MEASUREMENTS AND CONTROL OF THE MICROSTRUCTURE OF ETHYLENE-PROPYLENE COPOLYMERS

Jing-shan Mu; Yue-sheng Li

doi:10.3724/SP.J.1105.2013.13111

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MEASUREMENTS AND CONTROL OF THE MICROSTRUCTURE OF ETHYLENE-PROPYLENE COPOLYMERS

Research Article | 更新时间：2021-03-19

- MEASUREMENTS AND CONTROL OF THE MICROSTRUCTURE OF ETHYLENE-PROPYLENE COPOLYMERS
- Acta Polymerica Sinica Issue 12, Pages: 1492-1500(2013)
- 作者机构：
  
  1. 宁波大学材料科学与化学工程学院,宁波,315211
  2. 中国科学院长春应用化学研究所高分子物理和化学国家重点实验室,长春,130022
- 作者简介：
- 基金信息：
- DOI：10.3724/SP.J.1105.2013.13111
  CLC：
- Published：20 December 2013，
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Jing-shan Mu, Yue-sheng Li. MEASUREMENTS AND CONTROL OF THE MICROSTRUCTURE OF ETHYLENE-PROPYLENE COPOLYMERS. [J]. Acta Polymerica Sinica (12):1492-1500(2013)
DOI：

Jing-shan Mu, Yue-sheng Li. MEASUREMENTS AND CONTROL OF THE MICROSTRUCTURE OF ETHYLENE-PROPYLENE COPOLYMERS. [J]. Acta Polymerica Sinica (12):1492-1500(2013) DOI： 10.3724/SP.J.1105.2013.13111.

摘要

研究了[N，O]螯合钒（Ⅲ）催化剂（[PhN=C（CH3）CH=C（Ph）O]VCl2（THF）2（2a），[PhN=CHC6H4O]VCl2（THF）2（2b）和 [PhN=CHC（Ph） CHO]VCl2（THF）2（2c）催化乙烯和丙烯的共聚合行为.聚合得到了不同丙烯插入率（0 mol%~20 mol%）和较窄分布（Mw/Mn3.0）的聚合物.借助高温核磁13C-NMR和高温GPC对所得聚合物的共单体插入率、序列结构、分子量及分布进行测试.研究表明，助催化剂、再活化剂、聚合温度以及反应时间等条件对聚合活性、聚合物分子量以及共单体插入率有重大影响.通过计算亚甲基序列分布（xi）以及聚合物链中连续亚甲基数均序列长度n0和n2+，证实了上述条件还能够对聚合物微结构起到微调作用.此外，虽然催化剂的共聚合活性相当，而且所得聚合物中共单体插入率也很接近，但是通过比较不同催化剂所获的聚合物的xi，n0和n2+，所得聚合物的序列结构却有明显差别，2a 催化体系最不容易发生单体的反向插入，而且链结构中存在更多长的亚甲基序列.通过Fineman-Ross方法计算出单体的竞聚率乘积rErP1.0，说明共单体的插入不受链末端单体单元种类的影响，使得k11/k12=k21/k22，催化剂 2a ~ 2c 均能催化乙烯与丙烯共聚合得到理想的无规共聚物.

Abstract

The copolymerizations of ethylene with propylene were investigated by the vanadium (Ⅲ) catalysts bearing bidentate [N

O] ligands (2a

[PhN=C(CH3)CHC(Ph)O]VCl2(THF)2; 2b

[PhN=CHC6H4O]VCl2(THF)2; 2c

[PhN=CHC(Ph)CHO]VCl2(THF)2).Ethylene-propylene copolymers with different comonomer incorporations (P=0 mol%~20 mol%) and narrow molecular weight distributions (Mw/Mn 3.0) were obtained.The molecular weights and molecular weight distribution of copolymers were determined by gel permeation chromatograhpy (GPC).The incorporation of comonomer and microstructure of copolymers were confirmed by 13C-NMR methods.On activation with cocatalyst (Et2AlCl) and reactive agent (ETA)

catalytic activity

comonomer incorporation

and molecular weights of the resultant polymers can be controlled over a wide range by tuning reaction parameters

such as concentration of Et2AlCl

dosage of ETA

temperature

feed composition and so on.Furthermore

the microstructures of polymer chains can also be adjusted by changing reaction parameters above

which were confirmed by calculating the monomer sequence distribution (xi) and continuous methylene sequence length (n0 and n2+).The reactivity ratios of copolymerization (r1r2 1.0) were evaluated by the Fineman-Ross method

indicating the insertion of comonomers will not be influnced by the kinds of the last inserted monomers

and ideal random copolymer can be obtained by catalysts 2a ~ 2c

which can also be proved by 13C-NMR and calculation of xi

n0 and n2+.

关键词

共聚合序列分布竞聚率无规共聚物

Keywords

CopolymerizationSequence distributionReactivity ratioRandom copolymer

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Related Institution

Department of Polymer Science and Engineering, University of Science and Technology of China

State Key Laboratory of Fine Chemicals, Department of Polymer Science and Engineering, School of Chemical Engineering, Dalian University of Technology

Key Laboratory of Polymer Ecomaterials, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences

School of Applied Chemistry and Engineering, University of Science and Technology of China

School of Materials Science and Engineering, Shenyang Ligong University

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