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Water scarcity and pollution rank equal to climate change as the most urgent environmental turmoil for the
21st century. To date, the percolation of textile efuents into the waterways and aquifer systems, remain an
intricate conundrum abroad the nations. With the renaissance of activated carbon, there has been a steadily
growing interest in the research eld. Recently, the adoption of titanium dioxide, a prestigious advanced
photo-catalyst which formulates the new growing branch of activated carbon composites for enhancement
of adsorption rate and discoloration capacity, has attracted stern consideration and supports worldwide.
Conrming the assertion, this paper presents a state of art review of titanium dioxide/activated carbon
composites technology, its fundamental background studies, and environmental implications. Moreover, its
major challenges together with the future expectation are summarized and discussed. Conclusively, the
expanding of activated carbons composites material represents a potentially viable and powerful tool,
leading to the plausible improvement of environmental conservation.
2010 Elsevier B.V. All rights reserved.
Contents
1.
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.
Emergence of textile waste towards the public health and environmental concern . . . .
3.
Denition, physiochemical properties and historical study of the titanium dioxide . . . .
4.
Revolution of titanium dioxide/activated carbon composite materials in the dye treatment
5.
Characterization, surface science study and mechanism chemistry . . . . . . . . . . . .
6.
Major challenges and future prospects . . . . . . . . . . . . . . . . . . . . . . . . .
7.
Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
1. Introduction
Over the past several decades, the exponential population and
social civilization expansion, changes afuent lifestyles and resources
use, and continuing progress of the industrial and technologies has
been accompanied by a sharp modernization and metropolitan
growth [1]. Hitherto, the deleterious disruptions of the textile waste
seepage, specically governed by the precipitation, irrigation, surface
runoff, rainfall, and groundwater intrusion, has intensied numerous
threatening deteriorations towards the public health and food chain
interference. In the formal practice, it was a convenient way to dispose
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130
131
131
132
136
141
142
142
142
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
131
directly into water channels, that constitutes an accumulative, persistent, carcinogenic, mutagenic and detrimental impact towards the
survival of aquatic compartments, ora, fauna and environmental
matrix (water and soil) [19]. The real hazard setting aside aesthetic
considerations is exacerbated when coloured agents interfere with the
transmission of light (reection and absorption of sunlight), retard
photosynthetic activities, inhibit the growth of biota terrestrial
ecosystems, affect the symbiotic process, damage the quality of the
receiving water courses and impede the propagation of algae, thus
upsetting biological processes within streams, riding to the bilateral
environmental agenda shifted [20].
Additionally, fairly intensive studies has inferred that such colored
allergens may undergo chemical and biological assimilations, eutrophication, consume dissolved oxygen, prevent re-oxygenation in
receiving streams and have a tendency to sequester metal ions
accelerating genetoxicity and microtoxicity [21]. In a wider sense,
sporadic and excessive exposure to coloured efuents is susceptible to
a broad spectrum of immune-suppression, respiratory, circulatory,
central nervous and neurobehavioral disorders presage as allergy,
autoimmune diseases, multiple myeloma, leukemia, vomiting, hyperventilation, insomnia, profuse diarrhea, salivation, cyanosis, jaundice,
quadriplegia, tissue necrosis, eye (or skin) infections, irritation to
even lung edema [22].
3. Denition, physiochemical properties and historical study of
the titanium dioxide
In general, titanium dioxide (also dened as titanium (IV) oxide or
titania) is the naturally occurring oxide of titanium, notably exists in
the crystalline allotropes of rutile, anatase and brookite, or unique
metastable modications of -PbO2, baddeleyite, cotunnite, monoclinic, tetragonal and orthorombic baddeleyite structures [2325].
Crude titanium dioxide is typically extracted from minerals ilmenite,
leucoxenes ores, rutile beach sands, and commercially synthesized via
sulphate (digestion of ground slag or ilmenite with strong sulphuric
acids subsequent by hydrolysis and precipitation) [Eqs. (1)(3)] and
chloride (calcination of synthetic rutile, coke and chlorine, subsequent
by condensation and heating in hot oxygen) [Eqs. (4)(5)] processes
[26,27].
FeTiO3 2H2 SO4 TiOSO4 FeSO4 2H2 O
heat
132
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
Table 1
Advantages and drawbacks of current methods of dye removal from industrial efuents
[61].
