Science Journal of Energy Engineering

2017; 5(4): 87-94

http://www.sciencepublishinggroup.com/j/sjee
doi: 10.11648/j.sjee.20170504.12
ISSN: 2376-810X (Print); ISSN: 2376-8126 (Online)

Separation of Free Glycerol and Glycerides from Biodiesel

by Means of Liquid-Liquid Extraction
Ana Petracic1, Aleksandra Sander1, *, Lana Magic2
1
Department of Mechanical and Thermal Process Engineering, Faculty of Chemical Engineering and Technology, University of Zagreb,
Zagreb, Croatia
2
INA-Industrija Nafte, d.d., Zagreb, Croatia

Email address:
apetracic@fkit.hr (A. Petracic), asander@fkit.hr (A. Sander), lana.magic@ina.hr (L. Magic)
*
Corresponding author

To cite this article:

Ana Petracic, Aleksandra Sander, Lana Magic. Separation of Free Glycerol and Glycerides from Biodiesel by Means of Liquid-Liquid
Extraction. Science Journal of Energy Engineering. Vol. 5, No. 4, 2017, pp. 87-94. doi: 10.11648/j.sjee.20170504.12

Received: July 2, 2017; Accepted: August 2, 2017; Published: October 31, 2017

Abstract: This paper investigates glycerol and glycerides extraction process from fresh and waste sunflower oil biodiesel.
Deep eutectic solvent choline-chloride: ethylene-glycol (molar ratio 1:2.5) was used as extraction media in both batch
experiments and continuous Karr column. Biodiesel was synthesized in an alkali catalysed chemical transesterification
reaction. Three process variables, namely hydrodynamic conditions, solvent to biodiesel ratio and extraction duration were
investigated and their impact on the extraction efficiency was found to be largely negligible. Throughout the whole range of
process variables the extraction efficiency was relatively high, getting slightly lower only during the continuous experiments.
After the extraction, free glycerol content was below the limit for all samples, but the total glycerol and glycerides content was
too high to fully comply with biodiesel quality standards. Selected extraction solvent has proved to be efficient for free
glycerol removal in the tested range of conditions, but further process modifications and possible raw material and biodiesel
processing will be needed to reduce the content of total glycerol and glycerides.
Keywords: Biodiesel, Deep Eutectic Solvents, Glycerol, Liquid-Liquid Extraction

triglycerides with homogeneous or heterogeneous catalysts,

1. Introduction wherein the homogeneous catalysts may be alkaline or acidic,
In the past few decades, energy demand in all economic and heterogeneous catalysts may be solid catalysts or enzymes
sectors has been growing steadily. Increase in fuel [5]. The fastest and most commonly used method for biodiesel
consumption, most notably in the transport sector, has resulted synthesis is the alkali-catalyzed transesterification of vegetable
in increased emissions of combustion products that are harmful oils, but its downside is its high dependence on the oil quality,
to human health and play a significant role in global climate namely the concentration of free fatty acids and water in the
changes [1]. Over the past decade, great efforts have been feedstock [6]. The reaction product is a mixture formation of
devoted to development of alternative fuels that could replace alkyl (usually methyl or ethyl) esters of fatty acids, i.e.
the existing fossil ones [2]. The greatest potential has been biodiesel and glycerol as by-product [7].
observed in biodiesel because previous studies showed that the The increase in global demands for biodiesel production
combustion of biodiesel reduced emissions, so biodiesel is results in increasing interest for the use of waste materials of
now the most widely used renewable energy source [3]. In plant and animal origin or non-edible oils. The main
addition, biodiesel production will greatly relieve the transport problems associated with the use of waste materials are high
sector i.e. its dependence on fossil fuels and it will encourage proportion of free fatty acids that must be reduced to below
economic development, due to the availability, renewability 1% and frequent presence of water [1].
and easy-to-use raw materials [4]. Sunflower oil is the most commonly used cooking oil in
Biodiesel is synthesized by transesterification of central Croatia, both in households and in student restaurants
in Zagreb. Due to its high smoke point it can be used for
 Science Journal of Energy Engineering 2017; 5(4): 87-94 88

