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正交设计在乙烯基POSS制备中的应用
引用本文:孙彩云,李芝,宋云.正交设计在乙烯基POSS制备中的应用[J].河北农业大学学报,2012,35(4):114-117.
作者姓名:孙彩云  李芝  宋云
作者单位:1. 华北科技学院基础部,北京,101601
2. 河北农业大学理学院,河北保定,071001
3. 华北科技学院资产管理处,北京,101601
基金项目:中央高校基本科研业务费资助(JCB1205B);河北省自然科学基金(E2011508001)
摘    要: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6 mL.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%.

关 键 词:乙烯基POSS  正交试验  方差分析  结构表征

Application of orthogonal design in the preparation of POSS
SUN Cai-yun , LI Zhi , SONG Yun.Application of orthogonal design in the preparation of POSS[J].Journal of Agricultural University of Hebei,2012,35(4):114-117.
Authors:SUN Cai-yun  LI Zhi  SONG Yun
Institution:1.Basic Department,North China University of Science & Technology,Beijing 101601,China;2.College of Science,Agricultural University of Hebei,Baoding 071001,China;3.Office of Asset Management,North China Institute of Science and Technology,Beijing 101601,China)
Abstract:The orthogonal design was utilized to study vinyl POSS prepared by hydrolysis of vinyl 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 hydrochloric acid had no great effects on the vinyl POSS yield.Optimum conditions for preparation of the vinyl POSS were 9 h for reaction time,65 ℃for reaction temperature,and 6 mL 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 ℃.
Keywords:vinyl POSS  orthogonal test  variance analysis  structure characterization
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