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Title: | Quantitative analysis of high free fatty acid crude palm oil separation and synthesis of palm palmitic acid based bioplastic |
Authors: | Abd Al-Wali Mohammed Mohammed Japir (P78249) |
Supervisor: | Muhammad Rahimi Yusop, Dr. |
Keywords: | Palm oil Fatty acid Bioplastic Molecular distillation |
Issue Date: | 12-Feb-2017 |
Description: | This study involves the quantitative analysis of high free fatty acid crude palm oil, the separation of palmitic acid (PA) and synthesis of palm palmitic acid based bioplastic. The separation of free fatty acids (FFA) from crude oil was done by using molecular distillation. The separation parameters were at their stillationboiling points, a feed amount of 2.3 mL/min, an operating pressure of 10 torr, a condenser temperature of 60 °C, and a rotor speed of 300 rpm, respectively. The physicochemical characteristics of crude palm oil after distillation showed that the decreasing in FFA% from 8.7±0.3 to 0.9±0.1 %, iodine value from 53.1±0.4 to 52.7±0.5 g I2/100 g, hydroxyl value of 32.5±0.6 to 13.9±1.1 mg KOH/g, unsaponifiable value from 0.30±0.05 to 0.20±0.02%, moisture content from 0.31±0.01 to 0.24±0.01 %, respectively. Gas chromatography (GC) results showed that the major fatty acids in crude palm oil (CPO) were palmitic acid (PA) 45% followed by oleic acid (OA) 39.8%. High performance liquid chromatography (HPLC) results showed that the major triacylglycerol (TAG) were 1,3-dipalmitoyl-2-oleoyl-rac-glycerol (POP) (32.4%) followed by 1-palmitoyl-2,3-dioleoyl-rac-glycerol (POO) (25.1%). Ethanolic potassium hydroxide (KOH) catalyzed reactions were used for hydrolysis the oil. The separation of saturated fatty acids (SFA) from palm fatty mixture acid (PFAM) by methanol crystallization was studied. Results showed that the PA composition increased to 90% at the optimal conditions of fatty acids-to-methanol ratio of 1:15 (w/v), the crystallization temperature of -15 °C, and the crystallization time of 24 h with a yield of 48.9%, respectively. Further separation and purification of PA from SFA by another methanol crystallization was also studied and optimized using response surface methodology (RSM) with D-optimal design. Results showed that the PA increased to 96.7% at 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 h with a yield of 87.5%, respectively. Esterification of PA was carried out using methanol, hydrochloric acid (HCl) to yield of methyl palmitate (MP) 92.7±2.5%. Synthesis of dimethyl 2-tetradecylmalonate (DMTDM) using MP with NaH in the presence of reactive solvent of dimethyl carbonate (DMC) was also carried out. The reaction conditions comprise at a mole ratio of MP: DMC: NaH: DMF (0.1:2:0.25:1) at 60 °C for 14 h with 88.3±1.4% yield. FTIR spectra of DMTDM showed the ester carbonyl group at 1740 cm-1. The polymerization of DMTDM with 1,6-hexandiol or 1,12-dodecandiol was carried out using titanium (IV) isopropoxide Ti(OiPr)4 as the catalyst and reaction time of 24 h. The results showed that the poly(dodecyl 2-tetradecylmalonte) (PDTDM) exhibited good thermal properties compared to poly(hexyl 2-tetradecylmalonte) (PHTDM). The increase of the chain length of diol in PDTDM improved the thermal properties of polyester with glass transition, Tg of 13 °C and melting point of 51 °C with a molecular weight of 12508 Da and polydispersity index (PDI) of 1.4. In general, the synthetic polyesters can be used as internal plasticizer in bio-based industry.,Certification of Master's/Doctoral Thesis" is not available |
Pages: | 196 |
Call Number: | TP247.2.J336 2017 tesis |
Publisher: | UKM, Bangi |
Appears in Collections: | Faculty of Science and Technology / Fakulti Sains dan Teknologi |
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