scholarly journals Determination of Free Fatty Acid by FT-NIR Spectroscopy in Esterification Reaction for Biodiesel Production

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Djéssica Tatiana Raspe ◽  
Camila da Silva
Keyword(s):  
Oleic Acid ◽  
Soybean Oil ◽  
Multivariate Calibration ◽  
Reaction Medium ◽  
Reference Method ◽  
Nir Spectroscopy ◽  
Biodiesel Production ◽  
Esterification Reaction ◽  
Experimental Conditions ◽  
Batch Mode

This work reports the use of FT-NIR spectroscopy coupled with multivariate calibration to determine the percentage of free fatty acids (FFA) in samples obtained by the esterification of FFA in vegetable oils. The analytical method used as calibration matrix samples of the reaction medium of esterification of oleic acid in soybean oil in proportions of 0.3 to 40 wt% (by weight) of oleic acid obtained under different experimental conditions and utilized the partial least squares (PLS) regression. The efficiency of the method was tested to predict the content of FFA in reactions of esterification of oleic acid in soybean oil catalysed by KSF clay and Amberlyst 15 commercial resin, both in a batch mode. Good Correlations were observed between the FT-NIR/PLS method and the reference method (AOCS). The results confirm that FT-NIR spectroscopy, in combination with multivariate calibration, is a promising technique for monitoring esterification reaction for biodiesel production.

scholarly journals DETERMINAÇÃO DE ÉSTERES ETÍLICOS DE ÁCIDOS GRAXOS POR ESPECTROSCOPIA FT-NIR E CALIBRAÇÃO MULTIVARIADA EM REAÇÕES DE TRANSESTERIFICAÇÃO

e-xacta ◽  
2013 ◽  
Vol 6 (1) ◽  
pp. 27 ◽  
Author(s):  
Djéssica Tatiane Raspe ◽  
Vitor Augusto Garcia ◽  
Camila Da Silva
Keyword(s):  
Soybean Oil ◽  
Multivariate Calibration ◽  
Reference Method ◽  
Nir Spectroscopy ◽  
Predictive Ability ◽  
Ethyl Esters ◽  
Biodiesel Production ◽  
Molar Ratio ◽  
Calibration And Validation ◽  
Flame Ionization

<p align="justify">O presente trabalho teve como objetivo estimar a O presente trabalho teve como objetivo estimar a concentração de ésteres etílicos de ácidos graxos (EEAG) em amostras da alcoólise de óleo de soja pela aplicação da espectroscopia FT-NIR associada à calibração multivariada. A amostra estudada foi obtida utilizando hidróxido de sódio como catalisador, em diferentes condições reacionais (temperatura, razão molar óleo, etanol, percentual de catalisador e tempo de reação), com o objetivo de obter amostras em diferentes concentrações de EEAG, a serem utilizadas nas etapas de calibração e validação da metodologia. Este trabalho utilizou a cromatografia gasosa com detector de ionização de chama (CG/DIC) como metodologia de referência e o método de mínimos quadrados parciais (PLS) no tratamento quimiométrico dos dados. Reporta uma alta correlação (r&gt;0,99) entre os dados obtidos pelo método FT-NIR/PLS e reportados pelo método CG/DIC. O modelo quimiométrico desenvolvido apresentou erro médio quadrático de 2,11 e 3,26 para as etapas de calibração e validação da metodologia. Além disso a capacidade de predição da metodologia FT-NIR/PLS foi testada com grupo independente de amostras, obtidas da alcoólise de óleo de soja. Os resultados obtidos demonstram que o método proposto apresenta-se como uma promissora técnica para avaliar o rendimento de reações de alcoólise de óleos vegetais, o que possibilitará o monitoramento de reações para produção de biodiesel.</p><p align="justify">Abstract</p><p align="justify">This study aimed to estimate the concentration of fatty acid ethyl esters (FAEE) in samples from the alcoholysis of soybean oil using FT-NIR spectroscopy associated with multivariate calibration. The samples were obtained using sodium hydroxide as a catalyst at different reaction conditions (temperature, molar ratio oil:ethanol percentage of catalyst and reaction time), in order to obtain samples at different concentrations of FAEE, to be used in steps calibration and validation of the methodology. Gas chromatography with flame ionization detector (GC / FID) was used as the reference method and the method of partial least squares (PLS) used for treatment of chemometric data. It was reported a high correlation (r&gt; 0.99) between the data obtained by the method reported by FT-NIR/PLS and method GC / FID. The chemometric model developed showed mean square error of 2.11 and 3.26 for the steps of calibration and validation of the methodology. The predictive ability of the FT-NIR/PLS method was tested with independent group of samples obtained from the alcoholysis of soybean oil. The results show that the proposed method is presented as a promising technique for evaluating the performance of reactions of alcoholysis of vegetable oils, which will allow the monitoring of reactions for biodiesel production.</p>

