Separation and Purification Technology 31 (2003) 141 /151

www.elsevier.com/locate/seppur

Nanofiltration of textile plant effluent for color removal and

reduction in COD
S. Chakraborty, M.K. Purkait, S. DasGupta *, S. De, J.K. Basu
Department of Chemical Engineering Indian Institute of Technology, Kharagpur 721 302, India

Received 20 May 2002; received in revised form 30 August 2002; accepted 12 September 2002

Abstract

A membrane based separation process (nanofiltration, NF) is used to treat the effluent from a textile plant. The dye
mixture contains reactive black dye (Cibacron Black B) and reactive red dye (Cibacron Red RB). An organic membrane
with molecular weight cut-off of 400 is used for the experiments. The experiments are conducted in an unstirred batch
and a rectangular cross flow cell. Separations with retentions up to 94 and 92% of the two dyes are achieved respectively
in the cross flow cell where steady state is attained quickly. It is important to note that NF techniques achieve a sharp
reduction in chemical oxygen demand (COD), (up to 94% in cross flow cell), as the dyes are removed from the
permeate. A parametric study of the separation process is undertaken to characterize the effects of the operating
variables, e.g., trans-membrane pressure, dye concentration in the feed and cross flow velocity in case of cross flow NF.
# 2002 Elsevier Science B.V. All rights reserved.

Keywords: Nanofiltration; Cross flow; Textile effluent; Dye; Chemical oxygen demand

1. Introduction pollution control mechanisms results in a gradual

decay of water quality.
Industrialization and urbanization have resulted Textile industries, particularly those involved in
in rapid deterioration of water quality. The finishing processes are major water consumers and
scientific evidences prove that the effluents re- the source of considerable pollution. The environ-
leased from different industries e.g. textile, leather, mental challenge for the textile industry is asso-
paint etc. comprise of different hazardous and ciated with liquid waste, which tends to dominate
toxic compounds, some of which are known over air-emissions and solid wastes in terms of the
carcinogens and others probable carcinogens. severity of environmental impacts. A typical textile
The emergence of industrial centers without a unit generates various types of wastewater differ-
corresponding growth in civic amenities and ing in magnitude and quality. The wastewater
from printing and dyeing units in a textile plant are
often rich in color, containing residual of reactive
* Corresponding author. Tel.:
/91-03222-83922; fax:
/91-
03222-75303 dyes and chemicals, and needs proper treatment
E-mail address: sunando@che.iitkgp.ernet.in (S. DasGupta). before releasing into the environment.
1383-5866/02/$ - see front matter # 2002 Elsevier Science B.V. All rights reserved.
PII: S 1 3 8 3 - 5 8 6 6 ( 0 2 ) 0 0 1 7 7 - 6
142 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151

Nomenclature
C0 feed concentration (ppm)
C1,0 concentration of dye 1 in feed (ppm)
C2,0 concentration of dye 2 in feed (ppm)
Cp permeate concentration (ppm)
CFC cross flow cell
COD chemical oxygen demand
CP concentration polarization
Lp membrane permeability (m3/N s)
NF nanofiltration
R0 observed retention
R0,1 observed retention for dye 1 (1/Cp,1/C1,0)
R0,2 observed retention for dye 2 (1/Cp,2/C2,0)
RO reverse osmosis
Tds total dissolved solid
TS total solid content
u0 cross flow velocity (cm/s)
UF ultrafiltration
Vw permeate flux (m/s)

