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Chapter 21
Distillation
Different methods:
yD y 1 f x (21.2)
y x F
yB x f f
1 f xF
Eq (21.2) y x (21.2)
f f
1 f
A straight line, slope :
f
Letting x = xF in Eq (21.2)
y = xF , that is (xF,xF) is a point on line Eq (21.2)
The material-balance line crosses the diagonal at x = xF for
all values of f.
4
1 f
slope :
f
Example 21.1
A mixture of 50 mole percent benzene and 50 mole percent toluene is
subjected to flash distillation at a separator pressure of 1 atm. The vapor-liquid
equilibrium curve and boiling-point diagram are shown in Figs. 21.2 and 21.3.
Plot the following quantities, all as functions of f, the fractional vaporization: the
temperature in the separator (T), the composition of the liquid leaving the
separator (xB), and the composition of the vapor leaving the separator (yD).
Solution
1 f x
Feed point (xF,xF) = (0.5,0.5), Operation line: y x F
f f
bubble
point line
(x)
0.5 0.71
0.455
7
Continuous Distillation with Reflux : Rectification
Flash distillation
Rectification
continuous distillation with reflux
liquid and vapor leaving the plate
are brought into equilibrium
xn+1 yn+1
xn yn
xn-1 yn-1
A : more volatile component
B : less volatile component V (in dew point)
(heat of vaporization)
low boiler, A
liquid vapor
high boiler, B
(heat of condensation)
Reflux
provides the
downflowing liquid in
the rectifying section that V
is needed to act with the
up flowing vapor.
13
Net Flow rates
Va = La + D
D = Va - La
La V>L
Xa
D Vn+1 = Ln + D
XD D = Vn+1 - Ln
F
XF
Lm = Vm+1 + B
B = Lm Vm+1
V<L
Lb = Vb + B
B = Lb - Vb
B
XB
Net flow rate
A material balance around the condenser and accumulator in Fig. 21.8 gives
Considering the part of the plant enclosed by control surface I in Fig. 21.8. A total
material balance around this control surface gives
D = Vn+1 Ln plate n (21.8)
D is the net flow rate of material upward in the upper section of the
column. Regardless of changes in V and L, their difference is constant and equal
to D.
Similar material balances for component A give the equations
Quantity DxD is the net flow rate of component A upward in the upper section of
the column. It, too, is constant throughout this part of equipment.
For Stripping section:
B = Lb-Vb=Lm-Vm+1 (21.10)
BxB = Lbxb-Vbyb=Lmxm-Vm+1ym+1 (21.11)
The slope of the line defined by Eq. (21.13) is, as usual, the ratio of the flow of
the liquid stream to that of the vapor stream.
Vn+1 = Ln + D
Ln DxD
yn 1 xn
Ln D Ln D (21.14)
17
Vn+1yn+1=Lnxn+DxD
Ln Dx
yn 1 xn D (21.13)
Vn 1 Vn 1
18
For striping section
A material balance over control surface 2 in Fig. 21.8 gives
Vm+1ym+1=Lmxm-BxB (21.15)
Lm Bx
ym1 xm B (21.16)
Vm1 Vm1
Lm Bx B
ym1 xm (21.17)
Lm B Lm B
19
Ln
Slope of op line :
Vn 1
Ln
for rectifying section, slope = 1
Ln D
Lm
for stripping section, slope = 1
Lm B
The slope of the operating line in the rectifying section is always less than 1.0
In the stripping section the slope is always greater than 1.0.
When Ln, Lm are constant, the op lines are straight, when Ln. Lm are
not constant, the op lines are curved, and the position of a curved op line
should be determined by mass balance and enthalpy balance.
