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Advances in Colloid and Interface Science 159 (2010) 130143

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Advances in Colloid and Interface Science


j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / c i s

Decontamination of textile wastewater via TiO2/activated carbon


composite materials
K.Y. Foo, B.H. Hameed
School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia

a r t i c l e

i n f o

Available online 1 July 2010


Keywords:
Activated carbon
Adsorption
Composites
Textile
Titanium dioxide

a b s t r a c t
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

Corresponding author. Tel.: + 60 604 5996422.


E-mail address: chbassim@eng.usm.my (B.H. Hameed).
0001-8686/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.cis.2010.06.002

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130
131
131
132
136
141
142
142
142

dye efuents by uncontrolled tipping or dumping, an operation in


which waste is spread or released to ll in low economic value open
dumps on selected pieces of land (inundated swampland, abandoned
sand mines and quarries), without taking care of the surrounding
environment, nor considering any precautions to compact, cover and
prohibit the inltration of contaminants into the underlying waterways [2].
Lately, the enforcement of environmental rules and regulations
concerning the monitoring of pollution from industrial efuent waste
streams by regulatory agencies are becoming more stringent and
restrictive, inevitably affect the design, planning, and operation of the
textile emitting industries. This has inspired a growing research in
establishing a leading selective, reliable and durable alternative for
judicious treatment of the heavily polluted dyes entities. In particular,
the potentiality of the titanium dioxide-mediated heterogeneous

K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143

photocatalytic process, exclusively featured by the high reactivity of


hydroxyl radicals for complete elimination of recalcitrant pollutants
and environmental remediation, has become the focus of intense
interest, owning to its synergetic oxidation strength, chemical and
photo stability, super-hydrophilicity, and superior ability for removing a broad range of organic and inorganic pollutants dissolved in
aqueous media, even from gaseous environment [3,4].
Despite its prolic use in pollutant purication, the biggest barrier
of its wide scale application is the cost-prohibitive reaction medium
associated with catalyst suspensions, leaching, settling, dissolution,
oatation and essentiality for eventual separation and recovery of the
ne photocatalyst particles during its post treatment process [5,6].
Realizing the complications, a growing exploration to immobilize,
anchor, embed or disperse titanium oxide photocatalyst onto an inert,
high surface area, well developed porosity, and suitable supporting
matrix (glass, ceramics, polymers silica, alumina, zeolites or activated
carbon) in different arrangements, which reacts as a noble sink
promoting energy and interfacial charge transfer within the particle
pertaining its photocatalytic efciency has been exerted [79]. With
the aforementioned, this bibliographic review attempts to postulate
an initial platform in describing the origin, distinct physiochemical
properties, development and environmental impacts of the titanium
dioxide/activated carbon composite materials. The present work is
aimed at providing a concise and up to date picture of the present
status of the textile waste treatment technologies. The comprehensive
literature together with the challenges and future perspectives has
been highlighted and outlined, to familiarize the knowledge deciencies regarding dyes treatment via titanium dioxide/activated carbon
composites treatment processes.
2. Emergence of textile waste towards the public health and
environmental concern
Since recent era, water pollution control has prevailed to be the most
thrust area and arduous task in the scientic community. Limited
availability of high-quality potable water supplies is forcing the
implementation of in-process water saving measures and advanced
treatment processes for water recycling and scavenging of the industrial
efuents [10,11].
With the escalating demand of the fabric, woven, leather, and
clothing devices, textile industries rank top seat among the most
imperative sources of contamination (dye manufacturing, pulp and
paper, tanneries, cosmetic, coffee pulping, pharmaceuticals, food
processing, electroplating and distilleries) responsible for continuous
perturbation of the environment. In the dyeing section of textile
industry, approximately 1000 L of water is used for every 1000 kg
clothes processed [12,13].
Accordingly, the Environmental Protection Agency (USEPA) has
classied textile wastes into four principal groups, namely the
dispersible, hard-to-treat, high-volume, and hazardous and toxic wastes
[14]. These textile wastewaters are usually a mixture of large complex,
particulates, processing assistants, salts, surfactants, acids and alkalis,
which diverse widely in chemical composition, chemical oxygen
demand and biodegradability, ranging from inorganic compounds to
polymers and organic products. Among different auxiliary compounds
of aquatic ecosystems, dyes (acid, basic, direct, reactive, disperse,
mordant and vat dyes) are a large and signicant group of industrial
chemicals with over 700,000 tons of waste produced annually [15].
Statistically, the total dyes and pigments available commercially is in
excess of 10,000 types and an estimated 10 to 15% of this ends during the
dyeing process [16]; while about 9000 types of them have been
incorporated in the color index [17].
By design, dyes are highly stable molecules; specically resist fading
upon exposure to sweat, light, water, heat and oxidizing agents [18].
Inefciencies in the dyeing sectors generate huge amounts of nonbiodegradable, toxic and inhibitory nature of spent dye baths being lost

