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JTICE-876; No. of Pages 5

Journal of the Taiwan Institute of Chemical Engineers xxx (2014) xxx–xxx

Contents lists available at ScienceDirect

Journal of the Taiwan Institute of Chemical Engineers

journal homepage: www.elsevier.com/locate/jtice

Micellar-enhanced ultrafiltration of soft drink wastewater using

anionic and mixed anionic/nonionic surfactants
Hamed Azizi Namaghi a,b, Seyed Mahmoud Mousavi a,*
a
Department of Chemical Engineering, Faculty of Engineering, Ferdowsi University of Mashhad, Mashhad, Iran
b
Research Center of Membrane Processes and Membrane, Faculty of Engineering, Ferdowsi University of Mashhad, Mashhad, Iran

A R T I C L E I N F O A B S T R A C T

Article history: In the present study, micellar-enhanced ultrafiltration (MEUF) of soft drink processing wastewater using
Received 27 October 2013 sodium dodecyl sulfate (SDS) surfactant and mixture of this surfactant with Triton X-100 (TX-100)
Received in revised form 4 March 2014 surfactant is investigated. The experiments were conducted to evaluate the effect of operating time,
Accepted 23 March 2014
surfactant concentration, transmembrane pressure (TMP), and TX-100/SDS molar ratio on the process
Available online xxx
performance. The results show that the flux is decreased by increasing SDS concentration, TX-100/SDS
molar ratio and operating time and decreasing TMP. Furthermore, increasing TX-100/SDS molar ratio
Keywords:
increases the rejections of total dissolved solids (TDS) and chemical oxygen demand (COD).
MEUF
ß 2014 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Mixed surfactants
Critical micelle concentration
Permeate flux
Rejection

1. Introduction osmosis (RO) membrane systems [7,10,11]. As a matter of fact,

Food processing industries generate relatively large amounts of
wastewater with highly variable characteristics. The wastewater
resulting from soft drink processing factory can have high values of
pollution indices such as COD and turbidity. Consequently, the
treatment is often required before discharging this wastewater to
either a receiving environment or the sewer [1,2]. Over the past
few decades, MEUF has been one of the alternative membrane
separation techniques where the performance of ultrafiltration
(UF) is improved by the formation of surfactant micelles in order to
remove various organic and inorganic contaminants [3–6]. In this
process, surfactants monomers play a vital role to aggregate and
form large micelles (spherical or cylindrical) above critical micelle
concentration (CMC) [3,7–9]. Organic compounds can be solubi-
lized in various sites in micelles such as inner core of micelles,
palisade layer and between the hydrophilic head groups; while
inorganic contaminants can be bound on the surface of oppositely
charged micelle [3,5]. In such circumstances, the diameter of
micelle containing contaminants is larger than the pore diameter
of UF membrane and consequently it is rejected by the membrane
using UF system which has higher flux, lower energy consumption
and less operating pressure than nanofiltration (NF) or reverse
* Corresponding author. Tel.: +98 511 8816840; fax: +98 511 8816840.
E-mail address: mmousavi@um.ac.ir (S.M. Mousavi).
MEUF is an alternative process to overcome the intrinsic
limitations of NF and RO processes [7,10].
So far, the use of MEUF process for removal of Zn [9,12,13], Cd [13–
15], Ni [16], Cu [17], Pb [18,19], Cr [20], di-butyl phosphate (DBP), tri-
butyl phosphate (TBP) and uranyl ions [21], adsorbable organic
halogens (AOX) [22], methylene blue [23,24], eosin [25], Safranin T
[26], naphthenic acids [27], chromate and nitrate [28], phenol/Cd [4],
phenol/Cu [29], etc. from aqueous solutions or wastewaters has been
investigated by researchers. Moreover, a few researches have been
done for treatment of different real wastewaters such as olive mill
[30], raisin [8], and edible oil [31] using MEUF process.
The aim of the present paper is to treat soft drink processing
wastewater by MEUF process. The effect of different parameters is
investigated on the flux and rejection of COD, TDS, and turbidity as
the pollution indices. The parameters of operating time, surfactant
concentration, TMP, and TX-100/SDS molar ratio are considered in
the present study.
2. Materials and methods
2.1. Materials
Wastewater used in the present study was sampled from a local
soft drink factory. The values of COD, TDS, and turbidity of the
wastewater were in range of 6900–7500 mg/l, 900–1800 mg/l,
and 2000–3000 NTU, respectively. SDS as an anionic surfactant and

