摘要
采用变温气相收集和恒温溶剂分级的方法采集了二氯化镁负载四氯化钛催化体系合成的反式-丁二烯-异戊二烯共聚橡胶(TBIR)中的可挥发及低分子量组份。采用核磁共振氢谱(^(1)H-NMR)、凝胶渗透色谱仪(GPC)及气相色谱/质谱联用仪(GC-MS)对收集的各组份进行表征。结果表明,沸腾乙醚抽提可溶物组份含量约50%(wt),由低分子量的反式-丁二烯-异戊二烯共聚橡胶及少量丁二烯与异戊二烯的二聚体和低聚物组成;丙酮可溶物组份含量约7.6%(wt),由聚合过程中助催化剂三异丁基铝引发生成的重均分子量为几百的异戊二烯-丁二烯二聚体和/或多聚体构成;低温气相收集挥发物组份中主要是异戊二烯单体,随气相收集温度的升高,挥发物中单体含量减少,异戊二烯-丁二烯二聚体出现并逐渐增加。
The low molecular weight fractions and volatile components of the trans-butadiene-co-isoprene copolymer rubber(TBIR), which synthesized by using the MgCl2 supported TiCl4 catalyst system, are collected by using constant temperature solvent fractionation and variable temperature gas phase collection methods. The collected components are characterized by 1H nuclear magnetic resonance(^(1)H-NMR), gel permeation chromatography(GPC) and gas chromatography/mass spectrometry(GC-MS). The results show that the content of ether soluble fraction is about 50%(wt). The ether soluble fraction is composed of high trans-butadiene-co-isoprene copolymers with lower molecular weight and a small amount of butadiene-isoprene dimer and oligomer. The content of acetone soluble component is about 7.6%(wt). The acetone soluble component is composed of isoprene-butadiene dimers and/or copolymers with the weight average molecular weight about several hundreds. The as-obtained copolymers and dimmers may generate during the copolymerization process by the triisobutyl aluminium cocatalyst. The volatile component obtained by the low temperature gas phase collection is mainly isoprene monomer residual in TBIR. With the increasing of the gas phase collection temperature, there appears butadiene-isoprene dimer and the content of butadiene-isoprene dimer increases as while as the content of isoprene in the volatile component decreases.
作者
任淑亭
邵华锋
贺爱华
REN Shu-ting;SHAO Hua-feng;HE Ai-hua(Shandong Key Laboratory of Olefin Catalysis and Polymerization,Key Laboratory of Ministry of Rubber and Plastic Materials and Engineering Education,College of Polymer Science and Engineering,Qingdao University of Science and Technology,Qingdao 266042,China)
出处
《高分子通报》
CAS
CSCD
北大核心
2021年第10期66-72,共7页
Polymer Bulletin
基金
国家自然科学基金
山东省重大基础研究项目(项目号ZR2017ZA0304)
泰山学者工程资助。
关键词
反式丁戊共聚橡胶
溶剂分级
挥发物
GC-MS
低聚物
trans-Butadiene-co-isoprene copolymer rubber
Solvent fractionation
Volatile
GC-MS
Oligomer
