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Polyacrylamide induced coagulation process removing suspended solids from

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ISSN: 0149-6395 (Print) 1520-5754 (Online) Journal homepage: http://www.tandfonline.com/loi/lsst20

Polyacrylamide-induced coagulation process

removing suspended solids from palm oil mill
effluent

Ali Akbar Zinatizadeh, Shaliza Ibrahim, Nasrin Aghamohammadi, Abdul

Rahman Mohamed, Hadis Zangeneh & Parviz Mohammadi

To cite this article: Ali Akbar Zinatizadeh, Shaliza Ibrahim, Nasrin Aghamohammadi, Abdul
Rahman Mohamed, Hadis Zangeneh & Parviz Mohammadi (2016): Polyacrylamide-induced
coagulation process removing suspended solids from palm oil mill effluent, Separation Science
and Technology, DOI: 10.1080/01496395.2016.1260589

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SEPARATION SCIENCE AND TECHNOLOGY
http://dx.doi.org/10.1080/01496395.2016.1260589

Polyacrylamide-induced coagulation process removing suspended solids from

palm oil mill effluent
Ali Akbar Zinatizadeha, Shaliza Ibrahimb, Nasrin Aghamohammadic, Abdul Rahman Mohamedd,
Hadis Zangeneha, and Parviz Mohammadie
a
Environmental Research Center, Department of Applied Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Iran; bDepartment of
Civil Engineering, Faculty of Engineering, University of Malaya, Kuala Lumpur, Malaysia; cDepartment of Social and Preventive Medicine,
Faculty of Medicine, University of Malaya, Kuala Lumpur, Malaysia; dSchool of Chemical Engineering, Engineering Campus, University of
Science Malaysia, NibongTebal, Malaysia; eDepartment of Environmental Health Engineering, Kermanshah University of Medical Science,
Kermanshah, Iran

ABSTRACT ARTICLE HISTORY

Palm oil mill effluent (POME) is a colloidal suspension with 2–4% suspended solids. About 50% of the Received 17 March 2016
suspended solids are cellulosic compounds, which are not degraded in the typical biological treatment Accepted 10 November 2016
systems. Chemical (polymer-induced coagulation) and physical (settling) pretreatment methods were KEYWORDS
examined to remove the suspended solids in this study. A novel physicochemical treatment with high Coagulation and
water recovery and sludge compressibility including three cationic polyacrylamides (C-PAM; as coagu- flocculation; polyacrylamide;
lant) and three anionic polyacrylamides (A-PAM; as flocculant) with different molecular weights and palm oil mill effluent;
charge densities was used. The coagulants used were biodegradable. The combination of a C-PAM volatile suspended solids
(Chemfloc1515C) with medium molecular weight and charge density and an A-PAM (Chemfloc 430A)
with high molecular weight and charge density at doses of 300 and 50 mg/dm3 showed the best total
suspended solids (TSS) and chemical oxygen demand (COD) removal (96.4 and 70.9%, respectively).
The optimal condition was found at pH 5, rapid mixing at 150 rpm for 1 min, and slow mixing at 40 rpm
for 30 s. As a conclusion, the physiochemical pretreatment using biodegradable coagulants was a
promising alternative to effectively separate TSS (96.4%) with high water recovery (76%).

