------------------------------------------