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Rafiq Irfan Zailana, Chien Hwa Chonga and Chee Ming Chooa
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Drying of Oleochemical Sludge
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1.0 Introduction
The production of sludge is mostly from waste water treatment and production of palm
oil and oleochemicals. The sludge is called sewage sludge and palm oil or oleochemical
sludge respectively. Palm Oil Mill Effluent (POME) is formed through the discharge of
water from the extraction of Crude Palm Oil (CPO) from fresh fruit bunches which
involves steam for sterilisation and water for dilution. Palm Oil Sludge is the floating
remains that is separated during the initial stage of POME discharge [1].
In Malaysia, the palm oil industry produces 18.79 million tonnes of CPO annually
which results in the production of POME. CPO produces three times more than the
amount of POME, which is also commonly called as Palm Oil Sludge [2]. Currently, the
wastewater treatment of the sludge is inefficient, uses plenty of resources and many of
the retention time is consumed which leads to high operating cost just for the treatment
of sludge [3]. The production of sludge has been a major problem since the cost which
includes treatment, transportation and disposal represents 50% to 60% of the total
exploitation cost. High moisture content, complex components and properties are the
difficulties faced during handling and managing the wastewater sludge [4].
1.0% of residual oil and 95% water content. Sludge also contains a high concentration of
Nitrogen [5]. As shown, the water content of the sludge is the main contributor to the cost
of sludge disposal. Palm Oil sludge is a highly polluting material as it has a high biological
oxygen demand, low pH and a colloidal nature. Developments have been made in order
as waste water treatment systems are common for the production of oleochemical [6].
Several drying techniques have been developed to reduce the water content of the
sludge. They can be reduced through convective drying, conductive drying and solar
drying [7]. The conventional drying method can be combined with a pre-treatment drying.
The method for drying pre-treatment considered are sun drying and ultrasonic buff
heating. Both of the methods mentioned will be combined with the conventional drying
Xue et al. [7] stated that shrinkage and cracking from the sludge is observed with
an increase of drying time with some small and shallow cracks appear and they become
deeper and wider. As for the effect of the sludge with voltage, it is observed from the
article that the residue content decreases when the voltage increases from 200V to 600V.
A higher rate of reduction can be obtained from a higher voltage whereas the rate of
reduction is lower from a lower voltage. In conclusion, a higher voltage leads to a higher
drying performance. Ultrasonic technique can transfer away the cyclic sonic wave emitter
with the assistance from water or air. Therefore, the ultrasound technique can be used as
a method for drying applications. There is a significant reduction of drying time compared
As for sun drying, the use of renewable energy can meet the process of drying for
countries [9]. In order to reduce the cost of the process, it is known that solar drying is a
viable solution. Whereas in order to increase the efficiency and decrease drying time for
solar drying, indirect solar dryers are used. Air is heated up by solar radiation and the air
consumes more electricity than solar drying which results to more greenhouse gas
emission. It is known that solar drying is a more sustainable alternative to sludge drying
as the heat transferred to the drying material is renewable. Recently it has been found that
greenhouse drying was converted from solar drying by controlling the drying area based
on findings from the agriculture industry. Greenhouse drying is the utilisation of solar
energy which is the recovery of additional energy from solar energy [10]. Without any
thermal energy, greenhouse drying allows the moisture content of the sludge can reach
approximately 30% as it also only uses solar energy. The cons of using solar or
greenhouse drying is these methods require a large drying area. For example, a 3.5 m 2 of
drying area is needed per tonne of sludge production per year. Furthermore, solar or
greenhouse drying takes a long time to obtain low moisture contents. Also, the duration
of drying depends on the region and season. Long period of drying encourages
accumulation of CH4 gas between 5 to 15% which can lead to a high risk of explosion
[11].
labelled as an efficient and sustainable method for sludge treatment. The advantages
include mass decrease, less energy use and energy recovery in the form of methane [12].
