Introduction to Column

Distillation
Maurizio Fermeglia
[email protected]
Department of Engineering & Architecture
University of Trieste
 Agenda
Flash drums in series
Developing a distillation cascade
Specifications
External column balances

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 2

 Introduction to Column Distillation
Distillation is important
 90-95% of separations in chemical industry
 Approximately 40.000 distillation column operate around the world
 Consuming 40% of the energy used in US process industry
 Equivalent to 1.2 million barrels of crude oil per day
Flash distillation provides a method of separation, but
the amount of separation obtained is limited.
What if we need to have a greater separation to obtain
essentially pure components?
We could place flash drums in series or as a cascade…

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 3

 Flash Drums in Cascade
One can obtain a high level of
separation using cascading flash
drums.
The problem with this arrangement
is that we generate a large
number of intermediate liquid
and vapor streams, which would
need to be separated.
 One could feed these intermediate streams to
another flash drum cascade, but even more
intermediate streams are formed, and so on
and so on.
Let’s look at what we can do with
the intermediate streams…
Cascade of flash chambers:
p1>p2>p3>p4>p5
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 4
 Flash Drums in Counter-Current
Use of intermediate steams Isobaric operation

Counter current cascade of flash Counter current cascade of flash chambers with intermediate
chambers: p1>p2>p3>p4>p5 reboilers and condensers. P= constant: T1<T2<T3<T4<T5

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 5

 Flash Drums in Counter-Current
Reflux and boilup Intermediate heat exchange

Counter current cascade of flash chambers with reflux Counter current cascade of flash chambers
and boilup. P= constant: T1<T2<T3<T4<T5 with intermediate heat exchangers.
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 6
 Distillation Column
Schematic of 5 stage column
 T1<T2<T3<T4<T5<T6

  
downcomer weir

   L
V
  

L   

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 7

 The idea of multistage distillation
zA yN yn+1 yn y y yD
2 1

rectifying section A D
N n 1 C a)
L
xN x N-1 xn x n-1 x1 x0 Q

y y
2 1

1 C
b)
x1 x0 Q
D xD

y0 y1' y n'-1 yn' y N'

V
stripping section R 1' n' N'
A
Q' x 2' x n' zA
R x R x 1' x n'+1 x N'

• Heat is supplied at the bottom only and withdrawn at the top only
• All other condensations/vaporizations are by direct internal contacts
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 8
 Distillation Column

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 9

 Specifications

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 10

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 11
 Distillation Column:
Typical Specified Variables
 Column pressure, Pc.
 Feed flow rate, F.
 Feed composition, z.
 Feed temp. TF; enthalpy, hF; or quality, q = L/F.
 Reflux temperature, TR; or enthalpy, hD.
 Reflux ratio, L/D; or distillate composition, xD.
 Bottoms composition, xB.
Tools for Solution
 Equilibrium relationships
 Mass balances
 Energy balances
Methods of solution
 External column balances
 Overall
 Condenser
 Reboiler
 Internal column balances
 Stage-by-stage calculations

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 12

 External Column Balances
Overall mass balance
F=B+D
More volatile component
FzF = BxB + DxD
Distillate Stream D
zF − xB
D= F
xD − xB

Bottoms Stream B
xD − z
B=F−D= F
xD − xB
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 15
 External Column Balances
Energy balance

FhF + Q C + Q R = DhD + BhB

With
 hF (z, TF, p), hD (xD, Treflux, p), hB (xB, saturated liquid, p)
 Can be calculated form enthalpy composition diagrams (or
correlations)
Energy balance equation
 2 unknowns (QR and Qc)
 1 more equation is needed  that comes from the condenser
condition

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 16

 Condenser Conditions
Partial – only part of the incoming vapor stream, V1, is
condensed.
 We have both vapor and liquid streams at saturated conditions.
 D is taken as a saturated vapor and the liquid reflux, Lo, is returned to
the column as a saturated liquid.
 Both must be at saturated conditions since we have equilibrium – in fact
the partial condenser is an additional equilibrium stage.
 We will look at partial condensers later.
Total – all of the incoming vapor stream, V1, is
condensed to liquid.
 We then split the resulting liquid outlet into the distillate stream, D, and
the reflux Lo, which is returned to the column.
 We will consider only total condensers for now.

