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∂ CL ( 0, t ) VSL
MATHEMATICAL MODEL = C L ( 0, t ) ; (5)
∂z Dax ∀t
∀t
1 − (1 − HS − H d,G )
+ K2 ρ V2 )
G SG The dimensionless parameters in Eqs. 11 to 16
(1 − HS − Hd,G )
3
are defined as
∂ ΓG ( ξ, t A ) ∂ ΓG ( ξ, t A )
+ SOLUTION OF SYSTEM EQUATIONS
∂ tA ∂ξ
(11) The partial differential equation system defined
+αΓ G ( ξ, t A ) = αΓ L ( ξ, t A )
by Eqs. 11 to 13 may be solved in the Laplace
domain, as reported in previous studies (Silva et al.,
∂ Γ L ( ξ, t A ) ∂ Γ L ( ξ, t A ) 1 ∂ Γ L ( ξ, t A )
2
2000b; Iliuta et al.,1999; Burghardt et al., 1995;
+κ −
∂ tA ∂ξ PE∗ ∂ ξ2 Ramachandran and Smith, 1979).
( )
= γΓG ξ, t A − γΓ L ( ξ, t A ) (12)
dΓ∗G ( ξ,s )
s Γ∗G ( ξ,s ) + + α Γ∗G ( ξ,s ) = α Γ∗L ( ξ, s ) (19)
dξ
−ϑ Γ L ( ξ, t A ) − Γ r (1, t A ) ∀t
∂ Γ r ( η, t A ) d Γ∗L ( ξ,s ) 1 d Γ L ( ξ, s )
2 ∗
∂ 2 ∂ Γ ( η, t A )
λ s Γ∗L ( ξ,s ) + κ −
= 2 η (13) dξ PE∗ dξ 2
∂ tA η ∂η ∂η
The dimensionless initial and boundary = γ Γ∗G ( ξ,s ) − γΓ∗L ( ξ,s ) (20)
conditions for Eqs. 11, 12 and 13 are given by
−ϑ Γ∗L ( ξ,s ) − Γ∗r (1,s )
Γ G ( ξ,0 ) =0; Γ G ( 0, t A ) =1 (14)
∀ξ ∀ tA
∂ 2 ∂ Γ r ( η,s )
∗
λ
s Γ∗r ( η,s ) = 2 η (21)
η ∂ η ∂ η
ΓL ( ξ,0) = 0; ∂ΓL ( 0,t A ) = PE ΓL ( 0,t A ) ;
∀ξ ∀tA
∂ξ ∀tA The boundary conditions in the Laplace domain are
(15)
defined by
∂ΓL (1,t A )
=0
∂ξ ∀tA Γ∗G ( 0,s ) = 1 s (22)
Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
378 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
Γ∗G ( 0,s )
Γ∗G ( ξ,s ) =
D (s)
{V ( λ
∗
1 2 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ1 ( s ) ξ + V2∗ ( λ1 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ 2 ( s ) ξ + V3∗
(38)
( λ1 ( s ) , λ 2 ( s ) ,a1 ( s ) ) exp λ3 ( s ) ξ }
where V1∗, V2∗and V3∗ are functions defined in the Laplace domain and are given in Appendix C.
For ξ = 1 it was possible to obtain the response of the gas tracer at the exit of the fixed bed with Equation 39:
ξ=1
Γ∗G (1,s ) = ∫Γ ( ξ,s ) δ ( ξ − 1) dξ
∗
G (39)
ξ= 0
Thus
Γ∗G ( 0,s )
Γ∗G (1,s ) =
D (s)
{ V1∗ ( λ 2 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ1 ( s ) + V2∗ ( λ1 ( s ) , λ 3 ( s ) ,a1 ( s ) ) exp λ 2 ( s ) + V3∗
(40)
( λ1 ( s ) , λ 2 ( s ) ,a1 ( s ) ) exp λ3 ( s )}
The transfer function of the system was defined by the ratio of the exit function to the entrance function
[G∗(1, s) = Γ∗G (1, s)/ Γ∗G (0, s)], so the final transfer function was
G ∗G (1,s ) =
1 ∗
D (s)
{
V1 ( λ 2 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ1 ( s ) + V2∗ ( λ1 ( s ) , λ 3 ( s ) ,a1 ( s ) ) exp λ 2 ( s ) + V3∗
(41)
( λ1 ( s ) , λ 2 ( s ) ,a1 ( s ) ) exp λ3 ( s ) }
The theoretical concentration at the exit of the where the Laplace variable (s) was substituted by iω
fixed bed, ΓG(1,tA)kCalc, was calculated by the in the Fourier domain.
