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Polynorbornene and cis-1,4-polybutadiene multi-block copolymer and preparation method thereof

A multi-block copolymer and polynorbornene technology, which is applied in the field of polymer materials, can solve problems such as poor elasticity, product structure characterization, uncertain multi-block copolymer, etc., and achieve the effect of good elasticity and excellent elasticity

Pending Publication Date: 2021-04-16
NINGBO POLYTECHNIC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Gringolts et al. used olefin metathesis reaction to synthesize polynorbornene and polybutadiene multi-block copolymers using polynorbornene and polycyclooctadiene as raw materials. However, in the polybutadiene segment, cis-1, 4-The structure content is less than 20% (see Polymer Science, Series C, 2019, 61(1), 65-75), because the low cis content leads to the multi-block copolymer of polynorbornene and polybutadiene Poor elasticity
Patent CN102321247 discloses the method of adopting olefin metathesis reaction to modify rubber, and butadiene rubber is respectively mixed with Eucommia gum, natural rubber, styrene-butadiene rubber, neoprene rubber, butyl rubber, nitrile rubber, isoprene rubber, EPDM Rubber, polyurethane rubber, ABS thermoplastic elastomer or SBS thermoplastic elastomer react to modify butadiene rubber, but the patent does not use PNB in ​​the raw material, and does not characterize the product structure. It is not sure whether multi-block copolymerization is generated thing

Method used

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  • Polynorbornene and cis-1,4-polybutadiene multi-block copolymer and preparation method thereof
  • Polynorbornene and cis-1,4-polybutadiene multi-block copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 2g cis-1,4-polybutadiene (cis-1,4 structural unit content is 98%, weight average molecular weight (Mw) is 300,000, molecular weight distribution Mw / Mn=3.0) and 0.2g polynorbornene (the content of the cis structural unit is 20%, the weight average molecular weight (Mw) is 2 million, and the molecular weight distribution Mw / Mn=1.2) is dissolved in dichloromethane (50mL) to obtain a polymer solution; at 20°C, the first Add 1mL of dichloromethane solution of 20mg of Grubbs catalyst (the molar ratio of the double bond in the raw material is 1:1557) to the above polymer solution, react for 0.5h, add terminator and react for 2h; slowly add the obtained solution to 500mL The polymer was precipitated in ethanol, and after drying, 1.8 g of the multi-block copolymer containing polynorbornene and cis-1,4-polybutadiene was obtained.

[0024] use 13 CNMR analyzes the copolymer, the content of the polybutadiene segment in the polybutadiene copolymer is 93mol%; the content of the PNB ...

Embodiment 2

[0026] 0.5g cis-1,4-polybutadiene (cis-1,4 structural unit content is 98%, weight average molecular weight (Mw) is 300,000, molecular weight distribution Mw / Mn=3.0) and 2g polynorbornene (the content of the cis structural unit is 90%, the weight average molecular weight (Mw) is 1.3 million, and the molecular weight distribution Mw / Mn=1.5) is dissolved in tetrahydrofuran (50mL) to obtain a polymer solution; at 40°C, will contain 100mg of the second Substitute Grubbs catalyst (the molar ratio of the double bond in the raw material is 1:256) tetrahydrofuran solution 1mL is added in the above-mentioned polymer solution, after reacting for 15h, add terminator to react for 12h; The solution obtained is slowly added in 300mL ethanol, and The polymer was precipitated, and after drying, 2.1 g of the multi-block copolymer containing polynorbornene and cis-1,4-polybutadiene was obtained.

[0027] use 13CNMR analyzes the copolymer, the content of the polybutadiene segment in the polybuta...

Embodiment 3

[0029] 2g cis-1,4-polybutadiene (cis-1,4 structural unit content is 98%, weight average molecular weight (Mw) is 80,000, molecular weight distribution Mw / Mn=3.0) and 2g polynorbornene ( The cis structural unit content is 40%, the weight average molecular weight (Mw) is 100,000, and the molecular weight distribution Mw / Mn=1.4) is dissolved in toluene (50mL) to obtain polymer solution; At 70 ℃, the third generation Grubbs catalyst 40mg (the molar ratio of the double bond in the raw material is 1:1210) of toluene solution 1mL was added to the above polymer solution, after 10 hours of reaction, a terminator was added to react for 2 hours; the obtained solution was slowly added to 1000mL of ethanol, and the polymerization After drying, 3.5 g of the multi-block copolymer containing polynorbornene and cis-1,4-polybutadiene was obtained.

[0030] use 13 CNMR analyzes the copolymer, the content of the polybutadiene segment in the polybutadiene copolymer is 65mol% in the copolymer; the...

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Abstract

The invention belongs to the field of high polymer materials, and particularly relates to a polynorbornene and cis-1,4-polybutadiene multi-block copolymer and a preparation method thereof. The structure of the multi-block copolymer is as follows: the content of a polybutadiene chain segment in the multi-block copolymer is 5-95 mol%, the content of cis-1,4 structure in the polybutadiene chain segment is 75-99 mol%, the content of a PNB chain segment is 5-95 mol%, and the content of cis- structure in the PNB chain segment is 8-95 mol%; the average molecular weight of the polybutadiene chain segment and the PNB chain segment is 500-80000; the average number of blocks of the copolymer is 3-120. The copolymer disclosed by the invention integrates excellent properties of polynorbornene and butadiene rubber, the 1,4-polybutadiene structural unit with a high cis- content has good elasticity, so that the copolymer has excellent elasticity, the PNB structural unit endows the copolymer with a thermally induced shape memory function, and the lengths and proportions of the two structural units can be regulated and controlled, and therefore, the regulation and control on the copolymer performance are realized.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a multi-block copolymer of polynorbornene and cis-1,4-polybutadiene and a preparation method thereof. Background technique [0002] Norbornene is polymerized by ring-opening metathesis to obtain polynorbornene (PNB), whose trade name is Norsorex, which is a new type of unsaturated polymer material. PNB can be blended with various elastomers or rubbers to increase the strength of the compound. In addition, PNB also has a thermally induced shape memory function, and can be restored to its original shape by heating even in the case of a large deformation, but it also has the defects of high brittleness and poor processability. Cis polybutadiene, referred to as butadiene rubber for short, is a synthetic rubber with regular structure formed by the polymerization of butadiene, and its cis structure content is above 95%. Butadiene rubber has excellent cold resistance, wear resistance ...

Claims

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Application Information

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IPC IPC(8): C08G81/02
Inventor 陈艳君李爱元
Owner NINGBO POLYTECHNIC