CN103483225A - Preparation method for epoxy resin curing agent - Google Patents
Preparation method for epoxy resin curing agent Download PDFInfo
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- CN103483225A CN103483225A CN201310438402.5A CN201310438402A CN103483225A CN 103483225 A CN103483225 A CN 103483225A CN 201310438402 A CN201310438402 A CN 201310438402A CN 103483225 A CN103483225 A CN 103483225A
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- curing agent
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- propylene carbonate
- epoxy curing
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Abstract
The invention discloses a preparation method for an epoxy resin curing agent, and belongs to the technical field of curing agents. The preparation method comprises the following steps: (1) adding aliphatic polyamine or cycloaliphatic polyamine into a three-necked reaction flask; (2) performing water-bath heating on the three-necked reaction flask, and dropping propylene carbonate into the three-necked reaction flask for reaction when the temperature inside the three-necked reaction flask is 40-50 DEG C, wherein the molar ratio of aliphatic polyamine or cycloaliphatic polyamine to propylene carbonate is (1:1)-(2:1); (3) dropping propylene carbonate for 30-40 min, and preserving heat for 2.5-3.5 h when the dropping is completed, so that the epoxy resin curing agent is obtained. The method has a simple technology, the reaction condition is moderate, the material is non-toxic and easy to get, and the curing speed is moderate.
Description
Technical field
The invention belongs to the solidifying agent technical field, be specifically related to a kind of preparation method of epoxy curing agent.
Background technology
Epoxy resin has good mechanical property, adhesiveproperties, electrical property and erosion resistance, is widely used in the fields such as caking agent, electric insulation encapsulation, coating.In the epoxy resin application, solidifying agent occupies very important position.Common aliphatics and alicyclic polyamine solidifying agent, there are the defects such as the very fast and fragility of curing speed in its cured article, and easy crystallization under some solidifying agent low temperature.Therefore by the whole bag of tricks, amine curing agent is carried out applying after modification again at present.But some starting material of method of modifying at present used are toxic, some raw-material selling at exorbitant prices, and the solidifying agent viscosity after modification is larger, and part still comes with some shortcomings.
Summary of the invention
The objective of the invention is to address the above problem and a kind of preparation method of epoxy curing agent is provided, the method technique is simple, and reaction conditions is gentle, starting material nontoxicly are easy to get, curing speed is moderate.
The technical solution adopted in the present invention is:
A kind of preparation method of epoxy curing agent comprises the following steps:
(1) aliphatic polyamine or alicyclic polyamine are put in three mouthfuls of reaction flasks:
(2) described three mouthfuls of reaction flasks are carried out to heating in water bath, when the temperature in described three mouthfuls of reaction flasks is 40 ℃～50 ℃, to dripping propylene carbonate in described three mouthfuls of reaction flasks, reacted, the mol ratio of described aliphatic polyamine or alicyclic polyamine and described propylene carbonate is 1:1～2:1;
(3) drip propylene carbonate 30～40 minutes, after dropwising, be incubated 2.5～3.5 hours, obtain epoxy curing agent.
Further, described step (1) is to carry out in the environment of drying nitrogen.
Further, on described three mouthfuls of reaction flasks, reflux condensing tube is housed, temperature is taken into account agitator.
Preferably, described aliphatic polyamine is hexanediamine, diethylenetriamine or triethylene tetramine.
Preferably, described alicyclic polyamine is m-xylene diamine or isophorone diamine.
The present invention has the following advantages:
Preparation method's technique of the present invention is simple, reaction conditions is gentle, starting material nontoxicly are easy to get, curing speed is moderate; Preparation method of the present invention adopts propylene carbonate to react with alicyclic polyamine or aliphatic polyamine, introduces in the solidifying agent molecule and increases ammonia ester bond flexible and that extend working time, has improved snappiness and the cementability of cured product.
Embodiment
Embodiment 1
The present embodiment provides a kind of preparation method of epoxy curing agent, comprises the following steps:
(1) under the protection of drying nitrogen, the 2mol isophorone diamine is put in three mouthfuls of reaction flasks, on three mouthfuls of reaction flasks, reflux condensing tube is housed, temperature is taken into account agitator.
(2) three mouthfuls of reaction flasks are carried out to heating in water bath, when temperature rises to 40 ℃ in the question response bottle, drip with the speed of 50mL per hour in propylene carbonate to the three mouthful reaction flask of 1mol and react.
(3) drip propylene carbonate 30 minutes, dropwise, be incubated 3 hours, obtain the light epoxy hardener of clear.
Embodiment 2
The present embodiment provides a kind of preparation method of epoxy curing agent, comprises the following steps:
(1) under the protection of drying nitrogen, the 1mol hexanediamine is put in three mouthfuls of reaction flasks, on three mouthfuls of reaction flasks, reflux condensing tube is housed, temperature is taken into account agitator.
(2) three mouthfuls of reaction flasks are carried out to heating in water bath, when temperature rises to 50 ℃ in the question response bottle, drip with the speed of 50mL per hour in propylene carbonate to the three mouthful reaction flask of 1mol and react.
(3) drip propylene carbonate 40 minutes, dropwise, be incubated 2.5 hours, obtain the light yellow epoxy hardener of clear.
Embodiment 3
The present embodiment provides a kind of preparation method of epoxy curing agent, comprises the following steps:
(1) under the protection of drying nitrogen, the 1mol diethylenetriamine is put in three mouthfuls of reaction flasks, on three mouthfuls of reaction flasks, reflux condensing tube is housed, temperature is taken into account agitator.
