Journal of Environmental Chemical Engineering 2 (2014) 56–62

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Journal of Environmental Chemical Engineering

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

Evaluation of a three-step process for the treatment of petroleum refinery

wastewater
Muftah H. El-Naas *, Manal Abu Alhaija, Sulaiman Al-Zuhair
Chemical and Petroleum Engineering Department, UAE University, P.O. Box 15551, Al-Ain, United Arab Emirates

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

Article history: In this study, a novel three-step process was developed and evaluated for the treatment of highly
Received 29 July 2013 contaminated refinery wastewater. The process consisted of an electrocoagulation cell (EC), a spouted
Accepted 25 November 2013 bed bioreactor (SBBR) with Pseudonymous putida immobilized in polyvinyl alcohol gel, and an adsorption
column packed with granular activated carbon produced from agricultural waste, specifically date pits.
Keywords: The units were evaluated individually and as combinations with different arrangements at different
Petroleum refinery wastewater operating conditions to treat refinery wastewater with varying levels of contaminants. The EC unit was
Electrocoagulation
found to be effective as a pretreatment step to reduce the large concentrations of COD and suspended
SBBR
Adsorption
solid and reduce the load on the bioreactor and the adsorption column. At optimum conditions and unit
COD arrangement, the process was able to reduce the concentration of COD, phenol and cresols by 97%, 100%
Phenol and 100%, respectively. The process was found to be highly competitive in comparison with other
combined systems used in the treatment of industrial wastewater and can handle highly contaminated
refinery or industrial wastewater with relatively wide range of operating conditions.
ß 2013 Elsevier Ltd. All rights reserved.

Introduction In petroleum and petrochemical industries, there is strong

With the remarkable economic growth envisaged in the world
nowadays, concerns are raised about many environmental
challenges. In petroleum and petrochemical industry, more than
2500 useful petroleum products are produced from crude oil [1]
and the annual worldwide consumption of petroleum hydro-
carbons is estimated to be approximately 1012 US gallons [2].
Depending on the size, type of crude oil, products and complexity
of operation, a petroleum refinery can be a large consumer of water
and can generate significant volumes of wastewater. The estimated
average water consumption in processing a barrel of crude oil is
65–90 gallon (246–341 L) [3]. Approximately 0.4–1.6 times the
volume of the processed crude oil is discharged as petroleum
refinery wastewater [4]. Thus, based on the current yield of 84
million barrels per day (mbpd) of crude oil, a total of 33.6 mbpd of
effluent is generated globally [5]. World oil demand is expected to
rise to about 107 mbpd over the next two decades, and oil will
account for 32% of the world’s energy supply by 2030 [5]. These
data clearly indicate that effluents from the oil industry will
continually be produced and discharged into the world’s main
water bodies.
* Corresponding author. Tel.: +971 3 713 5188; fax: +971 3 713 5188.
E-mail address: muftah@uaeu.ac.ae (M.H. El-Naas).
interest in improving wastewater management by optimizing
water use and introducing recycling technologies in production
units. In general, refinery wastewater contains many and diverse
contaminants, several inorganic substances, such as Mg2+, Ca2+,
S2 , Cl , and SO42 that upgrade the mineralization of water;
emulsified oil and grease, phenols, cresols, sulfides, ammonia and
cyanides contribute to the chemical oxygen demand (COD). As a
result, an effective approach should be developed to face stringent
environmental regulations on the quality of effluent discharged for
recycling purposes [6]. Table 1 summarizes the main pollutants in
different petroleum refining units.
The traditional treatment of refinery wastewater is based on
physicochemical, mechanical methods and further biological
treatment in the integrated activated-sludge treatment unit.
Several solutions are proposed including electrocoagulation
[1,7,8], photocatalytic oxidation [9], wet oxidation [10], photo-
degradation [11], catalytic vacuum distillation [6], coagulation–
flocculation [12,13], fenton oxidation [14], adsorption [15,16],
biodegradation [17], membrane [18] and membrane bioreactor
[19–21], ultrasound [22] and chemical precipitation [23]. Howev-
er, because of the variability of refinery wastewater composition,
the traditional methods become inadequate and could not be used
individually in full scale. So, there is still a need for advanced
techniques to remove non-biodegradable, high concentration
organic substance of petroleum refinery wastewater [10]. In other
words, researchers are attempting to design a combination of

2213-3437/$ – see front matter ß 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.jece.2013.11.024
 M.H. El-Naas et al. / Journal of Environmental Chemical Engineering 2 (2014) 56–62 57

Table 1 Table 2
Major water sources in petroleum refining process [3]. Characteristics of refinery wastewater samples as ranges of values.

