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Treatment of model oily waste water by microfiltration

Article  in  Periodica Polytechnica Chemical Engineering · January 2013

DOI: 10.3311/PPch.2166

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Ŕ periodica polytechnica Treatment of model oily waste water by
Chemical Engineering microfiltration
57/1–2 (2013) 21–24
doi: 10.3311/PPch.2166 Zsolt László Kiss / László Talpas / Zita Seres / Sándor Beszédes / Cecília Hodúr /
http:// periodicapolytechnica.org/ ch Zsuzsanna László
Creative Commons Attribution
RESEARCH ARTICLE
Received 2012-12-20, accepted 2013-04-24
Abstract
Microfiltration membranes made from polytetrafluorethylene
(PTFE) have been successfully used for the separation of oily
waste waters by membrane coalescence, but filtration of the oily
waste waters with high emulsifier content have not yet been in-
vestigated. Our aim was to examine the effect of emulsifier con-
tent on membrane coalescence on this type of membrane, and
to investigate the effect of surfactant addition on oil retention
and filtration parameters. It was found that the oil content of
the emulsion can be separated with MF PTFE membranes. Ef-
ficiency of the retention depends on the concentration of emul-
sion: increasing concentrations resulted in an increased reten-
tion. The addition of coagulant also affected filtration param-
eters: higher coagulant concentrations resulted in a significant
increase of the flux, while the retention marginally decreased.
Keywords
microfiltration · hydrophobic membrane · water miscible oil
emulsion
Acknowledgement
The authors are grateful for the financial support provided
by the project IPA Cross-border cooperation program (Serbia-
Hungary) HUSRB 1203/221/196 and the project TÁMOP-
4.2.1/B-09/1/KONV-2010-005 supported by the European Union
and co-financed by the European Regional Fund.
Zsolt László Kiss
László Talpas
University of Szeged, Faculty of Engineering, Moszkvai str, 9., Szeged, H-6725,
Hungary
Zita Seres
Faculty of Technology, University of Novi Sad, Bu. Cara Lazara 1., Novi Sad,
SRB-21000, Serbia
Sándor Beszédes
Cecília Hodúr
Zsuzsanna László
University of Szeged, Faculty of Engineering, Moszkvai str, 9., Szeged, H-6725,
Hungary
Treatment of model oily waste water by microfiltration
Introduction
Oil in water emulsions of waste waters are produced by indus-
tries such as the food industry, and metal-working [1, 2]. How-
ever, they cannot be discharged to the sewer because of a high
oil content and high residual organic pollution [3]. Hence, they
have to be treated in order to obtain a concentrated as possible
oily phase so that the oil and aqueous phase can be reused in
accordance with the regulation levels for industrial wastewater.
However, the conventional methods used for the treatment of oil
emulsions have several disadvantages, such as a low efficiency,
operational difficulties and high operation costs [4,5]. The prob-
lem becomes more pronounced when surfactants are present in
waste water, as these enhance the oily emulsion stability [6].
Several studies have reported on the use of membrane filtration
for the treatment of oil; however most studies focused on the use
of ultrafiltration (UF) and microfiltration (MF) [7]–[10]. Only a
few studies have been performed on the membrane filtration of
high emulsifier-containing oil-in-water (o/w) emulsions. Earlier
studies [4, 11, 12] found that a stable o/w emulsion (the water
miscible cutting oil concentration in the emulsion was 5 wt.%)
could be separated by cross-flow UF, and that the mixing has a
determinant role: the use of a static mixer led to a considerable
increase in the permeate flux.
Microfiltration membranes successfully made from polyte-
trafluorethylene (PTFE) were used for the separation of oily
waste waters by membrane coalescence [6]–[13]. Membrane
surface chemistry, membrane-solute and solute-solute interac-
tions determine the flux and the retention of oil and are the key
to understanding fouling phenomena. During filtration, the oil
droplets accumulate at the surface of the membrane, and the
concentration of the oil may be much higher than in bulk solu-
tion. If the concentration exceeds the critical micelle concentra-
tion (cmc), larger micelles form, which enhances the retention
[14]. The addition of surfactants may change the wettability
of hydrophobic surfaces, like membranes [15], enhancing the
separation efficiency of microfiltration; on the other hand, this
may destabilise the oily emulsions, increasing membrane coa-
lescence [16].
The aim of the present work was to investigate the microfil-
2013 57 1–2 21
tration of a high emulsifier-containing o/w emulsion by PTFE
membrane oil-in-water emulsion using a PTFE microfiltration
membrane, and to investigate the effect of surfactant addition on
oil retention and filtration parameters.
Methods
Microfiltration of oily model solutions