Among the conventional methods for removal by RO [3]. Permeate is reused as washwater and
of color from wastewater, viz. chemical coagula- the retentate is either reused or discarded. Bran-
tion, flotation, chemical oxidation and adsorption don et al. [4] and Porter and Goodman [5] used
[1], adsorption is the most common technique. But dynamically formed Zirconium Oxide/polyacry-
it is inherently a slow process and its performance late membrane in tubular form to treat textile dye
is limited by the equilibrium. Thus there is a house effluent. More than 95% of dye recovery
definite need to find alternative treatment pro- was observed. Similar results were obtained using
cesses. Membrane techniques hold great promise spiral-wound modules [6]. El-Nasher [7] studied
in this field, [2] as they have the potential to either economic feasibility of using RO to treat dye
remove the dyestuff and allow reuse of the containing effluent. It was concluded that mem-
auxiliary chemicals used for dyeing or to concen- brane based separation processes are technically
trate the dyestuffs and auxiliaries and produce and economically feasible processes to treat dye-
purified water. Microfiltration is suitable for containing effluent. Nowak et al., [8,9] studied
removing colloidal dyes from the exhausted dye cross flow ultrafiltration of a textile dye bath in a
bath and the subsequent rinses. Ultrafiltration is tubular membrane and reported up to 97% dye (of
effective as single-step treatment of secondary molecular weight /780) removal and removal of
textile wastewater. Nanofiltration (NF) allows chemical oxygen demand (COD) and TOC by 75 /
the separation of low molecular weight (B/1000) 85% and 50 /60%, respectively.
organic compounds and salts, with an appreciable Yazhen et al. [10] had used NF for the treatment
softening effect. Reverse osmosis (RO) is suitable of textile dye plant effluent. Experimental runs
for removing ions and larger species from dye bath with pure dye solutions as well as an industrial dye
effluents. The permeate produced is usually color- solution confirmed the potential of the process.
less and low in total salinity. Schrig and Widmer [11] undertook NF of a
Membrane based processes have been used to mixture of dye salt and sodium chloride in a
treat the textile dye house effluent. The wastewater spiral-wound module. Similarly, Yu et al. [12]
from different washing and rinsing steps is treated applied NF membrane technology for the desalt-
 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151 143

Conductivity/10 3 (mmho/cm) TS (ppm) Equivalent salt concentration (equivalent NaCl) (g/lit) COD (mg/lit)
ing and concentrating of aqueous dye at a dye
producing plant. The newly developed process
using NF was continuous in operation, was not

6312
labor intensive, and produced a high purity
product of consistent quality.
Recently, Dhale and Mahajani [13] reported a
combined process of NF and wet oxidation to
treat the dye bath waste stream. Rejections up to
99% of color and 97% of COD were reported in
NF and retentate was treated by wet oxidation
process. In the work of Van der Bruggen et al. [14]
different samples from the wastewater treatment
sequence of a textile factory were filtrated with
different NF membranes. It had been observed
that flux decline due to adsorption of organic
material on the membrane decreased the mem-
brane capacity by up to 73%, but the process water
flux, which is largely concentration dependent,
reached a stable value in all experiments. It was
concluded that membrane based separation pro-
1.05/105 56

cesses are technically and economically feasible

processes to treat dye-containing effluent.
However there are certain difficulties in predict-
ing membrane performance as the process is
influenced by several operating parameters. One
of the most important drawbacks of the membrane
separation processes is the decline in flux due to
concentration polarization (CP) and membrane
fouling during the operation [15,16]. CP refers to
the build up of solute species within a thin
boundary layer adjacent to the membrane surface.
The accumulation of species at the membrane
6.86 116.3

surface adversely affects the membrane perfor-

Characterization of the effluent from the textile plant

mance. Due to the limitations imposed by CP and

C1,0 MW 923 (ppm) C2,0 MW 854 (ppm) pH

membrane fouling, there is a need for a detailed

study of the effects of the controlling parameters in
the process.
The present work is a part of a larger work,
which is the combined use of adsorption comple-
mented by NF in the treatment of colored
industrial effluent. It is envisaged that the bulk
118

removal of the dye will take place in an adsorption

unit, whereas removal of remaining amount (10 /
30 ppm approximately) will be handled in the NF
unit. The present effluent is a mixture of two
reactive dyes namely Cibacron black B and
Table 1

Cibacron red RB which have been used in dyeing

173

of 100% cotton knits wear in a winch machine at a

144 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151

hosiery dye house, Singhal Brothers’, located at

Tangra, Kolkata. In this work, an extensive study
has been carried out to observe the effects of the
process parameters like applied pressure, bulk
velocity and feed concentration in the NF of the
effluent. Two different process configurations,
namely, unstirred batch cell and cross flow cell
have been used. Solution mixture characteristics
e.g., pH, total dissolved solid, conductivity etc. of
the feed, permeate and retentate streams have been
measured at different operating conditions.

