ARTICLE IN PRESS

Radiation Physics and Chemistry 69 (2004) 3137

Hydrocracking of cumene over Ni/Al2O3 as inuenced by

CeO2 doping and g-irradiation
G.A. El-Shobakya,*, M.M. Doheimb, A.M. Ghozzac
a

Laboratory of Surface Chemistry and Catalysis, National Research Center (NRC), Dokki, Cairo, Egypt
b
Egyptian Petroleum Research Institute (EPRI), Nasr City, Cairo, Egypt
c
Faculty of Science, Department of Chemistry, Zagazig University, Zagazig, Egypt
Received 6 January 2003; accepted 10 June 2003

Abstract
Cumene hydrocracking was carried out over pure and doped Ni/Al2O3 solids and also, on these solids after exposure
to different doses of g-rays between 0.4 and 1.6 MGy. The dopant concentration was varied between 1 and 4 mol%
CeO2. Pure and doped samples were subjected to heat treatment at 400
C and cumene hydrocracking reaction was
carried out using various solids at temperatures between 250
C and 400
C by means of micropulse technique. The
results showed that both CeO2 doping and g-irradiation of the investigated system brought about an increase in its
specic surface area. g-irradiation of pure samples increased their catalytic activities effectively. However, the doping
caused a decrease in the catalytic activity. g-irradiation of the doped samples brought about a net decrease in the
catalytic activity.
The catalytic reaction products over different investigated solids were ethylbenzene as a major product together with
different amounts of toluene, benzene and C1C3 gaseous hydrocarbons. The selectivity towards the formation of
various reaction products varies with the reaction temperature, doping and g-irradiation.
r 2003 Elsevier Ltd. All rights reserved.
Keywords: g-irradiation; CeO2 doping; Cumene hydrocracking; Ni/Al2O3

1. Introduction
Transition metals or metal oxides on support are
commonly employed to catalyze several reactions
including oxidationreduction, dehydration, dehydrogenation, cracking, alkylation, etc. (Muradov, 1993; Dos
Santos et al., 1997; Zhang and Amiridis, 1998; Velu and
Swamy, 1997; El-Shobaky and Al-Noaimi, 1987a; Luo
et al., 1997; El-Shobaky et al., 1997, 2001; Golchet and
White, 1978; Youssef et al., 1992; Mendes and Schmal,
1997; Li and Ding, 2000). The activities and selectivities
for these variety of solids could be modied by doping
with certain foreign oxides (El-Shobaky et al., 1988,
1989, 2000, 2002, 2003; El-Boohy et al., 2002; Doheim
et al., 2001a, b, 2002).

*Corresponding author. Fax: +20-2-3370-931.

E-mail address: elshobaky@yahoo.com (G.A. El-Shobaky).

Ionizing radiation induces some changes in textural,

surface structural, electric and magnetic properties of
a large variety of solids. g-irradiation resulted in a
decrease in the surface area of graphite as a result of a
progressive blocking of pores as bulk expansion took
place (Andreev et al., 1991). This treatment caused a
signicant increase in pore size of steam activated
carbon due to possible radiolytic decomposition of
complexes located on the carbon surface (Spalaris et al.,
1957). g-irradiation affected also a decrease in the
effective paramagnetic properties of CuO loaded on
Al2O3 (Youssef et al., 1992).
It has been also reported that g-rays led to removal of
chemisorbed oxygen of unloaded Co3O4 and those
loaded on g-Al2O3 (Youssef et al., 1992; El-Shobaky
et al., 1987b, c, 1994, 1998). Furthermore, g-irradiation
induced a progressive decrease in both microstrain and
lattice parameters of Co3O4 crystallites supported on
g-Al2O3 and precalcined at 650
C due to removal of

0969-806X/$ - see front matter r 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/S0969-806X(03)00444-4

ARTICLE IN PRESS
32

G.A. El-Shobaky et al. / Radiation Physics and Chemistry 69 (2004) 3137

excess oxygen and fragmentation of its crystallites (ElShobaky et al., 1987c). However, these catalysts undergo
deactivation due to the formation of cobalt aluminate
via metal oxidealumina interactions (Bolt et al., 1993).
The present work aimed at investigating the role of
doping Ni/Al2O3 system with CeO2 and treating the
same with g-irradiation on its surface and catalytic
properties. The techniques employed were XRD, nitrogen adsorption isotherm measured at 196
C and
cumene hydrocracking at 250400
C.

