Presented at the International Congress on Membranes and Membrane Processes (ICOM), Seoul, Korea,

2126 August 2005.

0011-9164/06/$ See front matter 2006 Published by Elsevier B.V.
Desalination 191 (2006) 1626
Performance of a crossflow membrane bioreactor (CFMBR)
when treating refinery wastewater
Muhammad Muhitur Rahman, Muhammad H. Al-Malack*
Box 1150, King Fahd University of Petroleum & Minerals, Dhahran 31261, Saudi Arabia
Tel. +966 (3) 860-4735; Fax: +966 (3) 860-3220; email:[email protected]
Received 21 March 2005; accepted 3 May 2005
Abstract
The use of a crossflow membrane bioreactor (CFMBR) in treating wastewater discharged by a petroleum refinery
was investigated. The performance of the CFMBR process was evaluated at MLSS concentrations of 5000 and
3000 mg/l. The process performance was measured in terms of the hydraulic efficiency as well as the COD removal
efficiency. A laboratory-scale experimental set-up comprised mainly of tubular ceramic membranes, aeration tank, and
circulation pump was used throughout the investigation. The results of the investigation showed that a COD removal
efficiency of more than 93% was obtained at both MLSS values. The study also showed that hydraulic retention time
did not have a significant effect on the systems performance. The relationship between permeate flux and crossflow
velocity was found to be best described by a power relationship (J = kV
n
) where constants k and n were affected by
MLSS concentration. The cleaning mechanism investigation showed that cleaning the membrane with an acidic
detergent, Superclean, with a pH value of about 1.5, produced the best results.
Keywords: Crossflow filtration; Membrane bioreactor; Ceramic membrane; Refinery wastewater
1. Introduction
The occurrence of oil-containing wastewater
and the corresponding contamination of water
sources by oil began with the production and
utilization of petroleum and its products. The
*Corresponding author.
major problem of oily wastewater is associated
with its proper disposal. The reclamation and
reuse of wastewater is needed especially in the
oil-producing arid regions due to water scarcity.
With the development of membrane technology,
membrane bioreactors have recently attracted
great attention in the field of industrial waste-
water treatment [15]. The performance of cross-
doi:10.1016/j.desal.2005.05.022
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 17
flow membrane bioreactor (CFMBR) processes
is affected by environmental and operating con-
ditions as measured by the quality and quantity of
permeate [6,7].
Hydraulic retention time (HRT) plays an
important role in the removal of pollutants in
activated sludge processes coupled with mem-
branes. In case of activated sludge systems, it is
a common conviction that with the increase of
HRT, the pollutant removal efficiency of the
system increases. The conflicting scenario is also
available where insignificant improvement was
observed with the variation of HRT [8,9].
The MBR process was found to be useful
when a long solid retention time is required and
physical retention and subsequent hydrolysis are
critical [4]. This process provides benefits over
conventional activated sludge systems in terms of
high effluent quality, reduced sludge wasting and
production, reduced vulnerability to upsets, and
improved biological degradation. It was observed
that the MBR process improved the quality of
degreasing solutions from surface refining pro-
cesses in the metal-working industry. Permeate
was found free of solid matter and hydrocarbon
concentration was reduced by 8590%.
Compared to conventional biological regene-
ration, a five-fold increase in the volumetric
biodegradation rate was achieved due to higher
biomass concentration [10]. In a feasibility study
of applying CFMBR to treat surfactants contain-
ing oil water emulsion, high efficiency (9498%)
in removing COD and TOC was observed at a
MLSS concentration of 48 g/l [11]. In another
study, hydrocarbon aggregation on bacterial flocs
was observed leading to larger particles, which
significantly increased the flux [12].
Fouling of membranes occurs with the appli-
cation of MBR. Fouling depends on the charac-
teristics of foulant and membrane materials. The
major contribution to fouling is the different
solute fractions resulting from activated sludge.
Suspended solid constituents that contribute to
membrane fouling consist mainly of bacterial
flocs with a concentration depending upon the
sludge age, colloids (polymers, fragments of
lysed cells) and dissolved molecules [13]. Many
inorganic elements dissolved in oily wastes can
also play a significant role in fouling membranes.
