Fuel Processing Technology 162 (2017) 1319

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Fuel Processing Technology

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Research article

Production and characterization of high quality activated carbon from

oily sludge
Jun Wang, Tian-Lu Liu, Qun-Xing Huang , Zeng-Yi Ma, Yong Chi, Jian-Hua Yan
Institute for Thermal Power Engineering, Zhejiang University, 38 Zheda Road, Hangzhou 310027, Zhejiang, China

a r t i c l e i n f o a b s t r a c t

Article history: To convert the hazardous oily sludge into high quality activated carbon for water pollutant adsorption, a new pre-
Received 13 November 2016 paring procedure has been proposed in current study by adding a de-oiling step before activation. The pore struc-
Received in revised form 15 March 2017 ture and surface chemistry of produced active carbons (ACs) were characterized by scanning electron
Accepted 15 March 2017
microscopy, N2 adsorption-desorption, XRD, FTIR and XPS. Due to the high content of asphaltene, oily sludge is
a promising material for activated carbon production. The surface area of the activated carbon prepared with
Keywords:
the proposed de-oiling step was 3292 m2/g which was two times higher than that of normally prepared AC.
Activated carbon Moreover, by applying the de-oiling step, the methylene blue adsorption capacities signicantly increased
Oily sludge from 17.8 mL/0.1 g to 64.6 mL/0.1 g reaching that of ACs generated from commercial asphalt. Moreover, the
High specic surface area heavy metal leaching values of the ACs prepared were far below that of hazardous materials. Therefore, the
Adsorption capability oily sludge could be promising raw material for activated carbon production and the de-oiling procedure could
improve the quality of ACs signicantly.
2017 Elsevier B.V. All rights reserved.

1. Introduction been devoted to producing adsorption carbon material from various

As a result of rapid economic development in recent years, massive
crude oil has been exploited and consumed worldwide [1]. In 2015,
around 500 million tons of crude oil have been consumed in China
and over 3 million tons of oily sludge were generated [2] during the
storage, transportation and rening. Oily sludge is a complex mixture
of water, oil and solid particles with extremely high viscosity. Generally,
approximately 30% to 60% of the oily sludge is oil, 20% to 40% is water,
and the remainder is solid particles. These components are strongly
mixed and sometimes stabilized as emulsion [3]. The oil phase primarily
consists of saturates, aromatics, asphaltenes, and resins [4,5]. In addition
to valuable hydrocarbons, many hazardous and toxic substances are
also presented in oily sludge, including chemical additives, benzene de-
rivatives, heavy metals, and pathogens [6]. Consequently, oily sludge is
classied as hazardous waste in European and China [7] (No. HW08, Na-
tional Catalogue of Hazardous Wastes, 2007, Ministry of Environmental
Protection of the People's Republic of China).
In order to reduce sludge disposal costs and to conserve limited nat-
ural resources, the conversion of sludge into valuable materials has
attracted extensive attention. Porous or activated carbon is widely
used for waste water purication due to its high surface area and ad-
sorption capability. Over the past several years, many researches have
Corresponding author.
E-mail address: hqx@zju.edu.cn (Q.-X. Huang).
sludge feedstock [8,9]. Jindarom et al. [10], Agraoti et al. [11] and Tan
et al. [12] have produced activated carbon from municipal sewage
sludge by pyrolysis. However, the specic surface area of the carbon
particles which they produced ranged from 60 to 90 m2/g which was
relatively low. To improve the adsorption surface, Li et al. [13] mixed
sewage and agricultural sludge (from corn stalks) to prepare AC
through chemical methods and they found that the surface area of the
produced AC could reach 769.0 m2/g at a corn stalk adding ratio of
25.0 wt%. Niasar et al. [14] used petroleum coke as material to prepare
AC with KOH as activator. They reported that due to the high carbon
content of the coke, the products had very high surface area and showed
excellent adsorption performance. Mohammadi et al. [15] studied the
possibility of producing porous carbons from oily sludge by thermo-
chemical treatment and found that the addition of activator could in-
crease the surface area and the pore volume of the product. Anom
Guritno [16] has synthesized porous carbon from oily sludge using
mesoporous silica as template. The elemental analysis results showed
the sludge he used contained 47.10% carbon and the produced porous
carbon was rich in mesopore structure (61% of total pore volume).
Previous research indicated that due to its high carbon content, oily
sludge was potential material for producing AC. However, the reported
adsorption capability of the AC derived from oily sludge was still not
good enough for industrial application. Moreover, the environmental
risks of using oily sludge derived AC in water treatment must be
assessed.

