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Thermosetting phenolic resin and preparation method, regeneration method and recovery method thereof

A phenolic resin, thermosetting technology, applied in the field of thermosetting phenolic resin and its preparation, can solve the problems of low commercial value, environmental pollution, high energy consumption, etc., and achieves a simple, green, and controllable method suitable for large-scale industrial production. Effect

Active Publication Date: 2021-07-20
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the treatment of cured thermosetting phenolic resin: traditional landfill, incineration and other treatment methods have serious environmental pollution, and high-temperature and high-pressure hydrogenation, alcoholysis, ammonolysis, pyrolysis and other treatment methods need to consume a lot of energy. And the environment is harsh, the quality of recovered phenolic resin is poor, and the commercial value is low

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  • Thermosetting phenolic resin and preparation method, regeneration method and recovery method thereof
  • Thermosetting phenolic resin and preparation method, regeneration method and recovery method thereof
  • Thermosetting phenolic resin and preparation method, regeneration method and recovery method thereof

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preparation example Construction

[0028] The preparation method of thermosetting phenolic resin provided by the invention comprises:

[0029] S1, provide phenolic resin and curing agent, wherein, described phenolic resin contains phenolic hydroxyl group, and described curing agent is the derivative of alcohol, and the derivative of described alcohol contains more than 2 vinyl ether functional groups (-O-CH= CH 2 );

[0030] S2, mixing the phenolic resin with the curing agent to obtain a thermosetting phenolic resin after curing, wherein the thermosetting phenolic resin contains an acetal functional group.

[0031] In step S1, the structural formula of the phenolic resin is shown in the following formula (I), which has unreacted phenolic hydroxyl groups to ensure the processability of the phenolic resin,

[0032] n≥2.

[0033] At the same time, in order to further improve the processability of the phenolic resin and the curing agent, the phenolic resin is preferably at least one of a novolac resin and a br...

Embodiment 1

[0074] 1 mol of novolak resin and 1 mol of 1,4-cyclohexanedimethanol divinyl ether were mixed and precured at 100° C. for 30 minutes to obtain a precured product. The pre-cured product was processed by a flat vulcanizing machine at 150° C. and 10 MPa for 20 minutes, and then cured in a vacuum oven at 160° C. for 2 hours to obtain the first thermosetting phenolic resin.

[0075] The first thermosetting phenolic resin was processed by a flat vulcanizing machine at 170° C. and 10 MPa for 30 minutes to obtain the second thermosetting phenolic resin.

[0076] The first thermosetting phenolic resin was hydrolyzed in a 0.1 M hydrochloric acid acetone mixed solution (pH=1), and the phenolic resin and 1,4-cyclohexanedimethanol were recovered. The recovered phenolic resin is re-crosslinked with 1,4-cyclohexanedimethanol divinyl ether to obtain a third thermosetting phenolic resin.

[0077] After testing, the glass transition temperature of the first thermosetting phenolic resin is 106°...

Embodiment 2

[0083] 1 mol of novolak resin and 0.5 mol of 1,4-cyclohexanedimethanol divinyl ether were mixed and precured at 100° C. for 30 minutes to obtain a precured product. The pre-cured product was processed by a flat vulcanizing machine at 150° C. and 10 MPa for 20 minutes, and then cured in a vacuum oven at 160° C. for 2 hours to obtain the first thermosetting phenolic resin.

[0084] The first thermosetting phenolic resin was processed by a flat vulcanizing machine at 150° C. and 10 MPa for 20 minutes to obtain the second thermosetting phenolic resin.

[0085] The first thermosetting phenolic resin was hydrolyzed in a 0.1 M hydrochloric acid acetone mixed solution (pH=1), and the phenolic resin and 1,4-cyclohexanedimethanol were recovered. The recovered phenolic resin is re-crosslinked with 1,4-cyclohexanedimethanol divinyl ether to obtain a third thermosetting phenolic resin.

[0086] Compared with the thermosetting phenolic resin in Example 1, the first thermosetting phenolic r...

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Abstract

The present invention relates to a thermosetting phenolic resin and a preparation method thereof, the preparation method comprises: providing a phenolic resin and a curing agent, wherein the phenolic resin contains a phenolic hydroxyl group, the curing agent is an alcohol derivative, the alcohol derivative contains more than two vinyl ether functional groups; and mixing and curing the phenolic resin and the curing agent to obtain the thermosetting phenolic resin, wherein the thermosetting phenolic resin contains an acetal functional group. The thermosetting phenolic resin disclosed by the invention can be recycled to obtain phenolic resin and alcohol, regeneration is realized in physical and chemical modes, and the performance of the regenerated thermosetting phenolic resin is basically kept unchanged. Therefore, the invention also provides a regeneration method and a recovery method of the thermosetting phenolic resin.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a thermosetting phenolic resin and a preparation method, regeneration method and recovery method thereof. Background technique [0002] Once the phenolic resin is cured to form a three-dimensional crosslinked network, the thermosetting phenolic resin is insoluble, insoluble, and cannot be reprocessed, reshaped and degraded. For the treatment of cured thermosetting phenolic resin: traditional landfill, incineration and other treatment methods have serious environmental pollution, and high-temperature and high-pressure hydrogenation, alcoholysis, ammonolysis, pyrolysis and other treatment methods need to consume a lot of energy. And the environment is harsh, the quality of the recovered phenolic resin is poor, and the commercial value is low. Therefore, the efficient and non-destructive recycling of thermosetting phenolic resins is still a very urgent goal. Contents of...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08J11/16C08L61/14C07C29/10C07C31/27C07C31/20C07C31/22C07C41/26C07C43/11
CPCC08G8/28C08J11/16C07C29/10C07C41/26C08J2361/14C07C2601/14C07C31/276C07C31/207C07C31/225C07C43/11Y02W30/62
Inventor 李琼马松琪朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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