Introduction
Palm oil is one of the world’s most important vegetable oils.
It is used mainly for edible purposes and has become an
important raw material for many applications since the past
few decades. A typical palm oil mill releases liquid effluent,
known as palm oil mill effluent (POME).[1] This effluent, if
not disposed properly, will have a great adverse impact on
the surrounding environment.[2,3] POME is highly pollut-
ing due to its organic nature, and its discharge to a relatively
small river can be devastating to its ecosystem, which is
caused by oxygen depletion owing to its high chemical
(COD) and biochemical (BOD) oxygen demands.[4–6]
POME is a thick, brownish, viscous liquid waste discharged
from the palm oil mills during the extraction of palm oil
from the fruits and is nontoxic but has an unpleasant odor.
POME is a colloidal suspension of 95–96% water, 0.6–0.7%
oil, and 4–5% total solids, including 2–4% suspended solids
with a BOD higher than 20 g/dm3 originating from a
mixture of sterilizer condensate, separator sludge, and
hydro cyclone wastewater.[2,3,7,8]
Complete anaerobic digestion of the raw POME with-
out pretreatment demands high hydraulic retention time
(HRT), which is not easily achieved due to the high
volume of POME produced by most palm oil mills.
Coagulation–flocculation is widely used for industrial
wastewater pretreatment, as it is efficient and simple to
operate and many factors can influence its efficiency, such
as the type and dosage of coagulant/flocculant, pH, mix-
ing speed and time, temperature and retention time.[9]
Recently, natural coagulants/flocculants such as rice
starch[10] and Cassia obtusifolia seed gum[11] were
attempted successfully in the treatment of POME. Shak
and Wu (2015) found that the combination between alum
and C. Obtusifolia seed gum treated POME adequately at
natural pH with lesser alum dosage and shorter settling
time, reflecting the importance of using both coagulant
and flocculant in the treatment of POME efficiently.[12]
As typical flocculants, polyelectrolytes are widely used to
decrease colloidal stability and thus initiate flocculation.
During polyelectrolyte-induced flocculation, polymer

CONTACT Ali Akbar Zinatizadeh zinatizadeh@razi.ac.ir Environmental Research Center, Department of Applied Chemistry, Faculty of Chemistry, Razi
University, Kermanshah, 67149-67346 Iran.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/lsst.
© 2017 Taylor & Francis
2 A. A. ZINATIZADEH ET AL.
adsorption onto colloid surfaces is vital.[13] High molecu-
lar weight water-soluble polymers are widely used to
induce the aggregation of aqueous colloids. In most
cases, the flocculants are slightly cationic, to encourage
adsorption, and are linear with molecular weights in the
millions. Cationic copolymers of polyacrylamide (PAM)
are typical examples.[14]
In one study, four different types of coagulant combina-
tions, aluminum sulfate, ferric chloride, ferric sulfate, and
ammonium sulfate, with a commercial polymer SR316 as
flocculant were investigated as a pretreatment of POME.
The coagulation and flocculation processes could reduce
turbidity by about 97% and COD removal by 64% by the
combination of coagulants (10% of ferric sulfate, 1% of
alum, and 1% w/w of ammonium sulfate with commercial
polymer SR316).[15] In another study, a modified indus-
trial-grade alum (Envifloc-40L) as a coagulant and Profloc
4190 as a flocculant were examined. Statistically designed
experiments were used to optimize three variables in the
coagulation–flocculation process, including the coagulant
dosage, the flocculant dosage, and pH. The optimum values
of the tested variables were determined as 15000 mg/dm3,
300 mg/dm3, and 6 for coagulant dose, flocculant dose, and
pH, respectively. Turbidity of 19 nephelometric turbidity
