Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity

The immobilization of three homogeneous catalysts namely; sulfonic acid, 1,1,3,3-tetramethyl guanidine and 1,5,7-triazabicyclo[4.4.0]dec-5-ene guanidine was carried out on silica from rice husk ash. Sodium silicate from the rice husk ash was immobilised with 3-(mercaptopropyl)trimethoxysilane. Th...

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Main Author: Batagarawa, Muazu Samaila
Format: Thesis
Language:English
Published: 2014
Subjects:
Online Access:http://eprints.usm.my/46167/
http://eprints.usm.my/46167/1/Muazu%20Samaila%20Batagarawa24.pdf
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author Batagarawa, Muazu Samaila
author_facet Batagarawa, Muazu Samaila
author_sort Batagarawa, Muazu Samaila
building USM Institutional Repository
collection Online Access
description The immobilization of three homogeneous catalysts namely; sulfonic acid, 1,1,3,3-tetramethyl guanidine and 1,5,7-triazabicyclo[4.4.0]dec-5-ene guanidine was carried out on silica from rice husk ash. Sodium silicate from the rice husk ash was immobilised with 3-(mercaptopropyl)trimethoxysilane. This was further oxidised to sulfonic acid in a simple one pot method. The solid acid catalyst was denoted as RHAPrSO3H. Analysis of the catalyst by nitrogen adsorption-desorption using Brunauer, Emmet and Teller (BET) method showed its surface area to be 340 m2g-1 with average pore volume of 0.24 cc g-1 and pore diameter of 2.9 nm. Acidity tests by cation exchange capacity and pyridine FT-IR adsorption, revealed the presence of acid sites on the catalyst surface. Similarly, the 29Si MAS NMR of RHAPrSO3H revealed the presence of Q4, Q3, T3, T2 and T1 silicon centres, while only Q4 and Q3 silicon centres were present in RHASiO2. The catalyst was used in the acetalization reaction of glycerol with benzaldehyde. Under the best reaction conditions of 120 °C temperature, 2:1 molar ratio of glycerol: benzaldehyde, 0.15g mass of catalyst and 8 h reaction time, significant conversion was achieved with high selectivity towards five member ring isomer.
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format Thesis
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institution Universiti Sains Malaysia
institution_category Local University
language English
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publishDate 2014
recordtype eprints
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spelling usm-461672020-02-11T02:41:17Z http://eprints.usm.my/46167/ Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity Batagarawa, Muazu Samaila TP1-1185 Chemical technology The immobilization of three homogeneous catalysts namely; sulfonic acid, 1,1,3,3-tetramethyl guanidine and 1,5,7-triazabicyclo[4.4.0]dec-5-ene guanidine was carried out on silica from rice husk ash. Sodium silicate from the rice husk ash was immobilised with 3-(mercaptopropyl)trimethoxysilane. This was further oxidised to sulfonic acid in a simple one pot method. The solid acid catalyst was denoted as RHAPrSO3H. Analysis of the catalyst by nitrogen adsorption-desorption using Brunauer, Emmet and Teller (BET) method showed its surface area to be 340 m2g-1 with average pore volume of 0.24 cc g-1 and pore diameter of 2.9 nm. Acidity tests by cation exchange capacity and pyridine FT-IR adsorption, revealed the presence of acid sites on the catalyst surface. Similarly, the 29Si MAS NMR of RHAPrSO3H revealed the presence of Q4, Q3, T3, T2 and T1 silicon centres, while only Q4 and Q3 silicon centres were present in RHASiO2. The catalyst was used in the acetalization reaction of glycerol with benzaldehyde. Under the best reaction conditions of 120 °C temperature, 2:1 molar ratio of glycerol: benzaldehyde, 0.15g mass of catalyst and 8 h reaction time, significant conversion was achieved with high selectivity towards five member ring isomer. 2014-02 Thesis NonPeerReviewed application/pdf en http://eprints.usm.my/46167/1/Muazu%20Samaila%20Batagarawa24.pdf Batagarawa, Muazu Samaila (2014) Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity. PhD thesis, Universiti Sains Malaysia.
spellingShingle TP1-1185 Chemical technology
Batagarawa, Muazu Samaila
Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity
title Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity
title_full Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity
title_fullStr Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity
title_full_unstemmed Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity
title_short Studies On The Heterogenisation Of Sulphonic Acid And Guanidines On Silica And Their Catalytic Activity
title_sort studies on the heterogenisation of sulphonic acid and guanidines on silica and their catalytic activity
topic TP1-1185 Chemical technology
url http://eprints.usm.my/46167/
http://eprints.usm.my/46167/1/Muazu%20Samaila%20Batagarawa24.pdf