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

TiOSO4 TiO2 nH2 O + H2 SO4

heat

TiO2 nH2 OTiO2 nH2 O

TiO2 impure 2Cl2 CTiCl4 CO2

TiCl2 O2 TiO2 pure Cl2

In the perspective, anatase is a 700 thick, transparent, colourless,


mesoscopic, epitaxial, and low temperature (500 C) stable tetragonal
system, characterized by the peculiar aptitude combining good
adsorptive and absorptive properties with respect to ultraviolet (UV)
irradiation, and the predominant morphology of the less orthorhombic
cubic lattice is usually the bipyramidal exposing well-developed (101)
faces (Fig. 1a) [28,29]. Whereas, rutile type titanium dioxide, is a
thermodynamically resistant (1.2 to 2.8 kcal mol 1 more stable than
anatase with temperature ranges from 700 to 1000 C), prismatic (unit
cell is stretched beyond a cubic shape) and needle-like substance,
intimately linked to a band gap energy of 3.0 eV, implying an aggressive
excitation of solar radiation (three-fold enhancement in photocurrents)
(Fig. 1b); while brookite, a rarely form of titanium dioxide that exhibits
no photocatalytic activity is often related to its orthorhombic crystalline
texture (Fig. 1c) [3032].

132

K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143

aqueous cyanide (CN) and sulphide (SO2


3 ) under the irradiation of
sunlight. Since then, the vigor of the titanium dioxide practice has
been well recognized, vigorously widens and entrenched into a
multidisciplinary grouping of physical (windows, tiles, cements,
aggregates, concrete and Portland reinforced materials), chemical
(plastic, food, medicines, drug, cosmetics, sterilizing, deodorizing and
anti-fouling products), biological (gene therapy, dental llings and
latent nger-mark development), engineering (lubricants, advanced
tyres, stain-resistant coatings, glass and photovoltaic industries) and
electronic (semiconductor, electrochemical electrodes, capacitors and
solar cells) frontiers [31,35,36].
4. Revolution of titanium dioxide/activated carbon composite
materials in the dye treatment industries
Within the last few years, intensive wide spread contamination of
atmosphere and surface water related to adverse industrial operations
has attested a fastidious concern for many environmentalists [37]. A
developing research by the invention of a wide variety of treatment
technologies (precipitation, coagulationocculation, sedimentation,
otation, ltration, membrane processes, electrochemical techniques,
biological process, chemical reactions, adsorption and ion exchange)
[3860] with varying levels of success has stimulated a dramatic
progress in the scientic society (Table 1). Of major interest, titanium
dioxide accommodated oxidation, usually a free radical or ultraviolet
mediated disinfection and destructive technology, has currently
emerged to be the most privileged and promising fundamental
approach in wastewater purication and detoxication processes.
Nevertheless, in practical applications, the system design is encountering enormous perpetual fatal limitations associated with aggregation or suspension of ne titanium dioxide powder (especially at high
concentrations), which requires an adequate separation step for
regeneration and recovery of catalyst from the slurry stream [7,62].
Additionally, the photocatalytic reaction is hampered by the
inherent mass transfer and kinetics bottlenecks, low mineralization
rate, high energy consumption, non-uniform and low ratio of light
penetration (scattering) within the treatment unit, thus imposing an

Table 1
Advantages and drawbacks of current methods of dye removal from industrial efuents
[61].
Physical/chemical Method description
methods
Fenton reagents

Membrane
ltration

Oxidation reaction using Effective


mainly H2O2Fe(II)
decolourisation of
both soluble and
insoluble dyes
Oxidation reaction using Application in
ozone gas
gaseous state: no
alteration of
volume
Oxidation reaction using No sludge
mainly H2O2UV
production
Oxidation reaction using Initial and
Cl+ to attack the amino acceleration of
azo-bond cleavage
group
Oxidation reaction using Breakdown
electricity
compounds are
non-hazardous
Dye removal by
Good removal of a
adsorption
wide variety of dyes
Physical separation
Removal of all dye
types

Ion exchange

Ion exchange resin

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].