baking, frying and cooking. Its acid value is normally very glycerol in different molar ratios [26]. Both papers report free
low even when used multiple times. Biodiesel is glycerol removal and substantial total glycerol reduction for
commercially produced mostly from the oils of rapeseed [8], almost all experiments conducted.
soybean [9] and palm [10]. This paper is based on used In this article, the applicability of deep eutectic solvent,
sunflower oil because of its availability and potential choline-chloride: ethylene-glycol (molar ratio 1: 2.5) for
environmental benefits of turning waste into fuel. Several extraction of glycerol from biodiesel was tested
papers have been published regarding sunflower oil experimentally in batch and continuous extractor. That
biodiesel; Naureen at al. focused on synthesis and particular DES was chosen because, unlike a lot of other
characterization [11], Saba et al. and Vahid et al. investigated DESs, its viscosity is relatively low what results in lower
different catalysts and influence of catalyst to fuel ratio on flow resistance effectively aiding the mixing process and
biodiesel conversion [12-14], Reyero at al. researched reducing the power needed to pump the solvent during
kinetics of NaOH catalyzed transesterification with ethanol continuous setup. It is fairly cheap, even when p.a. quality.
[15] and Santala et al. did experimental and simulation Having in mind a future scale-up to an industrial scale, it is
studies of transesterification in microchannel reactor [16]. important that all resistances in the system and the price of
Encinar et al. researched the variables affecting the yields components are minimised. Also, it is crucial that the solvent
and characteristics of the biodiesel [17] and Vicente at al. is stable in the entire expected temperature range (expected
compared the most common basic catalysts for methanolysis temperature in an open industrial environment, ranging from
of sunflower oil [18]. 0 to 60°C). During preliminary experiments for this work,
Various impurities contained in synthesized biodiesel DES choline-chloride: ethylene-glycol (molar ratio 1:2) was
adversely affect its characteristics, its storage properties as noticed to begin to crystallize at around 15°C so it was not
well as engine performance and lifetime. Aside from used in extraction experiments. Lastly, Shahbaz et al.
glycerol, biodiesel often contains methanol, water, soap, reported that among the choline-chloride: ethylene-glycol
catalyst, free fatty acids and unreacted tri-, di- and DESs they used for glycerol extraction, the solvent with
monoglycerides [19]. Liquid-liquid extraction is one of the molar ratio 1:2.5 appeared to be the most efficient one [20],
alternative methods for purification of the biodiesel so in this paper its utilisation was tested in both batch and
produced. Its advantages lie in mild conditions of the process continuous setup in an effort to determine the optimal
performed at room temperature and atmospheric pressure. process conditions for a possible future industrial use.
Some studies on vegetable oils have shown that the use of
deep eutectic solvents (DESs) reduces the content of all 2. Materials and Methods
impurities present in crude biodiesel [20-22]. Deep eutectic
solvents are mixtures of two or three economically and 2.1. Preparation of Deep Eutectic Solvent
environmentally acceptable components with a melting
temperature lower than the melting temperature of individual Choline chloride and ethylene glycol were dried in the
components [23]. Their use was investigated in various vacuum dryer at 60°C for 8 hours before use. Cholinium salt
processes because of their outstanding properties, the most and hydrogen bond donor (molar ratio 1:2.5) were directly
important of which being simplicity of synthesis from weighed in a flask and the mixture was placed on a rotary
environmentally friendly raw materials, non-volatility, vacuum evaporator (250 mbar and 60°C) until clear liquid is
thermal and chemical stability, non-toxicity, biodegradability obtained.
and non-flammability and potential for dissolving different 2.2. Biodiesel Synthesis
types of organic, inorganic and polymeric compounds [24].
Thanks to its properties, eutectic solvents are used in Biodiesel was synthesized by alkali-catalyzed (NaOH)
synthesis processes, as catalysts and biocatalysts, in transesterification of fresh and waste cooking sunflower oil
electrochemical synthesis, in analytical chemistry procedures of satisfactory quality with methanol. 0.6 g of NaOH was
as solvents or auxiliary solvents and in separation processes. dissolved in 20 mL of methanol. Sodium methoxide was
Due to their negligible environmental impact as well as added to the filtrated oil heated at 55°C and intensively
simple and inexpensive synthesis, DESs are interesting both mixed. Heterogeneous mixture was left for 24 hours to
on laboratory and industrial scale [25]. ensure complete phase separation. Three different types of
Using deep eutectic solvents for glycerol removal is a waste sunflower oil were used for the synthesis of biodiesel
fairly new method and only several papers have been (french fries, potato with paprika and doughnut).
published investigating different DESs, biodiesel to DES
ratios and temperatures during extraction. Among the DESs 2.3. Extraction of Free Glycerol
used, choline chloride seems to be the most common salt and Liquid-liquid extraction experiments were carried out in a
ethylene glycol and glycerol are the most common hydrogen laboratory batch extractor (internal diameter of 0.04 m)
bond donors. Shahbaz et al. used choline chloride with equipped with a magnetic stirrer and Karr column (column
ethylene glycol and with 2,2,2-trifluracetamide in different height: 0.43 m; column diameter: 0.05 m; perforated plate
molar ratios [20] while Ho et al. used ternary deep eutectic diameter: plate free flow area: 22%; 0.043 m; number of
solvents – choline chloride with both ethylene glycol and plates: 11; distance between plates: 0.04 m). Karr column
89 Ana Petracic et al.: Separation of Free Glycerol and Glycerides from Biodiesel by Means of
Liquid-Liquid Extraction

