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10/7/2017

SEPARATION TRAIN SYNTHESIS


PART I

INTRODUCTION
 Almost all chemical processes require the separation of
chemical species (components), to:
npurify a reactor feed
o
orecover un-reacted
t d species
i ffor recycle
l tto a reactor
t
pseparate and purify the products from a reactor
 Frequently, the major investment and operating costs of
a process will be those costs associated with the
separation equipment
 For a binary mixture
mixture, it may be possible to select a
separation method that can accomplish the separation
task in just one piece of equipment. However, more
commonly, the feed mixture involves more than two
components, involving more complex separation
systems.

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EXAMPLE OF FEED SEPARATION SYSTEM

Removal of C3 from a stream of propylene/C3


mixture. C3 is not involved in polypropylene
production
d ti so it iis removed d using
i a didistillation
till ti
unit.
Production of formaldehyde by air-oxidation of
MeOH using silver catalyst. Entering air is
scrubbed with aq NaOH to remove SO2 and
CO2 which are catalyst poisons.

Effluent Separation System and


Recycle

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EXAMPLE: BUTENES RECOVERY

Butenes Recovery System

2 columns, C3
& 1-Butene in
distillate (Total
150 trays)
y )
Depropanizer

Deoiler Unit: Extractive


Pentane Distillation Unit: n-
withdrawn as C4 and 2-C4=s
bottoms cannot be separated
byy ordinaryy
distillation (=1.03),
Furfural Stripper: 2- so 96% furfural is
C4=s withdrawn as added as an
distillate. Furfural is extractive distillation
recovered as agent ( 1.17). n-
bottoms and C4 withdrawn as
recycled to C-4 distillate.

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Separation is Energy Intensive

nthe creation by heat transfer, shaft work, or


pressure reduction of a second phase that is
immiscible with the feed phase (ESA energy
separating agent)
othe introduction into the system of a second fluid
(chemical) phase (MSA mass separating agent).
This must be subsequently removed/recovered.
pthe addition of a solid phase upon which
adsorption
d ti can occur.
qthe placement of a membrane barrier for selective
permeation.

SEPARATION FACTOR

 The separation factor, SF, defines the degree of separation


achievable between two key components of the feed.

 SF is arranged (for calculation) to give value >1.0; possible


separation The larger the SF
separation. SF, the easier is to separate the
mixtures.

 SF is generally limited by thermodynamic equilibrium.

 For example, in the case of distillation, using mole fractions as


the composition variable and letting phase I be the vapor and
phase II be the liquid,
p q , the limitingg value of SF is g
given in terms
of vapor-liquid equilibrium ratios (K-values) as,

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y /x K P s

SF = = = =
1 1 1
for ideal VLE
1

P
1, 2 s
y /x K
2 2 2 2

= Relative Volatility
1, 2

P = vapor pressure of species 1


1
s

Algorithm to Select Pressure and Condenser Type

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EXAMPLE
A liquid mixture containing 50 mole % propane (C3-), 50 mole % propene (C3=) is
fed at a rate of 1000 mol/h to a distillation unit. Estimate the operating pressure for
a column separating C3- from C3=, assuming cooling water at 30C is available for
use.
What would be the top temperature of the column?

Column Temperature

Tdew,C Tcw

Tbub,C

T dew,R

TST

T bub,R

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T bp (K) Tc (K) A B C
n-butane 272.6 425 15.68 2154.9 -32.42
Benzene 353 562 15.9 2788.51 -52.34
Toulene 384 593 16.014 3096.52 -53.67

lnP*=A - B/(T+C)
(mmHg, K); 1 bar
bar=750
750 mmHg

Scenario 1 Scenario 2
(kmol/h) FEED D1 B1 D2 B2
n-butane 20 20 20
Benzene 30 30 30
Toulene 50 50 50

Explain bubble point and dew point?


What are the bubble point and dew point of pure water?
Calculate column pressure and T bub at the column bottoms for each scenario.
Why cooling water can be used to condense n-butane (Boiling point=272.6K)?
Calculate T dew for each scenario.
Calculate relative volatility of the adjacent components if the feed entering at
310K.

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Choose the right column pressure!!

Consider the separation of a mixture of 50 mol/hr of C3H8 (1) and 50 mol/hr


C3H6 (2) at a pressure of 1.1 bar and a bubble point feed temperature of
230 K. Under these conditions, P02=930.5 mm Hg and P01=724.1 mm Hg
and 1/2=1.285. Setting the recoveries of the two components at 0.99
(lk,2) and 0.01 (hk,1), we find out that at total reflux, the minimum
number of trays Nm (by Fenske Eqn) is

0.99 0.99
Nm = ln . / ln lk / hk = 36.65
0.01 0.01

Now if the pressure is increased tenfold to P=10


P 10.94
94 bar
bar, we have a
bubble point feed temperature of 300 K and P02=8975.6 mm Hg, and
P01=7458.5 mm and 1/2=1.203. As a result, for the same recoveries,
the separation becomes more difficult and the minimum number of
trays increases to Nm=49.72.

Number of Sequences for Ordinary Distillation (OD)


Equation for number of different sequences of ordinary
distillation (OD) columns, NS, to produce P products:

[2(P 1)]!
Ns =
P ! (P 1)!

P # of Separators Ns
2 1 1
3 2 2
4 3 5
5 4 14
6 5 42
7 6 132
8 7 429

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EXAMPLE: SEQUENCES FOR 4-COMPONENT


SEPARATION
Direct sequence
All final products but one are
distillates.
Widely used in industry

Indirect sequence
All final products but one are bottoms
products.
Least desirable in industry.

5 possible Sequences for 4-component separation

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Determine The Best OD Sequence


For mixture with wide distribution of concentration
or wide variation of volatility, use direct
sequence.
or do detail design and costing for all sequences!
but this is possible only for number of product is
small (< 4).
Otherwise, use heuristics to reduce the number
of sequences for detailed examination

The Best Sequences using Heuristics


Guidelines to reduce the number of OD sequences:

n Remove thermally unstable, corrosive, or chemically reactive


components early in the sequence.
o Remove final products one-by-one
one by one as distillates (the direct
sequence).
p Separate early in the sequence, those components of greatest
molar percentage in the feed.
q Sequence separation points in the order of decreasing relative
volatility so that the most difficult splits are made in the absence
of other components.
r Sequence separation points to leave last those separations that
give the highest purity products.
s Sequence separation points that favor near equimolar amounts
of distillates and bottoms in each column. The reboiler duty is
not excessive. (especially if energy cost high)

You will likely end up with more than one sequences for further examination.

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Example: Paraffin Separation


Arrange in the
order of
increasing
boiling point

Question:
Use heuristics to determine a
sequence of OD columns to
meet the given specifications.

Variation of range of relative volatility and also


wide variation in molar percentage
1st column should separate C3 , the most volatile
Two most difficult splits are iC4/nC4 and
iC5/nC5, so two separate columns for these
separation
2nd column should be for separation of nC4 and
iC5 as LK and
d HK respectively.
ti l
The resulting sequence is as follows.

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Possible Solution

Guided by Heuristic 4,
the first column in
position to separate the
key components with the
greatest SF.

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