768 Ind. Eng. Chem. Res. 2001, 40, 768-773 http://www.paper.edu.

cn

Investigation of the Unsteady-State Oxidation of n-Butane to Maleic

Anhydride in Fixed-Bed Reactors

Xiao-Feng Huang,† Cheng-Yue Li,*,† Biao-Hua Chen,† Cong-Zheng Qiao,‡ and

Dong-Hai Yang†
College of Chemical Engineering, Beijing University of Chemical Technology, Beijing 100029, China, and
Department of Chemistry, Henan University, Kaifeng 475000, China

The periodic operation performance of n-butane selective oxidation to maleic anhydride over a
VPO catalyst in fixed-bed reactors was investigated. A temperature-programmed oxidation
experiment demonstrated that reoxidation sufficient to activate the catalyst could only be carried
out at a temperature higher than that of butane oxidation step. A periodic operation scheme,
simultaneous modulation of both composition and temperature, was proposed and examined in
a fixed-bed microreactor filled with 0.6 g of crushed catalyst and in a tubular fixed-bed reactor
packed with 30 g of catalyst. In both reactors, feed composition modulation enhanced selectivity
to maleic anhydride, but the conversion of butane and the yield of maleic anhydride dropped.
With a 1:0.4 cycle split and period of 4 min, reoxidation of the catalyst at 530 °C, and selective
oxidation at 405 °C, the yield of maleic anhydride by both composition and temperature
modulation was improved by 11.4% over that obtained for operation under steady-state conditions
with the same time-average flow of n-butane, which indicated that the higher reoxidation
temperature was effective in improving reactor performance.

1. Introduction oxidation, which leads to higher selectivity than that

Currently, the selective oxidation of n-butane to
maleic anhydride (MA) over vanadium phosphorus oxide
catalysts (VPO) is the only industrial process involving
the selective oxidation of a light alkane.1 It is commonly
recognized that the selective oxidation of n-butane
proceeds according to a redox mechanism with lattice
oxygen participation.2-4
In general, industrial chemical processes can be made
more economical and environmentally benign by im-
proving selectivity and decreasing the amount of byprod-
ucts and excess heat formed. Strategies for improving
selectivity have traditionally focused on developing new
catalytic materials or reducing product loss by improv-
ing heat removal for selective oxidation reactions.
Unsteady-state operation of chemical reactors may offer
a new means of controlling total oxidation by segregat-
ing the hydrocarbon feedstock from oxygen in the gas
phase,5 that is, splitting up the overall reaction spatially
or temporally into two steps, namely, hydrocarbon
selective oxidation and reoxidation of the reduced
catalyst. Each step can than be carried out under
suitable reaction conditions.
Dupont recently commissioned a new commercial
plant based on a circulating fluidized-bed (CFB) reactor
to produce maleic anhydride in a two-bed system
consisting of a riser reactor in which the VPO catalyst,
along with some supplementary air, oxidizes n-butane
to maleic anhydride and a fluidized-bed regenerator in
which the catalyst is reoxidized.6-8 In Dupont’s CFB
technology, gas-phase oxygen is limited during the
oxidation of hydrocarbon to reduce the extent of total
* Author to whom correspondence should be addressed.
E-mail: licy@buct.edu.cn.
† Beijing University of Chemical Technology.
‡
Henan University.
10.1021/ie0004390 CCC: $20.00 © 2001 American Chemical Society
Published on Web 01/12/2001
normally encountered in fixed-bed systems. The tech-
nology has the advantage of higher butane concentra-
tions and more efficient heat removal. However, the
process requires attrition-resistant catalyst and circu-
lates large amounts of catalyst. As indicated by Emig
et al.,3 a process based on the separation of the redox
cycle might not be economic, as energy costs and space-
time yield must be considered. Their pulse experiments
suggested that the limiting step was catalyst reoxidation
and that a high temperature might shorten the regen-
eration time.
