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<p>In this study, the transesterification of Palm Kernel Oil (PKO) with ethanol over an H<sub>2</sub>SO<sub>4</sub>-Itu clay catalyst was investigated. The clay sample was mined at Itu Akwa-Ibom state, Nigeria and PKO was sourced from a local dealer in Ogbomoso, Oyo State. Ethanol and the acid used are of analytical grade. Raw Itu Clay (RIC) was calcined, beneficiated, and modified with H<sub>2</sub>SO<sub>4</sub> to form Acid modified Itu Clay (AIC). RIC and AIC are characterized by Scanning Electron Microscope (SEM), Brunauer-Emmett-Teller (BET), Fourier Transform Infrared (FTIR) spectroscopy, X-ray fluorescence (XRF), and X-Ray Diffraction (XRD). In contrast, PKO and synthesized PKO Biodiesel (PKOB) are respectively characterized using physicochemical, FTIR, and GC-MS analysis. Definitive Screening Design (DSD) was used to optimize the transesterification of PKO with ethanol and AIC. The process parameters considered for the optimization study are agitation (100–400&#xa0;rpm), reaction time (1–3&#xa0;h), catalyst dosage (1–5 wt%), ethanol: oil molar ratio (6:1–12:1), and reaction temperature (45–65&#xa0;°C) while the responses are Yield of PKOB (YPKOB) and Density of PKOB (DPKOB) produced. The characterization results showed that the clay sample was calcium montmorillonite dominated with SiO<sub>2</sub>:Al<sub>2</sub>O<sub>3</sub>:CaO and AIC surface area, pore volume and pore sizes improved after acid modification. The result of optimization revealed that the highest yield of 96% was obtained with 1 wt% catalyst loading at 65&#xa0;°C, ethanol: oil molar ratio of 12:1, a reaction time of 2&#xa0;h, and agitation of 400&#xa0;rpm. The predicted values of fatty acid ethyl esters (FAEE) yield and DPKOB were found to agree with their observed values (R<sup>2</sup> = 0.9930 and Adj R<sup>2</sup> = 0.9719) and (R<sup>2</sup> = 0.9915 and Adj R<sup>2</sup> = 0.9688), respectively. These results revealed that the process parameters had a significant influence on the transesterification reaction. Hence, the H<sub>2</sub>SO<sub>4</sub>-Itu clay catalyst is a promising low-cost catalyst that possesses the great activity required for the transesterification of PKO. The future direction of this research is to determine the proof of concept and the feasibility study of the modified catalyst support.</p>

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Regression modelling and optimization study with risk assessment analysis of process parameters in the transesterification of palm kernel oil using acid modified Itu clay

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  • 发表日期：

    2025年12月16日

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  • Ibrahim A. Adekunle,
  • Kazeem. K. Salam,
  • Ebenezer O. Dada,
  • Taofiq O. Salawudeen,
  • Akeem O. Arinkoola

摘要

In this study, the transesterification of Palm Kernel Oil (PKO) with ethanol over an H2SO4-Itu clay catalyst was investigated. The clay sample was mined at Itu Akwa-Ibom state, Nigeria and PKO was sourced from a local dealer in Ogbomoso, Oyo State. Ethanol and the acid used are of analytical grade. Raw Itu Clay (RIC) was calcined, beneficiated, and modified with H2SO4 to form Acid modified Itu Clay (AIC). RIC and AIC are characterized by Scanning Electron Microscope (SEM), Brunauer-Emmett-Teller (BET), Fourier Transform Infrared (FTIR) spectroscopy, X-ray fluorescence (XRF), and X-Ray Diffraction (XRD). In contrast, PKO and synthesized PKO Biodiesel (PKOB) are respectively characterized using physicochemical, FTIR, and GC-MS analysis. Definitive Screening Design (DSD) was used to optimize the transesterification of PKO with ethanol and AIC. The process parameters considered for the optimization study are agitation (100–400 rpm), reaction time (1–3 h), catalyst dosage (1–5 wt%), ethanol: oil molar ratio (6:1–12:1), and reaction temperature (45–65 °C) while the responses are Yield of PKOB (YPKOB) and Density of PKOB (DPKOB) produced. The characterization results showed that the clay sample was calcium montmorillonite dominated with SiO2:Al2O3:CaO and AIC surface area, pore volume and pore sizes improved after acid modification. The result of optimization revealed that the highest yield of 96% was obtained with 1 wt% catalyst loading at 65 °C, ethanol: oil molar ratio of 12:1, a reaction time of 2 h, and agitation of 400 rpm. The predicted values of fatty acid ethyl esters (FAEE) yield and DPKOB were found to agree with their observed values (R2 = 0.9930 and Adj R2 = 0.9719) and (R2 = 0.9915 and Adj R2 = 0.9688), respectively. These results revealed that the process parameters had a significant influence on the transesterification reaction. Hence, the H2SO4-Itu clay catalyst is a promising low-cost catalyst that possesses the great activity required for the transesterification of PKO. The future direction of this research is to determine the proof of concept and the feasibility study of the modified catalyst support.