UNIT OPERATION A – DISTILLATION TUTORIALS 1

Tutorial 2 : Short Cut Multicomponent Distillation

These questions relate to determining top and bottom column temperatures/pressures through
bubble and dew point flash calculations:

1. A mixture containing 40 mole % n-butane, 60 mole % n-pentane is to be separated by

distillation into two high purity product streams. Discuss the relative merits of carrying out
this separation at :

i) 150 kPa
ii) 350 kPa
iii) 700 kPa
2. An equimolar mixture of n-butane, n-pentane, n-hexane, and n-heptane is to be flashed at
5.5 bara. Find for this mixture (as efficiently as possible):

a) bubble point
b) dew point
c) temperature at which the vapour fraction is 0.6
d) vapour fraction at 110oC
3. The top product from a distillation column comprises :

Propane 10 kmol/hr
i-butane 30
n-butane 50
n-pentane 10
The column has a total condenser producing a saturated liquid product at 50°C.
Find :
a) column pressure
b) top stage temperature
c) temperature and composition of the vapour stream to the top stage.
(R = 3, Assume constant molal overflow )

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4. The bottom product from a distillation column, leaving its kettle reboiler at 140°C,
comprises:

kmol/hr
propane 1
n-butane 9
n-pentane 20
n-hexane 25
Total : 55
The vapour rate from the reboiler, returning to the column, is also 55 kmol/hr.
Assuming constant molar overflow and negligible pressure drop, calculate the follwoing:
a. column pressure
b. composition and temperature of the reboiler feed
c. composition of the liquid and vapour streams above the bottom stage within the
column.
5. A distillation column is being used to separate butane and pentane, as ‘top’ product, from
heavier hydrocarbons, in the presence of small quantities of lighter components
(characterised here as ‘methane’). In order to achieve some separation between the light
components and butane and pentane, a partial condenser is used with its vapour output
being vented and its liquid output being refluxed to the column. The main butane/pentane
‘top’ product is drawn off as a sidestream from the liquid leaving the column’s top
equilibrium stage.

The composition of the vapour passing from the top equilibrium stage in the column to the
condenser is:
kmol/hr
‘methane’ 9
n-butane 165
n-pentane 123
n-hexane 3
The condenser operates at 4 bar and cools the overhead stream by 25K. The sidestream
flow is 40% of the liquid flow from the top equilibrium stage.
Assuming constant molal overflow and negligible pressure drop, show that approximately 7-
8 mole% of the overhead stream is vented and determine the temperature, composition
and flow of the sidestream.

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6. A mixture containing :

n-butane 20 mole%
n-pentane 50
n-hexane 30
is to be separated into three products of about 99% purity. Prepare a preliminary material
balance for this system and suggest suitable operating pressures for the two columns
required. (Assume that the non-key components are not distributed.)
7. A feed containing 80 mole% propane and 20 mole% of a heavy contaminant with volatility
similar to that of n-octane is to be separated by distillation. The heavy component
polymerises at temperatures in excess of 200°C.
Determine a suitable column pressure and the corresponding distillate temperature in each
of the following cases:
i) if virtually complete separation of the two components is essential
ii) if 3% loss of the propane from the feed can be tolerated in the bottom product.

What substantial advantage follows if the second, rather than the first, of these cases is
accepted?
The column is designed to operate as calculated in ii) above, with a reflux ratio of 0.3.
Assuming a bubble point feed and constant molal overflow, estimate the mole%
compositions of the inlet and vapour outlet streams for the column’s partial reboiler.
8. Show that there are 14 possible sequences of 2-product distillation columns for separating
a 5 component mixture into effectively pure products. State, and justify wherever possible,
some of the 'rules of thumb' which can be useful in cutting down the number of possible
sequences to be considered.

When three distillation columns are used to separate a four component mixture (A, B, C,
D) into virtually pure components, the most commonly used column sequence is that
which removes one component as a time as distillate, starting with the most volatile. If
the order of volatilities is A>B>C>D, the most common flowscheme is:

A B C

A, B, C, D

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Suggest, and justify, alternative flowschemes which would be worth considering in each of
the following circumstances:
i) The four components are methane, ethylene, ethane and propane.
ii) Component C is 90% of the total feed.
iii) Component D is heat sensitive and heavily fouling.

