J.

of Supercritical Fluids 38 (2006) 326331

Extraction of sunflower oil with supercritical CO2:

Experiments and modeling
Ugur Salgn a, , Onur Doker b , Ayla C
alml b
aCumhuriyet University, Faculty of Engineering, Department of Chemical Engineering, 58140 Sivas, Turkey
b Ankara University, Faculty of Engineering, Department of Chemical Engineering, 06100 Tandogan, Ankara, Turkey
Received 31 January 2005; received in revised form 1 July 2005; accepted 1 November 2005

Abstract
Extraction of sunflower oil from sunflower seeds (Heliantus annuus L.) using supercritical CO2 was studied. The shrinking core model was
applied to the modeling of the packed-bed extraction process. The experimental data were obtained for extraction conducted at the pressures of
20, 30, 40, 50 and 60 MPa; the temperatures of 313, 333 and 353 K, the CO2 flow rates of 14, and 6 cm3 CO2 min1 ; the mean particle diameters
of 0.23, 0.55, 1.09, 2.18 mm. The supercritical CO2 extraction process was modeled by a quasi steady state model as a function of extraction
time, pressure, temperature, CO2 flow rate, and particle diameter. The supercritical CO2 extraction process. The intraparticle diffusion coefficient
(effective diffusivity) De was used as adjustable parameter. The model using the best fit of De was correlated the data satisfactorily.
2005 Elsevier B.V. All rights reserved.

Keywords: Supercritical fluid extraction; Sunflower oil; Shrinking core model

1. Introduction of -tocopherol) than many other edible oils, and therefore, is

In the last years, the world production of sunflower seeds
(Heliantus annuus L.) has had a significant increase compared
to other seed oil cultivation. Sunflower seeds are very rich in oil
(about 50 wt.%) and from a chemical point of view the oil is con-
sidered very good for human consumption, because of its high
ratio polyunsaturated/saturated fatty acids and the high content
in linoleic acid. In addition, sunflower seeds represent an impor-
tant source of vegetable oil and its protein fraction characterized
by relatively well-balanced amino acid pattern, is recognized as
a potential source of proteins for human consumption [14].
The production of organic seed oil is based on technical
processes that respect the principles of the organic agriculture;
therefore, it is not possible to use toxic and pollutant organic
solvents, such as hexane [5]. However, extraction by just press-
ing the seeds has often a limited economical value because of
the high amount of oil that remains in the pressed cake, even
if the final content in the natural antioxidants of the oil is not
significantly affected by the pressing process. This is impor-
tant for sunflower oil that is richer in vitamin E (about 650 ppm
Corresponding author. Tel.: +90 346 2191010; fax: +90 346 2191179.
E-mail address: usalgin@cumhuriyet.edu.tr (U. Salgn).
very important to preserve this antioxidant fraction. Human diet
requires however the preliminary de-hulling of achenes and the
removing of polyphenolic compounds, particularly chlorogenic
acid. Polyphenolic compounds are present in high quantity and
negatively affect the color and nutritional value of protein prod-
ucts [6].
A possible alternative method could be represented by the
use of the supercritical fluid technology based on the utilization
of CO2 at supercritical conditions, a substance that has the status
of generally recognized as safe (GRAS).
Supercritical fluid extraction has been applied to the extrac-
tion of vegetable oils from several seeds as recently reviewed
by Eggers [7]. Supercritical fluid technology has attracted the
attention of both scientists and engineers. Recently, consider-
able progress has been made in the use of supercritical fluids and
mixtures. Examples of the applications and related advantages
are the use of supercritical fluids (CO2 and water, in particu-
lar) as environmentally readily available solvents, the ability to
adjusted selectively separations, the enhancement of separation
rates due to the low viscosity and high diffusivity, the ability to
solvate.
In this work, supercritical extraction of sunflower oil from
sunflower seeds by supercritical CO2 in a semi continuous sys-
tem was studied. The extraction rate and yield of sunflower