A similar technology, called an “in situ” redox fluid-
ized-bed reactor, was tested in the oxidation coupling
of methane.9 Oxygen was fed into the bottom of the
reactor, while alkane was fed through a distributor near
the top, so that oxidation of the catalyst occurred near
the bottom of the bed and reduction near the top.
However, complete separation of the oxidation and
reduction zones might be impossible in this system.
Another approach to an organized catalytic cycle is
forced periodic operation by temporal separation of
n-butane oxidation and catalyst reoxidation in a fixed-
bed reactor. Feed composition cycling of the selective
oxidation of butadiene to maleic anhydride over a
vanadium molybdate catalyst was studied by Lang et
al.10 In some of their experiments, it was found that
selectivity to MA increased but conversion of hydrocar-
bon always decreased.
As part of a systematic investigation of the unsteady-
state oxidation of n-butane to maleic anhydride over a
domestic VPO catalyst, the reaction mechanism, dy-
namic kinetics, and reactor simulations have been
studied in our group.11-13 The objective of this paper is
to report the effect of composition and temperature
modulation on the time-average performances of fixed-
bed reactors. A new periodic operation scheme, simul-
中国科技论文在线
Figure 1. Schematic diagram of the TGA experimental setup.
taneous modulation of both composition and tempera-
ture, is proposed and examined at different reactor
scales.
2. Experimental Section
Three types of experiments were undertaken in this
investigation. First, regeneration of the VPO catalyst
was investigated by temperature-programmed oxida-
tion in a thermogravimetric (TGA) unit. Our objective
in this experiment was to examine the effect of temper-
ature on reoxidation of the catalyst. Next, composition
modulation experiments were performed in a fixed-bed
microreactor to investigate the time-average perfor-
mance. Finally, experiments of both composition and
temperature modulation were carried out in a tubular
fixed-bed reactor. The purpose of the last set of experi-
ments was to explore the effects of heat and mass
transfer in a tubular reactor on the time-average
performance under modulated reaction conditions.
Figure 1 is a sketch of the thermogravimetric unit
employed for the TPO and kinetic measurements. The
TGA unit was a Perkin-Elmer TGS-2, a fully automatic
thermogravimetric balance with temperature control
that allowed operation up to about 800 °C. A feed array
was used equipped with a group of switching valves that
permitted the introduction of a controllable mixture of
O2 in He or a mixture of n-butane (C4) in He.
The experimental apparatus for composition modula-
tion experiments is shown in Figure 2. The CDS 804
micro pilot plant reaction system was used (Chemical
Data System Inc.), consisting of a fixed-bed microreac-
tor, a temperature-controlled furnace, a programmable
timer, and an on-line gas chromatograph. The reactor
was a stainless steel tube of 6.5 mm i.d. and a total
height of 250 mm. The reaction section was packed with
about 0.6 g of 60/80 mesh catalyst diluted with quartz
sand. An air-actuated eight-way valve controlled by the
programmable timer allowed for quick switching be-
tween two gas feeds with different compositions. One
feed comprised n-butane and oxygen in a He diluent,
while the other was 20% O2 with He as the diluent. The
reactor effluent was introduced into an absorber, where
it was bubbled through water to absorb maleic anhy-
dride, and then cooled in a condenser. Only maleic
anhydride was found in the solution. To obtain the time-
average composition of product, the noncondensed gas
Ind. Eng. Chem. Res., Vol. 40, No. 3, 2001 769
was mixed in a glass vessel before being analyzed with
two gas chromatographs connected in series. The rela-
tive difference in reproducibility for measuring selectiv-
ity to MA and conversion of butane is less than 3%.
