J. Shanghai Jiaotong Univ. (Sci.

), 2012, 17(3): 373-376

DOI: 10.1007/s12204-012-1290-0

Preparation of Benzene Adsorption Materials Using

Waste Activated Alumina
PAN Jin-feng (),

WU Ren-ping (),

CHEN Xiao-juan ()

(College of Material Science and Engineering, Fuzhou University, Fuzhou 350108, China)

Shanghai Jiaotong University and Springer-Verlag Berlin Heidelberg 2012

Abstract: A new type of benzene adsorption material was prepared by using the airtight heat treatment method.
This method can directly transform the organic impurities of the activated alumina waste into carbon with
adsorption capability. The microstructure and carbon content of materials were characterized by scanning electron
microscope (SEM), X-ray diraction (XRD), BET (Brunauer Emmett Teller) surface area analysis and elemental
analysis. The inuences of heat treatment temperature on the properties of the composite materials were discussed.
The benzene adsorption capability of the material was investigated. The experimental results show that the
optimal heat treatment process condition is airtight heating at 400 for 2 h. The resulting sample has carbon
mass fraction of 3.57%, specic surface area of 234.70 m2 /g, pore volume of 0.41 m3 /g, and average pore size of
6.59 nm. The samples show excellent benzene adsorption capability with an adsorption rate of 21.80%.
Key words: waste activated alumina, heat treatment, carbonization, benzene adsorption
CLC number: X 32
Document code: A

0 Introduction
Activated alumina is a porous solid material with
large specic surface area and pore volume, controllable pore distribution, high mechanical strength after forming, and excellent thermal stability. The raw
materials are abundant and low in cost. It is extensively used in dierent elds such as pottery, abrasive,
medicine, absorbent, and catalyst carriers[1-2] . With
the rapid growth of industry, the extensive usage of
all kinds of catalysts and absorbents generates a lot
of wastes, which are usually discarded. Such practice
not only wastes resources, but also causes environment
pollution[3-4] . How to appropriately treat and recycle
the activated alumina wastes is one of the important
topics of environmental protection and the focus of this
paper.
Benzene is one of the primary indoor air pollutants.
It is highly toxic and a potential carcinogen. In the industries, the primary methods of removing benzene include chemical method, smooth accelerant decomposition method and adsorption method[5-8] . In this paper,
a new type of benzene adsorption material was prepared
Received date: 2011-09-25
Foundation item: the Special Fund for 2010 Petty Invention and Petty Creation of Fujian Provincial Development and Reform Commission (No. MFGT[2010]1093),
and the Natural Science Foundation of Fujian Province
(No. 2011J01291)
E-mail: wurenping@fzu.edu.cn

from the activated alumina waste by airtight heat treatment to carbonize the organic impurities. The inuences of heat treatment temperature on the properties
of the materials were discussed and the benzene adsorption capability was investigated in detail. This method
uses industrial wastes to control industrial pollution,
which is highly valuable for environmental protection.
Its process is simple and the cost is low; the resulting
material has excellent benzene adsorption performance.

1 Experimental Method and Process

1.1

Raw Material Treatment and Sample

Preparation
The activated alumina waste particles were washed
in water to remove the surface sediment, and dried in
the oven.
The dried activated alumina waste was loaded into
a crucible with a lid, and then placed in a computercontrolled electric kiln (Model M1231PK CK596,
SKUTT) for airtight heat treatment. The samples were
processed at temperatures of 400, 500, 550, 600, 700
and 800 for 2 h, respectively. Then samples were
cooled naturally.
1.2 Microstructure Characterization
The samples were studied with X-ray diraction
(XRD) (XD-5A, Shimazu) for phase analysis. Automatic specic surface area and porosity degree analyzer (ASAP 2010, MAX) was used for the specic surface area tests. Scanning electron microscope (SEM)

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J. Shanghai Jiaotong Univ. (Sci.), 2012, 17(3): 373-376

A(111) B(222)
A(220) B(440)
B(311) A
A(200) B(400)
B(220)
B(511)
B(111)
800 C

(XL30ESEM, Philips) was employed for the microstructure analysis. And the carbon content was measured by the element analysis apparatus (Vario EL III,
Elementary).
1.3

Characterization of Benzene Adsorption

Properties

700 C
600 C

Static adsorption method was used to study the benzene adsorption. Each of all samples (about 0.5 g, heat
treated at 400800 ) was placed in dierent weighing bottles. Weighing bottles were then immersed into
saturated benzene vapor in an airtight dryer. The temperature was maintained at 30 in the drying oven.
The benzene adsorption rate can be obtained from the
weight gain of each sample.

550 C
500 C
0

A (Al2O3)1.333, B Al2.85O3.45N0.55
Fig. 1

2 Results and Discussion

2.1

XRD Analysis

Figure 1 shows the XRD patterns of all samples at

dierent heat treatment temperatures. The diraction patterns of all samples are similar. Each has
sharp diraction peaks which appear at diraction angle 2 = 37.58, 45.7 , 66.8 . The spectra are consistent to the Joint Committee on Powder Diraction
Standards (JCPDS) card diraction pattern and related literature[9] . The above results suggest that when
the heat treatment temperature is lower than 800 ,
the main crystalline phase in the waste activated aluminum is -Al2 O3 . The carbon component does not
produce any XRD peak because it is amorphous.