0896-8446/$ see front matter 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.supflu.2005.11.015
 U. Salgn et al. / J. of Supercritical Fluids 38 (2006) 326331
oil was investigated as a function of pressure, temperature,
CO2 flow rate and particle size. In addition, the supercriti-
cal CO2 extraction process for various experimental condi-
tions was modeled using shrinking core model. More detail
information about the model was given in our previous study
[8].
2. Materials and methods
2.1. Plant materials
The sunflower seeds used were supplied by the region of
Thrace (Turkey). Seeds were pre-treated using the following
procedure prior to loading into the extractor. The seed hulls and
other unwanted substances were separated and then were packed
in polyethylene bags and stored at ambient temperature. The
clean de-hull seeds were rotary milled and the fractions were
separated, such as 0.212 mm < dp < 0.25 mm, 0.5 mm < dp < 0.6
mm, 1 mm < dp < 1.14 mm and 2 mm < dp < 2.36 mm. Particle
diameter of fraction is given arithmetical average, such as
0.23, 0.55, 1.09 and 2.18 mm. After then, the fractions were
stored in a glass bottle in a vacuum desicator until used
for extraction experiments. Moisture content in oilseeds was
determined according to the AOCS methods [14] Ca-2c-
25, and moisture content in sunflower seeds was 2.4 wt.%,
after then packed in polyethylene bags and stored at ambient
temperature.
2.2. Supercritical uid extraction
Sunflower oil was extracted from seeds of H. annuus L. using
supercritical CO2 . Experiments were performed using a semi
continuous supercritical fluid extraction system (SFXTM System
220, Isco Inc., Lincoln, NE, USA) [15].
In each experiment, known mass of dry milled seeds about 4 g
was put in 10 ml fixed-bed extraction column (57 mm 20 mm
i.d., ISCO stainless steel extraction cell) and 0.5 m filters were
placed at both ends of the extraction column to prevent any carry
over of particles.
The extract was collected in collection vials which con-
tained glass wool. In order to obtain extraction profiles with
time, the collection vials were changed every 10 min for the
first 90 min and then every 30 min along the overall supercrit-
ical extraction time. The water co-extracted with sunflower oil
was removed by vacuum oven at 373 K and then the mass
of extracted oil were determined gravimetrically. Each exper-
iment under certain condition was repeated at least 3 times.
Standard error among the data was about 3%. Therefore, the
arithmetical average of the repeated experiment data formed
each data in all figures. The extraction yield [m(t)/mo ] is
defined according to the weight of the extracted sunflower oil
[m(t)] divided by the weight of the oil which obtained from
Soxhlet extraction using hexane [mo ], on dry basis sunflower
seed.
The extraction runs were carried out in the range
of 2060 MPa pressures, 313353 K temperatures, 16 cm3
CO2 min1 flow rates and 0.232.18 mm mean particle sizes.
327
2.3. Soxhlet extraction
To compare the extraction strength of supercritical fluid
extraction with conventional organic solvent extraction Soxh-
let extractor was employed using hexane as the solvent. These
experiments were carried out at the boiling point of solvent until
any extractability of oil from seeds was obtained from the sun-
flower seeds. Until no further color change was observed for the
solvent leaching the sunflower seeds in thimble. The exhaustive
Soxhlet extraction process took about 360 min. The extracted
phase (sunflower and solvent) was then distilled in two stages
to separate sunflower oil from solvent. The first stage was a
simple distillation followed by a second stage, which was a
Rotavapour apparatus. Based on organic solvent extraction of
sunflower seeds, the seeds were found to contain 52 wt.% of
hexane extractable material.
3. Results and discussion
In this study, the effects of operating parameters as pressure,
temperature and supercritical CO2 flow rate and the effect of
pretreatment of solid as size reduction on the extraction yield
were investigated. Obtained extraction yields were compared
with model results.
The extraction process could be modeled using shrinking core
model. This model describes the situation of the irreversible
desorption followed by diffusion in the porous solid through
the pores. When the mass transfer rate of the solute in the non-
extracted inner part is much slower than that in outer part where
most of the solute has been extracted, or solute concentration is
much higher than the solubility of the solute in the solvent phase,
a sharp boundary may exit between outer and inner region. A
core of inner region shrinks with the progress of the extraction.
Mass transfer equations for bulk phase and solid phase that
were characterized the extraction of sunflower oil from the seeds
by supercritical CO2 were described in previous study [8]. The
differential equations coupled with boundary and initial condi-
tions were solved numerically by CrankNicholsons method
[9]. Proposed model equations solved at MATLAB 6.5.
The mass transfer coefficient (kf ) [8,10] in a packed bed
supercritical extractor and the axial dispersion coefficient (DL )
[8,11] in the bulk phase were estimated with using empirical
correlations. In addition, the solubility (Csat ) of sunflower oil
in supercritical CO2 was obtained using the data which were
plotted as the mass of sunflower oil extracted versus the mass of
CO2 utilized and then solubility was calculated from the slope
of the line fitted to the experimental values up to 30 min. The
effective diffusivity in the particle used as adjustable parame-
ter. The physical properties of both the solvent and solute at
the experimental conditions are shown in Table 1. The density
of CO2 was estimated by HankinsonBrobstThomson (HBT)
method [12]. The viscosity of CO2 was calculated by the viscos-
ity correlation of JossiStielThodos method [12]. Furthermore,
the value of particle porosity, calculated by (1 (p /s )) [18],
was 0.31, where p and s are densities of the solid matrix with
and without void volume of solid matrix, respectively. The den-
sities of p and s for sunflower seed were given as 922 kg m3
328 U. Salgn et al. / J. of Supercritical Fluids 38 (2006) 326331