Ample ancient historical documents, the ordinary black grains of


titanium dioxide, has been rstly discovered by William Gregor
(parish priest) on the beaches of Cornwall, England dating as early as
1790s, which in the 1960, the huge refractive index and prominent
role of titanium dioxide was revealed by two Norwegian chemists,
Jebsen and Farup in Fredrikstad, Norway. Likewise, in the United
States, Rossi and Barton has begun the extraction of titanium dioxide
from minerals ilmenite, titaniferous iron ores and rutile, which
eventually leading to the establishment of production site at Niagara
Falls towards the end of the World War I. Until the turn of the 1930s, a
gradually expanding of the uncoated anatase and rutile pigments
factories has been witnessed, driving to the full scale production of
titanium dioxide [26].
The modern chemical age of titanium dioxide was unfolded by the
pioneering research of Fujishima and Honda [33] in 1972, which
expressed the photocatalytic splitting phenomenon of rutile titania
electrode (in the presence ultraviolet) and simultaneously, Frank and
Bard [34] have extended the application for the decomposition of

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

uncertainty for large-scaling of variable water demands [63,64]. This


has prompted to a rapidly growing immobilization of catalyst
supporting particles or carrier surfaces, in the form of ber glass
beads, silica, alumina, zeolites, clay, sand, silica gel, activated carbon
and quartz optical bers, that manipulated through anodization,
electrodeposition, solgel, reactive dc magnetron sputtering, chemical
vapor deposition (CVD), electrostatic sol-spray deposition, aerosol
pyrolysis, metal coating, solvothermal, wet impregnation, hydrothermal (using an aqueous solvent as reaction medium), carbonization,
boil deposition, impregnationdesiccation, direct oxidation, physical
vapor deposition, sonochemical, Micelle and Inverse Micelle method,
microwave and ionized cluster beam (ICB) congurations
[6,31,65,66].
In this respect, the evolution of biphasic titanium dioxide/activated
carbon composite, which intercrossly xed titanium dioxide lm onto
activated carbon surface, has drastically facilitated the alteration of
chemical, physical, microcrystalline structure, chemical bonding and
energy band gap within the titania nanoparticles, narrowing its
electronic properties, improving the optical activity in the visible light
region, and successfully raises the mechanical, thermal, or chemical
migration and sintering effect strengthening its stability and durability
[31,66,84]. Moreover, the incipient titanium dioxide agglomerated
carbonaceous materials are inducing the combining cooperative and

133

quantum efciencies, generate new porous and adsorption centers


approaching contaminant molecules, bring them into close proximity to
the catalytic sites, thus creating a high concentration environment of the
targeted pollutants elevating the degradation rate and capacity (Fig. 2)
[31,76,77,89]. Increasingly, the titania coated photocatalyst is capable of
enhancing the dynamics of photo-induced charges, cause an acidication of the surface hydroxylic preceded with the intermediates
mineralization and detoxication, thereby preventing secondary pollution by the photodecomposition reactions [63,74]. Nonetheless, the
bimodal porosity (macro and micropores) hybrid catalyst could limit
the pore-plugging or pore-blocking of the accessible sites, thus provided
an easy ltering option for recovery and a new route increasing its
repeating circles and widening its applications [31,86,90]. Table 2 lists
physiochemical properties couple with the preparation method of the
titanium dioxide/activated carbon composite materials.
In the dyes processing industry, Fu et al. [71] has endeavoured to
advocate an initial study prepared an activated carbon bers supported
titanium dioxide photocatalyst using the molecular adsorption deposition (MAD) method following by the calcinations at 900 C in a
continuous ow of argon gas. The titanium dioxide mounted derivative
was illustrated retaining the same spatial distribution of the carbon
bers in their unmodied state, signifying a methyl blue removal of
99.1% with its BET surface area of 592.9 m2/g. A year later, similar works

