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Epoxy resin solvent-free low temperature curing agent, preparation method and application thereof

An epoxy resin and solvent-free technology, which is applied in the field of epoxy resin curing agent preparation, can solve the problems of low-molecular-weight thiol compounds with strong odor, respiratory system damage, and polyamine volatilization, so as to improve curing efficiency and improve Surface tension, effect of increasing curing rate

Active Publication Date: 2014-08-13
国科广化(南雄)新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are many kinds of epoxy resin curing agents, and room temperature and heating curing agents can meet the requirements of most occasions. However, in the field of low-temperature rapid curing, most of them are fatty polyamines or low-molecular mercaptan compounds on the market. The workplace has great advantages, but there are also some disadvantages. Polyamines are volatile and harmful to the skin and respiratory system of the human body. For temporary emergency use, it is urgent to develop a curing agent that can be quickly cured at low temperature and can be applied in water environment

Method used

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  • Epoxy resin solvent-free low temperature curing agent, preparation method and application thereof
  • Epoxy resin solvent-free low temperature curing agent, preparation method and application thereof
  • Epoxy resin solvent-free low temperature curing agent, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1: Preparation of epoxy resin solvent-free low-temperature curing agent

[0046] (1) Preparation of thiourea modified amine

[0047] Mix 44.6g of diethylenetriamine, 39.1g of m-phenylenediamine and 42.9g of thiourea, pass in an inert gas, heat at 60°C under mechanical stirring, and raise the temperature after the thiourea is completely melted to 140°C, reflux for 4 hours, lower the temperature to 55°C, continue the reaction for 1 hour, and cool to obtain 118.1 g of dark yellow thiourea-modified amine;

[0048] (2) Preparation of modified phenalkamine

[0049] Mix 113.5g of isophorone diamine with 118.1g of thiourea-modified amine and 80.7g of cardanol, heat at 50°C while stirring, add 24.5g of paraformaldehyde powder in batches, and raise the temperature to 95°C Reflux for 3 hours, cool, wash with warm water to remove unreacted polyamine and formaldehyde, distill off the water generated during the reaction at 110°C under reduced pressure, and cool to obtain...

Embodiment 2

[0052] Embodiment 2: Preparation of epoxy resin solvent-free low-temperature curing agent

[0053] (1) Preparation of thiourea modified amine

[0054] Mix 49.7g of diethylenetriamine, 35.7g of m-phenylenediamine and 39.1g of thiourea, pass in an inert gas, heat at 60°C under mechanical stirring, and raise the temperature after the thiourea is completely melted to 140°C, reflux for 4 hours, lower the temperature to 55°C, continue the reaction for 1 hour, and cool to obtain 116.5g of dark yellow thiourea modified amine;

[0055] (2) Preparation of modified phenalkamine

[0056] Mix 117.3g of isophoronediamine with 116.5g of thiourea-modified amine and 81.4g of cardanol, heat at 50°C while stirring, add 23.7g of paraformaldehyde powder in batches, and heat up to 95°C Reflux for 3 hours, cool, wash with warm water to remove unreacted polyamine and formaldehyde, distill off the water generated during the reaction at 110°C under reduced pressure, and cool to obtain 327.1 g of modi...

Embodiment 3

[0059] Embodiment 3: Preparation of epoxy resin solvent-free low-temperature curing agent

[0060] (1) Preparation of thiourea modified amine

[0061] Mix 45.4g of diethylenetriamine, 38.9g of m-phenylenediamine and 40.2g of thiourea, pass in an inert gas, heat at 60°C under mechanical stirring, and raise the temperature after the thiourea is completely melted to 140°C, reflux for 4 hours, lower the temperature to 55°C, continue the reaction for 1 hour, and cool to obtain 115.9g of dark yellow thiourea modified amine;

[0062] (2) Preparation of modified phenalkamine

[0063] Mix 115.9g of isophorone diamine with 117.4g of thiourea-modified amine and 79.6g of cardanol, heat at 50°C while stirring, add 23.2g of paraformaldehyde powder in batches, and raise the temperature to 95°C Reflux for 3 hours, cool, wash with warm water to remove unreacted polyamine and formaldehyde, distill off the water generated during the reaction at 110°C under reduced pressure, and cool to obtain ...

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Abstract

The invention belongs to the technical field of epoxy resin curing agent preparation technology, and discloses an epoxy resin solvent-free low temperature curing agent, a preparation method and an application. The curing agent can be better used in cement mortar and used for preparing epoxy grouting material under low temperature in water environment. The curing agent comprises the following components by mass percentage: 79.9-97.2% of modified phenolic amine, 0.8-5.6% of coupling agent, 1.7-9.1% of flexibilizer, 0.1-0.9% of antifoaming agent and 0.2-4.5% of catalyst. According to the invention, thiourea group is introduced, thiourea modified amine, polyamine, long chain alkylphenol and paraformaldehyde are performed a Mannich reaction to synthesize novel thioureido-containing Mannich base, so that solidification rate under low temperature environment is increased, disadvantage of poor solidification efficiency under wet surface and water can be overcome, and a silane coupling agent is added for improving surface tension of system contact surface and increasing the solidification efficiency under water environment.

Description

technical field [0001] The invention belongs to the technical field of epoxy resin curing agent preparation, and in particular relates to a solvent-free low-temperature curing agent for epoxy resin and its preparation method and application. Epoxy grouting material. Background technique [0002] Epoxy resin (EP) is an important class of thermosetting resin, which has the advantages of high bonding strength, low shrinkage, good stability, high mechanical strength and good processability. Used in machinery, electronics, civil engineering and construction and other fields. Nowadays, the research and development of epoxy resin materials at home and abroad are mainly focused on improving their environmental protection, including solvent-free epoxy resin materials and water-based epoxy resin materials. However, research on the improvement of bonding and curing properties of epoxy resin materials in low temperature and aqueous environments is not very mature. [0003] There are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/62C08L63/00C04B24/12
Inventor 庞浩马哲杨元龙廖兵薛巍徐宇亮李朋娟李海涛
Owner 国科广化(南雄)新材料研究院有限公司
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