正交设计在乙烯基POSS制备中的应用

Application of orthogonal design in the preparation of POSS

利用正交设计法研究由乙烯基三乙氧基硅烷酸性水解法制备乙烯基POSS。通过方差分析,探讨了反应温度、反应时间与盐酸用量对乙烯基POSS产量的影响。试验结果表明:反应时间和反应温度的改变对乙烯基POSS的产量影响显著,盐酸用量的改变对乙烯基POSS的产量无明显影响。乙烯基POSS制备的最佳条件为:反应时间为9h,反应温度为65℃,加盐酸量为6mL。采用红外分析和核磁共振对乙烯基POSS的结构进行了表征,采用TG分析了乙烯基POSS的热性能,空气介质中乙烯基POSS在800℃的剩炭率为68.5%。

The orthogonal design was utilized to study vinyl POSS prepared by hydrolysis of vi- nyl triethoxysilane. The effects of reaction temperature, time and contents of hydrochloric acid on the vinyl POSS yield were discussed. The experimental results showed that the varied reaction temperature and time had obvious influences on the vinyl POSS yield, and contents of hy- drochloric acid had no great effects on the vinyl POSS yield. Optimum conditions for prepara- tion of the vinyl POSS were 9 h for reaction time, 65℃ fot reaction temperature, and 6 mI. for contents of hydrochloric acid. IR and29Si NMR analysis were used to characterize the structure of the vinyl POSS. TG was used to study the thermal properties of the vinyl POSS. Residue of the vinyl POSS degradation in air was 68.5% at 800℃.