硫磺/萜烯低聚物的制备及其热稳定性  

Preparation and thermostability of terpenes/sulfur oligomer

作　　者：任圆圆[1,2] 许凯[1] 彭军[1,2] 邢玉秀[1,2] 高树曦 陈鸣才[1] 

机构地区：[1]中国科学院广州化学研究所,广东省电子有机聚合物材料重点实验室,广东广州510650 [2]中国科学院大学,北京100049

出　　处：《化工学报》2016年第4期1580-1585,共6页CIESC Journal

基　　金：国家自然科学基金项目(21174162)~~

摘　　要：以单萜烯烃(R)-(+)-苧烯为共聚单体,采用"反硫化"的方法将萜烯与单质硫磺直接混合进行本体熔融自由基共聚反应,得到具有良好溶解性的富硫低聚物。利用傅里叶变换红外光谱(FTIR)、核磁共振波谱(~~1H NMR和^(13)C NMR)、拉曼光谱(Raman)、元素分析(EA)和凝胶渗透色谱(GPC)对低聚物的化学结构和组成进行了表征,并且探索了投料比、反应时间以及反应温度对硫磺-萜烯低聚物(PSL)的结构和性能的影响。又采用热重分析(TGA)和差示扫描量热法(DSC)考察了该低聚物的热稳定性。结果表明:该聚合方法所制备产物具有良好的热稳定性、溶解性和粘接性。反应产物中硫磺的含量随硫磺投料的增多而增加。对于苧烯-硫磺的共聚物(PSL),当反应时间为2 h、反应温度为210℃时,所得产物综合性能最佳。How to develop a simple synthetic process to prepare novel materials with high sulfur content is still sorely lacking but urgent. Here a facile method which was termed ＂inverse vulcanization＂ to prepare thermally stable and processable polymeric materials was proposed through the direct radical copolymerization of elemental sulfur with limonene. FTIR, Raman spectroscopy, ^1H NMR, ^13 C NMR, elemental analysis（EA） and GPC were used to investigate the structural composition and molecular weight of the sulfur-limonene oligomers（PSL）. DSC and TGA were used to evaluate the thermal behavior of the obtained oligomers. Solubility experiments were also carried out to test whether these oligomers could be dissolved by several common organic solvents at room temperature. The results showed that the prepared sulfur-rich copolymers exhibited excellent thermostability, solubility and adhesion. The sulfur content in the obtained product increased with increasing initial feed ratios of sulfur. For PSL, when reaction time was 2 h and the reaction temperature was 210℃, the best product performance was obtained.

关 键 词：硫磺 萜烯 柠檬烯 反硫化 聚合 合成 稳定性 

分 类 号：O633.3[理学—高分子化学]