As a rule, mineral deposits are removed by acidic
solutions, while organic compounds are removed
by alkaline solutions [14]. Chemicals used as
cleaning agent for fouling control of ceramic
membrane include NaOH, HNO
3
, H
2
O
2
, Ultrasil
11, oxalic acid solution, citric acid solution, HCl
solutions and saturated KHCO
3
solutions [1518].
Several investigators studied the performance
of CFMBR in terms of removal efficiencies and
stability of flux with variation of different opera-
ting parameters for treating industrial wastewater
[19,20]. In the literature, there is a lack of
understanding of the interaction between the
biological and filtration unit for treating refinery
wastewater.
Based on the above, the main objective of the
study was to investigate the performance of the
CFMBR process when treating refinery waste-
water at different MLSS concentrations. The
performance of the process was measured in
terms of the hydraulic performance as well as the
COD removal efficiency. Additionally, the effect
of HRT on process performance and the mem-
brane cleaning mechanism was investigated.
2. Materials and methods
2.1. Experimental system
Fig. 1 shows a schematic diagram of the
experimental set-up used throughout the inves-
tigation. It is comprised of two main parts: the
crossflow membrane separation unit and the
activated sludge bioreactor. The effective volume
of the aeration tank was 20 l. The general charac-
teristics of the membrane are shown in Table 1.
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 18
Fig. 1. Schematic diagram of the CFMBR system.
Table 1
Characteristics of the membrane
Configuration Hollow tubular
Material Alumina (ceramic)
Pore size, m 0.2
Outer diameter, mm 10
Inner diameter, mm 7
Length, cm 520
Cross-sectional area, mm
2
38.5
Total surface area, m
2
0.022
Effective surface area, m
2
0.019
Max. thermal stability, EC 120
Max. filtration pressure, bar 15
pH range 114
2.2. Bioreactor feed
The oily wastewater used in the investigation
was collected from a petroleum refinery. The oil
content and COD of oily wastewater were found
to be 16010
3
mg/l and 37010
3
to 2300
10
3
mg/l, respectively. The COD was determined
by a modified approach of the closed reflux
titrimetric method. Essential nutrients such as
glucose, peptone and yeast extract were added to
the bioreactor.
2.3. Experimental Procedure and analytical
methods
Nutrients and oily wastewater were added to
the bioreactor and mixed completely. It is worth
mentioning that nutrients were supplied con-
tinuously while the oily wastewater was pumped
intermittently for 2 min every 2 h. Consequently,
the influent COD calculations were based on the
mass loading per day rather than concentration.
Initially the reactor was seeded using returned
activated sludge that was collected from a muni-
cipal wastewater treatment plant. The circulation
pump was used to pump the MLSS through the
membrane separation unit. Permeate was col-
lected in a permeate tank, while the concentrate
was returned to the aeration tank. Permeate flux
and inlet and outlet pressures were recorded.
The fouled membrane was chemically cleaned
to recover its permeability. The cleaning was
achieved by using three different chemicals,
namely Clorox (5.25% sodium hypochlorite),
Persil (washing detergent) and Superclean (acidic
detergent with a pH range of 1.411.48). The
chemicals were used individually and in com-
bination with each other, followed by water rins-
ing. Flux recovery (J
cleaned
/J
uncleaned
) was calculated
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 19
Table 2
Analytical methods of various parameters
Parameter Technique Methods
Turbidity Nephelometric SM-2130B
pH Potentiometric SM-4500-H
+
MLSS Filtration 4.5 m SM-2540D
DO Oxygen Probe SM-4500-O G
COD Closed reflux SM-5220C
BOD 5 days SM-5210B
TOC Combustion infrared SM-5310B
Phenol Mass spectrometric SM-6420C
Oil and grease Gravimetric EPA 1664
Ammonia Ion selective
electrode
SM-4500-NH
3
D
Microbial Heterotrophic plate
count
SM-9215B
based on the permeate flux of the cleaned and
uncleaned membranes [14].
During the experimental period, samples from
the bioreactor and permeate were collected
periodically and analyzed for different physical
and chemical parameters by standard analytical
methods [21]. Table 2 shows the analytical
methods used in this study.
