文献类型：期刊文献

中文题名：含硅芳炔树脂合成工艺优化

英文题名：Synthesis process optimization of poly-silicon-containing arylacetylene resin

作者：程利[1];邓诗峰[1];杜磊[1];周燕[1]

机构：[1]华东理工大学特种功能高分子材料及相关技术教育部重点实验室,上海200237

年份：2016

卷号：31

期号：1

起止页码：34

中文期刊名：热固性树脂

外文期刊名：Thermosetting Resin

收录：CSTPCD;;北大核心:【北大核心2014】；CSCD:【CSCD2015_2016】；

语种：中文

中文关键词：含硅芳炔树脂;2-甲基四氢呋喃;合成;工艺优化;热稳定性

外文关键词：poly-silicon-containing arylacetylene resin; 2-methyltetrahydrofuran; synthesis; process optimization; thermal stability

摘要：以二乙炔基苯和二甲基二氯硅烷为原料,2-甲基四氢呋喃为溶剂,合成了含硅芳炔树脂。采用核磁共振波谱、红外光谱、凝胶色谱、热失重分析和示差扫描量热分析研究了反应条件对树脂产率的影响,确定了最佳反应条件,并对树脂的结构和性能进行了表征。结果表明,2-甲基四氢呋喃与镁粉物质的量比为3∶1,反应温度85℃,反应时间1.5 h时合成树脂的产率达到93.8%。该树脂可在170℃固化,加工性能良好。树脂固化物具有优异的热稳定性,N_2气氛下5%热分解温度达到619℃,800℃下树脂残留率为91%左右。
The poly-silicon-containing arylacetylene resin was synthesized using diacetylene benzene and dimethyl dichlorosilane as raw materials and 2-methyhetrahydrofuran as a solvent. The effects of reaction conditions on the yield of the resin were investigated by nuclear magnetic resonance spectroscopy, infrared spectroscopy, gel chromatography, thermal gravimetric analysis and differential scanning calorimetry. The optimal reaction conditions were determined and the structure and properties of the resin were characterized. The results showed that the yield of synthetic resin reached 93.8% as the conditions as followed：molar ratio of 2- methyl-tetrahydrofuran to magnesium 3：1, reaction temperature 85℃ and reaction time 1.5 h. The resin could be cured at 170℃ and had good processing properties. The cured resin had excellent thermal stability. The 5% thermal decomposition temperature was up to 619 ℃ under N2 atmosphere and the resin residue at 800℃ was about 91%.