Optimisation of Free Fatty Acid Removal in Nyamplung Seed Oil (Callophyllum inophylum L.) using Response Surface Methodology Analysis

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.

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OPTIMIZATION OF TRANSESTERIFICATION OF TRA FAT WITH KOH/y Al2O3 CATALYST USING RESPONSE SURFACE METHODOLOGY

Science and Technology Development Journal ◽

10.32508/stdj.v12i13.2331 ◽

2009 ◽

Vol 12 (13) ◽

pp. 69-76

Author(s):

Huong Thi Thanh Le ◽

Tan Viet Le ◽

Tan Minh Phan ◽

Hoa Thi Viet Tran

Keyword(s):

Response Surface Methodology ◽

Reaction Time ◽

Response Surface ◽

Reaction Temperature ◽

Catalyst Concentration ◽

Molar Ratio ◽

Result Show ◽

Heterogenous Catalyst ◽

Central Composite ◽

Al2o3 Catalyst

In this study, biodiesel was produced from fat of tra catfish by methanolysis reaction with KOH/y-A12O3 heterogenous catalyst. This research was carried out using response surface methodology (RSM) based on four-variable central composite design (CCD) with a = 1,54671. The transesterification process variables and their investigated ranges were methanol/fat molar ratio (X1: 7/1 - 9/1), catalyst concentration (X2: 5%-7%), reaction time (X3: 60 min - 120 min), and reaction temperature (X4: 55 °C - 65 °C). The result show the biodiesel yield could be reach up to 92,8 % using the following optimized reaction condition: molar ratio of methanol/fat at 8,26/1, catalyst concentration of 5,79 %, reaction time of 96 min, and reaction temperature at 59,6 °C.

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Optimization of Enzymatic Synthesis of Betulinic Acid Amide in Organic Solvent by Response Surface Methodology (RSM)

Indonesian Journal of Chemistry ◽

10.22146/ijc.34903 ◽

2019 ◽

Vol 19 (4) ◽

pp. 849

Author(s):

Nurul Atikah Amin Yusof ◽

Nursyamsyila Mat Hadzir ◽

Siti Efliza Ashari ◽

Nor Suhaila Mohamad Hanapi ◽

Rossuriati Dol Hamid

Keyword(s):

Response Surface Methodology ◽

Reaction Time ◽

Response Surface ◽

Reaction Temperature ◽

Betulinic Acid ◽

Enzymatic Synthesis ◽

Acid Amide ◽

Molar Ratio ◽

Percentage Yield ◽

Substrate Molar Ratio

Optimization of the lipase catalyzed enzymatic synthesis of betulinic acid amide in the presence of immobilized lipase, Novozym 435 from Candida antartica as a biocatalyst was studied. Response surface methodology (RSM) and 5-level-4-factor central-composite rotatable design (CCRD) were employed to evaluate the effects of the synthesis parameters, such as reaction time (20–36 h), reaction temperature (37–45 °C), substrate molar ratio of betulinic acid to butylamine (1:1–1:3), and enzyme amounts (80–120 mg) on the percentage yield of betulinic acid amide by direct amidation reaction. The optimum conditions for synthesis were: reaction time of 28 h 33 min, reaction temperature of 42.92 °C, substrate molar ratio of 1:2.21, and enzyme amount of 97.77 mg. The percentage yield of actual experimental values obtained 65.09% which compared well with the maximum predicted value of 67.23%. The obtained amide was characterized by GC, GCMS and 13C NMR. Betulinic acid amide (BAA) showed a better cytotoxicity compared to betulinic acid as the concentration inhibited 50% of the cell growth (IC50) against MDA-MB-231 cell line (IC50 < 30 µg/mL).