Table 1
Physical properties of supercritical CO2 and sunflower oil at experimental conditions (40 MPa, 313 K, 4 cm3 CO2 min1 and 0.23 mm)

P (MPa) T (K) (kg m3 ) 105 (Pa s) Csat (g oil kg1 CO2 ) kf 106 (m s1 ) DL 1012 (m2 s1 ) De 1010 (m2 s1 )

20 313 848 2.15 3.02 4.77 1.75 6.15

333 729 1.72 2.60 4.30 1.89 5.53
353 587 1.33 1.04 3.68 1.99 4.73
30 313 920 3.30 6.41 5.24 1.92 6.71
333 837 2.76 6.69 4.44 1.99 5.83
353 748 2.33 6.46 3.92 2.28 5.03
40 313 962 4.42 10.41 5.54 2.45 7.15
333 894 3.77 12.27 4.92 2.47 6.32
353 822 3.27 17.60 4.53 2.67 5.87
50 313 1000 5.68 18.63 5.85 2.99 7.51
333 940 4.97 24.09 5.46 2.86 7.04
353 878 4.25 27.64 5.23 2.98 6.73
60 313 1031 6.99 22.35 6.39 3.76 8.21
333 980 6.06 24.83 6.16 3.56 7.91
353 924 5.29 28.23 5.85 3.45 7.58

