Application of ceramic membranes for the separation of dye particles

Katarzyna M. Majewska-Nowak
Wroclaw University of Technology, Wyb. Wyspianskiego 27, 50-370 Wroclaw, Poland
a b s t r a c t a r t i c l e i n f o
Article history:
Received 3 August 2009
Received in revised form 15 November 2009
Accepted 18 November 2009
Available online 6 January 2010
Keywords:
Anionic dyes
Sodium dodecyl sulphate
Ceramic membrane
Ultraltration
This study reports the results of ultraltration experiments on model dye solutions containing anionic dyes
and anionic surfactant. The ceramic membrane modules CeramINSIDE (TAMI Industries) of various cut-off
values (1, 5, 8, 15, and 30 kDa) were used in the experiments. The suitability of ceramic membranes for the
decolourization of dye solutions was evaluated. Seven anionic organic dyes of molecular weights ranging
from 327 to 1084 Da were used in the tests. The anionic surface active agent (sodium dodecyl sulphate, SDS)
was added to the dye solutions. The experiments were conducted at 0.030.1 MPa with the use of a
laboratory and semi-pilot UF installation. The effect of the molecular weight of the dyes as well as the SDS
presence in the separated solutions (in the range below the CMC) on the process efciency was studied. It
was found that membrane properties (permeability and dye separation factor) were almost identical for
membrane modules of cut-off equal to 1, 5, and 8 kDa. For high-molecular-weight dyes above 600 Da
retention amounted to 9598% and was slightly inuenced by the SDS presence in the dye solution. Ceramic
membranes with a cut-off of 15 and 30 kDa exhibited insignicantly poorer properties.
2009 Elsevier B.V. All rights reserved.
1. Introduction
The textile, dyestuff, paper and laundry industries consume large
volumes of water and chemicals for wet processing and generate
various types of coloured wastewater. The wastewater from dyeing
units in a textile plant is often rich in colour due to the residual of
applied dyes. Besides being rich in colour, they also contain mineral
salts and surface active agents. Because of increasingly stringent
restrictions on the organic and mineral content of industrial efuents,
it is necessary to eliminate the pollution load from wastewater before
it is discharged to the environment. In some cases, especially for
textile plants, treatment techniques enabling the recovery of valuable
substances may be preferred. A separation systemfor the recirculation
of dyes, salts and water would be advantageous compared to the
simple discharge to surface water.
Membrane processes, especially nanoltration and reverse osmo-
sis, are being increasingly used in the treatment and reuse of textile
wastewater [13]. These techniques, however, are characterized by
high energy consumption and a rather low hydraulic efciency. Low-
pressure membrane processes such as microltration and ultraltra-
tion may be economically more favorable in dye efuent treatment.
Notably, there is little available literature on the application of low-
pressure membrane processes (microltration and ultraltration) in
the industrial reuse of valuable chemical compounds of exhausted dye
or rinsing baths. Merely the recovery of polymeric dyes and low-
soluble dyes (indigo) by means of ultraltration was reported as an
efcient process in industrial applications [4]. In addition, Porter et al.
[5,6] found that it was possible to retain anionic dyes by ceramic
microlters and polymeric ultraltration membranes.
With respect to membrane installation, engineers demand process
stability, a low requirement for preliminary treatment and minimum
support and maintenance. Unlike polymeric membranes, ceramic
membranes are able to match these demands due to their extremely
high chemical and physical stability, their outstanding separation
characteristics and their long lifespan. Other advantages of ceramic
membranes include the ability to use steam sterilization and back
ushing, high abrasion resistance, high uxes, bacteria resistance,
possibility of regeneration and dry storage after cleaning.
The supports for the inorganic membrane elements are made from
aluminium oxides or silicon carbides. These materials can fulll high
requirements relating to mechanical stability. The supports can be
designed for a single-channel or multi-channels. The membrane layer
is only a few m thick and is placed on the inner side of the channel.
Since ceramic membranes are generally more expensive than
standard commercial polymer membranes, their use should focus on
applications demanding greater thermal or chemical resistance.