convolution of the experimental concentrations ΓGExp
(iω) with GG∗(1, iω). ΓG(1,tA)kCalc was obtained by
numerical inversion, using the numerical fast Fourier MATERIALS AND EXPERIMENTAL
transform (FFT) algorithm (Cooley and Twkey, METHODOLOGY
1965) that changed the time domain according to
following equation: To study the axial dispersion and the mass
transfer effects, a three-phase gas-liquid-solid reactor
was mounted according to Fig 1. The assembled
= TF−1 Γ EExp ( i ω) ∗ G∗G (1,i ω)
Calc
G (1, t A ) k
Γ
(42) system consisted of a fixed bed with a height of 0.16
Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
380 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
m and an inner diameter of 0.03 m; catalytic particles - residence time distribution (RTD); determination
were contacted by a cocurrent gas-liquid downward by the method of moments applied to the normalized
flow. Experiments were conducted under conditions curves. A comparison of experimental results with
such that the superficial velocities of the gas and the expressions obtained from the transfer function
liquid phases were maintained within the trickle-bed (GG∗(1,s); Eq.41) as developed for this system;
regime (Ramachandran and Chaudhari, 1983) VSL in - evaluation of the model parameters (Dax, KGL, kLS)
the range of 10-4 m s-1 to 3 10-3 m s-1 and VSG in the used as initialization values when obtained by the
range of 2 10-2 m s-1 to 45 10-2 m s-1. method of moments;
The gas phase (4% volume Ar +CH4), flowing - optimization of the model parameters by comparing
downward cocurrently in contact with 70.00g of the the calculated values of concentration with the
solid bed (γ-Al2O3, CGO-70, Rhone-Poulenc), was experimental data.
continuously measured using a thermal conductivity To calculate the concentrations within this
detector (TCD) coupled to an AD/DA interface. The numerical model, several numerical values for the
tracer was turned on and off at differing superficial CH4–Ar–H2O / γ-Al2O3 system are required; in Table
velocities; deviations in the signal from its baseline, 1 these values, obtained under similar experimental
negative steps, provided a measurement of its conditions, are listed (Silva, 1996).
concentration versus time at the entrance and exit of Performance of the trickle-bed is affected by
the bed. many factors, such as interphase mass transfer,
The methodologies applied to evaluate the axial intraparticle diffusion, axial dispersion, gas and
dispersion and the mass transfer parameters for the liquid holdup and partial wetting. These factors are
CH4 – Ar – H2O / γ-Al2O3 system were the incorporated into this model. As the liquid flow was
following: maintained constant, Silva’s tabulated values
- analysis of the negative - step curves at the entrance representing liquid holdup (Hd,L) and partial wetting
and exit of the bed; (fe) (1996) were adopted.
Numerical Values
-4
µL, kg m s -1 -1
8.91 10 VSG, m s-1 29.46 10-3 R, m 1.60 10-3
µG, kg m-1 s-1 1.23 10-5 VSL, m s-1 1.91 10-4 σL, kg s-2 7.22 10-2
ρL, kg m-3 1.01 103 aGL, m2 m-3 8.13 104 fe 3.50 10-1
-1 2 -3 3
ρG, kg m -3
6.63 10 aP, m m 1.14 10 H 5.70 10-2
δGL, kg m-2 s-2 1.14 101 KA, m3 kg-1 6.45 10-4 De, m2 s-1 4.56 10-3
ρP, kg m-3 3.15 103 L, m 1.60 10-1 εex 3.90 10-1
Hd,G 2.00 10-1 DP, m 3.20 10-3 W, kg 7.00 10-2
-1 -2 -1 -4 -2
Hd,L 5.40 10 GL, kg m s 5.07 10 g, m s 98.10 10-1
HS 2.60 10-1 GG, kg m-2 s-1 1.74 10-5 DR, m 3.210 10-2
RESULTS AND DISCUSSION coefficients for differing gas - phase flow are
reported below in Table 2.