20
Number of Ideal plates: McCabe-Thiele Method
Require:
(1) Equilibrium curve
(2) Operation line
straight line: constant molar flow
curve line: enthalpy balance is required
V, L upper column
V,L lower section
21
Reflux ratio
L V D
RD (Used in this text book) V
D D
L L (21. 18) D
RV L
V LD condenser
Ln DxD
Eq (21.14) yn 1 xn (divided by D)
Ln D Ln D
RD xD
yn 1 xn (21.19):
RD 1 RD 1 operation line for
rectifying section
RD L xD
Slope = , intercept =
RD 1 V RD 1
22
To determine the operation line, one point is required. RD x
yn 1 xn D
RD 1 RD 1
In Eq (21.19), set xn = xD RD x
yn 1 xD D xD
RD 1 RD 1
(xD,xD) is a point at the upper end of OP line or
OP line intersects the diagonal at point (xD,xD)
23
According to the properties of OP line, the upper terminus is (xc, y1)
(xD, xD)
y1
xc
xD = y'
condenser
Tc, Lc xc y1,V1 a(xc, y1) end point of column
T1 Plate 1
a'bc the top plate
L x1
V
If condensate is at its bubble point, Tc = Tbc,
xD = y'
L = Lc, V = Vc (V1)
If the reflux (condensate) is cooled condenser
below the bubble point, Tc Tbc, Tc, Lc xc y1,V1
then V1 V, L > Lc
T1
Plate 1
L x1
L = L - Lc V
LC C pC (Tbc TC )
L (21.21)
C
C : heat of vaporization of condensate)
L LC L LC [1 CPC (Tbc TC ) / C ]
The actual reflux ratio:
D D D
(21.22)
Normally Tbc = T1 (bubble point of condensate)
(p676 description)
26
Bottom plate and re-boiler
Lm Bx B Constant L. V L Bx B
Eq. (21.17) ym1 xm ym1 xm (21.23)
Lm B Lm B
LB LB
27
yb =yN
yr
yr
xB
abc:
bottom plate
xB reboiler:
(An ideal plate)
L V
29
(a) Cold feed, (b) Saturated liquid, (c) Partially vapor,
q1 q=1 0<q<1
31
Feed line
For 1 mole feed, to liquid: q, to vapor: (1-q)
F mole feed, to liquid: Fq, to vapor: F(1-q)
L L qF or L L qF (21.26)
V V (1 q) F or V V (1 q) F (21.27)
V ym Lxm1 Bx B (21.29)
(xB,xB)
33
Feed plate location optimum location
Transfer can be occurred between a - b
Optimum location
Criterion
Feed plate
the triangle that has one corner on the rectifying line, and
one corner on the stripping line.
Feed on the wrong plate may seriously affect the column performance.
Feed close to a or b will lower the quality of both the top and bottom product
Heating and cooling requirements
Heat effects of entire unit condenser and reboiler
Heat added in the reboiler : qr V (sensible heat change of liquid is
small)
V
Amount of stream required: ms (21.32) V
s D, HD
s: latent heat of steam qc= V up
: molar latent heat of mixture
If q = 1, feed at saturated liquid, (V V )
F, HF
heat supplied in reboiler = heat removed in the condenser
(V ) = (V )
Amount of cooling water required: V
V Lb
mW Xb
B, HB
T2 T1 (21.33) Hb
qr = V low
T2-T1 = temp. rise of cooling water
36
V
D, HD
qc= V up
F, HF
Lb
Xb
Hb B, HB
qr = V low
37
Base: Benzene (a): D= ?, B=?
XF = 0.4 (b): N =? , feed plate?
XD = 0.97 (c): steam required? (kg/h)
XB = 0.02
(d): cooling water required? (m3/h)
RD = L/D = 3.5/1
B = 7360 cal/gmole
T = 7960 cal/gmole
XF = 0.4
XD = 0.97
XB = 0.02
F = D + B,
0.44x78 + 0.56x92 =85.84 FXF = DxD + BxB
D xF xB
F xD xB
(b). Calculate number of ideal stage and feed position
(i) Feed at Tb (95) : q=1 (saturated liquid)
feed line: (xF,xF) = (0.44,0.44)
slope = -q/(1-q) =
rectifying line: (xD,xD) = (0.974,0.974)
intercept = xD/(RD+1)
= 0.974/(3.5+1)
= 0.216
stripping line: (xB,xB) = (0.0235,0.0235)
intersection of feed line
and rectifying line
41
(b)-(iii): feed is a mixture of 2/3 vapor, 1/3 liquid.
