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Fuel 106 (2013) 147151

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Fuel
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Gasication of coal combustion ash for its reuse as adsorbent


Marco Balsamo a, Francesco Di Natale a, Alessandro Erto a, Amedeo Lancia a, Fabio Montagnaro b,,
Luciano Santoro b
a
b

Department of Chemical Engineering, Universit degli Studi di Napoli Federico II, Piazzale Vincenzo Tecchio 80, 80125 Napoli, Italy
Department of Chemical Sciences, Universit degli Studi di Napoli Federico II, Complesso Universitario di Monte SantAngelo, 80126 Napoli, Italy

h i g h l i g h t s
" Ash gasication for adsorptive properties development was investigated.
" Steam gasication resulted slightly faster than CO2 gasication.
" Both gasication treatments were able to increase the ash porosity.
" A competition porosity development versus thermal sintering effects was observed.
" Gasication ended up in a particle size decrease with respect to the raw ash.

a r t i c l e

i n f o

Article history:
Received 9 June 2011
Received in revised form 2 May 2012
Accepted 22 November 2012
Available online 13 December 2012
Keywords:
Coal ash gasication
Waste beneciation
Adsorbent physico-chemical
characterization
Steam/CO2 treatments

a b s t r a c t
Beneciation through gasication of coal combustion ash coming from an industrial power plant aimed
at its reuse as adsorbent is dealt with. The raw ash was gasied in a tubular reactor at 850 C for times
ranging from 10 to 60 min, using either steam or CO2 as gasifying agent. The relationships among parent
ash properties, gasication treatments and properties of the gasied ash deserve investigation. Therefore,
ash characteristics (such as carbon content, porosimetric, diffractometric, chemical and granulometric
properties) were correspondingly determined. In the light of a critical analysis of the obtained results,
gasication conditions able to make the parent ash a potentially better adsorbent material were dened,
with a particular emphasis on similarities and differences between steam and CO2 gasication. Preliminary results concerning cadmium adsorption onto gasied materials were also reported.
2012 Elsevier Ltd. All rights reserved.

1. Overview
Adsorption is a consolidated technique widely used in many
environmental applications. Activated carbon is the most commonly employed sorbent, but there is a critical concern about the
high unit cost of virgin material and the disposal/regeneration of
exhausted one. In this scenario, non-conventional materials like
industrial residues, natural materials, agricultural by-products
and other biomasses can be used as cheaper alternatives to activated carbon [16]. This work deals with coal combustion ash
(CCA), an industrial residue whose disposal must be limited in
accordance with the issuing of recent specic regulations. Apart
from construction materials industry [7,8] and other possible environmental processes [9,10], adsorption applications are interesting
possibilities for CCA reuse, due to CCA moderately porous structure

Corresponding author. Tel.: +39 081 674029; fax: +39 081 674090.
E-mail address: fabio.montagnaro@unina.it (F. Montagnaro).
0016-2361/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.fuel.2012.11.077

and the presence of both an inorganic matrix and unburnt carbon


which can contribute to the pollutants capture [1121].
The CCA reutilization as adsorbent can take advantage from
proper beneciation techniques, such as chemical modication,
demineralization, gasication, mechanical sieving, pyrolysis,
aimed at improving the physical, chemical and morphological
characteristics of the raw material [6,13,15,18,21,22]. Gasication
is the activation treatment on which this paper is focused: it can
be carried out either with steam or carbon dioxide [23], and involves
the conversion of the CCA unburnt carbon into gaseous products
according to the following endothermic global reactions,
respectively:

CS H2 OG ) COG H2G

CS CO2G ) 2COG

Gasication, generally carried out at temperatures in the range


700900 C, is very effective in the development of ash porosity, as
reported by other authors in the literature [2426]. Nonetheless,

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M. Balsamo et al. / Fuel 106 (2013) 147151

Nomenclature
d50 [lm]
di [lm]
dS [lm]
m [g]
XC []
Xi []

median value of the particle size distribution


particle diameter
mean Sauter particle diameter
sample mass
carbon mass fraction
particles mass fraction

Greek symbols
d [lm] peak of the particle size distribution
n []
burn-off degree
w [mm3 g1] specic cumulative pore volume

issues concerning close relationships among ash properties, gasication treatments and properties of the gasied ash surely deserve
further investigation in order to establish treatment conditions
able to produce a potentially better sorbent. For example, in a recently-published paper [21] in which demineralization and
mechanical sieving were employed as ash beneciation treatments, it was demonstrated that exposed contact surface, porosity
and mineral content of the ash particles have signicant effects on
the adsorption of cadmium from model aqueous solutions.
Following the path drawn in that paper, in this work CCA has
been gasied by either steam or CO2 for different activation times,
and ash characteristics (such as carbon content, porosimetric, diffractometric, chemical and granulometric properties) have been
determined. The aim is to dene gasication conditions to make
CCA suitable as sorbent material, while a parallel investigation is
currently being carried out to characterize the gasied ash adsorption behaviour, whose results will be published in a forthcoming
paper.