Unit Wastewater main pollutants Parameter Value

Crude desalting Free oil, ammonia, sulfides and suspended solids pH 8.3–8.9
Crude oil distillation Sulfides, ammonia, phenols, oil, chloride, mercaptans Conductivity (mS/cm) 5.2–6.8
Thermal cracking H2S, ammonia, phenols Total suspended solid (g/l) 0.03–0.04
Catalytic cracking Oil, sulfides, phenol, cyanide, ammonia Total dissolved solid (g/l) 3.8–6.2
Hydrocracking High in sulfides SO4 (mg/l) 14.5–16
Polymerization Sulfides, mercaptans, ammonia COD (mg/l) 3600–5300
Alkylation Spent caustic, oil, sulfides Total phenol (mg/l) 160–185
Isomerization Low level of phenols Phenol (mg/l) 11–14
Reforming Sulfide o-Cresol (mg/l) 14–16.5
Hydrotreating Ammonia, sulfides, phenol m,p-Cresol (mg/l) 72–75
N-hexane (mg/l) 1.8–1.85

treatment methods for a complete and successful removal of such In this study, a combination of an electrochemical process, a
pollutants. biological treatment with a spouted bed bioreactor (SBBR) and an
Although biological treatment and bioremediation techniques adsorption fixed bed column packed with granular activated
are well established for the clean-up of petroleum contaminated carbon was evaluated for the treatment of refinery wastewater.
land and wastewater [11], there is a need for enhancement of The integrated three-step system was tested under different
enzymatic capacity of the employed microbial communities. An operating conditions and the experimental results obtained for the
improvement can also be achieved by pretreatment technologies, to optimized system were compared with those reported in the
decrease the priority pollutants concentration as much as possible literature for similar processes.
before the biodegradation step. Several solutions are proposed
including the use of coagulants and electrochemical oxidation
[13,24], fenton oxidation [25], electron-beam [26], ozonation [27]. Experimental methods
In recent years, there has been increased interest in the
application of electrocoagulation in the treatment and purification Wastewater characterization
of industrial wastewater [28]. Electrocoagulation is efficient in
removing suspended solids as well as oil and greases. It removes Refinery wastewater samples were obtained from a petroleum
metals, colloidal solids and particles, and soluble inorganic refinery and were preserved in dark, plastic containers. Analyses of
pollutants from aqueous media by introducing highly charged the samples are given as ranges of values in Table 2.
polymeric metal hydroxide species. These species neutralize the
electrostatic charges on suspended solids and oil droplets to Bacterial suspension
facilitate agglomeration or coagulation. Because of the many
advantages for this technique, electrocoagulation has been A special strain of the bacterium Pseudonymous putida was
suggested widely as one of those advanced alternatives used as obtained in a cereal form (AMNITE P 300) from Cleveland Biotech
a pretreatment step for industrial wastewater treatment. A Ltd., UK. A 100 g of the cereal was mixed in a 1 L of 0.22% sodium
combination between EC and TiO2 photocatalysis was applied hexametaphosphate buffered with Na2CO3 to a pH of 8.5. The
for the reduction of COD from pharmaceutical and cosmetic mixture was homogenized in a blender for about one hour,
industries wastewater [29]. 90% of COD reduction was achieved decanted and kept in the refrigerator at 4 8C for 24 h. Bacteria
after the EC process. Linares-Hernández et al. found a complete slurry was prepared by first low speed centrifugation at 6000 rpm
elimination of COD by combining EC with electrooxidation [30]; (4508  g) for 15 min. Then, the supernatant was collected and
whereas, 84% COD reduction efficiency was achieved using EC– centrifuged again at 10,000 rpm (12,522  g) for 20 min. The
biosorption process [31]. EC was also combined with a biological centrifugation was carried out using IEC CL31R Multispeed
treatment used for winery wastewater [32]. Centrifuge, Thermo Electron Cooperation, USA. Harvested bacteria
Combinations of different treatment techniques were recom- cells were collected and kept in the refrigerator for immobilization.
mended for the treatment of highly contaminated industrial Nutrients mineral media was prepared according to Table 3.
wastewater. Ultrafiltration with electrocoagulation [33] and
advanced oxidation with biodegradation [34] were suggested for Immobilization of bacteria in PVA gel
the treatment of olive mill wastewater with COD reduction
efficiency of about 96% and 91%, respectively. EC–irradiation Polyvinyl alcohol (PVA) gel was used for immobilizing the
treatment was another combination used in the treatment of bacteria cells as reported in a previous study [41]. A homogenous
highly colored and polluted industrial wastewater with COD 10 wt% PVA viscous solution was prepared by mixing 100 g of PVA
reduction of about 95% [35]. Chemical coagulation, electrochemi-
Table 3
cal oxidation and biological treatment were used as a combination
Composition of nutrient mineral media.
for the treatment of bactericide [24] and textile wastewaters [36].
3
Leather industry [37] and integrated dyeing [25] wastewaters Component Concentration (g m )