2. Experimental

tion isotherms measured at 196
C using conventional

volumetric apparatus. Before carrying out such measurements, each sample was degassed under a reduced
pressure of 105 Torr for 2 h at 200
C.
A PerkinElmer Sigma 3B gas chromatograph with a
bentone 34, 1 m and 1/8 in internal diameter, inj. 200
C,
oven 60
C isotherm, FID 200
C, 25 ml min1 and H2 as
a carrier gas. The reactant under investigation (cumene)
was introduced in microquantities (12  103 cm3) with
the aid of a microsyringe in the form of pulse, into a
small amount of catalyst (50 mg). The reaction products
were transferred directly by the carrier gas (hydrogen) to
the gas chromatograph.

2.1. Materials
3. Results and discussion
Nickel oxide supported on g-alumina was prepared by
treating a calculated amount of nely powdered
Al(OH)3 with a known amount of Ni(NO3)2 dissolved
in the least amount of distilled water. The obtained
solids were dried at 110
C to constant weight, then
subjected to thermal treatment at 500
C for 5 h. The
composition of the prepared solids after calcination was
0.1NiO/Al2O3, the NiO content was 10%. Three doped
samples were prepared by treating the Al(OH)3 support
material with cerium nitrate dissolved in the least
amount of distilled water. The obtained solids were
dried at 110
C to constant weight then treated with
Ni(NO3)2 dissolved in the least amount of distilled
water, dried and then calcined at 500
C for 5 h. The
amounts of dopant added, expressed as mol% CeO2
were 1, 2 and 4. The chemicals employed Ni(NO3)2,
Al(OH)3 and cerium nitrate were of analytical grade
supplied by BDH company, analar cumene was supplied
by Merck.
The calcined samples were exposed to different doses
of g-rays using a 60Co source. The doses were 0.2, 0.4,
0.8 and 1.6 MGy at a dose rate of 2.7  107 MGy s1.
The irradiated samples were left 2 weeks in sealed tubes
before the different measurements were carried out.
The reduction of the investigated samples was done by
heating at 400
C in a current of hydrogen owing at a
rate of 30 ml min1, followed by cooling to the reaction
temperature of the catalytic reaction. The reduction
process was conducted for 1 h.
2.2. Techniques
An X-ray powder diffraction was conducted over pure
and variously doped solids precalcined at 500
C and
also those exposed to g-irradiation using a Shimadzu
diffractometer type (D-D1). The patterns were run with
( at 60 kV
nickel-ltered copper radiation (l 1:5405 A)


and 25 mA with a scanning speed of 8 in 2y min1.
The specic surface areas of the various prepared
catalyst samples were determined from nitrogen adsorp-

3.1. XRD investigation of different solids

The X-ray diffractograms of pure, doped and girradiated samples precalcined at 500
C and being
reduced by hydrogen at 400
C in a current of hydrogen
were determined. The diffractograms obtained (not
given) show the amorphous nature of the different
investigated solids.
3.2. Specific surface area of different investigated solids
The BET surface areas of different investigated solids
were determined from nitrogen adsorption isotherms
conducted at 196
C. The computed values of SBET ;
which represent the specic surface areas of both NiO
and Al2O3 support material are given in Table 1. It is
clearly shown from this table that both CeO2 doping and
Table 1
Specic surface areas of different investigated solids precalcined
at 400
C
Dopant concentration
(mol% CeO2)

Dose of
g-rays (MGy)

SBET (m2 g1)

0.0
2
4
8
0.0
2
4
8
0.0
2
4
8
0.0
2
4
8

0.0
0.0
0.0
0.0
0.4
0.4
0.4
0.4
0.8
0.8
0.8
0.8
1.6
1.6
1.6
1.6

153
160
164
168
170
172
180
185
192
194
199
203
210
215
227
232

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G.A. El-Shobaky et al. / Radiation Physics and Chemistry 69 (2004) 3137

g-irradiation of Ni/Al2O3 system brought about a

measurable progressive increase in its SBET surface to
an extent proportional to the amount of dopant added
and the irradiation dose of g-rays. Similar results have
been reported by El-Shobaky et al. (1997, 1998, 1999,
2000) for CuOZnO/Al2O3, Cr2O3/Al2O3, Fe2O3
Cr2O3/Al2O3, CuO/MgO systems and by Doheim et al.
(2001a, b) for Co3O4/Al2O3 and ZnO-doped Co3O4/
Al2O3 systems. CeO2 doping of CuO/Al2O3 system has
been reported by El-Shobaky et al. (2001) to increase its
specic surface area. This increase has been attributed to
an effective decrease in the crystallite size of particles of
doped solids.

0.0 MGy
0.4 MGy

0.8 MGy
1.6 MGy

% Conversion

95

75

55

35
250

300

350
Temperature C

400

Fig. 1. Effect of g-irradiation on the total conversion for the

catalytic reaction conducted over pure catalyst samples.

