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Synthesis and characterization of cage octa(aminopropylsilsesquioxane)

机译:笼型八(氨基丙基倍半硅氧烷)的合成与表征

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The compound of cage octa(aminopropylsilsesquioxane) (POSS-NH2) was prepared in higher yield by the hydrolysis and polycondensation of trifunctional monomer H2NCH2CH2CH2Si(OC2H5)(3) in the mixture of solvents acetonitrile and 1-propanol, with tetraethyl ammonium hydroxide (Et4NOH) as the catalyst. The effects of various parameters influencing the reaction, such as monomer concentration, nature of solvents, and the content of catalyst, were investigated. Results showed that the better values of these reactive factors were nH(2)OXSiy(3) = 8-9/1 (molar ratio), nEt(4)NOHXSiy(3) = 0.0045 (molar ratio), respectively. The use of acetonitrile as a solvent favors the deposition and formation of the product. The existence of the higher boiling pointing I-propanol favors the higher reaction temperature, which accelerates the formation of octamer, reduces the reaction time and eventually increases the yield. The cage structure and its formula (H2NCH2CH2CH2)(8)Si8O12 of the synthetic compound were characterized by FTIR, MS, H-1, and Si-29 NMR. TG curve of POSS-NH2 shows that the cage-like compound has high decomposition temperature and higher thermal residue than the theoretical values during the thermal processing. (c) 2006 Wiley Periodicals, Inc.
机译:通过在溶剂乙腈和1-丙醇的混合物中将三官能单体H2NCH2CH2CH2Si(OC2H5)(3)与四乙基氢氧化铵(Et4NOH)水解和缩聚,可以更高收率制备笼八(氨基丙基倍半硅氧烷)(POSS-NH2)化合物。 )作为催化剂。研究了影响单体反应浓度的各种参数,例如单体浓度,溶剂性质和催化剂含量。结果表明,这些反应因子的最佳值分别为nH(2)O / nXSiy(3)= 8-9 / 1(摩尔比),nEt(4)NOH / nXSiy(3)= 0.0045(摩尔比) 。乙腈作为溶剂的使用有利于产物的沉积和形成。较高沸点的I-丙醇的存在有利于较高的反应温度,这加速了八聚物的形成,减少了反应时间并最终增加了产率。利用FTIR,MS,H-1和Si-29 NMR对合成化合物的笼结构及其式(H2NCH2CH2CH2)(8)Si8O12进行了表征。 POSS-NH2的TG曲线表明,笼形化合物的分解温度高于热处理过程中的理论值,且热残留量高于理论值。 (c)2006年Wiley Periodicals,Inc.

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