scholarly journals Synthesis of Magnetic Catalyst Derived from Oil Palm Empty Fruit Bunch for Esterification of Oleic Acid: An Optimization Study

2021 ◽  
Vol 17 (1) ◽  
pp. 65-77
Author(s):  
Shamala Gowri Krishnan ◽  
Fei-Ling Pua ◽  
Ee-Sann Tan

Biomass, renewable, abundantly available and a good source of energy. The conversion of biomass waste into valuable products has received wide attention. In this study, an empty fruit bunch (oil palm EFB) supported magnetic acid catalyst for esterification reaction was successfully prepared via the one-step impregnation process. The new magnetic catalyst achieved a higher surface area of 188.87 m2/g with a total acidity of 2.4 mmol/g and identified iron oxide as g-Fe2O3. The magnetization value of 24.97 emu/g demonstrated that the superparamagnetic catalyst could be easily recovered and separated after the reaction using an external magnet. The catalytic performance of oil palm EFB supported magnetic acid catalyst was examined by esterification of oleic acid. Esterification process parameters were optimized via Response Surface Methodology (RSM) optimization tool with Box-Behnken design (BBD). The following optimum parameters were determined: an amount of 9 wt% catalyst, molar ratio of methanol to oleic acid of 12:1, reaction time of 2 h and reaction temperature of 60 °C with a maximum conversion of 94.91% was achieved. The catalyst can be recycled up to five cycles with minimal loss in its activity. The oil palm waste-based magnetic acid catalyst indicates its potential replacement to the existing solid catalysts that are economical and environmentally friendly for the esterification process in biofuel applications. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0). 

2018 ◽  
Vol 156 ◽  
pp. 03002
Author(s):  
Iwan Ridwan ◽  
Mukhtar Ghazali ◽  
Adi Kusmayadi ◽  
Resza Diwansyah Putra ◽  
Nina Marlina ◽  
...  

The oleic acid solubility in methanol is low due to two phase separation, and this causes a slow reaction time in biodiesel production. Tetrahydrofuran as co-solvent can decrease the interfacial surface tension between methanol and oleic acid. The objective of this study was to investigate the effect of co-solvent, methanol to oleic acid molar ratio, catalyst amount, and temperature of the reaction to the free fatty acid conversion. Oleic acid esterification was conducted by mixing oleic acid, methanol, tetrahydrofuran and Amberlyst 15 as a solid acid catalyst in a batch reactor. The Amberlyst 15 used had an exchange capacity of 2.57 meq/g. Significant free fatty acid conversion increments occur on biodiesel production using co-solvent compared without co-solvent. The highest free fatty acid conversion was obtained over methanol to the oleic acid molar ratio of 25:1, catalyst use of 10%, the co-solvent concentration of 8%, and a reaction temperature of 60°C. The highest FFA conversion was found at 28.6 %, and the steady state was reached after 60 minutes. In addition, the use of Amberlyst 15 oleic acid esterification shows an excellent performance as a solid acid catalyst. Catalytic activity was maintained after 4 times repeated use and reduced slightly in the fifth use.


2019 ◽  
Vol 65 (1) ◽  
pp. 21-27
Author(s):  
Qiuyun Zhang ◽  
Dandan Lei ◽  
Qianqian Luo ◽  
Taoli Deng ◽  
Jingsong Cheng ◽  
...  

Biodiesel was synthesized from oleic acid using Ni (II)-exchanged heteropolyacids immobilized on silica (Ni0.5H3SiW / SiO2 ) as a solid acid catalyst. Based on detailed analyses of FT-IR, XRD, TG and SEM, the structural, surface and thermal stability of Ni0.5H3SiW / SiO2 were investigated. Obtained results demonstrated that the Keggin structure was well in the immobilization process and possess a high thermal stability. Various esterification reaction conditions and reusability of catalyst were studied. High oleic acid conversion of 81.4 % was observed at a 1:22 mole ratio (oleic acid: methanol), 3 wt. % catalyst at 70 °C for 4 h. The Ni0.5H3SiW / SiO2 catalyst was reused for several times and presented relatively stable. More interestingly, the kinetic studies revealed the esterification process was compatible with the first order model, and a lower activation energy was obtained in this catalytic system.


