Current Science International Volume : 09 | Issue : 01| Jan.- Mar.

| 2020
EISSN:2706-7920 ISSN: 2077-4435 Pages: 87-96
DOI: 10.36632/csi/2020.9.1.11
Study on Ferric Chloride Coagulation Process and Fenton’s Reaction for
Pretreatment of Dairy Wastewater

Omnya A. El-Battrawy, Mervat A. El-Sonbati, Ebtesam M. El-Awadly and Talaat A.

Hegazy

Department of Environmental Sciences, Faculty of Science, Damietta University, Egypt.

Received: 30 Nov. 2019 / Accepted 05 Feb. 2020 / Publication date: 25 Feb. 2020

ABSTRACT
Nowadays, much attention is given to dairy industries wastewaters because of their upward
pollution potential arising out of the industrialization and numerous anthropogenic activities.
Unplanned discharge of wastewaters to waterways can prompt environmental damage. Therefore,
treatment is necessary prior discharge or reuse of water. This research work on the laboratory scale is
utilized for the characterization and evaluation of the efficiency of chemical coagulation followed by
advanced oxidation process as a pretreatment technique for dairy industries wastewaters. Three
composite wastewater samples were collected from diary industries plant at New Damietta City
during the year 2018 and characterized for some physicochemical parameters to check their pollution
potential. One sample is chosen and subjected to pretreatment using chemical coagulation/
precipitation by FeCl3 with lime and polyacrylamide as coagulant aides followed by advanced
oxidation process with Fenton’s reagent. The results showed that concentration of chemical oxygen
demand is 76800 mg/L while for biochemical oxygen demand is 60000 mg/L. Removal efficiency of
COD after applying FeCl3 / lime was (94.2%) while for FeCl3 / polyacrylamide was (70%). The
optimum conditions of Fenton’s reaction were 30 ml/L (H2O2) and pH 7.35 that achieved 95% of
COD removal. It’s concluded that using Fenton oxidation process after coagulation by FeCl3 with
lime was found a little enhancement in the COD removal of dairy wastewater effluents.

Keywords: Dairy effluents, physicochemical parameters, coagulant aides, lime, COD removal.

Introduction
The dairy industry is one of the most contaminating of industries in terms of effluent volume
produced and its characteristics as well. Numerous dairies of various sizes have come up in different
places as a result of increasing demand for milk and milk products (Sivaprakasam and Balaji, 2019).
Dairy processing effluents are produced in an irregular manner and the flow rates of these effluents
change considerably (Shete and Shinkar, 2013). The nature and composition of wastes relies upon
type of goods produced and processing capacity of the plants (Jain et al., 2018).
Dairy wastewaters are characterized by high levels of chemical oxygen demand (COD) and
biochemical oxygen demand (BOD) (Patil and Hugar, 2015). The ratio COD / BOD shows the
biodegradability of organic materials in aerobic or anaerobic condition (Suman et al., 2017). Dairy
wastewater is often discharged intermittently to the near stream or land without earlier treatment
causing serious pollution issues. Dairy effluents deplete rapidly the dissolved oxygen level bringing
about anaerobic conditions of the receiving streams and release of foul odors (Prazeres et al., 2013).
Dairy wastewater should be pretreated before biological treatment due to the presence of
detergents and oil and grease that encourage the creation of filamentous organisms which forms scum
and foam layers in the aeration tanks and finally inhibit the treatment process (Ying et al., 2002). In
addition, adsorption of oil and grease on the sludge surface may constrain the exchange of oxygen and
soluble substrates to biomass which prompts decrease in the rate of substrate conversion (Farizoglu
and Uzuner, 2011)
Coagulation/flocculation is a commonly utilized process in water and wastewater treatment
(Khouni et al., 2011) in which coagulants such as ferric chloride and/or polymer are provided to
wastewater to destabilize the colloidal materials and allow small particles to agglomerate into larger
settleable flocs (Amud and Amoo, 2007). FeCl3 is a significant coagulant in wastewater treatment and

