39 Egypt. J. Chem. 58, No.6, pp.

609– 624 (2015)

Reliable Treatment of Petroleum Processing

Wastewater Using Dissolved Air Flotation in
Combination with Advanced Oxidation Process
M.H. El-Awady, I. Abdelfattah* and A. Abo El-Magd#
Water Pollution Research Department, National Research
Centre, 33 EL Bohouth St., P.O. 12622, Dokki, Giza and #Civil
Engineering Department, Faculty of Engineering, Shoubra,
Banha University, Egypt.

O IL refinery processes mill wastewater originating from highly

contaminated outlet with persistent organic pollutants is the main
polluted part in end-of pipe of oil industry. This study has been carried
out to investigate the application reliability of diffused air flotation
(DAF) and advanced oxidation processes (AOPs) with particularly
Fenton reaction for the treatment of this type of wastewater. Two
sequenced wastewater samples were collected from Petroleum Refinery
Company located at a coastal city, Egypt. The first was from the API-oil
separation discharging point where it has been treated by DAF- unit,
while the second was collected from Naphtha section outlet that highly
contaminated with phenolic compounds. It has been treated with Fenton
process in batch laboratory-scale. Results showed that at the optimal
operating conditions, DAF-experiment fulfilled appropriate removal of
total oil and grease up to 98%, while its efficiency in removing both
COD and TSS was exceeding 96% and 92%, respectively. On the other
hand, samples collected from Naphtha department outlet that subjected
to Fenton reaction showed remarkable destruction of phenolic contents
up to 99.9%; and 88% for COD, at their optimal operating conditions,
respectively.

Keywords: Refinery wastewaters, Treatment, DAF-unit, Fenton

reaction and Phenols.

Wastewater originating from Oil Refinery Processes Mill (ORPM) was highly
contaminated with hydrocarbons which represented the main source of pollution
in this industry. ORPM is discharging to the sea large quantities of partially
treated wastewater that characterized by high values of pH, Chemical Oxygen
Demand (COD), Total Suspended Solids (TSS), Oil and Grease (O & G),
respectively(1). Also, Coates(2) and Syllos et al.(3) reported that the generated
wastewater in oil industry contained several organic compounds, such as
Benzene, Toluene, Ethylbenzene, and Xylenes (BTEX), its disposal to the sea has
been regulated by National Law 4/1994. ORPM wastewater is considered as
dangerous compounds to the environment because of their migration abilities,
both in aquatic and land environments, and their acute and chronic toxicities. The
significant amount of refinery wastewater has to be treated and processed before
‫ــــــــــــــــــــــــــــــــــــ ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ‬
*
Corresponding author : iabdelhafiz@yahoo.com,
Tel: 0020-12-74999938, Fax 0020-2-374840077
610 M.H. El-Awady et al.

their discharge into water streams. The refinery wastewater treatment plants
employ physicochemical processes including American Petroleum Institute (API)
separator as a primary treatment and dissolved air flotation technique as a
secondary treatment, to achieve effluents of satisfactory oil content. Flotation is
investigated as a post-treatment process for the removal of emulsified hydrocarbons
and satisfactory results were obtained(4). On the other hand, Tony et al.(5) showed
that conventional treatment processes have difficulty in fully removing
emulsified oil or small oil droplets. Diffused Air Flotation (DAF) process
exhibited remarkable results in removing floatable and suspended materials and it
was an effective method to separate oil from aqueous dispersion, chemically
treated wastewater, and refinery wastewater(6 ,7). According to Metcalf & Eddy,
Inc.(8), the air to solids ratio (A/S) was considered one of the most important
parameter in the design of air flotation system. However, different types of
influent characteristics generated different ranges of A/S ratios. The optimal A/S
range for a particular feed must be determined experimentally. The
corresponding equation (1) for a system with only pressurized recycle is:

where A/S is the air to solids ratio in ml air to mg solids; : the air solubility
(ml/L); f: the fraction air dissolved at pressure P, usually 0.5; P: pressure, atm. =

; P: gage pressure, kPa; Sa: influent suspended solids,

(mg/L); R: the pressurized recycle; Q: the influent flow rate; The factor of 1.3 is
the weight in milligrams of 1 ml of air and the term (-1) accounts for the system
operating at atmospheric conditions (gage pressure). The dry density of dry air is
1.3 mg/ml at 1atm and 0 0C.

