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Effect of the Instant Controlled Pressure- Drop DIC Technique on the

Supercritical Carbon Dioxide Date Seeds Oil Extraction

Article in ARABIAN JOURNAL FOR SCIENCE AND ENGINEERING · November 2020

DOI: 10.1007/s13369-020-05061-w

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Arabian Journal for Science and Engineering
https://doi.org/10.1007/s13369-020-05061-w

RESEARCH ARTICLE-CHEMICAL ENGINEERING

Effect of the Instant Controlled Pressure-Drop DIC Technique

on the Supercritical Carbon Dioxide Date Seeds Oil Extraction
Mehdi Louaer1 · Ahmed Zermane1,2 · Colette Besombes3 · Karim Allaf3 · Abdeslam Hassen Meniai1

Received: 7 July 2020 / Accepted: 23 October 2020

© King Fahd University of Petroleum & Minerals 2020

Abstract
The present study deals with the effect of combining instant controlled pressure-drop DIC texturing as a pretreatment step
and the supercritical carbon dioxide extraction of date seeds oil in order to improve the extraction yield and/or time. Ground
samples with mean particle size of 0.9 mm and undergoing no further treatments were used. Since the impact of DIC texturing
mainly depends on the treatment time t and the absolute saturated steam pressure P, a response surface methodology RSM was
carried out using these two independent factors and the oil yields and effective diffusivity as the response variables. A scanning
electron microscope SEM showed that DIC pretreatment induced controlled modifications of the structure, breaking cell walls,
thus enhancing the extraction performance. The results showed that the optimum extraction yield of DIC pretreated samples
increased by an improvement over control of 15.48% and the extraction time reduced by 30%, which is quite encouraging.

Keywords Date seeds oil · DIC · Process enhancement · SFE · Texturing

Abbreviations have some drawbacks in terms of solvent toxicity, long pro-

cessing times, low yield and high energy consumption [1].
Adj MS Adjusted mean squares The interest in supercritical fluid extraction technology is
Adj SS Adjusted sum of squares getting greater due to the high quality of the extracts with
DF Degree of freedom desirable composition and also the absence of incidences on
DoE Design of experiments the environment. However, its high cost which is directly
F value Fisher’s function related to the extraction time seems to be the main imped-
P value Probability threshold iment to a larger use of this highly interesting extraction
SE coef Standard error for the estimated coefficient process, hence the search, the development and the test of
Seq SS Sequential sums of squares pretreatment techniques to improve these two criteria, i.e.,
T value Test statistics the extraction yield and the processing time, and the present
work fits into this perspective.
In fact, several pretreatment techniques including drying,
1 Introduction grinding, etc., are traditionally known and the main objective
of the present study is to test the use of the instant controlled
Supercritical fluid extraction (SFE) has been increasingly pressure drop DIC as a pretreatment step for the supercritical
presented as an alternative to conventional extraction tech- fluid extraction of oils from biomasses.
niques such as solvent extraction and hydrodistillation which Introduced in 1988, the instant controlled pressure-drop
DIC technique is mainly based on an instant drop in pres-
B Abdeslam Hassen Meniai sure to vacuum following a short-time heat treatment. DIC
meniai@yahoo.fr has been used in several industrial applications such as
1 swell/drying of vegetables [2, 3], texturing [4], autovaporiza-
Laboratory of Environmental Engineering Processes,
University of Constantine 3, Constantine, Algeria tion extraction of volatiles compounds [5, 6] and pretreatment
2 in solvent extraction of active molecules and vegetable oils
University Larbi Ben M’Hidi, Oum El Bouaghi, Algeria
[7, 8]. Similar to several other techniques such as grind-
3 Laboratory of Engineering Science for Environment, ing, ultrasound, microwaves and enzymes, DIC can be used
University of La Rochelle, La Rochelle, France