Corresponding Author: Omnya A. El-Batrawy, Associate Professor, Environmental Sciences Department,

Faculty of Science, Damietta University, New Damietta City, Box 34517, Damietta,
Egypt. E-mail: om_elbattrawy@du.edu.eg
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can be utilized for decolourization (Papic et al., 2000), treatment of organic pollutants (Jain et al.,
2018), treatment of detergent wastewater (Aygun and Yilmaz 2010), treatment of petrochemical
industries wastewater (Altaher et al., 2011), and treatment of diary wastewater (Prazeres et al., 2013).
Coagulation/flocculation has a preference in the primary treatment processes mostly because of the
ease of operation, high efficiency, and cost effective (AlMubaddal et al., 2009).
The application of advanced oxidation processes (AOPs) after the chemical and/or biological
processes can establish a promising alternative to reduce recalcitrant organic matter, principally,
because of the formation of hydroxyl radicals (Aygun and Yilmaz 2010). These radicals, acts as
powerful oxidizing agents, and have enough potential to efficiently destruct pollutants and make
wastewater less toxic (Ahmad et al., 2016). The Fenton process is a widely applied AOP which is a
mixture of ferrous/ferric iron (catalyst) and hydrogen peroxide (oxidizing agent) (Gu et al., 2013).
This work is conducted to investigate the efficiency of chemical coagulation using ferric
chloride with lime and polyacrylamide as coagulant aides as a pretreatment techniques for dairy
industries wastewater. The optimum conditions were determined for FeCl3 with both coagulant aids.
The efficiency of advanced oxidation process using Fenton reagent after coagulation with FeCl3 and
lime was also optimized and evaluated. Emphasis will be given to the removal efficiency of the COD.

Materials and Methods

Sampling Site
The wastewater samples were collected from a plant for manufacturing dairy products located
in the industrial Zone of New Damietta City, Damietta, Egypt. Three composite water samples (S1-
S3) were collected during the year 2018 according to the availability of sampling. The samples were
collected in high density polyethylene (HDPE) containers that were routinely acid-treated and well
rinsed with de-ionized water prior to use, dried, and stored with the caps on to prevent contamination.

Physico-Chemical Characterization
All the dairy wastewater samples were characterized for some physicochemical parameters
such as pH, Electrical Conductivity (EC), Turbidity, Salinity, Total Solids (TS), Total Dissolved
Solids (TDS), Dissolved Oxygen (DO), Biological Oxygen Demand (BOD), Chemical Oxygen
Demand (COD), Oil & Grease, Total Nitrogen (TKN),Total Phosphorus (TP), and have been
determined according to Standard Method (APHA, 2017). The pH of the samples was measured
directly by pH Meter (model, 211 HANNA, USA). Salinity, Electric conductivity (EC) and Total
Dissolved Solids (TDS) of the samples were determined by Digital Portable TDS/ Conductivity meter
(Model 8033 HANNA,USA).Turbidity of samples was measured by Turbidimeter (Al1000 aqualytic
Germany with measuring 0-200 NTU).The Total Solids (TS) are determined by the evaporation of a
sample at (105ºC) according to the method of Adams (1991).

Coagulation/Precipitation (C/P) Process

Sample (S3) was chosen to be subjected to pretreatment processes using FeCl3 as coagulants
where lime and polyacrylamide as coagulants aids. Lime was used after conversion to milk-of-lime
which is slurry of Ca (OH)2 in water (Asadi, 2006). The optimum condition (pH, doses, etc.,) were
determined for both FeCl3 and coagulant aides. Chemical coagulation experiments were conducted
with the jar test according to Rump (1999). Six beakers containing 1000 mL dairy industries
wastewaters sample were placed on a standard jar test apparatus. A flash/rapid mixing at 100 rpm for
2 min was carried out after adding the coagulant dose; then the slow mixing was carried out at 20 rpm
for 25 min. Thereafter, jars were kept standstill for 20 min to settle down the flocs. A series of jar tests
were performed to determine the effect of coagulant, coagulant aids doses and initial pH on COD
removal from dairy industries wastewaters. The removal percent of COD was calculated (Eq. 1).

