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Distillation, 2. Equipment
JOHANN STICHLMAIR, Technische Universit€at M€unchen, Garching, Germany
Figure 2. Schematic of a tray column showing the most important design parameters A) Vertical section
dcap ¼ cap diameter; dV ¼ valve diameter; dh ¼ hole diameter; hcl ¼ height of skirt clearance of downcomer; hw ¼ weir
height; H ¼ tray spacing; V_L ¼ volumetric flow rate of liquid
B) Cross section a) Small holes with narrow spacing; b) Bubble caps with wide spacing
Ad ¼ cross-sectional area of downcomer; Aac ¼ active cross-sectional area; Dc ¼ column diameter; lL ¼ length of liquid
path; lw ¼ weir length
Equations (5) and (6) are determined for sieve Figure 5. Minimum gas load of sieve trays for three different
trays operated with three different systems as systems a) Air–water; b) Benzene–toluene; c) Isobutane–n-
shown in Figure 5. At low hole diameters the butane
460 Distillation, 2. Equipment Vol. 11
ity forces which results in a limitation of the distribution of liquid. Accordingly, it is recom-
maximum liquid load. In practice, four empirical mended to ensure a minimum liquid-flow
rules of thumb are applied to the determination of rate over the exit weir larger than
maximum liquid load: V_L =lw 2 m3 m1 h1 . In small diameter col-
umns, however, the liquid load can be consider-
. The relative weir load V_L =lw should be lower ably lower.
than 60 m3m1h1.
. The liquid velocity in the downcomer should
not exceed the value 0.1 to 0.2 m/s. 2.3. Two-Phase Flow on Trays
. The volume of the downcomer should permit a
residence time of the liquid of more than 5 s. Decisive for the performance of tray columns is
. The height of the clear liquid in the downcomer the behavior of the two-phase layer on the trays.
should not exceed half of the tray spacing H. Three different structures of the two-phase layer
can be distinguished:
These rules have been developed by long term
practical experience. However, they do not per- . Bubble regime: The liquid constitutes the con-
mit any insight into the limiting physical phe- tinuous phase. The gas rises in the liquid in
nomena. In essence, liquid flow through a down- form of discrete bubbles
comer is comparable with the flow of liquid out of . Drop regime: The gas forms the continuous
a vessel, which is described by Torricelli’s equa- phase and the liquid is dispersed into fine
tion: droplets
. Froth regime: This regime represents the in-
pffiffiffiffiffiffiffiffiffiffiffiffi
uLd ¼ a 2gH ð7Þ termediate state between bubble and drop
regime. The two-phase layer is intensively
agitated and no univocally dispersed phase
This basic equation has to be adapted to the exists
conditions present at the outlet area of a down-
comer. According to Stichlmair [4, 11] the fol- The froth regime is the dominant regime at
lowing relationship holds for a standard tray normal column operation. Only in vacuum ser-
design: vices drop regime may sometimes exist on trays.
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
ffi
V_L max r r hDp þhL Relative Liquid Hold-Up. Relative liquid
¼ aeLd hcl 2gH L G 1 ð8Þ
lw rL eLd H hold-up eL is a very important parameter of the
two-phase layer on a tray. It is defined as the ratio
of clear liquid height hL and froth height hf :
Where eLd denotes the relative liquid hold-up in
the downcomer, hcl the height of the downcomer hL
eL ¼ ð9Þ
clearance, hDp the pressure loss of a tray ex- hf
pressed in clear liquid height, and hL the clear
liquid height on the tray (see Section 2.3). The There exists a large data base of relative liquid
orifice discharge coefficient a has, in most cases, hold-up data and many empirical correlations in
a constant value of 0.61. For non-foaming sys- literature. Most published data are well summa-
tems, a value of 0.4 is recommended for the rized in the following correlation [4, 11]:
relative liquid hold-up eLd in the downcomer.
eL ¼ 1ðF=Fmax Þ0:28 ð10Þ
pffiffiffiffiffiffi
for F 0:2 rG ð11Þ
Figure 7. Liquid isotherms in the two-phase layer of a bubble-cap tray operated with hot water and air. Data were determined on a
bubble-cap plate with a diameter of 2.3 m, at a relative liquid flow rate V_ L =lw of 10 m3 m1 h1 A) Gas load F ¼ 0.47 Pa1/2;
B) Gas load F ¼ 1.61 Pa1/2;
flow of the liquid across the tray. Here, significant in the froth. The shape of the isotherms in Figure
concentration gradients exist in the liquid on the 7 proves increased liquid velocities near the walls
tray due to cross flow of gas and liquid. and in the center of the tray.