Presently, successful implementation of ceramic membranes includes
all industries where media are ltered: the chemical industry (e.g.
product separation and cleaning), metal industry (e.g. recycling and
disposal of degreasing and rising baths, recovery of heavy metals),
textile industry (e.g. recovery of dyes), food and beverage (e.g.
clarication of juice and beer, sterilization of milk and whey) [611].
It should be pointed out that the limitation in polymer membrane
operation occurs when the chemical, thermal or mechanical stability
Desalination 254 (2010) 185191
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E-mail address: katarzyna.majewska-nowak@pwr.wroc.pl.
0011-9164/$ see front matter 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2009.11.026
Contents lists available at ScienceDirect
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j our nal homepage: www. el sevi er. com/ l ocat e/ desal
of the membrane is exceeded by the solution to be treated. Although
some polymeric membranes have been used to successfully treat
acids, bases and solvents [12,13], their long-term resistance has often
proved inadequate for industrial applications. Thus, many researchers
have been working on developing ceramic membranes for several
years. Weber et al. [14] described some tests conducted with ceramic
single or multi-channel membranes with an active layer of TiO
2
or
ZrO
2
.These tests proved that new ceramic NF membranes can be
applied for the treatment of textile wastewater, alkaline solutions
from washing machines and pickling bath solutions. During the
treatment of wastewater it has been found that salt retention
decreased strongly as the electrolyte concentration increased.
High permeability values, a good retention of organics as well as a
low fouling tendency make the newly developed ceramic membranes
advantageous in industrial applications.
2. Materials and methods
2.1. Ceramic modules
Commercially available ceramic membrane modules CeramINSIDE
(TAMI Industries) were used in the experiments. The modules were of
the tubular single- or multi-channel type with a titanium oxide active
layer. Technical parameters of the experimental modules used in the
tests are given in Table 1.
2.2. Ultraltration process
The transport and separation properties of the ceramic modules
were determined using the systems presented in Fig. 1 (ProFlux M12,
Millipore, installation for single-channel membranes) and in Fig. 2
(semi-pilot installation for 3-channel membranes). These installa-
tions enabled membrane testing in various module congurations.
The installations can operate at a constant concentration of circulated
solution via permeate recirculation between the feeding tank and the
membrane module.
The installation presented in Fig. 1 consists of a membrane module
(1), feeding tank (2), pressure pump (3), pressure sensors (4), and
valves (5). The effective volume of the installation is equal to 3 dm
3
.
The semi-pilot setup of the cross ow system (Fig. 2) includes the
following major parts: ultraltration module (1), hydraulic mem-
brane pump Milroyal C Dosapro Milton Roy (3), 25 m prelter
(5), feeding tank (2) and permeate tank (10). Additional sensors
protected the setup against an unexpected pressure increase.
Experimental solutions were passed through a 25 m cartridge lter
prior to the ultraltration module. The effective volume of the system
was 80 dm
3
.
The preliminary ultraltration experiments with single-channel
ceramic membranes were performed at 0.03, 0.06 and 0.09 MPa with
a cross ow rate of 1.52.0 m/s, whereas the long-term experiments
with 3-channel ceramic membranes were conducted at 0.1 MPa with
a cross ow rate of 22.5 m/s.
Prior to each cycle, the membrane module was treated with
distilled water at 0.10 MPa until constant permeate volume ux was
established. Permeate volume uxes and retention coefcients were
determined with respect to the experimental dyes after steady ow
conditions were achieved. The permeate ux was measured and the
concentration of anionic dye was analysed in the permeate and
concentrate at 60 minute intervals during the long-termexperiments.
Permeate volume ux (J) was calculated as follows:
J =
V
tA
; m
3
= m
2
day
where V is the permeate volume (m
3
), t stands for time (day), and A
denotes the effective membrane surface area (m
2
).
The dye retention coefcient (R) was determined by virtue of:
R =
c
k
c
p
c
k
100; %
where c
k
and c
p
denote the dye concentration (g/m
3
) in retentate and
permeate, respectively.
