scholarly journals Efektifitas Penggunaan Co immobilized - Lipase pada Reaksi Esterifikasi Asam Lemak Hasil Hidrolisis Minyak Kelapa

2018 ◽  
Vol 2 (1) ◽  
pp. 23
Author(s):  
Sigit Hadiantoro ◽  
Dwina Moentamaria ◽  
Muchamad Syarwani

Kinerja enzim immobilisasi dapat ditingkatkan dengan penambahan co immobilizer, hal ini dilakukan agar ikatan kovalen antara enzim dan matriks lebih kuat dan mempermudah reaksi dari gugus fungsional yang ada pada matriks sehingga tidak diperlukan penambahan bahan kimia sebagai pembawa. Pada penelitian ini digunakan matriks polyurethane foam (PUF) dengan penambahan co immobilizer yang terdiri dari gelatin, lesitin, MgCl2, dan polyethyleh glycol (PEG) 6000. Penelitian ini difokuskan untuk melihat efektivitas co immobilized-lipase pada reaksi hidrolisis-esterifikasi. PUF direndam dalam larutan co immobilizer dengan perbandingan 1:15; 1:20 dan 1:25 (b/b) selama satu jam setelah itu dipanaskan dalam oven selama satu jam pada suhu 30°C. Selanjutnya,  matriks PUF direndam dalam lipase selama 24 jam dan dikeringkan dalam oven pada suhu 30°C selama 24 jam sehingga terbentuk matriks lipase terko-immobilisasi pada PUF dengan yang digunakan untuk reaksi hidrolisis-esterifikasi sebagai biokatalis. Pada reaksi hidrolisis digunakan 10 gram minyak yang diemulsikan dalam air dengan variabel rasio minyak-air 1:0,6; 1:1; 1:3 dan 1:5 (b/b) dan waktu reaksi 5, 10, 15 dan 20 jam. Kadar FFA minyak kelapa awal sebesar 0,21%. Produk terbaik reaksi hidrolisis adalah asam lemak bebas dengan kenaikan kadar FFA menjadi 1,18% pada kondisi perbandingan minyak/air 1:5 (b/b). Reaksi esterfikasi dilakukan dengan cara mereaksikan asam lemak hasil terbaik hidrolisis dengan sitronelol dan co immobilized-lipase sebagai biokatalis. Reaksi ini dilakukan dengan variabel asam lemak: sitronelol 1:0,8 ; 1:1 dan 1:3 (b/b) serta waktu reaksi: 5, 10, 15 dan 20 jam. Produk yang dihasilkan adalah perisa alami sebagai ester. Analisis kadar sitronelol awal dan akhir reaksi esterifikasi dilakukan dengan menggunakan GC-FID. Hasil terbaik dari penelitian ini yaitu konversi sebesar 92,88% diperoleh pada ratio massa asam lemak/sitronelol 1:3.Immobilized enzyme performance can be enhanced by the addition of co-immobilizer, this is done so that the covalent bond between the enzyme and the matrix can become stronger and also to ease the reaction of the functional groups present in the matrix so that no addition of chemical as carrier is required. This study used Polyurethane Foam (PUF) as matrix with the addition of co-immobilizer which contain gelatin, lecithin, MgCl2, and PEG 6000. This study focused on looking at the effect of co-immobilized lipase on hydrolysis-esterification reactions. PUF is immersed in an co-immobilizer solution of 1:15; 1:20 and 1:25 ratio (w/w) for one hour and heated for another hour at 30°C. After that, PUF is immersed in the lipase for 24 hours, after which is heated at 30°C also for 24 hours. This research was conducted in 2 stages of reaction, which is hydrolysis then continued by esterification. In the hydrolysis reaction, we used variables such as oil-water ratio for 1:0.6; 1:1; 1:3 and 1:5 (w/w); the reaction time 5, 10, 15 and 20 hours; and also PUF:co-immobilized ratio in 1:15; 1:20 and 1:25 (w/w). The best fatty acid obtained from hydrolysis results in oil-water ratio of 1:5 (w/w), with FFA 1.18%.  Next is esterification reaction which is done by reacting  fatty acid from hydrolyzed coconut oil with citronellol, with the addition of immobilized lipase (as a biocatalyst). This reaction was carried out with variables like mass ratio of fatty acids-citronellol 1:0.8; 1:1 and 1:3 and reaction time: 5, 10, 15 and 20 hours. The resulting product is the flavor enhancer as ester. The analysis of the percentage of initial and final citronellol on the end of esterification reaction were performed using GC-FID. The best results of this study, conversion percentage respectively 92.88% obtained at mass ratio of fatty acid-citronellol 1:3.

