Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone

Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone

Rice husk ash (RHA) consisting more than 90% of amorphous silica obtained under controlled burning of rice husk was directly used in the synthesis of ferrierite type-zeolite. The synthesis was performed under hydrothermal condition in the presence of different organic templates, oxide compositions a...

Full description

Saved in:
Bibliographic Details
Main Author: Bahruji, Hasliza
Format: Thesis
Language:English
Published: 2005
Subjects:
QD Chemistry
Online Access:http://eprints.utm.my/id/eprint/4173/1/HaslizaBahrujiMFS2005.pdf
Tags: Add Tag
No Tags, Be the first to tag this record!
id my-utm-ep.4173
record_format uketd_dc
spelling my-utm-ep.41732018-01-15T06:59:56Z Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone 2005-06 Bahruji, Hasliza QD Chemistry Rice husk ash (RHA) consisting more than 90% of amorphous silica obtained under controlled burning of rice husk was directly used in the synthesis of ferrierite type-zeolite. The synthesis was performed under hydrothermal condition in the presence of different organic templates, oxide compositions and at various crystallization periods. Solid products obtained from the synthesis were characterized by XRD, FTIR, 29Si MAS NMR, N2 (g) adsorption and SEM techniques. Results showed that pure ferrierite can be formed from the initial molar oxide ratios in the range of 1.31 – 1.5 Na2O : Al2O3 : 10 – 30 SiO2 : 4 – 10.0 template : 410 H2O with only pyrrolidine (Py) as the organic template. In general, quartz was obtained at higher SiO2/Al2O3 and lower Py/Al2O3 ratios. The crystal phase changes from ferrierite to analcime and lastly to quartz, with increasing SiO2/Py ratios. RHA was directly transformed to ferrierite phase within one day and reached equilibrium after 4 days crystallization. The acidity study of the H-ferrierite samples at different SiO2/Al2O3 ratios (12, 20 and 30) using IR-pyridine adsorption method showed the increase of acid sites with the decrease of SiO2/Al2O3 ratios in ferrierite framework. In each case, the Brønsted acid site is higher than Lewis acid sites. The catalytic activity of ferrierite at different SiO2/Al2O3 ratios towards Friedel-Crafts reaction between anisole and acid anhydrides was investigated. Results from the catalytic activity showed that only p-methoxypropiophenone and propionic acid was produced as the main product and side product respectively when propionic acid was used as acylating agent. The optimum temperature for the reaction was 120oC and ferrierite catalyst with SiO2/Al2O3 ratio 12 gave the highest conversion of anisole (66 %) and the selectivity of the main product (80 %). When acetic anhydride was employed as acylating agent, the conversion of anisole (55 %) and the selectivity of desired product (98 %) showed a higher percentage as compared with propionic anhydride. In both cases, the main product obtained is in para orientations with higher selectivity proved that H-ferrierite is a selective catalyst for the production of para orientation products 2005-06 Thesis http://eprints.utm.my/id/eprint/4173/ http://eprints.utm.my/id/eprint/4173/1/HaslizaBahrujiMFS2005.pdf application/pdf en public 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
Bahruji, Hasliza
Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
description Rice husk ash (RHA) consisting more than 90% of amorphous silica obtained under controlled burning of rice husk was directly used in the synthesis of ferrierite type-zeolite. The synthesis was performed under hydrothermal condition in the presence of different organic templates, oxide compositions and at various crystallization periods. Solid products obtained from the synthesis were characterized by XRD, FTIR, 29Si MAS NMR, N2 (g) adsorption and SEM techniques. Results showed that pure ferrierite can be formed from the initial molar oxide ratios in the range of 1.31 – 1.5 Na2O : Al2O3 : 10 – 30 SiO2 : 4 – 10.0 template : 410 H2O with only pyrrolidine (Py) as the organic template. In general, quartz was obtained at higher SiO2/Al2O3 and lower Py/Al2O3 ratios. The crystal phase changes from ferrierite to analcime and lastly to quartz, with increasing SiO2/Py ratios. RHA was directly transformed to ferrierite phase within one day and reached equilibrium after 4 days crystallization. The acidity study of the H-ferrierite samples at different SiO2/Al2O3 ratios (12, 20 and 30) using IR-pyridine adsorption method showed the increase of acid sites with the decrease of SiO2/Al2O3 ratios in ferrierite framework. In each case, the Brønsted acid site is higher than Lewis acid sites. The catalytic activity of ferrierite at different SiO2/Al2O3 ratios towards Friedel-Crafts reaction between anisole and acid anhydrides was investigated. Results from the catalytic activity showed that only p-methoxypropiophenone and propionic acid was produced as the main product and side product respectively when propionic acid was used as acylating agent. The optimum temperature for the reaction was 120oC and ferrierite catalyst with SiO2/Al2O3 ratio 12 gave the highest conversion of anisole (66 %) and the selectivity of the main product (80 %). When acetic anhydride was employed as acylating agent, the conversion of anisole (55 %) and the selectivity of desired product (98 %) showed a higher percentage as compared with propionic anhydride. In both cases, the main product obtained is in para orientations with higher selectivity proved that H-ferrierite is a selective catalyst for the production of para orientation products
format Thesis
qualification_level Master's degree
author Bahruji, Hasliza
author_facet Bahruji, Hasliza
author_sort Bahruji, Hasliza
title Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
title_short Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
title_full Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
title_fullStr Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
title_full_unstemmed Synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
title_sort synthesis of zeolite ferrierite from rice husk ash, characterization and activity towards friedel-crafts acylation for the formation of p-methoxypropiophenone
granting_institution Universiti Teknologi Malaysia, Faculty of Science
granting_department Faculty of Science
publishDate 2005
url http://eprints.utm.my/id/eprint/4173/1/HaslizaBahrujiMFS2005.pdf
_version_ 1747814496639909888

Similar Items