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Art. 1 Empaque Estructurado
Art. 1 Empaque Estructurado
Department of Chemical Engineering, The University of Texas at Austin, Austin, Texas 78712
An Improved correlation of mass transfer rates for commercial-scale packed distillation columns has been de-
veloped. The correlation is based on effective area for mass transfer
a 0.498a (CaufieG)0392
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where ae is effective area for transfer, a p is specific surface of the packing material, Z is height of packed bed
(ft), is surface tension (dyn/cm), and CaL and fieG are dimensionless liquid capillary number and gas Reynolds
number, respectively. Packings represented are of the randomly arranged ring and saddle types. Basic data are
from a bank of 231 evaluated runs covering eleven distillation systems. The correlation Is shown to be more reliable
and more general than previously published models, with 96% of the calculated data falling within ±20% of the
observed values. For 95% confidence in design, a 1.6 safety factor is required.
Packed columns have been used extensively for distil- from simple, naturally occurring materials, such as chunks
lation applications, especially those in which pressure drop of coke, to carefully fabricated geometric shapes such as
Ind. Eng. Chem. Proc. Des. Dev. 1982.21:162-170.
is critical. The columns have usually been filled with metallic or ceramic saddles, and from tiny devices for
randomly arranged packing elements of the ring or saddle laboratory use to large commercial packing elements with
type, and it is on these “random packings" that most ex- nominal sizes of 3 in. and larger.
perimental investigations of mass transfer rates have been An extensive review of earlier data pertinent to com-
made. While there is increasing interest in the so-called mercial operations was presented by Cornell et al.
“regular packings” (mesh, grids, etc.), their applications (1960a,b). These data are mainly from studies that used
tend to be limited by high cost and incomplete perform- either Berl saddles or Raschig rings. Also, the data were
ance documentation. These latter packings are normally obtained largely from tests with unidirectional mass
handled on a proprietary basis through the experience of transfer, gas-to-liquid or liquid-to-gas. A more recent paper
their vendors. by Charpentier (1976) presents a good general overview
In 1979 Bolles and Fair described a large data base that of additional data and of some of the approaches that
they assembled from published tests of flooding, pressure investigators have used in dealing with the prediction and
drop, and mass transfer in columns containing random description of mass transfer in packed columns.
packings. They utilized the base to evaluate existing As noted earlier, the 1979 paper by Bolles and Fair
packed column models. They did not attempt to improve included an extensive data bank for a wide range of
the existing models for flooding or pressure drop, but did packings, column sizes, and systems. Many of the data
develop a mass transfer model that was superior to those in this bank are for distillation conditions and include
previously published. Their model generalized on fluid results of work done by Fractionation Research, Incorpo-
properties and flow rates, but required two inputs: prior rated (FRI). This data bank provided all of the model
validation for a specific packing type and size, and a validation material for the present work. As is appropriate
consistent (if not completely reliable) method for pre- for differential contacting, the Bolles and Fair model
dicting the flooding condition for the system and packing utilizes the transfer unit approach, equivalent to the mass
under scrutiny. transfer coefficient approach
The present work represents an attempt to develop a
general design model for distillation applications, a model 0 =
(1)
that would not require previous validation for the packing K0GaJ>MG
type or size and which hopefully could be extended to the where the effective interfacial area oe may differ from the
regular packings. Furthermore, the Bolles-Fair require- actual interfacial area.
ment of flooding knowledge was thought to be an encum- The volumetric mass transfer coefficient KGGae in eq 1
brance as well as a limitation on reliability, and it was
may be divided into coefficient and area components for
hoped that such requirement would not be needed with fundamental analysis, and this approach has been used by
a new model. The model, if successful, could then be
a number of workers (Shulman et al., 1955a-c; Yoshida and
applied to a variety of packing sizes and shapes while still Koyanagi, 1954; Onda et al., 1968,1972; Hughmark, 1980).
