Desalination 261 (2010) 6772

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Desalination
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 / d e s a l

Crossow microltration using ceramic membrane for treatment of sulphur black

efuent from garment processing industry
Priyankari Bhattacharya a, Shatrupa Dutta b, Sourja Ghosh a,,
Swami Vedajnananda b, Sibdas Bandyopadhyay a
a
b

Ceramic Membrane Division, Central Glass and Ceramic Research Institute, 196, Raja S.C. Mullick Road, Kolkata-700032, India
Department of Chemical Engineering, Heritage Institute of Technology, Kolkata-700107, India

a r t i c l e

i n f o

Article history:
Received 22 September 2009
Received in revised form 14 May 2010
Accepted 17 May 2010
Available online 9 June 2010
Keywords:
Sulphur black efuent
Crossow microltration
Ceramic membrane
Biosorbent
Chemical pretreatment
Permeate ux

a b s t r a c t
Crossow microltration (CMF) using ceramic membrane, developed from a low cost composition of alumina and clay in the tubular multichannel conguration with ltration area of 0.045 m2 was used alone, and
in combination with different physicochemical techniques, viz. adsorption and chemical coagulation for
treatment of wastewater collected from the sulphur dyeing process of a garment processing industry. The
concentrated efuent was enriched with sulphur black dye, with turbidity 5912 NTU and COD of 3910 mg/l.
Adsorptive treatment was carried out using a biosorbent prepared from the roots of an aquatic weed, E.
Crassipes. Chemical pretreatment was carried out using different inorganic coagulants. Effect of different
transmembrane pressures (TMP) in the range of 0.41.2 kg/cm2 was observed and constant pressure ltration
was conducted at 1 kg/cm2 TMP. Performance of the single stage CMF process was compared with that of twostage processes in terms of the permeate quality, viz. COD, color, turbidity and TSS etc. and permeate ux.
Encouraging result was found after microltration of the biosorbent treated feed as well as, efuent pretreated
with aluminium sulphate. Dye removal was about 99%, with 80% reduction of COD. The chemical pretreatment
process considerably increased the permeate ux compared to the single stage process.
2010 Elsevier B.V. All rights reserved.

1. Introduction
Different types of dyes are used in the textile industries. The chemical
structures of dyes vary enormously, and some have complicated aromatic
structures that resist degradation in conventional wastewater treatment
processes because of their stability under exposure to sunlight, oxidizing
agents and microorganisms. Dye containing wastewater usually consists
of a number of contaminants including acids, bases, dissolved solids, high
chemical oxygen demand (COD), toxic compounds, xing compounds
and color. The conventional treatments of wastewater containing dyestuff
include biological oxidation [1], chemical coagulation [24] and adsorption [5,6]. Biological methods are although cheap and simple to apply,
however, dyeing wastewater cannot be readily degraded by the
conventional biological processes. This is due to the complex structures
of most commercial dye compounds and their non-biodegradability. The
other treatment methods include ozonation [7], UV, UV/H2O2 decoloration [8], Fenton's reagent oxidation [9], chemical precipitation and ion
exchange [10] etc. Some of these methods are relatively expensive and
each has its merits and limitations in application. Membrane based
separation processes are gradually emerging as attractive alternative to
the conventional separation processes. However, one of the major

Corresponding author. Tel.: +91 33 2473 3469/76; fax: +91 33 2473 0957.
E-mail address: sourja@cgcri.res.in (S. Ghosh).
0011-9164/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2010.05.029