123

as an intensification way of extraction processes [9–11].
However, DIC has the specificity to be a relevant texturing
technique that allows the expansion and the modification of
the solid matrix’s microstructure, possibly leading to broken
cell walls. Adequate DIC treatment may also be suitable for
this purpose, particularly when used as a pretreatment step,
showing a positive impact on the extraction yields and time
[7, 8].
Among the extraction techniques, Supercritical fluid
extraction (SFE) has been increasingly presented as an alter-
native to conventional extraction techniques such as solvent
extraction and hydrodistillation which have some drawbacks
in terms of solvent toxicity, long duration, low yield and high
energy consumption [1].
In SFE, Carbon dioxide is the most widely used fluid. Due
to its specific properties such as being inert, nontoxic, non-
flammable, separates easily and completely from the extract,
available with high purity and at low cost, with relatively
low critical temperature and pressure (T c  31.1 °C, Pc 
73.8 bar), which make it an advantageous and a suitable
fluid for use in SFE for the extraction of thermosensitive
compounds [12, 13].
Date palm (phoenix dactylifera L) belonging to the fam-
ily of palmaceae is an important plant in arid and semiarid
regions and is of several types and varieties. Date seeds have
been used in the production of caffeine-free coffee and ani-
mals feeding. Nowadays, date seeds are also used for the
extraction of vegetable oil [14, 15]. Progressively, date seeds
oil has become an important product due to its high nutritional
content such as proteins, vitamins and antioxidants [16–18].
In addition, date seeds oil has shown a good oxidative and
thermal stability giving it a good shelf-life [19].
The objective of the current study was to enhance the
extraction of date seeds oil coupling SC-CO2- E (the super-
critical carbon dioxide extraction) to DIC texturing tech-
nique. This is tested for the first time with seed dates and
was already tested for other materials such as soybeans as
reported in [20].
2 Materials and Methods
2.1 Sample Preparation
Algerian date seeds from local “Ghars” variety were used in
this study and obtained from palms of Biskra, a region in the
southeast of Algeria. They were first cleaned and ground to
reduce the particles’ diameter. After that, the particles were
classified according to their sizes by mechanical sieving. The
fraction of particles having a mean diameter of 0.9 mm (rang-
ing between 0.8 and 1.0 mm) did not undergo any further
treatment and was used as control.
123
Arabian Journal for Science and Engineering
Carbon dioxide (purity 99.5%) (SIDAL SPA Air Liquide,
Algiers, Algeria) was used for oil extraction. The water con-
tent in the samples was obtained by drying in vacuum oven
at 105 °C for 24 h.
2.2 Instant Controlled Pressure-Drop DIC
2.2.1 DIC Equipment
The experimental setup of the instant controlled pressure-
drop DIC is composed of the following main elements: (1)
a treatment vessel, where the sample is placed and treated;
(2) a pressure control system, which ensures an instantaneous
(less than 0.2 s) connection between the treatment reactor and
the vacuum tank; (3) a 700 l Vacuum tank; and (4) a vacuum
water-ring pump ensuring a vacuum level of about 5 kPa in
the vacuum tank. A schematic drawing of DIC equipment is
shown in Fig. 1.
2.2.2 DIC Pretreatment Procedure
In order to study the effect of combining the DIC texturing
with SFE (SC-CO2 ) process, the ground date seeds were
first treated following various DIC conditions. For each
operation, 50 g of 0.9 mm date seeds powder was placed
in the treatment vessel where a vacuum stage was estab-
lished in order to ensure an intimate contact between the
product surface and the high-pressure saturated dry steam
(0.1–0.7 MPa), which was injected and maintained for the
whole DIC treatment time (20–60 s). By opening the instant
valve, an instant pressure drop toward a vacuum (4/5 kPa)
resulted in an autovaporization of water along with volatile
compounds and induced an instant cooling and texturing of
the seeds matrix.
2.2.3 DIC Pretreatment Optimization
A response surface methodology (RSM) based on the cen-
tral composite design with five levels and two factors: DIC
treatment time t DIC (s) and steam pressure PDIC (MPa), was
used to optimize the effect of the DIC pretreatment on the
date seeds oil SC-CO2 extraction using Minitab 16 software.
Levels of the two factors were chosen according to [15] where
DIC technique was performed to enhance the extraction per-
formance of date seeds oil using organic solvent.
Experimental process parameters levels are shown in
Table 1.
The design of experiments (DoE) consists in a number of
trials N  factorial trials 2 k + star trials 2 k + central replicate
points CP, where k is the number of factors [21]. In the current
case, k  2 and the required number of experiments was 12
(Table 1). Since DoE adopted in this case was an orthogonal
factorial design, α is defined as the axial distance and depends
Arabian Journal for Science and Engineering

