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Citation: LIU Xing, SONG Weiming, DENG Qigang. Synthesis and Characterization of the Trimethyltin Chloride Tethered on Mesoporous Molucular Sieve Al-MCM-41 and Its Catalytic Performance[J]. Chinese Journal of Applied Chemistry, ;2011, 28(6): 673-677. doi: 10.3724/SP.J.1095.2011.00467 shu

Synthesis and Characterization of the Trimethyltin Chloride Tethered on Mesoporous Molucular Sieve Al-MCM-41 and Its Catalytic Performance

1.
College of Chemistry and Chemical Engineering, Qiqihaer University, Qiqihaer 161006

Corresponding author: SONG Weiming,
Received Date: 9 August 2010
Available Online: 18 December 2010
Fund Project: 黑龙江省自然科学基金(B201010)资助项目 (B201010)

Trimethyltin chloride and mesoporous molecular sieve Al-MCM-41 were heated at 135℃ for 4.5 h under stirring conditions and nitrogen atmosphere,to obtain(CH₃)₃ Sn-O-MCM-41[(CH₃)₃ SnM].The composition,structure,and physical and chemical surface properties of the resulted solid were characterized by inductively coupled plasma mass spectrometry(ICP-MS),Fourier transform infrared spectroscopy(FTIR),N₂ adsorption-desorption,NH₃ chemisorption(NH₃-TPD),X-ray diffraction(XRD),and transmission electron microscopy(TEM).The results showed that the grafting yield was 14.44% for Sn in mass fraction.TPD acid(NH₃) of Al-MCM-41 before and after reaction with trimethyltin chloride increased from 0.652 6 mmol/g to 1.294 4 mmol/g.(CH₃)₃SnM resulted in a decrease of the surface areas and the pore size and an increase of the mesopous volume and surface acidity compared to Al-MCM-41.The thermal stability for the sample grafted with organotin was improved.The sample that was grafted with organotin on the Al-MCM-41 had the ordered hexagonal mesopore structure.The conversion rate is 96% when n(isoamyl alcohol):n(acetic acid)=1.0:1.0,w((CH₃)₃SnM)=5%,138℃ for 5 h,and the catalyst can be reused.A conversion rate of 86% can be attained when catalyst was reused five times under the same catalytic conditions.
- trimethyltin chloride,
- Al-MCM-41,
- grafting reaction,
- characterization
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