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Catalytic Dehydration of Methanol to Dimethyl Ether. Kinetic Investigation

and Reactor Simulation

Article  in  Industrial & Engineering Chemistry Research · November 1993

DOI: 10.1021/ie00023a006

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2478 Ind. Eng. Chem. Res. 1993,32, 2478-2484

Catalytic Dehydration of Methanol to Dimethyl Ether. Kinetic

Investigation and Reactor Simulation

Gorazd Ber6iEt and Janez Levee'**

Laboratory of Catalysis and Chemical Reaction Engineering, National Institute of Chemistry, and
Department of Chemical Engineering, University of Ljubljana, P.O.Box 537, 61001 Ljubljana, Slovenia

One-dimensional heterogeneous and pseudohomogeneous plug flow models were employed to model
an adiabatic fixed bed reactor for the catalytic dehydration of methanol to dimethyl ether.
Longitudinal temperature and methanol conversion profiles predicted by these models were compared
to those experimentally measured in a pilot reactor. The reactor was packed with 3-mm yAlzOs
pellets and operated in a temperature range of 29O-36OoCand a t a pressure of 2.1 bar. Intraparticle
mass transport was found to be the rate-controlling step.

Introduction some properties of the reactor and catalyst are listed in

Catalyticdehydrationof methanol over an acidic catalyst
offers a potential method for production of dimethyl ether
(DME),a new spray propellant. From the patent literature
(Woodhouse,1935; Brake, 1986),it can be concluded that
reaction takes place on pure y-alumina and on y-alumina
slightly modified with phosphates or titanates, in a
temperature range of 250-40O0C and pressures up to 10
bar. The kinetics of methanol dehydration on an acidic
catalyst has been studied extensively,resulting in different
kinetic equations. Most of the rate equations have been
derived from the experiments conducted in conditionsnot
found in an industrial reactor. The experimenta were
mainly performed with mixtures of methanol, water, and
nitrogen at low water vapor pressures. Since water
produced during the dehydration considerably retards the
reaction rate, the derived rate equations are not suitable
for the commercial reactor design,where the reaction takes
place at highconversions. BerEiE and Levec (1992) recently
reported an intrinsic rate equation in the form
which represents the kinetic behavior of the dehydration
reaction over 7-alumina more realistically than equations
published earlier. Equation 1thus offers a powerful tool
that can be used to simulate the dehydration reactor
performance. In the open literature, no information on
the reactor simulation is given in spite of the fact that the
methanol dehydration reaction is considered one of the
basic reactions in the so-called C-1chemistry (e. g., MTG
Process; Chang et al.,1983).
The aim of this work is to present the experimental and
simulated results of an adiabatic fixed bed dehydration
reactor operated at conditions typically employed in a
large-scale reactor. The global rates as well as the
temperature and concentration profiles predicted by
different models are compared with the experimental
results obtained in a pilot reactor having the production
capacity of about 150 kg of DMElday.
Experimental Section
The pilot-scale reactor system employed in this study
is illustrated in Figure 1. Operating conditions as well as
* Author to whom correspondence should be addressed.
+ Laboratory of Catalysisand Chemical ReactionEngineering.
* Department of Chemical Engineering.
Q888-5885/93/2632-2478$~4.00/0 1993 American Chemical Society
Table I. The reactor consisted of four stainless steel
segments connected by flanges. The radial temperature
gradient in the isolation shell was measured by thermo-
couples located at different radial positions in the shell
and connected to the microprocessor-based thermoreg-
ulator. By means of two independently powered heating
tapes in each element, one placed on the outside surface
of the reactor wall and the other placedwithin the isolation
shell, it was possible to maintain almost zero temperature
gradient in the shell, and therefore adiabatic conditione
existed within the catalyst bed. The radial and axial
temperatures in the catalyst bed were measured using a
HP 3421A data acquisitionlcontrolunit and a HP 150PC.
Thermocouples were located in the bed axis at different
axial positions, namely, at z = 0, 5, 10, 15, 25,36,45,55,
and 65 cm, respectively. At the axial positions of 10,25,
and 45 cm, thermocouples were also placed radial at F =
0, i = 0.5R, and i = 0.95R. Sampling tubes were located
within the catalyst bed at 7; = 0. Gas samples, taken at
different axial positions (z = 10,25, and 45 cm) and from
the reactor outlet, were led through a four-way Valco SD
flow path valve to a GC sampling valve.
Analysis of the gas samples was performed by means of
a HP 5890 GC equipped with a TCD. The SS column
(230cm X 118)waspackedwithPorapakT (100/120mesh),
while helium was used as the carrier gas. The oven
temperature was kept at llO°C for the first 17 min and
then continuously increased to 130 OC (at a rate of 4OoC/
min). A gas sample (0.25 mL) was injected by means of
the sampling valve kept at 110OC. A calibration curve
prepared for each component (methanol,water, and DME)
was used to determine the compositionof each gas sample.
Duration of the analysis was about 25 min.
Experiments with 3-mm particles were also carried out
in a differential fixed bed reactor in a temperature range
of 290-360 OC and the constant pressure of 146 kPa. The
reactor was operated free of the external mass- and heat-
transfer resistances. The inlet concentrationsof reactants
were varied between 15 and 90 mol 7% for methanol and
between 0 and 50 mol % for water. Even though DME
was not present in the feed,we simulatedan integral reactor
that is made up of series of differential reactors. The
objective was to determine the rate in these differential
reactors (BerEiE and Levec, 1992).
Reactor Model
A compromise between an excessive complexity (e.g., a
two-dimensional heterogeneous model) and oversimpli-
 Ind. Eng. Chem. Res., Vol. 32, No. 11,1993 2479