Materials: Model solutions were prepared from water-
miscible stable oil emulsion (MOL Makromil 200) (Table 1)
(denoted WMO), at concentrations of 0.1, 1.0 and 3.0 wt.%, and
a conventional petroleum motor-oil (AGIP 15W-50) (denoted
NWMO) at a concentration of 3.0 wt.%. BOPAC solutions were
made from BOPAC-S (polyaluminium-chloride), (Unichem Kft,
Kistelek, Hungary). Flat-sheet PTFE membranes (0.1 µm) on
PE series (New Logic, USA) were used. The membrane effec-
tive area was 0.001734 m2 .
Tab. 1. MOL Makromil 200 motor-oil content
Content Concentration
Petroleum motor oil (C24 -C50 )
Tetrapropylene succinic acid monobotyl ester
2-hydroxyethyl oleate
Sodium sulphonate
Alcohols, C12 -C16 >98%
2,2’,2”-(Hexahydro-1,3,5-triazin-1,3,5-triyl) triethanol
Experimental design
The MF experiments were carried out in batch stirred cell
(Millipore, Serial No 94) with a capacity of 50 cm3 . Before MF
experiments, the membrane was conditioned with a 1% concen-
tration of isopropyl-alcohol followed by 0.5 hour conditioning
with distilled water. The initial feed volume was 50 cm3 . The
MF experiments were carried out at 0.1 MPa, until 10 cm3 of
the total sample was filtered.
Analytical methods
The measured parameter was the chemical oxygen demand
(COD) retention. Determination of the COD was based on the
standard method involving potassium-dichromate oxidation; for
the analysis, standard test tubes (Lovibond, Tintometer GmbH,
Germany) were used. The digestions were carried out in a COD
digester (Lovibond, ET 108, Tintometer GmbH, Germany), and
the COD values were measured with a COD photometer (Lovi-
bond PC-CheckIt, Tintometer GmbH, Germany). The con-
ductivity was measured by a multiparameter analyser (Consort
C535, Belgium).
In order to investigate the membrane fouling, the different
fouling resistances were calculated on the basis of the resis-
tances in series model. The rate and extent of membrane fouling
and its effect on flux for any given system depends on various
parameters, such as the specific interactions between the mem-
brane surface and various fouling species, hydrodynamic forces
22 Per. Pol. Chem. Eng.
exerted by the flowing fluid and process parameters such as the
cross-flow velocity, TMP, feed concentration, pore size and tem-
perature.
The membrane resistance was calculated as:
∆p
RM = [m−1 ] (1)
Jw ηw
where RM is the membrane resistance, ∆p is the pressure differ-
ence between the two sides of the membrane [MPa], JW is the
water flux of the clean membrane and ηW is the water viscosity
[Pas].
RT is the total resistance [m−1 ], which can be evaluated from
the steady-state flux by using the resistance-in-series model:
RTotal = RM + RF + RP [m−1 ] (2)
where RF is the fouling resistance (mainly by the fouled pores)
[m−1 ] and RP is the polarisation layer resistance [m−1 ].
The resistance of the fouling was determined by measuring
water flux through the membrane after filtration and rinsing it
(wt%)
with deionised water to remove any particles of residue layer
Max. 62 from the surface, by subtracting the resistance of the clean mem-
Max. 6.3
brane:
Max. 12.3 ∆p
RF = − RM [m−1 ] (3)
Max. 4.4 JWA ηW
Max. 6.8
where JWA is the water flux after concentration tests. The resis-
Max. 2.0
tance of the polarisation layer can be calculated as:
∆p
RP = − RF − RM [m−1 ] (4)
JC ηWW
where JC is the constant flux at the end of the concentration and
ηWW is the wastewater viscosity. [17]
0.1 Determination of CMC
The cmc values were determined conductometrically [18] us-
ing a multiparameter analyser (Consort C535). The conductivity
of these solutions was measured at 293 K.
Results and discussion
Conditioning the PTFE membrane
In the first series of experiments, the conditioning of the hy-
drophobic PTFE membrane was investigated in order to make
it useable for the filtration of water-based solutions. The con-
ditioning was carried out in a 1% concentration of isopropyl-
alcohol for 30 min by increasing the transmembrane pressure
(TMP); then, the membrane was conditioned for 30 min in dis-
tilled water. It was found that this is an appropriate method for
wetting the hydrophobic membrane surface.
Comparison of filterability of WMO and NWMO-containing
model waste waters
Relative permeate fluxes (J/Jw ) show the flux decline dur-
ing filtration versus flux of the solvent (distilled water in this
case). The flux of distilled water was 47.18 ± 3.01 L · m−2 h−1 at
0.1 MPa TMP. Relative fluxes of 3% emulsions in the function of
Zs. László Kis et al.
 !1".3$%-.%01$%#02+!0+2$%&'%01$%3$,%,"4$2/%2$#+,0-.3%-.%
"2"B37>2,<=7925<2><2,7>C,&1752,52&73764=>,C:34>M,
1-31$2% ;$2*$"0$% ',+5$#% ".6% ,&<$2% ;&,"2-#"0-&.%
84963764=>?,, !"#$% &'% ()% $*+,#-&./% 01$% &-,% !&.!$.02"0-&.% &.% 01$% !
2$#-#0".!$9%%
3$,% ,"4$2% *"4% $5!$$6% 01$% 7897:)% !*!/% !"+#-.3% "% *
!"(
*+,- !1".3$%-.%01$%#02+!0+2$%&'%01$%3$,%,"4$2/%2$#+,0-.3%-.% 1
!"'
+,- 1-31$2% ;$2*$"0$% ',+5$#% ".6% ,&<$2% ;&,"2-#"0-&.% !
2$#-#0".!$9%% M
!"!#

