含环氧基团硅油的硅氢加成合成反应研究

以含氢硅油(PHMS)和甲基丙烯酸缩水甘油酯(GMA)为原料在铂催化剂的作用下,用硅氢加成反应合成了侧基含有环氧基团的硅油。利用红外光谱和核磁共振光谱对加成产物结构进行了表征。采用化学滴定法测定了未反应活泼氢的质量分数,从而确定了含氢硅油中活泼氢的转化率。讨论了反应温度、反应时间、催化剂用量及投料物质的量比等因素对转化率的影响。实验结果表明,含氢硅油中活泼氢的转化率随着温度的升高、时间的延长、催化剂用量和投料物质的量比的增加呈上升趋势,最终趋于平衡。确定了最佳反应条件:反应温度为100℃、反应时间为10 h、催化剂用量为单体(GMA)质量的0.020%、甲基丙烯酸缩水甘油酯与含氢硅油的物质的量比为1.2∶1.0。此时,活泼氢的转化率为62.5%。加成产物的红外光谱和核磁共振光谱结构表征证明,成功制得了含有环氧基团的硅油。

Synthesis of polysilicone containing epoxy group by hydrosilylation

The silicone oil with side group of glycidyl methacrylate(GMA) was prepared by the hydrosilylation reaction of polymethyl thydrosiloxane(PHMS) and glycidyl methacrylate(GMA) in toluene using the isopropanol solution of H2PtCl6 as a catalyzer.The product was characterized by FTIR spectra and1H-NMR spectra.The yield of the reaction was determined using chemistry titration by which the unreacted active hydrogen was detected.The effect of reaction temperature(T),reaction time(t),catalyst dosage and molar ratio of GMA to PHMS on the conversion yield were discussed.Tests showed that the conversion yield was increased with increasing reaction temperature(T),reaction time(t),catalyst dosage and molar ratio of GMA to PHMS.The optimal formula and reaction process were acquired:T=100 ℃,t=10 h,the mass fraction of catalyst was 0.020% of the reaction monomer GMA weight and the molar ratio of the GMA to PHMS was 1.2∶1.0.The conversion yield of active hydrogen was 62.5%.The structural determination by FTIR spectra and 1HNMR spectra showed that the silicone oil with side group of glycidyl methacrylate(GMA)was successfully prepared.