Fenton reaction(9), equation (2) is one effective process of Advanced

Oxidation Processes (AOPs); where the iron-salt-dependent decomposition of
hydrogen peroxide, generating the highly reactive hydroxyl radical ( .
(10)
Fenton's reagent can be used to destroy organic compounds utilizing the .
Haber and Weiss suggested the Fe2+ regeneration by in which a superoxide
radical as indicated in equations (3 and 4) (11).

AOPs provided a high degradation capacity for petroleum wastewater that

was extremely important in the oil industry, since they allowed the reuse of

Egypt. J. Chem. 58, No.6 (2015)

 Reliable Treatment of Petroleum Processing Wastewater … 611

water. After an extensive study, El-Awady et al., concluded that the addition of
H2O2 in photocatalytic reaction achieved detectable degradation of dissolved
organic pollutants in wastewater (12). It fulfilled efficient removal of contaminants
that persisted and were hard to remove using conventional methods.

The case study under investigation was representing a petroleum refinery

company located at a coastal city, Egypt. Its hourly discharging was 700 m3 of
insufficient treated industrial wastewater; mixed with 9000 m3 cooling water with
total wastewater exceeding 9700 m3/h to the sea. The existing treatment system
was based on the collection of Industrial Wastewater (IWW) from production
lines. Their discharges were 12.5 m3/h from Naphtha and 687.5 m3/h from API
oil separator, respectively. The total IWW then passed to Skim Basin (SB) where
the 9000 m3/h cooling water was thoroughly mixed with the industrial
wastewater discharged from Naphtha section division and API oil separator. The
last section represented the main source of organic pollutants, with high phenolic
content, high alkalinity and COD exceeding the trigger levels in Law 4/1994
regulating the discharge of water onto the sea. DAF was selected to remove
suspended solids, free and emulsified oils, while Fenton reaction was chosen to
destruct the high organic load in Naphtha waste.

Materials and Methods

Materials
Freshly prepared 1.0 N heptahydrated ferrous sulphate (FeSO4·7H2O),
hydrogen peroxide 30% (H2O2), dodecahydrated potassium aluminum sulfate
KAl(SO4)2.12H2O utilized in the DAF process for enhancement of oil separation
and removal, 50% sodium hydroxide and 30% sulphuric acid were prepared daily
for pH adjustment and naphtha wastewater outlet and API-oil separation unit
samples.

Methods and utilities

A solution of Fe2+ was prepared from ferrous sulfate heptahydrate
(FeSO4.7H2O) and hydrogen peroxide (30%, by weight) was used in the
experiments as the Fenton’s reagent for hydroxyl radical generation. Sulfuric acid
and sodium hydroxide were used to adjust the pH to the desired values.

Jar test experiment

Coagulation tests have been performed according to Jar-test method as shown
in Fig.1, using a standard Flocculation Stuart Scientific, equipped with two
mixing posts. This step was done by flash mixing step (200 rpm) for 2 min, while
flocculation step was done for 10 min, at (28-30) rpm, followed by a settling time
of 30 min. Tests have been performed in 1 liter cylindrical beakers, at room
temperature (20±1) °C, using raw inlet wastewaters.

Egypt. J. Chem. 58, No.6 (2015) 611

612 M.H. El-Awady et al.

Fig.1. Standard Jar test apparatus.

Chemical coagulation/flocculation using alum solution in-combination with

DAF process was performed to API outlet sample. DAF unit (Fig. 2) was
designed based on Jar-test criteria to achieve the optimum operating conditions.
The floatation unit (FU) was made from calibrated Plexiglas column, with 85 cm
length and 5 cm diameter. The pressurized air/water mixture was released from
the retention tank to the floatation cell through a pressure reducing valve (PRV)
at the tank bottom. Air /water in the pressure tank were saturated with air at a
pressure of 4 kg/cm2. The dissolved air was gradually released to the FU.

Fig.2. Schematic diagram of DAF Lab unit.