Author(s):  
Dwina Moentamaria ◽  
Maktum Muharja ◽  
Tri Widjaja ◽  
Arief Widjaja

Bio‐based fatty acids (FAs) produced through hydrolysis of natural oils and fats are promising chemical feedstocks for increasing  the economic value of renewable raw materials. In this work, lecithin, gelatin, PEG, and MgCl2 were employed as the co-immobilized material of crude lipase Mucor miehei immobilization on the polyurethane foam (PUF) matrix for hydrolysis of coconut oil to Free Fatty Acid (FFA). The unconventional immobilized technique was used through cross-linking and covalent bond. Single factor analysis and response surface method were utilized to determine the optimum conditions of the hydrolysis reaction. After optimization, co-immobilized lipase was examined for storage stability at a temperature of 4°C and reusability performance. The optimum conditions for coconut oil hydrolysis were obtained on the co-immobilized-PUF ratio, water-oil ratio, and reaction time of 20.17 w/w, 4.45 w/w, and 20 h, respectively. Under these conditions, the acid value as lauric acid enhanced 573% to 3.21 mg KOH/g oil. Storage stability attained through remaining activity on free lipase, PUF-lipase, PUF-co-immobilized-lipase were 9.89%, 42.3%, and 91.88%, respectively. In this study, the application of PUF-co-immobilized lipase in hydrolysis reactions can be reused up to 5 times. Characteristics of the addition of co-immobilized lipase have been analyzed using Fourier Transform Infra Red (FTIR) and Scanning Electron Microscope (SEM), showing the presence of functional groups binding and the changes in the surface matrix structure. Copyright © 2019 BCREC Group. All rights reserved 


2016 ◽  
Vol 5 (1) ◽  
pp. 13-19
Author(s):  
William ◽  
Johan Senjaya ◽  
Taslim ◽  
Tjahjono Herawan ◽  
Meta Rivani

Biodiesel production has rapidly grown over the last decades, and it has attracted much attention in the market as fuel that promising substitute for petroleum diesel, because its physical and chemical properties and energy content are similar to those of petroleum diesel. The main problem in producing biodiesel is its high cost which could be reduced by use of less expensive feedstock. Therefore, in this work biodiesel is synthesized by enzymatic esterification from low quality feedstock which is unrefined and much cheaper than the refined oil, such as palm fatty acid distillate (PFAD) with dialkyl carbonate using immobilized lipase (Novozym®435). Enzymatic process has certain advantages over the chemical process, as it is less energy intensive, allowing the esterification of glycerides with high free fatty acid contents (PFAD, 85-95% FFA) and no enzymatic activity loss. Methanol replaced by dialkyl carbonate, especially DMC due to esterification (methanolysis) is close to equilibrium reaction whereas using DMC the intermediate compound immediately decomposes to carbon dioxide and an alcohol, which have been investigated. Moreover, DMC are cheap, eco-friendly chemical, non-toxic properties and widely available. Factors affecting the reaction such as DMC to PFAD molar ratio, reaction temperature, reaction time and catalyst concentration were systematically analyzed by response surface methodology (RSM) with central composite design (CCD). The optimal condition is using 6:1 molar ratio of DMC to PFAD at 60 oC, for a reaction time 3h in the presence 10wt% of catalyst (based on oil weight). The results showed that synthesis of biodiesel through enzymatic esterification using PFAD suitable for biodiesel production.


