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Dicyclopentadiene-ethylidene norbornene copolymer and preparation method thereof

A technology of ethylidene norbornene and dicyclopentadiene is applied in the field of dicyclopentadiene-ethylidene norbornene copolymer and its preparation, and can solve the problems of complicated process, complicated operation and the like

Pending Publication Date: 2021-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome dicyclopentadiene copolymerization because bimetallic catalysts are sensitive to water and oxygen and high-purity dicyclopentadiene is a crystal at room temperature, resulting in complicated process and complicated operation, the present invention provides a dicyclopentadiene-ethylidene norbornene Dicyclopentadiene-ethylidene norbornene copolymer and its preparation method simplify the formula raw material types of dicyclopentadiene-ethylidene norbornene copolymer, adjust the proportion of formula raw materials, reduce the amount of catalyst, simplify the preparation process, and obtain strength, impact toughness and thermal stability. good copolymer

Method used

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  • Dicyclopentadiene-ethylidene norbornene copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] This example is used to illustrate the preparation method of dicyclopentadiene homopolymer when the amount ratio of dicyclopentadiene and catalyst substance in the present invention is 5000:1 (mass ratio is about 800:1)

[0029] (1) Configure catalyst solution A

[0030] Grubbs second-generation catalyst (424.5 mg, 0.5 mmol) was weighed in a glove box, and dissolved in 10.6 ml of dichloromethane to prepare a 40 mg / ml catalyst solution.

[0031] (2) configure dicyclopentadiene solution B

[0032] Add excess calcium hydride to dicyclopentadiene (purity greater than 95%), stir at 80°C for 12 hours under nitrogen protection, refine under reduced pressure, and then add dichloromethane solvent with 2%-5% dicyclopentadiene mass Fully dissolve in advance. Add dicyclopentadiene mass 0.01%-2% antioxidant (o-di-tert-butyl p-cresol) to the dicyclopentadiene solution under nitrogen protection, fully stir evenly on the low-temperature reaction bath, and control the temperature at 1...

Embodiment 2

[0038]This example is used to illustrate the preparation method of dicyclopentadiene homopolymer when the ratio of dicyclopentadiene and catalyst substance in the present invention is 10000:1 (mass ratio is about 1500:1)

[0039] (1) Configure catalyst solution A

[0040] Grubbs second-generation catalyst (424.5 mg, 0.5 mmol) was weighed in a glove box, and dissolved in 10.6 ml of dichloromethane to prepare a 40 mg / ml catalyst solution.

[0041] (2) configure dicyclopentadiene solution B

[0042] Add excess calcium hydride to dicyclopentadiene (purity greater than 95%), stir at 80°C for 12 hours under nitrogen protection, refine under reduced pressure, and then add dichloromethane solvent with 2%-5% dicyclopentadiene mass Fully dissolve in advance. Add 0.01%-2% antioxidant of dicyclopentadiene mass to the dicyclopentadiene solution under nitrogen protection, fully stir evenly on a low-temperature reaction bath, and control the temperature at 10-30°C.

[0043] (3) Hybrid cur...

Embodiment 3

[0048] This example is used to illustrate the preparation method of dicyclopentadiene homopolymer when the ratio of dicyclopentadiene and catalyst substance in the present invention is 15000:1 (mass ratio is about 2300:1)

[0049] (1) Configure catalyst solution A

[0050] Grubbs second-generation catalyst (424.5 mg, 0.5 mmol) was weighed in a glove box, and dissolved in 10.6 ml of dichloromethane to prepare a 40 mg / ml catalyst solution.

[0051] (2) configure dicyclopentadiene solution B

[0052] Add excess calcium hydride to dicyclopentadiene (purity greater than 95%), stir at 80°C for 12 hours under nitrogen protection, refine under reduced pressure, and then add dichloromethane solvent with 2%-5% dicyclopentadiene mass Fully dissolve in advance. Add 0.01%-2% antioxidant of dicyclopentadiene mass to the dicyclopentadiene solution under nitrogen protection, fully stir evenly on a low-temperature reaction bath, and control the temperature at 10-30°C.

[0053] (3) Hybrid cu...

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Abstract

The invention relates to the field of high polymer materials, in particular to a dicyclopentadiene-ethylidene norbornene copolymer and a preparation method thereof. The dicyclopentadiene-ethylidene norbornene copolymer comprises the following components in mass ratio: the mass ratio of a dicyclopentadiene monomer to a catalyst is (5000-50000): 1, the mass ratio of the dicyclopentadiene monomer to ethylidene norbornene is 100: (5-50), and the mass ratio of the dicyclopentadiene monomer to an antioxidant is 100: (0.01-2). The preparation method comprises the following steps of: fully and uniformly mixing an organic solvent in which dicyclopentadiene, ethylidene norbornene and the antioxidant are uniformly dissolved and an organic solvent in which the catalyst is uniformly dissolved, immediately injecting the mixture into a mold, carrying out curing molding at 40-80 DEG C, and carrying out post-treatment at 120-150 DEG C. The dicyclopentadiene-ethylidene norbornene copolymer disclosed by the invention has the advantages that the types of formula raw materials of the dicyclopentadiene-ethylidene norbornene copolymer are simplified, the ratio of the formula raw materials is adjusted, the dosage of the catalyst is reduced, the preparation process is simplified, and the copolymer with good strength, impact toughness and thermal stability is obtained.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a dicyclopentadiene-ethylidene norbornene copolymer and a preparation method thereof. Background technique [0002] Polydicyclopentadiene engineering plastic is a new type of engineering material with good mechanical properties. It has high tensile, flexural modulus and good impact strength. It also has relatively high heat distortion temperature and thermal stability. And acid and alkali resistance, and polydicyclopentadiene is a pure broken hydrocarbon, does not produce harmful substances when burned, can be recycled, energy saving and environmental protection, is a very good environment-friendly material, is a high-tech encouraged by the state, so in The automotive industry, construction machinery manufacturing, medical sports equipment, petrochemical pipelines, civil facilities and other fields have shown extremely broad application prospects. Especially famous c...

Claims

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Application Information

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IPC IPC(8): C08F232/08C08F236/20C08F4/80
CPCC08F232/08C08F4/80C08F236/20
Inventor 周飞何雪莲杨再兴翁羽飞奚军蒋方红罗群
Owner CHINA PETROLEUM & CHEM CORP
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