Figure 1. Schematic drawing of the experimental apparatus for catalytic dehydration of methanol: (1)gas cylinder (nitrogen), (2)methanol
reservoir, (3)mass flow controller, (4)metering pump, (5)evaporator, (6)ball valve, (7) preheater, (8) manometer, (9) needle valves, (10)tube
and shell heat exchanger, (11) phase separator, (12)coolers, (13)thermocouples, (14)calcium silicate insulation block, (15)glass wool, (16)
catalyst bed, (17)inert bed, (18)sampling valve.
Table I. Properties of Catalyst and Reactor and Operating Table 11. One-Dimensional Plug Flow Models of the Fixed
Conditions Bed Reactor Used in This Studv
catalyst Bayer SAS y-AhOs interfacial intraparticle model
diameter of catalyst particles (mm) 3 t w e of model eradients zradients desimation
catalyst bed height (mm) lo0 heterogeneous yes yes I
catalyst particle density (kp/m3) 1.47 heterogeneous no Yes I1
catalyst bed porosity (/) 0.40 heterogeneous yes nd I11
reactor diameter (mm) 78 pseudohomogeneous no nd IV
reactor height (mm) loo0
preheater packing height (mm) 250 a Intraparticle gradients are accounted for in the apparent rate
inlet temp (K) 551.15-56.15 coefficients (eq 12).
pressure (bar) 2.1
methanol feed rate (L/h) 4.34-6.74
V'JJM(T,C;) dV
'10 = (4)
fication (e.g., a one-dimensional pseudohomogeneous rM(P,CP)
model) is usually made when one wishes to reduce the where the reaction rateat the catalystactivesite, rM(T,Ci),
computational time without an appreciable loss of the is given by eq 1. Equations 2 and 3 are subject to the
accuracy of model prediction. An adiabatic reactor can initial conditions that specify the feed composition and
be well described by one-dimensional models. In this temperature:
study, we adopted heterogeneous models that account for
the intraparticle and/or interfacial gradients as well as a c,"=ck0 atr =O
pseudohomogeneous model. The models used are sum-
marized in Table 11. P=T$ atz=o (5)
In the heterogeneous model, the mass and heat balances
in the fluid phase with isobaric plug flow are governed by The objective is to solve eqs 2 and 3 for the temperature
the following equations: and concentration profiles in the gas phase along the
reactor longitudinal coordinate.
As indicated in eq 4, the overall effectiveness factor can
be obtained by integrating the rate of reaction over the
volume of the whole particle. The concentration and
temperature profiles within the catalyst particle are
obtained by the simultaneous solution of the governing
equations which result by writing a mass and heat balance
within the particle

where the overall effectivenessfactor, 70, accounts for the

intraparticle as well as interparticle mass- and heat-
transport limitations (model I). The overall effectiveness
factor is defined as a ratio of the actual (global)rate to the
rate based on bulk conditions, thus
2480 Ind. Eng. Chem. Res., Vol. 32, No. 11,1993
0.20.

