Production method of solid-thermosetting phenolic resin

A technology of phenolic resin and production method, which is applied in the production field of solid thermosetting phenolic resin, can solve the problems of equipment damage loss, product loss, cross-linking hardening, etc., and achieve the reduction of resin amount, energy consumption reduction, and improvement of softening point Effect

Active Publication Date: 2011-10-19
山东艾蒙特新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of these methods is that due to the formula, process, equipment and other reasons, and the dehydration is carried out in the evaporator or reactor, it is necessary to ensure a high enough temperature during dehydration to keep the resin with a satisfactory softening point in liquid state; due to the relatively high temperature in the kettle, the resin will continue to undergo condensation reaction at a higher temperature, the molecular weight will continue to increase, and the softening point will become higher and higher with time, and eventually it will be uncontrollable. Cross-linking and hardening take place, and detonation occurs, causing irreparable loss of product and destructive loss of equipment. Therefore, the reports of existing domestic thermosetting phenol-formaldehyde solid resins have no detailed reports on solving this problem, and Most of them are laboratory processes, and there are relatively few articles related to solid thermosetting phenolic resins

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A production method of solid thermosetting phenolic resin, completed by the following steps:

[0024] (1), measure 100 parts of used phenols by weight, 95 parts of 37% formaldehyde aqueous solution, 4 parts of alkali catalysts and 100 parts of toluene, and described alkali catalysts are sodium hydroxide;

[0025] (2), phenol and sodium hydroxide are mixed and stirred evenly;

[0026] (3), heat up, when heated to 60°C, add dropwise 37% formaldehyde aqueous solution, and after 3.5 hours of reaction at 60°C, take a sample to measure the water solubility, until the water solubility is qualified, add formic acid to adjust the pH value to 5- 6, stop the reaction;

[0027] (4) Add 100 parts of toluene to the reaction kettle, keep the temperature at 50-60°C and stir for 20 minutes, then cool down to 40-50°C and statically stratify;

[0028] (5), after separating the lower aqueous phase and the upper solvent phase, add 50 parts of methanol to the middle resin phase and stir to...

Embodiment 2

[0033] A production method of solid thermosetting phenolic resin, completed by the following steps:

[0034] (1), measure 100 parts of p-tert-butylphenol used in components by weight, 80 parts of 50% formaldehyde aqueous solution and 4 parts of alkali catalysts, and described alkali catalysts are sodium hydroxide;

[0035] (2), p-tert-butylphenol and sodium hydroxide are mixed and stirred evenly;

[0036] (3), heating up, when the temperature of the material is within the range of 50°C, add the measured 50% formaldehyde solution, when heated to 100°C, after 3.5 hours of heat preservation reaction, take a sample to measure the gel time, until the gel time is qualified, Add 25% sulfuric acid solution to adjust the pH to 4-5 to stop the reaction;

[0037] (4), cooling to 50-60 ℃ static stratification;

[0038] (5), after separating the lower water phase and the upper resin phase, add 50 parts of butanol to the resin phase and stir to dissolve for 20 minutes;

[0039] (6) Turn ...

Embodiment 3

[0043] A production method of solid thermosetting phenolic resin, completed by the following steps:

[0044] (1), measure 100 parts of phenols used by weight ratio component, 130 parts of 37% formaldehyde aqueous solution and 3 parts of alkaline catalysts, described alkaline catalysts are 25% aqueous ammonia solutions;

[0045] (2), phenol and 25% ammonia solution are mixed and stirred evenly;

[0046] (3), heating up, when the temperature of the material is in the range of 40-50°C, add 37% formaldehyde aqueous solution measured, when heated to 98°C, after 0.5 hours of heat preservation reaction, take a sample to measure the gel time until the gel time is qualified Stop reaction after;

[0047] (4) Add 100 parts of toluene to the reaction kettle, keep the temperature at 50-60°C and stir for 20 minutes, then cool down to 40-50°C and statically stratify;

[0048] (5), after separating the lower aqueous phase and the upper solvent phase, add 50 parts of butanone to the middle r...

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PUM

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Abstract

The invention discloses a production method of a solid-thermosetting phenolic resin. The production method is characterized by comprising the following steps: mixing and evenly stirring phenol, a base catalyst and aldehyde which are respectively weighed, and heating for the reaction; after the reaction is finished, adding an acidic neutralizer for neutralization, and then adding a non-proton organic solvent; standing for layering the material into a lower-layer water phase, a middle-layer resin phase and an upper-layer solvent phase, separating out the lower-layer water phase and the upper-layer solvent phase, and retaining the middle resin phase; adding an alcohol or ketone organic solvent in the middle-layer resin phase; turning on a film evaporator, transporting the dissolved material to the film evaporator for vacuum dehydration; directly cooling and granulating the qualified resin and packaging; and recovering the solvents for repeated use. By the production method, the softening point of the resin is improved, evaporation efficiency is improved, energy consumption is reduced, and process time is shortened.

Description

technical field [0001] The invention relates to a production method of phenolic resin, in particular to a production method of solid thermosetting phenolic resin, the solid thermosetting phenolic resin produced by this method is suitable for epoxy curing agent, electronic molding compound, friction material, phenolic fiber , Foundry coated sand and other industries. Background technique [0002] Phenolic resin has heat resistance, insulation, high temperature resistance, corrosion resistance and good mechanical processing properties, and can be used in the manufacture of copper clad laminates for printed circuit boards, plastic packaging materials, molding compounds, laminated plastics, foam plastics, honeycomb plastics, etc. It can be used as paint raw material, adhesive, phenolic epoxy resin, anti-corrosion cement, phenolic fiber and ion exchange resin based on phenolic resin, etc. It can also be used as an adhesive for grinding wheels and brake pad metal casting models. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10C08G8/12
Inventor 吕虎李长彬郑超吕华刘常玉乐碧兰褚宪锋
Owner 山东艾蒙特新材料有限公司
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