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


Dye TiO2 ecb Dye


IV

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

r = k1 vMO + k2 vHO vMO

16

r = kHO vMO + k1 vMO

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

where L, K, , and are representatives of the crystalline size in nm,


equation constant (usually taken as 0.89), wavelength of the X-ray
radiation (0.15418 nm) and full width at half-maximum of the (101)
plane (in radius) for the peak at 2 = 25.15.
Accordingly, Shi et al. [80] has performed a comparative test
evaluating the decomposition of acid fuchsine and methyl orange
dyes onto a solgel immobilized titanium dioxide/activated carbon
composite. Degradation rate of methyl orange was noted slightly higher,
mainly correlated to the lower pore diameter and molecular size,
occupying the obverse, end and side tropisms of 1.54 nm 0.48 nm,
1.54 nm 0.28 nm, and 0.48 nm 0.28 nm respectively. In the latter
case, Zhu and Zou [65], and Wang et al. [87] have conducted a
discoloration experiment assessing the solgel and dip-hydrothermal
anchored photocatalysts onto numerous types of activated carbons.

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

Type of study/ow rate

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

Result elucidated a consistently raise relationship proportional to the


rises in porosities, surface area and adsorption capacities (activated
carbon), ascribed to a better dispersion of titanium dioxide particles
within the carbon matrix. Subsequently, a tentative research augmenting the photo-oxidation efciency of the dip-hydrothernmal composites, calcinated at different temperature ranges (from 300 C to 800 C)
has abounded by Wang et al. [64]. Composite calcinated at 600 C has
exhibited the best photocatalytic performance, verifying the vital
inuence of average pore size, total pore volume and mesopores surface
area towards the activated carbon agglomerated catalyst.
5. Characterization, surface science study and mechanism chemistry
Morphological studies for enormous types of titanium dioxide/
activated carbon hybrid composites are depicted in Figs. 37. In most
cases, the agglomerated spherical to sub-spherical cubic titanium
dioxide crystals, varying from 5 to 100 nm, fall typically in the range
of nanosize ne particles forming a relatively integrated layer, blocking
some micropores of activated carbons lead to the reduction of specic
surface area (Fig. 3) (ascertained with EDAX microanalysis of the
representative portion of TiO2: AC showing Ti bands) [70,72,92,94].
Meanwhile, rather small clusters of the rib and furrow titanium dioxide
crystals was found sparsely attached to the lm surface on almost all

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

Fig. 4. Scanning electron micrograph images of the titanium dioxide/activated carbon


bers composites (a) with 2000 [73] (b) cross-sectional view with 20,000 [71].

pore size gradient (dark spots corresponding to titanium dioxide


nanoparticles) are well dispersed at the exterior surface in the vicinity of
the macropores forming a thin layer surrounding and partially
stabilizing activated carbon aggregates (Fig. 9). These compounds
exhibit a narrow distribution with diameters between 5 and 8 nm,
where the interplanar distance lies between 0.32 and 0.35 nm
consistent with the lattice spacing of titanium dioxide, proven that the
particles are crystallized rather than amorphous [81,84,96].
Fig. 10 displays Fourier Transformed Infra-red (FTIR) spectrum of the
titanium dioxide/activated carbon composites with different ratios of
activated carbon content. The region between 3200 and 3600 cm 1 is
related to the OH groups of alcohol or phenols on the adsorbent surface,
and a broad band at 1400 to 1600 cm 1 is assigned to the skeleton
vibration of C C groups in the aromatic rings. Similarly, the presence of
COC structure, shows a signal between 870 and 1150 cm 1 and a
broad peak from 400 to 800 cm 1 is corresponds to the bulk titania
skeletal; while an intensive peak at 1060 cm 1 is identical to the TiO
stretching, anticipated the surface conjugations (through oxygen
atoms) between the bulk activated carbons with the TiO bonds
[77,97]. Fig. 11(a) demonstrates distinctive X-ray diffraction (XRD)
patterns of the activated carbon and titanium dioxide/activated carbon
composite derivative prepared by AP-MOCVD technique under a
deposition temperature of 500 C. Peaks at 2 = 25.3, 37.8, 48.0,
53.8, 54.9 and 62.5 detected diffractions (101), (004), (200), (105),
(211) and (204) planes, indicating developed crystallinity of the anatase
state [63,64]. Increasing sintering temperature identied a sharper,
narrower and higher diffraction intensity suppressed the transformation from anatase to rutile structure [Fig. 11(b)], while the mean size of