http://dx.doi.org/10.1016/j.jtice.2014.03.015
1876-1070/ß 2014 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Please cite this article in press as: Namaghi HA, Mousavi SM. Micellar-enhanced ultrafiltration of soft drink wastewater using anionic
and mixed anionic/nonionic surfactants. J Taiwan Inst Chem Eng (2014), http://dx.doi.org/10.1016/j.jtice.2014.03.015
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JTICE-876; No. of Pages 5

2 H.A. Namaghi, S.M. Mousavi / Journal of the Taiwan Institute of Chemical Engineers xxx (2014) xxx–xxx

TX-100 as a nonionic one were supplied from Merck. The values of 450
CMC of SDS and TX-100 are 8.15 [9] and 0.25 mM [4], respectively. C=0 mM
400 C=3 mM
Sodium hydroxide, hydrochloric acid and distilled water were used
C=6 mM
for removal of membrane fouling. PAN-350 polyacrylonitrile flat
350 C=9 mM
membrane, used in the experiments, was prepared from Sepro. As C=12 mM
reported by the supplier, this membrane has provided 80% 300

Stable flux (lit/m2.h)

rejection for 20 kDa poly(ethylene glycol). The membrane thick-
ness is 0.165 mm. Maximum process temperature for this 250
membrane is 100 8C.
200
2.2. Experiments
150
All MEUF experiments were carried out by a cross-flow
100
experimental setup, shown in Fig. 1, in a batch mode with total
recycle of the retentate (stream 10) and permeate (stream 9) in order
50
to maintain constant feed concentration. The effective membrane
area in the module was 70.88 cm2. The temperature was kept 0
constant at 25  2 8C. The experiments were done using an initial feed 0 5 10 15
volume of 8000 ml. In preparation of the feed solutions, the surfactant t (min)

with predetermined concentration was added into 1000 ml wastewater
and mixed completely for about 10 min using a magnetic stirrer at a
constant speed of 600 rpm. After that, the solution was added to 7000 ml
wastewater and stirred at a constant speed of 110 rpm for about 10 min
to obtain effective agitation. Finally, the feed was settled down
approximately for 90 min and then was subjected to the UF system.
After each experiment the membrane was washed in order to
overcome its fouling. For this purpose, the membrane was
thoroughly and successively washed with distilled water, 1%
sodium hydroxide solution, distilled water, 0.1 M hydrochloric
acid solution and distilled water and finally was placed into the
digital ultrasonic bath (PS-30A) and was sonicated. It should be
noted that, after each cleaning process, the pure water flux of the
membrane was determined with using distilled water and if it was
different from its original value, the membrane would be replaced
by a new one.
In this set of experiments, the rejection value of three pollution
indices i.e. COD, TDS, and turbidity was determined via the
measurement of their concentration in the feed and permeate. In
this regard, the rejection percent (%R) was determined using the
following equation in order to evaluate the filtration efficiency:
 