being general with respect to properties and flow condi- Most of the work was confined to Raschig ring and Berl
tions; in view of the continuing development of packing saddle packings.
types, such a model should be well received by process The work by Shulman can be considered as the basis
engineers and packing vendors alike. for the present effort, as it has been for most other mass
Previous Work transfer efficiency studies that describe the transfer
A vast amount of literature dealing with mass transfer coefficient and the effective area.
in randomly packed columns is available. Studies have The work by Onda and co-workers is based on the
covered a wide variety of packing types and sizes ranging concept of wetted packing area, as opposed to interfacial
area. The work draws on the earlier efforts by Yoshida Both correlations for the individual mass transfer
and co-workers and uses the wetted area as a geometric coefficients show the same type of dependence on key
parameter in determining the Reynolds number for the variables such as diffusivity and velocity.
liquid. The equations describing kL and kG in the Shulman
The Onda and Shulman models, which form a part of model are
the basis for the present model, will be described fully in
the next section.
1.195 (ScG),-2/3
=
kGpGMRT/G (8)
Model Development
The two-film mass transfer model as well as the concept
of the transfer unit provide the basis for this work. Al-
ternate mass transfer models based on the penetration and Mp/Dl-25.1
[¥]" (ScL)10.50 (9)
-
(13)
apPh
The integration of the general flux equation, coupled
with the definition of the number of transfer units, leads aX2
to defining expressions for the heights of individual ^ 2
(14)
transfer units SPl
Hg =
G/(kGaePMG) (3) L2
WeL (15)
Hl = L / (kLaepi) (4) OpCPL
Thus, an effective area can be calculated from available future work leading to improved methods for predicting
mass transfer coefficients kG and kh, themselves based on kL and kG could lead to improvements in the present work.
known values of G, L, MG, ML, P, and pL. Because of the nature of the hydraulics and geometry
Clearly, the selection of a specific mass transfer coef- of packed beds with gas and liquid in counterflow, a cor-
ficient correlation is critical to the present work. The respondence between liquid holdup and effective transfer
correlations by Onda and co-workers (1968,1972) and by area is to be expected; thus, the trends observed in liquid
Shulman and co-workers (1955a-c) were selected for our holdup behavior at varying loading conditions should apply
analysis because they conform to the commonly accepted for effective area. Also, an added gas kinetic energy effect
functionalities should be included for the area analysis because of its
influence on film surface rippling, liquid droplet dispersion,
koPMa/G =
QReGuScGv (6) and the occurrence of gas bubbling in puddles. It can be
and reasoned that the behavior of liquid holdup for different
flow conditions should be similar to that of the interfacial
klC^M^/L —
Q'ReLrScL‘ (7) area, the latter possibly showing a greater influence from
164 Ind. Eng. Chem. Process Des. Dev., Vol. 21, No. 1, 1982
gas velocity and density. Accordingly, a significant gas Table I. Symbols for Figures 1-17
effect was included in the present work since it is generally
A Cyclohexane/n-Heptane 5.0 psia
practical to operate commercial packed columns at high
gas loadings and relatively close to flooding conditions.
In analyzing the various forces acting in such systems, X Cyclohexane/n-Heptane 24.0 psia
it was concluded that an improved correlation should be
able to deal with the following considerations, (a) The + n-Butane/1-Butane 165.0 psia
effective transfer area should be proportional to the liquid
rate since increased liquid velocities would provide a better
o l-Propanol/water 14.7 psia
wetting of the packing, rippling of the film surface, and
a more effective renewal of the liquid in the puddles, (b)
Systems with low surface tensions should provide increased
X Ethylbenzene/Styrene 2.0 psia
wettability as well as smaller droplets yielding in this sense
more interfacial area. On the other hand, a lower surface X Methanol/Ethanol 14.7 psia
tension would make the liquid separate more easily from
the packing at high gas rates, thus reducing the effec- Q Ethanol/water 14.7 psia
tiveness of the packing, (c) Increased kinetic energy of the
gas should tend to increase the effective area, (d) A
CD Ethylbenzene/Styrene 1.0 psia
packing with a high specific surface should yield a rela-
tively high value for the net interfacial area under similar
flow conditions, (e) A correlation for liquid maldistribution X n-Heptane/Toluene 14.7 psia
due to column height and diameter should be expected.