unit (NTU) and water recovery of 76% were obtained at the
optimum condition.[16] Moringaoleifera, as an environ-
mental-friendly and natural coagulant, was tested for the
pretreatment of POME.[17] In that study, 95% suspended
solids removal and 52.2% COD removal were reported.
Sludge produced in the process had a high sludge volume
index (SVI) (210 cm3/g), indicating low water recovery
(50.25%).[17,18]
Due to high suspended solids concentration in raw
POME and its adverse effect on microbial flocs, a pre-
treatment process is necessary before this effluent can be
anaerobically treated by a high-rate anaerobic digester.[8]
A fraction of total suspended solids (TSS) that is not
digestible gradually accumulated in the bioreactors by
attaching to the sludge flocs, causing degradation in
process efficiency. From a practical point of view and
in order to have a reliable, stable, and efficient high-rate
anaerobic process, the oil-bearing suspended solids need
to be removed (partially or completely) before the anae-
robic treatment. About 50% of the suspended solids are
cellulosic compounds, which are not degraded in the
typical biological treatment systems. With regard to
POME characteristics, alternative/complementary com-
binations of physical-chemical-biological processes are
needed for the adequate treatment of this wastewater.
Thus, the combination of coagulation–flocculation and
anaerobic/aerobic biotreatment processes might sub-
stantially reduce the HRT operating conditions using
six different biodegradable cationic polyacrylamides
(C-PAM) and anionic polyacrylamides (A-PAM),
which have not been reported to date. Therefore, the
present work is focused on investigating the efficiency
of a pretreatment coagulation–flocculation stage under
different operating conditions using six different biode-
gradable C-PAM and A-PAM.
Experimental
Wastewater characteristics
POME samples were weekly taken from a nearby palm
oil mill in Nibong Tebal, Penang, Malaysia. The sam-
ples were stored in a cold room (4°C) before use. This
storage step had no observable effect on its composi-
tion. The characteristics of the POME sample used in
this study are as shown in Table 1.
Settling characteristics of POME’s suspended solids
In order to study the settling ability of suspended solids’
content of POME, the zone settling test was carried out. A
transparent cylinder with 1 m height and 5 cm diameter
was used as the settling vessel (Fig. 1). The column was
equipped with six sampling ports at various heights to
analyze the water composition at each height. By using a
thin rod, the suspension near the vessel wall over the
entire depth of suspension was gently stirred at a low
peripheral speed. Raw POME was maintained in a con-
tainer under a uniformly mixed condition. A well-mixed
sample was taken from the container and the settling
vessel was filled to its height (100 cm). The height of the
solid–liquid interface was recorded at intervals of 30 min
for 3 h and samples were then taken from each sampling
port to measure TSS to represent the suspended solids’
concentration in the sample. At the end of the experi-
ment, a suitable settling time was obtained and applied for
the pre-settled POME biological digestion.
Physicochemical pretreatment (coagulation and
flocculation)
A standard jar test unit (SW1, Stuart scientific, UK) was
applied as the flocculator in this study. It is equipped
Table 1. Characteristics of POME sample used in the chemical
pretreatment study.
Parameter Amounta
COD (mg/dm3) 49200
Soluble COD (mg/dm3) 22800
SS (mg/dm3) 19800
Oil and grease (mg/dm3) 5100
pH 4.0
a
Values are averages of three measurements. The differences between the
measurements for each parameter were less than 1%.
 SEPARATION SCIENCE AND TECHNOLOGY 3