!"& C
!"% ;
!"$ <
"2"B37>2,<=7925<2><2,7>C,&1752,52&73764=>,C:34>M, ;
!"#
84963764=>?,, *
! *
! $ & ( ) #! #$
*+,-
!"( $%&'(&)*& +,(-. ,
+,-
, Fig.!"'1. Relative permeate flux as a function of permeate volumes of different Fig. 3. Average permeate flux and polarisation layer resistances of model
%
+4M?, of'?,
kinds !"& $29764I2, &23"2762, 89:;, 75, 7, 8:><64=>, =8, =-39%
emulsions. (9% >?$2"3$% ;$2*$"0$% ',+5% ".6% ;&,"2-#"0-&.%
!"!#

waste waters with different WMO concentrations during MF

&23"2762,I=9:"25,=8,C488232>6,U4>C5,=8,2":954=>5?, ,"4$2% 2$#-#0".!$#% &'% *&6$,% <"#0$% <"0$2#% <-01%
!"%
permeate volume are shown in Fig. 1. In the case of WMO, the 6-''$2$.0%@AB%!&.!$.02"0-&.#%6+2-.3%A=9%
!"$
#!!.
relative permeate flux decreases in the first part of the batch, but =-39% concentration. This can probably be explained by oil concen-%
(9% >?$2"3$% ;$2*$"0$% ',+5% ".6% ;&,"2-#"0-&.%
in the!"#0!. part of the batch it increases. This surprising result tration in the polarisation layer. In the case of 0.1 and 1% oil
second ,"4$2%
!""#$%&
emulsions,
2$#-#0".!$#%
'"&the
$'()*+(,%& &'% ',&
*&6$,%
oil concentration
<"#0$% <"0$2#%
-.$/'".+%/(%.',&
does not exceed the'"&
<-01%
012&
cmc, and
can be )!.
explained by interaction between the surfactant compo- 6-''$2$.0%@AB%!&.!$.02"0-&.#%6+2-.3%A=9%
!/!. #-*+3.',3&
the resistance is higher at higher concentrations. In the case of
nents of emulsion and the membrane surface. In the case of
(!.! $ & ( ) #! #$ 3% emulsion, the oil concentration on the gel layer may exceed
NWMO emulsion, a decrease of the relative -. permeates flux was
!""#$%& '"& $'()*+(,%&
cmc, causing ',& -.$/'".+%/(%.',&
in the structure'"&of012&
3.