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Response Surface Methodology for Biodiesel Production Using Calcium Methoxide Catalyst Assisted with Tetrahydrofuran as Cosolvent

Journal of Chemistry ◽

10.1155/2017/4190818 ◽

2017 ◽

Vol 2017 ◽

pp. 1-9 ◽

Cited By ~ 9

Author(s):

Nichaonn Chumuang ◽

Vittaya Punsuvon

Keyword(s):

Response Surface Methodology ◽

Reaction Time ◽

Response Surface ◽

Catalyst Concentration ◽

Acid Methyl Ester ◽

Waste Cooking Oil ◽

Biodiesel Production ◽

Quadratic Model ◽

Molar Ratio ◽

Standard Requirement

The present study was performed to optimize a heterogeneous calcium methoxide (Ca(OCH3)2) catalyzed transesterification process assisted with tetrahydrofuran (THF) as a cosolvent for biodiesel production from waste cooking oil. Response surface methodology (RSM) with a 5-level-4-factor central composite design was applied to investigate the effect of experimental factors on the percentage of fatty acid methyl ester (FAME) conversion. A quadratic model with an analysis of variance obtained from the RSM is suggested for the prediction of FAME conversion and reveals that 99.43% of the observed variation is explained by the model. The optimum conditions obtained from the RSM were 2.83 wt% of catalyst concentration, 11.6 : 1 methanol-to-oil molar ratio, 100.14 min of reaction time, and 8.65% v/v of THF in methanol concentration. Under these conditions, the properties of the produced biodiesel satisfied the standard requirement. THF as cosolvent successfully decreased the catalyst concentration, methanol-to-oil molar ratio, and reaction time when compared with biodiesel production without cosolvent. The results are encouraging for the application of Ca(OCH3)2 assisted with THF as a cosolvent for environmentally friendly and sustainable biodiesel production.

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Optimisation of Second-Generation Biodiesel Production from Australian Native Stone Fruit Oil Using Response Surface Method

Energies ◽

10.3390/en11102566 ◽

2018 ◽

Vol 11 (10) ◽

pp. 2566 ◽

Cited By ~ 31

Author(s):

Mohammad Anwar ◽

Mohammad Rasul ◽

Nanjappa Ashwath ◽

Md Rahman

Keyword(s):

Response Surface Methodology ◽

Response Surface ◽

Reaction Temperature ◽

Second Generation ◽

Catalyst Concentration ◽

Biodiesel Production ◽

Stone Fruit ◽

Quadratic Model ◽

Molar Ratio ◽

Contour Plots

In this study, the production process of second-generation biodiesel from Australian native stone fruit have been optimised using response surface methodology via an alkali catalysed transesterification process. This process optimisation was performed varying three factors, each at three different levels. Methanol: oil molar ratio, catalyst concentration (wt %) and reaction temperature were the input factors in the optimisation process, while biodiesel yield was the key model output. Both 3D surface plots and 2D contour plots were developed using MINITAB 18 to predict optimum biodiesel yield. Gas chromatography (GC) and Fourier transform infrared (FTIR) analysis of the resulting biodiesel was also done for biodiesel characterisation. To predict biodiesel yield a quadratic model was created and it showed an R2 of 0.98 indicating the satisfactory performance of the model. Maximum biodiesel yield of 95.8% was obtained at a methanol: oil molar ratio of 6:1, KOH catalyst concentration of 0.5 wt % and a reaction temperature of 55 °C. At these reaction conditions, the predicted biodiesel yield was 95.9%. These results demonstrate reliable prediction of the transesterification process by Response surface methodology (RSM). The results also show that the properties of the synthesised Australian native stone fruit biodiesel satisfactorily meet the ASTM D6751 and EN14214 standards. In addition, the fuel properties of Australian native stone fruit biodiesel were found to be similar to those of conventional diesel fuel. Thus, it can be said that Australian native stone fruit seed oil could be used as a potential second-generation biodiesel source as well as an alternative fuel in diesel engines.

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Application of Response Surface Methodology for Optimization of Biodiesel Production from Microalgae Through Nanocatalytic Transesterification Process.