Fig. 1 Schematic representation of DIC equipment

Table 1 Different extraction trials and the different effective diffusivities Deff including nontreated and DIC-treated samples
Trials P T Yields IOC for yield R2 Effective diffusivity Deff IOC for effective
E10 diffusivity
(MPa) (s) (g Oil/g ddb) % NER modeling (%) m2 /s %

Control – – 0.0646 0 99.11 1.291 0

DIC1 0.4 40 0.0725 12 98.42 1.706 32
DIC2 0.697 40 0.0743 15 (optimum) 98.93 2.065 60
DIC3 0.4 60 0.0738 14 98.46 1.988 54
DIC4 0.4 40 0.0731 13 98.05 1.697 31
DIC5 0.61 54 0.0742 15 99.12 2.180 69 (optimum)
DIC6 0.61 26 0.0739 14 99.18 2.018 56
DIC7 0.4 40 0.0729 13 99.34 1.863 44
DIC8 0.19 26 0.0711 10 99.43 1.738 35
DIC9 0.19 54 0.073 12 98.15 1.779 38
DIC10 0.4 40 0.0727 13 98.74 1.755 36
DIC11 0.103 40 0.0719 11 99.76 1.659 29
DIC12 0.4 20 0.0721 12 99.46 1.783 38
<CP-DIC> 0.4 40 0.0728 ± 0.0003 12.7% ± 0.4% 99.06 1.748 ± 0.076 35 ± 6%
Central composite design

√4 Response  β0 + β1 × PDIC + β2 × tDIC + β11 PDIC

2
on the number of factors k: α  2k [15]. In this work, k  2
and α  1.414213562. + β22 × tDIC
2
+ β12 × PDIC × tDIC (1)
The statistical analyses of the two considered responses
which are the extraction yield and the effective diffusivity where β0 is a constant, β1 and β2 are the linear coefficients,
allow the expression of a second-order polynomial mathe- β11 and β22 are the quadratic coefficients and β12 is the inter-
matical empirical model in terms of the operating factors active coefficient.
PDIC (MPa) and t DIC (s):

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 Arabian Journal for Science and Engineering

2.3 Supercritical Carbon Dioxide Extraction supercritical fluid within the plant matrix. This model was
identified for all materials: untextured (control) and different
A mass of 50 g of DIC-pretreated and nontreated date seeds DIC-textured samples, leading to the determination of the
was used for dynamic SC-CO2 extraction. The experiments effective diffusivity Deff [8].
were carried out using a dynamic pilot plant (Separex 4343, Most of extraction operations depend upon how easily the
type SF2) supplied by Separex (Champigneulles, France) that solvent penetrates into the solid, its affinity with the solute
mainly consists of (A) high-pressure pump; (B) extraction and the diffusion of this latter. Therefore, the governing equa-
vessel; (C) pressure regulation system and (D) two separator tion for this process is the Fick diffusion equations which was
vessels in series. expressed in terms of the densities as reported in the literature
The extraction process was run at a temperature of 40 °C, [15]:
a pressure of 25 MPa, a constant solvent flow rate of 50 g/min  
ρe −
→ −→ ρe
for all the experiments and a total dynamic extraction time ve − −
v− 
matrix  −Deff ∇ (4)
of about 210 min, according to the following steps: ρmatrix ρmatrix

