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Epoxy curing agent synthesized through mercapto-vinyl addition

An epoxy curing agent, mercaptoethylene technology, applied in organic chemistry, sulfide preparation and other directions, can solve the problems of difficult curing, poor leveling, easy to form salt, etc.

Inactive Publication Date: 2014-07-23
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organic amine or modified organic amine curing agents are highly toxic, highly irritating to the human body, easy to form salts, poor leveling, and require a curing step during construction; acid anhydride and latent curing agents have high curing reaction temperature and no catalyst assistance not easy to solidify

Method used

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  • Epoxy curing agent synthesized through mercapto-vinyl addition
  • Epoxy curing agent synthesized through mercapto-vinyl addition
  • Epoxy curing agent synthesized through mercapto-vinyl addition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a three-necked flask with a stirring device and a thermometer, add 50.5 parts of ethoxytrimethylolpropane triacrylate, 38.5 parts of 3-mercaptopropionic acid, and 1 part of azobisisobutyronitrile. Stirring was started, and the temperature was raised to 70° C. under nitrogen bubbling, reacted for 8 hours, cooled and discharged. The resulting product was a colorless, clear, viscous liquid. Since this product has three active carboxyl groups, it can be used as a curing agent for epoxy resins. The H NMR spectrum of the product was tested with an NMR instrument ( 1 HNMR) such as figure 1 , showing the obvious proton signal of propyl sulfide (2.55-2.88ppm), at the same time, the C=C double bond peak at 5.81-6.22ppm has completely disappeared, indicating that the C=C unsaturated double bond has been completely converted to carboxyl. In addition, after mixing 1.275g of the product with 1.000g of bisphenol A epoxy resin (E-51), the reaction performance of the mixture was ...

Embodiment 2

[0024] In a three-necked flask with a stirring device and a thermometer, add 55.4 parts of propoxytrimethylolpropane triacrylate, 38.5 parts of 3-mercaptopropionic acid, and 2.5 parts of benzoin dimethyl ether. Stirring was started, under the condition of nitrogen bubbling, the reaction was irradiated with ultraviolet light for 2 hours, the temperature was cooled and the material was discharged. The resulting product was a colorless, clear, viscous liquid. Since this product has three active carboxyl groups, it can be used as a curing agent for epoxy resins. The H NMR spectrum of the product was tested with an NMR instrument ( 1 HNMR) such as image 3 , showing significant proton signals of propyl sulfide (2.55-2.88ppm) and hydrogen protons on carboxyl groups (7.39-8.45ppm). It shows that the C=C unsaturated double bond has been completely converted into a carboxyl group.

Embodiment 3

[0026] Add 40 parts of trimethylolpropane diallyl ether, 59 parts of 3-mercaptopropionic acid, and 1 part of azobisisobutyronitrile (AIBN) into a three-necked flask with a stirring device and a thermometer. Stirring was started, and the temperature was raised to 70° C. under nitrogen bubbling, reacted for 8 hours, cooled and discharged. The obtained product is a colorless or pale yellow, transparent, viscous liquid. In order to confirm that the obtained product can be used as an epoxy curing agent, it was mixed equimolarly with bisphenol A type epoxy resin (E-44). The reaction performance of the mixture was measured by differential scanning calorimeter (DSC), and the reaction curve is shown in Figure 4 .

[0027]

[0028] Mercapto-Vinyl Addition Reaction of Trimethylolpropane Diallyl Ether with 3-Mercaptopropionic Acid

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Abstract

The invention discloses an epoxy curing agent synthesized through mercapto-vinyl addition. The epoxy curing agent is synthesized through carrying out addition reaction on a C=C double-bond containing acrylate or vinyl ether compound with difunctionality or polyfunctionality and a mercapto compound under the condition of light or heat initiation. A preparation method of the epoxy curing agent comprises the steps of adding a C=C double-bond containing difunctional or polyfunctional compound, the mercapto compound, a proper volume of solvent (such as 1,4-dioxane) and a free radical initiator or photoinitiator into a three-mouthed flask, reacting for certain time under the condition of heating or lighting, and removing the solvent, thereby obtaining the product. The epoxy curing agent overcomes the disadvantages of the existing modified amine and polymercaptan epoxy curing agents that the odor is strong, the toxicity is high, the heat release quantity is large during curing and the like; and the epoxy curing agent has the advantages of light color and luster, high index of refraction, low toxicity and the like and accordingly is particularly suitable for serving as a curing agent of epoxy encapsulation materials of electronic products, such as LED (Light Emitting Diode).

Description

Technical field: [0001] The invention relates to a novel epoxy curing agent, especially the application of epoxy coatings, adhesives and potting glue, and the specific content is a preparation method of a modified epoxy curing agent. technical background: [0002] Epoxy resin is an important compound in the field of synthetic resins. It is widely used in composite materials, Electronics, chemical industry, civil engineering and other fields. High-performance coatings, inks, adhesives and composites that can be made from epoxy resins. [0003] Since epoxy resin is a low-molecular thermoplastic polymer, to make epoxy resin exert its excellent performance, it is necessary to carry out cross-linking reaction between epoxy resin and curing agent to form a linear or cross-linked macromolecule. There are many kinds of curing agents for epoxy resins, commonly used are amines or modified amines, acid anhydrides or latent curing agents. Organic amine or modified organic amine curin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/42C08G59/62C08G59/64C07C319/18C07C323/52C07C323/25
Inventor 郑耀臣薛清泉李婧任万忠
Owner YANTAI UNIV
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