limitations of the process is a rapid decline of the permeation ux due

to membrane fouling [11,12]. With pre treatment membrane fouling may
be considerably decreased. In the study of Papic et al. [13], combination of
coagulation by Al(III) and adsorption on activated carbon was found very
efcient for removal of reactive dyes. Chakraborty et al. [14] used
adsorption in combination with nanoltration for treatment of textile
dyehouse efuents. In the study of Harrelkas et al. [15], a comparative
study on real dyehouse efuents using combinations of coagulation/
occulation with microltration, ultraltration and adsorption on
activated carbon was carried out.
In the present study the potential of low cost ceramic membranes
indigenously developed by the Central Glass and Ceramic Research
Institute was explored for treatment of highly contaminated wastewater collected from a garment processing unit. The crossow ceramic
membrane module is used primarily for separating colloidal and
suspended particles in the range of 0.0510 m from highly turbid
wastewater at lower operating pressures. The ceramic microltration
membranes have been successfully used for separation of iron and
arsenic from ground water [16]. In this study, a concentrated and toxic
efuent sample of sulphur dyeing process was collected from a factory
located at Mahestala in Kolkata Metropolitan Area. The entire area of
Mahestala is under extreme environmental pollution. This prompted
the present research group to quest for an appropriate green separation
technology to treat dye wastewater for its safe reuse. The porous
ceramic membranes have an excellent chemical, mechanical and

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P. Bhattacharya et al. / Desalination 261 (2010) 6772

Table 1
Characterization of the untreated sulphur black efuent.
pH

Table 2
Characterization of the biosorbent (WHR).

Conductivity TDS
Turbidity Dye concentration COD
TSS
(mS/cm)
(mg/l) (NTU)
(mg/l)
(mg/l) (mg/l)

12.07 36.9

20,200

5912

890

3910

5550

thermal resistance. Crossow membrane ltration was carried out in a

single stage process and in combination with different physicochemical
treatments, viz. adsorption and chemical coagulation. For adsorptive
treatment, a biosorbent was prepared from an aquatic weed. Chemical
pretreatment was carried out with different inorganic coagulants. The
objective of this study was to observe the separation efciency of the
ceramic microltration membrane alone or in combination with the
different physicochemical treatments. Batch scale studies were conducted for selection of the optimum conditions of pH and adsorbent/
coagulant doses during pretreatment. Performance of the two-stage
processes were compared with that of direct ltration of the efuent in
terms of the permeate quality, viz. dye removal, turbidity, total
suspended solid (TSS), COD etc. and the permeate ux.
2. Materials and methods
2.1. Wastewater
Sulphur dyes are one of the most popular dye classes for cellulosic
bers and are considered to constitute the largest class of dyes used in
terms of quantity consumed globally. Sulphur Black 1, in all its forms
(C.I. Sulphur Black 1, C.I. Solubilised Sulphur Black 1 and C.I. Leuco
Sulphur Black 1) is the most important black dye in the world. Sulphur
dyes are made up of high molecular weight compounds, obtained by
reaction of sulphur or sulphides with amines and phenols. The exact
chemical structure is not always known since these are mixtures of
molecules of a high level of complexity. In the present study, sulphur
black efuent was collected from the dyebath which was rich in dye
concentration. The efuent was characterized in terms of color,
turbidity, pH, total dissolved solid (TDS), conductivity, COD, TSS etc.
(Table 1). Turbidity of the samples was measured in a turbidimeter,
[2100AN IS Turbidimeter, Hach]. The pH, conductivity and TDS of
samples were measured using Sension 156 meter of Hach. COD of the
samples was measured using dichromate reux method followed by
titration with standard ferrous ammonium sulphate solution. Absorbance spectra of the samples were measured in a UVVis. spectrophotometer of Perkin Elmer. Particle size distribution of the efuents
was analyzed in a Mastersizer 2000 of Malvern Instruments (Fig. 1).
2.2. Adsorption study
The potential of Eichhornia Crassipes (Water Hyacinth) was
explored for treatment of sulphur black efuent. Eichhornia Crassipes
is a fast growing perennial aquatic weed and can grow in severe

Properties

Quantitative value

Raw material
Bulk density (kg/m3)
Moisture content (%)
Ash content (%)
Surface area (m2/g)
Average particle size (mm)