By definition: q = 1/3
Slope of q line =
- q/(1-q) = -0.5, (xF = 0.44)
43
(d) Calculate the cooling water required
(in: 25, out: 40) = 996.3 kg/m3)
(7360 is more reasonable)
V 690x7960
mw 366160 Kg/h
CPW (T2 T1 ) 1(40 25)
366160
Volume flow rate = 367.5 m3/h
996.3
44
q Steam req. No. ideal Satu. Liq. Cold feed
cold plate (N)
2 1.37 12500 10
Satu.
1 1.0 10520 11 vapor.
3 0.33 6960 12
45
Minimum number of plates (Nmin)
Slope of rectifying line: RD/(RD+1) = (L/V)
RD increase slope increases Nideal decreases
RD infinite total reflux, (V=L), (L/V = 1), slope = 1
(RD = L/D = ) , OP line = diagonal
At total reflux, the number of plates is a minimum,
but the rates of feed and of both the
overhead and bottom products are zero.
---- one limiting case in the operation
of fractionating columns.
No feed, no discontinuity
Between the upper and lower section
46
Slope of rectifying line:
RD/(RD+1) = (L/V)
RD increase
slope increases
Nideal decreases
R()
47
Simple method for calculating Nmin
--- for ideal mixture and constant AB y Ae / x Ae
AB (21.34)
AB : relative volatility yBe / xBe
y A / x A PA ' / P PA '
AB PA/PB does not change much with
yB / xB PB ' / P PB ' temperatures column, so the relative
volatility can be taken as constant.
48
For a binary system yA/yB and xA/xB may be replaced by yA/(1-yA) and xA/(1-xA),
so Eq. (21.34) can be written for plate n+1 as
y Ae / x Ae y Ae / y Be yn 1 x
AB AB n 1 (21.37) ---- EQ line
yBe / xBe x Ae / xBe 1 yn 1 1 xn 1
For the total reflux , D = 0 and L/V = 1, slope=1, the operating line is the 45 line.
OP line: (xn, yn+1) , yn+1 = xn --- OP line
xn x
combine EQ and OP lines: AB n 1 (21.38)
1 xn 1 xn 1
At the top of the column, if a total condenser is used, y1 = xD, so Eq.(21.37) becomes
xD x
for n=0, Eq. (21.37) AB 1 (21.39)
1 xD 1 x1
49
xD x
AB 1 (21.39)
1 xD 1 x1
xn x
Writing Eq. (21.38) for a succession of n plates gives AB n 1
1 xn 1 xn 1
x1 x
n=1 AB 2
1 x1 1 x2
(21.40)
xn 1 x
AB n
1 xn 1 1 xn
If Eq. (21.39) and all the equations in the set of Eqs. (21.40) are multiplied together:
xD x
( AB ) n n (21.41)
1 xD 1 xn
xD x
( AB ) N min 1 B
1 xD 1 xB
50
Solving the equation for Nmin by logarithms gives
xD x
( AB ) N min 1 B
1 xD 1 xB
ln[ xD (1 xB ) / xB (1 xD )
N min 1
ln AB (21.42)
Equation (21.42) is the Fenske equation, which applied when AB is constant. If the
change in the value of AB from the bottom of the column to the top is moderate, a
geometric mean of the extreme values is recommended AB.
51
Minimum reflux, RDm
La
minimum reflux ratio RDM --- No of plates is infinity.
