Further Reading
Diwekar UM (1995) Batch Distillation: Simulation, Optimal Design and Control. Series in Chemical and Mechanical Engineering. Washington, DC: Taylor & Francis.
1081
and 1980s all major mass-transfer equipment manufacturers developed structured packings. Compared
to the traditional tray columns spectacular improvements in plant capacity were achieved, but also some
projects were pitfalls, when the expected beneRts did
not materialize. Manufacturers started realizing that
liquid distributors had to be improved, but there was
no coherent understanding, nor correlations, that
could lead to a safe distributor-column system design.
Many manufacturers returned to trays, producing
new improved designs, using the area under the
downcomer for vapour Sow: these trays are offered
with new names that indicate their increased vapour
Sow capacity (MaxySow, Superfrack, etc.). The need
for good distribution and its effect on the column
efRciency are now well understood, allowing safe
design and efRcient applications for random and
structured packings in large industrial columns.
General Concepts
Distillation separation is based in relative volatility
that makes it possible to concentrate the more volatile
components in the vapour phase while the less volatile ones remain in the liquid phase. Distillation
columns are countercurrent vapour}liquid masstransfer devices, where the required separation and
puriRcation of components is achieved.
1082
Random packings
First generation,
before 1950
Second generation,
1950}1970
Rashing rings
Lessing rings
Saddles
Intalox (Norton)
Pall Ringsa
IMTP (Norton)
CMR (Koch Glitsch)
Chempakb
Fleximax (Koch Glitsch)
Nutter Ring (Nutter)
Grids
Structured packing
Wire-mesh typed
Sulzer BX and CY
Mellapack (Sulzer)
Flexipack (Koch Glitsch)
Gempack (Koch Glitsch)
Intalox (Norton)
Montz packing (Montz)
Developed by BASF, still marketed (or variations of it) by most packing manufacturers.
Developed by Leva, marketed by Nutter.
c
Variations of these grids are now offered by most packing manufacturers.
d
Developed by Sulzer, they are now offered by other manufacturers.
b
reSux, so that there is no net product. The minimum reSux sets the limiting slope of the operating
line, required to achieve a given separation.
E At constant , the NTS increases as the product
purity increases. The increase is proportional to the
logarithm of the key components purity ratio.
It can be also demonstrated that:
E At constant product purity, the minimum reSux
decreases as increases.
E At constant product purity, the minimum number
of stages decrease as increases.
E At constant , the minimum reSux decreases as the
product purity decreases.
Figure 1 Number of stages required vs. relative volatility at several product purities.
1083
E At constant , the minimum number of stages increases as the product purity increases.
All these statement say that deRnes the separation
difRculty. For values around 1.1 and lower, separation by distillation becomes very difRcult, requiring
very large and expensive columns. For "1 the mixture is azeotropic and would require the addition of
selective entrainers if azeotropic or extractive distillation is to be applied.
Packing Selection
Figures 3 and 4 illustrates random and structured
packings. There are many parameters to be considered in the selection of packings; in some cases,
there are one or two considerations that dictate the
selection, such as capacity for a revamp, which could
favour structured packing. There are also some considerations or applications, such as high-pressure
distillation, that could make structured packing a
questionable choice. Table 2 gives some general guidlines on packing selection.
[1]
1084
Figure 3 Random packings: (A) IMTP. (Photo courtesy of Norton Chemical Process Products Corporation.) (B) Nutter Ring.
(Photo courtesy of Sulzer Chemtech.) (C) Cascade Mini-Rings (CMR2+) and Fleximax. (Courtesy of Koch}Glitsch Inc.) (D) Pall
Rings metal and plastic. (Courtesy of Koch}Glitsch Inc.)
where:
Pi"C110@ u .
Gf"G(0.075/g)0.5(Fp/20)0.5100.024 Mg
u1
2
g g
P"C2G2f 10C3Lf
#0.4(Lf/20 000)0.1(C2G2f10C3Lf)4
[2]
1085
Figure 4 Structured packings: (A) Wire gauze structured packing. Close view, packing and wiper bands. (Photo courtesy of
Koch}Glitsch Inc.) (B) Two structured packing layers rotated 903. (Photo courtesy of Koch}Glitsch Inc.) (C) One structured packing
element for small towers. (Photo courtesy of Sulzer Chemtech.) (D) Structured packed bed for a small tower. (Photo courtesy of
Koch}Glitsch Inc.) (E) Packed bed for a large tower built in sections. (Photo courtesy of Norton Chemical Process Products Corp.)