Fig. 1. Schematic of unstirred batch NF cell.

2. Experimental
metal support forms one side of the channel. The
2.1. Materials width of the membrane is 4.5 cm, length is 26 cm
and the channel height is 1.65 mm. The retentate
2.1.1. Dyes solution is recycled to the feed tank. In the
The present industrial effluent, which has been retentate line of the cell, a rotameter is placed to
collected from a textile dye house, contains a measure the flow rate. The pressure inside the cell
mixture of two reactive dyes, namely Cibacron is maintained by operating the two valves manu-
Black B and Cibacron Red RB, which will be ally. Permeate samples are collected from the
denoted by dye 1 and 2 respectively in the rest of bottom of the cell.
the paper. The molecular weights of the two dyes
are 923 and 854, respectively. The characterization
2.3. Experimental methods
of feed effluent is presented in Table 1.
The experimental process involved the following
2.1.2. Membrane
steps:
An organic membrane (thin film composite
polyamide) of molecular weight cut-off 400, sup-
plied by M/s Permionics, Baroda was used in the 2.3.1. Compaction of membranes
experiments. Before using a fresh membrane, it was com-
pacted at a pressure of 690 kPa for 3 h using
2.2. System configuration distilled water.

2.2.1. Unstirred batch cell 2.3.2. Preparation of feed solution

Fig. 1 represents the flow diagram of the batch Required concentrations for NF were prepared
cell operation. The feed solution from the feed by diluting the feed using distilled water.
tank is pumped to the batch cell. Inside the cell a
circular membrane is placed over a metallic sup- 2.3.3. Determination of membrane permeability
port. The diameter of the membrane is 65 mm. The Membrane permeability was determined using
permeate is collected from the bottom of the cell. pure distilled water. Flux values of distilled water
at different operating pressures were measured and
2.2.2. Cross flow cell were plotted against pressure difference. The
Fig. 2 represents the flow diagram of the average value of membrane permeability as mea-
continuous cross flow NF unit. From the feed sured was 2.42 /1011m3/m2 sPa, which remained
tank, the feed solution is pumped to the cell, where almost constant through out the conduction of all
it flows through a channel. The membrane on a experiments.
 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151 145

spectrophotometer, supplied by Shimadzu Cor-

poration, Japan (at wavelengths of 599 and 535
nm, for dye 1 and 2, respectively) to measure the
permeate concentration. The standard method by
Vogel [17] was used for the determination of
concentration of each dye in the effluents.

2.3.6.2. Measurement of chemical oxygen demand.

The COD is the measure of oxygen consumed
during the oxidation of the oxidizable organic
Fig. 2. Schematic of continuous cross flow NF cell. matter by a strong oxidizing agent. The sample
(feed, permeate and retentate stream at each
2.3.4. Conduction of experiments operating condition) was refluxed with potassium
Experimental runs were conducted in the two dichromate and sulphuric acid in presence of
cells. The operating parameters were the feed mercuric sulphate (to neutralize the effect of
concentration and trans-membrane pressure dif- chlorides), and silver sulphate (catalyst). The
ference for unstirred batch system and cross flow excess of potassium dichromate was titrated
velocity, feed concentration and pressure differ- against ferrous ammonium sulphate using ferroin
ence for cross flow system. During each experi- as an indicator. The amount of potassium dichro-
ment, cumulative volumes of the permeate were mate used is proportional to the oxidizable organic
collected. The permeate flux values were obtained matter present in the sample [18].

(b  a)  (N) of Ferrous Ammonium sulphate  1000  8

COD mg=l
Volume (in ml) of sample

from the slope of the plot of the cumulative b, ml of titrant using blank; a, ml of titrant using
permeate volume versus time. Permeate samples sample.
were collected at different time and permeate
concentration is measured. Duration of each 2.3.6.3. Measurement of conductivity. The conduc-
experiment was 50/60 min in batch cell and 45 tivities of all samples (feed, permeate and retentate
min in cross flow cell. streams at each operating conditions) were mea-
sured by an autoranging conductivitymeter Che-
2.3.5. Determination of the new permeability mito 130, manufactured by Toshniwal Instruments
After thoroughly cleaning the system several (India) Ltd.
times by distilled water, the membrane permeabil-
ity was reevaluated. It was observed that the 2.3.6.4. Measurement of total solid. Total solid
membrane permeability remained almost constant (TS) of all the samples were measured by taking 10
between successive runs. ml. of each sample in a watch glass and keeping in
a oven till complete drying of the sample.
2.3.6. Analysis of the samples
w
TS 1000 mg=lit
volume (in ml) of sample
2.3.6.1. Measurement of dye concentration. Feed
and permeate samples were analyzed by UV-2100 Here, w is the weight of the sample after drying.
146 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151