D min
La La
( x , y )
D min D
When RD decreases
RD
slope decreases ( line upward)
1
D
R
OP lines moves upwards toward the EQ line,
no. of plates increases. ( N : )
At RDm (minimum reflux)
OP line, feed line intersect at EQ line (ad, bd, fd)
RDm x y'
slope : D
RDm 1 xD x'
x
At RDm, the plates required to obtain x D is .
B
For EQ curve which is
If RD < RDm, even the N is , the separation concave downward
xD xD y '
x B cannot be approached. R (21.44) (Eq 24.11)
y ' x'
Dm
52
for system with EQ curve of concavity upward --- ethanol / water
Line correspondings to the minimum
reflux ac
small RD The OP line that is tangent to the
EQ line.
higher RD
RD, min
feed line
53
Invarient zone, ( pinch point )
At minimum reflux ratio, the number of ideal plates is infinite. There are regions
where liquid or vapor concentrations do not change from plate to plate ( xn = xn-1 ; yn+1 =
yn ). These regions are called invariant zone, or pinch point ()
The d point in Fig 21.19 (intersection of q
line and EQ line)
the concentrations at feed plate
the concentrations of invarient zone
above feed plate : L / V the only difference of
the two zones
below feed plate : L/ V
rectifying
feed section
plate
invariant
zone
stripping
section
54
Optimum reflux ratio --- consider the total fixed charges
(1) Fixed charges on the heat exchange equipment, (the reboiler and condenser)
increase steadily with the reflux ratio
(2) Fixed charges on equipment
cost of unit: total plate area
(No. of plates cross sectional area)
N x Area
for a given production ( D is constant ),
when RD is increased, L , V
No. of plate decreases (N ) ,
V, L increase, column diameter increases.
(Area ) RDm
Total cost: (1) + (2)
drop sharply at first with increasing RD, then
pass through a very shallow minimum
optimum reflux ratio
N , decreases
Area , increases
L V
Lb
Xb
Hb B, HB
qr = V low
56
When energy costs are relatively high RD (optimum) closer to RDm
Actually, most plants are operated at reflux ratios somewhat above the optimum,
because the total cost is not sensitive to reflux ratio in this range.
EXAMPLE 21.3. What are (a) the minimum reflux ratio and (b) the minimum number of
plates for cases (b)(i), (b)(ii), and (b)(iii) of Example 21.2 ?
Solution: in example 21.2. xD = 0.972 xF = 0.44
(a) minimum reflux ratio:
intersection of feed line EQ line, (x, y)
(xD , yD) (0.972 , 0.972)
q=1
= 1.37
= 0.333
RDm y y xD y '
slope : D RDm
RDm 1 xD x y ' x'
57
(b) minimum number of plates
the OP lines coincide with the
diagonal, the results have no
difference between the three
cases.
59
EXAMPLE 21.4. A mixture of 2 mol percent ethanol and 98 mol percent water is to be
stripped in a plate column to a bottom product containing not more than 0.01 mol percent
ethanol. Steam, admitted through an open coil in the liquid on the bottom plate, is to be
used as a source of vapor. The feed is at its boiling point. The steam flow is to be 0.2 mol
per mole of feed. For dilute ethanol-water solutions, the equilibrium line is straight and is
given by ye = 9.0xe. How many ideal plates are needed ? V
L
L 1 xa = 0.02 ya
Solution: dilute solution L, V constant, V 0.2
H CP, T Tref
at Tb
H V H V,B y B H V,T yT ( function of T )
d
HV ,B B,ref T dTref CP,V ,B
toluene at