http://dx.doi.org/10.1016/j.fuproc.2017.03.017
0378-3820/ 2017 Elsevier B.V. All rights reserved.
14 J. Wang et al. / Fuel Processing Technology 162 (2017) 1319

Fig. 1. The new procedure for preparing activated carbon from oily sludge.

2. Materials and methods pyrolysis treatment. The de-oiling procedure was based on the different
solubility of heavy asphaltene and other light oil in the solvent. The
2.1. Materials asphaltene contained can be concentrated after the procedure. Other
relatively light oil fraction such as saturates, aromatic species was dis-
Sludge samples were obtained at Zhoushan national crude oil stor- solved into n-pentane with a mass ratio of 1:1 at room temperature
age base located at east of China. Over 50 crude oil tanks are built and removed at a centrifugation speed of 3000 rpm for 10 min. The ef-
there and each tank has a capacity of more than 100,000 m3. Each of fect of this step was evaluated by comparing the properties of AC with or
these tanks will be cleaned every 2 to 3 years to remove bottom sludge. without de-oiling treatment. During the oxidation procedure, the sepa-
The oily sludge used in this paper was collected from two different spots rated product was heated at a heating rate of 2 C/min and maintained
during tank cleaning and mixed before test to make it more representa- at 420 C for 110 min in the air, and then the product was cooled to
tive. The SARA (saturates, aromatics, resins, asphaltenes) content of the room temperature. Then the intermediate product was milled to a par-
oily components were obtained according to the ASTM method D2007- ticle size of less than 2 mm and mixed with solid KOH. The mixture was
02. The water content was determined by ASTM-D95-05 procedure, and carbonized at 400 C for 30 min under nitrogen atmosphere. The prod-
the total hydrocarbon content was derived according to Soxhlet extrac- uct was heated directly from 400 C to 850 C at 4 C/min and held for
tion. The total contents of heavy metals were determined by ICP-AAS. 80 min for the activation treatment. The products were then washed
For comparing purpose, commercial asphalt purchased from China Pet- with deionized water to remove residual alkali and dried at 105 C for
rochemical Corporation was also used as material for AC preparing. 5 h to obtain the nal AC. The activated carbons prepared with and
without de-oiling treatment were respectively ACde-oil and ACoil.
2.2. Modied AC producing procedure All chemical agents used for the AC production, including n-pentane
and KOH, were analytical grade and purchased from the Sinopharm
The AC producing procedure is illustrated in Fig. 1 along with activa- Group Co., Ltd.
tion setups. To remove large solid particles and free moisture, the raw
oily sludge samples were centrifuged at 3000 rpm for 15 min. After cen- 2.3. Active carbon characterization
trifugation, the oily sludge was separated into four layers (light oil,
water, heavy oil and solid particles) and the heavy oil layer was subject- The morphologies of the produced active carbon were assessed by
ed to AC preparation. In current work, the traditional procedure was scanning electron microscopy (SEM, SIRON, FEI Co., Netherlands). The
modied by adding a new de-oiling step, which was used to remove specic surface area and pore structure were determined via nitrogen
light fraction of the oil and enhance the purity of heavy asphalt before adsorption at 196 C by the surface area analyzer (Quantachrome,
Autosorb-IQ2-MP, USA). Before test, the sample was degassed at 300
C for 20 h. The surface area (SBET) was estimated by the Brunauer-
Emmett-Teller (BET) method, while the t-plot method and Barret-
Table 1 Joymer-Hanlenda (BJH) method were used to calculate the micropore
Composition of oily sludge. (Smic) and mesopore (Smec) surface area. The total pore volume (Vtotal)
Composition Sludge sample was obtained based on nitrogen adsorption at a relative pressure (p/
p0) of approximately 0.99. Density functional theory (DFT) were
Water by distillation 23.25 0.93
Water, solid, oil fraction
Solid residues 34.67 4.33
employed to retrieve the pore size distribution [17].
(wt%) X-ray diffraction (XRD) analysis of the AC samples was carried out
Oil by solvent extraction 41.93 3.25
Saturates 27.58 2.66 using an X Pert Pro diffractometer (PANalytical B.V., Netherlands)
Aromatics 29.44 3.53 with a Cu K radiation source. Fourier Transform Infrared Spectroscopy
SARA fraction of oil/(wt%)
Resins 18.23 2.37
(FTIR) of all samples were obtained with a Nicolet 5700 (ThermoFisher
Asphaltenes 24.76 3.81