Physical/chemical Method description
methods
Fenton reagents
Membrane
ltration
Ion exchange
Electrokinetic
coagulation
Addition of ferrous
sulphate and ferric
chloride
Fig. 1. Bulk crystalline structures of the rutile (a), anatase (b) and brookite (c) type
titanium dioxide [32].
Advantages
Ozonation
Photochemical
NaOCl
Electrochemical
destruction
Activated carbon
Regeneration: no
adsorbent loss
Economically
feasible
Disadvantages
Sludge
generation
Short half-life
(20 min)
Formation of
by-products
Release of
aromatic
amines
High cost of
electricity
Regeneration
difculties
Concentrated
sludge
production
Not effective
for all dyes
High sludge
production
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
133
Fig. 2. The role of activated carbon in enhancing the concentration of contaminant molecules [77].
134
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
Table 2
Physiochemical properties couple with the preparation method of titanium dioxide/activated carbon composite materials.
Preparation
method
Chemical co-precipitation
Dip-hydrothermal
Surface area
(m2/g)
373.56
1060
Pore volume
(cm3/g)
Remarks
Reference
0.21
Coated with magnetic activated carbon in the Fe3O4/activated carbon/TiO2 ratio of 1:5:12.
Prepared by dispersing magnetic activated carbon with titania sols in an ultrasonic bath for
1 h subsequent by drying in a rotatory evaporator under vacuum at 75 C.
Prepared by dissolving H2TiO3 in the mixture solution of H2O2 and NH4OH (hydrothermal
treatment), subsequent by drying at 120 C for 2 h and calcinations at 400 C.
Synthesized by dissolving 50 mL titanium butoxide [Ti(OC4H9)4] in 200 mL ethanol,
followed by vigorous stirring with deionized water and nitric acid and heat treatment at
200 C in atmosphere.
Synthesized by coated sonicated TiO2 suspension onto support (activated carbon) subsequent
by evaporation in an oven at 100 C.
Precipitation of TiO2 particles onto the surface of poly(vinyl butyral) (PVB) through
hydrolysis of tetraisopropyl orthotitanate subsequent by carbonization under the ow of
carbon dioxide at 700 C.
Mechanical mixing of anatase powder with poly(vinyl alcohol) (PVA) and heating at 700 C
with a heating rate of 10 C/min for 1 h under the ow of nitrogen gas.
Continuous stirring of activated carbon and 15 mL titanium tetraisopropoxide, with the
droping of water for 24 h, subsequent by drying in vacuo at 50 C for 24 h and 600 W
microwave treatment for 3 h.
Hydrolysis of TiCl4 with saturated water vapor at 298 K, subsequent by calcinations with
viscose rayon-based activated carbon at ambient pressure in a stream of argon gas at
different temperatures for 1.5 h.
Impregnation of 5 g activated carbon powder with 30 mL of titanium isopropoxide solution
in 30% isopropyl alcohol during 12 h, and calcinations under static air at 325 C for 5 h.
Impregnation of activated carbon with the mixed suspension of 5 g TiO2 and 120 ml acetone
solution containing 1.18 g epoxy, followed by drying at room temperature and calcinations
at 460 C for 2 h in the ow of nitrogen.
Chemical composition of the starting alkoxide solution was Ti(OC4H9)4/C2H5OH/H2O/NH(C2H4OH)2
in a 1:25.6:2:2 molar ratio.
Prepared by dissolving tetrabutyl orthotitanate and diethanolamine (2.6 ml) in 64.82 ml
of ethanol subsequent by immersion with activated carbon grains, and heat-treated at 250 C
for 2 h in air and 500 C in nitrogen for 2 h.
Prepared by immersion of several pieces of activated carbon bers into the mixed solution of
titanium tetrapropoxide, hydrochloric acid, and ethanol under stirring, subsequent by 7 days
aging at 25 C, and calcinations in N2 at 500 C for 2 h.
Synthesized by dissolving 0.1 mol of Ti(OC3H7)4 and activated carbon additives in 200 ml
of ethyl alcohol, stirred magnetically for 30 min, with the addition of 1.56 ml of nitric acid and
calcinations at 300 C in the ow of air for 2 h.
Prepared by continuous stirring of the mixture of activated carbon powder (200 mg) and TiCl4
(25 mL) in an aqueous solution [(NH4)2SO4, HCl and water (1:2:10 by mol)] for 30 min, heated
at 98 C at a rate of 5 C/min for 1 h, aging at room temperature for 10 h, and heated in an N2
atmosphere to 500 C at 20 C/min for 2 h.