When transient measurements were needed, effluent
was introduced directly into a mass spectrometer after
being split through a heated quartz capillary.12
Further experiments were carried out in a tubular
fixed-bed reactor with a single tube of 19 mm i.d. and
1.2 m length, where the wall temperature was controlled
to keep it constant. Cylindrical pellets of VPO catalysts
(6 mm diameter × 6 mm height) were diluted with
ceramic beads and packed in the middle section, while
6 mm Al2O3 pellets were packed in both ends. The
reactor was placed in a split aluminum block that was
surrounded with six separately controlled electric heat-
ing coils. Six thermocouples inserted in the tube wall
of the reactor at 150 mm axial intervals were used to
measure the wall temperatures and control the heating
coils so as to maintain a nearly uniform reactor wall
temperature. An additional thermocouple jacket in-
serted in the catalyst bed was used to measure temper-
ature along the axis of the reactor. The reactor effluent
was collected in a gas bag after water absorption, and
the time-average composition of the mixture was ana-
lyzed by gas chromatograph.
The vanadium pyrophosphate catalyst used in this
work was a domestic commercial VPO catalyst devel-
oped by the Beijing Research Institute of Chemical
Technology. It had undergone 7000 h of steady-state use
in a pilot plant with a single-tube wall-cooled reactor
and gave a selectivity to MA of approximately 60-63%
at 85-90% conversion. The catalyst was sufficiently
characterized by XRD, XPS, and FTIR measurements.11
XRD measurements showed that the fresh catalyst was
primarily (VO)2P2O7. The other component was the
orthophosphate, VOPO4. The catalyst as received was
crushed and sieved to give a fraction between 60 and
80 U.S. mesh but was not otherwise pretreated.
3. Results and Discussion
3.1. Temperature-Programmed Oxidation Ex-
periments. The temperature-programmed oxidation
measurement was performed with fresh catalyst. A 45-
mg sample was brought to 50 °C in flowing He, and then
the temperature was brought to 800 °C at a rate of 10
°C/min under a flow of 21 vol % O2 in He at 20 mL/min.
Figure 3 shows the response to temperature ramping.
Ait-Lachgar et al.14 undertook the same experiment and
found similar results.
Initially, the sample loses water, and the weight
decreases up to 280 °C. The weight increases after 500
°C, indicating oxidation of the catalyst. The weight gain
is rapid and continues to about 680 °C, where crystal
changes weaken the structure and spalling occurs,
leading to weight loss. The selective oxidation of butane
to maleic anhydride on the VPO catalyst normally
occurs at about 400 °C; the reoxidation of the catalyst
at this temperature is so slow that this step is certainly
rate-controlling.
A temperature of at least 500 °C is needed for the
oxidation process to proceed rapidly, which suggests
that modulation of both composition and temperature
might lead to improved reactor performance.
In Dupont’s CFB technology,7,8 the reaction temper-
ature in the regenerator in which the catalyst is
reoxidized appears to be the same as that in the
770 Ind. Eng. Chem. Res., Vol. 40, No. 3, 2001
Figure 2. Schematic diagram of a fixed-bed microreactor system.
Figure 3. TGA curves as a function of temperature in a flowing mixture of oxygen with He.
selective oxidation reactor. This experiment indicates
that such a policy is not suitable, at least not for the
VPO catalyst studied. Emig et al.3 investigated the
influence of the regeneration temperature from 340 to
430 °C in a pulse reactor. It seems that this temperature
range is still low for rapid reoxidation of the catalyst.
3.2. Composition Modulation in a Fixed-Bed
Microreactor. In this type of experiment, a mean feed
composition of 1.5% n-butane was used, which follows
industrial practice. That is, when a 1:1 cycle split
between reduction and reoxidation of the catalyst was
used, the feed to the reactor was alternated between
20% oxygen with He as the diluent and a mixture of
3% n-butane and adjustable oxygen in a helium carrier
gas.
The effect of the oxygen concentration in the reduction
half-cycle was examined by varying the oxygen content
in the butane-containing feed from 0 to 25% at a period
of 4 min and 1:1 cycle split. Figure 4 shows the
comparisons of the conversion, selectivity, and yield at
http://www.paper.edu.cn
different oxygen concentrations. Al though no or limited
oxygen in the butane-containing feed was suggested in
Dupont’s two-bed system, the experiments completed in
the fixed-bed microreactor indicate that the optimal
hydrocarbon/oxygen ratio is 1:5, a value between the
stoichiometric amounts of selective oxidation and total
oxidation. Figure 5 gives the transient response behav-
ior of maleic anhydride for cycling operation with a feed
containing no oxygen, which indicates that the concen-
tration of maleic anhydride reaches a maximum just
after switching but drops to quite a low level after only
several seconds. In this experiment, a poor time-average
yield was obtained. Of course, this also relates to the
contact time of the catalyst with butane. Shortening the
contact time gives a higher time-average conversion and
yield if the catalyst can rapidly be reoxidized to main-
tain its activity. In the riser of a CFB reactor system, it
is possible to use a feed with a lower oxygen concentra-
tion and to employ a short catalyst residence time.