were also treated using biological and fenton oxidation process. MgSO4
7H2O 300
Jung et al. [38] suggested the combination between adsorption and K2HPO4 250
microfiltration membrane bioreactor for advanced tertiary waste- CaCl2
2H2O 150
(NH4)2CO3 120
water treatment. Pre-oxidation, co-precipitation, adsorption and
FeSO4
7H2O 3.5
coagulation were used as a combined process for the treatment of ZnSO4
7H2O 1.3
high arsenic content industrial wastewater [39]. A combination of MnCl2
4H2O 0.13
PAC’s and coagulant with ultrafiltration [40] and microwave- CuSO4
5H2O 0.018
CoCl2
6H2O 0.015
assisted catalytic wet air oxidation [10] were investigated for
Na2MoO4
2H2O 0.013
refinery wastewater treatment.
[(Fig._1)TD$IG]
58 M.H. El-Naas et al. / Journal of Environmental Chemical Engineering 2 (2014) 56–62
Fig. 1. SEM photo for immobilized bacteria in PVA.
powder with 900 ml of distilled water at about 70–80 8C. PVA is a
synthetic polymer that has better mechanical properties, and it is
more durable than Ca-alginate which is biodegradable and can be
subject to abrasion [42]. The formed mixture was allowed to cool
to room temperature before adding 10 ml of the bacterial
suspension prepared as in Bacterial suspension section, then well
stirred for 10–15 min to ensure homogeneity of the solution. The
solution was then poured into special molds and kept in a freezer at
20 8C for 24 h, then transferred to the refrigerator and allowed to
thaw at about 4 8C. The freezing–thawing process was repeated 3–
4 times, with 5 h for each cycle. The frozen molds were cut into
1 cm3 cubes, washed with distilled water to remove any uncross-
linked chains, and sent for acclimatization as per the procedure
described in [41]. Fig. 1 shows the distribution of immobilized
bacteria in PVA.
Date pits activated carbon
Date pits activated carbon (DP-AC) was prepared from raw date
pits granules. The granules were washed, dried, grinded and
screened. The collected granules were carbonated and activated to
produce DP-AC. The carbonization was performed in a tube furnace
(Thermolyene, USA) which was initially purged with a flow of
nitrogen for 10 min. After that, the furnace was heated at a rate of
10 8C/min up to 600 8C and then kept at this temperature for 4 h.
[(Fig._2)TD$IG]
Fig. 2. A schematic diagram of the integrated system. (1) Feed tank, (2) feed pump, (3) electrocoagulation reactor, (4) magnetic stirrer, (5) DC power supply, (6) settling tank,
(7) pump, (8) biological reactor, (9) adsorption column and (10) product tank.
After cooling to room temperature, the material is considered
carbonized, but still inactive. After weighing the inactive carbon, it
was activated in the same tube furnace at a temperature of 900 8C
using a flow of carbon dioxide instead of nitrogen. The resulting AC
was then degassed under vacuum (Shel Lab, USA) for about 2 h
before use [15].
Experimental setup
Refinery wastewater samples were treated using the integrated
system shown in Fig. 2. The wastewater was pumped to the
1500 ml cylindrical electrocoagulation reactor (14 cm in diameter
and 6 cm height) using peristaltic pump (GILSON Mini plus 3) with
a flow rate of 10 ml/min. The aluminum plate electrodes
(4 cm  6 cm  1 mm) were dipped into the wastewater and
connected to a DC power source (POPULAR PE-23005) to provide a
current of 0.1 A (current density of 3 mA/cm2) and a voltage of
about 17 V; the voltage depends on the conductivity of the
wastewater. The distance between the anode and the cathode was
kept constant at 7.5 cm. The effluent from the electrocoagulation
unit was sent to a settling tank, where the overflow was pumped to
the spouted bed bioreactor (SBBR). The spouted bed bioreactor was
made of Plexiglas with a total volume of 1.1 L and was equipped
with a surrounding jacket for temperature control. Detailed
description of the SBBR can be found elsewhere [43,44]. The
temperature of the reactor system was controlled by circulating
water into the reactor jacket from a water bath set at the desired
temperature. Air was continuously introduced through the bottom
of the reactor at a flow rate of 3 L/min to enhance mixing and at the
same time provide excess oxygen to sustain aerobic conditions.
The reactor was initially filled with standard nutrient media
containing 30 vol% PVA gel cubes with immobilized bacteria. The
temperature of the water bath, and hence the reactor system, was
set at 30 8C. This temperature was found to be the optimum in a
preliminary runs which also agrees with previous studies in the
literature [45]. The product from the bioreactor was then fed to the
adsorption column, which was made of a Plexiglas column (50 cm
in length and 3 cm inside diameter). The column was packed with
130 g of granular activated carbon. More details about the
adsorption kinetics and equilibrium data as well as the regenera-
tion of the saturated activated carbon can be found elsewhere
[15,16]. At regular intervals, samples were collected from the
effluent of each treatment unit and analyzed for COD and phenol
concentrations. All experiments were carried out at room
temperature.
 [(Fig._4)TD$IG]
M.H. El-Naas et al. / Journal of Environmental Chemical Engineering 2 (2014) 56–62 59