Removal % = × 100 ……………………………………………………………...........(1)

where ci and cf are the initial and final COD concentration, respectively.

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Advanced Oxidation Process by Fenton’s Reagent

The Fenton’s reagent was prepared according to (Benatti and Tavares, 2014) which consists of
H2O2, ferrous ions with pH adjustment. Fenton’s reaction was applied on the dairy wastewater after
C/P with FeCl3 and lime. The effects of ferrous ion, hydrogen peroxide concentration and pH on the
treatment of the dairy industries wastewater were investigated. All experiments were performed in a
Jar Test apparatus (Rump, 1999).

Results and Discussion

Physico-Chemical Characterization
The characterization of the dairy industries wastewater samples was shown in Table (1). The
results showed that concentration of COD ranged from 20520 to 76800 mg/L while BOD ranged from
14290 to 60000 mg/L. Oil and grease, TP, TKN and TS are (672.4-774.8 mg/L), (3133-5193.11
mg/L), (1424-1772.5 mg/L) and (11732-131686 mg/L), respectively. The broad range of the
concentrations of the investigated parameters of samples may be attributed to the differences of
organic content of dairy wastewater during the year (Slavov, 2017). The high organic load was mainly
due to dissolved milk protein and sugars. Tawfik et al. (2008) studied wastewaters from Arab Dairy
Factory and found COD, BOD and TS (3383±1345 mg/L), (1941±864 mg/L), and (831±392 mg/L),
respectively. Deshannavar et al. (2012) examined wastewaters from Dairy effluent and found that the
concentration of COD, BOD and TS were (1900-2700 mg/L), (1200-1800 mg/L), and (900-1350
mg/L), respectively.

Table 1: The physicochemical characterization of the dairy industries wastewater samples.

Parameter Unit S1 S2 S3
pH - 5.99 4.56 4.35
Total Dissolved Solids (TDS) g/L 41.5 41.8 34.2
Electrical Conductivity (EC) ms/cm 50.9 54.1 48
Salinity % 42.8 43 35.7
Turbidity NTU 100 3595 2505
BOD mg/L 14290 35000 60000
COD mg/L 20520 70400 76800
Oil and grease mg/L 672.4 774.8 723.8
Total Phosphorous (TP) mg/L 10636 5193.11 3133.4
Total Solids (TS) mg/L 127818 131686 117312
TKN mg/L 1682.54 1772.5 1424.606

Coagulation/Precipitation Process
Coagulation and flocculation are the procedures used to remove the particles responsible for
colour and turbidity. The colloidal particles found in wastewaters generally have a negative electrical
charge and are surrounded by an electrical double layer because of attachment of positively charged
ions from the surrounding solution. They remain suspended because of their low specific gravity.
Coagulants are added to flocculate colloidal particulates into bigger particles that can be evacuated by
sedimentation or flotation (Loloei et al., 2019).
The effect of ferric chloride concentration (0 - 0.6 g/L) on the coagulation process was critically
examined (Fig. 1). It is obvious that, COD removal percentage increased from 33.2 to 51.4% with
increasing ferric chloride dose up to 0.1 g/L. This may be attributed to increase the super saturation of
Fe (OH)3 which improved the nucleation rate and consequently the floc growth rate. Therefore,
removal of larger amounts of COD was attained because of the availability of bigger surface area on
which organic matter adsorption occurred. On the contrary, low doses of FeCl3 prompted the
development of larger but fewer flocs because of faster growth rate comparative with nucleation rate
resulting in a smaller surface area (Amud and Amoo, 2007). Increasing the ferric chloride dose over
0.4 g/L exerts adverse effect in the coagulation efficiency. Therefore, the optimum ferric chloride
dose that improved COD removal will not exceed 0.1 g/L. Moreover, the percent removal of COD at
zero ferric chloride dose is 33.2 %, this due to plain sedimentation, the suspended solids or settable