To determine the optimal Fe2+, H2O2 dosages, the optimal pH and reaction
time, in addition to achieve maximal removal of chemical oxygen demand
(COD) and phenol; Fenton reaction has been carried out and performed
according to Jar Test (Fig. 2). Hydrated ferrous sulphate (FeSO4·7H2O) as well as
30% hydrogen peroxide (H2O2) were used as components of Fenton reaction.

Six Jars of naphtha wastewater and Fenton reagents were carefully mixed at
50 rpm for 10 min.

Egypt. J. Chem. 58, No.6 (2015)

 Reliable Treatment of Petroleum Processing Wastewater … 613

FeSO4 & H2O2 doses, reaction time, and other optimal operating conditions
were calculated. Because Fenton reaction is exothermic; the reactors were cooled
during chemical addition. Freshly prepared sodium hydroxide (50%) and (30%)
sulphuric acid were added to adjust the pH-value of the treated effluent.

Operational principals
Coagulants were mixed with wastewater, pressurized air was introduced,
released as micro-bubbles (30- 100) microns, Oil droplets were rapidly migrated
to the top, sludge as floated blanket was skimmed and clean treated wastewater
was collected from outlet.

To determine the optimal coagulant dose and Fenton’s operating conditions; a

flotation column and cooled Jar test experiment were used, respectively. Alum
was used as coagulant during flotation experiments, while Fe2+ and H2O2 reagents
were used in the experimental work of Fenton reaction. The optimal pH and
reaction time were calculated to achieve maximal removal of chemical oxygen
demand (COD) and phenol. Both flotation and Fenton reaction experiments were
carried out in accordance with Syllos et al.(3). All measured parameters of raw
and treated wastewaters have been analyzed according to procedures given in the
American standard methods (13).

Results and Discussion

Characterization of raw wastewaters

Table 1 shows the main physico-chemical characteristics of the raw
wastewaters outlets from: Naphtha Dept.; oil separator; cooling water of API
(American Petroleum Institute) and final tank, respectively.

TABLE 1. Physico-chemical analysis of raw wastewaters from different outlets.

Result *
Naphtha Oil Cooling Law 4/
Parameters Unit Final Tank
Dept. Separator water 1994 **
pH -- 13.6 7.5 7.5 6.5 6-9
COD mgO2/L 8200 1384 1326 4360 100
BOD5 mgO2/L 3286 554 523 NI 60
TSS mg/L 438 3314 22 68 60
TDS mg/L 55600 65300 56130 NI ==
H2 S mg/L N.D. ND N.D. N.D. 1
Phosphate mg/L 0.4 0.18 N.D. NI ==
Chlorides mg/L 420 52000 51000 NI ==
Phenol mg/L 160 0.2 2.0 0.12 0.01
TKN mg/L 17 106.5 NI NI 10
O&G mg/L NI 707 12 15 10
Discharging- 3
m/h 12.5 687.5 9000 9700 ==
Capacity
* Results of three successful replicates. NI: Not identified, ND: Not detected.
** Trigger levels of Law 4/1994; regulating the limits of discharging wastewater to the sea.

Egypt. J. Chem. 58, No.6 (2015) 613

614 M.H. El-Awady et al.

Due to the highly organic content of the Naphtha Department outlet (160 mg
phenol/l and 8200 mg O2/L), with about 7.0% from the total discharging
capacity, it was suggested to be segregated and treated separately using Fenton
reaction. Although Fenton reaction was costly, but it saved lots of chemicals and
infrastructures, running costs if compared with an overall treatment system of the
total discharging wastewater.

On the other hand, DAF unit will be effectively for the removal of all floated
as well as oily matters from the final wastewater. After carrying out this
treatment method, the final treated wastewater from all separate sectors will meet
the trigger values of discharging the treated wastewater onto the sea and to fulfill
the requirements of the Environmental Egyptian Law 4 /1994.

Detection of the optimum removal of Oil, TSS & COD from API outlet using DAF
unit
The optimum operating conditions of the treatment was carried out according
to coagulation/ flocculation followed by dissolved floatation process DAF. Alum
was chosen as relevant coagulant because the produced sludge was fluffy to be
floated and skimmed. Its optimum detected dose was of Al 3+ at the original pH
6.5-7.0 of the wastewater was measured. Table 2 reveals the average of three
replicates of raw and treated samples including the mean removal efficiencies.