2. Experimental
The CCA adopted in this work was generated in an Italian power
plant operated by Enel, and it was characterized in a former work
by Balsamo et al. [21]. CCA was gasied by either steam (Eq. (1)) or
CO2 (Eq. (2)) in an electrically-heated tubular reactor (Nabertherm
R60/750/13, i.d. = 60 mm). The reactor was kept, in both cases, at
the temperature of 850 C. Samples (1 g) of CCA were charged into
the reactor and kept in contact with a stream of either steam or
CO2: steam was generated by feeding liquid water (ow-rate at
room temperature equal to 60 mL h1) through a pump (Stepdos
03RC) to the reactor, while CO2 was fed at a ow-rate of 80 L h1
(at room temperature). It is highlighted that both steam and CO2
ow-rates at the operating temperature (850 C) assume the value
of about 300 L h1. Steam gasication (SG) and carbon dioxide (socalled dry) gasication (DG) were carried out for times equal to
10, 30 and 60 min, giving rise to the following two terns of samples: SG10, SG30, SG60 and DG10, DG30, DG60.
Solid materials were characterized by the following techniques:
(a) carbon content determination by means of a Leco CHN-2000
analyzer; (b) porosimetric analysis, carried out by a mercury intrusion Thermo Finnigan Pascal 240/140 porosimeter operated in the
pore size range 3.7500 nm; (c) X-ray diffraction (XRD), performed
by a Bruker D2 Phaser diffractometer operated at diffraction angles
ranging between 10 and 602h with a scan velocity equal to
0.052h s1; (d) infrared spectroscopy, carried out by a FT-IR 430
Jasco spectrometer operated in the wavenumber range 400
4000 cm1; (e) laser granulometric analysis, performed by a Malvern Instruments Master Sizer 2000 granulometer operated down
to a minimum particle size of 0.02 lm.

Acronyms
CCA
coal combustion ash
DG10
CO2 gasied ash (@10 min, 850 C)
DG30
CO2 gasied ash (@30 min, 850 C)
DG60
CO2 gasied ash (@60 min, 850 C)
SG10
steam gasied ash (@10 min, 850 C)
SG30
steam gasied ash (@30 min, 850 C)
SG60
steam gasied ash (@60 min, 850 C)

3. Results and discussion


The raw CCA was characterized by a carbon content (wet basis)
equal to 23.3%. The evolution of the gasication process was followed by weighing the ash sample before and after reaction, and
by determining the C-content of the gasied ash. This allowed to
calculate the burn-off degree n, alternatively for SG and DG samples, as:
SGDG

mCCA X CCA
 mSGDGXC
C
mCCA X CCA
C

where m is the sample mass and XC is the mass fraction of carbon.


The results reported in Table 1 show that steam gasication was
practically complete after 30 min, and that n = 48% even after
10 min (for the SG10 sample, it was XC = 0.144). Moreover, it can
be observed that the CO2 gasication treatment gave qualitatively
similar results; nonetheless, CO2 gasication was slightly less effective, with n = 98% for DG60 and n = 45% for DG10 (having
XC = 0.151).
Table 1 also reports the values of w, the specic cumulative pore
volume in the pore size range investigated, for the gasied ashes
and (for comparison) raw CCA. Steam and dry gasication produced similar results in terms of: (a) with respect to wCCA = 30 mm3 g1, each gasication treatment was able to increase the
ash porosity; (b) the w-versus-time trend was non-monotonic,
since w reached a maximum after 10 min (w = 63 and 49 mm3 g1
for SG10 and DG10, respectively) to decrease thereafter down to a
nearly asymptotic value for treatment times of 30 min. While the
feature (a) was expected and proved the effectiveness of the ash
beneciation treatment, the interesting feature (b) should be ascribed to a competition between the porosity development during
gasication (see n-values) and thermal sintering effects due to the
longer ash residence time at 850 C. In particular, sintering seemed
to exert a prevailing role in the time range 1030 min, where the
gasication process showed a burn-off increase up to very high values. The results obtained under the present operating conditions
suggested to limit the gasication time to obtain the highest development of the sample porosity without compromising the presence of residual C in the sorbent. Differences when comparing
steam and CO2 gasication arose for total pore volume, at each gasication time, as it resulted wSG > wDG. This resembled the observations already made when discussing about n, leading to the
conclusion that steam gasication (Eq. (1)) was slightly faster than
dry gasication (Eq. (2)). This was already observed in the literature, even if for different operating materials and under different
operating conditions: in particular, for example, Wigmans [23]
and Rodrguez-Reinoso et al. [27] studied the gasication of
carbonaceous materials and a char obtained from olive stones,
respectively, in a wider range of operating temperatures;