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fraction, are removed from the solution by gravitation to the floor of the container to form sludge
under near quiescent conditions. This process also removes settleable organic and inorganic materials
and thus reducing the organic load (Al-Asmar, 2006).
Mahvi et al. (2004) studied the removal of anionic surfactants in detergent wastewater by
chemical coagualation and found that when ferric chloride, alum and lime were utilized as a
coagulant, COD removal percents were 89%, 37% and 21%, respectively. Aygun and Yilmaz (2010)
used coagulation-flocculation process to treat detergent wastewater and found that the optimum dose
of the ferric chloride was 2 g/L with removal efficiency 71%. Altaher et al. (2011) used ferric chloride
coagulant for pretreatment of wastewater streams from petroleum/petrochemical industries and found
that FeCl3 had greater efficiency compared with other coagulants with optimum dose of 800 mg/L.
Loloei et al. (2019) studied the coagulation process in wastewater treatment of dairy industries and
found COD removal efficiency of dairy products industry wastewater was 68 and 62% at the optimum
conditions (1 g/L at pH 5) for alum and ferrous sulphate, respectively.

80000 COD (mg/l) COD Removal (%) 60

70000
50
60000

COD Removal(%)
40
COD (mg/l)

50000

40000 30

30000
20
20000
10
10000

0 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Dose of FeCl3(g/L)

Fig 1: Effect of FeCl3 dosages on the effluent COD and COD removal efficiency.
For determination the optimum pH of ferric chloride, pH values (4.66- 9.33) were examined at
ferric chloride dose of 0.1 g/L (Fig. 2). It is obvious that, the optimum pH is 8.36. Around pH 8.39, Fe
(OH)3 is found which is a hydrophobic compound and can adsorb contaminants in particulate form by
surface interactions (Dominguez et al., 2005).

COD(mg/l) COD Removal(%)

80000 60

70000
50
60000
COD Removal(%)

40
50000
COD (mg/l)

40000 30

30000
20
20000
10
10000

0 0
4.66 5.66 6.66 7.66 8.66 9.66
pH Values

Fig 2: Determination of optimum pH value at FeCl3 dose of 0.1 g/L.

El-Gohary et al. (2010) studied pretreatment of personal care products (PCPs) wastewater and found
two optimum pH values, 4.66 in the acidic range and 8.36 in the alkaline range. Aygun and Yilmaz
(2010) reported optimum pH was 11 at FeCl3 dose of 1.5 g/L as COD removal efficiency increased

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from 34% to 57% when pH increased from 4 to 11. Altaher et al. (2011) used ferric chloride
coagulant for pretreatment of wastewater streams from petroleum/petrochemical industries and found
that the best turbidity removal was achieved at pH range between 7 and 8.6.
The addition of different doses of polyacrylamide (0 to 2.5 g/L) with constant dose of ferric
chloride (0.1 g/L) was critically studied at pH 8.36 (Fig. 3). It is clear that the optimum dose of
polyacrylamide is 1.5 g/L. COD removal percentage reached to 70.7%. However, the results obtained
indicated that increasing the dose of polymer above 1.5 g/L, is not significant for COD removal.
Synthetic polyelectrolytes are currently the most widely utilized chemicals in industrial wastewaters
treatment. In general, small amount of polyelectrolyte is sufficient to attain high efficiency. The use of
anionic polyacrylamide raises the flocculation efficiency of the coagulant, decreasing the coagulant
amount required for the treatment, raising the settling speed and lowering the process cost (Aguilar et
al., 2005). Coagulation-flocculation process was applied to a slaughterhouse wastewater, utilizing
polyacrylamide as coagulant aid to enhance the settling velocity of the flocs (Mudhoo and Ragen,
2011). Flocculants applications not only caused a decrease of turbidity, but also decrease the soluble
pollutants concentration and consequently improve other quality parameters of wastewaters (Mostafa,
2013). Aygun and Yilmaz (2010) used coagulation-flocculation process to treat detergent wastewater
and reported that the use of FeCl3 with polyelectrolyte as coagulant aids at certain pH gave higher
removal efficiencies (87%) contrasted to coagulation with FeCl3 alone (71%).