2.3. Experimental solutions
The transport and separation properties of the CeramINSIDE
single-channel modules were determined for distilled water, aqueous
solutions containing various organic dyes (Merck, Zachem) (Table 2)
and aqueous solutions of organic dye and sodium dodecyl sulphate
(SDS) (Aldrich). The applied dyes were anionic and varied in
molecular weight.
The long-term tests were carried out with aqueous solutions of
Direct Black, aqueous solutions containing SDS and dye as well as
aqueous solutions containing dye, SDS and sodium salt (NaCl).
In the aqueous solutions, the dye and surfactant concentration was
equal to 100 g/m
3
. The initial concentration of SDS was below its
critical micelle concentration (CMC b2257 g/m
3
). The molecular
formula of the anionic detergent was CH
3
(CH
2
)
11
OSO
3
Na and the
molecular weight of SDS totalled 288.38 Da. Model dye solutions were
prepared by dissolving dyes (as supplied) in distilled water at room
temperature (approximately 20 C). Dye concentrations in the
aqueous solutions were determined spectrophotometrically using
the spectrophotometer UVMINI-1240 (Shimadzu) at the wavelengths
given in Table 2, which correspond to the maximumabsorbance of the
sample.
The salt concentration in the tested solutions was equal to 1 kg/m
3
.
3. Results and discussion
3.1. Membrane permeability
The experiments were aimed at evaluating the application of
ultraltration ceramic membranes for the decolourization of dye
solutions. The effects of the dye molecular weight and solution
Table 1
Characteristics of the experimental ceramic modules.
Parameter ProFlux M12 installation
(Millipore)
Semi-pilot
installation
Conguration Tubular Tubular-clover
Cut-off, kDa 1, 5, 8, 15 5, 30
Membrane material Titanium oxide/zirconium oxide
Effective surface area, m
2
0.0042 0.02
Number of channels 1 3
Internal channel diameter, mm 6 3.5
External membrane diameter, mm 10 10
Membrane length, mm 250 600
Fig. 1. Laboratory UF installation ProFlux M12: 1 ceramic membrane module, 2
feeding tank, 3 pressure pump, 4 pressure sensor, and 5 valve.
186 K.M. Majewska-Nowak / Desalination 254 (2010) 185191
composition on the process efciency were veried. Several tubular
ceramic membrane modules (CeramINSIDE Tami Industries) charac-
terized by different cut-off values (1, 5, 8, 15, and 30 kDa) were used
in the tests.
The basic transport and separation properties of the modules were
determined prior to the long-term experiments. The distilled water
volume uxes at three values of transmembrane pressure (0.03, 0.06,
and 0.09 MPa) are shown in Fig. 3.
The volume ux of distilled water varied from 0.14 to 0.59 m
3
/
m
2
day (0.16 to 0.68 10
5
m
3
/m
2
s) depending on the applied
pressure and membrane cut-off. Notably, the membrane permeability
is not a reection of the signicant difference in cut-off values the
water volume uxes are all the same order of magnitude with the
highest value for the highest cut-off. When the dye solution was
passed through the module, a considerable drop in membrane
permeability was observed for all the tested modules (Fig. 4). This
effect was most pronounced for the ceramic membrane with the
lowest cut-off value. In this case, permeate permeability decreased
from 0.49 m
3
/m
2
day for distilled water to 0.220.25 m
3
/m
2
day for
solutions containing high-molecular-weight dyes (Fig. 4A). The
presence of an anionic surfactant (SDS) in the dye solutions caused
a further drop in membrane permeability.