Analytical methods
The concentrations of COD, TSS, and oil and grease were
determined by using standard methods.[19] For COD, a
colorimetric method with the closed reflux method was
developed. A spectrophotometer (DR 5000, Hach,
Jenway, USA) at 600 nm was used to measure the absor-
bance of the COD samples. Oil and grease was measured
by the partition gravimetric method. In this method, oil
and grease content of the sample was initially extracted by
n-hexane as the solvent. n-hexane was then evaporated in
a rotary evaporator. The residual is reported as oil and
grease.[19] Scanning electron microscopy (SEM) was used
to examine the physical features of the suspended parti-
cles. The sample was examined using a Leo Supra 50 VP
Field emission SEM (UK) equipped with Oxford
INCA 400 energy-dispersive X-ray microanalysis system.

Results and discussion

Figure 1. 1-m column for the settling test.
Zone settling

Table 2. The properties of the polyacrylamides used. Primary sedimentation was used as a method to remove
Polyacrylamides Molecular weight Charge Charge density suspended solids and oil and grease as is currently done in
Organopol 5415 Very high Cationic Low the ponding system in most palm oil mills. Poor settlability
Chemfloc 3876 Medium Cationic High of the suspended solids makes the separation difficult.
Chemfloc 1515C Medium Cationic Medium
Chemfloc 430A High Anionic High As POME contains a high concentration of oil-bearing
AN 913 High Anionic Low suspended solids, both hindered or zone settling and com-
AN 913 SH Very high Anionic Low
pression settling usually occur in addition to discrete (free)
and flocculant settling. The settling phenomenon is illu-
with six paddles, diameter 6.4 × 10−2 m (6.4 cm) and strated in Fig. 2. Because of the high concentration of fine
the speed ranging from 0 to 227 rpm. Six C-PAMs particles, the liquid tended to move up through interstices
and A-PAMs of commercial grade in a wide range of of the contacting particles. As a result, the contacting
molecular weights and charge densities were used. particles tended to settle as a zone or blanket.[20] A recog-
Organopol 5415 was supplied by Ciba Speciality nizable interface developed between the upper region and
Chemicals. Chemfloc 1515C and Chemfloc 430A were the zone-settling region, as represented in Fig. 2. As
supplied by Chemkimia. AN 913 and AN 913SH, man- settling continued, a compressed layer of particles began
ufactured by SNF Floerger, were provided by Kempro. to be formed at the bottom of the settling column in the
The properties of the PAMs used are as shown in compression-settling region.
Table 2. As the compression layer formed, regions containing
In order to determine the optimum dosage of the lower concentrations of solids than those in the com-
PAMs, a range of dosage was examined for selected pression region extended upward in the settling column.
C-PAM and A-PAM as 100–600 and 10–110 mg/dm3, Thus, the zone settling region contained a gradation in
respectively. In every test, 500 cm3 of raw POME sample solids concentration from that found at the interface of
was used. After C-PAM (as the coagulant) was added the settling region to that found in the compression-
with a certain dosage, the sample was mixed rapidly at settling region. From Fig. 2, the height of the interface
150 rpm for 1 min. A-PAM was then added as a floccu- maintained almost constant after 3 h. Figure 3 depicts a
lant and the sample was mixed slowly at 40 rpm for 30 s. 3-D graph for TSS removal at different heights of settling
The flocs formed were allowed to settle for 30 min. After column and settling time. It shows that 86.8–62.5% TSS
settling, TSS, COD, and oil and grease of the supernatant removals (corresponding to TSS concentrations of 2580
were determined. The experiments were conducted in and 7340 mg/dm3, respectively) were obtained from
duplicate. sampling ports 1 and 4, respectively, after 3 h, whereas
4 A. A. ZINATIZADEH ET AL.

100

100 90

90 80
Zone settling

Height of interface, cm
80 70

Height of interface, cm
70 60
60 50 Transition settling
50
40
40
30
30 Compression
20 settling
20
10 10

0 0
0 60 120 180 240 300 360
0

0
50

80

12

18

22

27

36
Time, min
Time, min
(a) (b)

Figure 2. Definition sketch for POME zone settling: (a) settling column and (b) the corresponding interface settling curve.

about 50% water recovery was obtained. The results
showed that the fiber suspended particles are light and
bulky. SEM of the fiber-shaped particles is shown in
Fig. 4.
Physicochemical pretreatment
Initially, the effect of various C-PAMs and A-PAMs was
examined separately. Figure 5 shows the effect of C-PAMs
on the TSS removal at various dosages (100–600 mg/dm3).
From Fig. 5, Organopol 5415 and Chemfloc1515C showed
a better performance compared with Chemfloc 3876.
Despite the relatively high molecular weight of
Organopol 5415, more compacted sludge was obtained
with Chemfloc1515C (with medium molecular weight
and charge density). The sludge volume obtained with
Chemfloc1515C was 860 cm3/dm3 after 30 min of settling,
100
80
TSS removal, %
whereas it was 940 cm3/dm3 for Organopol 4515. This
result was due to the lower charge density of Organopol
5415 to sufficiently neutralize a large number of negatively
charged particles present in POME. Another contributing
factor was based on the fact that polyelectrolytes with very
high molecular weights do not readily dissolve in water but
tend to form gel lumps.[21]
As can be seen in Fig. 5, only 10% of TSS removal was
obtained without the addition of C-PAM, which was
attributed to gravity settling. Around 92.4 and 91.7%
TSS removals were achieved at 200 mg/dm3 of both
Organopol 4515 and Chemfloc1515C. No further
improvement in TSS removal was observed at dosages
higher than 200 mg/dm3 for all C-PAMs. The same
experiments were carried out with A-PAMs at various
dosages (10–100 mg/dm3), but no positive improvement
in the removal of TSS and COD was achieved for the
three A-PAMs. This result was associated with the inten-
sification of repulsion forces between negatively charged
particles in POME and the A-PAM molecules.
0
20
Due to poor compressibility of the sludge (high sludge
40
60
volume) obtained with C-PAMs and in order to improve
80 the effectiveness in the removal by C-PAMs, two selected
100
C-PAMs (Organopol 5415 and Chemfloc1515C) were
tested with subsequent addition of the various A-PAMs.