0.16

0.12

0.08

0.04

0.00
0.00 0.02 0.04 0.05 0.0s 0.00 0.04 0.08 0.12 0.f6 C !O

t O'JO T=613 K
+loa a I
0.40

4? 0.20 0.30

0.20

0.10

0.00 k- - 0.00
0.00 0.10 0.20 0.30 0.oo o.<o 0.20 0.30 0.40 0.50
Measured rate Measured rate
Figure 2. Comparison between experimentally measured global reaction rates for 3-mm catslyst pellets and those calculated by eqs 1 and
12. Area marked corresponds to the pilot reactor operating conditions.
and the following boundary conditions Kutta method while the surface conditions (C'and P )in
the heterogeneous model were determined by a Newton
iteration method. In these calculations, p. cp and AHr
were considered as a function of temperature. Nonlinear
equations (eqs 6 and 7), coupled through the concentration
dCi and temperature within the catalyst particle, had to be
ki(Cp - q)= -D.~;T; at r = d42 (9)
solved in each node of the computational grid used in the
integration of the mass and heat balances. Due to the
h ( T - f i =-A d- T
at r = d42 (10) complex rate equation, the solution is not so straightfor-
e dr ward. However, one canuseeither Bischoff 8 approximate
When the reaction rate is small compared to the external solutionwithageneralizedThiele modulus (Bischoff,1965)
heat- and mass-transfer rates, the surface concentration or a numerical solution. In this study, the numerical
and temperature both approach those in the bulk gas appr0acbwasused;the boundaryvalueproblem (eqs6-10)
phase, hence was first converted into an initial value problem by adding
an appropriate transient term to eqs 6 and I and then
q = C p and T= integrated according to the initial conditions to the steady
and consequently state (Riggs, 1988; Hindmarsh, 1986).
?I?,= 1 To avoid a time-consuming numerical calculation of the
effectivenessfactors, one can employ eq 1with the intrinsic
This leads to the one-dimensional heterogeneous model rate coefficients replaced by apparent coefficients that
where only the intraparticle resistances have to be account for the intraparticle mass- and heat-transport
considered (model 11). Equations 2 and 3 with initial limitations. For that purpose, the rate per catalyst particle
conditions (eq 5) still apply, but the overall effectiveness can be calculated from the relation
factor, qo. has to be replaced by the particle effectiveness
factor, 7, defined as

where the apparent coefficients(n.,i<~,&) are evaluated

Results and Discussion
Integration of the reactor mass and heat balances (eqs
2 and 3) was performed by using a fourth-order Runge-
from the experiments performed with particles employed
in the pilot reactor. However, eq 12 also represents an
approximate solution of the integral in eqs 4 and 11,
respectively, for the concentration range investigated.
Employing eq 12 in the heterogeneous models, they can
 Ind. Eng. Chem. Res., Vol. 32, No. 11, 1993 2481
Table 111. Intrinsic and Apparent Coefficient Valuations
for 3-mm ?Ala08 Catalyst Pellets
parameter intrinsic (ea 1) amarent (ea l2)O
k, 5.35 X 1013exp(-17280/T) 6.60 X 108exp(-10800/T)
KM 5.39 X lo-’exp(8487/T) 0.72 X exp(830/T)
Kw 8.47 X le2exp(5070/T) 0.45 X 1(F2exp(ll3O/T)
Component concentrations are expressed by mole fraction.
Constanta I?, are dimensionless in this case.
1.00 , I
- 670

\0.80 - 650
Y
I
0 - 630
+
0.60 3 0.00 0.10 0.20 0.30
+
Y- - 610 E 700’
lA a,
VI
a, 0.40 - 590 Q
E
S
.->
+ - 570 I-
0)
.6 6 0 -
0 PI
a, 0.20
Y-
L 640-
+ S
- 550 +
w 0 620 -
L