Experiments were conducted at a constant liquid In Figs. 2 and 3 results of the two sets of
flow of QL = 0.50 10-6 m3 s-1 and the gas phase was experiments presented show normalized profiles for
varied in the range of QG = (41.69 to 9.97) 10-6 m3 s- concentration of gas tracer as a function of time.
1
. The mean residence times, (tM)G = (tM)S,G – (tM)E,G, A model validation process was established by
were obtained from the experimental curves; (tM)G comparing the theoretical results obtained with the
was found to be in the range of 0.43 s to 8.47 s. values of the optimized parameters and the
The axial dispersion coefficient and the gas-liquid experimental data for two test cases. These results,
and liquid-solid mass transfer coefficients were presented in Figures 4 and 5, confirm that this
determined simultaneously by comparison between reactor is represented by this model.
the experimental and theoretical data, obtained at the The axial dispersion and the interphase mass
exit of the fixed bed, subject to the minimization of transfer phenomena characterized in the three-phase
objective function (F) where process studied are influenced by changes in gas
flow. It was noted that at fixed liquid flow rates and
2 with fixed liquid retention and partial wetting of the
∑ {[Γ }
N
F= G (1, t A ) ]Exp
k
− [ Γ G (1, t A ) ] Calc
k (43) bed, the highest gas-liquid and liquid-solid mass
k =1 transfer effects were obtained for the highest gas -
phase flow. Consequently, parameters Dax, KGL and
The initial values of Dax, KGL and kLS were kLS can be described by empirical correlations.
Correlations taken from Stiegel and Shah (1977),
determined from the first absolute moment, (µ1)G, of
Fukushima and Kusaka (1977) and Chou et al.
the transfer function. The first absolute moment can
(1979) were applied in modified form by the authors.
be related to the experimental mean residence time
These data were reformulated with dimensionless
(tM)G as follows:
numbers as FrG, WeG and ScG (Table 3) and were
fitted by the nonlinear least-squares method; they are
dG ∗ (1,s )
L H d,G lim restricted to the following ranges of operation: dP =
( µ1 )G = ( t M )G = − S→0 ds (44) 3.20 10-3 m, 21.36 ≤ ReG ≤ 92.56, 10-4 ≤ FrG ≤ 3.23
VSL lim G (1,s )
∗
10-3, 5.30 10-2 ≤ ScG ≤ 2.28 10-1 and 10-5 ≤ WeG ≤
S→0
8.30 10-4.
Development of this expression is given in Appendix Figs. 6, 8 and 10 show plots of Dax, KGL and kLS
D. as a function of ReG, FrG, ScG and WeG. Figs. 7, 9
The numerical procedure for optimization of and 11 contain parity plots of the results obtained
these parameters involved numerical inversion in the through the method applied in this work for each gas
Fourier domain followed by an optimization flow utilized in the three-phase operation vs those
subroutine (Cooley and Twkey, 1965; Box, 1965). results predicted from the correlations expressed by
The initial and optimized values of these three Eqs. 45, 46 and 47.
Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
382 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
Table 2: Initial and optimized values of the dispersion coefficient and mass
transfer parameters. QL = 0.50 10-6 m3 s-1 .