Carbon Content and Benzene Adsorption

Performance Analysis
Figure 2 shows the inuences of the heat treatment
temperature on the carbon mass fraction wC and the
benzene adsorption capability. The graphs suggest that
both the carbon content and benzene adsorption rate
of the samples decrease with the higher heat treatment
temperature, especially when the heat treatment temperature exceeds 500 . The graph indicates that carbon loss at higher temperature is correlated with the
decrease of benzene adsorption capability. The carbon
content of the samples directly aects the benzene adsorption performance; higher carbon content leads to
better adsorption capability.

1
400
500
600
700
800
Heat treatment temperature/C
Fig. 2

22
Benzene adsorption rate/%

w(C)/%
2

XRD patterns of the samples at dierent heat treatment temperatures

2.2

400 C
10 20 30 40 50 60 70 80 90
2/()

21

20

19
400
500
600
700
800
Heat treatment temperature/C

Inuence of the heat treatment temperature on the carbon mass fraction and the benzene adsorption capability

Because anthraquinone degradants adsorbed in the

waste activated alumina usually decompose at about

400 , airtight heat treatment is required to avoid

the release of toxic gases into the atmosphere. These

J. Shanghai Jiaotong Univ. (Sci.), 2012, 17(3): 373-376

toxic organic impurities are carbonized directly in the

airtight condition without oxygen. In addition, the
benzene adsorption rate of sample without heat treatment is only 10.56%, while the adsorption rate of the
samples after 400 heat treatment reaches 21.80%,
which is the highest among all samples. Considering
the above results, the optimal heat treatment temperature is 400 . Therefore, we choose the samples after
400 airtight heat treatment for 2 h to do the following analysis.
2.3 SEM Analysis
SEM photographs of samples after 400 heat treatment for 2 h and new activated alumina are shown in

2 m

Acc.V Magn WD Exp

20.0 kV 10000x 6.8 1

2 m

(b) New activated alumina

Fig. 3

SEM photographs of the samples

2.4

Specific Surface Area and Pore Structure

Analysis
N2 adsorption-desorption isotherms of the sample are
shown in Fig. 4; p is the Nitrogen partial pressure; p0
is the standard atmospheric pressure. According to the
classication of International Union of Pure and Applied Chemistry (IUPAC), this is a type IV adsorption isotherm. From the isotherms the specic surface area of the multiphase material is calculated to be
234.70 m2 /g, while the pore volume is 0.41 m3 /g. The
distinct lag ring in the adsorption isotherm can be explained by the mesoporous structure in the materials.

Figure 5 shows the pore size distributions of the sample. Pore size distribution curves are calculated from
the adsorption and desorption isotherms. The particle structure and size of the samples are very complex,
and there are large amount of absorbed substances in
the samples which cause network-stemming. The network eects[10] are taken into consideration in this calculation, which makes the adsorption isotherm much
closer to the real situation. As the graph indicates,
the pore size distribution of micropores of the material ranges from 5 to 9 nm, and the average pore size is
6.59 nm.

250
200

Adsorption
Desorption

150
100
50
0

0.2

0.4

p
p0

0.6

0.8

1.0

N2 adsorption-desorption isotherms of the sample

Pore volume/(cm3g1)

Volume adsorbed/(cm3g1)

Fig. 3. The sample in Fig. 3(a) is composed of a large

number of small particles, and the particle sizes are all
smaller than 1 m, which is similar to the microstructure of new activated alumina shown in Fig. 3(b). Combined with the analysis of XRD in Fig. 1, these particles
can be determined to be -Al2 O3 which has strong adsorption capability. Most of the organic matters have
been carbonized by the airtight heat treatment. However, because of the small charcoal grain size, low content and wide dispersion in the mesoporous activated
alumina, the carbon particles cannot be observed in the
SEM photographs. However, it is known that such ne
carbon particles have the stronger adsorption ability.

Acc.V Magn WD Exp

20.0 kV 10000x 6.9 1

(a) 400 C-2 h

Fig. 4

375

0.08
Adsorption
Desorption

0.06
0.04
0.02

0
Fig. 5

10

20 30 40 50
Pore diameter/nm

60

70

pore size distribution of the sample

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J. Shanghai Jiaotong Univ. (Sci.), 2012, 17(3): 373-376

3 Conclusion
(1) A new type of benzene adsorption material was
prepared from the activated alumina waste by the airtight heat treatment. The heat treatment directly carbonizes the organic impurities. And the benzene adsorption rate of the material can reach over 20%.
(2) The carbon content of material is correlated to
the benzene adsorption ability. The optimal airtight
heat treatment condition is at 400 for 2 h.
(3) The test and analysis results show that the material is composed of a large number of ne -Al2 O3 and
carbon particles, the carbon content of sample is 3.57%,
the specic surface area is 234.70 m2 /g, the pore volume
is 0.41 m3 /g, and the average pore size is 6.59 nm.

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