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M. Balsamo et al. / Fuel 106 (2013) 147151


Table 1
Relevant parameters for gasied ashes and raw CCA.
n ()

w (mm3 g1)

d (lm)

dS (lm)

CCA

0.233

30

45

10

25

SG10
SG30
SG60

0.144
n.d.
n.d.

0.481
1
1

63
47
45

42

12

DG10
DG30
DG60

0.151
0.011
0.008

0.446
0.966
0.976

49
37
37

42

19

d50 (lm)

Serrano-Talavera et al. [28] investigated the gasication of materials obtained from a Spanish coal pre-treated following several
methods. In all cases, the faster kinetics related to the steam treatment was commonly ascribed to the larger dimensions of the CO2
molecule that would imply a slower gassolid diffusion than in the
case of steam diffusion. It is thus interesting to highlight that similar reasons could be invoked in commenting the results here obtained, even if starting from a material that should be actually
regarded as a coal combustion y ash. Finally, a different porosimetric analysis (carried out by a N2 intrusion Sorptomatic 1990
apparatus able to investigate the microporosity range) did show
that, for all samples, the development of porosity in size ranges
smaller than 2 nm was negligible. The relevance of the build-up
of porosity other than microporosity upon gasication, observed
in this work, is of particular interest for adsorption applications,
as already underlined in the literature [22,24].
On the basis of the previous results, further experiments were
carried out on SG10 and DG10 samples. First of all, the specic surface area was evaluated for SG10 and DG10, and compared with
that of CCA: having as a reference the value of 2.7 m2 g1 for the
raw ash, the gasication treatments ended up into an increase of
this parameter, up to 8.8 m2 g1 (DG10) and 11.8 m2 g1 (SG10),
in accordance with porosimetric data reported in Table 1. Then,
more detailed porosimetric analysis results concerning in particular the pore size distribution in the size range investigated are reported in Fig. 1. Apart from observing, in agreement with Table 1,
that both gasication treatments promoted an increase in CCA
porosity (more marked for SG10 sample), post-processing of data
in Fig. 1, reported in Fig. 2, also revealed that the relevance of pores
in the range 3.710 nm and 10100 nm increased from 1920%
(CCA) to 3741% (gasied samples), and that of pores in the range
100500 nm correspondingly decreased from 61% (CCA) to 19
22% (gasied samples). This highlights the effect of the gasication
treatment not only related to the overall porosity increase, but also

Cumulative distribution, mm g

70
60
50
40
30
20

CCA
SG10
DG10

10
0
0

50

100

150

200

250

300

350

400

450

500

Pore size, nm
Fig. 1. Cumulative pore size distributions for gasied ashes and raw CCA.

CCA
SG10
DG10

60
50
40
30
20
10
0

3.710

100500

10100

Pore size, nm
Fig. 2. Absolute volumetric pore fractions for gasied ashes and raw CCA.

Peak intensity, a.u.

XC ()

Absolute volumetric fraction, %

70

Q
M

M M M M MM

M M

50

55

DG10

SG10

CCA
10

15

20

25

30

35

40

45

60

Diffraction angle, 2
Fig. 3. XRD patterns for gasied ashes and raw CCA. M = mullite, 3Al2O32SiO2;
Q = quartz, SiO2.

