长链烷基酯/环氧基(聚)醚改性硅油的合成及表征

Synthesis and characterization of co-modified silicone oil with long-chain alkyl ester and epoxy ether

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、反应时间对Si-H转化率的影响关系，设计了均匀正交试验，在正交试验结果基础上借助反应条件的单因素分析，得到了最佳反应条件：催化剂用量为反应物质量的0.004%， n(PHMS)与n(C=C) 的物料比为1:1.05，反应温度为72℃，反应时间为3h。采用傅立叶红外光谱(FTIR)和傅立叶核磁氢谱(1H-NMR)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。

Abstract:

Co-modified silicone oil with long-chain alkyl ester and epoxy ether (PEESO) was synthesized using hydrosilylation of poly (hydromethyl, dimethyl) siloxane (PHMS) with stearyl methacrylate (SMA), allyl epoxy (poly) ether in the presence of platinum ((trimethyl)cyclopentadienylplatinum) catalyst. The effect of reactive conditions，such as dosage of catalyst, molar ratio of reactants, reaction temperature and time, on the Si-H conversion rate was discussed well. By orthogonal experiment and the corresponding single factor experiments, the preferential experimental conditions were obtained as follows. The amount of catalyst is 0.004% of material mass, the molar ratio of PHMS and alkene compounds 1:1.05, the reaction temperature 72℃, reaction time 3h. The molecular structure of the product was determined by FTIR and 1H-NMR. The experimental results indicated that the chain of long-chain alkyl ester and epoxy (poly) ether is grafted in the chain of polysiloxane.