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Polydicyclopentadiene composite material and preparation method thereof

A technology for polydicyclopentadiene and dicyclopentadiene is applied in the field of polydicyclopentadiene composite materials and their preparation, which can solve the problems of affecting product performance, difficult to achieve mixing effect, etc., so as to achieve cost saving of raw materials and uniform and compact products , high active effect

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

[0005] The RIM process routinely uses two materials A and B to be mixed and injected at a ratio of 1:1. However, when the ruthenium carbene catalyst is used, the ratio of A and B materials is 1000-10000:1. It is difficult to achieve the mixing effect by using traditional technology, which affects product performance.

Method used

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  • Polydicyclopentadiene composite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 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)

[0028] (1) Configure catalyst solution A

[0029] 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.

[0030] (2) configure dicyclopentadiene solution B

[0031] 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 the protection of nitrogen, fully stir evenly on the low temperature reaction bath, control the temperature at ...

Embodiment 2

[0037] 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)

[0038] (1) Configure catalyst solution A

[0039] 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.

[0040] (2) configure dicyclopentadiene solution B

[0041] 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 the protection of nitrogen, fully stir evenly on the low temperature reaction bath, control the temperature at 10-30...

Embodiment 3

[0047]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 20000:1 (mass ratio is about 3000:1)

[0048] (1) Configure catalyst solution A

[0049] 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.

[0050] (2) configure dicyclopentadiene solution B

[0051] 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 the protection of nitrogen, fully stir evenly on the low temperature reaction bath, control the temperature at 10-30 ...

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Abstract

The invention relates to the field of high polymer materials, in particular to a polydicyclopentadiene composite material and a preparation method thereof. The polydicyclopentadiene composite material comprises the following components in mass ratio: the mass ratio of a dicyclopentadiene monomer to a catalyst is (5000-50000): 1, and the mass ratio of the dicyclopentadiene monomer to an antioxidant is 100: (0.01-2). The preparation method comprises the following steps of: mixing an organic solvent in which dicyclopentadiene and an antioxidant are dissolved and an organic solvent in which a catalyst is dissolved through a multi-section tubular mixer, immediately injecting the mixture into a mold, carrying out reaction molding at 40-80 DEG C, and carrying out post-treatment at 120-150 DEG C. A multi-section tubular micro-channel mixing polymerization process is adopted, so that the mixing effect is greatly improved, the dosage of a catalyst is reduced, the production process is simple, and the obtained polydicyclopentadiene composite material is excellent in performance.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a polydicyclopentadiene composite material and a preparation method thereof. Background technique [0002] Polydicyclopentadiene (PDCPD) is a new type of engineering plastic, which is polymerized by dicyclopentadiene (DCPD) under the action of a ring-opening metathesis catalyst. It has good heat resistance, creep resistance, size Stability, corrosion resistance, wear resistance and other characteristics. At present, the catalyst system used in the preparation of polydicyclopentadiene includes tungsten-molybdenum complexes or carbene catalysts of molybdenum and ruthenium. The process used is the reaction injection molding (RIM) process, which has the advantages of fast molding speed, high efficiency and low energy consumption. , can be used to manufacture various large thin-walled and complex-shaped parts. [0003] The PDCPD material processed by RIM technology has e...

Claims

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Application Information

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IPC IPC(8): C08F132/08C08F232/08C08F236/20C08F4/80C08F2/01B01F13/00B01F3/08
CPCC08F132/08C08F232/08C08F4/80C08F2/01B01F23/45B01F33/30C08F236/20
Inventor 周飞翁羽飞蒋方红奚军许艾娜罗群
Owner CHINA PETROLEUM & CHEM CORP