Preparation and Characterization of 1,4-Bis(dimethylhydroxysilyl)benzene
1,4-Bis(dimethylmethoxy silane)benzene was synthesized by Grignard reaction from p-dibromobenzene,dimeth-yldimethoxy silane and magnesium chips,and then the target product 1,4-bis(dimethylhydroxy silane)benzene was prepared by hydrolysis.The product structure was characterized by infrared spectroscopy,and the effects of stirring rate,dropping time,ratio of raw materials and solvent on the yield of phenylenedisiloxane were discussed.The effects of hydrolysis catalyst and feeding time on the yield of phenylenedisiloxane hydroxyl monomer were also studied.The results showed that phenylenedisiloxy silane and phenylenedisiloxy were successfully synthesized by Grignard reaction and hydrolysis,and the optimum conditions were as follows:stirring rate 200 r/min,dropping time 3 h,the ratio of p-dibromobenzene and dimethyldimethoxy silane to magnesium 1∶2.4∶2,1400 mL tetrahydrofuran as solvent,and the yield of phenylenedisiloxy silane monomer was 64.2％.The optimum conditions for preparing phenylenedisiloxane hydroxyl monomer by hydrolysis of phenylenedisiloxane were as follows:2500 mL H3PO4(5 wt％)phosphoric acid as hydrolysis catalyst,feed for 3.5 h,thus the yield of phenylenedisiloxane hydroxyl monomer was 77％.
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