2022 ◽  
Vol 30 (1) ◽  
pp. 377-395
Author(s):  
Hasanudin Hasanudin ◽  
Qodria Utami Putri ◽  
Tuty Emilia Agustina ◽  
Fitri Hadiah

Free fatty acid esterification (FFA) in palm oil mill waste (POME) was carried out using a sulfonated carbon-zeolite composite catalyst. The catalyst is synthesized with carbon precursor obtained from molasses, which is adsorbed on the surface of the zeolite and then carbonized and sulfonated with concentrated H2SO4 to form a sulfonated carbon-zeolite catalyst composite, which will be used for the esterification catalyst and the optimization process for the esterification reaction is carried out using the response surface methodology (RSM) and experimental central composite design (CCD). Importantly, the observed independent variables were temperature, catalyst weight, and reaction time to produce fatty acid methyl ester (FAME) products. The catalyst was successfully synthesized, which was shown from the SEM characterization strengthened by the presence of a sulfate group in the FTIR results and the calculation results of high acidity properties. Optimization of FFA esterification with SCZ catalyst obtained optimal conditions with a temperature of 79oC, a catalyst weight of 3.00 g, and a reaction time of 134 minutes with a FAME product of 93.75%, considering that the viscosity of biodiesel is below that required by the API.


2021 ◽  
Vol 29 (4) ◽  
Author(s):  
Ratna Dewi Kusumaningtyas ◽  
Haniif Prasetiawan ◽  
Radenrara Dewi Artanti Putri ◽  
Bayu Triwibowo ◽  
Siti Choirunisa Furi Kurnita ◽  
...  

Nyamplung seed (Calophyllum inophyllum L.) oil is a prospective non-edible vegetable oil as biodiesel feedstock. However, it cannot be directly used in the alkaline catalysed transesterification reaction since it contains high free fatty acid (FFA) of 19.17%. The FFA content above 2% will cause saponification reaction, reducing the biodiesel yield. In this work, FFA removal was performed using sulfuric acid catalysed esterification to meet the maximum FFA amount of 2%. Experimental work and response surface methodology (RSM) analysis were conducted. The reaction was conducted at the fixed molar ratio of nyamplung seed oil and methanol of 1:30 and the reaction times of 120 minutes. The catalyst concentration and the reaction temperature were varied. The highest reaction conversion was 78.18%, and the FFA concentration was decreased to 4.01% at the temperature of 60℃ and reaction time of 120 minutes. The polynomial model analysis on RSM demonstrated that the quadratic model was the most suitable FFA conversion optimisation. The RSM analysis exhibited the optimum FFA conversion of 78.27% and the FFA content of 4%, attained at the reaction temperature, catalyst concentration, and reaction time of 59.09℃, 1.98% g/g nyamplung seed oil, and 119.95 minutes, respectively. Extrapolation using RSM predicted that the targeted FFA content of 2% could be obtained at the temperature, catalyst concentration, and reaction time of 58.97℃, 3%, and 194.9 minutes, respectively, with a fixed molar ratio of oil to methanol of 1:30. The results disclosed that RSM is an appropriate statistical method for optimising the process variable in the esterification reaction to obtain the targeted value of FFA.


Molekul ◽  
2016 ◽  
Vol 11 (2) ◽  
pp. 256 ◽  
Author(s):  
Suci Amaliyah

The aims of this study were to determine the optimum conditions of enzymatic esterification between stearic acid with bacterial cellulose using immobilized lipase and to characterize the obtained ester. The optimum condition was observed by the effects of time and mass ratio of cellulose: stearic acid towards degree of esterification. The esterification reaction carried out in a heterogeneous system using n-butanol as solvent at 50 °C. The effect of reaction time on esterification degree is done by variating incubation time for 6, 12, 18, 24 and 30 hours. The influence of the mass ratio of cellulose: stearic acid to the esterification degree was carried out by variating 1: 1, 1: 2, 1: 3, 1: 4, 1: 5 and 1: 6. Products characterization consist of functional group analysis by Fourier Transform Infra Red (FTIR), determining degree of substitution (DS) by saponification, swelling index by gravimetric method, and cristallinity by X-Ray Diffraction (XRD). The results showed that condition of esterification was optimum in 18 hours of reaction with mass ratio 1:5. The success of esterification was confirmed by FTIR spectrum that showed ester carbonyl peak at 1718.46 cm-1 . DS of  cellulose stearate ester was 0.35. The swelling and crystallinity index of cellulose stearate was smaller than bacterial cellulose.