(a)

0.0 MGy

Preliminary experiments showed that unreduced

NiO/Al2O3 solids exhibited no catalytic activity in
cumene hydrocracking. So each catalyst sample was
reduced by heating at 400
C for 2 h in a current of H2
owing at a rate of 20 ml min1. The reduced samples
were then cooled to the reaction temperature which
varies between 250
C and 400
C.
The effects of CeO2 doping, g-irradiation and both of
them on its activity and selectivity of the investigated
system in hydrocracking of cumene are represented
graphically in Figs. 17. Inspection of these gures
shows the following: (i) Ethylbenzene represents the
main reaction product of the catalyzed reaction conducted over the different investigated solids, together
with different amounts of toluene, benzene and gaseous
hydrocarbons (C1C3). (ii) The selectivity towards ethylbenzene formation decreases progressively by increasing
the reaction temperature. (iii) The selectivity towards
benzene and gaseous hydrocarbons formation increases
progressively by increasing the reaction temperature. (iv)
g-irradiation of pure Ni/Al2O3 solid brought about a
progressive increase in the percentage of total conversion measured at different reaction temperature. (v) This
treatment led to an increase in its selectivity towards
benzene formation. (vi) CeO2 doping of the investigated
system led to a progressive decrease in its catalytic
activity. This treatment brought about also an increase
in the selectivity towards ethylbenzene formation.

1.6 MGy

0.0 MGy

300
350
Temperature C
0.4 MGy

0.8 MGy

10
5
0
300
350
Temperature C

1.6 MGy

5
0
250

(b)

1.6 MGy

0.8 MGy

15
10

400

15

250

0.4 MGy

20

0.0 MGy
% Selectivity

% Selectivity

0.8 MGy

50
40
30
20
10
0
250

(c)

0.4 MGy

3.3. Catalytic activity and selectivity of different solids

towards cumene hydrocracking

% Selectivity

% Selectivity

0.0 MGy

33

400

0.4 MGy

0.8 MGy

400

1.6 MGy

100
80
60
40
20
0
250

(d)

300
350
Temperature C

300
350
Temperature C

400

Fig. 2. (a) Effect of g-irradiation on the selectivity towards the ethylbenzene formation for the catalytic reaction conducted over pure
catalyst; (b) g-irradiation on the selectivity towards the toluene formation for the catalytic reaction conducted over pure catalyst;
(c) g-irradiation on the selectivity towards the benzene formation for the catalytic reaction conducted over pure catalyst; and
(d) g-irradiation on the selectivity towards the gases formation for the catalytic reaction conducted over pure catalyst.

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G.A. El-Shobaky et al. / Radiation Physics and Chemistry 69 (2004) 3137

34
0.0 mol%

1 mol%

2 mol%

Cumene hydrocracking reaction proceeds in contact

with nely divided metallic nickel particles yielding
different reaction products, the formation of these
products takes place according to

4 mol%

% Conversion

100
80
60
40

(a)
0.0 mol%

300
350
TemperatureC
1 mol%

400

C6 H5  CHCH3 2

- C6 H5  CH3 gases;

2 mol%

Cumene

4 mol%

Toluene

C6 H5  CHCH3 2
Cumene

120
% Conversion

- C6 H5  CH2  CH3 gases;

1
Ethylbenzene

20
0
250

- C6 H5 gases:
Benzene

100

Toluene can also be produced via:

80
60

C6 H5  CH2  CH3
Ethylbenzene

40
20
0
250

(b)

C6 H5  CHCH3 2
Cumene

300
350
TemperatureC

C6 H6 CH4
Benzene

400

Fig. 3. (a) Effect of dopant concentration on the total

conversion for the catalytic reaction conducted over the
CeO2-doped catalyst sample; and (b) effect of 1.6 MGy dose
of g-rays on the total conversion for the catalytic reaction
conducted over the CeO2-doped catalyst sample.

0.0 MGy

- C6 H5  CH3 gases;
Toluene

- C6 H5  CH3 :
Toluene

Benzene can also be produced via:

C6 H5  CH2  CH3
Ethylbenzene

1 mol%

2 mol%

- C6 H6 gases;
Benzene

4 mol%

% Selectivity

50
40
30
20
10
0
250

% Selectivity

0.0 MGy

350

400

1 mol%

2 mol%

4 mol%

80
70
60
50
40
30
20
10
0
250

(b)

300

Temperature C

(a)

300

350

400

Temperature C

Fig. 4. (a) Effect of dopant concentration on the selectivity towards the ethylbenzene formation for the catalytic reaction conducted
over CeO2-doped catalyst; and (b) effect of 1.6 MGy dose of g-rays on the selectivity towards the ethylbenzene formation for the
catalytic reaction conducted over CeO2-doped catalyst.

