Chinese Journal of Chemical Engineering, Vol.25, No.12, 1771-1776, 2017
Pt-H2SO4/Zr-montmorillonite: An efficient catalyst for the polymerization of octamethylcy-clotetrasiloxane, polymethylhydrosiloxane and hexamethyldisiloxane to low-hydro silicone oil
The liquid phase ring-opening of octamethylcy-clotetrasiloxane (D-4) was investigated over Pt-H2SO4/Zr-montmorillonite catalyst. Montmorillonite (Mt), Zr-Mt, H2SO4/Mt, H2SO4/Zr-Mt and Pt-H2SO4/Zr-Mt were also detected for evaluation. The catalysts were characterized by X-ray fluorescence, X-ray diffraction, nitrogen adsorption-desorption, NH3-TPD and pyridine-FTIR measurements. In comparison to activate clay which is used in the industry of catalyst, Zr-Mt catalyst displayed stronger acidity and more excellent catalytic activity in the polymerization of D-4, polymethylhydrosiloxane (D-4(H)) and hexamethyldisiloxane (MM) to low-hydro silicone oil. Relative to Zr-Mt, the acidity of H2SO4/Zr-Mt was noticeably improved and the catalyst exhibited a higher capability of ring-opening of D-4 conversion and yield of low-hydro silicone oil. To enhance the stability of H2SO4/Zr-Mt catalyst, a small amount of metals (Pt) was doped. The nitrogen adsorption-desorption results indicated that pore textural parameters of the Pt-H2SO4/Zr-Mt had not changed with larger specific surface area. Compared with H2SO4/Zr-Mt, the total acidity of Pt-H2SO4-Zr/Mt catalyst retained, but the content of the Bronsted acid increased and the content of the Lewis acid decreased. The Pt-H2SO4-Zr/Mt catalyst displayed higher catalyst reproducibility. After 40 h reaction of polymerization, the yield of low-hydro silicone oil decreased from 93% to 42% over H2SO4/Zr-Mt catalyst, while the yield of low-hydro silicone oil reduced from 93% to 78% over Pt-H2SO4/Zr-Mt catalyst. A sharp decrease in catalytic activity after 35 h of Pt-H2SO4/Zr-Mt catalyst was detected. Furthermore, Pt-H2SO4/Zr-Mt was completely regenerated under appropriate condition and appeared good repeatability in the D-4, D-4(H) and MM to low-hydro silicone oil. (C) 2017 The Chemical Industry and Engineering Society of China, and Chemical Industry Press. All rights reserved.