Synthesized by SBA-15 as a silica template and furfuryl alcohol as a carbon precursor, calcinated
at 700 C for 2 h in a N2 ow.
Prepared by dispersing 3 g of magnetic activated carbon with 200 ml of titania sols in an
ultrasonic bath for 1 h subsequent by drying in a rotatory evaporator under vacuum at 75 C.
Synthesized by dissolving 17 mL tetra-n-butyl titanate into 30 mL ethanol under vigorous
magnetic stirring for 60 min at room temperature, drop added on 6.4 g activated carbon ber
felt, dried at 80 C and calcined at 600 C for 2 h in nitrogen atmosphere.
Prepared by dissolving Titaniumtetraisopropoxide (TTIP) and acac (2,4-pentadion) in 100 ml
of solvent (EtOH or PrOH) by stirring for 1 h, subsequent by aging at 200 C for 12 h and
calcinations at 200 C for 3 h under aerobic conditions.
Prepared by dispersing 3 g of magnetic activated carbon with titania sols in an ultrasonic
bath for 1 h subsequent by drying in a rotatory evaporator under vacuum at 75 C.
Synthesized by vigorously stirred tetrabutylorthotitanate and diethanoiamine in ethanol for
2 h at 20 C, followed by heat treatment with activated carbon grains at 250 C for 2 h in air,
and 700 C for 2 h in a ow of high purity nitrogen.
Pyrolysis of activated carbon/titanium dioxide under the ow of helium at 0.02 m s 1
[6]
0.52
Solgel
983.0
0.56
Coating
745.0
Pyrolysis
510.8
Coating
170
Solgel
615.0
0.36
Molecular adsorption
deposition
592.9
Solgel
784
Epoxy
504.3
0.05
Solgel
462
0.08
Solgel
845
0.38
Solgel
427.0
Hydrothermal
296.35
Evacuation
813
0.83
Solgel
386.4
0.24
Solgel
555.1
0.31
Solgel
212
0.11
Chemical co-precipitation
373.56
0.21
Solgel
478
0.08
Nanoreactor ash
pyrolysis
Dispersion
680.0
0.61
344.8
0.17
Solgel
2054
1.30
Dip-hydrothermal
1044
0.54
Dip-coating
138.10
Prepared by stirring 5 g of powdered Fe-activated carbon bers with 20 mL of titanium n-butoxide aqueous
solutions for 5 h at 333 K, subsequent by vaporization at 343 K for 1 h and heating at 973 K for 1 h.
Prepared by immersion of activated carbon aerogel monoliths in the TiO2 solgel solution under
vacuum, subsequent by heating under the ow of nitrogen at 1400 C for 4 h.
Synthesized by dissolving H2TiO3 in the mixture solution of H2O2 and NH3H2O (hydrothermal
treatment), stirred with granular activated carbons for 12 h, heating at 180 C for 8 h. dried at 120 C
for 2 h and alcinations at 600 C for 2 h.
Immersion of pretreated activated carbon into 46.4 ml of newly prepared colloidal solution for 5 min,
followed by sonication for 30 min and drying for 7 to 8 h at 373 K.
have been advance by Li et al. [91] and Zhang et al. [63] using the solgel
and atmospheric pressure metal organic chemical vapor deposition (APMOCVD) coated catalysts for the degradation of methyl orange, the
photocatalytic efciency was greatly maintained even after a regeneration of 10 cycles, accomplishing the peak decolouration of 95.4 and
[64]
[65]
[67]
[68]
[69]
[70]
[71]
[72]
[73]
[74]
[75]
[76]
[77]
[78]
[79]
[80]
[81]
[82]
[83]
[84]
[85]
[86]
[87]
[88]
89.0% respectively. The corresponding growth and nucleation rate (APMOCVD) in the uid matrix are expressed as:
Gr = BC S1
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
A
Nr = Sc Fr n exp 3 3 2
k T log S
with Sc, Fr, n, T, Cg/C, Cg, C, k, B and A are devoted to the surface of the
critical germ of nucleus, rate of xation of the dissolved monomer
entities by surface, number of monomer entities by volume,
temperature, super-saturation ratio, concentration of gaseous species
near the growing surface, concentration of gaseous species near to the
solid formed, Boltzmann constant, growth rate constant and nucleation rate constant.