9. 100 kmol/hr of a mixture containing 25 mole% each of propane, butane, pentane and
hexane is separated in a distillation column operating at 7 bar into two product streams: a
liquid top product in which 90% of the butane is recovered, and a bottom product in which
75% of the pentane is recovered. Assuming that all components are distributed, determine
a material balance for the unit.

10. Carry out a preliminary design for a column to fractionate 10 tonnes/hr of the following feed
:
Mole Fraction in feed
i-butane 0.12
n-butane 0.31
n-pentane 0.17
n-hexane 0.40
Assume an operating pressure of 3.5 bar, a saturated liquid feed, a total condenser and that
the reflux ratio is 1.2 times its minimum value.
The distillate is required to contain 99.0% of the n-butane from the feed and the bottoms to
contain 99.5% of the pentane.

11. A saturated liquid mixture containing 40 mol% n-hexane, 40 mol% cyclohexane, 20 mol%
n-heptane is distilled, into a distillate containing 95% n-hexane and 5 mol% cyclohexane.
The column operates at 2 bara pressure and has a total condenser which gives a saturated
liquid distillate at 94ºC, and a reboiler which gives a vapour return to the column at 120ºC .
Short cut calculation suggests there are 18.1 minimum stages and a minimum reflux ratio of
6.
a) Determine actual number of stages in this column, given that the actual reflux ratio is
1.2xRmin.
b) What would you expect to happen to the condenser and reboiler temperature if the
column pressure were to increase? As a consequence, what would you expect to
happen to the distribution of the heptane and the size of the column?
c) Determine the composition of the bottoms product.

K values are given in the following plot

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UNIT OPERATION A – DISTILLATION TUTORIALS 6

Answers
As many of the questions use dew and bubble point calculations, your answers may differ
from these – but not by much. Note that many questions also need a text answer.
Q1 – You need to find the average volatility and need some way of finding the top and bottom
temperatures. Have you tried this for 100% pure split? From this you should see what the
condenser and reboiler temperatures are. Think about what governs the CAPEX and OPE

Q2 Approximate Answers –
(To gain maximum benefit from this question, start with ‘poor’ 1st guesses for bubble point and
dew point. Perhaps 30o or so away from the answer provided.)
a) 99oC
b) 134oC
c) 122oC
d) 28%

Q3 Approximate Answers –
a) 6.5 bar
b) 62°C
c) 73°C (Mole Frns - 0.05, 0.24, 0.48, 0.23)

Q4 Approximate Answers –
a) 12.5 bar
b) (Mole Frns – 0.05, 0.25, 0.35, 0.35), 128oC
c) (Liq Mole Frns – 0.09, 0.28, 0.33, 0.30)
d) (Vap Mole Frns – 0.16, 0.40, 0.29, 0.15)

Q5 Approximate Answers –
Sidestream Composition: (Mole Frns – 0.001, 0.323, 0.639, 0.037)
Temperature: 66oC
Flowrate: 110 kmol/hr

Q6 Approximate Answers –
3.5bar, 1 bar, C4 (19.8, 0.2,0) C5 (0.2, 49.5, 0.3), C6 (0, 0.3, 29.7) )

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UNIT OPERATION A – DISTILLATION TUTORIALS 7

Q7 Approximate Answers –
i) Under this assumption, for K=1 for octane, 5 bar and -1°C.
ii) Under this assumption, the column should operate at about 13.5 bar.

Mole Fractions

Inlet Vapour Outlet

propane 0.51 0.60

‘octane’ 0.49 0.40

Q8 Approximate Answers –
Current scheme is A/BCD, B/CD, C/D.
i) A/BCD, BC/D, B/C – Carry out difficult separations in absence of other
components
ii) AB/CD, A/B & C/D = Separate the majority component as soon as possible
iii) ABC/D, A/BC, B/C – take out the problem component first

Q9 Approximate Answers –
About 0.1 kmol C3 in bottoms
About 0.4 kmol C6 in distillate

Q10 Approximate Answers –

Since the top product is all C4’s, makes little difference if total or partial condenser is used.
Select total condenser. Bubble Pt distillate temp is 33°C. Bubble Pt reboiler temp is 103°C.
Fenske equation number of stages is 10.1, average volatility taken with mean column temp of
68°C. Remember distribution of non-keys. Minimum reflux is 0.818 giving 25 stages. Feed is 15
from top.
Q11 Answers depend on accuracy in reading K values
a) 36 stages, c) (2.09, 38,20) kmols/hr on a basis of 100 kmols/hr feed.

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