摘要
以多面体低聚八苯基硅倍半氧烷（OPS）和发烟硝酸为原料,控制硝化温度为12℃~15℃,系统研究了硝酸质量分数和硝化时间对硝基苯基硅倍半氧烷（NPS）硝化度的影响。利用元素分析、红外、核磁和凝胶渗透色谱对八硝基苯基硅倍半氧烷（ONPS）的化学结构进行了表征。结果表明,控制硝化时间为20 h,随初始硝酸质量分数的降低,对OPS的硝化能力逐渐减弱,当初始硝酸质量分数为90.06%,硝化时间为20 h时,可制得八硝基苯基硅倍半氧烷,其硝化位置发生在间位和对位,比例约为33.2%和66.8%;在90.06%的初始硝酸质量分数,随硝化时间的延长,硝化度会有所增加,但硝化度不会超过8。
Nitrification of polyhedral oligomeric octaphenylsilsesquioxane（OPS） by fuming nitric acid was studied to synthesize the octanitrophenylsilsesquioxane（NPS）.Effects of the concentration and the nitrification time of nitric acid on numbers of nitryl groups in NPS molecule were investigated by controlling the nitrification temperature at 12 ℃～15 ℃.The chemical structure and molecule weight of NPS were characterized by elementary analysis,FT-IR,1H-NMR and GPC.Controlling the nitrification time at 20 h,it was found that the lower nitric acid concentration,the weaker nitrification ability to OPS.NPS of one nitryl group on every phenyl could be prepared when the initial nitric acid concentration was 90.06 % and the nitrification time was up to 20 h.With the initial nitric acid concentration of 90.06%,number of the nitryl groups of every NPS molecule increased with the nitrification time increasing,but maximum number of the nitryl groups was not more than 8.
出处
《高分子材料科学与工程》
EI
CAS
CSCD
北大核心
2012年第7期144-147,共4页
Polymer Materials Science & Engineering
基金
国家863计划(2007AA03Z538)
关键词
八苯基硅倍半氧烷
八硝基苯基硅倍半氧烷
硝酸
硝化度
octaphenylsilsesquioxane
octanitrophenylsilsesquioxane
fuming nitric acid
nitrification