With these considerations in mind, and after different Y 14.7 psia
schemes were tried unsuccessfully, the following func- NH3/H20/air
tionality was proposed X 14.7 psia
02/H20/air
ß/ =
f{L,G,ZJ)c,a) (16)
* Benzene/Dichloroethane 14.7 psia
The values for aep (the effective mass transfer area for the
packing alone) were obtained by correcting the total ef-
fective area (oe) for column wall effects if i-Octane/Toluene 20.0 psia
aep
=
o8
-
1/2 '
'CERAMIC fi. fi. 1.5' 'CERAMIC R. R.
Q- -
cr :
*
c
ü
-«
" r
r,rm,| 111111-rr'r m»|-
10° 101 102 IQ3 104
.
'CERAMIC R.R.
'
3
xz,x
X /
- /
:
V
/
X
/
/
/
/
z>
z ^Master correlation
_
riii
mi|-1—I II I
III]- -r I > r rrrn
-ioD 101 102 103 1q4 1 q5
CAL*REG*1E 03
Figure 6. Area ratio for 3-in. ceramic Raschig rings.
166 Ind. Eng. Chem. Process Des. Dev., Vol. 21, No. 1, 1982
METAL ñ.B.
’ 1
1
-
:
Master correlation /
X/
%/
X"·
X, ,X'
tt-
10° 101 io2 io3 104
CAL*ñEG*1E 03
Figure 7. Area ratio for 1-in. metal Raschig rings. Figure 10. Area ratio for 6/g-in. metal Pall rings.
1. 5
'
'METAL ñ. R. 1
'
'METAL P.R.
/
Master correlation Master correlation /
/
/
X*0
o
X/Z oj8®
X/"
x,x
ib°
M
"'io1
TTTTj-1—r
L2
lb2
i r
rrq-1—
ir>3
io:
rm|-1—r-
lb4 IO5 10u "iV 102 IQ3 ""io4 "To3
CAL*REG*1E 03 CAL*REG*1E 03
Figure 8. Area ratio for 1.5-in. metal Raschig rings. Figure 11. Area ratio for 1-in. metal Pall rings.
1.5' 'METAL P. R.
2' ' E T AL R.R.
/
/
*
c
X / */
*/
X / /
X7 X
Master correlation
/
Jq x
-
........
r"l ........I TTTT ""
10*, io2
-
o
MASTER CORRELATION FOR DISTILLATION
a
These are absorption systems; all others are distillations.
168 Ind. Eng. Chem. Process Des. Dev., Vol. 21, No. 1, 1982
Table IV. Model Reliability Analysis and Comparison the present time, such an extension is not recommended.
Bolles and Fair this work Conclusions and Recommendations
0.042 -3.42 X 10'14 The independent treatment of the individual mass
OFm
S 0.323 0.286 transfer coefficients and the effective interfacial area for
Fs (95% confidence) 1.70 1.60 mass transfer appears to provide a logical and fundamental
approach to the description of mass transfer in counterflow
1.042. (d) For the 231 points, 96% of the calculated values gas-liquid packed column. Transfer rates within a single
of o* were within ±20% of the observed values, 71% phase should depend on the available concentration gra-
within ±10%, and 40% within ±5%. dient, the degree of turbulence in that phase, and on the
Bolles and Fair (1979) used and recommended a relia- physical properties of the fluid. The bulk-to-interface
bility analysis procedure based on a logaritmic ratio ob- transfer rates (or the individual mass transfer coefficients)
jective function, which in the case of this work is should be much more heavily dependent on the system
itself than on the geometric characteristics of the packing.