In order to estimate the fouling intensity, the relative ux of the
tested membranes was taken into account (Table 3). Among the
membranes investigated, the 15 kDa membrane was characterized by
the highest relative ux values (0.580.90). It is worth noting that all
ceramic membranes under study exhibited rather low relative ux
values (0.410.90) in the ultraltration experiments of model dye
solutions. This could be an indication that adsorption of anionic dye
particles in the membrane structure occurred. This phenomenon may
be the result of electrostatic attraction between the positively charged
membrane and the negatively-charged dye particles. According to
Kabsch-Korbutowicz et al. [15] ceramic membranes made of TiO
2
or
ZrO
2
are characterized by an isoelectric point (IEP) of 6 and 7.5,
respectively. Similarly, Kuca and Szaniawska [16] found that the point
of zero charge for ceramic membranes consisting of TiO
2
/ZrO
2
layers
amounted to about 6.9, whereas Fernndez et al. [17] conrmed that
the IEP of the ZrO
2
active layer is slightly belowpH 6. Treated solution
pH values below the IEP will lead to a positive charge of membrane
material. Considering the pH values of dye solutions (Table 2) during
ultraltration, it can be anticipated that in most cases the ceramic
membranes will be positively charged. This phenomenon can
facilitate adsorptive fouling of ceramic membranes, especially in the
ultraltration of anionic, low-molecular-weight dyes.
Furthermore, it is likely that the worsening of membrane transport
properties (in terms of membrane permeability to distilled water)
was also caused by the rather hydrophobic nature of experimental
dyes (Table 4). This explanation could be crucial for solutions of high-
molecular-weight dyes characterized by a pH slightly above the IEP.
This means that in the ultraltration of dye solutions containing Direct
Blue and Direct Black, ceramic membranes can be slightly negatively-
charged. Nevertheless, due to permeate drop, the adsorptive fouling of
Fig. 2. Semi-pilot installation: 1 - membrane module, 2 - feeding tank, 3 - pump, 4 - pressure accumulator, 5 - preliminary lter 25 m, 6 - manometer, 7 - rotameters, 8 - control
valves, 9 drain valve, and 10 permeate tank.
Table 2
Characteristics of the experimental dyes.
Dye Molecular weight, Da Classication pH
a
Dye Symbol
max
b
, nm Structural formula
Methyl Orange 327 Acid dye 5.7 MO 465 C
14
H
14
N
9
O
9
SNa
C.I.
c
13025
Indigo Carmine 466 Acid dye 5.5 IC 610 C
16
H
8
N
2
Na
2
O
8
S
2
C.I. 73015
Amido Black 615 Acid dye 5.7 AB 618 C
22
H
14
N
6
Na
2
O
9
S
2
C.I. 20470
Titan Yellow 696 Direct dye 5.5 TY 399 C
28
H
19
N
5
Na
2
O
6
S
4
C.I 19540
Direct Green 878 Direct dye 6.1 DG 370 C
35
H
21
N
8
Na
3
O
12
S
2
C.I. 30315
Direct Blue 1029 Direct dye 7.2 HB 577 C
40
H
23
N
7
Na
4
O
13
S
4
C.I. 34140
Direct Black 1084 Direct dye 7.6 DB 585 C
44
H
32
N
13
O
11
S
3
Na
3
C.I. 35435
a
Determined for the dye solutions of concentration equal to 100 g/m
3
.
b
Wavelength corresponding to the maximum absorbance of the dye solution.
c
Colour Index number.
187 K.M. Majewska-Nowak / Desalination 254 (2010) 185191
high-molecular-weight dyes in the membrane structure prevails over
the electrostatic repulsion between the membrane material and
anionic dye particle.
It is worth noting that the decrease in dye permeate ux is less
pronounced for the ceramic membrane of the highest cut-off value
(15 kDa) (Fig. 4D), i.e. when the size of separated particles is
anticipated to be much smaller than the mean pore radius.
As was previously stated, the presence of ananionic surfactant indye
solutions brought about a further drop in volume ux. Since the pH of
the surfactant solutions usedinthe experiments was inthe range of 5.1
5.6, this phenomenon could also be explained by adsorptive fouling
caused by electrostatic attraction between the positively charged
membrane and the negatively-charged SDS particles.
The obtained results indicate that the ceramic modules were
susceptible to membrane fouling. This contradicts the general view
that ceramic membranes exhibit excellent properties [14]; although
as shown in Section 3.3, after the initial drop in volume ux, the
membrane permeability remains almost constant during the long-
term experiments. Such membrane behavior can be an indication of
the superiority of ceramic over polymeric membranes.