3. Results and discussion
3.1. Hydraulic performance of the process
The hydraulic performance was assessed by
investigating the effect of operating conditions on
flux rate of the membrane unit. In the study of a
crossflow filtration system, selection of the circu-
lation pump plays a significant role. The pump is
responsible for maintaining sufficient transmem-
brane pressure (TMP) as well as flow, which are
directly related to the variation of flux. At the
beginning of this study (1st to 12th day), a pump
with a cast iron impeller was used for circulation
purposes. When not in operation, the impeller of
the pump becomes corroded. In this case and
when the pump was used, an enormous quantity
of fine particulates was noticed to be produced
and came in contact with the membrane, which
resulted in rapid membrane fouling. This pheno-
menon can be observed in Fig. 2 where the
variation of flux, TMP and the MLSS during the
whole study period are shown.
The data presented in this figure were
recorded from the beginning of the operation. The
above-mentioned reason might be the cause of
lower initial maximum flux (65 l/m
2
/h on the first
day) than the latter part of the study period (123,
123, 140 and 114 l/m
2
/h on the 13th, 26th, 29th
and 83rd days, respectively) when the pump with
a plastic impeller was used.
The variation of flux showed a decreasing
pattern that can be attributed to membrane foul-
ing. When the flux dropped below the critical
level (35 l/m
2
/h), the membrane unit had to
undergo chemical cleaning.
For the determination of MBR performance,
HRT is a key issue. The system was operated at
an average HRT of 21 h. During most of the
experimental period, it was observed that the flux
increased with the increase of pressure and vice
versa. This phenomenon can be observed in
Fig. 2 where, before the 47th day, the flux had a
decreasing pattern that increased suddenly when
the pressure increased from 12.1 to 18.6 psi.
Similar phenomena were observed on the 40th
and 74th days.
Thus, in this case the flux can be described as
pressure dependent, but some exceptions were
also found. From the 83rd to the 92nd day the
flux declined exponentially even though the pres-
sure remained constant. This might happen solely
because of fouling of the membrane, and the flux
can be described as pressure independent.
Throughout the study period, the TMP varied
within a range of 11.5 to 24.0 psi.
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 20
Fig. 2. Variation of cumulative flux, TMP and MLSS with time.
The biomass content of the reactor was
measured twice a day. One measurement was to
monitor the MLSS concentration present in the
reactor and then calculate the volume of MLSS to
be wasted in order to keep the suspended solids
around 5000 or 3000 mg/l. The other measure-
ment was taken after the wasted volume was
replaced by tap water in order to check the
adjusted MLSS concentration. For that reason,
the variation of MLSS in Fig. 2 has a crisscross
shape. In this regard it should be mentioned that
the error associated for replacing the MLSS by
tap water was not calculated in this study. In
Fig. 2 a decreasing shape of MLSS variation is
observed during the period of the 29th to the 34th
day. The reason behind this is the excessive foam
that occurred in the reactor. The foam was full of
attached biomass and carried a considerable
amount of MLSS out of the reactor.
Sometimes, at the beginning of the run and
after cleaning, the flux was found to decrease
sharply with time, which is a classic phenomenon
in membrane filtration, but later the flux started to
recover slightly. This increase in flux could be
attributed to the increase in temperature. This
increase in temperature resulted in a reduction in
viscosity of the fluid, thus allowing more fluid to
pass through.
To keep the aerobic condition in the bio-
reactor, air was supplied continuously and the
dissolved oxygen (DO) was measured frequently
using a DO probe. The DO level was never less
than 4.0 mg/l, which shows that aeration provided
in the reactor was in excess of the DO require-
ment. The pH of the aeration tank content was
also within the limit of 6 to 8, which ascertains
the suitable condition for biomass growth.
