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MODULE
10
M10.1
Background
Conceptual Description
iVI 10.3
iVI 10.4
iVI I0.5
iVI 10,6
iVI 10,7
Multipliei tyBehavior
BACKGROUND
Distillation is a common separation technique for liquid slre-anlS cOlltaining two or more
components and is one of the more important unit operations in chl~mical manufacturing
processes. Design and control of distillation is important in order to produce product
streams of required purity, either for sale or for lise in other chemical processes.
597
598
Module 10
vapor
x
liquid
O.B
00
'"
0.6
"'"
OA
cQ
0,
>
:';;
02
0.5
x, liqUid phase light component
Sec. Ml0.2
599
For ideal mixtures, it is cOlllmon to model the phase equilibriulll relationship based
on constant relative volatility
o:x
}'=
(MIO.I)
+ (o:-I)x
where (~is known as the relative volatility. FigurcMIO.2 was generated based
tion (M 10.1) with (X ~ 2.5.
M10.2
011
equa-
Condenser
(Heat removed from condenser)
Overhead receiver
_...-'::=r=::.-=-----...
Reflux
Distillate Product
Feed
Stream
-----1>1
NF
Vapor Boil-up
NS
(Heat added
to Reboller)
Bottoms Product
FIGURE MlO.3
600
Module 10
8c
,
o
FIGUIU: 1\'110.4
for
it
Schematic diagraol
centratcd amount of the heavy component), while the rest is vaporized in the rcboiler and
returned to the column.
'file liquid from one tray goes over a weir and cascades down to the next tray
through a downcomcr. As the liquid moves across a tray, it comes in contact with the
vapor from the tray below. The schematic diagram for a sieve tray is shown in Figure
MUlA.
Generally, as the vapor from the tray below comeS in contact with the liquid, turbulellt mixing is promoted. Assuming that the mixing is perfect, allows one (0 IlHldcl the
stage as a lumped parameter system, as shown in !'igurc M 10.5. Notice that the vapor
fronl stage i is modeled as a single stream with molar flowrate Vi and light component
vapor composition (mole fraction) Yi' The liquid leaving stage i through the downcomer is
modeled as a single stream with molar fJowrate Li and light component liquid composition (mole haction) xi'
The conceptual diagram for the feed stage is shown in Figure MIO.6. It differs from
Figure M 10.5 in that an additional input to the stage is from the feed to the column.
Li__ l
Xil
Lixi
Lnfxnf
ViYi
Vi-t-l Yill
VIlf11
Ynf-t-l
Sec. Ml0.3
M10.3
601
The component balance for the liquid phase of a lypical stage as shown in Figure
MIO.S is:
accumulation liquid frolll
tray above
dNlrt i
dl
(M 10.2)
and that the liquid leaving the stage is equal to the liquid flowing from olle stage ahove:
(MIOA)
M10.3.2
Feed Stage
Let {{F' represent the quality of the fccdstrcam. If the feed is a saturated liquid, thcn qF =: (,
while 'iF ~ 0 fbr a saturated vnpor. The vapor molar f10wratc leaVing the feed stage is
(where NF =: number of the feed stage)
(M 10.5)
Similarly, the liquid molar nowrate of the slrcanl leaving the feed stage is:
(M I0.6)
M10.3.3
Condenser
A total condenser removes cnergy from the overhead vapor, resulling in a saturated liquid. Assuming a constant molar holdup in the distillate receiver, the total liquid nowrate
from the distillate receiver (reflux + distillate flows) is equal to the nowrate of the vapor
frotH the top tray:
V2
where Lv and D represent thc reflux and distillate molar nowratcs, respectively.
(MI0.7)
602
M10.3.4
Module 10
Reboiler
Ii = L NS _ 1 where
Vreboilcr
M10.3.5
Vrehoi1er
(MIO.8)
is the reboiler molar llowrate and B is the bottoms product molar flow rate.
The rectifying section (top section of column, above the feed stage) liquid molar nowrates
arc:
L R = L{)
(MIO.9)
The stripping section (bottom section of column, below the feed stage) liquid molar
flowratcs are
(MIO.IO)
The stripping section vapor molar flow rates are:
(MIO.II)
The recti fying section vapor molar flowrates arc:
(MIO.12)
In the following ~e assume a constant liquid phase molar holdup (dM/dt) = 0).
