Huynhd a Department of Chemical Engineering, College of Engineering, De La Salle University, 2401 Taft Avenue, 1004 Manila, Philippines b Department of Chemical Engineering Technology, S
Trang 1Hoang N Nguyena,∗, Pag-asa D Gaspilloa, Julius B Maridablea, Roberto M Malaluanb,
Hirofumi Hinodec, Chris Salimc, Ha K.P Huynhd
a Department of Chemical Engineering, College of Engineering, De La Salle University, 2401 Taft Avenue, 1004 Manila, Philippines
b Department of Chemical Engineering Technology, School of Engineering Technology, Iligan Institute of Technology, Mindanao State University, Andres Bonifacio Avenue, Tibanga,
9200 Iligan City, Philippines
c Department of International Development Engineering, Graduate School of Science and Engineering, Tokyo Institute of Technology, 2-12-1-I4-1, Ookayama, Meguro-ku, Tokyo 152-8550, Japan
d Department of Inorganic Chemistry, Faculty of Chemical Engineering, Ho Chi Minh City University of Technology, 268 Ly Thuong Kiet Street, District 10, Ho Chi Minh City, Viet Nam
Article history:
Received 26 March 2011
Received in revised form 4 July 2011
Accepted 9 August 2011
Available online 27 August 2011
Keywords:
Moringa oleifera seed oil
Supercritical carbon dioxide
Optimization
Ethanol for pretreatment
Response surface methodology
ThestudyinvolvedtheextractionofoilfromMoringaoleifera(MO)kernelsusingsupercriticalfluid extraction(SFE)technique.Thearraysofoperatingparametersareextractioncondition,loading con-figuration,andSC-CO2withethanoladditionforsubstratepretreatment.Itidentifiesacombinationof operatingparametersthatprovideahigheryield.Theexperimentswereconductedinthepressurerange
of15–30MPa,35–60◦Ctemperatureinterval,averageparticlesizeof0.16–1.12mmandCO2flowrate
of0.5m3/h.Adding10%EtOHforsubstratepretreatment,increased10%intheyield.Nosignificant dif-ferenceinyieldandfattyacidcontentbetweentheoilfromSC-CO2-EtOHandSoxhletextractionwith n-hexanewasdetected.Loadingtheseedsinmultiple-stagedtraysincreasedtoasmuchas26.89%inthe yieldagainstrandomlypackedconfiguration.Responsesurfacemethodology,predictedanoptimaloil yieldof37.84%atapressureof28.97MPa,44.30◦Ctemperature,andparticlesizeof0.54mm.Acrossover pressurepointofBenoilwasfoundwithintherange22.5–30MPa
© 2011 Elsevier B.V All rights reserved
∗ Corresponding author Tel.: +63 2 5240563; fax: +63 2 5240563.
E-mail address: ngochoang.ibft@gmail.com (H.N Nguyen).
0255-2701/$ – see front matter © 2011 Elsevier B.V All rights reserved.
Trang 2condition
Fig 1. (a) The packing arrangement in the extractor unit (b) Flow scheme of the CO 2 supercritical fluid extraction pilot plant (F: flow meter; H1: freezer; H2: heater; H3:
Trang 3Table 1
Coded levels and real values of independent variables.
Factor Symbols coded Levels
Temperature (◦C) X 1 35.00 47.50 60.00
Pressure (MPa) X 2 15.00 22.50 30.00
Particle size (mm) X 3 0.16 0.64 1.12
Table2showsallthetwentyexperimentswhichincludedeight
Table 2
Central composite design for experiment and results of oil yield.
3 Results and discussion
Table 3 shows the oil yield of SC-CO2-EtOH using random
Table3showsthatdecreasingthethicknessofthesamplelayer
Table 3
Oil yield of SFE using random packing and multiple stages packed bed (extraction conditions were at pressure of 30 MPa, temperature of 47.5◦C, average particle size
of 0.32 mm, CO 2 flow rate of 0.5 m 3 /h and 10% by weight EtOH).
Number
of layers
Thickness
of a layer (mm)
Oil yield (% wt.)