(CH4) and carbon dioxide (CO2) in the absence of oxygen with a sequence of
treatment methods has been researched such as hydrolysis, ozone oxidation, alkaline
hydrolysis and ultrasound [12]. Among all of the methods, ultrasonication is a well-
known technique for sludge degradation as it has essential merits efficient sludge
disintegration by 95% [12]. Whereas, the results of the degradation depend on the power
2.1 Materials
The sludge sample used for this experiment was obtained from the palm oil industry from
KLK Oleochemical plant in Pulau Indah (2.972829, 101.334271). The samples are stored
at the fridge approximately at 3°C. The sludge samples used were produced on 28th May
2018. Each sludge sample were formed by a shape moulder which is usually used for
baking purposes. For every sample, usually it requires two “moulds” as it is required for
2.1.2 Apparatus
The experiments were carried out by using a drying oven (Memmert Universal Oven,
UF55) with dimensions of 400 mm x 400 mm x 330 mm (length x height x breadth). The
solar drying, the equipment used is a fabricated solar dryer designed for heat conduction
2.2 Methodology
The sludge samples were tied-up in a plastic bag. Then, the plastic bag was placed in a
removable basket which the basket was placed in the ultrasonic heater which was filled
with distilled water. The heating temperature was set at 80°C and the timer for the heating
can be set. After the sludge was heated, the weight of the sludge samples was recorded
The 100 g sludge sample was prepared with a mould as mentioned previously. The weight
loss during drying was measured using an electronic scale (Smith, A3021-LT302) with a
range of 0 to 300 g with a system error of 0.001 g of system. The weight of the sludge
samples was recorded at a 15 mins interval for a drying period of 60 mins. After 60 mins,
the weight loss of the samples was recorded at a 60 mins interval. The weight loss was
measured until the weight reached the same weight for three (3) weight measurements.
At this point, the sludge sample has reached at equilibrium stage. After it has reached
equilibrium stage, the samples will be dried for 24 hours at 110°C to obtain the Bone-Dry
Weight. The Bone-Dry Weight was used to calculate the moisture content of the samples.
The oven was be operated at fan open at 100% and the flap setting at 0%. Whereas
the temperature of the dryer will be operated at 70 °C and 80 °C to obtain different sets
of data. Each of the two operating temperatures of the oven dryer was combined with the
ultrasonic heating which was conducted at 10 mins and 30 mins with each of the
combinations has its own set of data. The experiment was conducted three times to get
100 g sludge sample was dried in the solar dryer and the weight of the sample was
recorded every 15 mins for the first hour of drying. The weight of the sample was
measured again at the second hour of drying. Next, the samples proceed to thermal oven
drying at 80°C oven temperature. The weight of the samples was recorded at every
subsequent hour until no loss of weight is observed. This also means that the sample go
through two hours of solar drying and the rest goes through thermal oven drying until
equilibrium is reached.
Figure 1: Solar dryer pictures
Theoretical models have been used by many authors in their respective literatures to
determine the kinetic behaviour of thin-layer drying processes which in this for this
project. The Lewis model [14] is used to determine whether experimental and predicted
data have a good fit and they were evaluated based on statistical analysis. The value of
the root Coefficient of determination (R2) was found to determine whether both of the
data mentioned is a good fit. The higher the value of R2 the better the fit.
Theoretical models were used to determine the drying kinetics of oleochemical
sludge. The fitting performance were assessed by modifying the Fick’s Second Law to
get a satisfactory Coefficient of Determination (R2) value. The Moisture Ratio (MR) can
𝑀𝑡 −𝑀𝑒
𝑀𝑅 = (1)
𝑀𝑖 −𝑀𝑒
The moisture ratio (MR) is found through Error! Reference source not found.
and it is used as a dependant variable to find the moisture effective diffusivity (Deff). The
MR relates with the initial moisture content (Mi), equilibrium moisture content (Me) and
the moisture content in actual time (Mt). The moisture content used were on a dry basis.
solution of Fick’s second law [15] which is based on Equation 2. The moisture effective
diffusivity can represent the properties of the mass transfer of the moisture from the centre
of the sludge sample. Factors that can influence the moisture effective diffusivity is the
drying temperature, the moisture content, components of the sludge and any pre-treatment
applied.
𝜋 2 𝜋 2 𝜋 2
8 1 1
𝑀𝑅 = 𝜋2 [𝑒 −𝐷𝑒𝑓𝑓 𝑡(2𝑙) + 9 𝑒 −9𝐷𝑒𝑓𝑓 𝑡(2𝑙) + 25 𝑒 −25𝐷𝑒𝑓𝑓 𝑡(2𝑙) + ⋯ ] (2)
Based on Equation 2, only the first term is used for long drying times as the second
and third term are not significant. Therefore, Equation 2 can be simplified into Equation
3 below [8].
