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机构地区:[1]陕西科技大学教育部轻化工助剂重点实验室,陕西西安710021
出 处:《精细化工》2014年第1期132-136,共5页Fine Chemicals
基 金:陕西省教育厅产业化培育项目(2011JG25)~~
摘 要:以三甲基环戊二烯基铂为催化剂,将甲基丙烯酸十八酯(SMA)、烯丙基环氧(聚)醚和低含氢硅油(PHMS)通过硅氢加成反应,合成了长链烷基酯/环氧基(聚)醚共改性硅油(PEESO)。根据催化剂用量、原料配比、反应温度以及反应时间对Si—H转化率的影响关系,设计了均匀正交实验。在正交实验结果基础上借助反应条件的单因素分析,确定了最佳反应条件:催化剂用量为反应物质量的0.004%,物料比n(PHMS)∶n(CC)=1∶1.05,反应温度为72℃,反应时间为3 h。采用傅里叶变换红外光谱(FTIR)和核磁共振氢谱(1HNMR)对产物结构进行表征,结果表明,长链烷基酯和环氧基(聚)醚成功接枝到聚硅氧烷主链中。A new silicone oil with long alkyl ester and polyether epoxy groups (PEESO) has been synthesized by hydrosilylation of polyhydromethylsiloxane ( PHMS ) with stearyl methacrylate ( SMA ) and polyether epoxy groups in the presence of platinum [ (trimethyl) cyclopentadienylplatinum catalyst. The factors affecting Si--H conversion rate, such as dosage of catalyst, molar ratio of reactants, reaction temperature and time, have been studied. And then a uniformly orthogonal experiment has been designed to obtain the better experimental conditions. Finally, the optimum experimental conditions have been determined by means of orthogonal experiment and the corresponding single factor experiments. The amount of catalyst is 0. 004% of raw materials, the molar ratio of PHMS to alkene compounds is 1:1.05 ,the reaction temperature is 72 %, and the reaction time is 3 h. In addition,the chemical structure of PEESO was characterized by means of Fourier transform infrared spectrum (FTIR) and proton nuclear magnetic resonance spectrum (1HNMR). As expected, long alkyl ester group and (poly) ether epoxy group were successfully grafted in the polysiloxane backbone.
关 键 词:有机硅蜡 硅氢加成 长链烷基 表征 精细化工中间体
分 类 号:TQ324.21[化学工程—合成树脂塑料工业]
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