scholarly journals Study of Soybean Oil Hydrolysis Catalyzed by Thermomyces lanuginosus Lipase and Its Application to Biodiesel Production via Hydroesterification

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
Keyword(s):  
Soybean Oil ◽  
Methyl Esters ◽  
Reaction Medium ◽  
Acid Catalyst ◽  
Biodiesel Production ◽  
Thermomyces Lanuginosus ◽  
Molar Ratio ◽  
Esterification Reaction ◽  
Thermomyces Lanuginosus Lipase ◽  
Niobic Acid

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.

scholarly journals Biodiesel Synthesis Monitoring using Near Infrared Spectroscopy

2018 ◽  
Vol 12 (1) ◽  
pp. 95-110 ◽  
Author(s):  
Estela Kamile Gelinski ◽  
Fabiane Hamerski ◽  
Marcos Lúcio Corazza ◽  
Alexandre Ferreira Santos
Keyword(s):  
Fossil Fuels ◽  
Near Infrared ◽  
Reference Method ◽  
Nir Spectroscopy ◽  
Transesterification Reaction ◽  
Biodiesel Production ◽  
Molar Ratios ◽  
External Data ◽  
Biodiesel Synthesis ◽  
Biodiesel Production Monitoring

Objective: Biodiesel is a renewable fuel considered as the main substitute for fossil fuels. Its industrial production is mainly made by the transesterification reaction. In most processes, information on the production of biodiesel is essentially done by off-line measurements. Methods: However, for the purpose of control, where online monitoring of biodiesel conversion is required, this is not a satisfactory approach. An alternative technique to the online quantification of conversion is the near infrared (NIR) spectroscopy, which is fast and accurate. In this work, models for biodiesel reactions monitoring using NIR spectroscopy were developed based on the ester content during alkali-catalyzed transesterification reaction between soybean oil and ethanol. Gas chromatography with flame ionization detection was employed as the reference method for quantification. FT-NIR spectra were acquired with a transflectance probe. The models were developed using Partial Least Squares (PLS) regression with synthetic samples at room temperature simulating reaction composition for different ethanol to oil molar ratios and conversions. Model predictions were then validated online for reactions performed with ethanol to oil molar ratios of 6 and 9 at 55ºC. Standard errors of prediction of external data were equal to 3.12%, hence close to the experimental error of the reference technique (2.78%), showing that even without using data from a monitored reaction to perform calibration, proper on-line predictions were provided during transesterification runs. Results: Additionally, it is shown that PLS models and NIR spectra of few samples can be combined to accurately predict the glycerol contents of the medium, making the NIR spectroscopy a powerful tool for biodiesel production monitoring.

Preparation of the F−-SO42-/MWCNTs catalyst and kinetic studies of the biodiesel production via esterification reaction of oleic acid and methanol

2019 ◽  
Vol 135 ◽  
pp. 836-845 ◽  
Author(s):  
Qing Shu ◽  
Wenqiang Zou ◽  
Jiangfan He ◽  
Herry Lesmana ◽  
Caixia Zhang ◽  
...  
Keyword(s):  
Oleic Acid ◽  
Kinetic Studies ◽  
Biodiesel Production ◽  
Esterification Reaction

scholarly journals Application of a Multienzymatic System from Natural Latex in Key Reactions for oil-Based Biorefineries