Cd 16.20 0.30 Co., USA) over the range of 400 to 4000 cm1. X-ray photoelectron
Cu 999.95 476.65 spectroscopy (XPS) was acquired with an X-ray photoelectron spec-
Heavy metal (mg/kg) Pb 51.75 6.05 trometer (VG ESCALAB MARK II, UK) to analyze the surface characteris-
Zn 1706.4 548.8 tics of the AC samples. The binding energies of all core levels were
Cr 69.85 2.25
referenced to the C 1s C\\C bond at 284.6 eV [18].
 J. Wang et al. / Fuel Processing Technology 162 (2017) 1319
Fig. 2. SEM micrographs of (a) ACoil and (b) ACde-oil, samples.
2.4. Methylene blue adsorption test
To evaluate the adsorption capability of the ACs with respect to the
organic contaminants in water phase, methylene blue (MB) adsorption
trials were carried out [19,20]. The MB standard solution (1.5 g/L) was
prepared by dissolving 1.5 g dried MB in 1.0 L of a buffer solution
(14.3 g disodium hydrogen phosphate and 3.6 g monopotassium phos-
phate in 1.0 L deionized water at a pH of approximately 7). MB concen-
trations ranging from 0.3 to 15 mg/L were then calibrated by diluting
the stock solution. In each test, 0.1 g AC sample was mixed with a certain
amount of standard MB solution and then the mixture was stirred at a
Fig. 3. (a) Nitrogen adsorption/desorption isotherms and (b) pore size distribution.
15
constant speed of 200 rpm for 30 min. Then MB concentration was de-
termined by UVvisible spectrophotometer (UV 752 N, Yoke Co., China)
at 665 nm. Prior to analysis, the light intensity for solution with different
MB concentration was calibrated. Samples with MB concentrations over
upper limit were diluted to the calibration range before test.
2.5. Heavy metal leaching
As mentioned in previous reports, when waste derived active carbon
is used for water purication, heavy metal leaching is the most con-
cerned environmental risk as toxic organic compounds have been
destroyed already [21]. In this study, leaching tests were carried out to
evaluate the environmental safety of the AC prepared from sludge
when it is used to adsorb pollutants in water. Prior to analysis, all sam-
ples were prepared according to Toxicity Characteristics Leaching Pro-
cedure (TCLP) of EPA. The concentrations of Cd, Cu, Zn, Pb and Cr
were determined by inductively coupled plasma optical emission spec-
trometry (iCAP6300, Thermo, USA).
3. Results and discussion
3.1. Composition of oily sludge samples
The water, oil and solid fractions of the studied oily sludge, along
with the results of saturates, aromatics, resins and asphaltenes (SARA)
and heavy metal analyses were summarized in Table 1. Around 20% of
the oily sludge was water and the oil fractions were close to 40%,
which was much higher than those of municipal sewage sludge. The
oil components were further analyzed by dividing into saturates, aro-
matics, resins and asphaltenes (SARA). As we can notice, heavy compo-
nents, resins and asphaltene, totally accounted for half of the oil fraction.
Asphalt was reported to be very suitable for producing high quality car-
bon materials [22]. Unfortunately, the heavy metal contents of both bot-
tom and tank cleaning sludge samples were relatively high and the most
enriched metals are cadmium, copper, lead, zinc and chromium espe-
cially for copper and zinc whose concentration exceed 1 g per kg. There-
fore, the leaching concentrations of the active carbon products must be
lower than the applicable regulatory limits.
3.2. Characterization of the active carbon
After pretreatment and activation, the oily sludge samples were
milled into powder for properties analysis. Their micro-structure was
examined and the SEM micrographs are presented in Fig. 2. Results
showed that the surface of the intermediate was consisted of aggregates
of spherical small irregular balls and appeared to be relatively smooth. It
may be caused by the molten sem-coke after pre-oxidation. After car-
bonization and oxidation with KOH, the micro surface of both ACoil
and ACde-oil became fractured and porous. This could be observed in
Fig. 2(b) and (c). It indicated that activation has generated a rugged
16 J. Wang et al. / Fuel Processing Technology 162 (2017) 1319
Table 2
Specic surface area (SBET), total pore volume, and micro pore volume.
Sample SBET(m2/g) Smic(m2/g) Smes(m2/g)
ACoil 1103 1002 101
ACde-oil 3292 3033 259
SBET: BET surface area, Smic: micropore surface area, Smec: mesopore surface area, Vt: total pore volume, Vmic: micropore volume, Vmec: mesopore volume, Dp: average diameter.
structure, which was essential for higher specic surface area. Although