2.3.6.5. Measurement of pH. After each experi-

ment, pH of the samples was measured, by a pH-
meter, supplied by Toshniwal Instruments (India)
Ltd.

2.4. Operating conditions

2.4.1. Batch cell

For batch cell, three feed concentrations are
used. These are a mixture of (i) 25, 15 ppm (ii) 13,
7 ppm and (iii) 20, 10 ppm of the dye 1 and 2,
respectively. In the subsequent tables and figures
C1,0 and C2,0 refer to the feed concentrations of
dye 1 and 2, respectively. The operating pressures
selected are 276, 484, 550 kPa.

2.4.2. Cross flow cell

Two feed concentrations are chosen for experi- Fig. 3. Variation of observed retention of dye 1 (MW 924.5) in
ments (i) 25, 15 ppm and (ii) 13, 7 ppm of the dye 1 a mixture of dyes 1 and 2 with time in the batch cell for different
conditions of DP and C0.
and 2, respectively. Cross flow velocities are 14, 21
and 28 cm/s and applied pressures are 276, 415 and
550 kPa.

3. Results and discussions

3.1. Batch cell

Figs. 3 and 4 represent the variation of observed

retention (R0 /1/Cp/C0) with time of dye 1 and 2
respectively at different conditions of feed con-
centration and operating pressures. For dye 1 the
expression for the observed retention is R0,1 /1/
Cp,1/C1,0 and that for dye 2 is R0,2 /1/Cp,2/C2,0.
It is observed from the figure that initially reten-
tion decreases sharply (specially for higher feed
concentrations) and gradually thereafter, for a
fixed feed concentration. This may be explained
by the phenomena of CP. CP leads to a build up of Fig. 4. Variation of observed retention of dye 2 (MW 855.5) in
the solute particles over the membrane surface, a mixture of dyes 1 and 2 with time in the batch cell for different
enhancing the solute permeation by convection conditions of DP and C0.
through the membrane. Therefore, initially the
permeate concentration increases rapidly, thereby decrease in retention becomes gradual. It must be
resulting in a sharp decrease of R0. During pointed out here that in the case of a batch cell, the
extended operations, the flux due to backward membrane surface concentration will keep on
diffusion from the membrane surface towards the increasing and a steady state, as far as the
bulk solution becomes competitive with the con- permeate concentrations are concerned will never
vective flux through the membrane and the be attained. It may also be observed from the
 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151 147