137

Fig. 5. Top-view SEM photographs of the titanium dioxide/activated carbon composites


prepared from the (a) aggregates, and (b) small titanium dioxide particles deposited at
500 C [63].

crystallite texture is determined from the full-width at half-maxima of


XRD peak using the Scherrer's equation [Eq. (19)].
Fig. 12 illustrates representative Ti2p, O1s and C1s spectrum of the
titanium dioxide coating surfaces. Ti2p spectra is deconvoluted into
two spin-orbit components, Ti2p3/2 and Ti2p1/2 at binding energies
(Gaussian line proles) of 458.6 and 464.4 eV, that assigned to the
fractions of Ti4+ (TiO2), Ti3+ (Ti2O3) and metallic titanium, with a
peak separation of 5.7, 456.7 and 453.1 eV. The obtained spectrum at
O1s has shown three chemical states of oxygen corresponding to TiO
bind of TiO2 [binding energy (B.E.) = 529.7 eV], CO bind of carbon
bers (B.E. = 532.7 eV) and hydroxyl groups (B.E. = 531.6 eV), which
react as an electron donor generating H+ and hydroxyl radicals (OH)
[Eq. (20)].
H2 O TiOTi2TiOH

20

The resolution of C1s has been resolved into four individual


component peaks representing graphitic carbon/CHn (CC and CHn),
ether/hydroxyl (CO), carbonyl (C O) and carboxyl (COOH) groups as
the major peaks, located at binding energies of 284.6, 286.2, 287.1 and
288.2 eV respectively [71].
Fig. 13 depicts electron paramagnetic resonance (EPR) spectra of
the titania synthesized catalyst in air after the irradiation of visible
light. An escalating of the signal intensities proportional to the rises of
wavelengths (up to 550 nm) was noticed, attributed to the increased
photocatalytic activity (radicals formation) due to electron trapping at
the interior sites of the carbon-doped titania [81]. Fig. 14 presents

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].

conceptual reaction pathway of the photocatalytic degradation of


organic molecules diffused to the vicinity of the titanium dioxide/
activated carbon composites surface [98]. Generally, there are 5
essential key steps in the heterogeneous photocatalysis, namely the
(1) photoexcitation; (2) diffusion; (3) recombination; (4) hole trapping
and (5) oxidation [76,93,99104].
(1) Photoexcitation
hv

Fig. 7. Titanium dioxide/activated carbon nanocomposites calcined at (a) 600 C, and


(b) 800 C [80].

TiO2 ecb + hvb

21

ecb etr

22

hvb htr

23

Upon subjected to an input of ultra-band excitation by UV light


with wavelengths below b 411 nm, charge separation within
the electron hole pairs generated on the metal oxide is
induced, promotes a bound electron to the conduction band
(cb) and formation of positive hole in the valence band (vb).

IV

Ti

IV

(3) Recombination

IV

H2 OOL H Ti OH
IV

H2 OTi H2 O

24
25

26

In this stage, pollutant (R), moisture and lattice oxygen (O2


L )
are diffused to the catalyst surface interface forming spatial
bonding with the particles matrix.

e h heat

(2) Diffusion
OL Ti

site R1 R1;ads

27

Excited electrons and holes are recombined dissipating input


energy as heat, get trapped in the metastable surface states, or
react with electron donors and electron acceptors on the
composite surface or within the surrounding electrical double
layer of the charged particles.

K.Y. Foo, B.H. Hameed / Advances in Colloid and Interface Science 159 (2010) 130143

139

Fig. 9. Schematic diagram illustrating distribution of activated carbon onto different


ratios of titanium dioxide/activated carbon [95].