surface of both ACoil and ACde-oil appeared to be similar, the pores of the
ACoil had lamellar structure while the pores of the ACde-oil were more
network-like.
3.3. Specic surface area and pore size distribution
The nitrogen adsorption/desorption isotherms of ACoil and ACde-oil
and the corresponding pore size distribution (PSD) were shown in Fig.
3(a) and (b), respectively. The isotherms of these two AC samples ex-
hibited different adsorption and desorption proles. According to the
International Union of Pure and Applied Chemistry (IUPAC) classica-
tion, it could be classied as typical Type I mixed with Type IV [23].
The Type I isotherm represents micropores, and Type IV demonstrates
mesopores. This result suggested that a small quantity of mesopores
was also generated during the preparation processes. The isotherm pro-
le of ACoil showed that the adsorption quantity increased rapidly at rel-
atively low pressures (close to 0) and then reached plateau rapidly with
increasing pressure. The isotherm of the ACde-oil was similar, but the
adsorbed quantity continued to increase after the sharp rise, demon-
strating a larger amount of mesopores in the carbon network, together
with well-developed porosity.
The pore size distributions were also evaluated by DFT, and the re-
sults were shown in Fig. 3(b). Obviously, the activated carbons had a
narrow pore size distribution (less than 5 nm). Most pores were less
than 2 nm, and the total pore volume for ACde-oil was signicantly larger
than that of ACoil.
The values of BET surface area, total volume, micropore and mesopore
surface area and average diameter were given in Table 2. Both ACoil and
ACde-oil had high porosity and specic surface area values. The specic sur-
face area of ACde-oil (3292 m2/g) was almost two times higher than that of
ACoil, and the micro-porosity value of the ACoil and ACde-oil was 90.8% and
92.1%, respectively. In addition, the specic surface area, total volume, and
micro-porosity of the ACde-oil were all signicantly higher than that of
ACoil. It indicated that the de-oiling procedure could evidently improve
the quality of ACs. The extremely large specic surface area and high
Fig. 4. XRD patterns of ACoil, and ACde-oil.
Vt(cm3/g) Vmic(cm3/g) Vmes(cm3/g) Dp(nm)
0.71 0.56 0.15 2.57
1.85 1.53 0.32 2.24
micro-porosity made the prepared activated carbons to be promising
products with ideal adsorption capacity. Previous study on active carbon
production from tank bottom oil sludge showed that the AC produced
with KOH activation had surface area, total pore volume and micropore
surface area of 328.0 m2/g, 0.21 cm3/g and 289.10 m2/g [15] which
were much lower than that of ACoil and ACde-oil. However, there are also
high specic area active carbons derived from sewage sludge, petroleum
coke, and biomass. Biomass derived porous carbons had the highest BET
surface area of 1994 m2/g [24], highly mesoporous carbon from sawdust
showed specic surface area of 2108 m2/g [25], and 1443 m2/g of AC
from petroleum coke [14]. Most of the active carbons had surface area
lower than the ACde-oil, demonstrating the high quality of the active car-
bon prepared in this work. Besides, the ACoil had surface area over
1000 m2/g which is higher than common sludge based active carbons
[10,11], indicating the potential for oily sludge based AC.
3.4. Carbon existence forms and functional groups
X-ray diffraction (XRD) was used to determine the chemical structure
of the carbon in AC products. FTIR and XPS were employed to identify the
oxygen-containing functional groups on the surface of the samples.
As shown in Fig. 4, The XRD proles of the intermediate showed two
obvious peaks at approximately 26 and 43, demonstrating the pres-
ence of carbonaceous crystalline structure [26]. The (002) plane is asso-
ciated with standard graphite, while the (100) plane corresponds to the
diffractions of graphitic layers [23]. The relative weak and broadened
peak at 26 as showed in ACoil and ACde-oil, indicated that the products
had more irregular amorphous carbon structures after the activation
with KOH. Researches also showed the same rule that the AC activated
by KOH was more amorphous [26]. It could be concluded that the crys-
talline structure of the carbon was destroyed during the chemical acti-
vation process.
The FTIR spectra of ACoil and ACde-oil were illustrated in Fig. 5. The
peaks at 3420.65, and 3424.91 cm 1 were all corresponding to the
O\\H stretching bands of water, alcohol or phenols [27].
Fig. 5. The functional groups analyzed by FTIR.
 J. Wang et al. / Fuel Processing Technology 162 (2017) 1319 17

