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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| Format: | Thesis |
| Language: | English |
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2006
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| Online Access: | http://eprints.utm.my/4597/9/NgEngPohKPFS2006.pdf |
| _version_ | 1825909586566053888 |
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| author | Ng, Eng Poh |
| author_facet | Ng, Eng Poh |
| author_sort | Ng, Eng Poh |
| collection | ePrints |
| 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. |
| first_indexed | 2024-03-05T18:04:23Z |
| format | Thesis |
| id | utm.eprints-4597 |
| institution | Universiti Teknologi Malaysia - ePrints |
| language | English |
| last_indexed | 2024-03-05T18:04:23Z |
| publishDate | 2006 |
| record_format | dspace |
| spelling | utm.eprints-45972017-10-12T04:46:21Z http://eprints.utm.my/4597/ Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride 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 NonPeerReviewed application/pdf en http://eprints.utm.my/4597/9/NgEngPohKPFS2006.pdf Ng, Eng Poh (2006) Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride. Masters thesis, Universiti Teknologi Malaysia, Faculty of Science. |
| spellingShingle | QD Chemistry Ng, Eng Poh Synthesis and characterization of sulphated AIMCM-41 and its catalytic activity in dibenzoylation of biphenyl with benzoyl chloride |
| title | 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_short | 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 |
| topic | QD Chemistry |
| url | http://eprints.utm.my/4597/9/NgEngPohKPFS2006.pdf |
| work_keys_str_mv | AT ngengpoh synthesisandcharacterizationofsulphatedaimcm41anditscatalyticactivityindibenzoylationofbiphenylwithbenzoylchloride |