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A kind of controllable preparation method of conjugated diene and polar olefin monomer copolymer

A conjugated diene and polar olefin technology, which is applied in the field of controllable preparation of conjugated diene and polar olefin monomer copolymers, can solve the problems of complex process, wide molecular weight distribution, difficult control, etc. Simple, narrow molecular weight distribution, high molecular weight effect

Active Publication Date: 2022-08-05
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the technical problems of the existing traditional copolymerization method of conjugated dienes and polar monomers, which are complicated and difficult to control, the separation of products is complicated, and the obtained polymerization products have small molecular weight, wide molecular weight distribution, residual emulsifier and difficult microstructure regulation. , and provides a controllable preparation method for copolymers of conjugated dienes and polar olefin monomers

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  • A kind of controllable preparation method of conjugated diene and polar olefin monomer copolymer
  • A kind of controllable preparation method of conjugated diene and polar olefin monomer copolymer
  • A kind of controllable preparation method of conjugated diene and polar olefin monomer copolymer

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Embodiment 1

[0027] Embodiment 1: The controllable preparation method of a conjugated diene and polar olefin monomer copolymer of the present embodiment is carried out according to the following steps:

[0028] Under argon atmosphere, in a 50mL reaction flask, add azobisisobutyronitrile (AIBN, 3.7mg, 23μmol, 1equiv.), 2.2mL of toluene solution, and then add methyl acrylate (2.1mL, 23mmol, 1000equiv. ) and isoprene (2.3 mL, 23 mmol, 1000 equiv.) to form a homogeneous solution, which was polymerized at 70 °C for 24 h, quenched with cold methanol, the polymer was precipitated, washed twice with methanol, and dried in vacuo to constant weight, A colloidal polymer, ie a copolymer of conjugated diene and polar olefin monomers, is obtained.

[0029] Result: Yield 71%. The NMR characterization showed that the 1,4-selectivity content of the polyisoprene segment was 96%, and the 3,4-selectivity content was 4%. The polar monomer methyl acrylate content is 39%; characterized by GPC: M n It was 5103...

Embodiment 2

[0032] Embodiment 2: The controllable preparation method of a conjugated diene and polar olefin monomer copolymer of the present embodiment is carried out according to the following steps:

[0033] Under argon atmosphere, in a 50mL reaction flask, add azobisisobutyronitrile (AIBN, 3.7mg, 23μmol, 1equiv.), 4.4mL of toluene solution, and then add methyl acrylate (2.1mL, 23mmol, 1000equiv. ) and isoprene (2.3 mL, 23 mmol, 1000 equiv.) to form a homogeneous solution, which was polymerized at 70 °C for 24 h, quenched with cold methanol, the polymer was precipitated, washed twice with methanol, and dried in vacuo to constant weight, A colloidal polymer, ie a copolymer of conjugated diene and polar olefin monomers, is obtained.

[0034] Result: The yield was 62%. The NMR characterization showed that the 1,4-selectivity content of the polyisoprene segment was 96%, and the 3,4-selectivity content was 4%. The polar monomer methyl acrylate content is 38%; characterized by GPC: M n It ...

Embodiment 3

[0035] Embodiment 3: The controllable preparation method of a conjugated diene and polar olefin monomer copolymer of the present embodiment is carried out according to the following steps:

[0036] Under argon atmosphere, in a 50mL reaction flask, add azobisisobutyronitrile (AIBN, 3.7mg, 23μmol, 1equiv.), 22mL of toluene solution, and then add methyl acrylate (2.1mL, 23mmol, 1000equiv.) and isoprene (2.3 mL, 23 mmol, 1000 equiv.) to form a homogeneous solution, which was polymerized at 70 °C for 24 h, quenched with cold methanol to precipitate a polymer, washed twice with methanol, and dried in vacuo to constant weight to obtain Gum-like polymers, ie, copolymers of conjugated dienes and polar olefin monomers.

[0037] Result: Yield 53%. The NMR characterization showed that the 1,4-selectivity content of the polyisoprene segment was 95%, and the 3,4-selectivity content was 5%. The polar monomer methyl acrylate content is 38%; characterized by GPC: M n It was 19820 g / mol, and...

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Abstract

A controllable preparation method of conjugated diene and polar olefin monomer copolymer. The present invention belongs to the field of free radical polymerization. The present invention solves the technical problems that the existing traditional copolymerization method of conjugated diene and polar monomer is complicated and difficult to control, product separation is complicated, and the obtained polymer product has small molecular weight, wide molecular weight distribution, emulsifier residue and difficulty in microstructure control. . The preparation method of the present invention: in an argon atmosphere, the free radical initiator, polar olefin monomer, conjugated diene and solvent are added to the reaction system in any order to form a homogeneous solution, and polymerized at 50-100 DEG C The reaction is carried out for 2 hours to 48 hours to obtain a copolymer of conjugated diene and polar olefin monomer; the free radical initiator is an azo-based free-radical initiator or a peroxy-based free-radical initiator. The method of the invention has simple polymerization process and strong universality, can realize arbitrary copolymerization of various conjugated dienes and polar monomers, the obtained polymer has high molecular weight, narrow molecular weight distribution, and no other impurities remain.

Description

technical field [0001] The invention belongs to the field of free radical polymerization, in particular to a controllable preparation method of a conjugated diene and polar olefin monomer copolymer. Background technique [0002] The polymer obtained by polymerizing conjugated diene as monomer is one of the main materials of synthetic rubber. According to its excellent stereoselectivity, mechanical properties, thermal stability and processing properties, it is widely used in aviation, automobile tires, Health care and many areas of daily life. However, because the obtained polyolefin is a non-polar chain, its printability and compatibility with other materials are poor, which greatly limits the application range of polyconjugated diene materials. The introduction of polar groups or polar polymer chains solves this problem well, improves the surface wettability, coloring, oil resistance, heat resistance, adhesion, etc. Compatibility with other polymer materials and rubber vu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F236/08C08F220/14C08F220/18C08F220/44C08F236/14C08F236/06C08F236/22C08F2/06
CPCC08F236/08C08F220/14C08F220/1804C08F220/44C08F236/14C08F236/06C08F236/22C08F2/06
Inventor 王庆刚朱广乾王亮周丽匡佳
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI