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An amine-based curing agent, a high-temperature-resistant epoxy resin containing the curing agent, its preparation method and application

A technology of epoxy resin and epoxy resin matrix, which is applied in the direction of epoxy resin glue, epoxy resin coating, adhesive, etc., can solve problems such as difficult to meet high temperature resistance, and achieve good bonding strength at room temperature, low energy consumption, and good durability Effect of High Temperature Aging Properties

Active Publication Date: 2021-10-29
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operating temperature of ordinary epoxy resins generally does not exceed 300°C, which has been difficult to meet the high temperature resistance requirements of epoxy resin materials with the continuous development of modern science and technology such as aerospace, aviation, and electronics.

Method used

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  • An amine-based curing agent, a high-temperature-resistant epoxy resin containing the curing agent, its preparation method and application
  • An amine-based curing agent, a high-temperature-resistant epoxy resin containing the curing agent, its preparation method and application
  • An amine-based curing agent, a high-temperature-resistant epoxy resin containing the curing agent, its preparation method and application

Examples

Experimental program
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Effect test

preparation example Construction

[0064] Preparation of amine-based curing agent containing m-carborane in structure A: Add 1 part of m-carborane to 2 parts of NaN under the protection of nitrogen flow 3 in toluene, stirred at 110°C and refluxed for 4h, filtered to remove excess NaN 3 And wash the filtrate with distilled water. Under the protection of nitrogen flow, the mixture was stirred and heated at 60°C for 2 hours. The reaction mixture was poured into ice water, the pH value of the mixture was adjusted to neutral with lye and extracted with ether, and anhydrous MgSO was added. 4 After removing the distilled water, the amine-based curing agent containing meta-carborane with the structure shown in formula (A): diamine-based meta-carborane can be obtained.

[0065] The preparation of the amine-based curing agent containing m-carborane in B structure: (1) the m-carborane of 1 part of substance is dissolved in the dry ethylene glycol dimethyl ether of 10 parts by volume, in an ice-water bath Under the prote...

Embodiment 1

[0068] Use novolac epoxy resin F51 as the epoxy resin matrix, use A-structure diamino-meta-carborane as the curing agent, and mix according to the mass ratio of F51 and A-structure diamino-meta-carborane as 100:20 , after curing at 180°C for 2 hours, a high temperature resistant cured epoxy resin was obtained.

[0069] Test the thermal weight loss of the cured product in an air atmosphere: the mass retention rate at 800 ° C is 76% ( figure 1 Curve e) in .

[0070] According to the bonding strength test, the bonding strength of the cured epoxy resin is 14.5MPa at room temperature, and 2.8MPa after aging in air at 600°C for 1 hour.

Embodiment 2

[0072] Take the novolac epoxy resin F44 as the epoxy resin matrix, take the bis (m-aminophenyl) m-carborane in the B structure as the curing agent, according to the quality of F44 and bis (m-aminophenyl) m-carborane The mixture was mixed at a ratio of 100:50, and cured at 160°C for 4 hours to obtain a high temperature resistant epoxy resin cured product.

[0073] Test the thermal weight loss of the cured product in an air atmosphere: the mass retention rate at 800 ° C is 71% ( figure 1 Curve d) in .

[0074] According to the bonding strength test, the bonding strength of the cured epoxy resin is 15.8 MPa at room temperature, and 2.6 MPa after aging in air at 600°C for 1 hour.

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Abstract

The invention discloses an amine-based curing agent, a high-temperature-resistant epoxy resin containing the curing agent, a preparation method and an application thereof. The amine-based curing agent has a structure shown in the following formula (C): the raw materials for the preparation of the epoxy resin include an epoxy resin matrix and an amine-based curing agent, and the amine-based curing agent includes a carboryl group and two amine groups , the two amine groups are respectively the end groups of the amine-based curing agent, the amine groups are directly connected to the carborane group, or the amine groups are respectively connected to the carborane group through an aromatic hydrocarbon structure, a silicon group or a siloxy group. The cured epoxy resin has good bonding strength at room temperature and can be used at a high temperature of 600°C. The epoxy resin is suitable as a high temperature resistant adhesive and a resin matrix of a high temperature resistant coating.

Description

technical field [0001] The invention belongs to the field of high-temperature-resistant materials, and relates to a high-temperature-resistant epoxy resin and a preparation method and application thereof. Background technique [0002] Epoxy resin has become an important resin matrix widely used in bonding sealing materials and coatings due to its good mechanical properties, especially strong adhesion to metals, low curing shrinkage, excellent chemical resistance and electrical insulation Material. However, the operating temperature of ordinary epoxy resins generally does not exceed 300°C, which has been difficult to meet the high temperature resistance requirements of epoxy resin materials for the continuous development of modern science and technology such as aerospace, aviation, and electronics. How to develop new technical methods to greatly improve the high temperature resistance of epoxy resin while maintaining its certain mechanical properties to meet the requirements...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C09J163/00C09D163/00
CPCC08G59/504C09D163/00C09J163/00
Inventor 张学忠张志杰崔美丽戴丽娜孔书轩汪倩
Owner INST OF CHEM CHINESE ACAD OF SCI
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