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Preparation method of room-temperature regenerated phenolic resin and recycling technology and application thereof

A phenolic resin, room temperature technology is applied in the field of preparation of renewable phenolic resin at room temperature, which can solve the problems of high recovery cost, inability to realize re-solidification and recycling of resin recovery products, and difficulty in PR recovery, and achieves the effect of promoting heat resistance.

Active Publication Date: 2017-05-31
XI AN JIAOTONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen that although the traditional recovery method has solved the difficult problem of PR recovery to a certain extent, it is still unable to realize the resolidification and recycling of the recovered resin product, and the mixture of phenol and its derivatives is usually obtained, and the recovery cost is relatively high. High, while the recovery conditions are relatively harsh (need high temperature or catalyst)

Method used

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  • Preparation method of room-temperature regenerated phenolic resin and recycling technology and application thereof
  • Preparation method of room-temperature regenerated phenolic resin and recycling technology and application thereof
  • Preparation method of room-temperature regenerated phenolic resin and recycling technology and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A new type of boron-containing thermoplastic phenolic resin was obtained by melting and blending 20g of high-ortho thermoplastic phenolic resin and 11g of phenylboronic acid at 70°C; using a staged heating program of 130°C / 3h+190°C / 5h in a tubular The novel boron-containing thermoplastic phenolic resin is cured under a nitrogen atmosphere in a furnace to obtain a cured resin.

[0036] At room temperature, dissolve 10 g of cured resin in 50 mL of a mixed solvent of ethanol and water (the mass ratio of ethanol and water is 3:1), let it stand for 30 min, and place it in a vacuum oven at 90 °C (vacuum degree is 0.09 MPa), After drying for 5 hours to remove the solvent, the regenerated phenolic resin at room temperature can be obtained.

[0037] Under magnetic stirring, 20g of high-ortho thermoplastic phenolic resin and 4g of naphthylboronic acid were dissolved in ethanol to obtain a new boron-containing thermoplastic phenolic resin ethanol solution, and the boron-containing...

Embodiment 2

[0045] 30g of bisphenol A type thermoplastic phenolic resin and 6g of diphenylboronic acid were blended by heating at 60°C to obtain a new type of boron-containing thermoplastic phenolic resin; a staged heating program of 140°C / 4h+195°C / 6h was used in vacuum The novel boron-containing thermoplastic phenolic resin is cured in a nitrogen atmosphere in an oven to obtain a cured boron-containing thermoplastic phenolic resin.

[0046] At room temperature, dissolve 10g of boron-containing thermoplastic phenolic resin in 50mL of ethanol, let it stand for 50min, and dry it in a vacuum oven (vacuum degree: 0.09MPa) at 80°C for 2.0h to remove the solvent to obtain a regenerated phenolic resin .

[0047] Under magnetic stirring, dissolve 30g of high-ortho thermoplastic phenolic resin and 6g of diphenylboronic acid in ethanol to obtain a new boron-containing thermoplastic phenolic resin ethanol solution, which is prepared by compounding the boron-containing thermoplastic phenolic resin et...

Embodiment 3

[0050] A mixture of 25g of ordinary thermoplastic phenolic resin and 4.6g of biphenylboronic acid and dihydroxyphenylboronic acid was blended at 100°C to obtain a new boron-containing thermoplastic phenolic resin; using 125°C / 4h+160°C / 2h+200°C / The new boron-containing thermoplastic phenolic resin was cured in a tube furnace nitrogen atmosphere with a staged temperature rise program of 4 hours to obtain a cured resin.

[0051] At room temperature, dissolve 10 g of cured resin in 50 mL of a mixed solvent of ethanol and water (mass ratio: 2:1), let it stand for 35 min, and then dry it in a vacuum oven at 80 °C (vacuum degree: 0.09 MPa) for 2 h to remove Solvent, you can get regenerated phenolic resin.

[0052] Under magnetic stirring, a mixture of 25 g of ordinary thermoplastic phenolic resin and 4.6 g of biphenylboronic acid and dihydroxyphenylboronic acid was dissolved in ethanol to obtain a new boron-containing thermoplastic phenolic resin ethanol solution for the preparation...

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Abstract

The invention relates to a preparation method of room-temperature regenerated phenolic resin and a recycling technology and application thereof. The preparation method comprises the following steps of according to parts by mass, melting and blending 100 parts of thermoplastic phenolic resin and 18.4 to 55 parts of boric acid compound at the temperature of 60 to 100 DEG C, so as to obtain boron-containing thermoplastic phenolic resin; or, dissolving 100 parts of thermoplastic phenolic resin and 20 to 50 parts of boric acid compound into an organic solvent with low boiling point at the temperature of 40 to 60 DEG C, so as to obtain the boron-containing thermoplastic phenolic resin; curing, so as to obtain the room-temperature regenerated phenolic resin. The preparation method has the advantages that the preparation technology of the resin is simple; the resin is dissolved into the mixing solvent of ethyl alcohol and water at room temperature, so that the resin can be recycled; the resin can be used for preparing the recyclable fiber reinforced boron-containing thermoplastic phenolic resin-based composite material. The prepared boron-containing thermoplastic phenolic resin has the advantages that the function of arylboronic acid ester structure promoting the heat-resistant property of the thermoplastic phenolic resin is fully realized, and the technology of the resin and the mechanical property of the composite material can be simultaneously realized.

Description

technical field [0001] The invention relates to a preparation method of a room-temperature renewable phenolic resin, a recovery process and application thereof. Background technique [0002] Phenolic resin, as one of the important thermosetting resin varieties, has a history of more than one hundred years so far. Due to the availability of raw materials, low cost, and good mechanical properties, heat resistance, and electrical properties, phenolic resins are widely used in the field of advanced composite materials, for example, for processing into resin-based composites with good ablation resistance and carbon / carbon composite. As we all know, only when phenolic resin is cured to form a three-dimensional cross-linked structure can it become a material with practical value. However, cured phenolic resins are quite stable, both to heat and to media (including common inorganic media such as acidic, alkaline, and neutral water, and various organic solvents). This valuable p...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08J11/08C08L61/14C08K7/06C08K7/14C08J5/04
CPCC08G8/28C08J5/042C08J5/043C08J11/08C08K7/06C08K7/14C08J2361/14C08L2201/08C08L2207/20C08L61/14Y02W30/62
Inventor 王淑娟井新利辜朝辉王晓行小龙
Owner XI AN JIAOTONG UNIV
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