OF¡ = In ((o*/op)obsd/(a*/ap)calcd) (24) On the other hand, the effective interfacial area for mass
transfer at any given point in the bed should depend only
The lower bound of this objective function was selected
on the relative kinetic energy of the phases, the geometry
to be the critical one since the conservative approach is
of the packing, the wettability of the packing surface, and
to assume that the actual design value for the effective area
the tendency toward rippling and/or droplet formation in
will be smaller than the one obtained from the model. (For
the liquid. The extrapolation of this “point” area to a
an Hqq objective function like the one proposed by Bolles
and Fair, the upper bound will be the critical one since the complete column should be some function of the overall
dimensions of the bed.
height of a transfer unit is inversely proportional to the The product of the capillary number for the liquid
effective area.)
(which accounts for the liquid viscous and surface tension
Following the procedure presented by Bolles and Fair,
the following expression for lower bound critical is obtained forces) and the Reynolds number for the gas (which de-
scribes the inertial and viscous forces in the gas) seems to
(o*/op)deeign
=
e0Fme~tS(a* / ap)cM (25) provide an appropriate parameter for describing effective
areas.
where OFm = mean of the objective function = OF¡/n, Through the course of this work it was observed that
= number of
observations, OF¡ = objective function for for similar flow conditions the available area for mass
the ith observation, S = standard deviation of the objective transfer was substantially higher in distillation systems
function = [ (0- ;- OFm)2/(n l)]0·5, and t = Student’s
-
a* =
corrected effective area, (ft2/ft3)(ft0·4/(dyn/cm)0·5) ScG
=
Schmidt number for the gas
ae
=effective interfacial area, ft2/ft3 Sch = Schmidt number for the liquid
oep
= effective area provided by packing alone, ft2/ft3 S = standard deviation
=
specific surface of the packing, ft2/ft3 T = absolute temperature
aw
=
wetted area, ft2/ft3 t = Student’s t
b = exponent in eq 22 u, v exponents in eq 6
—
CaL = capillary number for the liquid WeL = Weber number for the liquid
Dc = column diameter, ft Z =
height of packing in column, ft
Dg = diffusion coefficient for the gas Greek Symbols
Dl = = diffusion coefficient for the liquid
dp diameter of a sphere with the same surface area as one a = factor to correct for available column wall surface
packing element e = void fraction
dp = nominal diameter of the packing element
= X = ratio of slopes (equil. line/operating line =
mGm/Lm)
safety factor for model reliability viscosity
=
Fs µ
FrL = Froude number for the liquid density
=
p
G = gas superficial mass velocity = surface tension, dyn/cm
Gm
=
gas superficial molar mass velocity ac
=
critical surface tension, dyn/cm
g -
acceleration of gravity
Subscripts
gc
=
force/mass conversion factor G = referred to the gas
Hg = height of a gas transfer unit, ft
Hh = height of a liquid transfer unit, ft
L = referred to the liquid
GM = molar property for the gas
Hqq = height of an overall gas transfer unit, ft
HETP = height equivalent to a theoretical plate, ft Literature Cited
kG
=
mass transfer coefficient for the gas phase
Bolles, W. L; Fair, J. R. Inst. Chem. Eng. Symp. Ser. 1979, 56 3/35.
kL = mass transfer coefficient for the liquid phase
,
Robert J. Hurtublse
Chemistry Department, University of Wyoming, Laramie, Wyoming 82071
Hydrogen donor characteristics are one of the most important properties of a coal-derived recycle solvent used
In the direct liquefaction of coal. This property can be modified by direct catalytic hydrogenation to increase the
solvent hydrogen content. Results of this work using 22 solvents derived from three coals Indicate that recycle
solvent effectiveness goes through a maximum as the hydrogen content of the solvent Increases. However, the
solvent hydrogen content at which the observed maximum occurs differs for different solvents. Weight percent
hydrogen in a solvent at observed maximum liquefaction effectiveness has been correlated as a linear function
of a Watson-type characterization factor, /fw.