Optimization of methanol crystallization for highly efficient separation of palmitic acid from palm fatty acid mixture using response surface methodology





Biodiesel, D-optimal design, Methanol crystallization, Palmitic acid, Response surface methodology (RSM)


The objective of the current study was to develop parameters for the separation of palmitic acid (PA) from a crude palm oil saturated fatty acid (SFAs) mixture by using the methanol crystallization method. The conditions of methanol crystallization were optimized by the response surface methodology (RSM) with the D-optimal design. The procedure of developing the solvent crystallization method was based on various different parameters. The fatty acid composition was carried out using a gas chromatography flame ionization detector (GC-FID) as fatty acid methyl esters. The highest percentage of SFAs was more than 96% with the percentage yield of 87.5% under the optimal conditions of fatty acids-to-methanol ratio of 1: 20 (w/v), the crystallization temperature of -15 °C, and the crystallization time of 24 hours, respectively. The composition of separated SFAs in the solid fraction contains 96.7% of palmitic acid (C16:0) as a dominant component and 3.3% of stearic acid (C18:0). The results showed that utilizing methanol as a crystallization solvent is recommended because of its high efficiency, low cost, stability, availability, comparative ease of recovery and its ability to form needle-like crystals which have good filtering and washing characteristics.


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Ba-Abbad MM, Kadhum AAH, Mohamad AB, Takriff MS, Sopian K. 2013. Optimization of process parameters using D-optimal design for synthesis of ZnO nanoparticles via sol–gel technique. J. Ind. Eng. Chem. 19, 99–105. https://doi.org/10.1016/j.jiec.2012.07.010

Box GEP, Hunter WG, Hunter JS. 1978. Statistics for experimenters: an introduction to design, data analysis, and model building: Wiley Interscience. PMCid:PMC1818711

Brown J, Kolb DK. 1955. Applications of low temperature crystallization in the separation of the fatty acids and their compounds. Prog. Chem. Fats Lipids. 3, 57–94. https://doi.org/10.1016/0079-6832(55)90004-5

Bowden NB, Gupta A. 2014. Methods for Separating Mixtures of Compounds, Google Patents.

Cermak SC, Kenar JA, Evangelista RL. 2012. Distillation of natural fatty acids and their chemical derivatives: INTECH Open Access Publisher.

Chu B, Quek S, Baharin B. 2003. Optimization of enzymatic hydrolysis for concentration of vitamin E in palm fatty acid distillate. Food Chem. 80, 295–302. https://doi.org/10.1016/S0308-8146(02)00178-4

Fang G, Li H, Cao L, Shan F. 2012. Preparation and thermal properties of form-stable palmitic acid/active aluminum oxide composites as phase change materials for latent heat storage. Mater. Chem. Phys. 137, 558–564. https://doi.org/10.1016/j.matchemphys.2012.09.058

Henderson, J, Osborne, D J. 2000. The oil palm in all our lives: how this came about. Endeavour 24, 63–68. https://doi.org/10.1016/S0160-9327(00)01293-X

Japir AA-W, Salimon J, Derawi D, Bahadi M, Yusop MR. 2016. Purification of High Free Fatty Acid Crude Palm Oil Using Molecular Distillation. Asian J. Chem. 28, 2549– 2554. https://doi.org/10.14233/ajchem.2016.20095

Japir AA-W, Salimon J, Derawi D, Bahadi M, Al-Shuja'a S, Yusop MR. 2017. Physicochemical characteristics of high free fatty acid crude palm oil. OCL.

Jiang S, Shao P, Pan L, Zhao Y. 2006. Molecular distillation for recovering tocopherol and fatty acid methyl esters from rapeseed oil deodoriser distillate. Biosystems Eng. 93, 383– 391. https://doi.org/10.1016/j.biosystemseng.2006.01.008

Kempers P, Schörken U, Wolf T, Sato S, De Almeida WB, Bizzarri PS, Araujo, AS. 2013. Process for production of fatty acids, fatty acid esters and sterolesters from soapstock. Patent No. US8426622 B2.

