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abstract
Article history:
In this paper, the mass transfer performance of the 10 mm metal Pall ring packing for am-
gated. The experimental setup is described and the experimental procedure and data
15 May 2007
reduction method are explained. Experimental results of the top vapour temperature, con-
centration and mass flow rate are presented for different operating conditions, including
reflux ratio values from 0.4 to 1 (total reflux conditions). Vapour phase mass transfer coef-
Keywords:
ficients are calculated from the measured data and the results are compared with different
Absorption system
mass transfer correlations found in the open literature. In this paper, a correlation is pro-
Ammoniawater
posed for the packing analysed which was fitted from the experimental data. Finally,
Rectification
a comparison is made between the actual packing height used in the experimental setup
Aqueous solution
and the height required to obtain the same ammonia rectification in AARS with the first
Experiment
generation packings: 12
Packing
Novalox saddles. It was found that a packing height reduction between a factor of 2.5 and
Packed column
00
00
ceramic
Mass transfer
1.
Introduction
Nomenclature
aef
ap
Cpk, Cv
dc
D
F
Fc
h
H
k
_
m
M
n_
p
Q
r
T
u
V_
x
x~
y
z
271
Greek symbols
DT
temperature deviation, Tv;out TNH3 (K)
Dx~v;lm
logarithmic mean driving force in vapour phase
3
r
F
c
Subscripts
i
interface
l
liquid
o
overall
sat
saturation conditions
v
vapour
Superscripts
*
vapour in equilibrium with liquid
272
columns filled with random or structured packings. They adjusted the vapour and liquid mass transfer coefficients by specific parameters depending on the packing type, material and
dimensions. Wagner et al. (1997) developed a new model for
the prediction and correlation of mass transfer in distillation
columns containing modern, high efficiency random packings
of the high-void-fraction and through-flow type. This model is
also based on the penetration theory and the only packing parameter needed is a packing characteristic Cpk which must be
determined from experimental results. They found that 95%
of the predicted values were within 25% of 326 experimental
data points at total reflux. Finally, Piche et al. (2002) proposed
a set of artificial neural network correlations for the vapour
and liquid mass transfer coefficients and interfacial area in
randomly packed towers. They gathered data of interfacial
area and volumetric mass transfer coefficients from the literature to generate a working database including over 3780
measurements; however, mass transfer coefficients relevant
to distillation were not processed.
A number of mass transfer models for packed columns
have been published in the literature. However, quite different
results are obtained when these models are applied at the normal operating conditions found in AARS. Therefore, some experimental validation of the current mass transfer models for
being applied to the ammonia purification process in AARS is
needed. In a recent paper, Sieres and Fernandez-Seara (2007b)
investigated the mass transfer performance of 15 mm glass
Raschig rings, 12 00 ceramic Berl saddles and 12 00 ceramic Novalox saddles random packings for the ammonia rectification in
AARS. They showed that experimental mass transfer coefficients in the vapour phase were well represented by the
Onda et al. (1968) correlation. In a similar work, the same authors (Sieres and Fernandez-Seara, 2007a) tested the Sulzer BX
packing and found discrepancies with available mass transfer
models for structured packings.
In this paper, the mass transfer performance of the 10 mm
metal Pall ring random packing is examined. Experimental
data are obtained from several tests carried out in an experimental facility designed and built at our laboratory. The facility operates at the typical operating conditions found in AARS.
Experimental results of the top vapour temperature, ammonia
concentration and mass flow rate at variable and total reflux
conditions are presented. Mass transfer coefficients are
reported and compared with different correlations proposed
in the literature. Finally, a comparison between the performance of the tested packing and the first generation random
packings previously tested (Sieres and Fernandez-Seara,
2007b) for the ammoniawater rectification in AARS is made.
2.
Experimental setup
0.08
0.238
Pall ring
Stainless steel
10
515
0.94
273
card contains four lines of digital outputs that are used to control the electrical power in the electric heater.
The experimental facility was charged with a mixture of
ammonia and water to obtain the desired mixture concentration. Previously, the installation was purged with a vacuum
pump to avoid the presence of air.
3.
Experimental procedure and
data reduction
3.1.
Experimental procedure
3.2.
Data reduction
(1)
The bottom liquid concentration is obtained from the density and temperature measured by the Coriolis flow meter
M2, according to Eq. (2).
xl;out fl;sat TM2 ; rM2
(2)
(3)
_ M2 m
_ M3
_ v;in m
m
(4)
274
_ M3 xv;out
_ M2 xl;out m
m
_ M3
_ M2 m
m
(5)
The reflux ratio (r) is defined as the ratio of the liquid mass
flow entering the column to the vapour mass flow leaving the
column, as stated in Eq. (6).
r
_ l;in
m
_ v;out
m
dV_ V_
dy
_ M2
_ v;in m
m
(8)
xv;in xl;out
(9)
_ is obtained from
where the vapour superficial molar flow V
_ v and the column diameter dc ,
the vapour mass flow m
according to Eq. (12).
4
xv
1 xv
_v
(12)
V_
m
2
pdc
MNH3
MH2 O
A mass and species balance over a differential cross-section
of the packed column yields Eqs. (13) and (14).
_ ef dy
dV_ na
(13)
d V_ x~v V_ dx~v dV_ x~v n_ NH3 aef dy
(14)
dx~v
Dx~
dx~v
V_
v;lm
!
Fv $aef z x~v x~ x~v
z x~v
z x~v
v
ln
z x~v
1
(16)
(7)
n_ NH3
n_
V_
Fv aef
(6)
_ M1
_ l;in m
m
(15)
dx~v
z x~v
x~v x~v
z x~v
ln
z x~v
(17)
4.