$ +,(
smooth, as expected. The average retention values show (Fig. 2) , C.%&26$2%0&%-.?$#0-3"0$%01$%$''$!0%&'%!&"3+,".0%&.%&-,%
'!. %&'(&)*& the 12.16% a change the gel
&!. #-*+3.',3&
,that higher
%!.
retention values can be achieved in the case of non- 2$0$.0-&.%
layer, resulting".6% '-,02"0-&.%
in higher ;"2"*$0$2#/%
permeate fluxes DBE>F%
and lower polarisation =
+4M?, '?,
$!.$29764I2,
water-miscible &23"2762,
oil emulsion 89:;, 75, 7,
due to membrane 8:><64=>,
coalescence and=8,!&.!$.02"0-&.% <"#% #$0% 0&% G9H)% ".6% G9()% -.% <"#0$%
resistance.

&23"2762,I=9:"25,=8,C488232>6,U4>C5,=8,2":954=>5?,
phase separation
#!. during filtration. C.%&26$2%0&%-.?$#0-3"0$%01$%$''$!0%&'%!&"3+,".0%&.%&-,%
<"0$2% #&,+0-&.9% C0% <"#% '&+.6% 01"0% 1-31$2% 8
!. 2$0$.0-&.%
!&.!$.02"0-&.#%
Effect of ".6% &'%
coagulant '-,02"0-&.%
on !&"3+,".0% ;"2"*$0$2#/%
microfiltration 2$#+,0$6% DBE>F%
-.%
of WMO emulsions 1-31$2%
#!!. !&.!$.02"0-&.%
2$,"0-?$%
In order ;$2*$"0$% <"#% #$0%
to investigate the0&%effect
',+5$#% G9H)%of ".6%
I=-39% G9()%
JK9%
coagulant on-.%
L1-#% <"#0$%
oil!".%
reten-M$%
%.1+2- %.1*+2- O
0!. <"0$2%
tion and #&,+0-&.9%
filtration C0%
parameters, <"#%
BOPAC '&+.6%
$5;,"-.$6%M4%01$%!&"3+,".0%$''$!0%&'%DBE>F/%<1-!1% 01"0%
concentration 1-31$2%
was set to
41567".8 *
)!. , M2$"N#%
!&.!$.02"0-&.#%
0.5% and 0.3% &'% water
01$% in#0"M,$%
waste !&"3+,".0%
&-,%solution. 2$#+,0$6%
$*+,#-&./% -.%that1-31$2%
!1".3-.3%
It was found 01$%
higher
1
/!. 2$,"0-?$%
concentrations ;$2*$"0$%
of ',+5$#%
coagulant
+4M?, O?, $262>64=>, I79:25, =8, .W, )(_, 7>C, .W, !&*;"!0%#02+!0+2$%&'%01$%;&,"2-#"0-&.%,"4$29%% resultedI=-39%
in JK9%
higher L1-#%
relative !".% M$%
permeate
$
(!.
`)(_,<=>674>4>M,"=C29,07562,076235?, $5;,"-.$6%M4%01$%!&"3+,".0%$''$!0%&'%DBE>F/%<1-!1%
fluxes (Fig. 4). This can be explained by the coagulant effect
<
3.