3.2. COD removal efficiency
During the same set of experiments, the
performance of the CFMBR was studied to
assess the ability and stability of the system to
provide the required COD removal efficiency. At
the beginning of the study, the MLSS concen-
tration was maintained at 5000 mg/l. The liquor
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 21
Fig. 3. Variation of influent and effluent organic mass loading at MLSS 5000 and 3000 mg/l, respectively, with time.
was light brown in color and made up of
dispersed non-flocculent particles. Fig. 3 repre-
sents the variation of influent and effluent mass
loading at MLSS value of 5000 and 3000 mg/l,
respectively. The influent mass loading was
calculated as follows:
Mass loading = [Concentration of oily waste
(mg/l) flowrate of oily waste (l/d)]
+ [Concentration of nutrient (mg/l)
flowrate of nutrient (l/d)]
The influent mass loading presented in Fig. 3
is the average of the mass loading applied during
a certain period of time needed for getting the
steady-state condition at each adopted loading.
When the steady-state period was obtained, the
flowrate of oily waste was increased to get a
higher mass loading. However, oil flowrate was
insignificant to the total feed flow and did not
affect the permeate flux and HRT. The variation
of influent substrate can be clearly noticed by a
steady horizontal line. To keep a resemblance, the
effluent loading is also presented in average
values. The sharp peaks in the permeate COD are
due to the sudden increase in influent COD
concentration. Occasionally it was found that the
increase of effluent COD due to the change of
influent loading was not rapidly responding and
was apparent after one or two days. On the 42nd
day, the effluent loading was noticed to be lower
than the previous days, although the influent
loading increased, and the effluent COD concen-
tration remained the same. This was due to the
calculation of the effluent mass loading with a
lower volume of effluent (due to low flux) at this
higher adopted loading stage.
The influent mass loading at MLSS of
5000 mg/l varied from 24 to 67 g/day. The COD
removal efficiency ranged from 82 to 97% with
an average of 93%. Performance of the unit when
operated with MLSS of 3000 mg/l was impres-
sive with changing the influent mass loading from
30 to 65 g/day (Fig. 3). The average COD
removal efficiency at this MLSS (3000 mg/l) was
94%. The food to microorganism (F/M) ratio
during the whole study period was found to range
between 0.20 and 1.15 d
!1
.
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 22
3.3. Effect of HRT on the performance of the
process
Experiments were carried out to investigate
the effect of variation in HRT on the system
performance in terms of flux stability and COD
removal efficiency at different MLSS concen-
trations. To calculate the HRT, the following
formula was used:
HRT = [Reactor Volume] / [Permeate Flux
Membrane Surface Area]
The experiments were conducted at three HRT
values. After finishing each experiment, the
membranes were cleaned to restore the flux. The
experiment began with the MLSS concentration
of 5000 mg/l. The corresponding average HRTs
were 17, 22, and 34 h, and CFVs were 3.24, 2.69,
and 2.21 m/s. To find the COD removal per-
formance of the system, various organic mass
loadings were applied under different HRT con-
ditions. The system was put in with an average
influent mass loading of 42.75, 40.78 and
35.86 g/day that resulted in the effluent mass
loading of 2.66, 2.45 and 1.71 g/day at the HRTs
of 17, 22 and 34 h, respectively. Fig. 4 presents
the COD removal efficiency for different HRTs
at the MLSS of 5000 mg/l. Although the highest
removal efficiency (95%) was observed at the
HRT of 34 h, the removal efficiencies at HRTs of
22 and 17 h were very close (94%) to this value.
Therefore, it can be postulated that HRT did not
affect the system in COD removal efficiency,
which varied in a narrow range of 9395%.
After finishing the experiment at the MLSS
value of 5000 mg/l, the biomass was treated to
maintain an MLSS concentration of 3000 mg/l.
At this MLSS concentration, the HRTs were 16,
20, and 33 h and CFVs were 3.39, 2.76, and
2.25 m/s. The system was fed with an average
influent mass loading of 42.75, 39.97 and
36.35 g/d resulting in the effluent mass loadings
of 2.61, 2.26 and 1.84 g/d, respectively.
Fig. 5 shows the COD removal efficiency for
different HRTs at a MLSS of 3000 mg/l. The
highest removal efficiency (95%) was observed at
the highest HRT of 33 h. The removal efficiency
at rest of the HRT values remained same as
previously (94%). It was observed that COD
removal efficiency is independent of HRT at
different MLSS concentrations in this study. This
might happen because the adopted HRTs were
too close to each other to demonstrate the varia-
tion in COD removal efficiency, and the experi-
ments ran for a short time to allow degradation of
the high-molecular-weight compound derived
from the oily waste.