Predicting the degree of liquid mixing, Liquid maldistribution affects mass transfer
expressed in Peclet Pe-number, requires knowl- efficiency of columns. However, in tray columns
edge of the dispersion coefficient DE . Only few maldistribution is restricted to a single tray since
experimental data have been published in litera- the liquid is well mixed in the subsequent down-
ture. The following correlation is recommended: comer and evenly redistributed to the next tray.
1=2 Therefore, tray columns are better suited for
eL large-diameter columns than packed columns
DE ¼ 1:06hf F ð13Þ
rL rG where the detrimental effects of maldistribution
accumulate over the packing height (see Section
3.4).
Maldistribution of Liquid. Undisturbed
plug flow of liquid across the tray provides the Interfacial Area. One of the most important
highest mass transfer rate attainable in a tray quantities of the two-phase layer on a tray is the
column. In small diameter columns the plug flow size of the interfacial area contributing to mass
is disturbed by back-mixing of some liquid. In transfer. Present knowledge on interfacial
large diameter columns, however, back-mixing area on trays is rather poor and contradicting.
of liquid is of minor importance. Here maldistri- Figure 8 shows the result of a theoretical estima-
bution, i.e., non-uniform liquid flow across the tion [4, 11] of the relative interfacial area a
tray, is the prevailing mechanism. Some charac- (interfacial area referred to the volume of the
teristic flow patterns are shown in Figure 7 two-phase layer) for three systems with different
[4, 11]. The lines plotted in the active area of surface tensions. This rough estimation shows
the trays are liquid isotherms experimentally that in aqueous systems the relative interfacial
determined in the system air–water (hot). In such area is in the range of 500–600 m2/m3. In organic
a system the mass transfer from water into air systems, however, the relative interfacial area
causes a temperature decrease of water (like in a typically reaches values up to 1000 m2/m3 or
cooling tower). In a first approximation, the even larger.
isotherms are lines of constant residence time of
the liquid in the froth. In case of plug flow the Pressure Drop. The pressure drop of a gas
liquid isotherms are supposed to be parallel flowing through a tray is a very important quan-
straight lines. Any deviations from straight lines tity. Generally, the pressure drop (better pressure
are caused by local variations of liquid velocities loss) should be as low as possible, in particular in
Vol. 11 Distillation, 2. Equipment 463
vacuum services. Pressure loss of the gas signifi- Dry Pressure Loss of Bubble-cap and Valve
cantly depends on both gas and liquid load as Trays. Bubble-cap and valve trays have very
shown in Figure 9. During operation the pressure complex geometrical structures that make the
drop exerts an upward force on the mechanical rigorous prediction of the orifice coefficients
structure of the tray. rather difficult. As such elements are built in
The pressure loss is caused by the gas flow great numbers, the orifice coefficients are exper-
through the openings in the tray and by the liquid imentally determined by the vendors.
Figure 9. Pressure drop of a sieve tray versus gas load. The parameter lines denote constant liquid flow rates across the outlet
weir.
Liquid load V_L =lw , m3/(m h): a) 0 (dry pressure drop); b) 4; c) 10; d) 20; e) 40; f) 60
464 Distillation, 2. Equipment Vol. 11
Figure 10. Orifice coefficient jo for a very small relative free area j and for sharp edged holes of a sieve tray
Dashed lines indicate theoretical limits.
For the calculation of the dry pressure loss of 2.4. Mass Transfer in the Two-Phase
bubble-cap and valve trays a slightly different Layer
approach is recommended. The orifice coeffi-
cient is not related to the velocity in the smallest At the present state of the art the mass transfer on
geometrical open area but to the whole active a tray is expressed by tray efficiencies. Two
area of the tray since the quality of tray design definitions of tray efficiencies have to be distin-
depends not only on the pressure loss of a single guished, i.e., point efficiency EOG and tray effi-
element but also on the number of elements ciency EOGM .
arranged on the tray. The following definition
implies both quantities:
0 r
Dpdry x u2 ð16Þ
2
yyn1
EOG ð17Þ
y ðxÞyn1
Packed columns are as important as tray columns . Random packings consist of a dumped bed of
in the process industry. Due to novel develop- particles made of ceramic, metal, or plastic
ments of packing elements the industrial use of (Fig. 15). The shape of the particles should
packed columns is steadily increasing. In packed ensure a homogeneous structure of the dumped
columns there exists a genuine countercurrent bed and a low pressure drop of gas flow.