(2) three mouthfuls of reaction flasks are carried out to heating in water bath, when temperature rises to 45 ℃ in the question response bottle, drip with the speed of 50mL per hour in propylene carbonate to the three mouthful reaction flask of 1mol and react.
(3) drip propylene carbonate 35 minutes, dropwise, be incubated 3.5 hours, obtain the light yellow epoxy hardener of clear.
Preparation method's technique of the present invention is simple, reaction conditions is gentle, starting material nontoxicly are easy to get, curing speed is moderate; Preparation method of the present invention adopts propylene carbonate to react with alicyclic polyamine or aliphatic polyamine, introduces in the solidifying agent molecule and increases ammonia ester bond flexible and that extend working time, has improved snappiness and the cementability of cured product.
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (5)
1. the preparation method of an epoxy curing agent, is characterized in that, comprises the following steps:
(1) aliphatic polyamine or alicyclic polyamine are put in three mouthfuls of reaction flasks:
(2) described three mouthfuls of reaction flasks are carried out to heating in water bath, when the temperature in described three mouthfuls of reaction flasks is 40 ℃～50 ℃, to dripping propylene carbonate in described three mouthfuls of reaction flasks, reacted, the mol ratio of described aliphatic polyamine or alicyclic polyamine and described propylene carbonate is 1:1～2:1;
(3) drip propylene carbonate 30～40 minutes, after dropwising, be incubated 2.5～3.5 hours, obtain epoxy curing agent.
2. the preparation method of epoxy curing agent according to claim 1, is characterized in that, described step (1) is to carry out in the environment of drying nitrogen.
3. the preparation method of epoxy curing agent according to claim 1, is characterized in that, on described three mouthfuls of reaction flasks, reflux condensing tube is housed, temperature is taken into account agitator.
4. the preparation method of epoxy curing agent according to claim 1, is characterized in that, described aliphatic polyamine is hexanediamine, diethylenetriamine or triethylene tetramine.
5. the preparation method of epoxy curing agent according to claim 1, is characterized in that, described alicyclic polyamine is m-xylene diamine or isophorone diamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310438402.5A CN103483225A (en) | 2013-09-24 | 2013-09-24 | Preparation method for epoxy resin curing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310438402.5A CN103483225A (en) | 2013-09-24 | 2013-09-24 | Preparation method for epoxy resin curing agent |
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| Publication Number | Publication Date |
|---|---|
| CN103483225A true CN103483225A (en) | 2014-01-01 |
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| CN201310438402.5A Pending CN103483225A (en) | 2013-09-24 | 2013-09-24 | Preparation method for epoxy resin curing agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744670A (en) * | 2015-04-14 | 2015-07-01 | 湖南大学 | Epoxy acrylate prepolymer and application thereof |
| CN109824869A (en) * | 2019-01-31 | 2019-05-31 | 厦门源创力科技服务有限公司 | A kind of epoxy curing agent and preparation method thereof |
| CN112708109A (en) * | 2021-01-11 | 2021-04-27 | 安徽工业大学 | Modified aliphatic polyamine curing agent with long service life and preparation method thereof |
| CN115637125A (en) * | 2021-07-20 | 2023-01-24 | 中蓝晨光化工研究设计院有限公司 | Environment-friendly epoxy resin adhesive and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4820830A (en) * | 1987-03-02 | 1989-04-11 | King Industries, Inc. | Certain hydroxyalkyl carbamates, polymers and uses thereof |
| US20100249337A1 (en) * | 2009-03-26 | 2010-09-30 | Polymate, LTD. Nanotech Industries, Inc | Epoxi-amine composition modified with hydroxyalkyl urethane |
-
2013
- 2013-09-24 CN CN201310438402.5A patent/CN103483225A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4820830A (en) * | 1987-03-02 | 1989-04-11 | King Industries, Inc. | Certain hydroxyalkyl carbamates, polymers and uses thereof |
| US20100249337A1 (en) * | 2009-03-26 | 2010-09-30 | Polymate, LTD. Nanotech Industries, Inc | Epoxi-amine composition modified with hydroxyalkyl urethane |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744670A (en) * | 2015-04-14 | 2015-07-01 | 湖南大学 | Epoxy acrylate prepolymer and application thereof |
| CN104744670B (en) * | 2015-04-14 | 2017-03-01 | 湖南大学 | A kind of epoxy acrylic ester prepolymer and its application |
| CN109824869A (en) * | 2019-01-31 | 2019-05-31 | 厦门源创力科技服务有限公司 | A kind of epoxy curing agent and preparation method thereof |
| CN112708109A (en) * | 2021-01-11 | 2021-04-27 | 安徽工业大学 | Modified aliphatic polyamine curing agent with long service life and preparation method thereof |
| CN112708109B (en) * | 2021-01-11 | 2022-10-28 | 安徽工业大学 | Modified aliphatic polyamine curing agent with long service life and preparation method thereof |
| CN115637125A (en) * | 2021-07-20 | 2023-01-24 | 中蓝晨光化工研究设计院有限公司 | Environment-friendly epoxy resin adhesive and preparation method thereof |
| CN115637125B (en) * | 2021-07-20 | 2023-09-12 | 中蓝晨光化工研究设计院有限公司 | Environment-friendly epoxy resin adhesive and preparation method thereof |
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Application publication date: 20140101 |