and 637 kg m3 , respectively [13]. The bed void fraction for our
experimental system was determined 0.62.
3.1. Effect of pressure
As expected, the rate of supercritical CO2 extraction of sun-
flower oil largely increased with pressure shown in Fig. 1ac
where oil yield data obtained 20, 30, 40, 50 and 60 MPa are
reported for experiments performed at 313, 333 and 353 K tem-
peratures, 4 cm3 CO2 min1 flow rate, and 0.23 mm mean par-
ticle size. The effect of the extraction pressure can be explained
taking into account the large increased (from 3.63 to 18.63 g
oil kg1 CO2 for 313 K, 20 MPa and 313 K, 60 MPa, respec-
tively) in the solubility of the oil constituents (mainly triglyc-
erides) with pressure. Moreover, a large part of the extraction
process controlled by this thermodynamic parameter, as sug-
gested by the experimental data: this first part of yield data could
be fitted using a straight line. A lot of scientific literature signals
an increase of the seed oil solubility with the extraction pres-
sure [1520]. Fig. 1ac indicate that the extraction at pressures
lower than 20 MPa was not feasible. This may be due to the fact
that sunflower oil has very small solubility in CO2 at and below
20 MPa. At 50 and 60 MPa, the of about 90 wt.% was obtained
over very short extraction times (ca. 40 min) (see Fig. 1ac)
This is a combined result of the large solubility of triglycerides
at these pressures and of the relatively small quantity of oil con-
tained in this kind of seed. Comparison of all figures reveals that
higher yields (99%) were obtained at the higher temperature,
i.e. 353 K. The mathematical model described satisfactorily the
experimental data in Fig. 1ac. The overlap between experimen-
tal data and model curves is good for all the pressures studied.
3.2. Effect of temperature
The effect of temperature has been studied for experiments
performed from 20 to 60 MPa pressures, 0.23 mm main parti-
cle size and a 4 cm3 CO2 min1 flow rate. Temperatures of 313,
333 and 353 K were explored for each pressure. Several scientific
literature signals an increase of the seed oil solubility with the
extraction temperature that can be significant when the process is
performed at pressures higher than 40 MPa [7,21,22]. Our exper-
imental results at a pressure of 30 and 20 MPa show an opposite
effect of the temperature increase on the sunflower extraction
rate; i.e. the experimental points at different temperature prac-
tically overlap as shown in Fig. 2ac. Instead, the experiments
performed at pressures greater than 30 MPa pressure give extrac-
tion rates at different temperatures that could be in agreement
with the previous cited literature. However, at further 30 MPa
pressure the extraction is very fast and the number of experi-
mental points collected in the first part of the extraction process
was not sufficient to obtain conclusive information about the
effect of temperature. As in the previous paragraphs, that the
equilibrium solubility of sunflower oil controls at least the first
part of extraction process.
The solubility of sunflower oil in supercritical CO2 increased
slightly with temperature at higher pressures (above 30 MPa).
However, solubility of sunflower oil in supercritical CO2 at the
pressure of 20 MPa decreased significantly with temperature.
Such retro-gradation behavior of solubility isotherms has been
reported previous [24,25]. This is due to the fact that an increase
in temperature at constant pressure leads to a drop in CO2 density
as well as an increase in the vapor pressure of solutes. The drop
in CO2 density is substantial at pressures near the critical point,
resulting in a drop in solubility. However, at higher pressures the
drop in CO2 density due to the similar temperature increase is
small, which is overcome by the vapor pressure increase and the
net effect is a solubility increase [26]. Similar solubility behavior
has been reported for other vegetable and seed oils [27,28].
It is clear that with the increase of temperature, the extrac-
tion yield at 20 MPa increased. The yield obtained at the end of
the extraction period was about 4.5-fold when the temperature
increased from 313 to 353 K (Fig. 3a). Due to retro-gradation
behavior of solubility at higher pressure (above 30 MPa), the
 U. Salgn et al. / J. of Supercritical Fluids 38 (2006) 326331
Fig. 1. Effect of pressure on the extraction yield at 4 cm3 CO2 min1 flow rate
and 0.23 mm mean particle size (a) 313 K; (b) 333 K; and (c) 353 K.
yields obtained at the end of the extraction period was constant
ca. 0.90 kg kg1 (Fig. 3c).
The mathematical model described satisfactorily the experi-
mental data in Fig. 2ac. The overlap between experimental data
and model curves is good for all the temperature studied.
3.3. Effect of supercritical CO2 ow rate
The effect of CO2 flow rate is shown in Fig. 3a and b. Fig. 3a
is a plot of the extraction yield versus the extraction time, and
Fig. 3b is a plot of the extraction yield versus the total weight
of supercritical CO2 that has been passed through the packed
bed extractor. It is seen that the extraction rate is affected sig-
329
Fig. 2. Effect of temperature on the extraction yield at 4 cm3 CO2 min1 flow
rate and 0.23 mm mean particle size (a) 20 MPa; (b) 30 MPa; and (c) 40 MPa.
nificantly CO2 flow rate. The extraction rate increases with the
increase in CO2 flow rate as in Fig. 3a, while Fig. 3b shows that
the extraction curve is not affected by supercritical CO2 flow
rates all curves lie on a single line. This increase in extraction
rate with time is almost linear in the early stages of extraction.
It is interesting to note that all the data points for all the flow
rates fall on a single curve indicating the accuracy and consis-
tency of the data and emphasizing that not the flow rate but
the total amount of CO2 used in a given time per fixed amount
of seeds account for the success of extraction. This also led to
the conclusion that solubility but not the external mass trans-
fer resistance controls the extraction process over the range of
experimental conditions investigated here. Several researcher in
330 U. Salgn et al. / J. of Supercritical Fluids 38 (2006) 326331

the literature reported similar observation. This indicates by Roy

et al. [23] that the exit concentration of the extracts in indepen-
dent of supercritical CO2 flow rate, and therefore, it is considered
that the process is in equilibrium, and the intraparticle diffusion
resistance is not dominant in this extraction process.
Mass transfer coefficient (kf ) increased with increase in super-
critical CO2 flow rate (Table 2). This was due to the decrease
in mass transfer resistance, because of increase in convection.
The comparison between model curves and experimental data
was also successful in given experimental conditions. This result
confirms that the extraction process is mainly controlled by equi-
librium in the first part and then the linearly increasing mass
transfer resistance controls the behavior of the extraction pro-
cess (Table 3).