Tb = 110.6oC HV ,T T ,ref T d Tref CP,V ,T
(benzene) benzene
80oC
61
_
V
The enthalpy balance for the entire system V
D, HD
FH F qr DH D BH B qc (21.45) qc= V up
FH F DH D BH B ( feed at Tb )
Lb
Xb
Hb B, HB
qr = V low
63
Enthalpy balance in rectifying and stripping sections
Va H y ,a DH D La H D qc
qc Va H y ,a La H D DH D
(21.47)
64
(21.47) into (21.46) f (yn+1) f (xn) La
Ln xn DxD
material balance yn 1 (21.49)
Vn 1 Vn 1
known : xn , Vn1 Ln D (21.50)
solve : Ln, Vn+1, yn+1
Find Vn+1 and Ln at specified xn value by trialanderror,
using (21.48), (21.49), (21.50)
Known : VaHy,a , RHD , D , xD
Tb
Chosen : xn Hx,n (From Fig 21.24)
(Vn) (Ln-1)
Trial and error : (1) assume Vn+1 = Va , Ln = La (constant molar flow rate)
(2) calculate yn+1 (Eq 21.49) Hy,n+1 (Fig 21.24) ; (3) Ln = Vn+1 D (Eq 21.50)
(4) calculate new Vn+1 by Eq (21.48), Ln by (21.50) ; (5) repeat steps (2) (4)
65 until (yn+1) (yn+1)
step m step m+1
Hx,n Hy,n+1
Tb try Ln = La Td enthalpy Ln OP
Assume xn yn+1 new new yn+1
OP net flow rate Vn+1 line
line Vn+1 = Va
compare or repeat
f (yn+1) f (xn)
La
Vn1H y ,n1 Ln H x,n Va H y ,a RH D
Ln xn DxD
yn 1
Vn 1 Vn 1
Vn1 Ln D La D
HD HD
LmHx,m + qr = Vm+1Hy,m++BHB
69
Calculate RD ( = 1.2RDm ), q = 1.0
0.72
Eq (21.3)
xD y
RDM ( based on L constant )
y x V
x = 0.5 = xF , y = 0.72 ( EQ curve)
xD y 0.98 0.72
RDM 1.18
y x 0.72 0.5
La
R
RD 1.2 RDM 1.42 ( )
D
La = R = 1.42D = 1.42 50 = 71 mole
La
V1 = R + D = 71 + 50
= 121 mole
L1 = R = 71 mole
La
70
Enthalpy balance calculate first
Va 121
Eq (21.48) Vn1H y ,n1 Ln H x,n Va H y ,a RH D
La La 71
Reference Temp : 80oC ( Tb of Benzene)
H D H R 0 ( nearly pure benzene at Tb ) H x CP, T 80
Hx,a
for benzene vapor at T oC , Hy,B = 7360 + 23( T 80) --- (A)
for toluene vapor at T oC , Hy,T = 8174 + 33( T 80) --- (B)
vapor of
enthalpy of vaporization at T oC at 80oC liq. Toluene toluene
HV
T oC T oC
H V Cp (Tb T ) Cpv (T Tb ) H V,b
H V H V,b (Tb T )(Cp Cpv ) Cp Cpv
vaporization
at T = 80oC HV = 7960 + (110.6 80)(40 30)
= 8174 (cal / mole) Tb HV b = 7960 Tb
(110.6) (110.6)
So, toluene vapor at T oC , Hy,T = 8174 + 33(T 80 )
71
Evaluate Hy,1 ( Hy,a ) Top plate temp. 80oC Hy,B = 7360 + 23( T 80) --- (A)
yB yT Hy,T = 8174 + 33( T 80) --- (B)
Hy,1 = 0.98 Hy,B + 0.02 Hy,T Eq (A) and Eq (B)
= 0.98 7360 + 0.02 8174
= 7376 (cal mole)
72
Hx,n Hy,n+1
Tb try Ln = La Td enthalpy Ln OP
Assume xn yn+1 new new yn+1
OP net flow rate Vn+1 line
line Vn+1 = Va
compare or repeat
To estimate yn+1 :
use : Ln = L1 = 71 mole L/V value to draw the OP
Vn+1 = V1 = 121 mole Line , and get yn+1 , or ( 21.49 )
Ln DxD
y n 1 xn y
71
0.5 50 0.98 0.698
Vn 1 Vn 1 121 121
dashed line
yn+1 0.7
dew point Td 93oC ( Fig 21.3 )
Benzene : 0.7 , Toluene : 0.3
Hy,B = 7360 + 23( T 80) --- (A)
Hy,T = 8174 + 33( T 80) --- (B)
Fiqure 21.25
McCabeThiele diagram for Example 21.5 benzene-toluene distillation:
74
Calculate Hy,n+1 ( at 93oC ) Hy,B = 7360 + 23( T 80) --- (A)
Hy,T = 8174 + 33( T 80) --- (B)
Hy,n+1 = 0.7 HyB,n+1 + 0.3 HyT,n+1
= 0.7(7360 + 23 13) + 0.3(8174 + 33 13) = 7942
0
Eq (21.48) -- Vn+1 Hy,n+1 = Ln Hx,n + V1 Hy,1 R HD , ( Ln = Vn+1D )
Fiqure 21.25
McCabeThiele diagram for Example 21.5
benzene-toluene distillation:
, based on constant molar overflow;
, based on enthalpy balance.