TABLE 2. Physico-chemical analysis of floating cell influent, and effluent .

Parameter (mg/L) Raw IWW Treated IWW %R

COD 200 8 96%

TSS 1013 23 97.7
Oil & Grease 707 9 98.7

Design of DAF unit for the oily wastewater

A typical schematic and the diagram of DAF layout of the designed DAF
systems are shown in Fig. 3 & 4. The experimental results showed the
optimum operating conditions as: alum dose 75 mg Al 3+/L, surface loading
rate 70 liter of wastewater/ square meter of surface area per minutes and A/S
of 0.008 ml/L, respectively. Reference to equation (1), the calculated
recycled flow was 16500 m 3/h.

Egypt. J. Chem. 58, No.6 (2015)

 Reliable Treatment of Petroleum Processing Wastewater … 615

Fig. 3. Schematic diagram of dissolved-air flotation system.

Fig. 4. Layout plan for designed dissolved-air flotation system.

In the DAF treatment process, a compressed air was injected into a pressure
vessel of diameter 1.0 m and height of 1.2 m for one vessel or 0.8 m diameter and
1.0 m height for two vessels, containing part of the recycled treated wastewater
of a 2000 m3/d at 4 Bars. Sufficient time was being allowed in this vessel for air
saturation for about 3 min. Air compressor was used efficiently to mix air with
the purified recycled wastewater. The recycled flow was released toward the
base of the floatation tank via a pressure release valve (P.R.V), allowing the air to
come out through the wastewater matrix and creating fine homogenous air carpet.
The floatation tank was designed for influent and recycled flow with 30 min
retention time. To fulfill maximum removal efficiency, its design dimensions
Egypt. J. Chem. 58, No.6 (2015) 615
616 M.H. El-Awady et al.

were designed as: 10.0 m width, 20.0 m length and 2 m height. For one floatation
tank or 7.0 m width, 14.0 m length and 2.0 m height for two floatation tanks.

The obtained results revealed that DAF process exhibited good results in
removing floatable materials as well as suspended solids with remarkable
efficiency that exceeded 95%. Obtained results matched with that obtained by El-
Awady (6). Moreover, Abdel Megid et al.(4) concluded that different responses to
the coagulant treatment were observed within the tested samples, Ferrous
sulphate at pH = 10 removed 67% oil, Alum at pH =10 removed 73% oil, Ferric
chloride at pH = 8 removed 74 % oil, other combinations with manufactured
chemicals removed up to 87 % oil while normal DAF operations with no
additives removed only 61 % oil from the oily wastewater.

Fenton reagent (Fe2+ /H2O2) for phenols and COD destruction from Naphtha
outlet section
The presence of naphtha in the wastewater of this section caused a remarkable
increase in the organic matters. It was a result of the presence of phenols and other
organic pollutants. The segregated wastewater collected from naphtha processing
unit was treated using Fenton reaction, where the optimum operating conditions
were achieved. Optimal conditions for Fenton’s reagent were established and the
pH was adjusted to 3.0. The highest percentage COD removal achieved was 88%,
which occurred with pre-treatment including Fenton treatment(14).

Table 1 shows the characteristics of wastewater discharged from naphtha

department. Physico-chemical analysis showed that the waste was alkaline in
nature, with a pH- value close to 14. Its color was yellowish-brown due to the
presence of high content of phenol and other organic pollutants.

Phenolic content and COD were 160 and 8200 mg/L, respectively. The total
suspended solids exceed 400 mg/ L. On the other hand, results detected that the
iron in the raw sample reached 5 mg/L. The presence of this low concentration
of iron may behave as Fenton like’s reaction on addition of H2O2.

The optimal operating conditions of the Fenton’s reaction were carried out
according to the following variable conditions:

Detection the optimum 30% H2O2 dose

Its optimum dose was detected at 0.5 g Fe2+/L as a fixed dose, pH- value of
3.0, reaction time of 10 min, and stirring at 120 rpm. Two success replicates were
carried out to detect the optimum H2O2 dose.

