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以环梯形聚苯基硅倍半氧烷(CL-PPSQ)为原料,采用HNO_3-(CH_3CO)_2O硝化体系,在不同的条件下对其进行硝化,制备得到含硝基基团的NO_2-PPSQ.使用GPC、TGA、~1H NMR、FTIR、元素分析等测试手段对硝化产物进行表征.结果表明,75%HNO_3-(CH_3CO)_2O硝化过程温和,硝化能力适中,制备得到分子链不断裂且实现了苯基完全一硝化的硝化产物.对不同硝化试剂的硝化机理进行了分析,在发烟硝酸、HNO_3-H_2SO_4、KNO_3-H_2SO_4中,NO_2~+为硝化活化剂,硝化能力强,会导致CL-PPSQ分子链断裂;对于HNO_3-(CH_3CO)_2O体系,CH_3COONO_2为主要的硝化活化剂,硝化能力适中.
The ring-shaped polyphenylsilsesquioxane (CL-PPSQ) was used as raw material to nitrify the system under different conditions with HNO_3- (CH_3CO) _2O nitration system to prepare NO_2-PPSQ The nitration products were characterized by GPC, TGA, 1H NMR, FTIR and elemental analysis.The results showed that the nitration of 75% HNO_3- (CH_3CO) _2O was moderate and nitration was moderate, and the molecular chain was not broken and realized The nitration products of phenyl mononitration were analyzed.The nitration mechanism of different nitration reagents was analyzed.NO 2 + was nitrification activator in fuming nitric acid, HNO 3 -H 2 SO 4, KNO 3 -H 2 SO 4, -PPSQ molecular chain breakage; CH_3COONO_2 is the main nitration activator for HNO_3- (CH_3CO) _2O system with moderate nitrification ability.