1,4-双(二甲基羟基硅)苯的制备及表征  

Preparation and Characterization of 1,4-Bis(dimethylhydroxysilyl)benzene

作　　者：向世平 肖勇 陈海亚 黄赓乔 鲁明涛 王俊勋 熊风 张振燕 XIANG Shiping;XIAO Yong;CHEN Haiya;HUANG Gengqiao;LU Mingtao;WANG Junxun;XIONG Feng;ZHANG Zhenyan(Hubei Space Focus Technology Co.,Ltd.,Xiaogan 432000,China)

机构地区：[1]湖北航聚科技股份有限公司,湖北孝感432000

出　　处：《有机硅材料》2024年第3期10-15,21,共7页Silicone Material

摘　　要：以对二溴苯、二甲基二甲氧基硅烷、镁屑为原料,通过格氏法合成苯撑硅甲氧基硅烷单体1,4-双(二甲基甲氧基硅)苯,然后经水解反应制得目标产物苯撑硅羟基单体1,4-双(二甲基羟基硅)苯。通过红外光谱表征了产物结构,探讨了搅拌速率、滴料时间、原料配比、溶剂等对苯撑硅甲氧基硅烷单体收率的影响,还研究了水解反应催化剂、加料时间对苯撑硅羟基单体收率的影响。结果表明,格氏和水解反应成功合成了苯撑硅甲氧基硅烷单体和苯撑硅羟基单体;格氏法合成苯撑硅甲氧基硅烷单体的较佳条件为:搅拌速率200r/min、滴料时间3h、对二溴苯和二甲基二甲氧基硅烷与镁物质的量之比1:2.4:2、1400mL四氢呋喃作溶剂,此时苯撑硅甲氧基硅烷单体的收率为64.2%;苯撑硅甲氧基硅烷单体经水解反应制备苯撑硅羟基单体的较佳条件为:2500mL的磷酸(H_(3)PO_(4)质量分数5%)作水解催化剂、加料时间3.5h,此时苯撑硅羟基单体的收率为77%。1,4-Bis(dimethylmethoxy silane)benzene was synthesized by Grignard reaction from p-dibromobenzene,dimethyldimethoxy 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 fllows:2500 mL H,P04(5 wt%)phosphoric acid as hydrolysis catalyst,feed for 3.5 h,thus the yield of phenylenedisiloxane hydroxyl monomer was 77%.

关 键 词：1 4-双(二甲基甲氧基硅)苯 1 4-双(二甲基羟基硅)苯 单体 格氏法 收率 

分 类 号：TQ264.17[化学工程—有机化工]