(MIO.l3)
The rectifying section component balance is (from i = 2 to NF~l):
dX j
"I
(MIOI4)
dX NF
dl
(MIO.IS)
1 [
dt = M Lx
'S i
r
"Xi
(MIO.16)
dxNS' =
"I
1
M [L\"NS_l - BxNS - V\YNS]
(MJO.17)
Ii
Sec. M10.4
603
EQUILIBRIUM RELATIONSHIP
It is assumed that the vapor leaving a stage is in equilibrium with the liquid on the stage.
The relationship between the liquid and vapor phase concentrations on a particular stage
can be calculated using the constant relative volatility expression:
y-=
,
I
M10.4
O'X i
(MIO.18)
+ (IX - I )x,
I,
~ y,~X, ~
(M 10.19)
(M 10.20)
LgxN/' -J + VSYNr+ I + FZ r
~ LS'''-NF - VUYNI
'-co
(M 10.21)
f;
:0'::'
LSX i _ 1 +
V.SYill -
LSx i
VSYi
(MIO.22)
f:vs
= LSX NS _ 1 -
Bx NS
VSYNS
= ()
(MI023)
where B = L, - V,.
EXAlV1PLE MIO.l
Stead'y~State Operation
of a 41-Stage Column
Consider a 41-stage column with the overhead condenser as stage 1, the feed tray as stage 21
and the reboiler as stage 41. The following parameters and inputs apply
ex
F
1.5
::: 1 mol/min
zr
0.5 mole fraction of light component
R
2.706 mol/min
D "'" 0.5 mol/min
qF
1 (sat'd liquid feed)
Module 10
604
Ls
-j
Fqr
2.706
+ I
3.706 mol/min
c=.
3.206 mol/min
V\' ,."'" L s -- B ,=
3.706 -- 0.5
'[ he ll1-tJle d 1 st C,b, Tn (shown in the Appendix) is used to sol ve for the steady-state compositions.
fsolve(
'di~-oL
S,3' ,xO)
The resulting compositions are shown in Figure M 10.7. Notice the strong sensitivity to rellux
flowrate.
alpha
1.5. R
2.706.
3206
_-J
[_~
08
__:_
nominal
~11 O~O,,
0.0.6
:c
>04
0.2
____1...
__-------'__
10
15
20
stage
.-----L.-
25
l.,_ ...
30
-~
35
40
Sec. Ml0.5
605
but small when the reflux is greater than 2.71 1l1OlImin. 'T'hc opposite relatiollship holds for bottoms composition, where the gain is small when reflux is Jess than 2.7 mol/min, but large for n.>
flux greater than 2.71 mol/min. This sensitivity has important nnnificati{)HS for control system
design.
~ 0.95
2.66
2.68
2.7
2.72
2.74
reflux
0.06
~ 0.04
0.02
o ::--::.-----
_~J:_~_'::-
2.66
2.68
2.7
1_________
2.72
_ ----L _
2.74
reflux
M10.5
EXAMPLE lV110.2
Dynamic Response
Consider now the previolls problem, with the initial condiLions of Lhe stage compositions equal
to the steady-state solution or Example M 1O. L The ~\dditional parameters needed for the dymunic simulation are the molar holdups on each stage. Here we use the following parameters:
MJ=M o
tv}]
M 3 :::: 5
:::::;5 mol
= 0.5 mol
=5 mol
606
Module 10
To illustrate the nonlinear behavior we compan.' the results of J-, I (j{ step changes in the reflux
rate at time t:;:: 5 minutes.
[t,x]o::ode45( 'dist_dyn' IO,400,xO)
Note that the currenl version of ode4 5 docs 1101 allow model p,lnullClerS to be passed through
the argument list, so global parameters afC defined in the m-filc dis L_dyn. m shown in the Appendix.
The following results arc shown in l;'igurc MIO.9. A positive lr;::- step change in the reflux
rate yields a snlal! increase in the distillate composition; tbis makes since because the maximum
possible increase in distillate purity is (J.()J (the composition cannot he greater than I mole hac
lion) while it call decrease much more than that. A negative J (J{ step change ill reflux causes a
larger change in the distillate purity. 'fhe opposite effects arc observed l~)r bottoms composition,
where a positive reflux change yields a large bottoms composition change. A negative reflux
change yields a small bottoms composition change.
0.98
~
0.96
0.94
50
100
150
200
250
300
350
400
250
300
350
400
time, min
0.06
0.04
?
0.02
o
o
50
100
150
200
time, min
M10.6
x ,- A x' t
y' ;: : : C x'
n u'
(M 10.24)
(MI0.25)
Sec. M10.6
av.' =
ilx;
Xl :;:;: X -- x~,
0'.