Table 4
Operation conditions for the three unit system. 12

Phenol Concentration (mg/l)

Electrocoagulation SBBR Adsorption system
10
Electrodes type: aluminum PVA amount: 300 ml Adsorbent: AC
Current density: 3 mA/cm2 Temperature: 30 8C Adsorbent mass: 130 g
Current: 100 mA pH: 7.5 Room temperature 8
2
Area of the electrodes: 36 cm Air flow rate: 3 L/min Liquid flow rate: 10 ml/min
Liquid flow rate: 10 ml/min Liquid flow rate: 10 ml/min
6

Results and discussion

The electrocoagulation unit, spouted bed bioreactor and
adsorption column were connected in series with different
configurations and operated continuously for the treatment of
real refinery wastewater, which had a dark greenish color and a
strong, pungent odor, with initial concentrations ranging from
3600 to 5300 mg/l and 11 to 14 mg/l for COD and phenol,
respectively. The samples withdrawn after each treatment unit
were analyzed for their COD content and phenol concentrations as
a function of time. Table 4 summarizes conditions used in the
experiment for each treatment unit.
Electrocoagulation–adsorption–biodegradation arrangement
In this section, results for the arrangement of electrocoagula-
tion–adsorption–SBBR are shown for the reduction of COD and
phenol for about 3 h. Fig. 3 shows the COD reduction after each
treatment unit, with the electrocoagulation pretreatment step
contributing 46% to the overall reduction of COD. However, the
reduction percentage increased to about 83% by passing the
effluent through the adsorption column. The effluent from the
adsorption is sent to the bioreactor, where the COD reduction is
very low compared to the electrocoagulation and adsorption
stages. The cumulative COD reduction after the biodegradation
increased to only 85%. It is worth noting here that the adsorption
column reached the saturation after the third hour which
increased the load on the SBBR and consequently decreased the
efficiency of the overall treatment process.
Fig. 4 shows the reduction of phenol concentration for this
system. There is no significant reduction in phenol concentration
in the electrocoagulation unit, but a very high reduction occurs in
the adsorption column which initially reduces the phenol
concentration to zero in the first 3 h after the feed enters the
0
Feed EC Adsorption SBBR
Treatment Step
Fig. 4. Phenol concentration after each treatment step for the refinery wastewater in
electrocoagulation–adsorption–biodegradation system.
adsorption column then the concentration increases with time as
the activated carbon gets saturated.
Electrocoagulation–biodegradation–adsorption arrangement
Figs. 5 and 6 show the effluent concentrations of COD and
phenol at steady state conditions for electrocoagulation and after
24 h of operation for both biodegradation and adsorption systems.
The results show that the electrocoagulation unit reduced the COD
concentration by about 46%. The bioreactor further reduced the
feed contaminants, which came from the electrocoagulation step,
by about 73% for COD, 61% for the phenol. Nevertheless, most of the
reduction in COD and other phenols has taken place in the
adsorption unit, where the final cumulative reduction reached 97%
and 100% for COD and phenol, respectively. The final effluent after