1. The extraction autoclave was filled with 50 g of date seeds where Deff is the effective diffusivity (m2 /s), −
→
ve − − v−−→
matrix is
powder. the relative velocity of the solute (m/s) to solid dry material
2. Liquid CO2 was cooled and then pumped into the extrac- (m/s).
tor until the desired pressure was reached (25 MPa). ρe is the apparent density of the solute within the porous
Before entering the extraction autoclave, CO2 was pre- solid (kg/m3 ).
heated to the operating extraction temperature of 40 °C. Simplifying hypotheses including the absence of expan-
3. The expansion valve was opened, and a supercritical CO2 sion, shrinkage, etc., were used in [15] to give −
v−−→
matrix  0 and
flowed through the seed bed. The pressure was main- ρmatrix  constant, leading to the following simple Fick’s-
tained constant by using the expansion valve, and oil type law expression:
samples were taken every 15 min.
ρe −
→  e
ve  −Deff ∇ρ (5)
Extraction yield was expressed as:
  As reported in [8], the diffusivity coefficient can be
g Oil We
Yields  (2) regarded as constant by assuming a structural and thermal
g drybasis, db Ws
homogeneity to enable the use of the second Fick’s law
Here, We and Ws are the weight of the extracted oil and expressed as:
that of the initial seeds on dry basis of seeds (seeds free of
water and oil), respectively, which are expressed in grams. ∂ρe ∂ 2 ρe
 −Deff 2 (6)
The yields of the SC-CO2 extracted oil are expressed in ∂t ∂r
(g oil/g db).
The choice of the most appropriate numerical methods
Finally, to assess the impacts of DIC pretreatment on SFE
to solve the above equation along with appropriate initial
oil extraction, it is worth to introduce the improvement over
and boundary conditions is well detailed in [8], and the final
control (IOC%) defined as the relative increase in pretreated
solution of Eq. 6 is:
samples oil yield reported to control:
 
YDIC − YControl Y∞ − Y
IOC  (3) ln  [−K (t − t0 )] (7)
YControl Y∞ − Ytt0

Here, Y DIC and Y Control are the extraction yields for
DIC-treated sample and for control (untextured sample),
respectively.
2.4 Modeling of Extraction Kinetics
Once the operation reached the quasi-static evolution, the
external resistance within the supercritical CO2 can be con-
sidered as negligible (negligible external resistance—NER).
Thus, from a phenomenological point of view, the extraction
can be modeled through an internal diffusion process of the
Here, Y, Y ∞ and Ytt0 are the instantaneous, the maxi-
mum and the initial amounts of extracted solute (oil) in kg/kg
db, respectively, and K is a simplifying numerical constant
regrouping terms of the solution.
The relation to calculate the effective diffusivity Deff is
finally as follows:
dp2
Deff  K (8)
π2
Here, d p is the solid particles diameter.

123
Arabian Journal for Science and Engineering
The improvement over control for effective diffusivity
(IOCDeff %) was defined as the relative increase in pretreated
samples effective diffusivity reported to control:
DeffDIC − DeffControl
IOCDeff  (9)
DeffControl
2.5 Internal Structure Analysis
The internal structure of date seeds was examined by means
of a scanning electronic microscope SEM (JEOL JSM-
7100F). The samples were placed on carbon adhesive tapes.
The observations were made in partial vacuum with an accel-
eration voltage of 2 kV and magnifications ranging from ×
200 to × 500.
3 Results and Discussions
3.1 Water Content
Twelve samples were treated by DIC, and just one sample
was untreated. The water content of the studied samples was
obtained by drying at 105 °C and weighting after about 24 h, it
was 10% for the untreated sample and a mean value is 10.5%
with an average deviation of ± 0.38% for the DIC-pretreated
samples.
Since the DIC pretreatment of the date seeds resulted
in their texturing, the increase in porosity and surface area
resulted in lower water activity and higher water content of
pretreated samples as well as additional adsorption of air
humidity.
3.2 Effect of the DIC Pretreatment on the SFE
Performances
3.2.1 Effect of the DIC Pretreatment on the Extraction Yield
General Behavior Table 1 presents the date seeds oil yields
for both nontreated and DIC-pretreated samples using super-
critical carbon dioxide as solvent, at CO2 temperature T CO2 ,
pressure PCO2 and mass flow rate Q of 313 K, 25 MPa and
50 g/min, respectively. The extraction yield was calculated
according to Eq. 2.
Table 2 shows that the instant controlled pressure-drop
DIC texturing systematically allowed the extraction yield by
SC-CO2 to increase. The matrix textured by DIC would have
higher porosity (and possibly higher tortuosity) as reported in
[4, 20], hence improving the extraction kinetics. The higher
yield obtained by means of the above-mentioned SFE con-
ditions of temperature, pressure and mass flow rate would be
due to the possible cell wall rupture for the date seeds treated
by DIC. The best (optimized) DIC treatment was obtained at
saturated steam pressure of 0.7 MPa for 40 s.
Statistical Analyses As mentioned above, central composite
design was applied to obtain the effect of DIC pretreatment
conditions on extraction yields. The experimental results
were analyzed using Minitab 16 software. The mathemat-
ical empirical equations relating the extraction yield in terms
of the independent DIC pretreatment parameters: steam pres-
sure PDIC (MPa) and treatment time t DIC (s), can be written
using coded units as follows:
 