0.00 I
0.00
1

0.10
I

0.20
I

0.30
‘530
0.40
PI
n600-

Reactor length, m p&OXl Exp. points To=551.15 K

Figure 3. Particle and overall effectivenessfactors and temperature
as a function of the longitudinal reactor coordinate.
be further simplified: model I accounts then for the
interfacial gradients only and is termed as model 111,while
model I1 is transformed to a pseudohomogeneous model
(model IV). In this work, the apparent coefficients were
calculated by means of a nonlinear regression technique
from the results obtained in the differential reactor
employing 3-mm particles. These experiments were
carried out in the absence of external mass- and heat-
transfer limitations. The intrinsic and apparent coeffi-
cients are listed in Table 111. A parity plot (Figure 2)
shows the differences between the global rates calculated
numerically (based on eq 1) and by means of eq 12 to
those measured experimentally in the differential reactor.
The differences between predicted and measured rates
increase when the temperature increases, most likely due
to the simplification made in the rate calculation. Nev-
ertheless, at the operating conditions of the pilot reactor
(shaded area) the agreement is certainly within a 10%
error in both cases. Therefore, the rate equation with the
apparent coefficients (eq 12) may also be successfully
employed in simulation studies.
In Figure 3, the overall and particle effectiveness factors
as well as temperature are shown as a function of the reactor
length. For operating conditions used in this work, the
heat-transfer coefficient, h, between the bulk gas phase
and the catalyst surface was calculated by means of
Martin’s correlation (Martin, 1978). Values of the coef-
ficient lay between 0.1 and 0.14 W/m2.K. The mass-
transfer coefficient, ki,was calculated by using the concept
of heat- and mass-transfer analogy, and it ranges between
0.04 and 0.06 m/s. From this plot, it may be concluded
that the external mass- and heat-transfer resistances are
negligible in comparison to those within the particles. A
ratio of the overall effectiveness factor to the particle
effectiveness factor exceeds a value of 1 because the
reaction is exothermic. The differences between the
surface and bulk concentrations and temperatures, re-
spectively, vanish at the bed depth where the reaction
AAAAA Exp. points (T.=561.15 K]
- Model I
- - Model II
Model 111
__
.- - - - Model IV
540‘ I I I I I
0.00 0.10 0.20 0.30 0.40 0.50
Reactor length, m
Figure 4. Comparison between experimentally measured temper-
ature profiles and those predicted by the models at two different
methanol feed rates.
equilibrium is attained. At that length, the effectiveness
factors become equal.
Figure 4 shows the experimentally measured and
predicted temperature profiles along the reactor length at
different inlet temperatures and feed flow rates. In Figure
5, the measured conversion profiles in the pilot reactor
are compared to those predicted by both models. When
eq12 was employed in the heterogeneous model, the
external mass- and heat-transfer limitations were ac-
counted for only (overall effectiveness factor was equal to
a ratio of the rate evaluated at the surface conditions to
the rate evaluated at the bulk gas phase conditions), while
in the homogeneous model it was simply set: 70 = 7 = 1.
It is seen from Figures 4 and 5 that the predictions made
with the models neglecting interfacial gradients (models
I1 and IV) agree better with the experimental values than
the predictions obtained by the models accounting for the
interfacial gradients (models I and 111). On the other hand,
both models employing eq 12 (models I11 and IV) predict
almost the same profiles as those models using the
numerically calculated reaction rates (models I and 11).In
any heterogeneous model, a temperature (and concen-
tration) difference between the gas phase and the particle
surface is always established, no matter how large the heat-
transfer coefficient is. Since the dehydration reaction is
exothermic, the particle surface temperature is higher than
the temperature of the gas phase (Figure 3). The rate
calculated by the heterogeneous models accounting for
the interfacial gradients is therefore higher when the same
inlet temperature of the gas phase is imposed to the models.
Consequently, the temperature profiles predicted with
2482 Ind. Eng. Chem. Res., Vol. 32, No. 11, 1993
1.00 I
1
"1"

To = 5 5 1 . 1 5 K

\ Oa80 t
P = 2.1 b a r
/ ,r7- J g/
0

!
E 0.60
I

.-
P
$ 0.40
S
0 03333 Experimental points
Qu=4.34 I/h - Model 111
0
0.20
0u=6.74 I/h _ - h' = 1.2 h
. _ _ h'__
_ _ h' == 0.8
5.0 * h
h
..-.
.... h' = 0 . 2 * h
0.00 0.40 I-"