the adsorption column had COD and phenol concentrations within
the acceptable discharge limits. A summary of the complete
system results is shown in Table 5, where after the last treatment
step the effluent showed almost complete reduction for phenols
and 97% reduction for COD content.
To demonstrate the effectiveness using a combination of
electrochemical process, biological treatment using SBBR and
[(Fig._5)TD$IG]

[(Fig._3)TD$IG] 4000
COD Concentration (mg/l)

4000
COD Concentration (mg/l)

3000

3000

2000
2000

1000
1000

0
0
Feed EC Adsorption SBBR Feed EC SBBR Adsorption

Treatment Step Treatment Step

Fig. 3. The COD concentration after each treatment step for the refinery wastewater Fig. 5. The COD concentration after each treatment step for the refinery wastewater
in electrocoagulation–adsorption–biodegradation system. in electrocoagulation–biodegradation–adsorption system.
[(Fig._6)TD$IG]
60 [(Fig._7)TD$IG]
M.H. El-Naas et al. / Journal of Environmental Chemical Engineering 2 (2014) 56–62

12 100
COD
Phenol Concentration (mg/l)

Phenol

Percentage Reduction %
10 80

8
60

6
40

4
20

2
0
EC SBBR AD (8h) EC-SBBR-AD
0
Feed EC SBBR Adsorption Treatment Setup
Treatment Step Fig. 7. Comparison for the percentage reduction of COD and phenol after individual
unit treatment and the three units in series.
Fig. 6. Phenol concentration after each treatment step for the refinery wastewater in
electrocoagulation–biodegradation–adsorption system.
could not be used as an individual treatment unit for the refinery
wastewater treatment as a pretreatment step is needed in
Table 5 conjunction with this sensitive technology. Electrocoagulation
Summary of the results of EC–SBBR–AD treatment system.
reduced the contamination of the refinery wastewater by 46% and
Test Electrocoagulation SBBR Adsorption 34% for COD and phenol, respectively. Meanwhile, passing refinery
In Out In Out In Out wastewater through the packed bed of activated carbon showed a
reduction of 65% and 85% for COD and phenol. However, the
pH 7.2 9.1 7.8 8.2 8.2 8.2
activated carbon was saturated after only 8 h of operation. On the
Conductivity (mS) 5.4 6.2 6.2 6.73 6.73 8.24
TSS (g/l) 0.072 0.244 0.11 0.17 0.05 0.01 other hand, 97% reduction for COD and a complete reduction of
TDS (g/l) 3.38 3.6 3.6 4.03 4.03 4.95 phenol were achieved when using the three units in series for a
COD (mg/l) 4190 2267 2267 1116 1116 110 longer operating time of 24 h, giving a clear indication that this
Phenol (mg/l) 12.2 8.1 8.1 4.8 4.8 0
combination can be considered to be the most efficient unit
m,p-Cresol (mg/l) 75 64 64 33 33 0
arrangement and as one of the most effective alternatives for the
treatment of refinery wastewater.
A comparison of the percentage reduction in COD in this study
adsorption for treating refinery wastewater, results were com- with those reported in the literature using different combined
pared to the percentage reduction for both COD and phenol after processes for the treatment of several types of industrial waste-
the treatment of such wastewater using the same continuous waters in batch and continuous studies is presented in Table 6. It
treatment units individually. Fig. 7 shows that biological method shows that this combined process of electrocoagulation, spouted