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 17

 Condenser conditions
Partial Total

Important note for total condenser

the mole fraction, y1, of the vapor stream from the top of the column is
equal to both the mole fractions, xD and xo, of the liquid streams!

y1 = xD = xo

The condition of the outlet of the condenser has to be specified as either a

saturated liquid or a subcooled liquid in order to use the energy balance.
The state of the liquid determines the heat duty of the condenser.
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 18
 Total-Condenser Mass Balance
Total mass balance
V1 = Lo + D
Component mass balance
V1 y1 = Lo xo + DxD

Since external reflux ratio Lo/D is

specified we can substitute its value
Lo Lo
V1 = D+D= 1+ D
D D

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 19

 Total-Condenser Energy Balance

V1 H1 + Q C = DhD + Lo ho

Lo
QC = 1 + D(hD − H1 )
D
Recall the D from the total material balance.
Lo zF −xB
QC = 1 + F(hD − H1 )
D xD −xB

Note that Qc< 0 because the liquid enthalpy is less than

that of vapor

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 20

 Reboiler Conditions
Partial – only part of the incoming liquid stream, L, is
vaporized.
 We have both vapor and liquid streams exiting the reboiler at saturated
conditions.
 B is taken as a saturated liquid and the boilup, Vn+1, is returned to the
column as a saturated vapor.
 Both streams must be at saturated conditions since we have equilibrium
in the reboiler – in fact the partial reboiler is an additional equilibrium
stage.
Total – the incoming liquid stream, L, is split first to
obtain our bottoms stream, B, as a saturated liquid.
 It has to be a saturated liquid since it leaves the equilibrium stage at the
bottom of the column.
 We then reboil all of the remaining liquid and return it to the column as
a vapor stream, V.

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 21

 Reboiler Conditions
Partial Total

Important note for total reboiler

the mole fraction, xN, of the liquid stream from the bottom of the column is
equal to the mole fraction, xB, of the bottom liquid stream and that fed to
the partial reboiler!

xB = xN

The condition of the outlet of the reboiler has to be specified as either a

saturated vapor or a superheated vapor in order to use the energy balance.
The state of the vapor determines the heat duty of the reboiler.
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 22
 Partial-Reboiler Energy Balance
Q R = DhD + BhB − FhF − Q C

Lo
Q R = DhD + BhB − FhF + 1 + D(H1 − hD )
D

zF − x B x D − zF Lo
QR = FhD + FhB − FhF + 1 + D(H1 − hD )
xD − x B xD − xB D

Note that QR> 0 because the liquid enthalpy is less than

that of vapor

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 23

 Example: external balances for binary distillation
A steady-state, countercurrent, staged distillation column
is to be used to separate ethanol from water.
 The feed is a 30 wt % ethanol, 70 wt % water mixture at 40°C. Flow rate
of feed is 10,000 kg/h.
 The column operates at a pressure of 1 kg/cm2.
 The reflux is returned as a saturated liquid. Reflux ratio L/D=3.0 is used.
 We desire a bottoms composition of xB = 0.05
(weight fraction ethanol) and a distillate composition
of xD = 0.80 (weight fraction ethanol).
 The system has a total condenser
and a partial reboiler.
Find D, B, Qc, and QR.

Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 24

 Example: external balances for binary distillation
From mass balance eq.

 And B = F − D = 10,000 − 3333 = 6667 kg/h

From Ponchon – Savarit graph, enthalpies are
 hD(xD = 0.8, saturated liquid) = 60 kcal/kg
 hB(xB = 0.05, saturated liquid) = 90 kcal/kg
 hf(z = 0.3, 40 ° C) = 30 kcal/kg
 H1(y1 = xD = 0.8, saturated vapor) = 330 kcal/kg
From energy balance around the condenser

From the column external energy balance:

 QR = DhD + BhB − FhF − QC
 QR =(3333)(60)+(6667)(90)−(10,000)(30)−(−3,599,640)=4,099,650 kcal/h
Separation Processes – Maurizio Fermeglia Trieste, 22 March, 2021 - slide 25