3.2. Membrane separation characteristics
The separation characteristics (i.e. the relation between mem-
brane rejection and the molecular weight of the treated substance)
are of crucial signicance for the membrane manufacturer and the
end user. With this information, it is possible to establish the limit
Fig. 4. Membrane volume ux for various model dye solutions and for dye solutions containing SDS: A) membrane cut-off 1 kDa, B) membrane cut-off 5 kDa, C) membrane cut-off
8 kDa, and D) membrane cut-off 15 kDa (P=0.09 MPa).
Table 3
The relative ux of ceramic membranes in the ultraltration of dye solutions.
Dye
symbol
Relative ux of the membrane
a
Membrane
cut-off 1 kDa
Membrane
cut-off 5 kDa
Membrane
cut-off 8 kDa
Membrane
cut-off 15 kDa
Dye Dye +
SDS
Dye Dye +
SDS
Dye Dye +
SDS
Dye Dye +
SDS
MO 0.80 0.71 0.74 0.71 0.83 0.68 0.90 0.70
IC 0.67 0.63 0.74 0.65 0.72 0.61 0.84 0.69
AB 0.69 0.63 0.77 0.65 0.76 0.70 0.88 0.68
TY 0.46 0.41 0.61 0.52 0.57 0.54 0.70 0.58
DG 0.46 0.41 0.68 0.58 0.63 0.52 0.70 0.61
HB 0.45 0.43 0.65 0.55 0.67 0.54 0.71 0.60
DB 0.54 0.49 0.65 0.52 0.72 0.61 0.86 0.77
a
Calculated at 0.09 MPa, as a ratio of J
v
/J
w
(J
v
volume ux of dye solution, m
3
/m
2
day; J
w
volume ux of distilled water, m
3
/m
2
day).
Fig. 3. Volume ux of distilled water at three transmembrane pressures for CeramIN-
SIDE membrane modules.
188 K.M. Majewska-Nowak / Desalination 254 (2010) 185191
molecular weight (LMW), i.e. the minimum molecular weight of the
substance which is entirely retained by membrane. LMW is an
important parameter which determines the possible uses of the
membrane. The shape of the plot may, to some extent, reect the pore
size distribution in the membrane. Thus, a greater angle of inclination
indicates a less distinct pore size distribution.
Fig. 5 gives the separation characteristics for the single-channel
ceramic membranes of various cut-off values. The organic dyes
involved in the tests differed considerably in molecular weight. Thus,
the plotted curves cover nearly the entire retention range (5 to 100%).
As shown by these plots, the separation characteristics of CeramIN-
SIDE membranes are almost identical, irrespective of the membrane
cut-off value. In the case of the model dye solutions containing SDS,
the plots are shifted insignicantly to the left (Fig. 5B). For all tested
membranes, the LMW amounted to approximately 620650 Da. For
aqueous solutions containing only dyes, the obtained curves are quite
evenly shaped and very steep which is an indication of a small pore
size distribution. It is worth noting that low-molecular-weight dyes
were rejected between 5 and 20% by ceramic membranes irrespective
of the membrane cut-off value. This could be to some extent the effect
of adsorptive fouling described in Section 3.2. SDS addition to the feed
solution resulted in a decrease in curve slope. This result could be
attributed to the fouling and surfactant adsorption in the membrane
pores, which affect the size of the pore radius.
The obtained results reveal that there is no distinct difference in
separation properties between 1, 5 and 8 kDa ceramic modules. A slight
deterioration in dye rejection is observed for the 15 kDa ceramic
module; however, this module is characterized by the highest
permeability making it particularly advantageous.
3.3. Membrane properties for a long operation time
The effect of operation time on the volume ux of dye (Direct
Black) solutions during UF for the CeramINSIDE modules (5 KDa and
30 kDa) is presented in Fig. 6A and in Fig. 7A, respectively. Generally,
it was found that the membrane permeability remained almost
constant during 10 h of operation. An insignicant diversity in ux
values depending on the solution composition was observed for the
tested modules. The highest uxes were observed for the solution
containing only dye, whereas the lowest permeability was found for
the mixture of dye and salt. These results correspond well to data from
literature. Weber et al. [14] also found a worsening of membrane
properties with increasing salt content.