10.21203/rs.3.rs-771200/v1 ◽

2021 ◽

Author(s):

Vaishali Mittal ◽

Uttam Kumar Ghosh

Keyword(s):

Response Surface Methodology ◽

Reaction Time ◽

Response Surface ◽

Process Parameters ◽

Reaction Temperature ◽

Methyl Esters ◽

Biodiesel Production ◽

Molar Ratio ◽

Impregnation Method ◽

The Impact

Abstract Production of biodiesel from microalgae is gaining popularity since it does not compromise food security or the global economy. This article reports biodiesel production with Spirulina microalgae through nanocatalytic transesterification process. The nanocatalyst calcium methoxide Ca(OCH3)2 was synthesized using wet impregnation method and utilized to carry out the transesterification process. The nanocatalyst was characterized to evaluate its structural and spectral characteristics using different characterization techniques such as Thermogravimetric analysis (TGA), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and Brunaeur-Emmett-Teller(BET) measurement for surface area. The result demonstrates that calcium methoxide Ca(OCH3)2 possesses a high catalytic activity compared to a heterogeneous catalyst such as calcium oxide (CaO). The impact of several process parameters such as reaction temperature, the molar ratio of methanol to oil, catalyst concentration, and reaction time used in the transesterification process was optimized by employing central composite design(CCD) based response surface methodology(RSM). The polynomial regression equation of second order was obtained for methyl esters. The model projected a 99% fatty acid methyl esters (FAME) yield for optimal process parameters of reaction time 3hrs,3 wt.% of Ca(OCH3)2 catalyst loading, 80°C reaction temperature, and 30:1 methanol to oil molar ratio.

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Optimization and Kinetic Study of Biodiesel Production from Diseased Swine Carcasses

Journal of Biobased Materials and Bioenergy ◽

10.1166/jbmb.2019.1883 ◽

2019 ◽

Vol 13 (4) ◽

pp. 464-474 ◽

Cited By ~ 1

Author(s):

Youzhou Jiao ◽

Yahe Mei ◽

Le Wang ◽

Jiaao Liu ◽

Zhiping Zhang ◽

...

Keyword(s):

Reaction Time ◽

Kinetic Analysis ◽

Reaction Temperature ◽

Catalyst Concentration ◽

3D Ultrasound ◽

Biodiesel Production ◽

Molar Ratio ◽

Esterification Reaction ◽

Control Group ◽

Ultrasound Group

The innocuous utilization of diseased swine carcasses is a key issue in reducing environmental pollution and ensuring safety in animal husbandry. In this study, by using fat from diseased swine carcasses as raw materials, response surface experiments were conducted to investigate the influences of reaction time, catalyst concentration, reaction temperature, and methanol/oil molar ratio on the biodiesel purity and the optimum conditions for biodiesel production were determined. Furthermore, three-dimensional (3D) ultrasound assistance was adopted and kinetic analysis was performed. The results show that the influencing factors on biodiesel purity, in descending order, were determined to be reaction temperature > catalyst concentration > reaction time > methanol/oil molar ratio. Moreover, the maximum biodiesel purity was 93.7% under the following optimal conditions: catalyst concentration of 5.0 wt%; reaction temperature of 68 °C; methanol/oil molar ratio of 10:1; reaction time of 37 h. When 3D ultrasound assistance was adopted, the maximum biodiesel purity of 98.1% was obtained for the reaction process of 8 h under the ultrasound power and frequency of 500 W and 20 kHz, respectively. And the esterification reaction time was significantly reduced, compared to without ultrasound assistance. The results of kinetic analysis demonstrate that the reaction rate constants of the ultrasound group were 4.45–5.52 times greater than that of the control group. And the activation energy for the ultrasound group was 25.58 kJ/mol, which is 22.81% lower than that of the control group. This study will help to conduct large-batch biodiesel production from diseased swine carcasses in the future.