'!. M2$"N#% !"* 01$% #0"M,$% &-,% $*+,#-&./% !1".3-.3% 01$%

of+,+-
BOPAC, #9/:;<=//!='9/><?@A
which breaks the stable oil emulsion, changing the
&!. #9/:;<=/!=$9/><?@A M
!&*;"!0%#02+!0+2$%&'%01$%;&,"2-#"0-&.%,"4$29%%
compact structure of the polarisation layer.
499",&'%!.-9' -+%' ,-),")&7(&+-)' -)' 9+%&7(&+-)' !")
#9/:;< ;
!"(
8(7(5"&"7#,
$!. +,+- #9/:;<=//!='9/><?@A 0
!"*
!"'
#!.
!")
#9/:;<=/!=$9/><?@A 0
!"&
!.
R>, 612, >2;6, 523425, =8, 2;&234"2>65S, C488232>6, !"(
#9/:;< $
!"%
%.1+2-
<=><2>63764=>5, =8, )(_, 2":954=>, 0232, 8496232C?, %.1*+2- !"' !
!"$
@12, 3254567><25, 0232, <79<:9762C, 41567".87<<=3C4>M, 6=, 612, , !"& -
!"#
3254567><25, 4>, 523425, &
values of "=C29,
3% WMO -Ta?,
and 3%'VG/?,
NWMOR6, 075, 8=:>C, !"%!
+4M?, O?, $262>64=>,
Fig. 2. Retention
I79:25, =8, .W, )(_, 7>C,model
containing
.W, <
6176, 612, C2<94>2, =8, 612, 89:;25, 075, <7:52C, BA,
waste waters
!"$
! $ & ( * #! #$
`)(_,<=>674>4>M,"=C29,07562,076235?, !"# #
B:49C4>M, =8, 612, &=97345764=>, 97A23S, 01492, 612, 2882<6, ./01231451 673 %8
%
!
=8, 8=:94>M, =>, 89:;, C2<327525, 075, >2M94M4B92?, @12, =-39% J9% O$,"0-?$% ;$2*$"0$% ',+5$#% "0% 6-''$2$.0% 6
Effect of-9'
oil concentration on filtration parameters ! $ & ( * #! #$
499",&'
7I237M2, &23"2762,-+%' 89:;,
,-),")&7(&+-)' -)' 9+%&7(&+-)'
7>C, 612, &=97345764=>, 97A23, !&.!$.02"0-&.#% &'% !&"3+,".0% ./ 673 %8 ".6% 7)% @AB%
In the next series of experiments, different concentrations of
8(7(5"&"7#,
3254567><2, I79:25, 732, 51=0>, 4>, +4M?, G?, @12, 89:;, 45, $*+,#-&.#9%
01231451
% 9
WMO emulsion were filtered. The resistances were calculated =-39% J9% O$,"0-?$% ;$2*$"0$% ',+5$#% "0% 6-''$2$.0%
32<4&3=<799A, &3=&=364=>79, 6=, &=97345764=>, 3254567><2S, !&.!$.02"0-&.#% Fig. 4. Relative permeate fluxes at different concentrations of coagulant and
according to the resistances in series model (Eq. 1–4). It was 1% WMO emulsions &'% !&"3+,".0% ".6% 7)% @AB%
32I2794>M,612,2882<6,=8,612,&=97345764=>,97A23,=>,89:;,
R>, 612, >2;6, 523425, =8, 2;&234"2>65S, C488232>6,$*+,#-&.#9% L
found that the decline of the fluxes was caused by building of the 4#%#,%.',&5(+*#3&6*/.,)&17&
C2<94>2?, _>, 612,=8,
<=><2>63764=>5, =6123,
)(_, 17>CS, 612, 89:;,0232, C2<94>2, 7>C, ;
polarisation layer, while the effect2":954=>, 8496232C?,
of fouling on flux decreases
&=97345764=>,
@12, 3254567><25,3254567><2, 45, >=6,
0232, <79<:9762C, &3=&=364=>79, 6=,
6=,=49, N
was negligible. The average permeate flux 7<<=3C4>M,
and the polarisation 612,@1$.% !",!+,"0-.3%
4#%#,%.',&5(+*#3&6*/.,)&17&
Retention values during 01$%
MF 2$0$.0-&.% &'% 01$% &23".-!%
<=><2>63764=>?,
3254567><25, @145,
