Abstract
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)3Sn-O-MCM-41 [(CH3)3SnM].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.
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