to the positive shift of the pore distribution toward ner sizes [24].
Fig. 3 shows XRD patterns for the gasied ashes and (for comparison) raw CCA. It can be observed that the inorganic crystalline
structure of the raw ash (mainly silico-aluminous and based on
quartz and mullite) was fully retained upon gasication, thus
underlining that the only chemical process to take into consideration is, for practical purposes, the steam (or dry) gasication of
the carbon content.
Fig. 4 shows the infrared spectroscopy results for the gasied
ashes and (for comparison) raw CCA. Two main regions could be
recognized: an inorganic and an organic imprint region for wavenumbers in the range 4001400 and 14004000 cm1, respectively. In the inorganic imprint region, CCA was characterized by
four main peaks, centered at 1383, 1090, 560 and 460 cm1,
respectively: peak 1 (related to inorganic carbonate structures),
peak 2 (asymmetric stretching of Al, SiO groups), peak 3 (presence
of Al in aluminosilicates such as mullite) and peak 4 (SiOSi bending) [29,30]. In the same region, infrared spectra for SG10 and DG10
resulted very similar to each other: gasied samples showed again
the peaks 1, 3 and 4, even if characterized by a greater intensity,
highlighting an increase in the ash inorganic fraction promoted
by gasication, as expected. Moreover, the peak 2 (formerly observed for CCA) seemed to deconvolute in the stronger peaks 5
and 6 (centered at 1255 and 1165 cm1, respectively), possibly
due to the high-temperature treatment inducing reticular
distortions. In the organic imprint region, CCA appeared lacking

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M. Balsamo et al. / Fuel 106 (2013) 147151

100

Transmittance, a.u.

DG10

3
4

5
91
8

7
SG10

5
91

6
2

34

CCA
4000

3400

2800

2200

1600

1000

400

Fig. 4. Infrared spectroscopy results for gasied ashes and raw CCA. Marked peaks
are commented in the related text.

5.0

CCA
SG10
DG10

Absolute distribution, %

4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
0.0
0.01

0.1

10

100

1000

Particle diameter, m
Fig. 5. Absolute particle size distributions for gasied ashes and raw CCA.

in signicant peaks (its graphitic structure did not show infrared


signals [31]). On the other hand, both gasied materials were characterized by the band 7 (in the wavenumber range 2820
3000 cm1) and by the peaks 8 and 9 (centered at 1735 and
1454 cm1, respectively). All these signals revealed the role of both
gasication treatments in modifying the ash organic matrix. In particular, the band 7 and the peak 9 could be related to the stretching
and the bending, respectively, of the CH groups [31,32] possibly
generated following the opening of the graphitic aromatic rings
upon steam/CO2 gasication. Finally, the peak 8 would be ascribed
to the stretching of carbonylic groups, formed upon ash partial oxidation following both gasication treatments [30,32].
Figs. 5 and 6 report the absolute and cumulative, respectively,
particle size distributions for the gasied ashes and (for comparison) raw CCA. Relevant parameters are again listed in Table 1. From
the absolute values (Fig. 5), while it is recalled that CCA was characterized by a unimodal distribution having a peak (d) at 45 lm
and a mean Sauter diameter:

70
60
50
40
30
20

0
0.01

0.1

10

100

1000

Particle diameter, m

Wavenumber, cm

X Xi

80

CCA
SG10
DG10

10

dS

Cumulative distribution, %

90

!1

di

for X i mass fraction of particles having diameter di 4


of 10 lm, and that particles coarser than 150 lm were substantially
absent, the following results for the gasied CCA can be underlined:

Fig. 6. Cumulative particle size distributions for gasied ashes and raw CCA.

(a) the absolute distributions for SG10 and DG10, though still unimodal, appeared more polydisperse with respect to raw CCA; (b)
a non-negligible fraction of very ne (smaller than 0.7 lm) particles
was now detectable; (c) both d and dS decreased (down to 42 and
6 lm, respectively) and no differences in these values were observed when comparing SG10 and DG10 (therefore, the exposed
contact surface 6/dS is the same for both SG10 and DG10 particles). While quantitative differences between gasied ashes will
be highlighted looking at the cumulative distributions, it is here
noted that the feature (a) should be ascribed to dishomogeneities
in particle size induced by the gasication treatment, and the feature (b) is due to fragmentation following gasication. Moreover,
the very interesting feature (c) should be analyzed in the light of
the results published in the recent work by Balsamo et al. [21],
where it was observed that the demineralization treatment (associated with a decrease in the inorganic fraction) ended up in an increase of the mean particle size. In this scenario, apart from the
contribution given by the already-noted fragmentation phenomena,
gasication can be considered as the opposite treatment with opposite results, since it led to a decrease of the mean particle size.
Apparently, C-rich particles in the raw CCA sample are the coarser
ones, and this is also in line with the consideration that these char
particles were not able to undergo extensive combustion in the
industrial plant. From the cumulative distributions (Fig. 6) the following values for d50 (i.e., the particle diameter for which 50 wt%
of the material is ner and 50 wt% is coarser) can be observed:
25, 12 and 19 lm for CCA, SG10 and DG10, respectively. Thus it is
underlined that, coherently with data concerning gasication evolution (burn-off) and cumulative porosity, the more extensive
steam treatment was able to give a gasied ash characterized by ner particle sizes.
The considerations hitherto developed should make the steam
gasied ash as the more interesting sorbent for future applications,
even if issues concerning sorbent/sorbate chemical afnity suggest
to investigate both materials (SG10 and DG10) as sorbents for reference pollutants, and to interrelate their adsorption properties
with the characteristics of the materials as obtained in this study.
In this context, explorative adsorption tests were carried out at
room temperature, by contacting the sorbent (either raw CCA or
SG10 or DG10) with a cadmium aqueous solution and analyzing
the specic cadmium uptake under equilibrium conditions,
according to the procedure reported in Balsamo et al. [21]. Experiments showed that the maximum equilibrium adsorption capacity
experimentally observed, around 2.0 mg g1 for CCA, increased up
to 3.2 mg g1 after the gasication treatments. Moreover, cadmium

M. Balsamo et al. / Fuel 106 (2013) 147151

uptake efciency increased by more than 50% for the gasied CCA
respect to that of raw CCA. In spite of the analogies between the
two gasied materials, the cadmium uptake efciency was higher
for DG10 with respect to SG10: in particular, at a pollutant-to-sorbent mass ratio equal to 0.5 mg g1, the efciency was around 96%
and 86% for DG10 and SG10, respectively. This difference can be related to the specic interactions between the cadmium ions and
the two sorbents. At this moment, the very nature of these interactions cannot be deduced only from the chemistry of cadmium and
the physico-chemical and morphological characteristics of the sorbents, thus other information deriving from dedicated adsorption
tests is required. The role played by the gasied CCA properties
in determining the development of the ash adsorptive behaviour
toward a specic pollutant, as cadmium, will be dealt with in detail
in a forthcoming paper.

4. Conclusions
In this work, the gasication of a coal combustion ash, as beneciation treatment for adsorptive properties development, has
been investigated. Steam gasication resulted, under comparable
operating conditions, slightly more effective than carbon dioxide
gasication as far as burn-off degree is concerned: while the former showed a burn-off of 48% after 10 min-gasication and was
practically complete after 30 min, the latter was characterized by
a burn-off of 45% after 10 min and 98% after 60 min. This was related to differences in gaseous molecule size which would make
the CO2 diffusion into the solid matrix slightly slower.
Both gasication treatments were able to increase the ash
porosity (from 30 mm3 g1 to 63 and 49 mm3 g1 for steam and
CO2 treatment, respectively), but it was observed a competition between porosity development upon gasication and thermal sintering effects. This suggested to limit the gasication time to 10 min
in order to maximize porosity while retaining a residual carbon
content in the sorbent. Porosimetric results also revealed that gasication treatments promoted both an increase in the specic surface area and a shift of the pore distribution toward ner sizes.
Infrared spectroscopy analysis on the treated ash showed that
both gasication processes were able to induce the desired partial
oxidation of the parent material.
Particle size distribution analyses revealed, in particular, that
gasication ended up in a decrease of the mean particle size with
respect to the raw ash (this was related to the coarser size of C-rich
particles in the parent material) and that, coherently with previous
data, the more extensive steam treatment was able to give a material with ner particle sizes.
The results obtained in this study will be critically considered in
a forthcoming paper where gasied materials will be used in
adsorption processes for reference pollutants, to interrelate the
adsorption properties with the sorbent characteristics. Preliminary
results reported in this paper and concerning cadmium adsorption
from aqueous solutions showed a relevant increase in both the
adsorption capacity and the uptake efciency when the gasied
ash is compared with the raw ash as sorbent material.

Acknowledgements
The authors thank Enel Produzione Ricerca (Italy) for having
supplied the raw ash, and are indebted with Dr. Massimo Urciuolo
(IRC-CNR, Italy), Dr. Antonio Telesca (University of Basilicata, Italy)
and Dr. Giuseppina Carotenuto (University of Naples, Italy) for
their help in some solid characterization. The authors also
acknowledge Mr. Fabio Magri for his experimental work.

151

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