Explicitly, Gao and Liu [5] has attempted to examine the destruction
performance of a solgel suspended catalyst towards the oxidation of
acridine dye and phenol in a uidizing sedimentation container. Under
the irradiation of visible light, the photo-oxidation reaction was driven
primarily by the excitation of dyes, subsequent by electron injection to
the conduction band (cb) of titania forming numerous oxidizing species
(O
2 , OOH and OH radicals) [Eqs. (8)(10)]
Dye hvDye
e
cb O2 N Ti OH O2
10
The extent of effort has proliferated for the next 5 years, and today,
a variety of scientic publications and manifestations covering the
disruption chemistry of textile waste have been executed tremendously (Table 3).
In China, a separated study investigating the discrimination of
methyl orange and methyl blue dyes encompassing the titanium
dioxide naked carbon composite has been individually regulated by Li
et al. [74] and Liu et al. [75] using the hydrolytic precipitation and
hydrothermal calcinations. Degradation of methyl orange dyestuff
was tted well by the mono-exponential curve, suggesting a pseudorst-order homogeneous reaction kinetics behaviour with respect to
the bulk concentration, (C) [Eqs. (11)(12)] LangmuirHinshelwood
kinetic [Eqs. (13)(15)], and contribution combining Langmuir
Hinshelwood and rst order decomposition model [Eqs. (16)(18)]
derived as:
dC
= kapp C
dt
11
135
C
ln 0 = kapp t
C
12
r = k
13
dC
dt
14
=
=k
KC
1 + KC
15
16
17
vMO =
KC C
1 + KC C + i Ki Ii
18
which k, kapp, k1, k2, vMO, vHO, KC, Ki, K and I are referred to the reaction
rate constant, apparent pseudo-rst-order rate constant affected by the
dyestuff concentration, the rst and second-order surface rate constants, fraction of sites covered by methyl orange dyestuff, fractional site
coverage by HO radical, adsorption equilibrium constants and
intermediate products of methyl orange degradation. The hybrid
photocatalyst was demonstrated dominated by the anatase type of
titanium dioxide, while the average size of microsphere crystalline
structure was well estimated using the Scherrer's equation [77]:
L=
K
cos
19
Table 3
Dyes removal via titanium dioxide/activated carbon composite material.
Dyes
Acridene
Reactive red X-3B
Methyl orange
Methyl orange
Mixed colour compounds
Methyl blue
Methyl orange
Methyl blue
Chromotrope 2R
Methyl orange
Methyl orange
Methyl orange
Rhodamine B
Methyl orange
Methyl orange
Indigo carmine
Acid orange II
Removal
(%)
Operating conditions
Reference
Concentration
(mg/L)
Weight of catalyst
(mg)
Solution volume
(mL)
pH
Irradiation/time
96.0
83.0
89.0
95.0
68.2
99.1
89.0
100
81.0
100.0
92.0
95.0
96.0
92.0
95.4
91.1
90.5
4000
500
100
50
2000
800
100
80
1000
120
50
30
120
2300
23
200
`36
200
2000
500
50,000
500
800
250
500
500
75
500
500
30
120
200
1000
250
1000
400
200
100
800
250
250
250
50
250
250
50
100
6.4
7.5
No irradiation/240 min
80 min UV irradiation
60 min UV irradiation
60 min UV irradiation
No irradiation/60 min
180 min UV irradiation
100 min UV irradiation
No irradiation/60 min
120 min UV irradiation
80 min UV irradiation
120 min UV irradiation
60 min UV irradiation
20 min UV irradiation
120 min UV irradiation
120 min UV irradiation
240 min UV irradiation
No irradiation/720 min
Batch
Batch
Column/400 mL/min
Batch
Column/600 mL/min
Column/90 mL/min
Batch
Batch
Batch
Batch
Batch
Column/600 mL/min
Batch
Batch
Batch
Batch
Batch
[5]
[6]
[63]
[64]
[65]
[71]
[74]
[75]
[76]
[77]
[80]
[87]
[88]
[90]
[91]
[92]
[93]
136
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
activated carbon bers with a thickness of about 100 nm. The inner
space between the neighboring adjacent carbon bers connected to the
deposited titanium dioxide particles remained unlled, allowed the
penetration of UV light into the felt-form photocatalyst providing an
ideal passageway for the transport and adsorption of organic molecules
(Fig. 4) [71,73].