The effect of operation time on the efciency of dye removal for
ceramic modules of cut-off equal to 5 kDa and 30 kDa is given in Figs. 6B
and7B, respectively. Based on the results obtained fromthe UF testing, it
was concluded that the applied CeramINSIDE modules were character-
ized by excellent separation properties towards high-molecular-weight
dye (Direct Black) dye retention coefcients exceeded 97%, irrespec-
tive of the operation time and solution composition. Notably, dye
rejectioncoefcients remained nearly constant during 10 hof operation.
Agradual worsening of separation efciency was observed, however, for
dye solutions containing both mineral salt and anionic surfactant.
Fig. 5. Dye retention versus dye molecular weight for ceramic membranes of various cut-off values: A) 1 kDa, B) 5 kDa, C) 8 kDa, and D) 15 kDa (P=0.09 MPa).
Table 4
The octanolwater partition coefcient (K
ow
) referred to as the logK
ow
for chosen
experimental dyes.
Dye logK
ow
a
Methyl Orange 3.29
Indigo Carmine 1.53
Amido Black 3.37
Titan Yellow 4.75
Direct Black 5.04
a
Calculated with the use of VCCLAB [18].
189 K.M. Majewska-Nowak / Desalination 254 (2010) 185191
The observed unfavorable inuence of anionic surfactant and
mineral salt on anionic dye removal efciency can be explained by
possible molecular interactions. Since the experimental dye and SDS
have the same charge, it can be anticipated that they do not interact
with one another and repulsive electrostatic interactions prevent the
formation of a complex between negatively-charged dye particles and
anionic SDS molecules. Furthermore, a conversion of dye pre-
aggregates to single dye particles, a result of electrostatic repulsion
between dye and surfactant particles, can occur, increasing the dye
concentration in the permeate. It is also well known that the presence
of salts decreases the CMC of ionic surfactant as well as the
concentration at which the pre-micelles can appear (especially at
the near-membrane layer). This salt impact is caused by the
electrostatic shielding effect. As a consequence, a worsening of dye
rejection can be observed. On the other hand, it is likely that particles
of anionic surfactant can play a role similar to that of mineral salts. In
aqueous solutions they probably weaken the membrane charge, but
to a lesser extent due to their low ionic strength.
The effect of mineral salts on the separation efciency of ionic
macroparticles has been investigated by many researchers [1922], but
the reported results are inconsistent. Likely, when feeds of high ionic
strength are treated, the counter ions in the solution (Na
+
or Cl

depending on the pH of treated solution) can shield the surface

membrane charge. Taking into account that the long-term tests were
carried out with aqueous solutions of Direct Black (pHNIEP), it can be
anticipatedthat thepositive salt ions (i.e. Na
+
) inthe solutionwill shield
the negative charge of membrane surface. The neutralization of the
negative charges of anionic compounds by positive cations in the
solution can also be observed. Hence, the electrostatic repulsion
between anionic dye particles, anionic surfactant molecules, and
membrane ionic groups is markedly weakened. As a result, the
molecular sieve effect can be dominant and the membrane selectivity
decreases. Akbari et al. [23] found that salt added to dye solutions
brought about an increase in ionic strength, shielding the membrane
charge. As a consequence, the Donnanexclusioneffect was considerably
reduced; however, the steric effect remained and the dye rejection was
in accordance with the membrane separation characteristics.
4. Conclusions
1. Ultraltration ceramic membranes can be applied in the removal of
organic anionic dyes from aqueous solutions. The membranes are
able to completely retain dyes of molecular weight higher than
600 Da.
2. Transport properties of the ceramic membranes are signicantly
inuenced by the composition of the treated solution. In general, the
presence of mineral salt and anionic surfactant causes a decrease in
membrane permeability.
3. Ceramic membrane permeability and the dye separation factor
remain almost constant during long-termUF irrespective of solution
composition.
4. Ceramic membranes arecharacterizedbyasmall poresizedistribution.
Acknowledgement
This work was supported by a grant from the Department of
Environmental Engineering, Wroclaw University of Technology.
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