was equipped with two phase separators and two peristaltic wgF − wgR
pumps. For the batch extraction, the influence of extraction ε= ⋅100% (1)
wgF
duration (15 – 60 min), hydrodynamic conditions (150, 300,
500, 700 rpm) and the mass ratio (solvent: crude biodiesel)
Standard uncertainties were calculated by the following
(0.25, 0.50, 0.75, 1.00 kg kg-1) on the extraction efficiency
equation:
and the quality of the purified biodiesel was investigated.
Continuous extraction was performed at different pulsation 1/ 2
 n 
∑( )
rate (27, 34, 54, 63 pulsation per minute) and extraction 1 2
u ( wi ) =  ⋅ wi , k − wi  (2)
duration (5 – 20 min).  n ⋅ ( n − 1) 
 k =1 
2.4. Characterization of Deep Eutectic Solvent, Oil and
3.1. Batch Extraction
Biodiesel
3.1.1. The Influence of the Quality of Raw Material on the
Analytical methods used for biodiesel characterization are:
Extraction Efficiency
FTIR (Bruker Vertex 70), GC Shimadzu GC-2014) and 1H
In order to investigate the influence of the type of raw
NMR (Bruker Avance 300). Viscosity was measured on a
material used for biodiesel (fresh and waste sunflower oil) on
Brookfield DV-III Ultra Programmable Rheometer. Density
the extraction of free and total glycerol from biodiesel, one
was measured with a Mettler Toledo densitometer Densito
set of batch experiments (mass ratio DES: biodiesel: 0.25 kg
30PX. Biodiesel heating value (LHV) was measured with
kg-1 at 500 rpm for 30 minutes) was conducted.
calorimeter IKA C 2000. Acid number of waste cooking oil
Concentrations of free and total glycerol in crude biodiesels
was determined according to the standard method HRN EN
as well as in purified biodiesels were measured three times.
ISO 660:2010 and iodide number according to the standard
Standard uncertainties were lower than 0.006. Based on the
method HRN EN ISO 3961:2013.
obtained results (Figure 1) it can be concluded that the
extraction efficiency is influenced by the concentration of
3. Results and Discussion free and total glycerol. Higher concentrations of free and
total glycerol resulted with higher efficiency. Since the
This study covers preparation of choline-chloride: ethylene-
extraction time was the same for all experiments, higher
glycol (molar ratio 1:2.5), synthesis of biodiesel from fresh and
concentration means larger driving force for mass transfer
waste cooking sunflower oil and its purification as well as
and consequently lower final concentration of free and total
characterization of the obtained products. Synthesized
glycerol in biodiesel. After extraction, all biodiesel samples
biodiesels were purified by means of liquid–liquid extraction
had the final concentration of free and total glycerol higher
with choline-chloride: ethylene-glycol (molar ratio 1: 2.5) in
than the maximum allowed, probably due to the low DES:
different process conditions. For the best of our knowledge the
biodiesel mass ratio. Biodiesel synthesised from fresh
influence of the process conditions (hydrodynamic conditions,
sunflower oil had the lowest concentration of free and total
mass ratio solvent/biodiesel and time of extraction) wasn’t
glycerol before extraction, and the highest concentrations
investigated previously.
after extraction. All other experiments were carried out with
The applicability of the selected DES for the extraction of
biodiesel with the highest concentration of glycerol.
glycerol from biodiesel is evaluated in terms of extraction
efficiency, which is calculated from the mass fraction of
glycerol before and after extraction, obtained by GC analysis:

