Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction

Sodalite (SOD) is a microporous zeolite having ultra-fine size of pore about 2.8 Å. This property limits its role as a catalyst for the reaction involving bulky molecules. To overcome this disadvantage, suitable mesotemplate can be added to create mesoporosity in microporous SOD. This study focused...

Full description

Saved in:

Bibliographic Details
Main Author:	Othman, Mohamad Faiz
Format:	Thesis
Language:	English
Published:	2016
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/78201/1/MohamadFaizOthmanMFS2016.pdf
Tags:	Add Tag No Tags, Be the first to tag this record!

id	my-utm-ep.78201
record_format	uketd_dc
spelling	my-utm-ep.782012018-07-28T06:26:26Z Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction 2016-08 Othman, Mohamad Faiz QD Chemistry Sodalite (SOD) is a microporous zeolite having ultra-fine size of pore about 2.8 Å. This property limits its role as a catalyst for the reaction involving bulky molecules. To overcome this disadvantage, suitable mesotemplate can be added to create mesoporosity in microporous SOD. This study focused on the synthesis of SOD having mesoporosity using dual templates approach. A series of SOD were synthesized by mixing tetrapropylammonium (TPA) with different quaternary ammonium cations. As comparison, microporous SOD (Na-SOD) has also been synthesized without the presence of templates. The resulting SOD samples were characterized using XRD, FTIR and N2 adsorption-desorption measurement. The successful formation of SOD crystal phase for all SOD samples was confirmed from XRD patterns and supported by FTIR results that showed all SOD samples have the characteristic of SOD framework. However, N2 adsorption-desorption results confirmed that only SOD sample prepared by mixing TPA with organosilane (SODTO) showed the characteristic of mesoporosity with a narrow pore distribution peak centered at ca. 66 Å. For basicity study, Hammett indicator test showed that the strength of the basicity of all SOD samples was estimated in the range: 8.2 = pKa = 18.4. The results from back titration method found that the SOD-TO sample possessed the highest average amount of basicity as compared with other SOD samples. The comparison of the strength and the amount of basicity for microporous SOD, Na-SOD and mesoporous SOD, SOD-TO samples were measured using TPDCO2 analysis. The results showed that the SOD-TO sample has higher strength and amount of basic sites than the Na-SOD sample at temperature below 500°C. The catalytic testing of all SOD samples in the Knoevenagel condensation reaction of benzaldehyde and diethyl malonate was carried out giving diethyl-2- benzylidenemalonate as a main product. Results showed that all SOD catalyst were active for the Knoevenagel condensation reaction. From the result of catalyst testing, the basicity and surface area does give an impact during the reaction. The SOD-TO catalyst possessing the highest amount of basicity and the highest surface area with mesoporosity in its structure gave the highest percentage of conversion which was 96.29%. 2016-08 Thesis http://eprints.utm.my/id/eprint/78201/ http://eprints.utm.my/id/eprint/78201/1/MohamadFaizOthmanMFS2016.pdf application/pdf en public http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:94257 masters Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	QD Chemistry
spellingShingle	QD Chemistry Othman, Mohamad Faiz Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
description	Sodalite (SOD) is a microporous zeolite having ultra-fine size of pore about 2.8 Å. This property limits its role as a catalyst for the reaction involving bulky molecules. To overcome this disadvantage, suitable mesotemplate can be added to create mesoporosity in microporous SOD. This study focused on the synthesis of SOD having mesoporosity using dual templates approach. A series of SOD were synthesized by mixing tetrapropylammonium (TPA) with different quaternary ammonium cations. As comparison, microporous SOD (Na-SOD) has also been synthesized without the presence of templates. The resulting SOD samples were characterized using XRD, FTIR and N2 adsorption-desorption measurement. The successful formation of SOD crystal phase for all SOD samples was confirmed from XRD patterns and supported by FTIR results that showed all SOD samples have the characteristic of SOD framework. However, N2 adsorption-desorption results confirmed that only SOD sample prepared by mixing TPA with organosilane (SODTO) showed the characteristic of mesoporosity with a narrow pore distribution peak centered at ca. 66 Å. For basicity study, Hammett indicator test showed that the strength of the basicity of all SOD samples was estimated in the range: 8.2 = pKa = 18.4. The results from back titration method found that the SOD-TO sample possessed the highest average amount of basicity as compared with other SOD samples. The comparison of the strength and the amount of basicity for microporous SOD, Na-SOD and mesoporous SOD, SOD-TO samples were measured using TPDCO2 analysis. The results showed that the SOD-TO sample has higher strength and amount of basic sites than the Na-SOD sample at temperature below 500°C. The catalytic testing of all SOD samples in the Knoevenagel condensation reaction of benzaldehyde and diethyl malonate was carried out giving diethyl-2- benzylidenemalonate as a main product. Results showed that all SOD catalyst were active for the Knoevenagel condensation reaction. From the result of catalyst testing, the basicity and surface area does give an impact during the reaction. The SOD-TO catalyst possessing the highest amount of basicity and the highest surface area with mesoporosity in its structure gave the highest percentage of conversion which was 96.29%.
format	Thesis
qualification_level	Master's degree
author	Othman, Mohamad Faiz
author_facet	Othman, Mohamad Faiz
author_sort	Othman, Mohamad Faiz
title	Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
title_short	Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
title_full	Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
title_fullStr	Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
title_full_unstemmed	Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
title_sort	synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2016
url	http://eprints.utm.my/id/eprint/78201/1/MohamadFaizOthmanMFS2016.pdf
_version_	1747817931788517376

Synthesis of mesoporous sodalite by mixed quaternary ammonium cation templates for knoevenagel condensation reaction

Similar Items