Preparation method of cardanol-containing polyphenol modified amine epoxy resin curing agent

A technology of cardanol polyphenol modified amine epoxy resin and curing agent, which is applied in the direction of epoxy resin glue, adhesive, adhesive type, etc., and can solve the problems of poor heat resistance, limited application, and poor bonding performance at high temperature of the cured product. Good and other problems, to achieve the effect of good heat resistance, low price and excellent toughness

Inactive Publication Date: 2017-08-18
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cured product has poor heat resistance and poor hig

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0014] Specific implementation mode 1: The preparation method of the cardanol-containing polyphenol-modified amine epoxy resin curing agent of this embodiment is implemented in the following steps:

[0015] 1. Add cardanol and phenols to the reaction device according to the molar ratio of 1:1~3, start stirring, heat to 40~50℃, (slowly) add the acid catalyst, and wait for the acid catalyst to dissolve after 10-30 minutes , The temperature is raised to 95-100°C, and the reaction is kept for 1 to 3 hours to obtain the intermediate product;

[0016] 2. Lower the temperature of the intermediate product obtained in step 1 to 20-50°C, add polyamines dropwise, keep the temperature unchanged at 20-50°C after dropping, and then (slowly) add aldehydes and raise the temperature to 90-100°C. Heat insulation reaction for 2 to 5 hours, after the reaction is completed, the temperature is lowered to 75 to 85°C, and dehydration is carried out under reduced pressure until anhydrous is removed to obta...

Example Embodiment

[0020] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the phenols described in step 1 are a mixture of one or more of phenol, o-cresol, and resorcinol. Other steps and parameters are the same as in the first embodiment.

Example Embodiment

[0021] Specific embodiment three: This embodiment is different from specific embodiment one or two in that the acidic catalyst described in step one is concentrated sulfuric acid, p-toluenesulfonic acid or Lewis acid. Other steps and parameters are the same as those in the first or second embodiment.

[0022] The mass concentration of concentrated sulfuric acid in this embodiment is 95% to 98%.

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PUM

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Abstract

The invention relates to a preparation method of an epoxy resin adhesive curing agent, in particular to a preparation method of a cardanol-containing polyphenol modified amine epoxy resin curing agent and aims to improve the toughness of phenolic amine curing agents in consideration with the heat resistance of the curing agents. The preparation method comprises the steps as follows: 1, cardanol and phenols are added to a reaction device and heated to 40-50 DEG C, an acid catalyst is added, the mixture is heated to 95-100 DEG C and reacts at the constant temperature for 1-3 h, and an intermediate product is obtained; 2, the intermediate product is cooled to 20-50 DEG C, polyamine is dropwise added, aldehydes are added after addition, the mixture is heated to 90-100 DEG C and reacts at the constant temperature for 2-5 h and then cooled to 75-85 DEG C after the reaction ends, reduced pressure dehydration is performed until no water exists, and the cardanol-containing polyphenol modified amine epoxy resin curing agent is obtained. The prepared cardanol-containing polyphenol modified amine curing agent has good heat resistance of phenol phenolic amine epoxy curing products and has 90-degree stripping up to 2-5 KN/m.

Description

technical field [0001] The invention relates to a preparation method of an epoxy resin adhesive curing agent. Background technique [0002] Epoxy resins are widely used in coatings, adhesives, composite materials and other fields. In order to meet their application requirements in different fields, different types of curing agents are required. Traditional aliphatic amine curing agents are brittle due to their high volatility and toxicity. The Mannich base curing agent obtained through Mannich reaction modification can well solve the problems of high volatility and high toxicity of traditional aliphatic amine curing agents. The more successful ones are T31 series phenalkamine curing agents. The phenolic hydroxyl group on the benzene ring of the phenalkamine curing agent promotes the ring opening of the epoxy group. The curing agent has a very high room temperature curing ability, and can quickly cure epoxy resin even in humid, underwater and other environments. It has been ...

Claims

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Application Information

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IPC IPC(8): C08G14/073C08G59/62C09J163/00
CPCC08G14/06C08G59/62C09J163/00
Inventor 谢保存刘晓辉赵颖李欣朱金华张大勇王刚荣立平米长虹
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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