Figure 1. Influence of the type of biodiesel on the extraction efficiency (DES: biodiesel mass ratio = 0.25; t = 30 min; n = 500 rpm).
 Science Journal of Energy Engineering 2017; 5(4): 87-94 90

3.1.2. The Influence of the Process Conditions on the maximum quantity of mono-, di- and triglycerides was
Extraction Efficiency transferred from biodiesel to DES. Higher amount of the
Table 1 shows influence of the hydrodynamic conditions, extracted di- and triglycerides can be attributed to the higher
mass ratio DES: biodiesel and extraction duration for batch DES: biodiesel mass ratio (5: 1) than used for batch
extraction on the extraction efficiency. The initial experiments (up to 1: 1). It is obvious that the solubility is
concentration of free and total glycerol in biodiesel was increased from triglycerides to monoglycerides. It is also
1.939 and 2.836% respectively. Increase of the mixing possible that the rate of mass transfer from biodiesel to DES
intensity, mass ratio DES: biodiesel and extraction duration is the highest for monoglycerides which are smaller
do not significantly influence the extraction efficiency. High molecules of simpler structure than di- or triglycerides. In
extraction efficiencies for free glycerol were obtained at all batch extraction experiments, the capacity of solvent for di-
process conditions investigated for the batch extraction. and triglycerides is reduced due to the increased
Since the concentration of total glycerol was also decreased concentration of monoglycerides in DES.
for more than 64%, selected solvent was efficient for
extraction of mono-, di- and triglycerides.

Table 1. The influence of the process conditions on the extraction efficiency.

Extraction efficiency/%
Process conditions Free glycerol Total glycerol
Batch extraction
150 98.40 70.53
Hydrodynamic 300 98.45 67.86
conditions/ rpm 500 97.32 64.95
700 98.40 70.76
0.25 97.32 64.95
Mass ratio DES: 0.50 99.07 70.46
biodiesel/ kg kg-1 0.75 96.36 67.05
1.00 98.40 71.86
15 96.91 68.25
Extraction 30 97.32 64.95
duration/min 45 97.83 65.47
60 97.11 66.81
Figure 3. The influence of the extraction time on the extraction efficiency
(DES: biodiesel mass ratio = 5:1; pulsation rate = 54 pul min-1).

3.2. Continuous Column Extraction

In order to investigate the influence of oil type on the

composition and properties of biodiesel, biodiesel was
synthesised from fresh sunflower oil and purified by the
same solvent in the column extractor. The influence of the
extraction duration on the extraction efficiency is shown in
table 2. Higher extraction efficiency for glycerides was
obtained for continuous extraction experiments. Low value
after 5 minutes means that stable state wasn’t achieved.
Higher extraction efficiency is achieved since higher DES:
biodiesel mass ratio (5: 1) was used.

Table 2. The influence of extraction duration on the extraction efficiency.