(I+I-I)x)'
607
(MIO.26)
V/JC
A11)
.;01'
(M 1(28)
i = 2 to NF-] :
ill;
JX i 1
(M 10.29)
M[
(M 10.30)
Au I
ill;
I
-)
(-t'i+ 1
VnJ(;
I'vf/
(MI031)
illy/
(MI032)
ANF,NF I
JXA'V_I
ill"
(MIO.33)
()x NP
A,V/<Nr+ I
ill,,
V)<',/
M,
dX,vF' I
(M I 0.34)
Fori=NF+1 toNS-I:
(If;
ax;
M[
(ivlIO.35)
(M 10.36)
A iJI
and for the rcboiler (stage iV,,')
ill;
V/<i-+J
()Xi i I
iVf/
(ivlI0.37)
608
A NS,NS-l
at;
."C:_-
O.li_ I
(M 10.38)
Mil
_(13 + V,K
ANS,NS
N ,)
(M 10.39)
MlJ
Module 10
ttl ;;;;:
LR
;;;;:
L! and
aj,
B,.2
Ill::::
Vii':::::
(M IOAO)
au?
VrehoJler:
For i = I to NS-I:
Mr
B'.2
aj;
Yil
Mr
OllZ
(MIOAI)
aj;
N.'),
ill,
.....
I ~--
au]
M NS
!!"\2
'. ~
1'_,. ~ aU
2
- Yvs
MNS
(M I OA2)
If the output variables arc the overhead and bottoms compositions, tIlcn:
C u " 1, while
C?NS
M10.6.1
= 1, while
eli .c.
C'!.i -::0'
0 for i
(M I 0.43)
0 for i ;f!
(M I OA4)
j.
(M IOA5)
M10.7
MULTIPLICITY BEHAVIOR
Even simple ideal binary distillation columns have been shown recently to have interesting steady~state and dynamic behavior, including multiple steady-states. Nice cxalnples
are shown by Jacobsen and Skogestad (1991, 1994). The key assumption that must be
made for this behavior to occur is that mass flows, rather than molar flows, arc manipu-
609
lated. The reader is encouraged to read these papers and modify the MArLAB m-files
presented in this chapter to illustrate the behavior shown by Jacobsen and Skogestad.
SUMMARY
In this chapter wc have dcveloped modeling equations to dcscribe tile steady-state and dynamic behavior of ideal, binary distillation COIUlllllS. The 41-stagc column example shows
that stcady-statc distillate and bottom compositions arc a nonlinear function of the manipulated inputs (distillate and vapor boil~up flows). Also, the dynarnic responses or these COll1positions depends on the magnitude <lnd direction of changes in the manipulated inputs.
610
Module 10
STUDENT EXERCISES
1. Consider a simple I tray (3 stage) column with the overhead condenser as stage I,
the feed tray as stage 2 and the reboilcr as stage 3. Usc the following parameters and
inputs:
R =
ifF
F
lJ
Zp
=
=
=
5
3 mol/min
I
1 mol/min
0.5 mol/min
0.5 mole fraction of light component
Find the bottoms product Jlowratc, the stripping section flowratc and the vapor boilup rate (stripping section vapor Ilowrate). Usc fsolve and dist_ss.m to find
the resulting compositions:
x =
0.703]
[
distillate composition
]
0.486 = composition of stagc 2 (the feed tray)
[
0.297
bottoms product composition
Consider now the dynamic behavior, with the initial conditions of the stage COITlPO~
sitions equal to the slcady~state solution. The additional paramcters needed for the
dynamic simulation are the molar holdups on each stage. Usc:
M,
M2
M,
kIn
=
=
5 mol
0.5 mol.
5 11101
At lime zero, the reflux is changed from 3.0 mol/min to 3.2 mol/min. Usc ode45
and dist_dyn. m to simulate the dynamic behavior shown in the figures below.