𝜋 2
8
𝑀𝑅 = 𝜋2 [𝑒 −𝐷𝐿 𝑡(2𝑙) ] (3)
8 𝜋
𝐿𝑛 𝑀𝑅 = 𝐿𝑛 𝜋2 − 𝐷𝑒𝑓𝑓 (2𝑙)2 𝑡 (4)
Equation 4 gives a linear equation which can be plotted in a straight line (Ln MR
vs t). The value of Deff can be evaluated from the slope of the ln MR vs t graph. Based on
𝜋
𝑆𝑙𝑜𝑝𝑒 = 𝐷𝑒𝑓𝑓 ( )2
2𝑙
8
𝑌 − 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 = 𝐿𝑛
𝜋2
The apparent activation energy (Ea) and the diffusivity constant (DO) can be found
𝐸
ln 𝐷𝑒𝑓𝑓 = ln 𝐷𝑂 − 𝑅𝑇𝑎 (5)
constant (m2/hr), Ea is the apparent activation energy (kJ/mol), T is the drying temperature
(K) and R is the gas constant (kJ/K.mol). The Ea value can be plotted from the slope of
Each set of data represents with a code name such as 70:80:10. Where the first number
represents the drying temperature in °C. The second number represents the temperature
of ultrasonic pre-treatment. The last number represents the duration of ultrasonic pre-
treatment in mins.
shows the experimental data for the drying curves of sludge at 70°C drying temperature
and 80°C drying temperature. During the experiments, the range for drying rates at
70°C is 1.37 – 0.108 g H2O/g DM (dry basis). Whereas at 80°C, the range of drying
rates is 1.082 – 0.057 g H2O/g DM (dry basis). It was shown that drying rate at 80°C
produces are a larger range of drying rate compared with 70°C. Furthermore, it was also
shown that at 80°C shows a greater steep in gradient at the second falling rate period
compared to 70°C. The increase in drying rate can increase the heat transfer rate and an
It was found that the drying of oleochemical sludge from this experiment
produces three distinctive drying rate periods which is the initial transient period, first
falling rate period and second falling rate period. The initial transient period occurs
when the drying rate increases because the sludge samples undergoes a heat exchange
with the surroundings in the oven dryer until it reaches the equilibrium temperature. It is
known that two falling rate periods are normal for drying of sludge. Where the
interstitial water is removed during the first falling rate period and the water being held
on the surface of the micro-particles is removed during the second falling rate period
[17]. The drying characteristics in Figure 2 also shows that it does not illustrate a typical
drying characteristic profile where the constant rate period does not exist. After the
initial transient period, it straight-away proceeds to the first falling rate period. The non-
existence of a constant rate period is due to the sample only consisting of little surface
moisture [16]. It was also reported that constant rate period does not exist in materials
that contains biological products [18]. It is known that oleochemicals sludge contains
biological components such as tricylglycerides, free fatty acids and phospholipids [19].
1.4 First falling rate Initial transient
Second
0.8
0.2
0
0 1 2 3 4 5 6
Moisture content (g H2O/g DM (dry basis))
ultrasonic-assisted heating only shows an increase in drying rates only when the
ultrasonic is at 80°C and for 30 mins. Where 70°C drying temperature without
ultrasonic. Whereas for drying temperatures at 80°C based on Figure 3b, it is shown that
observed that an increase in drying rate happens during the falling rate period. This is
mainly due to ultrasonic can induce the acoustic cavitation and produce inertial flux [8].
For drying temperature of 70°C and 80°C, the effect of ultrasonic bath pre-
treatment was observed. At 70°C without ultrasonic pre-treatment, the drying rate
ranges from 1.01 – 0.11 g H2O/m2.g DM.s at the falling rate period. For ultrasonic at
70°C for 10 mins, the drying rate ranges from 0.85 – 0.19 g H2O/m2.g DM.s As for
ultrasonic pre-treatment at 80°C for 10 mins, the drying rates ranges from 1.07 – 0.15 g
H2O/m2.g DM.s. As for ultrasonic at 70°C for 30 mins, the drying rate ranges from 1.01
– 0.11 g H2O/m2.g DM.s. Finally, for ultrasonic at 80°C for 30 mins, the drying rate
ranges from 1.08 – 0.12 g H2O/m2.g DM.s. The drying rates mentioned is during their
falling rate periods. For 80°C drying temperature without ultrasound pre-treatment, the
drying rate ranges from 1.16 – 0.057 g H2O/m2.g DM.s. For ultrasound at 70°C for 10
mins, the drying rate ranges from 1.16 – 0.055 g H2O/m2.g DM.s. For ultrasound at
80°C for 10 mins, the drying rate ranges from 1.19 – 0.068 g H2O/m2.g DM.s. For
ultrasound at 70°C for 30 mins, the drying rate ranges from 1.19 – 0.038 g H2O/m2.g
DM.s. For ultrasound at 80°C for 30 mins, the drying rate ranges from 1.32 – 0.080 g
ultrasonic pre-treatment was applied compared to thermal drying alone even though
various literatures proved that ultrasonic pre-treatment can reduce the duration of drying
of sludge from different industries. This could be due to the high contents of palm oil in
the sludge is concentrated. Another reason could be, the frequency ultrasonic waves
propagates is too high. It was reported by Martinez et al. [13] that ultrasonic
frequencies.
