Synthesis, characterization of triphenyltin grafted on SBA-15 mesoporous silica and its catalytic performance for the synthesis of 4-methylacetophenone

Qigang Deng; Zhile Qin; Ying Yang; Weiming Song

doi:10.1016/j.cjche.2013.12.001

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Synthesis, characterization of triphenyltin grafted on SBA-15 mesoporous silica and its catalytic performance for the synthesis of 4-methylacetophenone

催化、动力学与反应工程 | Updated：2026-01-06

- Synthesis, characterization of triphenyltin grafted on SBA-15 mesoporous silica and its catalytic performance for the synthesis of 4-methylacetophenone
- Chinese Journal of Chemical Engineering Vol. 23, Issue 2, Pages: 384-388(2015)
- Affiliations：
  
  College of Chemistry and Chemical Engineering of Qiqihar University,Qiqihar,China,161000
- Author bio：
- Funds：
- DOI：10.1016/j.cjche.2013.12.001
  CLC：
- Published：2015
- Accepted：
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Qigang Deng, Zhile Qin, Ying Yang, Weiming Song. Synthesis, characterization of triphenyltin grafted on SBA-15 mesoporous silica and its catalytic performance for the synthesis of 4-methylacetophenone[J]. , 2015, 23(2): 384-388.
DOI：

Qigang Deng, Zhile Qin, Ying Yang, Weiming Song. Synthesis, characterization of triphenyltin grafted on SBA-15 mesoporous silica and its catalytic performance for the synthesis of 4-methylacetophenone[J]. , 2015, 23(2): 384-388. DOI： 10.1016/j.cjche.2013.12.001.

摘要

Abstract

The production of Ph

Sn-O-SBA-15 (Ph

SnSBA) was achieved by heating triphenyltin chloride and SBA-15 in N-methylpyrrolidone at 190℃ for 5 h using triethylamine as a catalyst. The composition

structure

and surface physical and chemical properties of Ph

SnSBA were characterized using inductively coupled plasma-atomic emission spectroscopy (ICP-AES)

119

Sn and

Si solid-state nuclear magnetic resonance (NMR) spectroscopy in situ pyridine infrared spectroscopy (Py-IR)

adsorption-desorption isotherms

X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results of ICP-AES and organic elemental analysis showed that the grafting yield of Sn was 17% (by mass) for Ph

SnSBA. The elemental analysis and solid-state NMR results for Ph

SnSBA were consistent with grafting of triphenyltin on SBA-15. The N

adsorption-desorption

XRD and TEM analyses showed that Ph

SnSBA retained an ordered hexagonal mesoporous structure

resulting in decreases in the surface area

pore size and mesopore volume

and an increase in acidity as compared with SBA-15. The

Hammett acidity function (

) value and the number of acid sites for Ph

SnSBA

obtained by the Hammett methods

were 2.77-3.30 and 2.07 mmol·g

-1

respectively. The Friedel-Crafts acylation of toluene and acetic anhydride over Ph

SnSBA was investigated. The yield of methylacetophenone (MAP) and the selectivity for 4-methylacetophenone (PMAP) were 79.56% and 97.12%

respectively

when the conditions were

(toluene):

(anhydride)=2.0:1.0 with 6% (by mass) catalyst

and heating under reflux for 5 h. The PMAP selectivity still reached 93.11% when Ph

SnSBA was used for the fifth time under the same reaction conditions.

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