Epoxy resin curing agent, synthesis method and curing method

A technology of epoxy resin curing and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of imino compounds, etc. It can solve the problem of stickiness on the surface of cured products, failure of curing on the surface of the system, lack of color and yellowing resistance etc. to achieve excellent yellowing resistance, bright surface and excellent scratch resistance

Active Publication Date: 2016-06-08
雅安市弘利展化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aliphatic amines and their derivatives curing agents have high reactivity and polarity, so they can quickly initiate the ring-opening reaction of the epoxy structure, but they are also very easy to absorb moisture and CO in the air 2 , so that the surface curing of the system fails or is incomplete, and eventually leads to defects such as stickiness, oil bleeding, and dullness on the surface of the cured product, especially when curing at low temperature, this phenomenon is particularly prominent
[0003] In order to solve the above problems, fatty amines are usually subjected to hydrophobic pre-reaction, such as 593 curing agent (pre-reaction of diethylenetriamine and butyl glycidyl ether) and T31 curing agent (pre-reaction of fatty amine and phenolic aldehyde) on the market. , although this type of product can partially alleviate the surface defects of the product, the viscosity of the curing agent increases, which limits its application. At the same time, when curing at low temperature, the problem of surface defects is still serious
[0004] Another method is to add accelerators (such as: 2,4,6-tris(dimethylaminomethyl)phenol, N,N'-dimethylbenzylamine, etc.) to fatty amines or their derivatives. To increase the reaction speed, reduce the combination time of the curing agent and water vapor, and improve the surface properties of the cured product, but the curing agent treated by this method has serious deficiencies in color and yellowing resistance.

Method used

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  • Epoxy resin curing agent, synthesis method and curing method
  • Epoxy resin curing agent, synthesis method and curing method
  • Epoxy resin curing agent, synthesis method and curing method

Examples

Experimental program
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Embodiment 1

[0067] Step 1. To prepare ketimine, put 1.2kg of ethylenediamine into a 5L three-necked bottle equipped with a dripping reflux device, raise the temperature to 40°C, then slowly add 1.16kg of acetone dropwise, keep the temperature at 40-45°C and wait for 1 hour The acetone was added dropwise and closed, and after the dropwise addition was completed, the temperature was kept at 40-45° C. for 3 hours. After the reaction is completed, turn on the vacuum pump, keep the temperature at 80-90° C., and the vacuum at -0.08 MPa, and remove 360 ​​g of water by distillation under reduced pressure.

[0068] Step 2. To prepare the cyanoethylated adduct, lower the temperature in the three-neck flask to 70°C, slowly add 2.12kg of acrylonitrile dropwise, and keep the temperature at 70-80°C, and complete the dropwise addition of acrylonitrile within 2 hours , continue to maintain the temperature at 70-80 ° C for 1 hour, cool and discharge the material for later use.

[0069] Step 3. Prepare cy...

Embodiment 2

[0073] Step 1. To prepare ketimine, put 1.2kg of ethylenediamine into a 5L three-necked bottle equipped with a dripping reflux device, raise the temperature to 45°C, slowly add 1.44kg of methyl ethyl ketone dropwise, keep the temperature at 40-45°C and dissolve within 1 hour Stop the dropwise addition of methyl ethyl ketone, and keep the temperature at 50-60°C for 2 hours after the dropwise addition is completed. After the reaction is completed, turn on the vacuum pump, keep the temperature at 100-110° C., vacuum degree -0.08 MPa, and remove 360 ​​g of water by distillation under reduced pressure.

[0074] Step 2. To prepare the cyanoethylation adduct, cool down the temperature in the three-necked flask to 70°C, slowly add 2.12kg of acrylonitrile dropwise, and keep the temperature at 80-85°C, complete the dropwise addition of acrylonitrile within 2 hours, continue The temperature was maintained for 0.5 hours. Cool and discharge for later use.

[0075] Step 3. Prepare cyano h...

Embodiment 3

[0079] Step 1. To prepare ketimine, put 1.2kg of ethylenediamine into a 5L three-necked bottle equipped with a dripping reflux device, raise the temperature to 30°C, slowly add 1.5kg of methyl ethyl ketone dropwise, keep the temperature at 50±3°C and dissolve within 1.5 hours Stop the dropwise addition of methyl ethyl ketone, and keep the temperature at 60° C. for 2 hours after the dropwise addition is completed. After the reaction is completed, raise the temperature to 80°C, turn on the vacuum pump, keep the temperature at 100-110°C, and vacuum degree -0.08MPa, and distill off the water under reduced pressure.

[0080] Step 2. To prepare the cyanoethylated adduct, lower the temperature in the three-necked flask to 50°C, slowly add 2.3kg of acrylonitrile dropwise, and keep the temperature at 56±3°C, complete the dropwise addition of acrylonitrile within 2 hours, continue The temperature was maintained for 2 hours. Cool and discharge for later use.

[0081] Step 3. Prepare cy...

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Abstract

The invention provides an epoxy resin curing agent, a synthesis method and a curing method and belongs to the field of curing agent products. The epoxy resin curing agent is N,N'-bis(3-aminopropyl) ethanediamine and is synthesized from raw materials including ethanediamine, ketone, acrylonitrile and the like through multi-step reactions. The epoxy resin curing agent has high curing strength, wear resistance and scratch resistance and has a higher curing speed at a low temperature, a surface after curing is bright, is not prone to oxidation and has excellent yellowing resistance. The synthesis method of the epoxy resin curing agent is simple in process and convenient to control.

Description

technical field [0001] The invention relates to the field of curing agent products, in particular to an epoxy resin curing agent and a synthesis method. Background technique [0002] There are many kinds of epoxy resin curing agents. For room temperature curing transparent epoxy systems, aliphatic amines or their modified products are usually used as curing agents. Aliphatic amines and their derivatives curing agents have high reactivity and polarity, so they can quickly initiate the ring-opening reaction of the epoxy structure, but they are also very easy to absorb moisture and CO in the air 2 , so that the surface curing of the system fails or is incomplete, and eventually leads to defects such as stickiness, oil bleeding, and dullness on the surface of the cured product, especially when curing at low temperature, this phenomenon is particularly prominent. [0003] In order to solve the above problems, fatty amines are usually subjected to hydrophobic pre-reaction, such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50C07C211/11C07C209/28
CPCC07C209/28C07C211/11C07C249/02C07C251/08C07C253/30C07C255/25C08G59/5006C08G59/5013
Inventor 杨旭明吴洪斌闵峻徐庆鑫
Owner 雅安市弘利展化工有限公司
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