3.4. Effect of particle size

These experiments were performed using four particle frac-

Fig. 3. (a) Effect of supercritical CO2 flow rate on the extraction. (b) Variation of
extraction yield with the total weight of supercritical CO2 that has been passed
through the packed bed extractor at 40 MPa, 313 K and 0.23 mm mean particle
size.
tion ranges at a temperature of 313 K, pressure of 40 MPa, and
flow rate of 4 cm3 CO2 min1 . The highest oil yield obtained for
low mean particle size (0.23 mm) was about 91.7 wt.% at 90 min
whereas, the oil yield was 57.2 wt.% for 0.55 mm mean particle
size, 31.9 wt.% for 1.09 mm mean particle size and 26.9 wt.%
for 2.18 mm mean particle sizes. In Fig. 4, these results are
showed. As the extraction time increased, higher yields were
observed as expected. After the first 60 min, the effect of parti-
cle size on the extraction yield could be seen very clearly. Small
size particles provided higher yields. This was also an expected
result. Almost halving the mean size of the particle from 2.18
to 1.09 mm caused unappreciable improvement in the extraction
yield. Further decrease in the particle size by a factor of ca. 1/2
to 0.55 mm and ca. 1/4 to 0.23 mm did bring as much increase
in the yield; the improvement could still be regarded apprecia-
ble. Effect of intraparticle diffusion seems to gain importance
for large particles causing appreciable decrease in the extraction
yield. This figure also reveals that an extraction time of about
60 min was enough to reach the limiting highest possible yield
with the small particles at conditions specified. In addition, it

Table 2
Parameters of the mass transfer model at different supercritical CO2 flow rates (40 MPa, 313 K and 0.23 mm)

Q (cm3 CO2 min1 ) (kg m3 ) 105 (Pa s) Csat (g oil kg1 CO2 ) kf 106 (m s1 ) DL 1012 (m2 s1 ) De 1010 (m2 s1 )

1 8.58 5.02 3.19

2 962 4.42 11.04 5.11 3.07 7.15
3 11.79 5.32 2.90
4 10.41 5.54 2.45
6 9.82 5.73 2.02

Table 3
Parameters of the mass transfer model at different particle sizes (40 MPa, 313 K and 4 cm3 CO2 min1 )

dp (cm3 CO2 min1 ) (kg m3 ) 105 (Pa s) Csat (g oil kg1 CO2 ) kf 106 (m s1 ) DL 1012 (m2 s1 ) De 1010 (m2 s1 )

0.23 10.41 5.01 2.93 6.83

0.55 962 4.42 10.01 5.54 2.45 7.15
1.09 4.53 6.57 2.20 9.18
2.18 3.59 7.18 1.89 11.23
 U. Salgn et al. / J. of Supercritical Fluids 38 (2006) 326331
Fig. 4. Effect of mean particle size on the extraction yield at 40 MPa, 313 K and
4 cm3 CO2 min1 flow rate.
is possible to reach the limiting highest yields (88.8 wt.%) in
shorter times (60 min) with decreasing particle size from 2.18 to
0.23 mm. A similar behavior has been reported in the literature
in some cases of supercritical fluid extraction of oil from seeds
when large particle sizes were used [15,18,21,23]. In that case,
part of the oil was not extracted due to the very long diffusion
times of the solvent in the vegetable particles. The mathematical
model using model data in Table 3 described satisfactorily the
experimental data in Fig. 4.
4. Conclusions
Sunflower seed oil was extracted using supercritical CO2 . The
effects of pressure, temperature, supercritical CO2 flow rate and
mean particle size on the extraction yield was investigated. The
experimental results show that extraction yield increase linearly
with time in the early stages of extraction and the extraction
process is limited by the solubility of solute in the supercriti-
cal CO2 . Thus, intraparticle mass-transfer/diffusion limitations
are not dominant. The extraction rate increases with increas-
ing pressure because of increasing oil solubility. Moreover, the
extraction process was modeled using shrinking core model.
The model using the best fit of De correlates the data satisfacto-
rily. Experimental extraction yields were compared with model
results and the overlap between experimental data and model
curves was good for all the extraction conditions studied.
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