60

The experimental results in the first part showed that better

40
sludge characteristics were found at the dosage of C-PAM
20 and A-PAM of 250 and 100 mg/dm3, respectively.
180
160 Therefore, the obtained amounts were considered as
0 140
120 doses of the chemicals used in the following test to explore
in

100
m

the best combination of the selected C-PAMs and A-PAMs.

e,

80
6
m

5 60
Ti

4
3
40 Figure 6a and b shows the performance of the pretreatment
2 20
S am
p lin g 1 0 process in terms of TSS and COD removals for Organopol
p ort 0
5415 and Chemfloc1515C, respectively, in combination
Figure 3. 3-D graph for TSS removal at different heights of with various A-PAMs. As can be seen, the combination of
settling column and settling time. Chemfloc1515C and Chemfloc 430A showed the best result

Figure 4. SEM of the fiber-shaped particles in POME.
100
90
80
70
TSS removal, %
60
50
40
30
20
10
0
0 100 200 300
Dosage of C-PAM, mg/dm
Organopol 5415 Chemfloc 3876
Figure 5. TSS removal of C-PAM at various dosages.
with 95 and 70.8% TSS and COD removal, respectively,
with better sludge settling characteristics.
The aggregation of the particles occurred through
two mechanisms, i.e. charge neutralization and a
sweep-floc mechanism.[10] Apart from lowering the
surface charge on the particles (mostly by C-PAM),
these polymers formed bridges between particles and
polymer. Subsequently, the bridged particles become
intertwined with other bridged particles during the
flocculation process.[20] Finally, Chemfloc 430A as an
A-PAM enhanced the flocculation process through
bridging the intertwined flocs.
To determine the optimum dosage of the combined
PAMs, different combinations of Chemfloc1515C (as
C-PAM) and Chemfloc 430A (as A-PAM) at different
SEPARATION SCIENCE AND TECHNOLOGY 5
dosages were then examined. The ranges of explora-
tion for the C-PAM and A-PAM were 100–600 and
10–110 mg/dm3, respectively. Figure 7a and b, respec-
tively, shows TSS and COD removal by combinations
of various dosages of PAMs. It is noted in the
figures that at 300 mg/dm3 of Chemfloc1515C and
50 mg/dm3of Chemfloc 430A, the highest TSS and
COD removal (96.4 and 70.9%, respectively) were
achieved. At the optimum condition, sludge volume
400 500 600 700 after 30 min of settling was 660 cm3/dm3. Oil and
3
grease was measured throughout the experiments and
Chemfloc 1510C higher than 95% oil and grease removals were
achieved in all experimental conditions studied.
The sludge produced at the optimum condition is
shown in Fig. 8. This figure confirms the high com-
pressibility of the sludge. It must be noted that the
sludge compressibility is one of the important factors
to improve sludge dewatering. In the sludge dewater-
ing, the filtrate flow becomes independent of the pres-
sure applied for such an extremely compressible
solid.[22] As seen in the figure, residual turbidity of
the supernatant is very less due to high integrity in
the sludge produced. Ariffin et al.[23] reported lower
dosages of their synthesized PAMs compared with the
optimum dosages obtained in this study. This may be
due to the different compositions of the PAM used in
this study during the manufacturing processes. The
optimum conditions obtained from this study can be
used for the chemical pretreatment of POME prior to
its post-treatment in an anaerobic treatment process.
6 A. A. ZINATIZADEH ET AL.