Roots of E. Crassipes
133
9.6
44
81
0.038

polluted waters. The roots of E. Crassipes was collected and washed

thoroughly in distilled water to remove the impurities. The dried
biomass was powdered and sieved to select particle sizes of about
100 m to use as biosorbent. Characterization of the adsorbent
prepared from water hyacinth root (WHR) is given in Table 2.
Equilibrium studies were continued for 24 h in a temperature
controlled shaker at 200 rpm with 250 ml volume of efuent sample.
Experiments were conducted at different initial pH (412) with a
constant dose of adsorbent (1 g/l) and the effect of the adsorbent dose
(0.52 g/l) was observed. Kinetic study was conducted for 120 min
taking 1000 ml volume of efuent. The raw efuent and the treated
samples were characterized in terms of the dye concentration,
turbidity, TSS, COD, pH, conductivity, TDS etc. The optimum dose of
adsorbent and pH selected from the batch study was used for the
preparation of bulk amount of feed for the membrane ltration study.
2.3. Chemical pretreatment
The chemical pretreatment of the efuent was carried out using
different inorganic coagulants, viz. aluminium sulphate, ferric chloride and a combination of ferrous sulphate and lime, supplied by
Merck. Pretreatment was carried out at various pH (712) and
standard jar test method was used. For the jar test, efuent of 1 L was
transferred into the jar. The pH of efuent was adjusted with 1 N
H2SO4 and 1 N NaOH. After addition of the desired amount of
coagulant, the sample was mixed for 5 min at rapid mixing condition
(200 rpm) followed by slow mixing at 50 rpm for 10 min. Thereafter,
the solution was allowed to settle and the supernatant was collected
after 24 h. Similar to the adsorption study, pretreatment of bulk
volume of the efuent was carried out using optimum dose of the
chemicals and pH based on the results of the jar test.
2.4. Microltration
The CMF unit was tted with porous ceramic membrane prepared
from a low cost composition of -alumina and clay. In this study, the
uncoated porous membrane in tubular multichannel conguration
was used (outer diameter 35 mm, channel diameter 4 mm, 19
channel, length 200 mm, apparent porosity 36%, ltration area
0.045 m2). In Fig. 2, scanning electron micrograph (SEM) of external

Fig. 1. Particle size distribution of sulphur black efuent.

P. Bhattacharya et al. / Desalination 261 (2010) 6772

Fig. 2. SEM image of ceramic membrane surface.

surface of the membrane is shown. Experiments were conducted

taking 5.5 l of feed solution. Different transmembrane pressures
(TMP) were maintained in the range of 0.41.2 kg/cm2 to observe the
effect of operating pressure on the permeate ux. Subsequently,
ltration was continued for 2 h at a constant pressure of 1.0 kg/cm2
TMP. The permeate ux was measured at specic time intervals and
permeate samples were analyzed. After each run, the system was
thoroughly cleaned with deionized water. The ceramic membrane
was cleaned with dilute nitric acid solution and then deionized water.

69

Fig. 4. Effect of pH on turbidity and TSS reduction (WHR dose: 1 g/l).

reduction also (Fig. 4). Reduction of TSS decreased with the increase of
solution pH, at acidic pH TSS removal was 94% which decreased to 84%
at pH 12. Again, turbidity removal was found as pH independent and
over 98% reduction was obtained in the entire pH range studied. Based
on these results, pH 4 was selected as optimum pH for the further
study.

3.2. Effect of adsorbent dose

The effect of initial pH was observed in the adsorption study of

sulphur black efuent, using a xed adsorbent dose of 1 g/l. It may be
observed in Fig. 3 that pH did not have any signicant effect in the
adsorption of sulphur dye and removal of dye was almost constant
(9899%) at all the studied pH values. However, COD reduction by
WHR was inuenced by pH. At low pH, the number of H+ ions
increased. Due to the increase of positively charged surface sites, a
charge neutralization phenomenon occurred which in turn favored
the reduction of COD of efuent. At pH 4, about 68% removal of COD
was obtained, which decreased to about 28% at highly alkaline
condition (pH 12). Almost similar trend was observed for the TSS