76
To estimate the OP line of stripping section, qr should be known first, use of
overall enthalpy balance
F HF + qr = D H D + B HB + qc ------ (C)
HF : feed at boiling point ( xF = 0.5, TF = 92oC ) V1 Hy,1
H F CP, (T 80)
(0.5 33 0.5 40)(92 80) 438 cal
mole qc
HD : = 0
HB : TB 111oC ( close to Tb of toluene, 110.6oC ) La D
HD HD
x, benzene = 0.02 , x, toluene = 0.98
HB = (0.02 33 + 0.98 40)(111 80) = 1236 cal mole
qc : V1 Hy,1 = qc + (La + D)HD
0
qc = 121 7376 = 892,496 cal
From Eq(c) qr = 50 0 + 50 1236 + 892,496 100 438
= 910,496 cal ( 2% error for qr qc ) 77
Estimate , Lb , Vb
enthalpy balance around reboiler :
qr + Lb Hx,b = Vb Hy,b + B HB ------ (D)
? ?
Vb + B
50 1236 o
Lb , Hx,b 111 C, y = 0.05
x = 4% Vb , Hy,b
Hy,b : about 5% benzene at 111oC ( Fig 21.3 ) 110oC
78
Lb = Vb + 50 , into Eq (D) qr + Lb Hx,b = Vb Hy,b + B HB
(Vb + 50)
Eq (D)
qr 50 H x ,b BH B 910496 50(1192) 50(1236)
Vb 114.3
H y ,b H x ,b 9141 1192
Lb 114.3 50 164.3
79
Calculate an intermediate value of Vm+1
Eq (21.51) Vm+1 Hy,m+1 = Lm Hx,m + qr B HB
Lm BxB
ym1 xm
Eq (21.52) Vm1 Vm1 Eq (21.53) Lm = Vm+1 + B
80
Eq (21.51) Vm+1 Hy,m+1 = Lm Hx,m + qr B HB
8194 Vm+1 = (Vm+1 + 50)558 + 910,496 50 1236
Vm+1 = 114.8 ; Lm = 114.8 + 50 = 164.8
(Vb = 114.3) (Lb = 164.3)
84
Reason :
Eq (21.49) Vn+1 yn+1 = Ln xn + D xD
Ln = Vn+1 D or Vn+1 = Ln + D
or (Ln + D)yn+1 = Ln xn + D xD
Ln (yn+1 xn) = D(xD yn+1) --- (21.55)
Eq (21.55) Ln xD yn 1
(21.56)
Eq (21.54) Vn 1 xD xn
Ln
, slope of line connecting ( xD , xD ) , ( xn , yn+1 )
Vn 1
Lm y x
for stripping section m1 B ( xB , xB ) , ( xm , ym+1 )
Vm1 xm xB
85
File download (PDF files):
in FTP of Lab.
: 140.116.33.193
: units
: units
: 650
Lm Vm+1
xm ym+1
Hx,m Hy,m+1
Lb Vb
B, xB,
HB
qr