2017 ◽  
Vol 5 (2) ◽  
pp. 84-91
Author(s):  
Dwina Moentamaria ◽  
Girlian Agaian ◽  
Meilita Mustika Ridhawati ◽  
Achmad Chumaidi ◽  
Nanik Hendrawati

Free Fatty acid resulting from hydrolisis of various types of oil enzymatically has been great interest recently to save energy, in other hand that the product are environmentally friendly. Lipases as biocatalysts for synthesis reactions will be dissolved with the product, making difficult their reuse. Efficiency can be done with the use of enzyme immobilization, which can be used for repeated reaction. The products of free fatty acids from coconut oil by hydrolysis of lipase can be used as a natural substrate for making flavor that can be consumed and safe for health. The effect of free lipase and immobilization of lipase on hydrolisis were studied. Reaction time of hydrolisis was varied as 30, 60, 90, 120 and 150 minutes. The variation of concentration of lipase addition was 4, 5, 6, 7 and 8 % . The types of treatment were used in this research free lipase and the immobilized lipase. The results shows that the highest conversion on hydrolisis of coconut oil by using free lipase treatment was performed by 6 % of lipase addition with reaction time 60 minutes that are 52,31%. While, the highest conversion on hydrolisis of coconut oil by using the immobilized lipase was shown by 8% of lipase addition with reaction time 120 minutes that is 56,01%. The results of the hydrolysis process in the form of fatty acid was used as the base material esterification process resulting ester product (natural flavor). Ester yield was produced by free lipase esterification was 28,21 and 32,14 % in immobilized lipase esterification.


Author(s):  
Hani Hilmanto ◽  
Chusnul Hidayat ◽  
Pudji Hastuti

<p>The objective of this research was to modify the matrix surfaces to obtain both hydrophobic matrix (HM) and hydrophilic-hydrophobic matrix (HHM) for enzymatic synthesis of fructose oleic ester (FOE). The modification was performed by the attachment of 2-phenylpropionaldehyde (PPA) and PPA followed by polyethyleneimine (PEI) for HM and HHM, respectively. The results from FT-IR analysis showed that the peak of stretching vibration of NH<sub>2</sub> bond decreased and it was followed by an increase of the peak vibration of –C=N– bond at wave number 1667 cm<sup>-1</sup>. The peak of bending vibrations of the C=C bond also increased. It indicated that PPA was successfully attached on matrix. For HHM, an increase in the peak area of NH<sub>2</sub> bond indicated that PEI was also successfully attached on the matrix. The optimum conditions of lipase adsorption were obtained at buffer pH 7 containing 0.5 M NaCl (9.27 mg protein/g matrix) and without NaCl (9.23 mg protein/g matrix) for HM and HHM, respectively. For FOE synthesis, the best immobilized lipase concentration was about 8% and 6% for HM and HHM, respectively. The optimum time of esterification was 24 h and 18 h for HM and HHM, respectively, in which the yields were 75.96% and 85.29%, respectively. The immobilized lipase could be used up to 3 cycles of esterification reaction. Copyright © 2016 BCREC GROUP. All rights reserved</p><p><em>Received: 21<sup>st</sup> December 2015; Revised: 23<sup>rd</sup> February 2016; Accepted: 14<sup>th</sup> April 2016</em></p><p><strong>How to Cite</strong>: Hilmanto, H., Hidayat, C., Hastuti, P. (2016). Surface Modification of Macroporous Matrix for Immobilization of Lipase for Fructose Oleic Ester Synthesis. <em>Bulletin of Chemical Reaction Engineering &amp; Catalysis</em>, 11 (3): 339-345 (doi:10.9767/bcrec.11.3.573.339-345)</p><p><strong>Permalink/DOI:</strong> <a href="http://doi.org/10.9767/bcrec.11.3.573.339-345">http://doi.org/10.9767/bcrec.11.3.573.339-345</a></p>


2021 ◽  
Vol 1023 ◽  
pp. 111-118
Author(s):  
Jarernporn Thawornprasert ◽  
Wiriya Duangsuwan ◽  
Krit Somnuk