1.6
Second falling rate First falling rate Initial transient
1.4 period period period
a
Drying rate (g.H2O/m2.g.DM.s
1.2
1 70:00:00
0.8 70:70:10
0.6 70:70:30
70:80:10
0.4
70:80:30
0.2
0
0 1 2 3 4 5 6
Moisture content (g H2O/g of DM )
1.6
Second falling rate First falling rate Initial transient
Drying Rate (g H2O/m2.g DM.s)
1.4 period period period b
1.2
80:00:00
1
80:70:10
0.8
80:70:30
0.6
80:80:10
0.4 80:80:30
0.2
0
0 1 2 3 4 5
Moisture content (g H2O/g of DM)
As shown previously, the drying periods consist of two falling rate periods. The drying
kinetics can be observed separately at two falling rate periods to obtain a more accurate
drying kinetics of the sludge samples. Figure 4 shows the linear fitting at two falling
rate periods based on Error! Reference source not found. for 70°C ultrasonic for 30
mins at 70°C drying temperature. The values of effective moisture diffusivity are 1.26
10-4 and 3.59 10-4 m2/hr at the first falling rate period and second falling rate period
respectively. As for the values of effective moisture diffusivity for other conditions is
shown in Table 1. The Fick’s Second law equation can be modified in order to get a
satisfactory R2 value. It is shown in Table 1 that the R2 values are no less than 0.9 so the
Based on Table 1, the value of Deff increases from the first falling rate period to
the second falling rate period. The effect of ultrasonic pre-treatment on the Deff shows
no drastic change which can be expected after observations on the effect of ultrasonic
reported from Sun et al. [8] that the values for moisture effective diffusivity of
municipal sewage sludge is from 6.05 10-6 to 5.75 10-5 m2/hr. The moisture
effective diffusivity values stated is much smaller than the values from this study. This
is probably due to the study from Sun at al. [8] was conducted at higher temperatures
and the source of sludge comes from a different industry. The contents of municipal
sewage sludge and oleochemical sludge is different. Hence, the drying kinetics could be
different.
Table 1: Effective moisture diffusivities of Oleochemical sludge
Deff (m2/hr) Deff (m2/hr) R2 R2
First falling rate Second falling rate First falling rate Second falling rate
The linear fitting for ln Deff vs 1/T can be plotted by using Error! Reference
source not found. for oleochemical sludge. Figure 5 shows the ln Deff vs 1/T plot for
70°C drying temperature with ultrasonic pre-treatment at 70°C for 30 mins. The first
falling rate period and the second falling rate period. The values of apparent activation
energy are 9.367 and 13.303 kJ/mol for the first falling rate period and second falling
rate period respectively. Whereas for the diffusivity constant (Do) the values are 3.35
10-3 and 3.83 10-2 m2/hr for the first falling rate period and the second falling rate
period respectively. The rest of the values of Ea and Do at both falling rate periods is
shown in Table 2.
The apparent activation energy can indicate the minimum energy required for to
remove the inner moisture of the oleochemical sludge in both falling rate periods. In
simpler words, the smaller activation energy, the lesser the difficulty of the drying
process. As for the effect of ultrasonic pre-treatment on the Ea, some conditions produce
a higher value than thermal drying and some gives a lesser value than thermal drying
alone.
-8.88 -7.78
a 0.00282 0.00284 0.00286 0.00288 0.0029 0.00292 b 0.00282 0.00284 0.00286 0.00288 0.0029 0.00292
-7.8
-8.9
-7.82
-8.92
-7.84
ln Deff
ln Deff
-8.94 -7.86
y = -1126.7x - 5.7
-7.88
-8.96
-7.9
-8.98 y = -1600.1x - 3.2616
-7.92
-9 -7.94
1/T (K-1) 1/T (K-1)
Figure 2: ln Deff vs 1/T plot for ultrasonic at 70°C for 30 mins: a) First falling rate
period b) Second falling rate period
Table 2 also shows that the value of Ea increases form the first falling rate period
to the second falling rate period. Similar results were found for municipal sewage
sludge reported from Sun at al. [8] for municipal sewage sludge. The increase of
apparent activation energy is probably due to the moisture in the sample is strongly
bounded with the particles at the centre of the sludge during the second falling rate
period.
