Imidazole dinitrile resin based on acid-base co-melting and preparation method thereof

A technology of imidazole dinitrile resin and imidazole dinitrile is applied in the field of thermosetting resin materials to achieve the effects of lowering melting point, lowering initial curing temperature and high nucleophilic activity

Active Publication Date: 2021-12-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These characteristics have had a negative impact on the processing of imidazole dinitrile resins. Therefore, how to reduce the melting point of raw materials used in imidazole dinitrile resins, improve the curing reactivity of imidazole dinitrile resins, and reduce the curing temperature has become imidazole dinitrile resins. Important Questions for Research

Method used

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  • Imidazole dinitrile resin based on acid-base co-melting and preparation method thereof
  • Imidazole dinitrile resin based on acid-base co-melting and preparation method thereof
  • Imidazole dinitrile resin based on acid-base co-melting and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] In this embodiment, DCI1 and A3 Be raw material, the step of preparing co-melting imidazole dinitrile resin is as follows:

[0072] (1) Dissolve 10mmol of DCI1 and 10mmol of A3 in acetonitrile, then stir the reaction at 80°C for 0.1h, then spin the resulting solution to dryness, then add 0.5mL of ethanol to the resulting solid, grind it to a dry state, and then place it in After vacuum drying at 80°C for 3 hours, the acid-base eutectic was obtained; the melting point of the obtained acid-base eutectic was 128°C.

[0073] (2) Place the acid-base eutectic prepared in step (1) under an argon atmosphere, and perform the curing operation according to the following temperature gradient in sequence: heat preservation at 150°C for 5 hours, heat preservation at 200°C for 5 hours, heat preservation at 300°C for 5 hours, After curing, cool to room temperature with the furnace to obtain imidazole dinitrile resin based on acid-base fusion. DSC test data show that the glass tran...

Embodiment 2

[0075] In this embodiment, DCI2 DCI3 and A3 Be raw material, the step of preparing co-melting imidazole dinitrile resin is as follows:

[0076] (1) Dissolve 10mmol each of DCI2 and DCI3 and 10mmol of A3 in tetrahydrofuran, then stir and react at 0°C for 24h, then spin the resulting solution to dryness, then add 1.0mL of ethanol to the resulting solid, grind it to a dry state, and then in 80 °C for 3 hours in vacuum to obtain an acid-base eutectic; the melting point of the obtained acid-base eutectic is 189°C.

[0077] (2) Place the acid-base eutectic prepared in step (1) under a nitrogen atmosphere, and perform the curing operation according to the following temperature gradient in sequence: keep it at 200°C for 1h, keep it at 350°C for 4h, and cool it with the furnace to At room temperature, the imidazole dinitrile resin based on acid-base fusion is obtained. DSC test data show that the glass transition temperature Tg of the acid-base fusion-based fusion imidazole dini...

Embodiment 3

[0079] In this embodiment, DCI3 DCI4 DCI5 and A3 A4 A6 Be raw material, the step of preparing co-melting imidazole dinitrile resin is as follows:

[0080] (1) Add 10mmol each of DCI3, DCI4, DCI5, 20mmol each of A3, A4, and 10mmol of A6 into the grinding body, then add 1.5mL of ethanol, grind until it is dry, and then keep it at 90°C for 3 hours in vacuum to obtain the acid-base Co-melt; the melting point of the acid-base co-melt obtained through testing is 128°C.

[0081] (2) Place the acid-base eutectic prepared in step (1) in an air atmosphere, and perform the curing operation according to the following temperature gradient in sequence: keep warm at 199°C for 3h, keep warm at 300°C for 2h, and cool down with the furnace to At room temperature, the imidazole dinitrile resin based on acid-base fusion is obtained. DSC test data show that the glass transition temperature Tg of the imidazole dinitrile resin based on acid-base fusion is greater than 400°C.

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Abstract

The invention discloses imidazole dinitrile resin based on acid-base co-melting and a preparation method thereof, and the imidazole dinitrile resin is obtained by co-melting and curing at least one imidazole dinitrile compound and at least one organic base as raw materials, and the molar ratio of an N-H structure in the imidazole dinitrile compound to a basic group in the organic base is (3: 1)-(1: 3). Through construction of the imidazole dinitrile and organic alkali ion co-melt, the melting point of the acid-base co-melt is effectively reduced, and the curing temperature of the acid-base co-melt is reduced.

Description

technical field [0001] The invention belongs to the technical field of thermosetting resin materials, and relates to imidazole dinitrile resins, in particular to imidazole dinitrile resins based on acid-base fusion and a preparation method thereof. Background technique [0002] J. Hu et al. reported a high-performance thermosetting resin with imidazole dinitrile as the crosslinking group, which was obtained by self-curing reaction or adding a small amount of curing agent for isothermal curing using imidazole dinitrile compound as the raw material. It has excellent thermal performance and thermomechanical performance, but due to the strong intermolecular force introduced by its unique aromatic heterocyclic structure, the melting point of the raw material monomer is relatively high, such as even the imidazole bismuth containing flexible propyl linking unit The melting point of nitrile monomer is also as high as 236°C, and the curing reactivity of imidazole dinitrile resin is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06
CPCC08G73/0616
Inventor 杨刚胡江淮曾科朱正柱谭伟杨文杰
Owner SICHUAN UNIV
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