Figure 2: Concentration profiles for the methane gas tracer at the entrance and the
exit of the γ - Al2O3 bed in QG = 33.34 10-6 m3 s-1 and QL = 0.50 10-6 m3 s-1
Figure 3: Concentration profiles for the methane gas tracer at the entrance and
the exit of the γ - Al2O3 bed in QG = 18.32 10-6 m3 s-1 and QL = 0.50 10-6 m3 s-1
Brazilian Journal of Chemical Engineering
Experimental Analysis and Evaluation of the Mass Transfer Process 383
Figure 4: Validation of the tracer concentration at the Figure 5: Validation of the tracer concentration at the
exit of the γ-Al2O3 bed; ♦ results in gas and liquid exit of the γ-Al2O3 bed; ♦ results in gas and liquid
flows QG = 36.68 10-6m3 s-1 and QL = 0.5 10-6m3 s-1; flows QG = 14.98 10-6m3 s-1 and QL = 0.5 10-6m3 s-1;
results in parameters Dax = 2.98 10-4 m2s-1, KGL = 3.24 results in parameters Dax = 1.18 10-4 m2s-1, KGL = 1.72
10-3 m s-1 and kLS = 1.68 10-1 m s-1 10-3 m s-1 and kLS = 1.56 10-2 m s-1
Figure 6: Dax vs (ReG)0.088, (FrG) 0.432 for the Figure 7: (Dax)Exp vs (Dax)Calc for the H2O/Ar – CH4/ γ -
H2O/Ar – CH4/ γ - Al2O3 system in trickle- Al2O3 system in trickle-bed regime. QG = (41.69 to
bed regime 9.97) 10-6 m3 s-1 and QL = 0.50 10-6 m3 s-1
Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
384 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
Figure 8: KGL vs (ReG)-0.842, (WeG) – 1.576 for the Figure 9: (KGL)Exp vs (KGL)Calc for the H2O/Ar – CH4/ γ
H2O/Ar – CH4/ γ - Al2O3 system in trickle-bed - Al2O3 system in trickle-bed regime. QG = (41.69 to
regime 9.97) 10-6 m3 s-1 and QL = 0.50 10-6 m3 s-1
Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
386 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
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Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
388 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
1 d Γ G ( ξ,s ) a1 ( s ) ∗
∗
Eqs. B8 and B9 were introduced in to Eq. B1 to
Γ∗L ( ξ,s ) = + Γ G ( ξ,s ) (B3) obtain the following equation:
α dξ α
(C1)
where 3
fi ( s )
Γ∗L ( ξ,s ) = ∑ λ
( s ) − a ( s )
i =1
i 1
α i ( s )
exp λ
δ ( s ) = a1 ( s ) − PE∗ κ ;
In Eq. C1 the integration constants, fi (s), were
K1 ( s ) = a1 ( s ) κ + ν ( s ) PE∗ ; (B7)
calculated from the three boundary conditions given
in Eqs. 22 and 23, expressed in the Laplace domain.
K 2 ( s ) = αγ
− a1 ( s ) ν ( s ) PE
∗
They were evaluated by the following system of
algebraic equations:
Combination 2: The response in the liquid phase
was obtained as follows: isolating Γ∗G (ξ, s) from Eq. f1 ( s ) + f 2 ( s ) + f3 ( s ) = 1 s (C2)
B2 and then differentiating Γ∗G (ξ, s) with respect to ξ.
λ1 ( s ) λ 2 ( s )
λ1 ( s ) − a1 ( s )
PE
{
− 1 f1 ( s ) + λ
2 ( s ) −a1 ( s )
PE
{
− 1 f 2 ( s ) + λ 3 ( s ) − a1 ( s )
(C4)
λ3 ( s )
− 1 f 4 ( s ) = 0
PE
