Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride
Benzoylation of biphenyl with benzoyl chloride is an important acylation reaction, producing monosubstituted product, 4-phenyl benzophenone (4-PBP) and disubstituted product, 4, 4’- dibenzoylbiphenyl (4, 4’-DBBP). 4, 4’-DBBP is a monomer used as a component in emitting layer in polymer light e...
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my-utm-ep.45972017-10-12T04:46:21Z Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride 2006-03 Ng, Eng Poh QD Chemistry Benzoylation of biphenyl with benzoyl chloride is an important acylation reaction, producing monosubstituted product, 4-phenyl benzophenone (4-PBP) and disubstituted product, 4, 4’- dibenzoylbiphenyl (4, 4’-DBBP). 4, 4’-DBBP is a monomer used as a component in emitting layer in polymer light emitting (PLED) devices. The objective of this study is to synthesize and characterize a highly active sulphated AlMCM-41 acid catalyst by enhancing its acidity through sulphation. Firstly, the AlMCM-41 with various SiO2/Al2O3 ratios was prepared by direct synthesis, followed by conversion to H-AlMCM-41 via ion exchange of NaAlMCM-41 with ammonium nitrate. Finally, sulphated AlMCM-41 was prepared by impregnation of sulphuric acid in toluene. The sulphated MCM-41 materials possess high surface area (>500 m2/g) and large quantities of Brönsted acid sites after characterizing with surface analyzer and pyridine infrared spectroscopy. 27Al MAS NMR indicates the presence of octahedrally coordinated extra-framework sulphated aluminiums (EFAL) and aluminium sulphate. The Hammett indicators show that the acid strength of the sulphated AlMCM-41 materials was stronger than sulphuric acid and H-AlMCM-41 because of sulphate groups attached to aluminium atom in sulphated AlMCM-41. The results of comparative study on the dibenzoylation of biphenyl reaction indicate that only sulphated AlMCM-41 gives both monosubstituted 4-PBP and disubstituted 4, 4’-DBBP with the highest activity compared to sulphuric acid, H-AlMCM-41 and sulphated amorphous silica. 2006-03 Thesis http://eprints.utm.my/id/eprint/4597/ http://eprints.utm.my/id/eprint/4597/9/NgEngPohKPFS2006.pdf application/pdf en public masters Universiti Teknologi Malaysia, Faculty of Science Faculty of Science |
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Universiti Teknologi Malaysia |
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UTM Institutional Repository |
| language |
English |
| topic |
QD Chemistry |
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QD Chemistry Ng, Eng Poh Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| description |
Benzoylation of biphenyl with benzoyl chloride is an important acylation reaction, producing monosubstituted product, 4-phenyl benzophenone (4-PBP) and disubstituted product, 4, 4’- dibenzoylbiphenyl (4, 4’-DBBP). 4, 4’-DBBP is a monomer used as a component in emitting layer in polymer light emitting (PLED) devices. The objective of this study is to synthesize and characterize a highly active sulphated AlMCM-41 acid catalyst by enhancing its acidity through sulphation. Firstly, the AlMCM-41 with various SiO2/Al2O3 ratios was prepared by direct synthesis, followed by conversion to H-AlMCM-41 via ion exchange of NaAlMCM-41 with ammonium nitrate. Finally, sulphated AlMCM-41 was prepared by impregnation of sulphuric acid in toluene. The sulphated MCM-41 materials possess high surface area (>500 m2/g) and large quantities of Brönsted acid sites after characterizing with surface analyzer and pyridine infrared spectroscopy. 27Al MAS NMR indicates the presence of octahedrally coordinated extra-framework sulphated aluminiums (EFAL) and aluminium sulphate. The Hammett indicators show that the acid strength of the sulphated AlMCM-41 materials was stronger than sulphuric acid and H-AlMCM-41 because of sulphate groups attached to aluminium atom in sulphated AlMCM-41. The results of comparative study on the dibenzoylation of biphenyl reaction indicate that only sulphated AlMCM-41 gives both monosubstituted 4-PBP and disubstituted 4, 4’-DBBP with the highest activity compared to sulphuric acid, H-AlMCM-41 and sulphated amorphous silica. |
| format |
Thesis |
| qualification_level |
Master's degree |
| author |
Ng, Eng Poh |
| author_facet |
Ng, Eng Poh |
| author_sort |
Ng, Eng Poh |
| title |
Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| title_short |
Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| title_full |
Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| title_fullStr |
Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| title_full_unstemmed |
Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| title_sort |
synthesis and characterization of sulphated aimcm-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| granting_institution |
Universiti Teknologi Malaysia, Faculty of Science |
| granting_department |
Faculty of Science |
| publishDate |
2006 |
| url |
http://eprints.utm.my/id/eprint/4597/9/NgEngPohKPFS2006.pdf |
| _version_ |
1747814538742333440 |