Abstract

Silica-supported germania adsorbents were prepared by treating silica with GeCl 4 vapor, and then causing the GeCl n surface layer to react with H 2O. Infrared spectroscopic techniques were used to monitor the reactions at various stages. The data suggest the following mechanism: GeCl 4 reacts on the silanols and also with siloxane bridges; the initial exposure to H 2O at 25°C then causes the hydrolysis of Si Cl groups to form Si OH groups as well as partial hydrolysis of the GeCl n layer. Degassing at high temperature then causes the partially hydrolyzed GeCl n layer to become mobile and rearrange and further react with the surface, eliminating the newly-formed silanols, and causing the formation of partially-chlorided germania patches. Dechlorination and aggregation of these proceeds as hydration-degassing cycles are continued. The adsorbents prepared in this fashion have properties like those of adsorbents prepared by reacting silica with Ge(OCH 3) 4 and converting the methoxide layer to oxide.

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