笼形八(氨基苯基)硅倍半氧烷的合成与表征

Synthesis and Characterization of Octa(aminophenyl) Polyhedral Silsesquioxane

摘要: 以三氯化铁/活性炭为催化剂,用水合肼还原法合成了笼形八(氨基苯基)硅倍半氧烷,收率达到93%.利用傅里叶变换红外光谱、核磁共振光谱、元素分析和热分析等手段,对其结构和性质进行了表征.得到氨基以对位取代为主的产物,其失重5%时对应的温度为338.8℃,热稳定性较高.提出了Fe3+作为活性反应中心、活性炭作为吸附剂和导电体的三氯化铁/活性炭催化水合肼还原芳香族硝基化合物的反应机理.

Abstract: In the presence of FeCl3·6H2O/C catalyst,octa(nitrophenyl) polyhedral silsesquioxane(ONPS) was successfully reduced to octa(aminophenyl) polyhedral silsesquioxane (OAPS) using hydrazine hydrate with a yield of 93%.Structure and properties of OAPS are characterized by means of FTIR,NMR,elemental and thermal analysis.Its temperature corresponding to 5% weight loss is 338.8 ℃.This shows that OAPS has a high stability to heat.At the same time,mechanism of the reduction of ONPS by hydrazine catalyzed by FeCl3/C was proposed.