Results showed that, on addition of only the 0.5 g Fe2+/L as a coagulant, the
removal of total COD and phenol was limited to 2.0% and 12%, respectively.
The low efficiencies can be explained due to the removal of existing suspended
solids. These results were in accordance with that obtained by Petri et al.(15).
Moreover, the addition of a series of 30% H2O2 to the previous reaction, a
Egypt. J. Chem. 58, No.6 (2015)
 Reliable Treatment of Petroleum Processing Wastewater … 617

detectable removal in both COD and phenol was achieved as shown in Fig. 5 &
6. The results revealed that the optimal H2O2 dose for noticed COD and phenol
removal was 20 ml/L. Figure 5 shows that the reaction proceeds first order mode.
From the cost-effective factor, there was a little bit difference between the
highest dose of 40 ml/L and the chosen optimal dose.

Fig.5. Optimum H2O2 dose versus COD.

Fig.6. Optimum H2O2 dose versus phenol.

Egypt. J. Chem. 58, No.6 (2015) 617

618 M.H. El-Awady et al.

Detection of the optimum Fe2+ dose

The optimum ferrous dose was detected at 20 ml/L of 30% H 2O2/L, pH- value
3.0, reaction time of 10 min, and 120 rpm using Jar Test apparatus.

Results in Fig. 7 explain the partially decomposition 39% of organic matters

COD, without adding Fe2+ dose. This explains the effect of internal presence of 5
mg/L iron content, which behaved as Fenton like reaction. On the other side,
Fig. 8 represents the calculated optimal Fe2+ dose 0.2 g/L. It was enough to
decompose about 93% from phenolic compounds. The obtained results were
supported by results recorded by Steiner and Gec(16).

Fig.7. Optimum Fe2+ dose versus COD.

Fig. 8. Optimum Fe2+ dose versus phenol.

Egypt. J. Chem. 58, No.6 (2015)

 Reliable Treatment of Petroleum Processing Wastewater … 619

Detection of the optimum pH-value

At the optimum ferrous dose 0.5 g/L, 20 ml/L of 30% H 2O2/L, reaction time
of 10 min, and 120 rpm using Jar Test apparatus, the optimum pH- value was
concluded from three repeatable successful runs.

Results obtained from these experiments revealed that the Fenton reaction can
be obtained at the pH equal to 10.0 as illustrated in Fig. 9 & 10. When the pH-
value was reduced from 14.0 to 10.0 followed by addition of H 2O2, the pH was
consequently dropped to 3.0, which is the optimum value of Fenton’s reaction. In
this case, no need to reduce the initial pH to 3.0, and this pH- value was chosen
as effective cost value(17).

Fig. 9. Optimum pH versus COD removal.

Fig.10. Optimum pH versus phenol removal.

Egypt. J. Chem. 58, No.6 (2015) 619
620 M.H. El-Awady et al.

Detection of the optimum reaction time

At the optimum conditions of ferrous dose 0.5 g/L, 20 ml/L of 30% H 2O2/L,
120 rpm and pH 10.0 using Jar Test apparatus, the optimum contact time was
measured. These results were in accordance with that obtained by Szulbinski(17).

Results conducted that the optimum reaction time to obtain the required
results was 10 min as declared in Fig. 11 and 12.

Fig. 11. Optimum time versus COD removal.

These data were in accordance with that obtained by Syllos et al. (3), where
above 90% degradations were reached in all cases after 90 min of reaction.
Results were attaining 100% mineralization in the optimized concentrations of
Fenton reagents, and the process integration was adequate with 100% organic
load removal in 20 min.

Fig.12. Optimum time versus phenol removal.

Egypt. J. Chem. 58, No.6 (2015)

 Reliable Treatment of Petroleum Processing Wastewater … 621

The overall schematic diagram of Fenton reaction is illustrated in Fig.13.

Fig. 13. Schematic diagram of Naphtha destruction using Fenton reaction.