In Fig. 5, the effect of WHR dose on the removal of dye and COD
reduction (%) is shown, solution pH was adjusted at 4. At 0.5 g/l dose,
dye adsorption was over 99% which remained constant with increased
doses of WHR. Removal of COD gradually increased with increase of
adsorbent dose and at 1 g/l dose COD reduction was about 68%. This
could be attributed to the increased surface area with availability of
more effective sites for adsorption. However, with further increase of
adsorbent doses no improvement in the COD reduction was observed.
This might be due to overlapping of adsorption sites as a result of
overcrowding of adsorbent particles [17].
In Fig. 6, reduction of turbidity and TSS with variation of the
adsorbent dose is shown. It may be observed that turbidity reduction
was about 99% irrespective of the adsorbent dose. TSS reduction was
maximum (94%) at 1 g/l dose, thereafter it decreased. From these
results optimum dose was selected as 1 g/l which was used in the
further comparison study.

Fig. 3. Effect of pH on dye removal and COD reduction (WHR dose: 1 g/l).

Fig. 5. Dye removal and COD reduction with variation of adsorbent dose.

3. Results and discussion

3.1. Effect of initial pH in adsorption study of efuent

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P. Bhattacharya et al. / Desalination 261 (2010) 6772

Fig. 8. Effect of initial pH on dye removal in the chemical pretreatment study.

Fig. 6. Turbidity and TSS reduction with variation of adsorbent dose.

3.3. Determination of optimum coagulant dose in the chemical treatment

study
The effect of variation of dose of the coagulants is shown in Fig. 7
taking different doses of coagulants (14 g/l). The pH was adjusted at
7 for all the solutions. It may be observed that for aluminium sulphate,
dye removal varied from 95 to 97% with variation of dose from 3 to
1 g/l. Dye removal reduced to 85% at a higher dose of 4 g/l. Hence, 1 g/
l dose was selected as optimum dose for further experiments. For
ferric chloride, dye removal gradually increased from 75% at 1 g/l dose
to 91% at 3 g/l dose. Thereafter, dye removal decreased to 88% at 4 g/
l dose. Therefore, the optimum dose was selected as 3 g/l. For the
combination of ferrous sulphate and lime, an optimum dose was
found as 1.0 g/l of ferrous sulphate and 1.0 g/l of lime. Dye removal
was about 90% at this dose.
3.4. Determination of optimum pH in the chemical treatment study
The effect of pH on the pretreatment was observed by varying the
initial pH of solution from 4 to 10. A constant dose of 1 g/l of each
coagulant was used in this study. It was observed that for aluminium
sulphate, maximum dye removal (97%) was obtained at pH 4 (Fig. 8).
Thereafter removal decreased gradually. Dye removal decreased
sharply in the pH range 8 to 10. When aluminium sulphate is
dissolved in the aqueous solution, the metallic ion (Al3+) hydrates
and is hydrolysed to form various hydrated structures [18]. At pH
values above 3, hydrolysis occurs to form aluminium hydroxide, Al
(OH)3(solid) with large surface areas and positive charges. This

