双链梯形聚(1,3-二甲基-1,3-二氧二硅氧烷)的制备  

A Method for Synthesis of Double-Chain Ladder-Like Poly(1,3-dimethyl-1,3-dioxdisiloxane)

作　　者：贾修伟[1,2] 容敏智[1] 章明秋[1] 

机构地区：[1]聚合物复合材料及功能材料教育部重点实验室中山大学材料科学研究所,广州510275 [2]河南大学药学院,河南开封475004

出　　处：《河南大学学报（自然科学版）》2013年第6期625-630,共6页Journal of Henan University:Natural Science

基　　金：国家自然科学基金项目(50773095);广东省科技计划项目(2007A010500004;2008310004202465);广州市科技计划项目(2008J1-C231-1)

摘　　要：采用非水解缩合与水解缩聚相结合的方法,合成了双链梯形聚(1,3-二甲基-1,3-二氧二硅氧烷).第一步运用非水解缩合方法合成出1,3-二甲基-1,1-二氯-3,3-二甲氧基二硅氧烷单体;第二步,不分离提纯该二硅氧烷单体而直接加入适量水进行水解缩聚反应,成功得到双链梯形聚(1,3-二甲基-1,3-二氧二硅氧烷)(PMSQ).借助核磁共振光谱、红外光谱、凝胶渗透色谱、粉末X射线衍射、热失重、分子模拟等手段对PMSQ进行表征.研究结果表明,PMSQ为规整性较高的双链梯形结构,梯形结构宽度为0.87nm、厚度为0.40nm,用凝胶渗透色谱法测定的重均相对分子质量为3.5×105.A method combining non-hydrolytic condensation and polycondensation was used to synthesize doublechain ladder-like poly（1,3-dimethy-1,3-dioxdisiloxane） （PMSQ）. Firstly, the disiloxane monomer was obtained by non-hydrolytic condensation of methyltrichlorosilane with methyltrimethoxysilane. Then, PMSQ was produced via directly hydrolytic polycondensation of the above disiloxane monomer without further purification in the same reactor. Chemical structure and configuration of the resultant PMSQ were characterized by nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectrometry, powder X-ray diffraction, thermogravimetric analysis, and molecular structure simulations, respectively. All the experimental data demonstrated that the ladderlike PMSQ possessed satisfied regularity with chain-to-chain width of 0.87 nm and chain thickness of 0.40 nm. Weight average relative molecular weight of PMSQ was determined to be 3. 5 × 10^5 using gel permeation chromatography.

关 键 词：双链梯形 聚硅倍半氧烷 非水解缩合 水解缩聚 

分 类 号：O634.41[理学—高分子化学]