0.78
0.08
0.76
(J)
0.06
~ 0.74
.:- 004
~
0.02
0.72
0.7
S
time
is
10
time
Appendix
611
APPENDIX
function f
;::: dist_ss(x);
xO)
DIST~PAR
%
%
< 8;
disp ( not enough parametlC':rs given in
if 1engthIDIST_PAR)
I
disp ('
DIST~PAR ')
')
disp (' check to SQe that global DIS'I' PAR ha;" bCE"n defined ')
return
end
%
alpha
DIST_PAR(l) ;
DIST_PAR(2) ;
ns
nf
DIST~PAR(3) ;
feed
zfeed
DIS'r_PAR (4) ;
DIST_PAR('j) ;
IJIST_PAR I 6) ;
qf
%
reflux
vapor
DIST PAR(7)
-
D151'.. PAR(8) ;
96
612
~t,
f (i)
Ibot
II'
Is
%
%
Module 10
VI'
%
%
VS
x(i)
::0:-
%
%
y(i)
vapor flow
rectifying sec
reflux;
refl_ux + feed*qf;
lr
Is
%
vs
vapor;
vs + feed*(l-qf);
vr
%
dist_
Ibot
reflux;
Is - vs;
VI'
if dist < 0
disp('error in specifications, distillate flow < 0')
return
end
if Ibot < 0
disp{'error in specifications, stripping section ')
disp('
')
1;
f :::;: zeros(ns,l)
%
% calculate the equilibrium vapor compositions
%
for i=l:nsi
y(i)=(alpha*x(i))/(l.+(alpha-l.l*x(i));
end
9"
% material balances
%
% overhead receiver
%
f (1) = (vr*y(2) - (dist+xeflux) *x(I));
% rectifying (top)
section
Appendix
613
'r,
for i";2:nf-l;
flil=lr*xli-ll+vr*yli+ll-1r*x(il-vr*yli) ;
end
%
% feed stage
lr*x{nf-l)+vs*y{nf+ll-ls*x(nflvr*y(nf)+feed*zfeed;
f Infl
%
for i=n+1:n5-1;
flil ls*x(i-l)+vs*Yli+l)-ls*xli)-vs*y(il;
end
%
% reboiler
%
f(ns)=(ls*xlns-l)-lbot*x(ns)-vs*y(ns));
dist dyn.m
function xdot.
==
dist~ __dyn (t
x) ;
[t, xl
614
Module 10
return
end
%
alpha
n;:;
n
[cedi
zfeedi
DIST_PAR(I)
DIS'r__ PAH (2)
DIST PAR(3 )
DIS'I" PAR (4)
DIS'T' -- PAR ( ~) )
;
;
;
;
(0.5)
qf
DIST PAR(6) ;
rc;luxl
DIST .. PAR(7) ;
DIST_PAH(S) ;
~~
vapori
mel
mb
ml-
(3.206 )
d.1.stillatE' molar
~6
DIST_PAR(9) ;
DIS'I' PAR (10) ;
DIS'l' PAR (] 1) ;
hold~up
(5)
if length (DIST_Pt\R)
stepr
U:,:;tepr
==
19;
DIST_PAH(12);
st~cpv
rnS'l'. PAR(14);
tstepv
stepzf
tstepzf
stepf
DIS'1' YAR(15) i
DIST_PAR(16) i
Lst(~pf
else
stepr
st:epzf
end
~~-;
DIST_PAR(17)i %
DIST]AR (IS);
IHST PAR(19) i
';,
%
:(;
%
%
DI~_::T_PAR{9:19)
dist
Ibot
LI'
%
%
Is
vr
vs
x (i)
xdot(i)
y (i)
~6
Vs
<J(,
if t < tstepr;
vapor boil-up,
feed composit::.ion
Appendix
reflux
else
refLux
615
reflux,i;
refluxi
sLepr;
('Ond
if t < tstepv;
vapor i;
vapor
else
sLepv;
vapori
ViJ.por
end
if t: < tsLepzf;
zfeed. - zf(:,-cdi;
else
zfeed - zfeedi
end
stepzf;
if t < tstepf;
feec1i;
feed
else
feec1.i
feed
t-
SLOpr
end
(I, rectifying and strippi.nq section liquid flowrates
reflux;
reflux!
lr
1s
9,5
rectifying and
feed*qf;
st~.ripp_ing
vapor;
vs + feed*(l-qfl;
vs
VI'
vr -- reflux;
dist.
Ibc) t:
Is -
V~;;
if di;:3t: < 0
return
end
zeros (ns, 1) ;
%
Df:~gative ')
616
Module 10
for i==l:ns;
y(i)=(aIpha*x(i)I/(I.+(alpha-I.)*x(i)l;
end
% material balances
%
% overhead receiver
%
xdot(II=(I/md) * (vr*y(2) -(dist+reUux) *x(II);
%
% rectifying (top)
section
for i=2:nf-l;
xdot (i I = (I/mt)
end
% feed stage
%
xdot (nf)
r*y(nf)+feed*zfeed);
%
for i==0+1:os-1;
xdot(il=(l/mt)*(ls*x(i-ll+vs*y(i+l)-ls*x(il-vs*y(i)) ;
end
%
% reboiler
%
xdot (ns 1= (l/mb) * (18 *x (ns-l) -Ibot *x (ns) -vs *y (ns) I ;