COD(mg/l) COD Removal (%)

80000 80

70000 70

60000 60

COD Removal (%)

50000 50
COD (mg/l)

40000 40

30000 30

20000 20

10000 10

0 0
0 0.5 1 1.5 2 2.5 3
dose of polyacrylamide (g/l)
Fig 3: Effect of polyacrylamide dosages on the effluent COD and COD removal efficiency with fixed
dose of FeCl3 (0.1 g/L) at constant pH 8.36.

The influences of different doses of lime (0 to 1.5 g/ L) as coagulant aid in combination with
constant dose of ferric chloride (0.1 g/L) were examined at pH 8.36 (Fig. 4).
COD (mg/l) COD Removal(%)
60000 100
90
50000
80
COCD Removal(%)

70
40000
COD (mg/l)

60
30000 50
40
20000
30
20
10000
10
0 0
0 0.5 1 1.5 2
dose of Lime (g/L)
Fig 4: Effect of lime dosages on the effluent COD and COD removal efficiency with fixed dose of
FeCl3 (0.1g/L) at constant pH 8.36.

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It is obvious that the optimum dose of lime is 0.5 g/L that achieved 94.28% COD removal. However,
the results indicated that increasing lime dose above 0.5 g/L, has negligible effect on COD removal.
Moreover, removal efficiencies were higher than that in case of coagulation with FeCl3 alone. Lime
precipitation is very effective in particulate matter removal than other chemical treatment processes
(Gursoy-Haksevenler et al., 2014). Aygun and Yilmaz (2010) utilized coagulation-flocculation
process for detergent wastewater treatment and found the optimal condition was attained with the
dosage 2 g/L FeCl3 at pH 11 with COD removal efficiency of (71%).

Advanced Oxidation Process by Fenton’s Reagent

Fenton reaction is one effective mechanism of Fenton; iron-salt-dependent decomposition of
hydrogen peroxide, producing the highly active hydroxyl radical (HO•), which has a nonselective
oxidation properties for organic compounds. Regeneration of Fe2+ through formation of superoxide
radical was suggested (Nasr et al., 2016).
To obtain the optimum (Fe2+) dose, investigations were carried out using different Fe2+ doses
ranged between 0.4 g/L and 1.8 g/L. The results presented in Fig. (5) indicated that the maximum
COD removal percent (93.9%) was at zero addition of Fe2+. Hence it may be stated that Fe2+ converts
into Fe3+ as shown in Eq. (2), which acts as coagulant resulting in improved COD reduction and Fe3+
is already remaining in the sample from the previous coagulation/precipitation process. In addition,
according to De Laat and Gallart (1999), the Fe3+ remained can react with H2O2 to generate Fe2+ and
hydroperoxyl radicals [HO2•] in the reaction medium (Eq.3)
Fe 2+ + H2O2 → Fe 3+ + HO• + HO- …………………………………………….......(2)
Fe3+ + H2O2 → HOO• + Fe2+ + H+ ……………………………………………………………………………(3)

The oxidation capacity of HOO• is less comparable to OH•, which affects the overall COD
reduction (Nasr et al., 2016). It is desirable that the ratio of H2O2 to Fe2+ should be as small as
possible, so that the COD removal was not significant due to the remaining of Fe+3 in the sample from
the previous coagulation process. Only 52% of TC was removed by Photo catalytic AOPs (Azat,
2017). Therefore, there is no need for the addition of Fe2+ to the reaction mixture to minimize the cost
of treatment and reduce the formed sludge.