The objective of this research was to study the optimum condition of esterified oil production from low free fatty acid of mixed crude palm oil (LMCPO) by using a response surface methodology (RSM) with esterification reaction in a batch mode. LMCPO obtained from a vacuum refining process of mixed crude palm oil (MCPO) to extract the partial FFA in oil which was used as a raw materials in a food production. Therefore, remaining FFA of 6.170 wt.% in LMCPO should be reduced to less than 1 wt.% by using esterification when required these oils to use as feedstock for producing biodiesel. After esterification process, FFA in esterified oil was studied to optimize the four independent variables of methanol (5-25 vol.%), sulfuric acid (0.5-4.5 vol.%), reaction time (5-65 min) and speed of stirrer (100-500 rpm). The results showed that the optimal condition of 25 vol.% methanol, 2 vol.% sulfuric acid, 500 rpm speed of stirrer, and 30 min reaction time at 60°C reaction temperature can decreased the FFA level to less than 0.212 wt.%. However, it was found out that the high consumptions of methanol and sulfuric acid required for reducing FFA to lowest value. Thus, the selected condition of 17.4% methanol, 1.6% sulfuric acid, 300 rpm speed of stirrer, and 35 min reaction time was chosen to save the chemical contents because this condition achieved to reduce FFA to acceptable level of 1 wt.%. For the actual experiment, FFA can be decreased to 0.212 wt.%, and 1.028 wt.% respectively. The yields of 96.67 wt.% for crude esterified oil and 94.22 wt.% for pure esterified oil were achieved based on LMCPO under the selected condition.


Author(s):  
Syamsul Kamar Muhamad ◽  
Salina Mat Radzi ◽  
Siti Salhah Othman ◽  
Mohd Basyaruddin Abdul Rahman ◽  
Hanina Mohd Noor

The effects of important reaction parameters for enhancing flavour esters formation through lipase-catalyzed reaction were investigated in this study.Various commercial immobilized lipases were used to catalyze the esterification reaction between short-chain fatty acids and alcohols to produce flavour esters which are nonyl caprylate and ethyl valerate which differ in chain length of esters. These synthetic flavour esters with fruity notes are widely used in food, cosmetic and pharmaceutical industries. The effect of various reaction parameters was optimized to obtain a high yield of flavour esters. A maximum percentage for nonyl caprylate with conversion of flavour esters more than 90 % in a solvent-free system was successfully obtained under the following conditions: reaction time (RT), 5 hours; reaction temperature, 40 °C; amount of immobilized lipase, 25 % w/w of total substrate and shaking speed 200 rpm. Compared to ethyl valerate, a maximum percentage conversion of flavour ester more than 80 % in solvent free system was successfully obtained under following conditions: reaction time (RT), 45 minutes; reaction temperature, 40 °C; amount of immobilized lipase, 15 % w/w of total substrate and shaking speed 200 rpm. Comparison between these two ester showed that the chain length give an effect to optimize the reaction condition in esterification reaction.


2015 ◽  
Vol 9 (1) ◽  
pp. 19
Author(s):  
Nirwana ◽  
Irdoni HS ◽  
Joni Miharyono

Diversity of palm oil product in Indonesia is still limited, therefore it is needed to take an advantage of the development of downstream product of crude palm oil by esterification reaction. Esterification reaction is a reaction between carboxylic acid and alcohol to form ester. One of the emerging downstream product fatty acid alkyl ester is plasticizer. Plasticizer is an additive compound added to polymer to improve flexibility and workability. The purpose of this research was conducted to study the effect of reaction time and mole ratio and identify product of plasticizers isopropyl linoleic. In this research, plasticizer was synthesized by esterification of linoleic acid and isopropanol, using activated natural zeolite catalyst. The process was done with a variation of reaction time (4, 6, and 8 hours) and mole ratio (1: 6, 1: 9, and 1:12), with reaction temperature at  80 °C,  stirring speed at 200 rpm and 15% of composition of linoleic acid based catalyst as fixed variables. From the analysis of the results showed that the esterification reaction time and mole ratio affect the product conversion. The best operating condition obtained  in this research was 4 hours of reaction time and 1:12 of mole ratio which resulted the conversion of reaction was 67.09%. Characteristics of plasticizer produced from this research were viscosity (at 20 °C) 2.405 to 2.803 mPa.s and Specific Gravity (at 20 °C) from 0.863 to 0.872.


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