1086
Figure 4 Continued
Lf"L(62.4/1)(Fp/20)0.50.1
(for Fp over 15)
l
C2"7.4;10\8 and C3"2.7;10\5
For the case of dry packing Lf"0, the pressuredrop equation reduces to:
P"C2G2f"C2(0.075/20)FpG2/g.
[3]
Application in distillation
Random packing
Structured packing
Traditional trays
High-capacity trays
2
2
2
2
2
3
2
3
2
2
1
4f
2
3
2
1
1
4
1
1
4
1
4
1
2
2
2f
4
4
4
3
3
2
2
3
2
4
1
2
3
4
1e
1
1
1
3
2
1
3
4
1
4
1
2
3
4
1e
1
1
3
[4A]
[4B]
[5]
[6]
[7]
1087
Flooding Correlations
Several generalized Sooding and pressure-drop correlations have been proposed for commercial packings. Sherwood, Shipley and Holloway presented
the Rrst correlation between a Sow parameter X
deRned as:
X"(L/G) (g/l)0.5
[8]
[10]
[11A]
1088
Figure 6 Striegle pressure drop chart. (Permission from Gulf Publishing Company.)
[11B]
1089
Packing metal
Nominal size
Packing
factor (Fp)
Specific surface
ft 2 ft\3 (a)
Bulk density
(lb ft\3)
Pall Rings
0.625
1
1.5
2
3.5
81
56
40
27
18
103
61
39
30
18
0.918
0.953
0.971
0.969
0.972
39.9
23.1
14.3
14.1
13.9
CMR
0
1
1.5
2
2.5
3
4
5
60
38
33
26
21
14
12
8
103
76
57
44
38
32
23
15
0.957
0.968
0.961
0.970
0.974
0.979
0.985
0.989
20.96
15.51
18.66
14.29
12.54
10.22
7.36
5.46
IMTP
No
No
No
No
No
No
Nutter Rings
0.7
1.0
1.5
2.0
2.5
3.5
15
25
40
50
60
70
51
41
24
18
16
12
88.7
69.8
46.9
31.2
25.3
17.5
0.961
0.970
0.969
0.981
0.982
0.984
17.9
14.1
14.6
9.3
8.7
8.1
N/A
30
24
18
16
13
69
51
38
29
25
20
0.978
0.978
0.978
0.979
0.982
0.984
11.0
11.1
11.3
10.8
9.0
8.3
1090
Packing 453
Crimp angle
Size
Packing factor
Specific surface
ft2 ft\3 (a)
Bulk density
(lb ft\3)
Mellapack (Sulzer)
125Y
250Y
350Y
500Y
10
20
23
34
35
78
107
155
0.989
0.987
0.983
0.975
5.09
5.61
7.8
10.92
Sulzer BX (Gauze)
BX
21
150
Gempack (Koch
Glitsch)
4A
3A
2A
1A
55
23
15
9
138.1
91.4
67
35
0.942
0.962
0.972
0.977
17
9.9
6.3
4.7
Intalox (Norton)
1T
2T
3T
4T
5T
28.0
20.0
15.0
13.5
12.0
95.2
65.3
51.9
40.6
27.0
0.980
0.984
0.987
0.986
0.991
10.14
8.23
6.55
6.75
4.5
Montz
B1-100
B1-200
B1-250
B1-300
Structure packings
Surface-treated metals
Plain surface metals
30
61
76
91
20
33
Tray spacing
36
24
18
12
inches
inches
inches
inches
20
30
40
50
60
1.15
1.45
1.90
2.41
0.96
1.22
1.60
2.03
0.87
1.10
1.44
1.84
0.81
1.03
1.35
1.71
0.76
0.97
1.27
1.62
0.73
0.93
1.22
1.55
a
Tray capacity based on the column full cross-sectional area,
without discounting any area for downcomers (which implies highcapacity trays). For conventional trays the ratio of packing capacity/tray capacity will be higher. Tray capacity taken from the
generalized correlation of tray flooding proposed by Fair JR and
Matthews RL (Petroleum Refiner 37(4): 153). The packing capacity taken from the generalized correlations presented by RF
Striegle Jr and Figure 6).