0.oo 0.1 0 0.20 0.30 0.00 0.10 0.20 0.30 0.40 0.50

c
1.00 I 1 680 I I
To = 5 6 1 . 1 5 K Qu=6.74 I/h
P = 2.1 b a r 660 P = 2.1 bar

t
To=551.15 K
Y
\Oaso ,640 -
2)
.-$0.60 t
3 620 -
v)
L E -
>
a 0.40 Q)
a
600
S -
0 Ooxo Experimental points
Exp. points - Model 111
0 Exp. points - - k' = 1.2 k
0.20 Model I . _ _ k' __ = 0.8 k
Model II 560 __ k' = 5.0 k
Model 111 ........ k ' = 0.2 k
Model IV
0.00 5401 I I I I
0.00 0.10 0.20 0.30 0.40 0.00 0.10 0.20 0.30 0.40 0.50
Reactor length, m Reactor length, m
Figure 5. Comparison between experimentallymeasured conversion Figure 7. Effect of the heat- and mass-transfer Coefficients on
profiles and those predicted by the models at two different inlet temperature profile predicted by the heterogeneous model 111.
temperatures.
illustrated in Figure 7, where the temperature profiles are
plotted for different values of the mass and heat transport
0 coefficients, respectively. These two physically relevant
parameters were varied one at a time to assess their effect
on the model features. Results in Figure 7 show that
increasing the transport coefficients even by a factor of 5
does not significantly change the loci of the temperature
profiles. When the heat transport coefficient is decreased
by a factor of 5, the locus is moved far above the
experimental points. As a direct consequence of a lower
heat-transfer rate, both the catalyst surface temperature
-
,- f