positively charged surface attracts the anionic dye molecules in the

wastewater. Thus at low pH, the charge adsorptionneutralization
mechanism predominates resulting in an efcient color removal. For
ferric chloride, dye removal varied from 76% at pH 4 to 89% at pH 10.
The maximum dye removal (93%) was obtained at pH 6. From Fig. 8 it
may be observed that ferric chloride was effective in a wide range of
pH (610). The performance of dye removal by chemical coagulation
depends largely upon the solubility of the dyes. Sulphur dyes are
found initially in the insoluble oxidized (pigment) form. The low
solubility is attributed to different chemical structures including the
presence of sulde, C O, NH and aromatic groups in the dye
molecules. Therefore, they tend to be adsorbed by Fe(OH)x particles
and 90% dye removal was achieved in a wide range of pH. When
ferric salts are used as coagulants, monomeric and polymeric ferric
species are formed. Ferric species are almost completely insoluble in
the pH range between 4 and 8. Ferric chloride generates ferric
hydroxide particles during hydrolysis. These particles agglomerate
forming macroscopic ocs which are apparently readily adsorbed
onto colloids [19] and small changes in the dye removal efciency was
observed in a wide range of pH (610).
For the combination of ferrous sulphate and lime, the maximum
dye removal (95%) was obtained at pH 4. Thereafter, color removal
decreased gradually with the increase in pH.
3.5. Effect of adsorbent/coagulant addition in the particle size
distribution of the efuent
Particle size distribution (PSD) of the sulphur black efuent was
measured for the untreated efuent and for the adsorbent treated
efuent with WHR of 1 g/l dose at pH 4 and chemically pretreated
efuent using aluminium sulphate of 1 g/l dose at pH 4. In Fig. 9, the
PSD of these three samples is shown combinedly. The volume mean
diameter (D) of the untreated efuent was 17.14 m. The average
particle size was slightly increased after addition of the coagulant
where D value was found as 17.39 m. This is obvious since after
addition of coagulant, formation of ocs occurs which increases in size
gradually during mixing. The positively charged high surface area of
the ocs attracts the dye molecules to be adsorbed and neutralization
occurs. Signicant change in the PSD was observed after addition of
the adsorbent. It may be noted that the average particle size of the
adsorbent was about 38 m. After adsorption of dye molecules by
WHR, the D value of the efuent was increased to 24.39 m from
17.14 m.
3.6. Microltration study

Fig. 7. Dye removal with variation of the coagulant dose in the chemical pretreatment
study.

Membrane ltration of sulphur black efuent was carried out at

various conditions of with/without pretreatment and performance of
the different methods were compared in terms of the permeate

P. Bhattacharya et al. / Desalination 261 (2010) 6772

71

Fig. 9. Particle size distribution of the different samples of sulphur black efuent.

quality and permeate ux. Five types of feed were treated by CMF:
Feed 1: efuent treated with biosorbent (WHR, 1 g/l, pH 4); Feed 2:
efuent treated with aluminium sulphate (1 g/l); Feed 3: efuent
pretreated with ferric chloride (3 g/l); Feed 4: efuent pretreated
with ferrous sulphate (1 g/l) and lime (1 g/l) and Feed 5: untreated
sulphur black efuent. Removal of dye after CMF of untreated and the
pretreated efuents with time was studied (Fig. 10). In CMF study at
constant TMP of 1.0 kg/cm2, the similar trend like that of batch scale
pretreatment study was found. As expected, maximum dye removal
(N99%) was obtained for the WHR treated feed (Feed 1) within 15 min
of ltration. For the aluminium sulphate treated feed (Feed 2) also,
9899% removal of dye was found. For Feed 3, 90% removal of dye was
observed and for Feed 4 it was about 81%. For the pretreated feeds,
steady state was achieved within a short time of CMF and dye removal
was almost constant with time. However, removal of dye was
signicantly less for the direct CMF of efuent. After 15 min, 51%
removal was observed which gradually decreased to about 46% after
120 min.
The removal of COD from permeate samples for the different feeds
of sulphur black efuent was shown (Fig. 11). For Feed 1, COD
removal was initially 74% which gradually increased to 80% within 1 h
of ltration. For Feed 2, COD reduction was increased from 66% at
15 min to 79% within 1 h. Unlike dye removal, COD reduction was
higher for the ferrous sulphate and lime treated feed (Feed 4)
compared to the ferric chloride treated feed (Feed 3). For Feed 3 COD
reduction varied from 44 to 53% which was about 5160% for the Feed
4. For the direct microltration of efuent (Feed 5) about 2224%
reduction in the COD was found.
The ceramic microltration membrane was highly efcient for
turbidity removal, irrespective of the types of feed (Fig. 12). It can be
observed that turbidity removal was 98.5% for the untreated efuent,

Fig. 10. Dye removal with time in the microltration study of sulphur black efuent
(Feed volume: 5.5 l; Filtration area: 0.045 m2; TMP: 1.0 kg/cm2).

which reached to near 100% with time for the different types of
treated feed. For these feeds, turbidity of most of the permeate
samples was below 1 NTU.
Reduction in TSS during CMF study of the various types of feed is
shown in Fig. 13. Here for Feed 1, TSS removal was within 9498% in
the range of the ltration time used in the study. TSS reduction was
maximum (N99%) for the aluminium sulphate treated feed (Feed 2).

