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New epoxy resin curing agent and preparation method thereof

An epoxy resin curing and epoxy resin technology, applied in the field of new epoxy resin curing agent and its preparation, can solve the problems of poor compatibility, easy deposition of flame retardants, affecting flame retardant effect, etc., so as to reduce curing The effect of stable temperature, flame retardant performance and lower production cost

Inactive Publication Date: 2018-05-22
嘉兴市东方万达新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Additive flame retardants usually have poor compatibility with the resin in the system, and when left for a long time, the flame retardants are easy to deposit and affect the flame retardant effect
Moreover, the addition of general flame retardants can only improve the flame retardant performance of the system, and rarely can the system maintain excellent flame retardant performance and at the same time increase the Tg of the system, so that it has high temperature resistance

Method used

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  • New epoxy resin curing agent and preparation method thereof
  • New epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1 of the present invention provides a kind of novel epoxy resin curing agent and preparation method thereof, and its method is as follows:

[0020] 1) Preparation of modified epoxy resin: dissolve 10g isophorone diamine and 2.6g phenylphosphorus dichloride in 20g dimethylformamide (analytical pure), add 0.01g methanol (analytical pure) as Catalyst, heat up to 120 ° C and stir for 1 hour. After the reaction, the product obtained is washed several times with a mixed solution of ethyl acetate and petroleum ether, filtered and dried to obtain the product, and then the product is added to 100g YDF-170 epoxy resin Warming up to 140°C for 1.5 hours to obtain a modified epoxy resin;

[0021] 2) Preparation of novel epoxy resin curing agent: under the condition of 130°C, 26g of phenylphosphorous dichloride was added to the reactor, and then 8g of diethyl phosphite was added, stirred and reacted for 4 hours to obtain the novel epoxy resin Oxygen resin curing agent;

...

Embodiment 2

[0025] Embodiment 2 of the present invention provides a kind of novel epoxy resin curing agent and preparation method thereof, and its method is as follows:

[0026] 1) Preparation of modified epoxy resin: 20g isophorone diamine, 5.5g phenylphosphorus dichloride are dissolved in 40g dimethylformamide, add 0.01g methanol (analytical pure) as catalyst, heat up to Stir and react at 110°C for 1.5 hours. After the reaction, wash the product obtained several times with a mixed solution of ethyl acetate and petroleum ether, filter and dry to obtain the product, and then add the product to 100g of YDF-170 epoxy resin and heat up to 160°C Reaction 2 hours obtains modified epoxy resin;

[0027] 2) Preparation of novel epoxy resin curing agent: under the condition of 105°C, 26g of phenylphosphorous dichloride was added to the reactor, then 8g of diethyl phosphite was added, stirred and reacted for 3 hours to obtain the novel epoxy resin Oxygen resin curing agent;

[0028] 3) Add 36.1 g...

Embodiment 3

[0031] Embodiment 3 of the present invention provides a kind of novel epoxy resin curing agent and preparation method thereof, and its method is as follows:

[0032] 1) Preparation of modified epoxy resin: 30g isophorone diamine, 7.9g phenylphosphorus dichloride are dissolved in 50g dimethylformamide, add 0.01g triethanolamine (analytical pure) as catalyst, heat up Stir the reaction at 115°C for 2 hours. After the reaction, the product obtained is washed several times with a mixed solution of ethyl acetate and petroleum ether, filtered and dried to obtain the product, and then the product is added to 100g of YDF-170 epoxy resin and heated to 150 ℃ reaction for 2 hours to obtain modified epoxy resin;

[0033] 2) Preparation of novel epoxy resin curing agent: under the condition of 120°C, 26g of phenylphosphorous dichloride was added to the reactor, then 8g of diethyl phosphite was added, stirred and reacted for 3.5 hours to obtain the novel epoxy resin Oxygen resin curing agen...

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Abstract

The invention relates to a new epoxy resin curing agent and a preparation method thereof. The new epoxy resin curing agent has a structural formula shown as the figure in the description. The preparation method comprises: in a condition at 105-430 DEG C, reacting dichlorophenylphosphine with diethyl phosphite at a mol ratio of 3:1, raising the temperature to 150-160 DEG C, and performing a reaction for 3-4 h to obtain the new epoxy resin curing agent. The provided new epoxy resin curing agent is quite stable at the room temperature and long in storage period, and is used to graft phosphorus-series molecules to an epoxy resin structure during curing of an epoxy resin system. The new epoxy resin curing agent is excellent in flame retardance and thermal resistance, is quite stable, and can reduce the curing temperature.

Description

technical field [0001] The invention relates to a novel epoxy resin curing agent and a preparation method thereof, which belong to the technical field of coating chemical industry. Background technique [0002] As a thermosetting material, epoxy resin has always been a research hotspot. The multi-functional groups in the epoxy resin make the molecules have electromagnetic adsorption and strong bond energy, so the epoxy resin has very strong adhesion. Features The ring-opening addition polymerization of the epoxy group by the curing agent does not produce small molecular substances, and a large number of hydroxyl hydrogen bond associations, so the curing shrinkage of the epoxy resin is extremely low. After curing, it is a cross-linked compact structure without active and free groups and ions, so the epoxy resin has good stability, electrical insulation and excellent mechanical properties. In addition, epoxy resin has low water absorption, can be molded at low and high tempe...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08L63/00
CPCC08G59/4071C08L63/00C08L2201/02C08L2201/08
Inventor 殷国瑞
Owner 嘉兴市东方万达新材料股份有限公司
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