Disproportionation Termination Mechanism in the Free-radical Polymerization of Methyl Methacrylate

LU Yun-tao; JIANG Li; JIANG Qi-min; HUANG Wen-yan; JIANG Bi-biao

doi:10.14028/j.cnki.1003-3726.2023.02.011

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Disproportionation Termination Mechanism in the Free-radical Polymerization of Methyl Methacrylate

更新时间：2022-12-29

- Disproportionation Termination Mechanism in the Free-radical Polymerization of Methyl Methacrylate
- Polymer Bulletin Vol. 36, Issue 2, Pages: 241-247(2023)
- 作者机构：
  
  常州大学材料科学与工程学院，常州　213164
- 作者简介：
- 基金信息：
- DOI：10.14028/j.cnki.1003-3726.2023.02.011
  CLC：
- Published：20 February 2023，
  
  Received：26 April 2022，
  
  Revised：11 May 2022，
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LU Yun-tao, JIANG Li, JIANG Qi-min, HUANG Wen-yan, JIANG Bi-biao. Disproportionation Termination Mechanism in the Free-radical Polymerization of Methyl Methacrylate. [J]. Polymer Bulletin 36(2):241-247(2023)
DOI：

LU Yun-tao, JIANG Li, JIANG Qi-min, HUANG Wen-yan, JIANG Bi-biao. Disproportionation Termination Mechanism in the Free-radical Polymerization of Methyl Methacrylate. [J]. Polymer Bulletin 36(2):241-247(2023) DOI： 10.14028/j.cnki.1003-3726.2023.02.011.

摘要

首先用过氧化二苯甲酰(BPO)引发甲基丙烯酸甲酯(MMA)自由基聚合合成聚甲基丙烯酸甲酯(PMMA)

然后用偶氮二异丁腈(AIBN)为引发剂

研究PMMA中由歧化终止生成的末端双键与苯乙烯(St)的共聚合反应行为。采用体积排除色谱(SEC)、核磁共振波谱(NMR)对聚合物进行了分析表征。结果表明:与单体MMA相似

PMMA在化学位移

=6.20和5.47处有对应于聚合物末端双键氢的NMR信号。远程异核和近程异核相关NMR

C-NMR和DEPT-135 NMR分析和自由基共聚合实验确证:MMA自由基聚合的双基歧化终止为单一的链自由基末端

位甲基氢自由基转移机理

生成1

1-二取代甲基丙烯酸酯型双键。除双基歧化终止反应外

体系还明显地存在苯甲酰初级自由基和苯初级自由基与链自由基间的初级终止反应。

Abstract

Poly(methyl methacrylate) (PMMA) was prepared through free-radical polymerization using BPO as the initiator. Size-exclusion chromatography and several NMR analysis methods

including

H-NMR

CNMR

DEPT135-NMR

heteronuclear multiple-bond correlation

and heteronuclear single quantum correlation NMR were used to analyze the structure of the end vinyl group from disproportionation termination to disclose the mechanism.

H-NMR measurement indicates that there are two NMR proton resonances at

=6.20 and 5.47 ppm

the other NMR methods confirm that there is only one type of vinyl group formed from disproportionation and the transferred hydrogen radical comes from the side methyl group at the chain end. The polymerization behavior of the end vinyl group in PMMA provides further evidence to support the conclusion from NMR measurements. In addition

there is also marked primary termination besides disproportionation in the polymerization.

关键词

甲基丙烯酸甲酯自由基聚合歧化终止机理

Keywords

Methyl methacrylateFree-radical polymerizationDisproportionation

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常州大学材料科学与工程学院

The Institute of Polymer Science and Materials,Zhejiang University

Institute of Polymer Science, Zhongshan University

Polymerization Reaction Engineering Lab, Zhejiang University

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