2018 ◽  
Vol 80 (2) ◽  
Author(s):  
Muzakkir Mohammad Zainol ◽  
Nor Aishah Saidina Amin ◽  
Mohd Asmadi

Liquefaction of oil palm empty fruit bunch (EFB) using 1-butyl-3-methylimidazolium chloride was investigated in this study. The experiments were designed based on central composite by response surface methodology (RSM). The optimum conditions for the predicted liquefied EFB yield of 80.97 wt% was obtained at the temperature of 151.9 °C, a reaction time of 112.78 min and a ratio (Ionic liquid to EFB) of 4.27. The Regression coefficient (R2) for the model was 0.90 indicating a high correlation between observed and predicted values. The liquefied EFB mixture was used in the preparation of carbon cryogel via a sol-gel poly-condensation reaction and calcination process. The presence of sulfuric acid during the gel synthesis promoted an active site on the gel linkage and surface. The carbon cryogel prepared was tested as catalyst in an esterification reaction. The conversion of levulinic acid and yield of ethyl levulinate were reported as 58.7% ansd 57.2 mol%, respectively.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Elisa d'Avila Cavalcanti-Oliveira ◽  
Priscila Rufino da Silva ◽  
Alessandra Peçanha Ramos ◽  
Donato Alexandre Gomes Aranda ◽  
Denise Maria Guimarães Freire

The process of biodiesel production by the hydroesterification route that is proposed here involves a first step consisting of triacylglyceride hydrolysis catalyzed by lipase from Thermomyces lanuginosus (TL 100L) to generate free fatty acids (FFAs). This step is followed by esterification of the FFAs with alcohol, catalyzed by niobic acid in pellets or without a catalyst. The best result for the enzyme-catalyzed hydrolysis was obtained under reaction conditions of 50% (v/v) soybean oil and 2.3% (v/v) lipase (25 U/mL of reaction medium) in distilled water and at 60∘C; an 89% conversion rate to FFAs was obtained after 48 hours of reaction. For the esterification reaction, the best result was with an FFA/methanol molar ratio of 1:3, niobic acid catalyst at a concentration of 20% (w/w FFA), and 200∘C, which yielded 92% conversion of FFAs to soy methyl esters after 1 hour of reaction. This study is exceptional because both the hydrolysis and the esterification use a simple reaction medium with high substrate concentrations.


2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
W. N. R. W. Isahak ◽  
M. Ismail ◽  
N. M. Nordin ◽  
J. M. Jahim ◽  
M. A. Yarmo

The purpose of this work is to study the synthesis, characterization, and catalytic performance of two types of solid heteropoly acid catalysts, namely, silicotungstic acid bulk (STAB) and STA-silica sol-gel (STA-SG) compared with sulfuric acid. From the XPS analyses, there was a significant formation of W-O-Si, W-O-W, and Si-O-Si bonding in STA-SG compared to that in STAB. The main spectra of O1s (90.74%, 531.5 eV) followed by other O1s peak (9.26%, 532.8 eV) were due to the presence of W-O-W and W-O-Si bonds, respectively. The STA-SG catalyst was found to be the more environmentally benign solid acid catalyst for the esterification reaction between oleic acid and glycerol due to its lower toxicity supported by silica via sol-gel technique. In addition, the ease of separation for STA-SG catalyst was attributed to its insoluble state in the product phase. The esterification products were then analysed by FTIR and HPLC. Both the H2SO4and the STAB gave high conversion of 100% and 98% but at a lower selectivity of GME with 81.6% and 89.9%, respectively. On the contrary, the STA-SG enabled a conversion of 94% but with a significantly higher GME selectivity of 95%, rendering it the more efficient solid acid catalyst.