The system of algebraic equations given by Eqs. (C2), (C3) and (C4) was solved by Cramer’s method, so
determinants D(s) were defined by
1 ( s ) , λ 2 ( s ) ,a1 ( s ) + T2 λ
D(s) = T1∗ λ 1 ( s ) , λ 2 ( s ) λ 3 ( s ) ,a1 ( s ) + T3 λ
1 ( s ) , λ 2 ( s ) , λ 3 ( s ) ,a1 ( s )
∗ ∗
(C5)
where
λ 2 ( s )
T1∗ λ
1 ( s ) , λ 2 ( s ) ,a1 ( s ) =
λ 2 ( s ) − a1 ( s )
λ 2 ( s ) exp λ
2 ( s )
λ 2 ( s ) − a1 ( s ) P
− 1
E (C6)
λ1 ( s )
{ λ1 ( s ) − a1 ( s )
PE
− 1
λ2 (s )
1 ( s ) , λ 2 ( s ) , λ 3 ( s ) ,a1 ( s ) = λ1 ( s ) − a1 ( s ) λ1 ( s ) exp λ
T2∗ λ 1 ( s ) λ 2 ( s ) − a1 ( s ) − 1
PE
(C7)
λ2 (s )
{
− λ 2 ( s ) − a1 ( s )
P
− 1
E
T3∗ λ {
1 ( s ) , λ 2 ( s ) , λ3 ( s ) ,a1 ( s ) = λ 3 ( s ) − a1 ( s ) λ 3 ( s ) exp λ
{{
3 ( s ) λ
λ1 ( s ) − 1
1 ( s ) − a1 ( s )
PE
(C8)
λ 2 ( s )
{
− λ 2 ( s ) − a1 ( s )
−1
PE
D1 ( s ) = 1 s V1∗ λ
2 ( s ) , λ 3 ( s ) ,a1 ( s ) (C9)
D2 ( s ) = 1 s V2∗ λ
1 ( s ) , λ 3 ( s ) ,a1 ( s ) (C10)
D3 ( s ) = 1 s V3∗ λ
1 ( s ) , λ 2 ( s ) ,a1 ( s ) (C11)
where
λ 3 ( s )
2 ( s ) , λ3 ( s ) ,a1 ( s ) = λ
V1∗ λ 2 ( s ) − a1 ( s ) λ
3 ( s ) −a1 ( s ) P
− 1 λ 2 ( s ) exp λ
2 ( s ) −
E (C12)
λ 2 ( s )
− 1 λ 3 ( s ) exp λ 3 ( s )
PE
λ1 ( s )
1 ( s ) , λ3 ( s ) ,a1 ( s ) = λ
V2∗ λ 1 ( s ) − a1 ( s ) λ
3 ( s ) −a1 ( s ) P
− 1 λ 3 ( s ) exp λ
3 ( s ) −
E (C13)
λ 3 ( s )
− 1 λ1 ( s ) exp λ 1 ( s )
P E
Brazilian Journal of Chemical Engineering, Vol. 20, No. 04, pp. 375 - 390, October - December 2003
390 J.D.Silva, F.R.A.Lima C.A.M.Abreu and A.Knoechelmann
λ 2 ( s )
1 ( s ) , λ 2 ( s ) ,a1 ( s ) = λ
V3∗ λ 1 ( s ) − a1 ( s ) λ
2 ( s ) −a1 ( s ) P
− 1 λ1 ( s ) exp λ
1 ( s ) −
E (C14)
λ1 ( s )
− 1 λ 2 ( s ) exp λ 2 ( s )
PE
Di ( s )
fi ( s ) = , (i = 1, 2, 3) (C15)
D (s)
limG∗ (1,s) =
S→0
1
{
lim V∗ ( λ2 ( s ) , λ3 ( s) ,a1 ( s ) ) exp lim λ1 ( s) + lim V2∗ ( λ1 ( s) , λ3 ( s) ,a1 ( s) ) exp lim λ2 ( s) +
lim D( s) S→0 1 S→0 S→0 S→0
(D1)
}
S→0
S→0
( S→0
)
lim V3∗ λ1 ( s) , λ 3 ( s ) ,a1 ( s ) exp lim λ3 ( s)
dG∗ (1,s )
lim = lim A1 ( s ) + lim A 2 ( s ) + lim A3 ( s ) (D3)
S→0 ds S→0 S→0 S→0
where
1 d dD ( s )
lim A1 ( s ) = lim V1 ( λ 2 ( s ) , λ 3 ( s ) ,a1 ( s ) ) exp λ1 ( s ) lim D ( s ) − lim
∗
2
S→0 lim D ( s ) S→0 ds S→0 S→0 ds
(D4)
S→0
lim V1∗ ( λ 2 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ1 ( s )
S→0
}
lim A 2 ( s ) =
S→0
1
lim D ( s )
{lim
2 S→0
d ∗
ds
V2 ( λ1 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ 2 ( s ) lim D ( s ) − lim
S→0
dD ( s )
S→0 ds
(D5)
S→0
lim V2∗
S→0
( λ1 ( s ) , λ3 ( s ) ,a1 ( s ) ) exp λ 2 ( s )}
lim A3 ( s ) =
S→0
1
lim D ( s )
{lim
2 S→0
d ∗
ds
V3 ( λ1 ( s ) , λ 2 ( s ) ,a1 ( s ) ) exp λ 3 ( s ) lim D ( s ) − lim
S→0
dD ( s )
S→0 ds
(D6)
S→0
lim
S →0
V3∗ V3∗
( λ1 ( s ) , λ 2 ( s ) ,a1 ( s ) ) exp λ3 ( s )}
As the differentiations of the determinants are very lengthy, they are not shown.
Brazilian Journal of Chemical Engineering