Fig. 6. The XPS wide scan spectra of AC samples.

Previous studies [2729] have reported that the oxygen-containing

functional groups contained on the surface of AC could inuence its
chemisorption capabilities. Therefore, the abundance of C\\O and
O\\H is an important parameter to evaluate the possible adsorption
capacity.
To assess the effects of the dissolution procedure on ACde-oil, the sur-
face compositions of the AC were determined by XPS. As shown in
Figs. 6 and 7, a strong C 1s peak (284 eV) and an apparent O 1s peak
(533 eV) could be readily identied in the wide XPS spectra. This dem-
onstrated the signicant amount of oxygen in the ACs, which has been
observed in other works [24]. To further explore the surface carbon
and oxygen functional components, the XPS carbon and oxygen peaks
were deconvoluted and the results were plotted in Fig. 7.
As can be seen from Fig. 7, the C 1s spectra of the AC samples
were decomposed into four peaks after deconvolution, located at
284.60.2, 285.1 0.2, 286.4 0.2 and 288.9 0.2 eV which were re-
spectively corresponding to C\\C, C\\O, C_O and O\\C_O functional
band [30]. In the case of oxygen, there were three main peaks centered
at 530.3 0.2, 531.70.2 and 533.1 0.2 eV, which were ascribed to
highly conjugated forms of carbonyl oxygen (O\\I), \\C_O groups
(O-II), C\\OH groups and/or C\\O\\C groups (O-III) [23]. From upper
analysis, the carbon contained in ACoil and ACde-oil was mainly in the
form of amorphous carbon because the area of the 284.6 eV peak was
relatively small. As Fig. 7 shows, the O-I fraction decreased while the
O-II fraction increased after the asphaltene in oily sludge was concen-
trated by the de-oiling procedure. In addition, the spectra in Fig. 6 dem-
onstrated that the oxygen content of the ACde-oil was signicantly
higher than that of the ACoil. This indicated that there were more oxy-
gen-containing functional groups on the surface, giving the ACde-oil a
better adsorption ability and potentially a wider range of applications.