flow of gas and liquid as is shown in Figure 14. Standard particles (Raschig rings, Berl sad-
An intimate contact between gas and liquid dles) have a closed surface. Modern particles
phases is established by packings that represent are characterized by net structures (Pall rings)
a solid structure with large porosity and large or grid structures (Super rings). The size of the
internal surface. The liquid proceeds downwards particles must not exceed 5–10 % of the col-
on the packing in form of thin films or rivulets. umn diameter. The porosity of a bed is as high
Decisive for a good performance are a low as 70 % (ceramic particles) and more than
Vol. 11 Distillation, 2. Equipment 467
90 % (metal particles). The volumetric surface sure drop per equilibrium stage is typically as
of a bed depends on particle size and on column low as 0.5 mbar.
diameter. Typical values are 50–300 m2/m3
(Table 2). The separation efficiency of random Very important for all types of packings is a
packings strongly depends on column diame- uniform liquid distribution at the top of the bed
ter. Typical values of industrial columns are in and a bed-height limitation of 6–8 m. Beneath
the range of 1–2 equilibrium stages per meter each bed, the liquid has to be collected, mixed,
packing height. and redistributed. These measures intend to sup-
. Structured packings have been increasingly press the maldistribution of liquid because it
used since the mid 1960s because they better strongly affects mass transfer rates. The design
meet the requirements for homogeneous bed of liquid distributors, liquid collectors, support
structures. The standard design consists of grids etc. should provide a high open area in order
parallel corrugated metal sheets, ca. 20 cm in to assure the countercurrent flow of gas and liquid.
height, with alternating orientation of subse-
quent layers (Fig. 16). The porosity of struc-
tured beds is significantly higher than 95 %. 3.2. Operation Region of Packed
The specific surface area is typically Columns
250 m2 =m3 or higher (Table 3). Structured
packings have a lower pressure drop and a Packed columns can be operated within certain
better mass transfer efficiency than random limits of gas and liquid loads only. A typical
packings. Mass transfer efficiency is as high operation region of packed columns is shown in
as 2–4 equilibrium stages per meter. The pres- Figure 17. The mechanisms that set limitations to
468 Distillation, 2. Equipment Vol. 11
Type e a, m2/m3
Figure 17. Operation region of packed columns a) Minimum liquid load; b) Operating region of liquid distributor; c) Flooding;
d) Operating region of packing
ed packing. Flooding point and loading points are the following equation [16]:
also marked in this diagram.
2=9
A more rigorous approach to flooding is based r s3 g 1=2
uL min ¼ 7:7106 L4 ð22Þ
on pressure drop models of irrigated packed beds hL g a
(see Section 3.3).
Minimum Liquid Load. The minimum liq- For industrial practice the following values are
uid load of random packings can be estimated by recommended:
Figure 18. Correlation of flooding of packed columns according to Mersmann [14, 15]
Calculated cuves are shown for different values of the pressure drop in an irrigated packing, Dpirr / (H rL g): a) 0.2; b) 0.1;
c) 0.05; d) 0.04; e) 0.03; f) 0.02; g) 0.01; h) 0.005
470 Distillation, 2. Equipment Vol. 11
Dpirr 1eð1hL =eÞ ð2þcÞ=3 hL 4:65
¼ 1 ð27Þ
Dpdry 1e e
packing volume, are presented in Figure 21 [17].
Here, the experimental values of the hold-up hL
Evaluation of this equation demands knowledge are plotted versus the pressure drop in the packed
of the liquid hold-up hL in the bed. bed Dpirr =ðHrL gÞ. Two regions can be distin-
guished in this diagram:
Liquid Hold-up in Packed Beds. Liquid
hold-up is a decisive parameter of two-phase . A region of low pressure drop (low gas load)
flow in packed beds. Typical values of the where the hold-up depends on liquid load only
hold-up hL , defined as ratio of liquid volume to (horizontal parameter lines)
. A region of high pressure drop (high gas load)
where the hold-up is further increased by
pressure drop
Dpirr
D
HrL g Figure 22. Pressure drop and flooding of a packed column in
an irrigated packing composed of 25-mm Bialecki rings
Equation (31) can be solved by iteration only. As (metal). The values of the abscissa are determined from
Equation (28)
flooding of random packings typically occurs at Calculated curves are shown for different values of the
values of the dimensionless pressure drop pressure drop in an irrigated packing, Dpirr/(H rL g):
Dpirr =ðHrL gÞ 0:1 to 0:3, a value of D ¼ 0:1 a) 0.3; b) 0.2; c) 0.1; d) 0.06; e) 0.04; f) 0.02; g) 0.01;
is a good first estimation. h) 0.006; i) 0.004; j) 0.002
Figure 22 presents the result of the evaluation
of Equation (27) together with Equations (28)
and (29) for a random packing of Bialecki rings. stage (HETP) are also determined and applied to
This plot is almost identical with the empirical column dimensioning. A more rigorous approach
flooding correlation of Mersmann (Fig. 18). Just is based on the following equation valid for
the dimensionless liquid load is replaced by the undisturbed plug flow of gas and liquid within
liquid hold-up hLo below loading. the packing:
!