TSS removal,% TCOD removal, %

95 91 92

TSS and COD removal, %

100
90
80 71
70 61 60
60
50
40
30
20
10
0
Chemfloc 1510C & Chemfloc 430A Chemfloc 1510C & AN 913 Chemfloc 1510C & AN 913SH
Combination of A-PAM and C-PAM
TSS removal, % TCOD removal, %
TSS and COD removal, %

91 94 90
100
90
80 66
70 59
60 46
50
40
30
20
10
0
Organopol 5415 & Chemfloc 430 A Organopol 5415 & AN 913 Organopol 5415 & AN 913SH
Combination of C-PAM and A-PAM

Figure 6. TSS and COD removal by combinations of C-PAM and A-PAM; (a) a C-PAM (Organopol 5415) at a dosage of 350 mg/dm3
with various A-PAM at 100 mg/dm3, (b) Chemfloc 1510C at a dosage of 350 mg/dm3 with various A-PAM at 100 mg/dm3.

100 80

98 75
TSS removal, %

COD removal, %

70
96
65
94
60
92
55

90 50
0 20 40 60 80 100 120 0 20 40 60 80 100 120
3 3
Dosage of Chemfloc 430A (A-PAM), mg/dm Dosage of Chemfloc 430A (A-PAM), mg/dm
Chemfloc 1510C (C-PAM) = 100 mg/dm3 Chemfloc 1510C (C-PAM) = 200 mg/dm3 Chemfloc 1510C (C-PAM) = 100 mg/dm3 Chemfloc 1510C (C-PAM) = 200 mg/dm3
Chemfloc 1510C (C-PAM) = 300 mg/dm3 Chemfloc 1510C (C-PAM) = 400 mg/dm3 Chemfloc 1510C (C-PAM) = 300 mg/dm3 Chemfloc 1510C (C-PAM) = 400 mg/dm3
Chemfloc 1510C (C-PAM) = 500 mg/dm3 Chemfloc 1510C (C-PAM) = 600 mg/dm3 Chemfloc 1510C (C-PAM) = 500 mg/dm3 Chemfloc 1510C (C-PAM) = 600 mg/dm3

(a) (b)

Figure 7. (a) TSS removal and (b) COD removal by combinations of a C-PAM (Chemfloc 1510C) and an A-PAM (Chemfloc 430A) at
various dosages.

Figure 8. Sludge produced at the optimum condition.


Conclusions
Removal of the suspended solids from raw POME
using a novel physicochemical treatment with high
water recovery and sludge compressibility was
successfully performed using three C-PAMs (as the
coagulant) and three A-PAMs (as the flocculant)
with different molecular weights and charge densities.
The combination of a C-PAM (Chemfloc1515C) with
medium molecular weight and charge density and an
A-PAM (Chemfloc 430A) with high molecular weight
and charge density at dosages of 300 and 50 mg/dm3,
respectively, showed the best effectiveness in removing
TSS and COD (96.4 and 70.9%, respectively). Oil and
grease removal was higher than 95% in all experimen-
tal conditions studied. The chemical pretreatment
approach seemed more suitable with higher TSS and
COD removal efficiency and more compressible
sludge. As a conclusion, the chemical pretreatment
using the biodegradable coagulants is a promising
alternative to effectively separate TSS with high water
recovery (76%).
Funding
The financial support provided by Universiti Sains Malaysia
(USM) and University of Malaysia (UM) is gratefully
acknowledged. The greatest appreciation goes to the industry
personnel for their full cooperation.
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