(4) Hole trapping

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

Water molecules (H2O) and hydroxyl groups (OH) are


available as electron donors, react with the migrated charge
carriers (electron pairs) producing highly reactive and strongly
oxidizing hydroxyl radical (HO). Steady-state concentration of
oxygen has a profound effect and often presents as powerful
oxidants scavenging electrons from the conduction band
forming superoxide radical (O
2 ), that provide an additional
pathway capable of totally mineralizing of the dye molecules.
(5) Oxidation
(i) Decomposition of pollutants under different conditions

IV

IV

case I Ti OH R1;ads Ti

R2;ads

case II OH R1;ads R2;ads


Fig. 8. Transmission electron micrographs (TEM) of various titanium dioxide/activated
carbon bers composite samples (a) [96], (b) [84] and (c) [81].

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) Non-productive radical reactions

(ii) Reactions with other radicals

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

(iii) Reduction with metal ions (Mn+) (if present)

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

M metal in its ground state

43

2OH HCO3 CO3 H2 O

46

47

Repeated attacks of the superoxide, hydroxyl and hydroperoxide


(HO2) radicals in the reacting system essentially lead to the degradation
of dye molecules ultimately to carbon dioxide in a secondary autocatalytic dark reaction. Sometimes the reaction is provided with a
continuous supply of hydrogen peroxide, which has a tremendous and
redox potential producing highly polar radicals participate in the
oxidationreduction processes.
On the contrary, under the irradiation of visible light at N 440 nm,
dye molecules are activated by the electron in an upper orbital level
enabling its transportation into the conduction band. The decolorization

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].

is favored by a driving force of the adsorbed oxygen molecules


corresponds to the loss of conjugation of the double bonds within the
whole molecule.


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

The world is currently facing the worst environmental crisis in its


entire history. For the past two decades, the enthusiasm of huge waste

dye TiO2 dye

6. Major challenges and future prospects

50

42

51

dye O2 or O2 or HO peroxide or hydroxylintermediates


degraded or mineralized products

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].

production and the terminology of deliberate dyes exposure has been


one of the rapidly advancing dilemmas, which have attracted greatest
public considerations and spectacular attention towards the recovery of
contamination resources. Arising from the steep development of giant
dyeing factories and processing industries, numerous mitigating tactics
and imperative technologies have drastically been addressed and
confronted to utilize activated carbons and titanium dioxide (or its
integrated technologies) contemplated mainly for textile waste
treatment, in accruing worldwide environmental benet and shaping
the national economy. Although there have been some successful
industrial-scale applications and implications, generally the industry is
still facing various constrictions, the availability of economically viable
technology, sophisticated and sustainable natural resources management, and proper market strategies under competitive markets.
Amidst these shortcomings, the innovation of titanium dioxide/
activated carbon composites has embarked a huge revolution in the
environmental chemistry. Fluctuating upon the alterations of time,
place and context (type of catalyst support, degraded pollutants and
system condition), environmental effectiveness, technological feasibility, social acceptability and economical affordability (chemicals, energy
consumption, treatment facilities, labor, transportation, collection and
maintenance) are usually the key drivers deciding its capability,
reliability and sustainable manner. Parallel to the central principles of
waste management hierarchy, the paradigm shift of individual and
groups recycling, recovering, reuse and reduction (quantity, weight,
volume and toxicity) throughout the waste chain has seen a panacea
and new menu to the waste minimization strategy [105].
Accordingly, the urgency of conceiving and administering of
strategic, corrective and transparent policies, mandates and standards
which governing the collection, transportation, disposal, prevention,
recycling, monitoring, designing and supervision of the textile waste
management ought to be prudently pointed out and well-planned.
Moreover, the sound professional knowledge of creating environmental awareness for adequate nancial provisions, engineering and
operating standards, responsibilities sharing, public participation,
regular opinion survey, site rehabilitation and aftercare maintenance
need to be properly assigned and counteracted [106]. In Malaysia, the
enactment of the Environmental Quality Act of 1974 and the
subsequent formation of the Department of Environment in 1976
was amended in 1985 to include the submission of Environmental
Impact Assessment (EIA) reports on proposed development program to
the Department of Environment (DOE) for approval [107]. Ultimately,
full co-operation and joint venture between different parties (nations,
states, local government, private sector and communities) from
upstream till the bottom line with compatible technologies is a
directive motivation for the race to the end line.

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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