Recovery a
(%)
Working efficiency of extractor (%)
10 10 40.01 ± 0.71 100.0 66.7
5 20 38.01 ± 0.57 95.0 71.4
4 25 37.25 ± 0.72 93.1 83.3
2 50 34.49 ± 0.78 86.2 90.9
1 100 29.24 ± 0.97 73.1 100.0
a The recovery is the ratio of oil yield which is extracted in each experiment in
Trang 4Table 4
Oil yield with varying initial EtOH ratio (extraction conditions were at pressure of
22.5 MPa, temperature of 47.5◦C, average particle size of 1.12 mm, CO 2 flow rate of
0.5 m 3 /h).
With co-solvent 0% EtOH 10% EtOH 15% EtOH
Oil yield 28.71 ± 0.67 31.90 ± 0.51 31.74 ± 0.82
i +
i +
i
Table 5
Analysis of variance of three polynomial models.
Linear model 19.02 <0.0001 <0.0001 Quadratic model 1298.87 <0.0001 0.3273 Cubic model 2.29 0.1747 0.9833
a P < 0.01 highly significant; 0.01 ≤ P < 0.05 significant; P ≥ 0.05 insignificant.
Table6exhibitsallthecoefficientsofthequadraticmodel.All
Table 6
Co-efficients of quadratic regression model.
P a <0.0001 <0.0001 0.0005 <0.0001 0.2177 0.1297 <0.0001 <0.0001 0.0023
a P < 0.01 highly significant; 0.01 ≤ P < 0.05 significant; P ≥ 0.05 insignificant.
Trang 5Fig 2. Plot of predicted oil yield of the regression quadratic model related with
experimental values.
Table 2 shows that, at a pressure of 22.5MPa and below,
inFigs.3and4.Thisphenomenonwithtemperatureinfluenced
Fig 3. Response surface of oil yield to the variation of pressure and temperature at
average particle size of 1.07 mm, CO flow rate of 0.5 m 3 /h and 10% by weigh EtOH.
Fig 4.Response surface of oil yield to the variation of particle size and temperature
at pressure of 29.39 MPa, CO 2 flow rate of 0.5 m 3 /h and 10% by weigh EtOH.
Fig 5.Response surface of oil yield to the variation of particle size and pressure at temperature of 44.12 ◦ C, CO flow rate of 0.5 m 3 /h and 10% by weigh EtOH.
Trang 6Table 7
Relative ratio compositions of Moringa oleifera seed oil.
Fatty
acid
SC-CO 2
extract
SC-CO 2 -EtOH extract
Soxhlet extract This work Reported value a
C 14:0 0.19 ± 0.05 0.22 ± 0.01 0.30 ± 0.18 0.10 ± 0.05
C 16:0 6.53 ± 0.28 6.40 ± 0.13 5.66 ± 0.34 7.80 ± 1.25
C 16:1 1.91 ± 0.10 1.76 ± 0.19 1.37 ± 0.08 2.20 ± 0.06
C 18:0 5.93 ± 0.02 5.59 ± 0.02 5.62 ± 0.08 7.60 ± 0.05
C 18:1 69.70 ± 0.32 69.65 ± 0.51 70.23 ± 0.31 67.90 ± 0.75
C 18:2 0.84 ± 0.00 0.82 ± 0.01 0.89 ± 0.12 1.10 ± 0.10
C 18:3 0.28 ± 0.04 0.39 ± 0.04 0.34 ± 0.21 0.20 ± 0.00
C 20:0 4.15 ± 0.04 4.47 ± 0.27 4.38 ± 0.05 4.00 ± 0.06
C 20:1 2.71 ± 0.24 2.94 ± 0.07 2.58 ± 0.04 1.50 ± 0.06
C 22:0 6.71 ± 0.48 6.58 ± 0.06 7.55 ± 0.26 6.20 ± 0.50
C 24:0 1.00 ± 0.03 1.14 ± 0.00 1.03 ± 0.04 1.30 ±
a Abdulkarim et al [10]
study
Acknowledgements
compo-sition
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