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POTENSI KATALIS PADAT ASAM GAMMA ALUMINA TERSULFATASI PADA REAKSI ESTERIFIKASI MINYAK BIJI KARET

REAKTOR ◽

10.14710/reaktor.16.3.109-115 ◽

2016 ◽

Vol 16 (3) ◽

pp. 109 ◽

Cited By ~ 2

Author(s):

Maria Ulfah ◽

S Subagjo

Keyword(s):

Fatty Acid ◽

Free Fatty Acid ◽

Optimum Condition ◽

Seed Oil ◽

Catalyst Concentration ◽

Volume Ratio ◽

Esterification Reaction ◽

Rubber Seed Oil ◽

Rubber Seed ◽

Time Of Reaction

POTENTIAL OF SULFATET ALUMINA-HETEROGENEOUS ACID CATALYST IN ESTERIFICATION RUBBER SEED OIL. Two tipe of catalysts have been synthesed and evaluated ( free fatty acid conversion) in esterification of rubber seed oil. The first and the second catalyst have content SO3 8,821 % and 40,715 %, respectly. The optimum condition of reaction studied : volume ratio methanol/oil 0,9-1,8 v/v; catalyst concentration 1,67-10 % wt/v; time of reaction 1-7 hours and temperature of reaction 50-70 oC. This study showed, the second catalyst more active than the first catalyst. Maximum conversion from esterification reaction of rubber seed oil of the first and the second catalyst are 75 % and 97 %, respectly. The optimum condition of reaction achieved at volume ratio methanol/oil 1,8 v/v; catalyst concentration 1,67 % wt/v; time of reaction 7 hours and temperature of reaction 70 oC. Keywords: sulfated alumina, free fatty acid, eterification, rubber seed oil.AbstrakDua tipe katalis alumina tersulfatasi telah disintesis dan dievaluasi kinerjanya (berupa konversi Asam Lemak Bebas, ALB) pada reaksi esterifikasi asam lemak bebas minyak biji karet. Katalis tipe 1 dan tipe 2 berturut-turut memiliki kandungan SO3 8,821 % dan 40,715 %. Kondisi optimasi reaksi yang dipelajari: rasio volume metanol/minyak 0,9-1,8 v/v; konsentrasi katalis 1,67-10 % b/v; waktu reaksi 1-7 jam dan temperatur reaksi 50-70 oC. Hasil penelitian menunjukkan katalis tipe 2 lebih aktif dari tipe 1. Konversi ALB maksimum dari reaksi esterifikasi minyak biji karet dengan katalis tipe 1 dan tipe 2 berturut-turut 75 % dan 97 %. Kondisi optimum reaksi tersebut dicapai pada rasio volume metanol/minyak 1,8; konsentrasi katalis/minyak 1,67 % b/v; lama reaksi 7 jam dan temperatur reaksi 70 oC. Kata kunci: alumina tersulfatasi, asam lemak bebas, esterifikasi, minyak biji karet

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Saponification ofJatropha curcasSeed Oil: Optimization by D-Optimal Design

International Journal of Chemical Engineering ◽

10.1155/2012/574780 ◽

2012 ◽

Vol 2012 ◽

pp. 1-6 ◽

Cited By ~ 4

Author(s):

Jumat Salimon ◽

Bashar Mudhaffar Abdullah ◽

Nadia Salih

Keyword(s):

Fatty Acid ◽

Reaction Time ◽

Free Fatty Acid ◽

Experimental Design ◽

Optimal Design ◽

Optimum Condition ◽

Reaction Temperature ◽

Seed Oil ◽

Significant Variable ◽

Optimum Conditions

In this study, the effects of ethanolic KOH concentration, reaction temperature, and reaction time to free fatty acid (FFA) percentage were investigated. D-optimal design was employed to study significance of these factors and optimum condition for the technique predicted and evaluated. The optimum conditions for maximum FFA% were achieved when 1.75 M ethanolic KOH concentration was used as the catalyst, reaction temperature of65°C,and reaction time of 2.0 h. This study showed that ethanolic KOH concentration was significant variable for saponification ofJ. curcasseed oil. In an 18-point experimental design, percentage of FFA for saponification ofJ. curcasseed oil can be raised from 1.89% to 102.2%.

