Preparation and thermostability of terpenes/sulfur oligomer

REN Yuanyuan; XU Kai; PENG Jun; XING Yuxiu; GAO Shuxi; CHEN Mingcai

doi:10.11949/j.issn.0438-1157.20151351

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Preparation and thermostability of terpenes/sulfur oligomer

更新时间：2025-12-10

- Preparation and thermostability of terpenes/sulfur oligomer
- CIESC Journal Issue 4, Pages: 1580-1585(2016)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20151351
  CLC： 633.3
- Online First：05 April 2016，
  
  Published：05 April 2016
- 稿件说明：
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REN Yuanyuan, XU Kai, PENG Jun, et al. Preparation and thermostability of terpenes/sulfur oligomer[J]. CIESC Journal, 2016, (4): 1580-1585.
DOI：

REN Yuanyuan, XU Kai, PENG Jun, et al. Preparation and thermostability of terpenes/sulfur oligomer[J]. CIESC Journal, 2016, (4): 1580-1585. DOI： 10.11949/j.issn.0438-1157.20151351.

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13C 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。

Abstract

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

13C 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.

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