Extraction efficiency/%
Figure 2. The influence of the DES: biodesel mass ratio on the extraction Process conditions Free glycerol Total glycerol
efficiency (t = 30 min; n = 500 rpm). Continuous extraction
5 17.86 17.25
The ability of the selected solvent to extract mono-, di- and Extraction 10 96.39 80.52
triglycerides is clearly visible in Figures 2 and 3. For the duration/min 15 96.29 81.52
DES: biodiesel mass ratios lower than 0.5 kg kg-1, glycerides 20 97.78 82.26
were not transferred from biodiesel to DES. As the quantity
The extraction performance of the continuous
of DES was increased, higher extraction efficiencies could be
countercurrent column extraction was also studied at
observed, for mono- and diglycerides. Based on the presented
different mixing intensities. Time needed for stabilization
results, triglycerides were not transferred to the DES. When
was 20 minutes. The FTIR spectra for purified biodiesels
stationary state was achieved in the continuous process, the
obtained at different pulsation rates are presented in Figure 4.
91 Ana Petracic et al.: Separation of Free Glycerol and Glycerides from Biodiesel by Means of
Liquid-Liquid Extraction

In the region from 1800 – 1700 cm-1, peak that can be strong band between 3200 and 3600 cm-1 that corresponds to
attributed to the stretching of C=O, typical of esters, and thus alcohols is decreased with increasing pulsation rate. This is
common in FAME spectra, can be observed. The influence of clearly visible from the influence of the pulsation rate on the
the pulsation rate on the removal of glycerol from biodiesel area below this peak.
can also be observed in Figure 4. The intensity of broad

Figure 4. FTIR spectra of waste cooking oil biodiesel at different pulsation rates (DES: biodiesel mass ratio = 5:1).

Table 3 shows the most important physical properties of

purified biodiesel produced from fresh and waste cooking Table 4. Fatty acid methyl ester concentration in biodiesel (WO – waste oil;
FO – fresh oil).
sunflower oil (DES: biodiesel mass ratio = 5: 1; 20 minutes;
54 pul/min) as well as density and viscosity of DES. FAME structure
w/%
Experimentally determined acid number of both oils is low WO FO
Caproic acid methyl ester C6:0 0.0147 0.0156
enough to ensure high efficiency of the transesterification
Caprylic acid methyl ester C8:0 0.0274 0.0078
process. Viscosity and density of biodiesels meets the EN Capric acid methyl ester C10:0 0.0242 0.0357
14214 specification standard. Heating values are lower than Undecylic acid methyl ester C11:0 0.0074 0.0335
the heating value of fossil diesel (42.6 kJ g-1) as stated in the Lauric acid methyl ester C12:0 0.0158 0.0123
literature [27]. Tridecylic acid methyl ester C13:0 0.0021 -
Mystric acid methyl ester C14:0 0.0905 0.0769
Table 3. Properties of deep eutectic solvent, fresh (FSO) and waste Tetradeceonic acid methyl ester C14:1 0.0084 0.0112
sunflower oil (WSO) and biodiesel (from fresh oil: FSB; from waste oil: Pentadecylic acid methyl ester C15:0 0.0399 0.0379
WSB). Palmitic acid methyl ester C16:0 6.3641 5.9454
Palmitoleic acid methyl ester C16:1 0.1284 0.1238
ρ/k cm-3 η/Pa s mg(KOH)/g(oil) LHV/J g-1 Margaric acid methy ester C17:0 0.0589 0.0602
DES 1.122 0.0355 - - Stearic acid methyl ester C18:0 2.8827 2.8367
FSO 0.919 0.0584 0.560 - Oleic acid methyl ester C18:1 27.6185 26.4902
FSB 0.880 0.0388 - - Linoleic acid methyl ester C18:2 55.3307 55.6710
WSO 0.920 0.0509 0.688 39880.0 Linolenic acid methyl ester C18:3 0.2914 0.1918
WSB 0.887 0.0043 - 39876.5 Arachidic acid methyl ester C20:0 0.2619 0.2509
Paulinic acid methyl ester C20:1 0.1852 0.1717
The chemical structure of biodiesel in terms of carbon Eicosapentaenoic acid methyl ester C20:5 0.0174 0.0268
chains, saturated and unsaturated fatty acid methyl esters and Behenic acid methyl ester C22:0 0.6197 0.6021
Erucic acid methyl ester C22:1 0.0263 0.0223
mass percentage are given in Table 4, as determined by GC
Lignoceric acid methyl ester C24:0 0.2146 0.2052
analysis. According to Table 4, both biodiesels are composed Nervonic acid methyl ester C24:1 0.0253 0.0234
mainly from unsaturated fatty acid methyl esters and their Saturated 10.6239 10.1202
composition is similar. Monousaturated 27.9921 26.8426
Polyunsaturated 55.6395 55.8896
 Science Journal of Energy Engineering 2017; 5(4): 87-94 92