uG b M ^ r
HOG ¼ 1þm G L G ð33Þ
3.4. Mass Transfer in Packed Columns bG aeff bL M^G rL
Table 5. Values of critical surface tension in Equation (34) [19] Table 6. Selected values of the factors CV and CL in Equations (39)
and (40) according to [21]
Packing material scrit , N/m
Packing CV CL
Polyethylene 0.033
Poly(vinyl chloride) 0.040 Raschig rings (ceramic) 50 0.210 1.416
Ceramic 0.061 25 0.412 1.361
Glass 0.073
Raschig super rings (metal) 1 0.440 1.290
Stainless steel 0.071
2 0.400 1.323
Steel 0.075
3 0.300 0.850
Bialecki rings (metal) 50 0.302 1.721
35 0.390 1.412
25 0.331 1.461
aeff
¼ 1exp
a Pall rings (metal) 50 0.410 1.192
" 0:05 2 0:2 # 35 0.341 1.012
scrit 0:75 uL rL 0:1 u2L a u r
1:45 L L 25 0.336 1.440
s ahL g sa
Pall rings (ceramic) 50 0.333 1.278
ð34Þ
Intalox (ceramic) 0.488 1.677
Some values of the critical surface tension scrit Ralupak (metal) YC-250 0.385 1.334
are listed in Table 5. The corresponding equa-
Impuls packing (metal) 250 0.270 0.983
tions for the mass transfer coefficients are: (ceramic) 100 0.327 1.317
1=3
rG uG 0:7 hG Montz packing (metal) B1-200 0.390 0.971
bG ¼ C ðadN Þ2 ðaDG Þ ð35Þ (metal) B2-300 0.422 1.165
ahG rG DG
ghL 1=3 rL uL 2=3 rL DL 1=2
bL ¼ 0:0051 ðadN Þ2=5
rL aeff hL hL
uL DL 1=2
ð36Þ bL ¼ CL 121=6 ð40Þ
hL dh
The factor C is 2 for small ðdN < 15 mmÞ and
5.24 for larger packing elements. Values of the factors CV and CL are listed in
BRAVO and FAIR [20] published a model that Table 6.
combines the correlations of Onda for the mass
transfer coefficients with a new correlation for Problems of Mass Transfer Prediction. At
the effective interfacial area: the present state of the art all models for predic-
tion of mass transfer in packed columns are
aeff h uL uG rG 0:392
¼ 19:76s0:5 H 0:4 L ð37Þ insufficient to some degree. One problem is a
a s ahG
poor knowledge of the interfacial area effective
for mass transfer. Published studies differ signif-
In this correlation, the term H 0:4 accounts for the icantly and their results are often contradicting.
influence of maldistribution on mass transfer. Furthermore, the existing models for predicting
Equation (37) is valid for the units m and kg/s2 mass transfer coefficients are not sufficiently
for the height H and the surface tension s, reliable.
respectively. The main reason for the deficiencies of the
BILLET and SCHULTES [21] developed the present knowledge is, however, the maldistri-
following correlations for all three unknowns: bution of gas and liquid in packed beds. Many
0:75 2 0:45 studies reveal that there exist large deviations
aeff r uL dh 0:2 rL u2L dh uL
¼ 1:5ðadh Þ0:5 L from plug flow of gas and in particular of liquid
a hL s gdh
within the bed. The degree of maldistribution as
ð38Þ
well as its effect on mass transfer is unknown
1=2 1=3 and hence not accounted for in existing mass
a r uG 3=4 hG
bG ¼ CV ðehL Þ1=2 DG G transfer models. Thus, the published data for
dh ahG rG DG
interfacial area and mass transfer coefficients
ð39Þ
comprise the maldistibution in an undefined
474 Distillation, 2. Equipment Vol. 11
Figure 23. Maldistribution in a packed column indicated by liquid isotherms. Column diameter 0.63 m, packing height 6.8 m.
A) Uniform liquid feed; B) Single-point liquid feed
Bottom row: Orientation of vertical cross sections.
manner. The data are not true values but pseudo- causes a decrease of liquid temperature which
values which are not predictable within the plug can be easily measured. The lines drawn within
flow model. the packed bed are liquid isotherms that should
Figure 23 presents some experimental results be horizontal and straight in case of plug flow.
of a packed column operated with hot water and Any deviations from straight lines are caused by a
air (like a cooling tower) [6]. In this system the non-uniform gas and, in particular, liquid flow
mass transfer of water from liquid into gas phase through the packed bed.
Vol. 11 Distillation, 2. Equipment 475