Polymers ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 4056
Author(s):  
Nur Fattima’ Al-Zahara’ Tuan Mohamood ◽  
Abdul Hakam Abdul Halim ◽  
Norhazlin Zainuddin

Carboxymethyl cellulose (CMC) is modified cellulose extracted from oil palm empty fruit bunch (OPEFB) biomass waste that has been prepared through etherification using sodium monochloroacetate (SMCA) in the presence of sodium hydroxide. In this research, CMC hydrogel was prepared using calcium chloride (CaCl2) as the chemical crosslinker. Throughout the optimization process, four important parameters were studied, which were: (1) CMC concentration, (2) CaCl2 concentration, (3) reaction time, and (4) reaction temperature. From the results, the best gel content obtained was 28.11% at 20% (w/v) of CMC with 1% (w/v) of CaCl2 in 24 h reaction at room temperature. Meanwhile, the degree of swelling for CMC hydrogel was 47.34 g/g. All samples were characterized using FT-IR, XRD, TGA, and FESEM to study and compare modification on the OPEFB cellulose. The FT-IR spectrum of CMC hydrogel showed a shift of COO− peaks at 1585 cm−1 and 1413 cm−1, indicating the substitution of Ca2+ into the CMC molecular chains. The XRD diffractogram of CMC hydrogel showed no observation of sharp peaks, which signified an amorphous hydrogel phase. The CrI value also proved the decrement of the crystalline nature of CMC hydrogel. TGA–DTG thermograms showed that the Tmax of CMC hydrogel at 293.33 °C is slightly better in thermal stability compared to CMC. Meanwhile, the FESEM micrograph of CMC hydrogel showed interconnected pores indicating the crosslinkages in CMC hydrogel. CMC hydrogel was successfully synthesized using CaCl2 as a crosslinking agent, and its swelling ability can be used in various applications such as drug delivery systems, industrial effluent, food additives, heavy metal removal, and many more.


2021 ◽  
Vol 2021 ◽  
pp. 1-16
Author(s):  
Maryam Haghighi ◽  
Mehranoosh Fereidooni

In this study, ZSM-22 was synthesized using N,N-diethylaniline as a template through a hydrothermal method. The proton and various metals such as zirconium, strontium, and iron were immobilized on the surface of obtained zeolites through the ion exchange method. The catalysts were studied by Fourier-Transform Infrared Spectroscopy (FT-IR), X-Ray Diffraction (XRD), Brunauer–Emmett–Teller (BET) adsorption isotherms, Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) elemental analysis, and Temperature-Programmed Desorption of ammonia (TPD-NH3) technique for determining the number of acid sites. In the esterification reaction of oleic acid, the operating conditions such as catalyst dosage, temperature, molar ratio of methanol to oil, and reaction time were optimized and adjusted at 11 wt%, 70°C, 10 : 1, and 48 h subsequently. The maximum yield% of 48.07% was achieved in the presence of Zr-H-ZSM-22 at optimum conditions. In order to improve the efficiency of three zeolites Zr-H-ZSM-22, Fe-H-ZSM-22, and Sr-H-ZSM-22, the core-shell structures with SiO2 coating were prepared. Zr-H-ZSM-22@SiO2 was less active than Zr-H-ZSM-22 due to the SiO2 coverage of Lewis active sites.


2021 ◽  
Vol 17 (1) ◽  
pp. 16-19
Author(s):  
Yan Irawan ◽  
Ika Juliana ◽  
Emil Budianto

In this study, the synthesis of palm oil-based polymeric ester for application as a polymeric surfactant was carried out by a cationic addition polymerisation method through two steps. The initial step is a synthesis of fatty acid methyl esters oleate (FAMEO) through esterification reaction between oleic acid and methanol. The optimum conditions of the esterification reaction were carried out at a temperature of 70–80oC for 4 hours with the addition of 1wt% sulfuric acid as a catalyst. The molar ratio between oleic acid and methanol was 1:3. FAMEO was analysed using GCMS to determine the methyl ester content. The second step is the polymerisation of FAMEO. The polymerisation reaction of FAMEO was carried out at 120, 140, and 160oC with 1wt%, 3wt% and 5wt% of boron trifluoride dihydrate as a catalyst and an initiator of polymerisation reaction for 4 to 24 hours of reaction. The reaction conversion of the product was 66%. The polymeric ester was analysed H-NMR. Meanwhile, the molecular weight of that product was 1714 g/mol which analysed using GPC and the PDI was 1.12346 or equal to 1.12. It means that the polymerisation technique was controlled or living polymerisation, which indicates that the distribution type of this product was narrow monodisperse.


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