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G.A. El-Shobaky et al. / Radiation Physics and Chemistry 69 (2004) 3137

0.0 MGy

1 mol%

2 mol%

35

4 mol%

% Selectivity

20
15
10
5
0
250

300

0.0 MGy

% Selectivity

350

400

Temperature C

(a)

1 mol%

2 mol%

4 mol%

14
12
10
8
6
4
2
0
250

300

350

400

Temperature C

(b)

Fig. 5. (a) Effect of dopant concentration on the selectivity towards the toluene formation for the catalytic reaction conducted over
CeO2-doped catalyst; and (b) effect of 1.6 MGy dose of g-rays on the selectivity towards the toluene formation for the catalytic reaction
conducted over CeO2-doped catalyst.

% Selectivity

0.0 MGy

1 mol%

2 mol%

4 mol%

12
10
8
6
4
2
0
250

300

350

400

Temperature C

(a)

0.0 MGy

1 mol%

2 mol%

4 mol%

% Selectivity

15
10
5
0

250
(b)

300

350

400

Temperature C

Fig. 6. (a) Effect of dopant concentration on the selectivity towards the benzene formation for the catalytic reaction conducted over
CeO2-doped catalyst; and (b) effect of 1.6 MGy dose of g-rays on the selectivity towards the benzene formation for the catalytic
reaction conducted over CeO2-doped catalyst.

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G.A. El-Shobaky et al. / Radiation Physics and Chemistry 69 (2004) 3137

0.0 MGy

1 mol%

2 mol%

4 mol%

% Selectivity

100
80
60
40
20
0
250

(a)

0.0 MGy

300
350
Temperature C
1 mol%

2 mol%

400

4 mol%

% Selectivity

80
60
40
20
0
250
(b)

300
350
Temperature C

400

Fig. 7. (a) Effect of dopant concentration on the selectivity towards the gases formation for the catalytic reaction conducted over
CeO2-doped catalyst; and (b) effect of 1.6 MGy dose of g-rays on the selectivity towards the gases formation for the catalytic reaction
conducted over CeO2-doped catalyst.

C6 H5  CH3
Toluene

- C6 H6 gases:
Benzene

The formation of benzene according to reaction (3)

requires breaking of the bond between benzene ring and
the attached side chain, such process needs relatively
high energy greater than that needed to break a bond in
the side chain itself. The bond energies of these two
bonds are 406.3 and 286.6 kJ mol1, respectively (Benson, 1976). So, reaction (3) might occur over the most
active sites. While reactions (1) and (2) leading to the
formation of ethylbenzene and toluene, respectively,
might take place over less reactive sites. However,
ethylbenzene formation seems to be more probable than
the formation of toluene.
The observed changes in the catalytic activity and
selectivity of Ni/Al2O3 due to CeO2 doping and girradiation could be discussed in terms of the reduction
of NiO for the formation of the Ni metal (active
component in the cracking reaction). It has been
reported that CeO2 doping of the transition metal
oxides creates anion vacancies susceptible for oxygen
chemisorption. These vacancies act as oxygen storage. It
seems that CeO2 doping of the investigated system
which could create vacancies susceptible to chemisorb
oxygen from atmosphere hindering the reduction
process of the doped system to yield metallic Ni phase

(active site for cumene hydrocracking reaction). So, the

progressive decrease in the catalytic activity due to
doping with increasing amounts of CeO2 might reect a
progressive decrease in the concentration of metallic Ni
sites. The selectivity towards the formation of ethylbenzene decreases progressively by increasing the dopant
concentration, and increases by increasing reaction
temperature due to the presence of two methyl groups
in the side chain (El-Shobaky et al., 2001; Wei and
Stephanopoulos, 1995).

4. Conclusions
The results obtained lead to the following main
conclusions:
1. XRD-investigation of 0.1 Ni/Al2O3 system showed
its amorphous nature.
2. CeO2 doping and g-irradiation of Ni/Al2O3 increased
the specic surface area in proportion to the amount
of dopant added and the dose of g-irradiation.
3. CeO2 doping of the investigated solids brought about
a signicant decrease in their catalytic activities in
hydrocracking of cumene. The hydrocracking of
cumene led to the formation of ethylbenzene as a

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G.A. El-Shobaky et al. / Radiation Physics and Chemistry 69 (2004) 3137

major product with variable amounts of toluene,

benzene and gaseous hydrocarbons (C1C3).
4. g-irradiation, on the other hand, increased in the
catalytic activity of the treated solids.
5. g-irradiation of the CeO2-doped solids resulted in a
net decrease in the catalytic activity of the treated
solids.
6. The selectivity of the investigated system towards the
formation of various reaction products was strongly
dependent on the reaction temperature, CeO2 doping
and g-irradiation.

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