中国科技论文在线
Figure 4. Effect of oxygen concentration in butane-containing
feed on reactor performance. Reaction conditions: T ) 430 °C, CS
) 0.5, τp ) 4 min, feed was alternated between 3% butane and
adjustable oxygen with He as the diluent and 20% O2 + He.
Figure 5. Transient concentration responses of MA for cycling
operation with a feed in the absence of oxygen. Reaction condi-
tions: T ) 416 °C, CS ) 0.5, τp ) 4 min, feed was alternated
between 3% butane in a He carrier gas and 20% oxygen with He
as the diluent.
Figure 6. Transient concentration responses of MA for cycling
operation with an oxygen-containing feed. Reaction conditions: T
) 416 °C, CS ) 0.5, τp ) 4 min, feed was alternated between 3%
butane + 15% oxygen with He as the diluent and 20% oxygen in
a He carrier gas.
However, a short contact time is difficult for a fixed-
bed reactor.
The effects of the cycle period, cycle split, and reaction
temperature were also investigated by Qiao.11 The
optimal performance for unsteady state (USS) operation
of composition modulation was achieved at 416 °C, a
period of 4 min, and split of 1:1 for a feed with 3%
n-butane and 15% oxygen in the half-cycle of selective
oxidation. Transient responses of maleic anhydride for
composition modulation with an oxygen-containing feed
are illustrated in Figure 6. A distinct overshoot in the
concentration of maleic anhydride was observed just
after switching, which suggests that performance im-
provement might be achieved by composition modula-
Ind. Eng. Chem. Res., Vol. 40, No. 3, 2001 771
Table 1. Performance Comparisons between
Steady-State Operation and Composition Modulationa
T τp CB SMA YMA
operation (°C) (min) (%) (%) (%)
USS 416 4 75.0 67.0 50.3
SS1 416 - 56.5 63.5 35.9
SS2 416 - 88.1 65.5 57.7
a Space velocity ) 2100/h.
tion, provided a suitable cycling period is adopted. Two
steady-state experiments were also carried out at the
same reaction temperature for comparison with com-
position modulation. For the first (SS1), the reactor was
fed with the same composition used in the catalyst
reduction step with composition modulation, namely, 3%
n-butane and 15% oxygen, while for the other experi-
ment (SS2), the reactor was fed with 1.5% n-butane and
20% oxygen to reach the same time-average concentra-
tion of n-butane as employed in the composition modu-
lation experiment. Table 1 summarizes the perfor-
mances under steady-state and unsteady-state or
modulated operation. Both selectivity to maleic anhy-
dride and conversion of butane were enhanced by
reoxidation of the catalyst through modulation, com-
pared with the results obtained in SS1. However, a
comparison of the time-average performance with SS2
shows that the yield of maleic anhydride under unsteady-
state conditions dropped by 6.1% because of a loss in
conversion, even though there was an improvement in
selectivity.
3.3. Composition and Temperature Modulation
in a Fixed-Bed Microreactor. A new modulation
scheme, simultaneous modulation of both composition
and temperature in the fixed-bed microreactor, was also
investigated. That is, a butane- and oxygen-poor mix-
ture with a helium carrier was introduced during the
half-cycle of selective oxidation at a given reaction
temperature, and then the catalyst fixed-bed was rap-
idly heated to a given reoxidation temperature in
flowing helium. When this temperature was reached,
the flow was switched to 20% oxygen in helium. After
the reoxidation half-cycle, the catalyst was cooled by
blowing it with helium until the selective oxidation
temperature was reached again.