0.94
1091
Gravity-fed distributors
Pressure-fed distributors
POH
PAN
NTD
POH
SNH
Uniformity
High-purity fractionation
Maximum drip points per area
For large diameter towers (over 10 ft)
1
1
2
1
1
1
1
3
1
1
1
1
2
3
2
1
3
3
2
1
Leakage potential
For high liquid rates
For high vapour rates
Residence time
Solids handling
Turndown
Easy installation and levelling
Cost
C
2
1
C
3
1
1
B
Ha
1
3
A
3
1
3
A
C
2
1
B
2b
1
2
A
C
2
1
C
2
1
1
C
C
1
1
C
1
3
1
C
[12]
1092
Figure 10 NTD distributor: (A) Photo courtesy of Norton Chemical Process Products Corp. (B) Photo courtesy of Koch}Glitsch Inc.
Q"4.0nd 2(h!hd)0.5
Other Considerations
and:
n"0.25Q/d 2(h!hd)0.5
[13]
The minimum recommended oriRce diameter, to prevent plugging, is 3/8 inch for carbon steel and 1/8
inch for stainless steel. The minimum recommended
liquid level at minimum Sow is 2 inches. If a 50%
turndown is speciRed, the required liquid level at
normal liquid load becomes 8 inches.
The minimum recommended ratio of the tower diameter to the packing size is 8. In the case of structured
packings, this ratio applies to the ratio of the tower
diameter to the crimp size.
Fouling
1093
[14]
Distributor Testing
Water test of assembled distributors at the manufacturers workshop is always a good practice for all
high-efRciency distributors. The test should determine liquid rate gradients under the distributor,
liquid level in the distributor itself at design and
1094
Table 7 HETP correlation factors for a reference system, regressed by the authors for eqn [14]
Packing
Constant Kp Exponent f
Structured packings
Sulzer Mellapak
Koch Flexipac
Koch}Glitsch Gempak
Average of above structured
packings
126
100
120
106
0.73
0.69
0.76
0.70
73
198
250
110
0.43
0.69
0.69
0.50
properties:
HETP"HETPo(/Sg)n /(/Sg )n0
[15]
[16]
[17]
1095
Maldistribution
Liquid maldistribution has a very large effect on column distillation performance. Liquid maldistribution
is originated by uneven liquid Sow from the distributor to the top section of the packing. Some degree of
maldistribution cannot be avoided and it is related to
the following factors.
Drip points density (total drip points/column crosssection area) In principle, a smaller number of drip
points equates to a higher initial maldistribution. This
could be solved by constructing distributors with
a high number of drip points. However, there are
physical and mechanical limits that make it difRcult
to build distributors with more than 20 drip
points ft\2. It has also been demonstrated that if the
distributor deck is not levelled, the resulting maldistribution effect may increase as the number of drip
points is increased above an optimal number. The
optimal number of drip points is related to the liquid
irrigation Sow as follows (Figure 15):
Liquid irrigation
g ) m\1 ) ft\2
Optimum number drip
points per square foot
0.25 0.5
1.0
2.0
4.0
13
21
32
induce additional maldistribution. Operational problems such as plugging of the distributor deck areas
will cause large sectors to be dry, thus producing
a macroscopic or sectorial maldistribution.
Maldistribution and spreading factor Initial maldistribution produces a condition of uneven liquid/
vapour Sow ratio across the column cross-sectional
area. Some areas or spots are underirrigated and some
are overirrigated. The column packing does spread
the liquid resulting in some correction or attenuation
of the initial maldistribution. The overall weighted
maldistribution is attenuated better in small diameter
columns than in larger columns. This is determined
by the nondimensional number (Zb/CD2c), where Zb is
the bed height in feet, Dc the column diameter in
inches, and C is the spreading factor in ft ) in\2 units
(see Figure 16). The spreading factor is related to the
packing particle size and the liquid irrigation.
The lost column efRciency is proportional to the
liquid maldistribution, and this effect is ampliRed by
the number of theoretical stages required to achieve
the separation. Figure 17 presents a useful correlation
for the calculation of the column efRciency in packed
distillation columns.
Liquid distributor quality The liquid distributor intrinsic maldistribution, Md (related to its design and
manufacture) should be measured at the factory by
a water test measuring the liquid Sow under each
subsection of the column cross-section. The smaller
and more numerous the test area subdivisions,
the more precise will be the maldistribution
1096
[18]
[19]
[20]
[21]
[22]
h
hd
NTS"Z/HETPop.