COD CODRemoval(%)
8000 94

7800 93.8
COD Removal(%)

7600
93.6
COD(mg/l)

7400
93.4
7200
93.2
7000

6800 93

6600 92.8
0 0.5 1 1.5 2
Fe+2 Doses
Fig. 5: Determination of optimum dose of Fe+2 in Fenton reaction after coagulation by FeCl3 with
lime.

Different pH values ranging from 1.77 to 8.41 were investigated. The dose of H2O2 was kept
constant at (20ml). The optimum pH value (Fig. 6) was 7.35 where the higher COD removal (94.58
%) was achieved. Loannou et al. (2013) who treated winery wastewater using Fe (II) =10 mg/L,
[H2O2] =100 mg/L and COD removal was 35% at pH 3.5.

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COD(mg\l) COD Removal(%)

9000 95
8000
7000 94.5

COD Removal(%)
6000

COD(mg/l)
94
5000
4000
93.5
3000
2000 93
1000
0 92.5
0 2 4 6 8 10
pH Values

Fig. 6: Determination of optimum pH value of H2O2 in Fenton reaction after coagulation by FeCl3
with lime.
The effect of H2O2 on the COD reduction has been studied. It is expected that as dose of H2O2
to pollutant increased, more hydroxyl radicals are available to descent the organic pollutants and
therefore accelerate their decadence. To obtain the optimum H2O2 dose, investigations were carried
out using different H2O2volumes (0 to 40 ml). The results indicated that significant enhancement of
the COD removal at H2O2 dose of 30ml. Therefore the dose of (30 ml) has been selected as shown in
Fig. (7). The increase in COD removal is comparable to the results presented Gulkaya et al. (2006)
and Kang and Hwang (2000). Adding of H2O2 in amount overrides the stoichiometric ratio of COD:
H2O2=1:1 (55 g/L H2O2) did not improve the respective maximal organic degradation (Jain et al.,
2018). This may be due to auto-decay of H2O2 to oxygen and water (Eq. 4) and the recombination of
OH• radicals (Eq. 6) or play as a scavenger for the OH• radicals according to Haber and Weiss (1934)
(Eq.5)
H2O2 → 2H2O + O2 ………………………………………………………………………….(4)
2OH• ↔ H2O2 ………………………………………………………………………………..(5)
HO• + H2O2 → H+ + H2O + OO·- …………………………………………………………...(6)

Since the OH radical reacts with H2O2, the H2O2 itself plays as the OH• scavenger (Nasr et al.,
2016). Therefore, the H2O2 should be optimally added to achieve the best degradation. Mandal et al.
(2010) used [Fe (II)] =6 g/L and [H2O2] =220 g/L in the treatment of industrial wastewater and
obtained COD removal= ~95% where the optimum condition of [H2O2] =300–600 mg/L, Fe(II)=10
mg/L; pH=3–3.5, room temperature and reaction time =6h were chosen by Yalfani et al. (2009) in the
treatment of Phenol by the homogeneous Fenton reaction.

6200 COD(mg\l) COD Removal(%) 95.1

6100 95

6000
COD Removal(%)

94.9
COD(mg/l)

5900
94.8
5800
94.7
5700

5600 94.6

5500 94.5
0 10 20 30 40 50
H2o2 (ml)
Fig 7: Determination of optimum volume of H2O2 (ml) at pH=7.35 in Fenton reaction after
coagulation by FeCl3 with lime.

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Conclusion
It was observed that the dairy industry wastewater is easily amenable to physicochemical
treatment. This treatment will help in reducing the organic load to facilitate the biological treatment.
The results discussed above indicated that the maximum COD removal efficiency (94.2%) was
obtained from the combination of FeCl3/lime. COD removal efficiency of polyacrylamide with FeCl3
was 70.7%. Applying Fenton oxidation process after coagulation with FeCl3 and lime was achieved a
little refinement in the COD removal. The optimal operating conditions were; zero Fe2+, 30 ml of
H2O2 (30%) and 7.35 pH, the COD removal efficiency was 94.5%.

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