figure that at same feed concentration (25:15

ppm), R0 is lower for higher operating pressure
(square and triangle symbols in the figure). At
higher operating pressure, permeate concentration
is more due to an enhanced convective flux
through the membrane (because of higher driving
force) and permeate concentration increases with a
decrease in R0.
At a fixed applied pressure difference, permeate
concentration increases with increasing feed con-
centrations (C0). For example, at a pressure of 276
kPa, the permeate concentration values of dye 1
after a time of 1200 s is 2.30 and 1.50 ppm,
respectively for feed concentrations of 25:15 and
13:7 ppm, respectively. But the change in retention
values with feed concentrations is not apparent
here (R0,1 is 0.907 and 0.873, respectively), as the Fig. 5. Variation of percentage COD removal of effluent
effect of feed concentration (C0) is normalized. mixture with time in the batch cell for different conditions of
Fig. 5 represents the percentage removal of DP and C0.
COD with time for the same conditions of feed
concentration and operating pressures as in Figs. 3
and 4. As COD is directly proportional to the
concentration, the profile of the removal of COD
shows the same trend as in Figs. 3 and 4. It is
observed from the figure, that at a feed concentra-
tion of 25:15 ppm and operating pressure of 276
kPa, the maximum removal of COD can be upto
90% after a time of 1230 s from the starting of the
experiment.
Fig. 6 shows the variation of flux values with
time for the same conditions of feed concentra-
tions and operating pressures as in Figs. 3 and 4. It
is evident from the figure that the permeate flux
decreases with time of operation. As explained
earlier, during the experiments, the membrane
surface concentration goes on increasing due to
the CP phenomenon. This leads to an increase in Fig. 6. Variation of permeate flux of effluent mixture with time
osmotic pressure near the membrane-solution in the batch cell for different conditions of DP and C0.
interface and thereby, a decrease in the effective
driving force (i.e. trans-membrane pressure). This decreases. Increase in feed concentration results in
leads to a decline in flux. As the operating feed an increase in surface concentration and therefore
concentrations are of low range, the decrease in osmotic pressure increases and thereby leading to
the permeate flux values are not substantial, and decrease in driving force and reduction in flux.
the curves appear almost flat. From the figure, it is
observed that permeate flux is higher for higher 3.2. Cross flow cell
operating pressure (due to the enhancement in the
driving force) if feed concentration remains same. A summary of the results of each experiments
With increase in feed concentration permeate flux conducted in cross flow NF is presented in Table
148 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151

Table 2
Some properties measured for the textile industrial effluent during conduction of experiments in the cross flow cell

C1,0: C2,0 u0 (cm/s) DP (kPa) Stream Conductivity/10 3 (mmho/cm) TS (ppm) % COD removal % Color removal

Dye 1 Dye 2

25:15 14 276 Feed 19.9 1.17/104 90 89.1 92.0

Permeate 13.8 1.02/104
Retentate 20.5 1.25/104
25:15 21 276 Feed 19.8 1.18/104 92.9 90.3
Permeate 13.6 1.02/104 91.45
Retentate 20.3 1.25/104
25:15 28 276 Feed 18.9 1.23/104 94.6 93
Permeate 16.6 1.03/104 92.63
Retentate 19.1 1.27/104
25:15 14 415 Feed 14.48 1.23/104 86.7 84.5
Permeate 13.23 1.06/104 85.4
Retentate 14.6 1.27/104
25:15 21 415 Feed 9.41 5.16/103 89.4 88.7
Permeate 7.96 4.06/103 89.13
Retentate 9.53 5.97/103
25:15 28 415 Feed 9.28 4.58/103 91 89.3
Permeate 7.42 3.85/103 90.27
Retentate 9.56 4.62/103
25:15 14 550 Feed 6.91 3.41/103 79.1 79.7
Permeate 5.55 3.07/103 80.54
/ Retentate 6.98 3.57/103
25:15 21 550 Feed 4.37 2.05/103 82.7 85
Permeate 3.57 1.42/103 84.86
Retentate 4.48 1.98/103
25:15 28 550 Feed 1.49 9.0/102 87 88.3
Permeate 1.46 6.10/102 85.4
Retentate 1.12 9.80/102
13:7 14 276 Feed 1.25 1.47/103 90.8 87.6
Permeate 1.018 7.60/102 90.37
Retentate 1.272 1.65/103
13:7 21 276 Feed 1.18 1.78/103 92.6 88.2
Permeate 0.942 8.10/102 91.32
Retentate 1.185 9.70/102
13:7 28 276 Feed 0.881 3.80/102 93.9 92.1
Permeate 0.661 1.90/102 93.77
Retentate 0.872 4.20/102
13:7 14 415 Feed 0.614 3.10/102 88.5 84.2
Permeate 0.497 5.0/101 87.5
Retentate 0.646 3.60/102
13:7 21 415 Feed 0.455 1.20/102 90.5 86.8
Permeate 0.342 8.0/101 89.9
Retentate 0.466 1.15/102
13:7 28 415 Feed 0.332 1.15/102 91.4 89.3
Permeate 0.244 7.5/101 91.3
Retentate 0.342 1.20/102
13:7 14 550 Feed 0.199 5.40/102 74.1 67.4
Permeate 0.146 3.40/102 72.5
Retentate 0.204 6.50/102
13:7 21 550 Feed 0.252 1.03/103 79.3 77.1
Permeate 0.179 8.50/102 81.2
 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151 149