Conclusion and Recommendations

 Two different types of real wastewater samples were collected from the
petroleum refinery company under investigations, Egypt. The first was one
from the API-oil separation unit outlet. DAF- procedure was carried out unit,
where the unit showed an appropriate treatment method for removing of oil
and grease to 98%, COD to 96% and TSS to 92%.
 Wastewater from the API-oil separation unit outlet (I), DAF- unit (Table 1)
showed an appropriate treatment method for removing oil and grease; COD
and TSS were up to 99%, 96% and 98%, respectively.
 Wastewater collected from Naphtha department (II) subjected to Fenton
processes, which effectively oxidize and remove phenolic organics more than
99.9% (the initial phenol load =160 mg/L*12.5 m3/h *24 h = 0.048 kg/day;
phenol load after treatment= 0.1 mg/L*12.5 m3/h*24 h = 0.00003 kg/day) and
about 88% removal of COD (8200 mg/L *12.5 m3/h*24 h = 2.46 kg/day, COD
load after treatment = 1000 mg/L*12.5 m3/h * 24 h = 0.30 kg/day ) at optimum
condition, the Fe2+ dose was 0.5 g/L, the (30 %) H2O2 dose was 20 ml/L, the
reaction time is 10 min the starting pH value is 10 because of a cost-effective
factor because the target wastewater had an original pH near to 14.

From this study, it is apparent that the implementation of removal of oil from
wastewater (I) and destruction of phenolic compound via advanced oxidation of
wastewater (II) produces a good quality effluent that complying with the
Egyptian Environmental Regularity Standards for wastewater discharge into the
sea according to discharging levels.

Egypt. J. Chem. 58, No.6 (2015) 621

622 M.H. El-Awady et al.

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(Received 31/ 8/2015;

accepted 7/10/2015)

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‫‪624‬‬ ‫‪M.H. El-Awady et al.‬‬

‫معالجة المخلفات السائلة للصناعات البترولية باستخدام طريقتي‬

‫التعويم الهوائي واألكسدة الحديثة‬
‫*‬
‫محمد حمدي العوضي ‪ ،‬إبراهيم عبدالفتاح و أحمد ابوالمجد‬
‫قسم بحوث تلوث المياه ‪ -‬المركز القومي للبحوث ‪ 33 -‬شارع البحوث ص‪.‬ب‬
‫‪ -21611‬الدقى ‪ -‬الجيزة و * قسم الهندسة المدنية ‪ -‬كلية الهندسة بشبرا ‪ -‬جامعة‬
‫بنها ‪ -‬مصر‪.‬‬

‫أجريت هذه الدراسة الزالة الملوثات البترولية الخطرة والزيوت من المخلفات‬

‫السائلة باستخدام طريقتي التعويم الهوائي واالكسدة الحديثة‪ .‬تم تجميع المخلفات‬
‫السائلة من أحدى شركات البترول الكائنة على مدينة ساحلية شمال مصر‪ .‬لقد تم‬
‫تحديد نوعيين من المخلفات السائلة لمعالجتهما األول والذي تم تجميعه بعد وحدة‬
‫فصل الزيوت بالشركة حيث توجد بها كميات كبيرة من الزيوت‪ ،‬تم معالجتها‬
‫باستخدام طريقة التعويم المضغوط وفيها تم إزالة الزيوت والشحوم والحمل‬
‫العضوي متمثال" في االحتياج األكسوجيني الكيميائي وكذلك التخلص من المواد‬
‫الصلبـة العالقة عند الظـروف المثلــى للتشغيــل بنسب وصلت إلــى ‪ ٪89‬و ‪ ٪86‬و‬
‫‪ ٪81‬على التوالي‪ .‬أما النوع الثاني من المخلفات فقد تم تجميعه من مخرج وحدة‬
‫إنتاج النافثا حيث تتركز فيها أحمال عالية من الفينوالت والتي وصلت إلى‪261‬‬
‫مجم‪/‬لتر‪ .‬ونظرا" لهذا التركيز من المركبات العضوية فقد تم إختيار المعالجة‬
‫بإستخدام تفاعل فينتون لتكسير مركبات الفينول والتي تجاوزت اإلزاله ألكثر من‬
‫‪ ٪88.8‬من تركيزه في المخلف الخام ‪ ،‬هذا وقد تجاوزت ازالة االحتياج‬
‫األكسوجيني الكيميائي ألكثر من ‪ ٪99‬عند الظروف المثلى للتشغيل‪.‬‬

‫)‪Egypt. J. Chem. 58, No.6 (2015‬‬