1
H NMR spectrums of biodiesel before and after extraction conversion of vegetable oil in methyl esters by
are presented in Figure 5. The characteristic intense peak of transesterification reaction [28]. The relevant signals chosen
methoxy protons is observed at 3.624 ppm and α-CH2 for integration were those of the methoxy group in the methyl
protons signal at 2.279 ppm. These two peaks are the distinct esters at 3.624 ppm (AMe) and of the α-carbonyl methylene
peaks for confirmation of methyl esters present in the protons at 2.279 ppm (ACH2). The equation used to quantify
biodiesel. Other peaks were at 0.876–0.927 ppm of terminal the yield of transesterification was:
methyl protons, a strong signal at 1.182–1.461 ppm related to
2 ⋅ AMe
methylene protons and 5.206–5.433 ppm assigned to olefinic % FAME = 100 ⋅ (3)
hydrogens. 1H NMR can also be used to quantify the 3 ⋅ ACH2

Figure 5. 1H NMR spectra of biodiesel (WOB) before and after extraction.

Percentage conversion of triglycerides to the the standard specifications for biodiesel fuel in terms of free
corresponding methyl esters after extraction is slightly higher glycerine content. However, the ester content was slightly
than the one before extraction, probably due to the higher lower than the EN 14214 limit due to the higher
purity of biodiesel. Peaks characteristic for alcohols, from 3.4 concentrations of mono-, di- and triglycerides. Iodide number
to 4.0 ppm are significantly lower after extraction which is higher than the standard value (120 g (I2)/g (oil)) due to the
means that both methanol and glycerol were extracted from higher concentration of unsaturated FAME. Biodiesel of
biodiesel. slightly higher quality was produced from waste sunflower
Table 5 shows the biodiesel specifications according to the oil since the concentration of mono-, di- and triglycerides
EN 14214 standard. After purification, the biodiesel fulfilled was reduced, probably during frying.
93 Ana Petracic et al.: Separation of Free Glycerol and Glycerides from Biodiesel by Means of
Liquid-Liquid Extraction

Table 5. Specification of biodiesel after continuous extraction.

property unity FOB WOB standard method

Ester content % (m/m) 94.6 96.1 > 96.5 HRN EN ISO 23015:1997
Sulfated ash content % (m/m) 0.011 0.012 < 0.02 HRN EN ISO 3987:2011
Sulfur content mg/kg <3 <3 < 10 HRN EN ISO 20846:2011
Methanol content % (m/m) < 0.1 < 0.1 < 0.2 HRN DIN EN 14110:2003
Iodide number g I2/100 g 126.2 125 < 120 HRN EN 16300:2012
Linolenic acid methyl ester % (m/m) 0.2 0.3 < 12 HRN EN 14103:2011
Monoglyceride content % (m/m) 0.67 0.56 < 0.7 HRN EN 14105:2011
Diglyceride content % (m/m) 1.27 0.91 < 0.2 HRN EN 14105:2011
Triglyceride content % (m/m) 3.11 2.36 < 0.2 HRN EN 14105:2011
Free glycerine % (m/m) < 0.005 < 0.005 < 0.02 HRN EN 14105:2011
Total glycerine % (m/m) 0.677 0.521 < 0.25 HRN EN 14105:2011

FTIR – Fourier transformation infrared spectroscopy

4. Conclusions GC – gas chromatography
LHV – lower heating value/J g-1
In this study, deep eutectic solvent choline-chloride: WO – waste oil
ethylene-glycol (molar ratio 1:2.5) was employed as solvent WOB – waste oil biodiesel
for the removal of glycerol from biodiesel produced from
waste cooking sunflower oil. For this purpose, the
effectiveness of using the selected DES on the removal of References
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