Fermentation ◽  
2019 ◽  
Vol 5 (1) ◽  
pp. 18
Author(s):  
Daniel Sánchez ◽  
Susana Morcelle ◽  
María Fait ◽  
Gabriela Tonetto ◽  
María Ferreira
Keyword(s):  
Oleic Acid ◽  
Soybean Oil ◽  
Crucial Role ◽  
Esterification Reaction ◽  
Platform Chemicals ◽  
Excellent Activity ◽  
Comparable Activity ◽  
Biotechnological Processes ◽  
Hydrolysis Of

Oil-based biorefineries play a crucial role in the production of key platform chemicals that can be generated via biotechnological processes instead of a petrochemical route. This work focuses on the latex of the fruit of Araujia sericifera, which can be considered a multienzymatic system with applications in key reactions in oil-based biorefineries. The latex of Araujia sericifera (ASL) was used as a novel biocatalyst in the esterification of oleic acid and in the hydrolysis of triglycerides and p-nitrophenyl carboxylates. When ASL was compared to a commercial biocatalyst, it showed an excellent activity in the hydrolysis of soybean oil and p-nitropheyl laurate, and a comparable activity in the esterification reaction.

scholarly journals Kinetic Study on the CsXH3−XPW12O40/Fe-SiO2Nanocatalyst for Biodiesel Production

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Mostafa Feyzi ◽  
Leila Norouzi ◽  
Hamid Reza Rafiee
Keyword(s):  
Kinetic Study ◽  
Biodiesel Production ◽  
Molar Ratio ◽  
Esterification Reaction ◽  
Gravimetric Analysis ◽  
Time Data ◽  
Scanning Calorimetry ◽  
Experimental Conditions ◽  
Heterogeneous Catalytic ◽  
Operation Conditions

The kinetic of the transesterification reaction over theCsXH3−XPW12O40/Fe-SiO2catalyst prepared using sol-gel and impregnation procedures was investigated in different operational conditions. Experimental conditions were varied as follows: reaction temperature 323–333 K, methanol/oil molar ratio = 12/1, and the reaction time 0–240 min. The H3PW12O40heteropolyacid has recently attracted significant attention due to its potential for application in the production of biodiesel, in either homogeneous or heterogeneous catalytic conditions. Although fatty acids esterification reaction has been known for some time, data is still scarce regarding kinetic and thermodynamic parameters, especially when catalyzed by nonconventional compounds such as H3PW12O40. Herein, a kinetic study utilizing Gc-Mas in situ allows for evaluating the effects of operation conditions on reaction rate and determining the activation energy along with thermodynamic constants includingΔG,ΔS, andΔH. It indicated that theCsXH3−XPW12O40/Fe-SiO2magnetic nanocatalyst can be easily recycled with a little loss by magnetic field and can maintain higher catalytic activity and higher recovery even after being used 5 times. Characterization of catalyst was carried out by using scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), N2adsorption-desorption measurements methods, thermal gravimetric analysis (TGA), and differential scanning calorimetry (DSC).

Synthesis and Characterization of Different Transition Metal-Alginate Based Heterogeneous Catalyst for Esterification Reaction

2016 ◽  
Vol 709 ◽  
pp. 57-60
Author(s):  
Fei Ling Pua ◽  
Kah Thong Looi ◽  
Shamala Gowri Krishnan ◽  
Sharifah Nabihah
Keyword(s):  
Fatty Acids ◽  
Oleic Acid ◽  
Transition Metal ◽  
Free Fatty Acids ◽  
Heterogeneous Catalyst ◽  
Heterogeneous Catalysts ◽  
Biodiesel Production ◽  
Esterification Reaction ◽  
Homogeneous Catalyst

In recent years, attention has been drawn to produce heterogeneous catalyst to replace homogeneous catalyst in biodiesel industry. This study was focused on the synthesis of three different types of alginate based heterogeneous catalyst (Ferric-alginate, Copper-alginate, and Nickel alginate) and the effect of the catalyst on esterification of oleic acid. Morphology and elemental analysis was conducted to investigate the properties of the catalyst. The new heterogeneous catalysts were used to catalyze the esterification of oleic acid at reaction temperature of 60°C and 2 hours reaction time. Fe-alginate has achieved the highest free fatty acids (FFAs) conversation rate of 82.03%. The results and findings proved that transition metal-alginate heterogeneous catalyst has the potential and ability to esterify the free fatty acids prior biodiesel production from high free fatty acids feedstock.

scholarly journals Comparative Study on the Catalytic Performance of a 13X Zeolite and its Dealuminated Derivative for Biodiesel Production

2021 ◽  
Vol 16 (4) ◽  
pp. 763-772
Author(s):  
Balqees A. Alshahidy ◽  
Ammar S. Abbas
Keyword(s):  
Oleic Acid ◽  
Batch Reactor ◽  
Acid Leaching ◽  
Catalytic Performance ◽  
Zeolite Catalysts ◽  
Biodiesel Production ◽  
Esterification Reaction ◽  
X Ray ◽  
13X Zeolite ◽  
Esterification Reactions

Natural kaolin clay was used to successfully prepare 13X zeolite catalysts, which were modified by dealumination with citric acid. Acid leaching eliminates impurities and aluminum, and improves the Si/Al ratio of the zeolite framework. The X-ray diffraction (XRD) patterns of both the original and modified 13X zeolites were the same, indicating that the crystalline frameworks were not destroyed during the dealumination process. X-ray fluorescence data of the dealuminated 13X zeolite showed an improved Si/Al ratio. Also, Atomic Force Microscopy (AFM) was used for the characterization of the catalysts. The catalytic performance of the original and modified catalysts was tested in the esterification reaction of oleic acid in a batch reactor. A higher conversion of oleic acid was obtained using the modified 13X zeolite. The resulting experimental data from the esterification reactions were fitted to the heterogeneous Langmuir-Hinshelwood-Hougen-Watson (LHHW) kinetic model to determine the rates of reaction. The results of the reaction kinetics showed an increase in the rate of reaction velocity and a distinct decrease in the activation energy when using the modified zeolite, indicating that employing the modified catalyst will give a higher conversion over a shorter time through a reaction with less sensitivity to temperature. 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). 

scholarly journals MACROALGAE Fucus vesiculosus OIL: BIODIESEL PRODUCTION USING ALKALINE TRANSESTERIFICATION

Química Nova ◽  
2021 ◽  
Author(s):  
Bruno Petry ◽  
Rafael Rial ◽  
Osmar Freitas ◽  
Joyce Barbosa ◽  
Leandro Cavalheiro ◽  
...  
Keyword(s):  
Fatty Acids ◽  
Oleic Acid ◽  
Linoleic Acid ◽  
Soybean Oil ◽  
Oxidative Stability ◽  
Unsaturated Fatty Acids ◽  
Fucus Vesiculosus ◽  
Raw Material ◽  
Biodiesel Production ◽  
Alkaline Catalyst

This work studied the obtaining of methyl biodiesel and ethyl biodiesel using alkaline transesterification from macroalgae Fucus vesiculosos oil (FVO). FVO has 86.59% of its composition in unsaturated fatty acids, with a greater quantity of linoleic acid and oleic acid, a chemical composition near the soybean oil, the most used raw material for the production of biodiesel. Linoleic acid (47.88%), and oleic acid (34.66%) are the fatty acids present in the greatest amount in FVO, and unsaturated fatty acids correspond to 86.59% the composition of FVO, a composition of fatty acids close to that of soybean oil, which is the oil most produced and used for the production of biodiesel. To obtain methyl biodiesel (MBFVO) and ethyl biodiesel (EBFVO) the molar ratio oil: alcohol 1: 3 and 1% alkaline catalyst, NaOH, was used. The yield of the transesterification reaction was evaluated by varying the reaction time between 30 and 60 minutes and the highest yields were obtained after 60 minutes of reaction. In order to check the quality of the obtained biodiesel, the properties acidity index, iodine value, water content, specific mass at 20 o C, oxidative stability, cold filter lugging point and kinematic viscosity were evaluated. The oxidative stability had an induction period below the recommended, but it can be corrected with the addition of antioxidants to the biodiesel. All other physical and chemical properties had values within the stipulated by the regulatory agencies, indicating that the macroalgae Fucus vesiculosus can be a raw material in potential for production of biodiesel

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