CIESC Journal ›› 2021, Vol. 72 ›› Issue (2): 1001-1008.DOI: 10.11949/0438-1157.20200999

• Catalysis, kinetics and reactors • Previous Articles     Next Articles

Study on reaction characteristics of solution polymerization system for butyl rubber preparation in microreactor

HE Yuhang(),LIU Qingjie,LYU Yangcheng()   

  1. State Key Laboratory of Chemical Enginnering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
  • Received:2020-07-23 Revised:2020-11-02 Online:2021-02-05 Published:2021-02-05
  • Contact: LYU Yangcheng

微反应器内丁基橡胶溶液法制备体系的反应特性研究

何宇航(),刘晴捷,吕阳成()   

  1. 清华大学化学工程系,化学工程联合国家重点实验室,北京 100084
  • 通讯作者: 吕阳成
  • 作者简介:何宇航(1996—),男,博士研究生,heyh@mails.tsinghua.edu.cn
  • 基金资助:
    国家自然科学基金项目(21422603)

Abstract:

Reaction characteristics of solution polymerization system for butyl rubber preparation in microreactor has been studied. Results showed that polyisobutylene with Mn over 300000 can be quantitatively obtained in minutes when using H2O as proton source, EtAlCl2 as co-initiator, and keeping reaction temperature at -60℃, water concentration between 0 (control) and 0.27 mmol/L. Chain transfer was efficiently suppressed under this condition. Enhancing the initial mixing of reactants was good for improving product quality. Incorporating isoprene in the system will significantly decrease molecular weight of final products and reaction rate. Replacing EtAlCl2 with less acidic Et2AlCl can stabilize carbocation and inhibit chain transfer. Copolymer with Mn near 150000 can be obtained at -60℃, but the reaction rate was moderate and need further optimization of system water concentration to enhance this process.

Key words: butyl rubber, solution polymerization, microreactor, cationic polymerization, preparation, polymers

摘要:

研究了微反应器内丁基橡胶溶液法制备体系的反应规律。结果表明以H2O为质子源、EtAlCl2为共引发剂时,控制反应温度为-60℃、水含量在0(control)到0.27 mmol/L之间,可在分钟级时间内高转化率地得到数均分子量高于300000的聚异丁烯产品,此时链转移得到有效抑制,强化反应物料的初始混合对提升产品质量有利;引入异戊二烯会显著降低产物分子量和转化速度,可以通过使用酸性更弱的Et2AlCl代替EtAlCl2来稳定碳阳离子,抑制链转移,在-60℃下得到数均分子量接近150000的共聚产物,但反应速度缓慢,需要进一步优化和控制反应体系中的水含量来强化该过程。

关键词: 丁基橡胶, 溶液聚合, 微反应器, 阳离子聚合, 制备, 聚合物

CLC Number: