Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts

Environmental concerns in fossil fuel depletion intensified the search for alternative fuel from renewable resources. Biodiesel is commonly produced by transesterification of vegetable oil in the presence of homogeneous catalyst. These catalysts, however, dissolve into the vegetable oil and large am...

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Main Author:	Sulaiman, Nur Fatin
Format:	Thesis
Language:	English
Published:	2018
Subjects:	TA Engineering (General) Civil engineering (General)
Online Access:	http://eprints.utm.my/id/eprint/81490/1/NurFatinSulaimanPFS2018.pdf
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spelling	my-utm-ep.814902019-08-23T05:21:53Z Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts 2018 Sulaiman, Nur Fatin TA Engineering (General). Civil engineering (General) Environmental concerns in fossil fuel depletion intensified the search for alternative fuel from renewable resources. Biodiesel is commonly produced by transesterification of vegetable oil in the presence of homogeneous catalyst. These catalysts, however, dissolve into the vegetable oil and large amount of water is required to clean the biodiesel that can cause saponification. Previously, extensive studies have been conducted on alkaline earth metal oxides such as calcium and magnesium oxides with manganese, iron, zirconium and cerium as the dopants. This research thus focused on the use of heterogeneous base catalysts that are easily separated and environmentally friendly for the biodiesel production. Zinc and calcium oxides-based supported on alumina were used as catalysts for the transesterification reaction of refined used cooking oil due to their highly basic characteristic. In order to improve the catalytic activity, the bimetallic and trimetallic oxides catalysts with copper, nickel, chromium and titanium as their co-catalysts were investigated. All the alumina supported catalysts were prepared by wetness impregnation method. The screening of biodiesel production using synthesized catalysts was monitored by gas chromatography-flame ionization detector (GC-FID). The two most potential catalysts were selected for the optimization and characterization study. Cu/Zn/?-Al2O3 catalyst calcined at 800°C with 10:90 wt.% dopant ratio to based and 3 times of alumina coating, exhibited the highest biodiesel production (89.50%) at mild reaction conditions (65°C, 10 wt.% catalyst loading, 1:20 oil:methanol mole ratio and 2 hours of reaction time). Cr/Ca/?-Al2O3 catalyst calcined at 700°C with 10:90 wt.% dopant ratio to based and 3 times number of alumina coating gave 86.64% of biodiesel production at 65°C, 6 wt.% catalyst loading, 1:18 oil:methanol mole ratio and 3 hours of reaction time. The physicochemical properties of the potential catalysts were accomplished using nitrogen analysis (NA) and CO2-temperature programmed desorption (CO2-TPD) that indicated high surface area (>140 m2/g) and high basicity (>3 mmol/g). X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) analysis showed the polycrystalline structure with small particles sizes (<50 nm). Energy dispersive X-ray (EDX) spectroscopy, X-ray fluorescence (XRF), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) analyses confirmed the existence of Al, O, Zn, Cu, Ca and Cr species in each potential catalyst. The optimization of catalyst preparation conditions and biodiesel production parameters were verified by response surface methodology (RSM) method and they were in good agreement with the experimental values. The mechanistic study on both potential catalysts follows the Langmuir- Hinshelwood (LH) model which involves the initial adsorption of reactants molecules on active sites of the catalyst surface. The specification analysis of produced biodiesel utilizing Cu/Zn/?-Al2O3 and Cr/Ca/?-Al2O3 catalysts showed that the refined used cooking oil has potential to be used in large-scale biodiesel production using reaction conditions found in the present study. 2018 Thesis http://eprints.utm.my/id/eprint/81490/ http://eprints.utm.my/id/eprint/81490/1/NurFatinSulaimanPFS2018.pdf application/pdf en public http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:125091 phd doctoral Universiti Teknologi Malaysia Chemistry
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	TA Engineering (General) Civil engineering (General)
spellingShingle	TA Engineering (General) Civil engineering (General) Sulaiman, Nur Fatin Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
description	Environmental concerns in fossil fuel depletion intensified the search for alternative fuel from renewable resources. Biodiesel is commonly produced by transesterification of vegetable oil in the presence of homogeneous catalyst. These catalysts, however, dissolve into the vegetable oil and large amount of water is required to clean the biodiesel that can cause saponification. Previously, extensive studies have been conducted on alkaline earth metal oxides such as calcium and magnesium oxides with manganese, iron, zirconium and cerium as the dopants. This research thus focused on the use of heterogeneous base catalysts that are easily separated and environmentally friendly for the biodiesel production. Zinc and calcium oxides-based supported on alumina were used as catalysts for the transesterification reaction of refined used cooking oil due to their highly basic characteristic. In order to improve the catalytic activity, the bimetallic and trimetallic oxides catalysts with copper, nickel, chromium and titanium as their co-catalysts were investigated. All the alumina supported catalysts were prepared by wetness impregnation method. The screening of biodiesel production using synthesized catalysts was monitored by gas chromatography-flame ionization detector (GC-FID). The two most potential catalysts were selected for the optimization and characterization study. Cu/Zn/?-Al2O3 catalyst calcined at 800°C with 10:90 wt.% dopant ratio to based and 3 times of alumina coating, exhibited the highest biodiesel production (89.50%) at mild reaction conditions (65°C, 10 wt.% catalyst loading, 1:20 oil:methanol mole ratio and 2 hours of reaction time). Cr/Ca/?-Al2O3 catalyst calcined at 700°C with 10:90 wt.% dopant ratio to based and 3 times number of alumina coating gave 86.64% of biodiesel production at 65°C, 6 wt.% catalyst loading, 1:18 oil:methanol mole ratio and 3 hours of reaction time. The physicochemical properties of the potential catalysts were accomplished using nitrogen analysis (NA) and CO2-temperature programmed desorption (CO2-TPD) that indicated high surface area (>140 m2/g) and high basicity (>3 mmol/g). X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) analysis showed the polycrystalline structure with small particles sizes (<50 nm). Energy dispersive X-ray (EDX) spectroscopy, X-ray fluorescence (XRF), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) analyses confirmed the existence of Al, O, Zn, Cu, Ca and Cr species in each potential catalyst. The optimization of catalyst preparation conditions and biodiesel production parameters were verified by response surface methodology (RSM) method and they were in good agreement with the experimental values. The mechanistic study on both potential catalysts follows the Langmuir- Hinshelwood (LH) model which involves the initial adsorption of reactants molecules on active sites of the catalyst surface. The specification analysis of produced biodiesel utilizing Cu/Zn/?-Al2O3 and Cr/Ca/?-Al2O3 catalysts showed that the refined used cooking oil has potential to be used in large-scale biodiesel production using reaction conditions found in the present study.
format	Thesis
qualification_name	Doctor of Philosophy (PhD.)
qualification_level	Doctorate
author	Sulaiman, Nur Fatin
author_facet	Sulaiman, Nur Fatin
author_sort	Sulaiman, Nur Fatin
title	Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
title_short	Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
title_full	Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
title_fullStr	Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
title_full_unstemmed	Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
title_sort	preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts
granting_institution	Universiti Teknologi Malaysia
granting_department	Chemistry
publishDate	2018
url	http://eprints.utm.my/id/eprint/81490/1/NurFatinSulaimanPFS2018.pdf
_version_	1747818342890078208

Preparation, characterization and mechanistic study on transesterification of refined used cooking oil for biodiesel production using zinc and calcium oxides-based catalysts

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