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Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction

Coal fly ash (CFA) is a waste product from burning of coal fuel in the electrical power plant. It contains mostly silica and alumina which in powder form is considered hazardous material but can be utilized as precursor for the synthesis of zeolite. In this study, CFA has been converted to sodalite...

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Main Author: Mohamed, Mohd. Hilmi
Format: Thesis
Language:English
Published: 2014
Subjects:
QD Chemistry
Online Access:http://eprints.utm.my/id/eprint/48834/25/MohdHilmiMohamedMFS2014.pdf
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spelling my.utm.488342020-06-30T02:18:13Z http://eprints.utm.my/id/eprint/48834/ Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction Mohamed, Mohd. Hilmi QD Chemistry Coal fly ash (CFA) is a waste product from burning of coal fuel in the electrical power plant. It contains mostly silica and alumina which in powder form is considered hazardous material but can be utilized as precursor for the synthesis of zeolite. In this study, CFA has been converted to sodalite (SOD) and tested as a base catalyst in Knoevenagel reaction. Sodalite has been synthesized using microwave heating by varying alkaline concentration and heating time to obtain optimum parameter for formation of pure sodalite. The synthesis was also conducted by conventional oven heating for comparision. All synthesized products were characterized with XRD, FTIR, FESEM and 29Si MAS NMR. The results showed that quite pure sodalite (Na-SOD) crystal has been formed in 45 min by microwave heating as compared to 5 days by conventional oven heating.29Si MAS NMR showed the synthesized SOD has Si/Al ratio of 1 while FESEM gave irregularly-shaped crystal with the size ranging between 60 – 120 nm.The synthesized Na-SOD was ion exchanged with group 1 (K, Cs) and group 2 (Ca, Sr, Ba) metal ions in order to enhance sodalite basicity. The crystallinity of ion exchanged-SOD samples has decreased to - 70% and - 30% for samples exchanged with group 1 and group 2 metal ions, respectively. The catalytic testing of the catalysts in Knoevenagel reaction of benzaldehyde and dimethyl malonate was carried out, producing dimethyl-2-benzylidemalonate, methyl cinnamate and dimethyl-2,2- bis(hydroxyl(phenyl)methyl) malonate. Based on the conversion of reactant, K-SOD has shown the most active for the Knoevenagel reaction while Ca-SOD gave the lowest conversion. For the catalyst reusability, Cs-SOD gave the best performance in long-term application. The formation of dimethyl-2,2-bis(hydroxyl(phenyl)methyl) malonate as one of the products in this Knoevenagel reaction indicate that sodalitebased catalyst was highly basic but a non-selective catalyst. 2014-04 Thesis NonPeerReviewed application/pdf en http://eprints.utm.my/id/eprint/48834/25/MohdHilmiMohamedMFS2014.pdf Mohamed, Mohd. Hilmi (2014) Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction. Masters thesis, Universiti Teknologi Malaysia, Faculty of Science. http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:89356
institution Universiti Teknologi Malaysia
building UTM Library
collection Institutional Repository
continent Asia
country Malaysia
content_provider Universiti Teknologi Malaysia
content_source UTM Institutional Repository
url_provider http://eprints.utm.my/
language English
topic QD Chemistry
spellingShingle QD Chemistry
Mohamed, Mohd. Hilmi
Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
description Coal fly ash (CFA) is a waste product from burning of coal fuel in the electrical power plant. It contains mostly silica and alumina which in powder form is considered hazardous material but can be utilized as precursor for the synthesis of zeolite. In this study, CFA has been converted to sodalite (SOD) and tested as a base catalyst in Knoevenagel reaction. Sodalite has been synthesized using microwave heating by varying alkaline concentration and heating time to obtain optimum parameter for formation of pure sodalite. The synthesis was also conducted by conventional oven heating for comparision. All synthesized products were characterized with XRD, FTIR, FESEM and 29Si MAS NMR. The results showed that quite pure sodalite (Na-SOD) crystal has been formed in 45 min by microwave heating as compared to 5 days by conventional oven heating.29Si MAS NMR showed the synthesized SOD has Si/Al ratio of 1 while FESEM gave irregularly-shaped crystal with the size ranging between 60 – 120 nm.The synthesized Na-SOD was ion exchanged with group 1 (K, Cs) and group 2 (Ca, Sr, Ba) metal ions in order to enhance sodalite basicity. The crystallinity of ion exchanged-SOD samples has decreased to - 70% and - 30% for samples exchanged with group 1 and group 2 metal ions, respectively. The catalytic testing of the catalysts in Knoevenagel reaction of benzaldehyde and dimethyl malonate was carried out, producing dimethyl-2-benzylidemalonate, methyl cinnamate and dimethyl-2,2- bis(hydroxyl(phenyl)methyl) malonate. Based on the conversion of reactant, K-SOD has shown the most active for the Knoevenagel reaction while Ca-SOD gave the lowest conversion. For the catalyst reusability, Cs-SOD gave the best performance in long-term application. The formation of dimethyl-2,2-bis(hydroxyl(phenyl)methyl) malonate as one of the products in this Knoevenagel reaction indicate that sodalitebased catalyst was highly basic but a non-selective catalyst.
format Thesis
author Mohamed, Mohd. Hilmi
author_facet Mohamed, Mohd. Hilmi
author_sort Mohamed, Mohd. Hilmi
title Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
title_short Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
title_full Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
title_fullStr Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
title_full_unstemmed Microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
title_sort microwave synthesis of sodalite from coal fly ash as solid base catalyst for knoevenagel reaction
publishDate 2014
url http://eprints.utm.my/id/eprint/48834/25/MohdHilmiMohamedMFS2014.pdf
http://eprints.utm.my/id/eprint/48834/
http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:89356
_version_ 1672610474039967744
score 13.211869

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