Ip
%R ¼ 1  100
If
where Ip and If are the values of COD, TDS, and turbidity in the
permeate and feed, respectively [8]. The TDS value of the feed and
permeate was measured by Extech EC-400 (USA) electrical
conductivity meter. A thermoreactor (RD125) for heating and
digestion of COD vials solution, as well as COD photometer,
supplied from Lovibond Tintometer (Germany), was used to
Fig. 2. Effect of operating time on permeate flux in various SDS concentrations and
TMP = 3 bars.
measure the COD value. Lutron Electronic turbidity meter (TU-
2016, Taiwan) was applied to measure the turbidity value.
3. Results and discussion
3.1. Effect of different parameters on permeate flux
In pressure driven membrane processes, realization of phe-
nomena of fouling and concentration polarization is vital for
conducting a precise assessment of the process. In this regard,
variation of the permeate flux in terms of time at various SDS
concentrations (mM) and TMP of 3 bars (the optimum pressure in
which the maximum rejection was achieved) is depicted in Fig. 2.
According to this figure, there was a high flux in the beginning of
the process, but during a short period of time (up to 4 min), the
permeate flux declined quickly. This trend is attributed to
concentration polarization and accumulation of retained micelles
on the membrane surface and consequently the increase of
resistance against of the flux [4,9]. Finally, the variations of the
permeate flux decreased and it approached steady state.
(1)
The effect of feed SDS concentration (mM) and TMP (bar) on
stable or steady state permeate flux is shown in Fig. 3. With respect
80
TMP=2 bars
75 TMP=2.5 bars
TMP=3 bars
70
TMP=3.5 bars
TMP=4 bars
65
Stable flux (lit/m2.h)

60

55

50

45

40

35

30
Fig. 1. Schematic diagram of experimental setup: (1) feed reservoir, (2) water bath, 0 2 4 6 8 10 12
(3) pump, (4) valve, (5) heat exchanger, (6) thermometer, (7) pressure indicator, (8) SDS concentration (mM)
membrane module, (9) permeate stream, (10) retentate stream, and (11) bypass
line. Fig. 3. Effect of SDS concentration and TMP on stable flux.

Please cite this article in press as: Namaghi HA, Mousavi SM. Micellar-enhanced ultrafiltration of soft drink wastewater using anionic
and mixed anionic/nonionic surfactants. J Taiwan Inst Chem Eng (2014), http://dx.doi.org/10.1016/j.jtice.2014.03.015
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90 99.55

80 99.5

70 99.45

Turbidity rejection
COD rejection

99.4
60

99.35
50
TMP=2 bars
TMP=2 bars TMP=2.5 bars
TMP=2.5 bars 99.3 TMP=3 bars
40 TMP=3 bars TMP=3.5 bars
TMP=3.5 bars TMP=4 bars
TMP=4 bars 99.25
0 2 4 6 8 10 12
30
0 2 4 6 8 10 12 SDS concentration (mM)
SDS concentration (mM)
Fig. 6. Effect of SDS concentration and TMP on turbidity rejection.
Fig. 4. Effect of SDS concentration and TMP on COD rejection.

to this figure, the stable flux decreases when the SDS concentration
increases, but this decrease is more severe in the concentrations
below the CMC. At this section, concentration polarization, the
membrane fouling and the adsorption of surfactant on the
membrane surface result in the flux decrease [9,32]. Above the
CMC, formation of the deposited layer of micelles over the
membrane surface and consequently increase of the resistance
reduces the flux [23,32]. Regarding Fig. 3, the increase of the stable
flux with increasing TMP is due to increase in the driving force [33].
3.2. Effect of SDS concentration and TMP on rejection of the
wastewater pollution indices
Figs. 4–6 describe the effect of SDS concentration and TMP on
the rejection of the wastewater pollution indices. To find out the
optimum conditions of TMP and SDS concentration in order to
achieve the maximum separation, the concentration of SDS in the
feed was varied from 0 to 12 mM while TMP was changed from 2 to
4 bars. The results show that UF process without the surfactant can
not effectively decrease COD and TDS of the wastewater.
Theoretically, at the SDS concentrations below CMC, surfactants
are present in monomer form and no micelles are formed in the
60
55
50
45
40
TDS rejection
bulk solution. Nevertheless, a considerable rise in the rejections
was observed when the SDS concentrations were below the CMC.
This unusual behavior is due to the concentration polarization
phenomenon. In this status, monomers of the surfactant accumu-
late at the concentration polarization layer and therefore, the SDS
concentration reaches above the CMC in this layer and the micelles
are formed to trap the contaminants [9,19].
According to Figs. 4–6, by increasing TMP in low SDS
concentrations, the rejections are improved likely due to the
formation of thicker cake layer at higher applied pressures [34]. On
the other hand, UF is a pressure-driven membrane process in
which operating pressure has a positive effect on the passage of
water and other components through the membrane. However, by
increasing the TMP the flux of components remains lower than that
of water which leads to the rejection increase [8,31]. Unfortunate-
ly, at high concentration of the surfactant, the micelles became
compact and their solubilization capacity decreased at high TMPs
and also they were degraded and consequently the role of them in
reduction of pollutants decreased [8,31,35,36]. The results show
that the maximum rejections are almost obtained at TMP of 3 bars
and SDS concentration of 9 mM.
As shown in Fig. 6, in the presence or absence of SDS surfactant,
the turbidity rejection is above 99%. It means that the turbidity is
well removed by UF and adding the surfactant does not have a
noticeable effect on the turbidity removal.
3.3. Effect of TX-100/SDS molar ratio on the flux and rejection of the
pollution indices
The CMC of anionic surfactants is high. As a result, great values
of anionic surfactants are necessary in order to achieve the