3.5. Adsorption performance

The MB adsorption capacity of AC samples and commercial ACs were

summarized in Table 3. The adsorption value of ACoil was 17.8 mL/0.1 g,
which was slightly lower than that of the commercial AC. However,
considering its high ash content, the performance of ACoil was still
promising.
In this work, commercial de-oiled asphalt was also selected as raw
material for the synthesis of AC, using the same preparation procedure
for comparison purpose. As Table 3 shows, the AC derived from the
de-oiled asphalt had the highest MB adsorption value of 74.7 mL. This
was consistent with the results of previous studies [3133] and sug-
gested that asphalt was a very promising material with regard to the Fig. 7. C 1s spectra and O 1s spectra of ACoil and ACde-oil.
18 J. Wang et al. / Fuel Processing Technology 162 (2017) 1319
Table 3
Comparison of the MB adsorption of sludge-based and commercial ACs.
Adsorbents MB adsorption value (mL/0.1 g)
Commercial wood-based activated carbon 18.7
ACoil 17.8
ACde-oil 64.6
Commercial asphalt based activated carbon 74.7
generation of high quality AC with excellent organic pollutant adsorp-
tion capability. The adsorption value of ACde-oil (64.6 mL) was also
much higher than that of ACoil. One possible explanation was that the
sample was more like commercial asphalt after de-oiling procedure
and the produced ACde-oil was more porous shown in previous SEM g-
ure. This suggested that, the preparation procedure could signicantly
enhance the quality and adsorption capability of the AC. The prepro-
cessing de-oiling procedure using n-pentane employed in the current
study had played a role in improving the pore structure of the AC.
3.6. Heavy metal leaching behavior
According to the Chinese national standard for hazardous materials
identication (GB 5085.3-2007), the corresponding leaching upper
limits for Zn, Cu, Cr, Pb and Cd are 100, 100, 15, 5 and 1 mg/L. The
total heavy metal concentrations in the AC samples were summarized
in Table 1. These results showed that the heavy metal levels in the
raw material were relatively high. In order to be used as water pollutant
adsorbents, the leaching of heavy metals must be below the above
limits, and the leaching amounts of heavy metals from the oily sludge-
based ACs were presented in Table 4. The leaching levels of Zn (0.23
0.35 mg/L), Cu (0.140.26 mg/L), Cr (0.090.11 mg/L) and Pb (0.10
0.13 mg/L) were far below the regulatory limits. The leaching of Cd
was undetectable. It indicated that these ACs could be used as adsor-
bents, since the heavy metals contained in the raw materials have
been stabilized. Research on sewage sludge derived active carbon also
showed that the heavy metal compounds were changed into insoluble
substances and were xed on AC [13]. This demonstrated that active
carbon preparation could stabilize the heavy metal compounds in the
raw materials.
4. Conclusions
A new procedure was proposed in this paper to convert hazardous
oily sludge into valuable active carbon via solvent de-oiling treatment.
The effect of de-oiling on the micro structure and adsorption perfor-
mance of the produced AC particles were discussed. Results showed
that around 30% of the oily sludge collected from crude oil tank was
oil. After de-oiling treatment, the asphaltene was concentrated and
the surface area of the produced active carbon increased signicantly
from 1103 to 3292 m2/g with slightly reduced pore size. The adsorption
ability of ACde-oil (64.6 mL/0.1 g) was over two times higher than that of
ACoil (17.8 mL/0.1 g). Even so, the quality of ACoil was almost the same
with ordinary commercial ACs. Moreover, there was more irregular
amorphous carbon contained in ACde-oil than in ACoil. Both ACoil and
ACde-oil had abundant oxygen-containing functional groups. This dem-
onstrated that the de-oiling procedure could signicantly improve the
quality of AC.
Table 4
Leaching of heavy metals from oily sludge derived ACs.
Heavy metals (mg/L) Zn Cu Cr Pb
GB 5085.3-2007 100 100 15 5 1
ACoil 0.23 0.14 0.09 0.10
ACde-oil 3.56 22.0 0.54 0.04
The disposal of oily sludge requires specialized equipment due to its
hazardous composition. By converting the oily sludge into activated car-
bon, the nal treatment cost can be reduced signicantly. Moreover, the
light oil fraction extracted during de-oiling is also useful.
Acknowledgements
This work was supported by National Natural Science Foundation of
China (Grants 51576172), National Science & Technology Pillar Program
(Grants 2012BAB09B03), National High Technology Research and De-
velopment Program (Grants 2012AA063505), Environment Protection
Special Funds for Public Welfare (Grants 201509013), Program for In-
troducing Talents of Discipline to University (Grants B08026).
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