[24]
G
Gf
V
L
Lf
Li
Lav
Fp
Kp
n
HETP
Future Developments
With the ability to accurately design and predict the
performance of packings in distillation, it is expected
that the use of packings in distillation will become
better accepted, not only for plant revamps but also
for grass roots applications. The design and evaluation of liquid distributors needs to be better understood by users and equipment manufacturers; standard methods for distributor quality rating should be
implemented based on the basic concepts presented in
this contribution. Readers interested in further exploring the column design methods outlined in
this article may download a free demo of BDSIM
at url http://www.geocities.com/&combusem/
BDSIM.HTM
Nomenclature
Ac
P
C
Co
C1 , C2 , C3
d
Dc
Ez
Cs
g
l
ug
Column cross-sectional
ft2
area
Packing pressure drop
in ft\1
Packing spreading factor ft in\2
OriRce Sow coefRcient
Constants in pressure drop
correlations
OriRce diameter
in
Column diameter
in
Bed efRciency
%
Vapour capacity factor,
ft s\1
deRned by
Cs"ug(g /(l!g))0.5
Gas density
lb f\3
Liquid density
lb f\3
Vapour velocity
ft s\1
HTU
l
Sg
X
Y
Yf,YHf
a
a0
gc
NTS
R
Rm
Md
Mo
Mbz
Q
Qd
Zb
1097
inches of
liquid
inches of
liquid
lb ft\2 h\1
lb ft\2
lb h\1
lb ft\2 h\1
lb ft\2 h\1
gallons
min\1 ft\2
Liquid average mass Sow gallons
min\1 ft\2
Packing factor
HETP correlation factor
Number of measured points
(in distributor testing)
Height equivalent of a
in
theoretical plate
High of a transfer unit
in
Liquid viscosity
cP
Liquid speciRc gravity
Flow factor"
(L/G) (g /l)0.5
Vapour Sow parameter. At
Sooding Y"Yf
Flooding parameters,
deRned by eqns [10] and
[11]
Packing surface area
ft2 ft\3
Open area of one drip point
Relative volatility
Void fraction
Surface tension
dynes cm\1
Gravitational constant
32.2 ft s\2
Number of theoretical
stages
ReSux ratio
Minimum reSux ratio
Maldistribution originated %
by the distributor design
Total initial maldistribution%
Effective bed
%
maldistribution
Liquid Sow
gallons
min\1
Distributor quality
%
Bed height
ft
Kinematic viscosity
constant"l/Sg
Ratio of the equilibrium
curve slope to the operating
line slope
1098
See also: I/Distillation: Historical Development; Modelling and Simulation; Theory of Distillation; Tray Columns:
Performance; Tray Columns: Performance; Vapour-Liquid
Equilibrium; Correlation and Prediction; Vapour-Liquid
Equilibrium: Theory.
Further Reading
Bonilla J (1993) Dont neglect liquid distributors. Chemical
Engineering Progress 83(3): 47.
Eckert JS (1961) Chemical Engineering Progress 57(9): 54.
Fair JR and Matthews RL (1958) Petroleum ReTner 37(4):
153.
Klemas L and Bonilla J (1995) Accurately assess packedcolumn efRciency. Chemical Engineering Progress
91(7): 27.
Introduction
Laboratory distillation encompasses an operating
range from millilitres in bench-top devices to pilot
units with the capacity for producing several hundred
kilograms of product per day. While the design of
bench-top assemblies is generally geared towards the
achievement of a speciRed purity grade of the desired
product, quantitative predictions are not usually feasible for such equipment and their construction relies
a great deal on ingenuity and craftsmanship. For
dedicated applications, glassware companies offer
off-the-shelf equipment. This article will therefore
focus on the pilot-scale units, where the analytical
principles of mass and heat transfer can be applied
to the operation, design and optimization of the
equipment.
The section on theory presents analytical descriptions of batch distillation for three different approaches in order of decreasing complexity. It starts
with a comprehensive model for a nonadiabatic, nonzero hold-up, nonconstant molar overSow, nonideal
multicomponent column. The second model presented neglects stage hold-ups and assumes adiabatic
stages and constant molar overSows to arrive at a set
of equations describing the transient behaviour of the
equipment, which can be solved for a binary system
using a simple spreadsheet. If constant relative volatility and operation at minimum reSux are further