Table 6
Comparison in the COD reduction using different combined treatment methods for the treatment of different industrial wastewater.

Wastewater source Combined treatment method COD (mg/l) COD % reduction Ref.

Batch study
Dyeing Fenton oxidation–membrane bioreactor (B) 1100–1300 77–80 [25]
Rayon industry Electro-fenton + chemical precipitation 2400 88 [46]
Tannery Ozonation–sequencing batch biofilm reactor 3500–4000 97 [47]
Antibiotic Fenton–sequencing batch reactor (SBR) 675  20 89 [48]
Polyferric sulfate coagulation–fenton–sedimentation 3279 96.9 [49]
Biodiesel Chemical recovery + electrochemical 312,000–588,800 100 [50]
Olive mill Ultrafiltration + electrochemical 28,000 93 [33]
Advanced oxidation (O3)–biodegradation 117,100 91 [34]
Industrial wastewater Electrochemical–irradiation 3400  25 95 [35]
Electrocoagulation–sorption 1700–2500 84 [31]
Electrocoagulation–electrooxidation 800–1200 >99 [30]
Fenton’s peroxidation–coagulation 1596–2598 90 [51]
Pharmaceutical and cosmetic Electrocoagulation–TiO2 photo-assisted 1753 97 [29]
Fenton–sequencing batch reactor (SBR) 98 [52]
Winery Electrocoagulation–optional dilution–aquatic plants 10,168 98.2 [32]
Ammunition Ultrasound–fenton 1580  20 92 [53]
Leather Aerobic biological–fenton oxidation 2533 77 [37]
Semiconductor Fenton–sequencing batch reactor (SBR) 80,000 99.8 [54]
Printed circuit board Ferrite process–fenton method 406 80 [55]
Paper industry Ozonation-activated sludge process 75.5 [56]
Petroleum refinery Microwave-assisted catalytic wet air oxidation 5500 90 [10]

Continuous study
Dyeing Electron beam + biological 3220 60 [26]
Textile Fluidized biofilm + chemical coagulation–electrochemical oxidation 870 95.4 [36]
Petroleum refinery This work 4190 97
 M.H. El-Naas et al. / Journal of Environmental Chemical Engineering 2 (2014) 56–62
bed bioreactor (SBBR) and adsorption is highly competitive in
comparison to other combination systems used for the reduction of
COD in different industrial wastewaters.
Conclusions
Samples of heavily contaminated refinery wastewater with
high concentrations of COD and phenols have been treated by a
novel three-step process involving an electrocoagulation cell, a
spouted bed bioreactor (SBBR) and adsorption column packed with
activated carbon. The overall COD and phenol reduction reached
97% and 100%, respectively, indicating that the combined process
was effective for the treatment of petroleum refinery wastewater
and might offer a potential application for reusing the treated
water and will significantly contribute to reducing freshwater
consumption. The process was found to be highly competitive in
comparison with other combined systems used in the treatment of
industrial wastewater and can handle refinery or industrial
wastewater with varying concentrations of contaminants. Work
is currently underway at the pilot scale to further assess the
technical and economic feasibility of the process.
Acknowledgements
The authors would like to acknowledge the financial support
provided by the Japan Cooperation Center, Petroleum (JCCP) and
the technical support of the JX Nippon Research Institute Co., Ltd.
(JX-NRI).
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