Synthesis, characterization and catalytic performance of Al-MCM-41 molecular sieve containing silicon after modified by tributyltin chloride

The tributyltin chloride and Al-MCM-41 containing silicon(SiAlM) were heated at 180°C for 5 h under stirring conditions in nitrogen atmosphere,and a production of R₃Sn-O-Si-Al-MCM-41 ( R₃SnSiAlM ) was got. The composition .structure and surface physical and chemical properties of the samples were characterized by elemental analysis (EDS) , fourier transform infrared spectroscopy (FTIR), N₂ adsorption-desorption, NH₃ chemisorption (NH₃-TPD), X-ray diffraction (XRD), Transmission electron microscopy (TEM) and so on. The results show that the grafting yield is 11.14% of Sn for R₃SnSiAlM. TPD acid of Al-MCM-41 before and after reaction with tributyltin chloride increases from 0.6526 mmol(NH₃)/g to 3.0565 mmol(NH₃)/g. R₃SnSiAlM resultes in decease of the surface areas and the pore size and increase of the mesopours volume and surface acidity,compared to Al-MCM-41. The sample that the organotin was grafted on the Al-MCM-41 has the ordered hexagonal mesopore structure. R3SnSiALM is used in the synthesis of isoamyl acetate. The ester yield is 97% when n (isoamyl alcohol): n (acetic acid) = 1.0:1.0, w (R₃SnSiAlM) = 5%, 135°C for 5h, and the catalyst can be reused.