g oil
Y  0.073 + 0.0009P + 0.00058t
g seeds db
+ 0.00015P 2 + 0.00007t 2 − 0.00039Pt
(10)
Y gives the mass of extracted oil over the mass of seeds on
dry basis (db), i.e., totally free of water and oil.
The fitting quality of the model was assessed by the
coefficient of determination R2 , the adjusted coefficient of
determination R2 (adj) and the “lack-of-fit” parameter. The
effect of factors in the model was evaluated with P value and
F value, and a small P value (< 0.05) and a large F value
indicate that the effect is significant [22]. In this study, steam
pressure (P value  0.000) and treatment time (P value 
0.000) and the interaction coefficient (P value  0.008) have
significant effects on the response as confirmed by the results
shown in Table 2 where the predicted R2 , R2 (adj) and P (lack-
of-fit) values were 97.67%, 95.74% and 0.857, respectively,
indicating that this regression study was statistically satisfac-
tory. Value of R2 (pred)  93.38% indicated that the model
had a good capacity of prediction of new observations.
Quadratic effects of treatment time and steam pressure
were nonsignificant (P value  0.392, 0.111, respectively).
The empirical equation relating the extraction yield to
the independent parameters excluding nonsignificant terms
becomes:
 
g oil
Y  0.0730 + 0.000917P
g seeds, db
+ 0.0005757t − 0.03875Pt (11)
Response surface and isoresponse (Fig. 2) can be used
to visualize the effect of DIC operating parameters on the
extraction yield.
Figure 2 shows clearly how the DIC steam pressure and
the treatment time operating factors increased significantly
the extraction yield.
An increase in DIC steam pressure and treatment time
increases significantly the porosity of the seeds. This latter
increased the contact surface area with the fluid, which dif-
fuses more easily into the solid and accesses even distant
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 Arabian Journal for Science and Engineering

Table 2 Analysis of variance for

oil yield Source DF Seq SS Adj SS Adj MS F value P value

Regression 5 0.000010 0.000010 0.000002 50.41 0.000

Linear 2 0.000009 0.000009 0.000005 116.65 0.000
PDIC (MPa) 1 0.000007 0.000007 0.000007 167.33 0.000
t DIC (s) 1 0.000003 0.000003 0.000003 65.96 0.000
Square 2 0.000000 0.000000 0.000000 1.90 0.229
PDIC * PDIC (MPa) 1 0.000000 0.000000 0.000000 3.49 0.111
t DIC (s) * t DIC (s) 1 0.000000 0.000000 0.000000 0.85 0.392
Interaction 1 0.000001 0.000001 0.000001 14.94 0.008
PDIC (MPa) * t DIC (s) 1 0.000001 0.000001 0.000001 14.94 0.008
Residual error 6 0.000000 0.000000 0.000000 – –
Lack-of-fit 3 0.000000 0.000000 0.000000 0.25 0.857
Pure error 3 0.000000 0.000000 0.000000 – –
Total 11 0.000010 – – – –
R2 97.67%
R2 (adj) 95.74%

Fig. 2 (Right) Three-dimensional response surface of the effect of DIC parameters on yield (%) and Deff (m/s) and (Left) isoresponse showing the
effect of DIC parameters on yield and Deff (m/s) (%)

regions, enhancing the oil extraction yield and subsequently The optimization of operating conditions by means of
the extraction rate. Minitab 16 showed that the highest yield was estimated to be
0.0746 (g oil/g db) for a steam pressure of 0.7 MPa for 60 s.