Table 2: Values of apparent activation energy and diffusivity constant of oleochemical
sludge
Data set Ea (kJ/mol) DO (m 2/hr)
First falling
1.4 Second Initial transient period
Drying rate (g H2O/m2.g DM.s)
rate period
1.2 falling rate
1 period
0.8
70°C drying temp
0.6
80°C drying temp
0.4 solar drying
0.2
0
0 1 2 3 4 5 6
Moisture content (g H2O/g DM (dry basis))
As mentioned in previously, solar drying was conducted for the first two hours of
drying. The rest was conducted by using thermal oven drying at 80°C until it reaches
equilibrium. Figure 6 shows the drying characteristics of solar drying with traditional
method of drying. The drying periods consist the same rate periods as previous which
are the initial transient period and two falling rate periods. The initial transient period
only occurs at during solar drying with a range of drying rate of 0.050 to 0.24 g H 2O/g
DM (dry basis). The two falling rate periods happen during thermal drying with the
drying rate at first falling rate period ranges 1.30 to 0.31 g H 2O/g DM (dry basis).
Whereas the range of drying rate at the second falling rate period ranges at 0.31 to 0.064
was done for solar drying. Since the drying characteristics consist of two falling rate
periods, the linear fitting was analysed separately. Figure 7 shows the linear fitting at
two falling rate periods based on Error! Reference source not found. for solar drying.
The values for moisture effective diffusivity are 2.69 10-4 and 4.30 10-4 m2/hr for
the first falling rate period and second falling rate period respectively.
0
0 1 2 3 4 5 6 7 8 9
-0.5
-1
-1.5
-2
b
-2.5 y =) -0.9753x + 3.7449
R² = 1
-3
a y = -0.6091x + 1.2969
-3.5 R² = 0.9909
-4
-4.5
Figure 4: Linear fitting between ln MR vs t for solar drying: a) First falling rate period
b) Second falling rate period
First falling rate Second falling rate First falling rate Second falling rate
From Table 3 it is shown that the Deff values for solar drying is much higher for
both falling rate periods than traditional drying alone and drying combined with
It was found that the final moisture content of solar drying was approximately similar
with 80°C thermal drying which are 0.28 and 0.22 g H 2O/g DM (dry basis) for solar
dying and 80°C thermal drying respectively. But the final moisture content for 70°C
oven drying (0.60 g H2O/g DM (dry basis)) and solar drying is not similar since the
oven temperature after solar drying is 80°C. The final moisture of the drying methods
mentioned was reached after the sample went through drying for nine hours. For solar
drying, the nine hours of drying is inclusive of two hours of solar drying and seven
hours of thermal drying. The reason the sludge only goes through seven hours of
thermal drying after two hours of solar drying is due to the sludge has gone through the
initial transient period during solar drying. Basically, the sludge gone through the
“warm up” stage during solar drying which entirely skips the heating up process when it
was proceeded to thermal drying. This can be concluded that by doing two hours of
solar drying, two hours of electricity can be saved compared to thermal drying alone. At
the same time, an approximately similar final moisture content (for 80°C thermal
drying) can be achieved with the same amount of drying period. If an oleochemical
plant produces 1 tonne of sludge per day, the electricity cost can be saved by 22% daily
The drying time did not decrease when ultrasonic pre-treatment bath is added compared
with thermal drying alone. The drying characteristics of oleochemical sludge consist of
an initial transient period and two falling rate periods. The moisture effective diffusivity
at the first falling rate period ranges from 1.07 10-4 – 1.66 10-4 m2/hr. Whereas for
the second falling rate period, the moisture effective diffusivity ranges from 2.78 10-4
– 4.22 10-4 m2/hr. Theoretical model was used to determine the kinetic behavior of the
oleochemical sludge. The moisture effective diffusivity increases form the first falling
rate period to the second falling rate period. The moisture effective diffusivity also
increases when the drying temperature increases from 70°C to 80°C. As for the effect of
ultrasonic bath pre-treatment on the moisture effective diffusivity, there are no obvious
changes on the difference on the moisture effective diffusivity. As for solar drying, the
sludge managed to achieve a final moisture content of 0.28 g H2O/g DM (dry basis) for
a total drying time of nine hours (two hours of solar drying and seven hours of thermal
drying at 80°C). Comparing with the final moisture content of thermal drying alone at
80°C which is at 0.22 g H2O/g DM (dry basis) which is achieved after nine hours of
drying. This can be concluded that electricity can be saved by two hours when solar
drying combined with thermal drying is used to achieve the same moisture content
As for future recommendations to improve this study, the solar dryer can be
modified by adding a solar panel for using total green energy. Also, for solar drying can
attempt combining four hours of solar drying with thermal drying and observe how
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