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High-strength water-based phenolic resin and preparation method thereof

A phenolic resin, water-based technology, which is applied in the field of high-strength water-based phenolic resin and its preparation, can solve the problems of carbonization and poor flame retardant performance, and achieves reduced decomposition amount, good adhesion performance, and improved flame retardant performance. Effect

Pending Publication Date: 2021-12-24
ANHUI HONGYUAN CHEM SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The unmodified phenolic resin will undergo obvious oxidation when the temperature is higher than 200 ° C. As the temperature rises further, the phenolic resin will even undergo pyrolysis and carbonization, and the flame retardancy is poor.

Method used

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  • High-strength water-based phenolic resin and preparation method thereof
  • High-strength water-based phenolic resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Prepare the modifier:

[0037] Step S11, heat vanillin, acetone and anhydrous potassium carbonate to reflux for 1 hour, then add chloroethanol, heat to reflux for 12 hours, after the reaction is completed, cool to room temperature, add dichloromethane and deionized water, and adjust the water phase with sodium hydroxide The pH value is 7, the obtained organic phase is concentrated under reduced pressure, and the solvent is removed to obtain intermediate 1; wherein, the amount ratio of vanillin, acetone, anhydrous potassium carbonate and chloroethanol is 1.5g: 20mL: 1.4g: 0.8 g;

[0038] Step S12, mix phosphorus oxychloride and dichloromethane, add intermediate 1 and triethylamine at 0°C, stir and react for 1 hour after the addition is complete, then add anhydrous methanol and methanol solution of sodium methoxide, at temperature The intermediate 2 was obtained by reacting at 20°C for 5 hours; wherein, the dosage ratio of phosphorus oxychloride, intermediate 1, triethyl...

Embodiment 2

[0041] Preparation additives are prepared through the following steps:

[0042] Under the protection of nitrogen and the temperature at 0°C, mix 4,4'-diaminodiphenyl ether and N,N-dimethylformamide, stir until dissolved, add pyromellitic dianhydride and stir for 5 hours, then Add modifier and 4A molecular sieve and continue to stir and react for 2h to obtain the additive. Among them, the molar ratio of 4,4'-diaminodiphenyl ether and pyromellitic dianhydride is 1:1; the amount of 4,4'-diaminodiphenyl ether and N,N-dimethylformamide The ratio is 1g:10mL; the mass ratio of 4,4'-diaminodiphenyl ether to the modifier is 2:0.3; the modifier is prepared in Example 1.

Embodiment 3

[0044] A preparation method of high-strength water-based phenolic resin, comprising the steps of:

[0045] The first step, put phenol, triethylamine, dimethylethanolamine, N-methylethanolamine, additives, and sodium carbonate into the reaction kettle to heat, and drop the formaldehyde solution and liquid caustic soda within 2 hours, and control the temperature in the kettle to 60°C ;

[0046] In the second step, heat up to 75°C within 20min, and keep warm for 240min; when the emulsification point reaches 65°C, add caustic soda and urea in turn, keep the temperature at 55°C before the urea is added, add water and stir, and reduce the temperature in the kettle to 25°C , let it stand for 1 hour to discharge the material, and a high-strength water-based phenolic resin is obtained.

[0047] Among them, 160 parts of phenol, 400 parts of formaldehyde solution, 2.4 parts of liquid caustic soda, 0.5 parts of caustic soda, 10 parts of triethylamine, 5 parts of dimethylethanolamine, 5 p...

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Abstract

The invention relates to a high-strength water-based phenolic resin and a preparation method thereof, and belongs to the technical field of phenolic resins. The phenolic resin comprises the following raw materials by weight: 160 parts of phenol, 400 parts of a formaldehyde solution, 2.4 parts of liquid caustic soda, 0.5 part of caustic soda flakes, 10 parts of triethylamine, 5 parts of dimethylethanolamine, 5 parts of N-methylethanolamine, 2 parts of sodium carbonate, 250 parts of urea, 190 parts of water, and 20-40 parts of an additive. The water-based phenolic resin is generated by reaction of phenol and formaldehyde under alkaline conditions, and has the characteristics of no solid waste, no wastewater, no smoke and the like. The additive is added in the preparation process, so that the phenolic resin forms a heterocyclic structure with higher thermal stability, the aromaticity of the resin is improved, the decomposition amount of the resin at high temperature is reduced, and the flame retardant property is improved. The prepared water-based phenolic resin is good in comprehensive performance and low in toxicity; and the product is low in free aldehyde content and good in adhesive property.

Description

technical field [0001] The invention belongs to the technical field of phenolic resins, and in particular relates to a high-strength water-based phenolic resin and a preparation method thereof. Background technique [0002] Phenolic resin is composed of phenolic compounds (such as phenol, cresol, xylenol, resorcinol, tert-butylphenol, bisphenol A, etc.) and aldehyde compounds (such as formaldehyde, acetaldehyde, paraformaldehyde, furfural, etc.) Under the action of alkaline or acidic catalysts, the resins obtained by addition polycondensation reaction are collectively called phenolic resins. The reaction between phenol and aldehyde is more complicated. Due to the molar ratio of phenol and formaldehyde, the catalyst used is different, and the speed and products of addition and polycondensation reactions are also different. [0003] Phenolic resin has good acid resistance and mechanical properties, and is widely used because of its easy-to-obtain raw materials and convenient ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/12C08G14/08
CPCC08G14/12C08G14/08
Inventor 余海华江涛张立刚严厚磊
Owner ANHUI HONGYUAN CHEM SCI & TECH
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