123
Arabian Journal for Science and Engineering

Fig. 3 Extraction kinetics

Table 3 Analysis of variance for

effective diffusivity Deff Source DF Seq SS Adj SS Adj MS F value P value

Regression 5 0.002955 0.002955 0.000591 11.36 0.005

Linear 2 0.002427 0.002427 0.001213 23.34 0.001
PDIC (MPa) 1 0.002002 0.002002 0.002002 38.51 0.001
t DIC (s) 1 0.000424 0.000424 0.000424 8.16 0.029
Square 2 0.000503 0.000503 0.000251 4.83 0.056
PDIC * PDIC (MPa) 1 0.000202 0.000305 0.000305 5.86 0.052
t DIC (s) * t DIC (s) 1 0.000301 0.000301 0.000301 5.79 0.053
Interaction 1 0.000025 0.000025 0.000025 0.48 0.514
PDIC (MPa) * t DIC (s) 1 0.000025 0.000025 0.000025 0.48 0.514
Residual error 6 0.000312 0.000312 0.000052
Lack-of-fit 3 0.000037 0.000037 0.000012 0.13 0.933
Pure error 3 0.000275 0.000275 0.000092
Total 11 0.003267 – – – –
R2 90.45%
R2 (adj)

3.2.2 Effect of the DIC Pretreatment on the Extraction Time
It was very important to investigate the effect of the DIC pre-
treatment on the extraction rates. In fact, referring to Fig. 3,
the comparison of the kinetics of extraction of date seeds
oil for untreated and DIC-treated seeds clearly shows that
the extraction time was 210 min to achieve the highest oil
extraction yield value of 0.063 (g oil/g seeds db) when using
untreated seeds, whereas only 147 min was sufficient to reach
the same yield value [0.063 (g oil/g seeds db)] when seeds
were DIC-pretreated; hence, an important gain of 63 min was
observed in operating time.
3.3 Phenomenological Modeling of Extraction
Kinetics
The diffusion of supercritical fluid within plant matrix greatly
depends on the porosity, expansion ratio and/or tortuosity of
the material. By maintaining constant the extraction condi-
tions of SC-CO2 pressure and temperature, it was possible
to study and compare the extraction kinetics for different
types of samples depending on their texturing. It was also
possible for the high charge value of the fluid flow (mass
flow of 50 g/min) to assume that the internal resistance
corresponded to the limiting process (negligible external
resistance—NER). By assuming the effective diffusivity Deff
constant, along each entire extraction operation, it was pos-
sible to obtain the coefficients of correlation R2 of a similar
Fick’s diffusion law, always between 98.05 and 99.75%. DIC

123

Fig. 4 Scanning electronic microscope (SEM) micrographs (× 200): a control; b DIC2-treated sample
texturing allowed the diffusivity to increase up to 69% for
DIC processing conditions of 0.61 MPa for 54 s, as saturated
steam pressure and treatment time (Table 1 and Fig. 2).
Statistical analyses for effective diffusivity are shown in
Table 3 where P (values) showed that two terms in the full
quadratic model (Eq. 12) were significant: steam pressure and
treatment time. Interaction and quadratic coefficient values
with P value more than 0.05 are insignificant.
The variance analyses show that the coefficient of deter-
mination R2 was 90.45%, the adjusted coefficient of deter-
mination R2 (adj) was 82.49% and therefore the following
full quadratic model is suitable for data predictions:
Deff E 10 (m2 /s)  0.1775 + 0.0224P + 0.0104t
+ 0.0138P 2 + 0.0138t 2 − 0.0051Pt (12)
3.4 Internal Structure Analysis
As it can be seen in Fig. 4, the structure for control (left)
was unaltered compared to DIC2 pretreated sample (right)
where a development of a porous texture was observed with
the availability of more diffusion channels.
123
Arabian Journal for Science and Engineering
4 Conclusion
This study showed that the DIC texturing technique had a
positive effect on supercritical carbon dioxide extraction of
date seeds oil, with respect to oil extraction yield and time.
The higher yields would still be more important at industrial
scale because it also implies shorter extraction time. More-
over, DIC pretreatment can also be used to overcome the
well-known difficulties of hardness and compactness of the
date stone matrix; thus, grinding may become easier.
Finally, the use of the DIC technique as a pretreatment
technique in the supercritical carbon dioxide extraction of
date seeds oil can be regarded as a performing mean for the
intensification of this process.
Authors’ Contribution Authors 1, 2 and 3 designed and performed the
experiments, derived the models and analyzed the data. All authors con-
tributed to the interpretation of the results. Authors 4 and 5 contributed
to the final version of the manuscript.
Funding Not applicable.
Availability of Data and Material The authors confirm that the data
supporting the findings of this study are available within the article.
Compliance with Ethical Standards
Conflict of interest Not applicable.
Arabian Journal for Science and Engineering
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