Two cyclic experiments were performed with the
optimal feed conditions for composition modulation as
described in the last section. In the first, both partial
oxidation of C4 and reoxidation of the catalyst were
carried out at 416 °C, while in the second experiment,
reoxidation was performed at 560 °C. Although both
the oxidation and reduction portions of the cycle totaled
only 4 min, a whole cycle took about 110 min because a
much longer time was needed to change the tempera-
ture of the catalyst. Measurements were taken in the
second full cycle of the experiment. It is, of course, not
certain that a reproducible cycling steady state was
reached in these limited experiments, as laboratory
facilities made longer runs impossible. However, our
purpose in these experiments was just to demonstrate
that carrying out the steps in the two-step process at
different temperatures could give significantly better
results. Table 2 shows the conversion of butane, selec-
tivity, and yield of maleic anhydride in each experiment.
There is a remarkable improvement in all three indexes.
This confirms the efficacy of the modulation scheme.
The transient concentration response for the modula-
tion of both composition and temperature, as illustrated
772 Ind. Eng. Chem. Res., Vol. 40, No. 3, 2001 http://www.paper.edu.cn
Table 2. Comparison of Performances between Table 4. Results of Orthogonal Experiments for
Composition Modulation and Simultaneous Modulation Simultaneous Modulation of Both Composition and
of Both Composition and Temperaturea Temperature in a Tubular Fixed-Bed Reactor
TROX (°C) TSOX (°C) CB (%) SMA (%) YMA (%) A B C D
CB SMA YMA
416 416 77.5 64.1 49.7 no. TW (°C) W
TSOX (°C) τp (min) CS (%) (%) (%)
ROX
560 416 89.8 67.4 60.5
1 500 405 8 0.5 86.2 74.7 64.4
a Space velocity ) 2100/h. 2 500 415 4 0.6 90.2 65.9 59.4
3 500 425 6 0.4 82.9 70.2 58.2
Table 3. Comparison of Performances between 4 530 405 4 0.4 89.0 76.3 67.9
Steady-State and Unsteady-State Operation in a Tubular 5 530 415 6 0.5 84.3 68.9 58.1
Fixed-Bed Reactor 6 530 425 8 0.6 89.0 59.0 52.5
TW W
TSOX τp CB SMA YMA 7 560 405 6 0.6 85.0 64.7 55.0
ROX
operation (°C) (°C) (min) (%) (%) (%) 8 560 415 8 0.4 86.7 64.3 55.7
9 560 425 4 0.5 87.3 63.0 55.0
SS 410 410 - 82.6 61.6 50.9
USS1 400 400 4 68.9 69.9 48.0 R 16.3 21.6 11.0 14.9
USS2 400 400 6 68.6 73.0 50.0 prior 530 405 4 0.4
level

mixing during switching, but nevertheless, the yield was

Figure 7. Transient response of MA for simultaneous modulation
of both composition and temperature. Reaction conditions: TROX
) 560 °C, TSOX ) 416 °C, CS ) 0.5, feed was alternated between
3% butane + 15% oxygen with He as the diluent and 20% oxygen
in a He carrier gas, τp ) 8 min with helium blowing between two
half-cycles.
in Figure 7, is similar to Figure 6. However, the
attenuation of the overshoot here is slower than that
in Figure 6, which suggests that the higher reoxidation
temperature leads to more storage of lattice-oxygen in
the near-surface layer of the catalyst and improved
reactor performance. Correspondingly, the FTIR spectra
of the catalyst indicated the partial transformation from
(VO)2P2O7 to β-VOPO4.12
The necessity of cooling and heating the catalyst
reduces the reactor throughput for a fixed-bed reactor.
However, this drawback disappears in a two-bed process
with catalyst circulation between beds. Optimization of
the temperatures of the two steps is possible so that the
performance can certainly be further improved.