/
' EExperimental
- - T-' .
Model Ill
. " = T." + 2 K
points
and the reaction rate increase. Due to the increase of the
reaction rate, the temperature profile becomes steeper.
rcn-
To' = To - 2 K
The same decrease of the mass transport coefficient results
in a shift of the temperature profile in the opposite
540' I I I I I direction. It should be noted that both transport coef-
0.00 0.10 0.20 0.30 0.40 0.50
ficients (k, h) change proportionally to the Reynolds
Reactor length, m number; in our case of exothermic reaction, their influence
Figure 6. Effect of ,the inlet temperature on temperature profile on the predicted temperature profile is almost counter-
predicted by the heterogeneous model 111. balanced.
The catalyst particles can be considered isothermal
these models are found above those predicted by the (BerEiE, 1990);thus, only the intraparticle mass transport
models with neglected interfacial gradients. Figure 6 shows may retard the reaction. Figure 8 shows the temperature
the temperature profiles for different inlet temperature profiles predicted by the heterogeneous model 11, where
of the gas phase. As can be seen, only a slight difference a value of the effective diffusion coefficient was changed
in the inlet temperature causes quite a bit of change in the for f20%. The effective diffusion coefficient was esti-
profile location. However, by decreasing the inlet tem- mated from the relation
perature by only 2 K, certainly within the error of
temperature measurement, one can match the predicted De,i= 9.636 X 1 0 4 m (cm2/s) (13)
and experimental profiles quite well. This further alludes
that the dehydration rate is not controlled by the external which is based on the parallel pore model for Knudsen-
transport processes. Confirmation of this hypothesis is type diffusion (BerEiE, 1990). Influence of the particle size
 Ind. Eng. Chem. Res., Vol. 32, No. 11, 1993 2483
--- I Conclusions
The intrinsic rate of dehydration reaction is realistically
expressed by eq 1. Using this equation and an appropriate
numerical procedure, one can reasonably well predict the
global reaction rates that account for the intraparticle heat-
and mass-transfer limitations. The axial temperature and
conversion profiles in an adiabatic fixed bed reactor for
the DME production are well predicted by models
neglecting interfacial gradients where the source term is
either in the form of eq 1with the intrinsic rate parameters
(model 11)or in the form of eq 12 with the apparent rate
Experimental parameters (model IV). The apparent rate parameters
Model II can be easily determined by experiments in a differential
,,I = 0.8 reactor employing particles of the same size that are going
5401 1 I I I
to be used in a commercial reactor.
0.00 0.10 0.20 0.30 0.40 0.50
Reactor length, m Acknowledgment
We acknowledge support from the Ministry of Science
Figure 8. Effect of the effective diffusivity on temperature profile and Technology of Slovenia under Grant No. C2-0541-
predicted by the heterogeneous model 11. 104 and from Nafta-Lendava for making it possible to run
680 I I
a pilot reactor at their facilities for more than 2 months.
We also thank Bayer, A. G., Germany, for the catalyst
supply.
Nomenclature
Ci = concentration in fluid phase, kmol/m3
cp = specific heat of fluid, kJ/(kg-K)
D,i = effective diffusion coefficient, m2/s
d, = particle diameter, m
AHr = heat of reaction, kJ/kmol
h = heat-transfer coefficient, W/(m2.K)
K = thermodynamic equilibrium constant
Fi = adsorption constant, m3/kmol
. _ _P'_ _3.8 = P Ki = apparent adsorption constant
_ _ d,' = 2.0 * d,
- -...- -. d,' = 0.5 d, ki = mass-transfer coefficient, m/s
540
0.00
' 0.10
I
0.20
I
0.30
I
0.40
I I
0.50
k, = reaction rate constant, kmol/(kg-h)
k, = apparent reaction rate constant, kmol/(kg.h)
Reactor length, m Mi = molecular weight, kg/kmol
P = pressure, bar
Figure 9. Effect of the particle size and operating pressure on R = reactor radius, m
temperature profile predicted by the heterogeneous model 11. r = particle radial coordinate, m
0.10
F = reactor radial coordinate, m
rM = rate of methanol disappearance, kmol/(kg.h)
T = temperature, K
0.08 0 u = superficial velocity, m/s
\
0 ' 8 V = particle volume, m3
0 0 z = reactor longitudinal coordinate, m
\
- 0.06
0 8
0
Xi = mole fraction
Greek Letters
E 0.04 Mixture composition
MeOH:DME:H,O:N2 4~ = methanol feed rate, L/h
n 0003035 : 9 : 9 : 47 7 = effectiveness factor
E 00000 41 : 13: 13: 33
0.02 k X ? 0 Q 5 0 : 9 : 9 : 32 70 = global effectiveness factor
I A, = particle effective thermal conductivity, kJ/(ms.K)
W
0.00 ui = stoichiometric coefficient
0 1 2 3 4 5 6 7 8 9 10 p = gas-phase density, kg/m3
Pressure, b a r p~ = catalyst bed density, kg/m3
pp = catalyst particle density, kg/m3
Figure 10. Effect of the operating pressure on global reaction rate
for 3 mm y-Al2O3 catalyst pellets. Subscripts and Superscripts
b = bulk conditions
and the operating pressure on the longitudinal temperature E = dimethyl ether
profile is depicted in Figure 9. It is obvious that the effect e = effective
of particle diameter is appreciable. It is somewhat i = ith component (methanol, DME, water)
surprising that the total pressure has almost no effect on M = methanol
0 = inlet conditions
the predicted temperature profile. One can speculate that s = surface conditions
the reduction of the intrinsic reaction rate due to the W = water
pressure rise is compensated by the increase of the
effectiveness factor. The net result is, however, almost Literature Cited
the same global reaction rate. This conclusionis confirmed BerEiE, G. Dehydration of Methanolover y-Al203. Kinetica of Reaction
with the experimental results obtained in a CSTR system and Mathematical Model of an Industrial Reactor. Ph.D. Thesis,
using the same catalyst pellets (Figure 10). The University of Ljubljana, 1990.
 2484 Ind. Eng. Chem.Res., Vol. 32, No. 11, 1993
BerEiE, G.; Levec, J. Intrinsic and Global Reaction Rata of Methanol
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Brake, L. D. U.S. Patent 4,695,786,1986.
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York, 1983;p 76.
Hindmarsh, A. C. Solving Ordinary Differential Equations on an
IBM-PC Using LSODE. LLNL Tentacle Magazine; LLNL:
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Transfer in Packed Beds. Chem Eng. Sci. 1978,33,913-919.
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Woodhouse, J. C. U.S.Patent 2,014,408,1935.
Received for review March 1, 1993
Revised manuscript received July 1, 1993
Accepted July 27, 19930
@ Abstract published in Advance ACS Abstracts, October 1,
1993.