Whereas, it was established that small titania aggregates were
uniformly dispersed, creating more reactive sites than agglomerated
particles encapsulated a three-dimensional environment not accessible
by the reactants (Fig. 5) [63]; while catalysts with lower activated
carbon contents (homogeneously covered by titanium dioxide conglomerates) promoted a stronger interphase interaction than larger
activated carbon contents which presented irregularly and lack
discernment in the pore arrangement (Fig. 6) [95]. Nucleation of titania
deposited groove at 400 C appears to be rougher and thicker,
apparently attributed to the preferential formation of anatase nanocrystals spread onto the activated carbon lm; in contrast, as the
calcined temperature was ascended to 800 C, the puckered dispersed
microstructure was gradually destroyed, with several titanium dioxide
fragments broken away from the surfaces (Fig. 7) [80].
Fig. 8 shows transmission electron micrographs (TEM) of the titanium dioxide/activated carbon composites of different magnications.
Spheroidal titanium dioxide nanoparticles with a relatively uniform
Fig. 3. Scanning electron micrograph (SEM) photographs of the titanium dioxide/activated carbon composites (a) prepared at 450 C with titanium dioxide loading of 80 wt.% [76],
(b) coated with solgel method [70], (c) with titanium dioxide/activated carbon in the weight ratio of 2:1 [94], (d) (i) titanium dioxide particles adhered onto activated carbon
surface; (ii) portion enlarged; (iii) showing titanium dioxide particles impregnated up to a few microns depth of activated carbon; (iv) EDAX spectra of highlighted portion [92].
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
137
20
138
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
Fig. 6. SEM images for the 13% activated carbonTiO2 (a), and 37% activated carbon
TiO2 photocatalysts [95].
21
ecb etr
22
hvb htr
23
IV
Ti
IV
(3) Recombination
IV
H2 OOL H Ti OH
IV
H2 OTi H2 O
24
25
26
e h heat
(2) Diffusion
OL Ti
site R1 R1;ads
27
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
139
IV
IV
Ti OH h Ti OH
IV
IV
28
Ti H2 O h Ti OH H
29
30
III
31
R1;ads h R1;ads
IV
Ti
e Ti
III
IV
Ti O2 Ti O2
32
IV
IV
case I Ti OH R1;ads Ti
R2;ads
IV
case III Ti OH R1 Ti
case IV OH R1 R2
33
34
IV
R2
35
36
140
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
Fig. 11. XRD patterns titanium dioxide/activated carbon composited (a) prepared by
MOCVD method deposited at source temperature of 873 K [63], (b) calcinated at
different heat treatment temperature [64].
Fig. 10. Fourier Transformed Infra-red (FTIR) spectrum of the titanium dioxide/
activated carbon composites (a) in comparison to activated carbon and titanium
dioxide [97] (b) with different ratios activated carbon content [77].
IV
IV
IV
e Ti O2 2H Ti H2 O2
IV
Ti O2 H Ti HO2
H2 O2 OH
HO2
H2 O
H2 O2 ecb OH OH
45
39
41
42
2HO2 H2 O2 O2
38
40
2HO2 H2 O2 O2
ne M
44
2OH H2 O2 H2 O O2
O2 H HO2
37
2OH H2 O2
43
46
47
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
141
Fig. 12. X-ray photoelectron spectroscopy (XPS) survey spectrum for the titanium/dioxide/activated carbon supported photocatalyst, (a) overall, and individual lines of (b) Ti2p,
(c) O1s and (d) C1s measured at high resolution [71].
dye hvdye
TiO2 e
48
49
TiO2 e O2 TiO2 O2
H O2 HO2
40
2HO2 O2 H2 O2
41
O2 e 2H H2 O2
H2 O2 eHO OH
50
42
51
Fig. 13. EPR spectra of carbon-doped titania irradiated with different wavelengths of
light [81].
142
K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143
Fig. 14. Conceptual diagram for the primary processes involved in photomineralisation of organic compounds [98].
7. Conclusion
Over the years, the world's giant factories and manufacturing
industries are gradually expanding, driving towards the overwhelming waste generation. Predictions for the next 20 years indicate an
embraced failing of dye processing sectors and subsequently in textile
waste generation. Today, the growing discrepancy and limited success
of remediation in eld applications has raised apprehensions over the
use of titanium dioxide/activated carbon composites material as a
measure to the environmental pollution control. The evolution has
turned from an interesting alternative approach into a powerful
standard technique by offering a numbers of advantages. Although it
is still in the infancy, a widespread and great progress in this area can
be expected in the future.
Acknowledgement
The authors acknowledge the research grant provided by the
University of Science Malaysia under the Research University (RU)
Scheme (Project No. 1001/PJKIMIA/814005) and RU-PRGS grant
scheme (Project No. 8043030).
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