Maddikeri GL, Pandit AB, Gogate PR. 2012. Adsorptive removal of saturated and unsaturated fatty acids using ion-exchange resins. Ind. Eng. Chem. Res. 51, 6869–6876. https://doi.org/10.1021/ie3000562

Montgomery D. 2001. Design and analysis of experiments (5thed.). New York, USA Wiley.

Myers RH, Montgomery DC, Anderson-Cook CM. 2009. Response surface methodology: process and product optimization using designed experiments (3rd ed.): John Wiley & Sons, USA.

Nakahara H, Lee S, Shoyama Y, Shibata O. 2011. The role of palmitic acid in pulmonary surfactant systems by Langmuir monolayer study: Lipid–peptide interactions. Soft Matter 7, 11351–11359. https://doi.org/10.1039/c1sm06345f

Permukaan MKGB, Wong Y, Tan Y, Taufiq-Yap Y, Ramli I. 2015. An Optimization Study for Transesterification of Palm Oil using Response Surface Methodology (RSM). Sains Malaysiana 44, 281–290. https://doi.org/10.17576/jsm-2015-4402-17

Prasanth Kumar P, Gopala Krishna A. 2015. Physicochemical characteristics of commercial coconut oils produced in India. Grasas Aceites 66, e062. https://doi.org/10.3989/gya.0228141

Salimon J, Abdullah BM, Salih, N. 2011. Hydrolysis optimization and characterization study of preparing fatty acids from Jatropha curcas seed oil. Chem. Cent. J. 5, 1–9. https://doi.org/10.1186/1752-153X-5-67 PMid:22044685 PMCid:PMC3377924

Salimon J, Abdullah BM, Salih N. 2012. Selectively increasing of polyunsaturated (18: 2) and monounsaturated (18: 1) fatty acids in Jatropha curcas seed oil by crystallization using D-optimal design. Chem. Cent. J. 6, 1–15. https://doi.org/10.1186/1752-153X-6-65

Saravanan K, Tyagi B, Shukla RS, Bajaj HC. 2016. Solvent free synthesis of methyl palmitate over sulfated zirconia solid acid catalyst. Fuel 165, 298–305. https://doi.org/10.1016/j.fuel.2015.10.043

Strohmeier K, Schober S, Mittelbach M. 2014. Solvent-assisted crystallization of fatty acid alkyl esters from animal fat. J. Am. Oil Chem. Soc. 91, 1217–1224. https://doi.org/10.1007/s11746-014-2456-8

Wanasundara UN, Wanasundara P, Shahidi F. 2005. Novel Separation Techniques for Isolation and Purification of Fatty Acids and Oil by-Products. Bailey's Industrial Oil and Fat Products. https://doi.org/10.1002/047167849X.bio065

Weisberg S. 2005. Applied linear regression (3rd ed. Vol. 528): John Wiley & Sons INC, New York. https://doi.org/10.1002/0471704091

Wu M, Ding H, Wang S, Xu S. 2008. Optimizing conditions for the purification of linoleic acid from sunflower oil by urea complex fractionation. J. Am. Oil Chem. Soc. 85, 677–684. https://doi.org/10.1007/s11746-008-1245-7

Yang K, El-Haik BS. 2009. Design for Six Sigma, A Roadmap for Product Development (2nd ed.). United States of America: The McGraw-Hill Companies.

Zhang N, Yuan Y, Yuan Y, Li, T, Cao, X. 2014. Lauric–palmitic–stearic acid/expanded perlite composite as form-stable phase change material: Preparation and thermal properties. Energy Buildings 82, 505–511. https://doi.org/10.1016/j.enbuild.2014.07.049

Zhang Z, Zheng H. 2009. Optimization for decolorization of azo dye acid green 20 by ultrasound and H2O2 using response surface methodology. J. Hazard. Mater. 172, 1388–1393. https://doi.org/10.1016/j.jhazmat.2009.07.146 PMid:19717231



How to Cite

Japir AA, Salimon J, Derawi D, Yahaya BH, Jamil MS, Yusop MR. Optimization of methanol crystallization for highly efficient separation of palmitic acid from palm fatty acid mixture using response surface methodology. Grasas aceites [Internet]. 2017Dec.30 [cited 2024Apr.17];68(4):e224. Available from: https://grasasyaceites.revistas.csic.es/index.php/grasasyaceites/article/view/1691