4>,values
523425, <7>, &3=B7B9A, B2, 2;&974>2C, BA, <
layer resistance are"=C29,
shown in-Ta?,
Fig. 4.'VG/?, R6, 075,
The flux 8=:>C,!&.0$.0%&'%01$%$*+,#-&.%I$5;2$##$6%M4%FBPK/%-0%<"#%
is recipro- When calculating the retention of the organic content of the
=49,
6176, <=><2>63764=>,
612, C2<94>2, 4>,
=8,612,612,&=97345764=>,
89:;25, 075, 97A23?,
<7:52C,R>, 612,
BA,'&+.6% !
cally proportional to polarisation resistance, revealing the effect emulsion01"0%
@1$.% 01$% 2$0$.0-&.%
(expressed
!",!+,"0-.3% by 01$% -.!2$"#$6%
COD),2$0$.0-&.%
it was found &'%<-01%
that the
01$% -.!2$"#-.3%
retention
&23".-!%
<752,
B:49C4>M, =8, X?', 7>C,
=8, 612,layer 'W,
&=97345764=>, =49, 2":954=>5S,
97A23S, 01492, 612, =49, 7
of the polarisation on flux decline. On the other612,
hand,2882<6,
the !&.!$.02"0-&.#%
increased with &'% $*+,#-&.% I=-39% HK9% L1-#% ;2&M"M,4%
increasing concentrations
!&.0$.0%&'%01$%$*+,#-&.%I$5;2$##$6%M4%FBPK/%-0%<"#% of emulsion (Fig. 5).
<=><2>63764=>,
=8, 8=:94>M, =>, C=25,
89:;, >=6, 2;<22C,
C2<327525, 612,
075, <"<S, 7>C,
>2M94M4B92?, 612,
@12, G
flux decline and polarisation resistance is not proportional to oil '&+.6% This probably can be
01"0% 01$% explained-.!2$"#$6%
2$0$.0-&.% by the interactions between the
<-01% -.!2$"#-.3%
3254567><2,45,14M123,76,14M123,<=><2>63764=>5?,R>,612,
7I237M2, &23"2762, 89:;, 7>C, 612, &=97345764=>, 97A23,!&.!$.02"0-&.#% &'% $*+,#-&.% I=-39% HK9% L1-#% ;2&M"M,4% X
3254567><2, I79:25, 732,water
51=0>, 4>, +4M?, G?, @12, 89:;, 45, F
Treatment of model oily waste by microfiltration 2013 57 1–2 23
32<4&3=<799A, &3=&=364=>79, 6=, &=97345764=>, 3254567><2S,
32I2794>M,612,2882<6,=8,612,&=97345764=>,97A23,=>,89:;,
!".% M$% $5;,"-.$6% M4% 01$% -.0$2"!0-&.#% M$0<$$.% 01$%
*$*M2".$%".6%#+2'"!0".0%!&.0$.0%&'%01$%#&,+0-&.Q%-.%
1-31$2% !&.!$.02"0-&.#% &'% @AB% I!&.0"-.-.3% 1-31$2%
!&.!$.02"0-&.#% &'% content
membrane and surfactant #+2'"!0".0#K% 01$% in *$*M2".$%
of the solution; higher con- and its antifouling research, Separation and Purification Technology, 66,

M$!"*$% ,$##% 1462&;1&M-!/% -*;2&?-.3% &-,% 2$0$.0-&.9%% 6 (2009),

centrations of WMO (containing higher concentrations of sur- 347–352.
Hong A, Fane AG, Buford R, Factors affecting membrane coalescence of
factants)
C0% ",#&% the
!".%membrane became
M$% .&0$6% 01"0%less01$%
hydrophobic, improving
!&.6+!0-?-04% &'% oil
01$% stable oil-in-water emulsions, Journal of Membrane Science, 222, (2003),
retention. It also can be noted that the conductivity
;$2*$"0$% -#% 2$,"0-?$,4% 1-31% I2$0$.0-&.% $5;2$##$6% of the per-
19–39.
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