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Study on Preparation of Biodiesel with Monomer Acid

Applied Mechanics and Materials ◽

10.4028/www.scientific.net/amm.521.72 ◽

2014 ◽

Vol 521 ◽

pp. 72-75

Author(s):

Xiao Feng Liu

Keyword(s):

Reaction Time ◽

Reaction Temperature ◽

Catalyst Concentration ◽

Diesel Oil ◽

Molar Ratio ◽

Esterification Reaction ◽

Optimum Conditions ◽

Toluenesulfonic Acid ◽

Acid Reaction ◽

Single Factor Experiment

An esterification reaction of monomer acid with methanol using p-toluenesulfonic acid as catalyst for the preparation of biodiesel was studied. The process variables that influence the esterification of monomer acid, such as catalyst concentration, molar ratio of methanol to acid, reaction time and reaction temperature, were investigated and optimized. Through the single factor experiment, the optimum conditions obtained for the esterification were molar ratio of methanol to acid 3:1, usage amount of p-toluenesulfonic acid 6% and reaction time 3h, reaction temperature 70°C.The produced biodiesel was found to exhibit fuel properties within the limits prescribed by the latest American Standards for Testing Material (ASTM) and 0#diesel oil.

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Mathematical Modeling and Optimization Studies by Artificial Neural Network, Genetic Algorithm and Response Surface Methodology: A Case of Ferric Sulfate–Catalyzed Esterification of Neem (Azadirachta indica) Seed Oil

Frontiers in Energy Research ◽

10.3389/fenrg.2020.614621 ◽

2020 ◽

Vol 8 ◽

Author(s):

Kelechi E. Okpalaeke ◽

Taiwo H. Ibrahim ◽

Lekan M. Latinwo ◽

Eriola Betiku

Keyword(s):

Neural Network ◽

Genetic Algorithm ◽

Artificial Neural Network ◽

Response Surface Methodology ◽

Reaction Time ◽

Response Surface ◽

Seed Oil ◽

Ferric Sulfate ◽

Molar Ratio ◽

Modeling And Optimization

High free fatty acids (FFA) content in oils poses challenges such as soap formation and difficulty in the separation of by-products in direct transesterification of oil to biodiesel, which is of environmental concern and also increases the cost of production. Thus, in this study, the ferric sulfate-catalyzed esterification of neem seed oil (NSO) with an FFA of 5.84% was investigated to reduce it to the recommended level of ≤1%. The esterification process for the NSO was modeled using response surface methodology (RSM) and artificial neural network (ANN). The effect of the pertinent process input variables viz. methanol/NSO molar ratio (10:1–30:1), ferric sulfate dosage (2–6 wt%), and reaction time (30–90 min) and their interactions on the reduction of the FFA of the NSO, were examined using Box Behnken design. The optimal condition for the process for reducing the FFA content of the oil was established using RSM and ANN-genetic algorithm (ANN-GA). The results showed that the models developed described the process accurately with the coefficient of determination (R2) of 0.9656 and 0.9908 and the mean relative percent deviation (MRPD) of 6.5 and 2.9% for RSM and ANN, respectively. The ANN-GA established the optimum reduction of FFA of 0.58% with methanol/NSO molar ratio of 18.51, ferric sulfate dosage of 6 wt%, and reaction time of 62.8 min as against the corresponding values of 0.62% FFA, 23.5, 5.03, and 75 min established by the RSM. Based on the statistics considered in the study, ANN and GA outperformed RSM in modeling and optimization of the NSO esterification process.

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