摘要
将八甲基环四硅氮烷 (OMCT)与Ph2 SiCl2 在 190～ 2 10℃反应 ,获得的产物以正己烷溶解 ,分离出 1,3 二氯 1,1,3,3 四苯基二硅氮烷 (DCTPS) (Ⅰ ) ,并得到滤液 (Ⅱ )。滤液 (Ⅱ )经减压加热反应 ,得到馏出液 (Ⅲ )及残留物。采用1H NMR、2 9Si NMR谱、场解吸质谱 (FD)、色质联用质谱等 ,对上述残留物及滤液 (Ⅱ )、馏出液 (Ⅲ )的二乙胺氨基化产物进行表征 ,确定各组分的结构。研究发现 ,OMCT与Ph2 SiCl2 的反应相当复杂 ,DCTPS等化合物是由不同的硅氮键断裂方式及不同的—SiMe2 — /—SiPh2 —交换反应形成的 ;滤液 (Ⅱ )中的化合物经减压加热反应 ,形成产率约为 2 0 3%的六苯基环三硅氮烷 (HPCT)及一定量的DCTPS、Ph2 SiCl2 、Me2 SiCl2
Reaction of octamethylcyclotetrasilazane with Ph 2SiCl 2 was carried out at temperature of 190～210?℃, and the mixture product was dissolved by n hexane. By filtrating, 1,3 dichloro 1,1,3,3 tetraphenyldisilazane(DCTPS)(Ⅰ) and filtrate(Ⅱ) were obtained. After distilling the solvent, filtrate(Ⅱ) was conducted a reaction at 260?℃ under reduced pressure of 5?065?Pa, and a distilled mixture (Ⅲ) was collected and a residue mixture was remained. The components of the residue mixture as well as the aminolysis products of the distilled mixture (Ⅲ), and filtrate(Ⅱ) were characterized by 1H NMR, 29 Si NMR spectrum and field desorption (FD) mass spectrum. From the results, it was found that the reaction of OMCT with Ph 2SiCl 2 was very complicated, and DCTPS and other compounds were formed through different breaking modes of Si-N bonds in OMCT and different exchange reactions of -Me 2Si- groups with -SiPh 2- groups. Further reaction of filtrate(Ⅱ) formed 20 3% hexaphenylcyclotrisilazane(HPCT) and some amount of DCTPS, Ph 2SiCl 2, Me 2SiCl 2 and so on.
出处
《北京化工大学学报（自然科学版）》
CAS
CSCD
2003年第2期28-31,共4页
Journal of Beijing University of Chemical Technology(Natural Science Edition)
基金
国家自然科学基金资助项目 (2 9374 186 )