4.1.
Experiments were carried out with heat powers of 3.6, 4.8, 6.0
and 7.2 kW. For each one of the heating powers, different operating pressures and reflux ratios were tested. Table 2 summarizes the range of values for different variables of interest
measured during all the experiments. For test runs with
heat powers of 3.6 kW, only total reflux conditions were tested
because of the difficulties to measure low mass flow rates in
the flow meter M3. In contrast, for test runs with heat powers
of 7.2 kW, it was not possible to operate the column at total
reflux conditions, because the high values of vapour and liquid mass flow rates caused flooding of the column.
For each set of experimental data, the top vapour ammonia
concentration and different mass transfer performance parameters were determined. A detailed analysis of the experimental uncertainties was carried out and the typical
uncertainty bands are included in the results. The uncertainties have been determined from the analysis of the experimental measurements and the accuracy specifications of the
different sensors, as indicated in ISO (1995).
Min
Max
11.2
29.1
6.0
2.5
29.5
635
0
5.2
0.4
15.5
79.0
20.4
10.6
70.1
839
11.3
16.5
1
Fig. 2a shows the difference between the top vapour temperature and the saturation temperature of pure ammonia
as a function of the reflux ratio for a set of experimental tests
carried out for a constant operating pressure of 11.3 bar and
heat powers of 3.6, 4.8 and 6.0 kW. This temperature difference has been denominated in the following as temperature
deviation DT Tv;out TNH3 . The top vapour water content
and mass flow rate for the same experiments are shown in
Fig. 2b and c, respectively. The reflux ratio tested ranges
from total reflux (r 1) down to r 0.5.
It can be seen in Fig. 2a that when decreasing the reflux ratio the temperature deviation increases slightly, but below
a reflux ratio of rz0:6 a sharp increase of DT is obtained, which
indicates an increase of the vapour water content, as confirmed in Fig. 2b. Fig. 2c shows that the vapour flow rate
increases slightly when increasing the reflux ratio, but remains nearly constant for reflux ratio values higher than
rz0:6. This behaviour is reasonable because when increasing
the reflux ratio the column performs better and the ammonia
vapour concentration in the vapour phase is higher. Since the
heat of vaporization for water is greater than for ammonia,
the condensation of a certain amount of water from the vapour to the liquid phase implies that a greater amount of ammonia can be transferred to the vapour phase, thus increasing
the vapour mass flow rate. However, for high values of the
reflux ratio, an increase of the liquid reflux may cause a very
small variation of the top ammonia concentration or even
obtaining pure ammonia, thus no significant variations in
the vapour mass flow are observed.
On the other hand, Fig. 2c shows the behaviour of an increasing top vapour mass flow rate with increasing heat
power. Moreover, the experimental results indicate that the
column performs better as the vapour mass flow rate increases, since the temperature deviations in Fig. 2a decrease
with Q. This means that lower water contents are obtained
in the vapour phase, as it can be seen in Fig. 2b.
It should be noted that during some experiments (especially those at total reflux), the top vapour temperature is
very close to the ammonia saturation temperature. As an example, in the case of the 6.0 kW test at total reflux, the temperature deviation DT is within the typical uncertainty of the
experimental measurements. Therefore, the ammonia
concentration of the top vapour is very high, but the experimental procedure does not allow the determination of
the concentration with precision for water contents below
10 ppm, as can be confirmed from the uncertainty bands
shown in Fig. 2b.
In Fig. 3 results of experiments carried out at a constant
heat power of 4.8 kW and operating pressures of 11.3, 13.4
and 14.4 bar as a function of the reflux ratio are presented.
Fig. 3a shows that the top vapour temperature deviation DT increases when reducing the reflux ratio, thus deviating from
pure ammonia conditions, as confirmed in Fig. 3b. The temperature deviation increases sharply for reflux ratio values
lower than 0.6. On the other hand, it can also be seen that
for total reflux or high reflux ratio values, the top vapour water
content increases with decreasing values of the operating
pressure. Fig. 3c also shows that the vapour mass flow increases slightly for low reflux ratios, but remains nearly constant for reflux ratios greater than 0.6.
4.2.
275
276
4Fv Dv uv
p3 hc
0:5
(18)
277
(19)
where H is the packing height and Cpk is a dimensionless packing constant which must be determined from experimental
results.
The effective area for mass transfer is obtained from
Eq. (20).
aef 1 3 h
1
13
ap
(20)
4.3.
Finally, in this section a comparison is made between the performance of the 10 mm metal Pall ring packing and the three
different random packings: 12 00 ceramic Berl saddles, 15 mm
glass Raschig rings and 12 00 ceramic Novalox saddles, previously tested (Sieres and Fernandez-Seara, 2007b) for the ammoniawater rectification in AARS.
Fig. 6 compares of the packing height used in the experimental setup with 10 mm metal Pall rings with the height required to obtain the same ammonia rectification in AARS with
the three different first generation packings indicated above.
The packing heights were calculated from the correlations
reported in Sieres and Fernandez-Seara (2007b) for AARS. Results show that with the three first generation packings larger
heights are required than with the 10 mm metal Pal ring packing in order to obtain the same ammonia concentration. Moreover, the differences increase with the column load factor
p
Fc uv rv . Therefore, results in Fig. 6 point out that the column height in AARS could be reduced in a factor between 2.5
and 3 if 10 mm metal Pall rings are used instead of the first
generation packings considered in this analysis.
5.
Conclusions
278
Acknowledgments
The authors would like to acknowledge the financial support
from the Ministerio de Ciencia y Tecnologa (project DPI
2002-04536-C02-02).
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