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Preparation method for solid thermosetting phenolic resin

A phenolic resin and thermosetting technology, applied in the field of fast-curing high molecular weight thermosetting phenolic resin and its preparation, can solve the problems of unstable quality, slow curing rate, low molecular weight of thermosetting resin, etc., and achieve fast curing rate and simple synthesis reaction. Effect

Inactive Publication Date: 2011-12-21
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aiming at the problems of low molecular weight, slow curing rate and unstable quality of thermosetting resins, the invention discloses a simple and convenient preparation method of solid thermosetting phenolic resins and their curing process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Get 94g phenol and be placed in the three-necked reaction flask that reflux condenser, thermometer and stirrer are housed, add 100mL dehydrated alcohol as solvent, add 0.1g sulfuric acid (98wt%) simultaneously as catalyst; Add 27g paraformaldehyde in batches; To the reflux reaction for 4h to obtain a brownish red solution. Cool to 40°C, neutralize with 40wt% sodium hydroxide solution and basify to pH9-10; add 12g of paraformaldehyde, and continue to react at 50°C for 8h. After cooling to room temperature, neutralize to pH 6 with 18wt% hydrochloric acid; remove the formed salt by filtration to obtain a brown-red viscous liquid; remove the solvent in vacuum at 70° C. to obtain a solid (semi-solid) phenolic resin. Gel permeation chromatography (GPC) analysis showed that the average molecular weight of the resin was 1180. The gel time at 150°C was about 55s.

Embodiment 2

[0032]Get 94g phenol and be placed in the three-necked reaction flask that reflux condenser, thermometer and stirrer are housed, add 100mL dehydrated alcohol as solvent, add 0.2g hydrochloric acid (37wt%) simultaneously as catalyst; Add 28g paraformaldehyde in batches; To the reflux reaction for 4h to obtain a brownish red solution. Cool to 40°C, neutralize with 40wt% sodium hydroxide solution and basify to pH 9-10; add 13g of paraformaldehyde, and continue the reaction at 45°C for 12h. After cooling to room temperature, it was neutralized to pH 6 with 18 wt% hydrochloric acid; the generated salt was removed by filtration to obtain a brown-red viscous liquid; the solvent was removed in vacuo at 70° C. to obtain a solid phenolic resin. Gel permeation chromatography (GPC) analysis showed that the average molecular weight of the resin was 1400. The gel time at 150°C was about 35s.

Embodiment 3

[0034] Get 94g phenol and be placed in the three-necked reaction flask that reflux condenser, thermometer and stirrer are housed, add 100mL dehydrated alcohol as solvent, add 0.1g sulfuric acid (98wt%) simultaneously as catalyst; Add 29g paraformaldehyde in batches; To the reflux reaction for 4h to obtain a brownish red solution. Cool to 40°C, neutralize with 40wt% sodium hydroxide solution and basify to pH 9-10; add 13g of paraformaldehyde, and continue the reaction at 50°C for 8h. After cooling to room temperature, it was neutralized to pH 6 with 18 wt% hydrochloric acid; the generated salt was removed by filtration to obtain a brown-red viscous liquid; the solvent was removed in vacuo at 70° C. to obtain a solid phenolic resin. Gel permeation chromatography (GPC) analysis showed that the average molecular weight of the resin was 2850. The gel time at 150°C was about 18s.

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Abstract

The invention discloses a preparation technology of solid thermosetting phenolic resin with high molecular weight. The thermosetting phenolic resin with stable and reliable quality can be prepared in an ethanol solvent by using a sequential acid and alkali process, gel can be formed in 1 minute by thermally treating the thermosetting phenolic resin at the temperature of between 150 and 180 DEG C,and the thermosetting phenolic resin is totally cured in 30 minutes. The preparation method is environment-friendly, simple, convenient and reliable; and the solid thermosetting phenolic resin has broad application prospect in adhesive, coating and composite matrix.

Description

technical field [0001] The invention relates to a fast-curing high-molecular-weight thermosetting phenolic resin and a preparation method thereof. Specifically, a high-molecular-weight thermoplastic phenolic resin is prepared by acid-catalyzed polymerization, and then the thermosetting phenolic resin is prepared by methylolation under alkali catalysis. technical background [0002] Since the American scientist Buckland systematically studied the synthesis and application of phenolic resins in 1905, as one of the earliest three synthetic thermosetting resins, phenolic resins are used as electrical insulation materials, wood adhesives, molding materials and ablation heat-resistant materials. Used in transportation, construction, mining and military industries, etc. Phenolic resins offer high temperature, impact, low smoke and chemical resistance at low cost. However, the synthesis reaction of phenolic resin is very complicated and difficult to control accurately; the molecula...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10C09D161/10C09J161/10C08L61/10
Inventor 杨丽君王明存
Owner BEIHANG UNIV
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