3.4. Periodic Operation in a Tubular Fixed-Bed
Reactor. A steady-state experiment was carried out in
a tubular fixed-bed reactor with a feed of 1.5% n-butane
and 20% oxygen at a wall temperature of 410 °C and a
space velocity 2000/h. The selectivity was 61.6% at
82.6% conversion, which was close to the performance
measured in a pilot plant constructed by Beijing Re-
search Institute of Chemical Technology, who provided
the catalyst used in this investigation.
With the same optimal feed compositions as used in
the fixed-bed microreactor, a composition modulation
experiment at a wall temperature of 400 °C and a space
velocity of 2000/h was also performed in the tubular
reactor. As shown in Table 3, the selectivity to maleic
anhydride was improved by 8.3% over that obtained at
steady state, but the conversion dropped by 13.7%. A
longer cycle period of 6 min brought higher selectivity,
which might come from the smaller contribution of back-
still a little lower than that in the steady-state experi-
ment.
Modulation experiments of both composition and
temperature for different cycling strategies were carried
out according to an L9(34) orthogonal design. Feed
compositions for different half-periods are the same as
in the composition modulation experiment mentioned
above. The wall temperatures of the tubular reactor in
each step, cycle period, and split were considered as
independent factors.
Results of the orthogonal design experiments are
shown in Table 4. The yield of maleic anhydride was
used to evaluate the performance, which was improved
in all experiments over that obtained in steady-state
operation. The best yield, 67.9%, was found at a tem-
perature of 405 °C for selective oxidation, a temperature
of 530 °C for reoxidation, a cycle period of 4 min, and a
split of 0.4. It can be seen that the effects of the factors
on the yield of maleic anhydride are as follows: tem-
perature for selective oxidation > temperature for
reoxidation > cycle period > cycle split.
The experiments in the tubular reactor confirmed the
efficacy of the simultaneous modulation of both compo-
sition and temperature. It suggests that splitting of the
redox cycle into two steps requires that each step be
matched with suitable reaction conditions.
It must be noticed that the results reported above
were obtained for a limited duration of experimental
investigation, and the conclusion should not be adopted
directly for application purposes. Taking account of
possible phosphorus loss at higher regeneration tem-
peratures, new catalysts that can efficiently be regener-
ated at a lower temperature should be developed or
some way of supplementing phosphorus is considered.
Conclusion
The periodic operation performance of n-butane selec-
tive oxidation to maleic anhydride over a VPO catalyst
in fixed-bed reactors with different scales was investi-
gated. The temperature-programmed oxidation experi-
ment revealed the effect of temperature on the extent
and rate of reoxidation of the catalyst. A periodic
operation scheme, simultaneous modulation of both
composition and temperature, was proposed and exam-
ined at two different reactor scales. A higher reoxidation
temperature improves reactor performance.
Simultaneous modulation of both composition and
temperature might not be feasible in industry because
中国科技论文在线
of the difficulty in frequently and tempestuously chang-
ing temperature. However, it is possible to realize
different temperatures in a two-bed process, as men-
tioned before. The simulation study of a riser-regenera-
tor system13 demonstrated the advantage of tempera-
ture modulation in comparison to maintaining the same
temperature in two reactors. Taking account of possible
phosphorus loss at higher temperatures, the develop-
ment of a new catalyst that can efficiently be reoxidated
at a lower temperature is needed for unsteady-state
oxidation technologies of n-butane to MA.
Acknowledgment
The present work was financially supported by the
National Natural Science Foundation of China under
Grant 29792073-3.
Notation
CB ) conversion of butane, %
CS ) cycle split
SMA ) selectivity to MA, %
T ) temperature, °C
TROX ) temperature of reoxidation, °C
TSOX ) temperature of selective oxidation, °C
W (12) Huang, X. F. Dynamic kinetic model of butane selective
TROX ) wall temperature of reoxidation, °C
W
TSOX ) wall temperature of selective oxidation, °C
YMA ) yield of MA, %
τp ) cycle period, min
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Received for review April 28, 2000
Revised manuscript received October 26, 2000
Accepted November 6, 2000
IE0004390