Table 2 (Continued )

C1,0: C2,0 u0 (cm/s) DP (kPa) Stream Conductivity/10 3 (mmho/cm) TS (ppm) % COD removal % Color removal
Dye 1 Dye 2

Retentate 0.266 1.15/103

13:7 28 550 Feed 0.162 5.70/102 86.1 80
Permeate 0.105 3.60/102 85.1
Retentate 0.174 6.20/102

2. Figs. 7 and 8 represent the variation of observed

retention of the two dyes with pressure difference
for two different feed concentrations (25:15 and
13:7 ppm, respectively) and three different cross
flow velocities (14, 21 and 28 cm/s). For the cross
flow cell the retentions mentioned are the steady
state value since the system reaches steady state in
a very short time. In these figures hollow and solid
symbols represent dye 1 and 2, respectively. From
the figure it is observed that R0 decreases with
increase in applied pressure for a particular feed
concentration and cross flow velocity. At higher
pressure permeate concentration is more (as ex-
plained earlier) resulting in lower retention. From
the figure it is also clear that as the cross flow
velocity increases, R0 increases, for same feed
concentration and applied pressure. As cross Fig. 7. Variation of observed retention of the two dyes in the
flow velocity increases, CP on the membrane effluent mixture with trans-membrane pressure drop at a same
feed concentration (25:15) and different cross flow velocities.
surface decreases, hence membrane surface con-
centration decreases leading to a decrease in
permeate concentration. It may be observed from
Fig. 7 that at a pressure of 276 kPa and bulk
velocity of 28 cm/s, retention can go up to 95 and
93% for the two dyes respectively.
Fig. 9 shows the percentage removal of COD
with pressure at three different cross flow velocities
for effluent feed mixture at two different feed
concentrations. With increase in pressure at con-
stant cross flow velocity, observed retention of dye
decreases and hence COD of permeate increases,
and therefore percentage removal of COD de-
creases. For a feed concentration of 13:7 ppm, a
maximum of 94% of COD has been removed at a
pressure of 276 kPa and cross flow velocity of 28
cm/s.
The variations of permeate flux with operating Fig. 8. Variation of observed retention of the two dyes in the
pressure for different combinations of feed con- effluent mixture with trans-membrane pressure drop at a same
centrations and cross flow velocities are presented feed concentration (13:7) and different cross flow velocities.
150 S. Chakraborty et al. / Separation and Purification Technology 31 (2003) 141 /151

Fig. 9. Variation of COD removal with cross flow velocity and Fig. 10. Variation of permeate flux of the industrial effluent
trans-membrane pressure drop during cross flow NF. with trans-membrane pressure drop at two different feed
concentrations.

in Fig. 10. It is clear from the figure that the flux present study. It has been found that substantial
profile is higher for higher operating pressure. removal of the two dyes (upto 94%) is achieved in
With increase in operating pressure (at a fixed feed a cross flow cell with a marked reduction in the
concentration), the driving force across the mem- chemical oxygen demand of the permeate. A
brane increases leading to an enhancement of detailed parametric study is conducted to study
permeate flux. Also, the permeate flux follows the effect of process variables on the separation
the expected trends with variation in feed concen- efficiency of the nanofiltration process.
tration at a fixed operating pressure, i.e. flux
decreases with increase in feed concentration (solid
and hollow circle). With increase in feed concen- Acknowledgements
tration, the CP is more. This leads to an increase in
osmotic pressure near the membrane surface and This work is partially supported by a grant from
the trans-membrane pressure drop decreases. Thus the Ministry of Human Resource and Develop-
for higher feed concentration, the permeate flux is ment (MHRD), Government of India under the
lower. At a fixed feed concentration, flux increases scheme no. F. 27-6/2000 TS V. Any opinions,
with cross flow velocity due to reduction in CP, findings and conclusions or recommendations
although the difference is marginal as observed expressed in this paper are those of the authors
from the figure (hollow circle and triangle). and do not necessarily reflect the views of MHRD.

4. Conclusion References

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