Fig. 4. COD removal efficiency with time at different HRTs at MLSS 5000 mg/l.
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 23
Fig. 5. COD removal efficiency with time at different HRTs at MLSS 3000 mg/l.
To investigate the effect of CFV on the
hydraulic performance of the process, flux was
correlated with CFV described by the following
power relation [22]:
J = kV
n
where J is the permeate flux (l/m
2
/h), V is the
crossflow velocity (m/s), and k and n are con-
stants. To find k and n, the steady-state flux
values were used at the corresponding MLSS
concentration and CFV value. The values of
(log J) were plotted against (log V), and by linear
regression k and n were determined. The values
of k were 11.30 and 11.03, while the values of n
were 1.75 and 1.6 at the MLSS concentrations of
3000 and 5000 mg/l, respectively.
It can be seen that as the MLSS concentration
increased, the values of k and n decreased. Since
two MLSS concentrations were investigated, the
relationship between the MLSS concentration and
the constants k and n was not developed. It is
worth mentioning that the values of constants k
and n may only be used with this type of mem-
brane and under similar conditions.
3.4. Permeate quality
Throughout the study period, different para-
meters indicating the quality of permeate were
Table 3
Summary of permeate quality parameters
Parameter Range Mean
value
BOD, mg/l 0.21.2 0.8
COD, mg/l 68220 105
TOC, mg/l 10.431.3 19.2
Phenol, mg/l 0.853.75 1.95
Oil and grease, mg/l 1.13.5 2.04
Ammonia, mg/l 0.2121.23 7.88
Turbidity, NTU 0.210.97 0.40
Heterotrophic plate
count, CFU/ml
1.910
3
6.910
3
4.410
3
examined. The summary of organic constituent
analyses is shown in Table 3. To find the viable
bacterial count in the reactor as well as permeate,
a heterotrophic plate count method was adopted.
Following the incubation, two types of surviving
colonies were found, i.e., large spongy-white
colonies and small whitish-yellow colonies. On
average, one log reduction in permeate colony
forming units was observed during the experi-
mental period.
3.5. Membrane fouling control
At the beginning of the study, the cleaning
procedure was attempted by the use of Clorox
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 24
Fig. 6. Variation of flux before and after cleaning with PersilClorox and Superclean.
Fig. 7. Summary of the cleaning procedure with PersilClorox and Superclean.
only. The cleaning process continued for about
10 h to restore the flux of the new membrane.
Although cleaning the membrane with Clorox
restored the flux significantly, the cleaning time
was not satisfactory. To obtain a reasonable
cleaning time it was decided to use Persil and
Clorox in different sequences followed by water
rinsing, but this did not improve the cleaning
time. Another cleaning agent, Superclean, fol-
lowed by a backwash, was tested to improve the
cleaning time and the flux restoration. It can be
observed in Fig. 6 that washing the membrane
with Superclean caused the peak flux to be
constant for around 27 h, thus establishing a
wider peak than the previous cleaning agents
(Persil and Clorox). In relation to cleaning time,
M.M. Rahman, M.H. Al-Malack / Desalination 191 (2006) 1626 25
the Superclean needed 85% less time than that of
the other cleaning agents (Fig. 7). Therefore,
chemical washing with Superclean was regarded
as the best solution for fouling control and was
adopted as the cleaning technique throughout the
study period.
4. Conclusions
The performance of a laboratory-scale cross-
flow MBR treating wastewater discharged by a
petroleum refinery was investigated. The study
showed that a COD removal efficiency of more
than 93% was obtained, and removal efficiency
was not significantly affected by the increase in
MLSS concentration.
The fluxCFV relationship was best described
by a power relationship whose constants were
found to be affected by MLSS concentration. The
study also showed that COD removal efficiency
was independent of HRT.
Chemical cleaning of the membrane with the
acidic detergent Superclean, followed by a back-
wash, was found to produce the best results in
terms of cleaning time and recovered flux.
Acknowledgements
The authors would like to thank King Fahd
University of Petroleum & Minerals (Dhahran,
Saudi Arabia) for financial and technical support.
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