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
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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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