Fig. 11. COD reduction (%) with time in the microltration study of sulphur black
efuent (Feed volume: 5.5 l; Filtration area: 0.045 m2; TMP: 1.0 kg/cm2).

Fig. 12. Turbidity reduction (%) with time in the microltration study of sulphur black
efuent (Feed volume: 5.5 l; Filtration area: 0.045 m2; TMP: 1.0 kg/cm2).

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P. Bhattacharya et al. / Desalination 261 (2010) 6772

Fig. 13. TSS reduction (%) with time in the microltration study of sulphur black
efuent (Feed volume: 5.5 l; Filtration area: 0.045 m2; TMP: 1.0 kg/cm2).

For Feed 3, reduction was comparatively lower (7879%), whereas, for

Feed 4 this varied from 94 to 98%. For the untreated feed, about 80%
reduction in TSS was observed.
Flux prole of the various types of sulphur black efuent at
constant TMP of 1 kg/cm2 is shown in Fig. 14. The untreated sulphur
black efuent being the most polluted one (turbidity 5912 NTU),
showed the lowest value of permeate ux. Initially, the ux value was
about 131 LMH, thereafter a sharp decline in the ux value was
observed, after 2 h ux was about 65 LMH. The reduction in ux value
was due to the concentration polarization across the membrane
surface. The pretreatment of the sulphur black efuent resulted in an
enhancement of the ux prole. For the coagulant treated feeds
(Feeds 2, 3 and 4), steady state ux values were obtained within short
time and ux prole remained almost constant during the process.
However, for the adsorbent treated feed (Feed 1), a lower value of
permeate ux was obtained. This may be due to the accumulation of
some adsorbent particles across the membrane surface. For this feed,
initial ux value was about 111 LMH, which gradually decreased with
time and after 2 h, ux value was about 96 LMH.
The effect of variation of operating pressure in the permeate ux
was observed by varying the TMP from 0.4 to 1.2 kg/cm2 (Fig. 15).
Increase in TMP increased the ux due to an enhancement of the
driving force. For the different types of feed, almost linear increase in
the permeate ux was observed. A sharp increase in ux value was

Fig. 15. Variation of permeate ux with pressure during cross ow microltration of

sulphur black efuent (Feed volume: 5.5 l; Filtration area: 0.045 m2).

observed for Feed 1 up to 1 TMP, thereafter, the rate of increase

decreased. For the untreated efuent, ux value was not signicantly
improved with increase in the TMP.
4. Conclusions
A comparative performance study was made involving the use of
low cost and chemically stable ceramic microltration membrane for
treatment of highly contaminated sulphur black efuent. Optimum
pH was found as 4 from the batch scale pretreatment study. An effective
separation was found in CMF of the biosorbent (1 g/l) treated
efuent and for efuent pretreated with aluminium sulphate (1 g/l).
After 1 h of ltration, dye removal was N99% with 80% reduction of
COD. Reduction of TSS was higher for the coagulant treated feed
(N99%) compared to the adsorbent treated feed (9498%). In CMF of
the untreated efuent, dye removal and COD reduction were low,
however TSS reduction was 80%. The overall turbidity removal was
N99% for all the permeate samples, irrespective of with/without
pretreatment. Concentration polarization effect was signicant in
permeation rate of the untreated efuent, after 1 h about 40% decline
in permeate ux was observed in constant pressure ltration study.
Flux value was considerably improved for the chemically pretreated
feeds which remained almost constant with time.
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Fig. 14. Permeate ux prole with time during cross ow microltration of sulphur
black efuent (Feed volume: 5.5 l; Filtration area: 0.045 m2; TMP: 1.0 kg/cm2).

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