appropriate rejection. Using these surfactant values makes the

35
MEUF process less economical. Therefore, the MEUF process using
30 the mixture of ionic and nonionic surfactants was applied for
separation of the contaminants. The variation of permeate flux
25 versus TX-100/SDS molar ratio is shown in Fig. 7. The results reveal
TMP=2 bars
that when the TX-100/SDS molar ratio increases from 0 to 0.8 at a
20 TMP=2.5 bars
TMP=3 bars
fixed SDS concentration of 6 mM, the decline in the flux occurs due
15 TMP=3.5 bars to the membrane fouling and solution viscosity [9]. At the same
TMP=4 bars time, the rejections of COD, TDS and turbidity increase as shown in
10 Figs. 8–10. In fact, increase of the rejections is the result of CMC
0 2 4 6 8 10 12
decrease because of increasing the concentration of the nonionic
SDS concentration (mM)
surfactant and thus, the participation of more SDS molecules in the
Fig. 5. Effect of SDS concentration and TMP on TDS rejection. micelle formation [9]. Addition of the nonionic surfactant is not

Please cite this article in press as: Namaghi HA, Mousavi SM. Micellar-enhanced ultrafiltration of soft drink wastewater using anionic
and mixed anionic/nonionic surfactants. J Taiwan Inst Chem Eng (2014), http://dx.doi.org/10.1016/j.jtice.2014.03.015
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56 99.6
TMP=2.5 bars
TMP=3 bars
54 TMP=3.5 bars 99.55

52

Turbidity rejection
Stable flux (lit/m2.h)

99.5

50
99.45

48

99.4
TMP=2.5 bars
46
TMP=3 bars
TMP=3.5 bars
99.35
44 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Molar ratio (CTX100/CSDS)
TX100 SDS
Molar ratio (C /C )
Fig. 10. Effect of TX-100/SDS molar ratio and TMP on turbidity rejection.
Fig. 7. Effect of TX-100/SDS molar ratio and TMP on stable flux.

very effective on the turbidity rejection due to the high desirable

76 results of the turbidity rejection using UF process.

74
4. Conclusions

MEUF process was applied for treatment of wastewater of soft

72 drink processing industry. The effect of SDS concentration, TMP,
and TX-100/SDS molar ratio was investigated on the flux and
COD rejection

70 rejection percent of COD, TDS, and turbidity as the pollution

indices. According to the results, increasing SDS concentration,
operating time and TX-100/SDS molar ratio decreased the flux,
68
while increasing TMP enhanced it. Rejection of TDS and COD was
mostly increased by increasing SDS concentration and TX-100/SDS
66 molar ratio, but these two parameters did not affect turbidity
rejection very much due to high rejection of turbidity by UF
TMP=2.5 bars process. The best rejection values of COD, TDS, and turbidity using
64
TMP=3 bars SDS surfactant were almost 81.3%, 56.7% and 99.5%, respectively;
TMP=3.5 bars therefore, MEUF could effectively treat the aforementioned
62 wastewater.
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
Molar ratio (CTX100/CSDS)
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and mixed anionic/nonionic surfactants. J Taiwan Inst Chem Eng (2014), http://dx.doi.org/10.1016/j.jtice.2014.03.015
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