Preparation method of high-modulus heterocyclic epoxy resin

An epoxy resin, high modulus technology, applied in organic chemistry and other directions, can solve the problems of brittleness, peeling, inconvenient operation, etc., and achieve the effect of simple preparation method, good compatibility, and improved overall performance

Active Publication Date: 2021-04-23
山东天茂新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Epoxy resin has excellent mechanical properties and adhesive properties, but its weather resistance is poor, especially in the western outdoor areas, and it will become brittle, peeled, and cracked in less than two or three years.
At present, the usual solution on the market is to add anti-ultraviolet fillers to the epoxy resin and curing agent system. The above method is not only inconvenient to operate, but also often needs to add organic solvents to adjust its viscosity. The generation of VOCs brings great harm to the environment. pressure
At the same time, even if the anti-ultraviolet ability is improved by adding fillers, it is difficult to have both good flexural modulus and anti-ultraviolet performance

Method used

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  • Preparation method of high-modulus heterocyclic epoxy resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: the preparation of high modulus heterocyclic epoxy resin

[0027] 1) Add 126g of 1,2,4-glucinol and 76.5g of allyl chloride into a 500ml four-neck flask equipped with a heating mantle, stirrer, and reflux condenser, and stir for 3 hours at a controlled temperature of 55-60°C;

[0028] 2) Then add 0.0665g of catalyst aluminum trichloride, heat up to 250°C, under negative pressure of 0.4MPa, transposition and cyclization occur for 80min, wash with water 3 times, and dry to obtain 152g of heterocyclic bisphenol;

[0029] 3) Weigh 100g of heterocyclic bisphenol and 100g of epichlorohydrin and heat to 30°C to fully dissolve, continue to heat up to 55°C, add 20g of 30% sodium hydroxide solution, keep warm for 2 hours, and continue to add 50% sodium hydroxide 46g of the solution was heated to 78°C, kept for 4 hours, washed 3 times with water, extracted 3 times with 200ml of acetone, combined the extracts, concentrated under reduced pressure to remove the solvent ...

Embodiment 2

[0035] Embodiment 2: Preparation of cured product of high modulus heterocyclic epoxy resin

[0036] 1) Add 126g of 1,2,3-glucinol and 77g of allyl chloride into a 500ml four-neck flask equipped with a heating mantle, stirrer, and reflux condenser, and stir for 2.5 hours at a controlled temperature of 55-60°C;

[0037] 2) Then add 0.08g of catalyst aluminum trichloride, raise the temperature to 260°C, and under the negative pressure of 0.4MPa, transposition and cyclization occur for 1.5h, wash with water 3 times, and dry to obtain 151g of heterocyclic bisphenol;

[0038] 3) Weigh 100g of heterocyclic bisphenol and 100g of epichlorohydrin and heat to 30°C to fully dissolve, continue to heat up to 58°C, add 22g of 30% sodium hydroxide solution, keep warm for 1.5h, continue to add 50% hydroxide 45g of sodium solution was heated up to 80°C, kept for 3.5h, washed 3 times with water, extracted 3 times with 200ml of toluene each time, combined the extracts, concentrated under reduced ...

Embodiment 3

[0039] Embodiment 3: Preparation of cured product of high modulus heterocyclic epoxy resin

[0040] 1) Add 126g of 1,3,5-glucinol and 77g of allyl chloride into a 500ml four-neck flask equipped with a heating mantle, stirrer, and reflux condenser, and stir for 2.5 hours at a controlled temperature of 55-60°C;

[0041] 2) Then add 0.07g of catalyst aluminum trichloride, raise the temperature to 260°C, and under negative pressure of 0.4MPa, transposition and cyclization occur for 1.5h, wash with water 3 times, and dry to obtain 151g of heterocyclic bisphenol;

[0042] 3) Weigh 100g of heterocyclic bisphenol and 100g of epichlorohydrin and heat to 30°C to fully dissolve, continue to heat up to 58°C, add 20g of 30% sodium hydroxide solution, keep warm for 1.5h, continue to add 50% hydroxide 45g of sodium solution was heated up to 80°C, kept for 3.5h, washed with water three times, added xylene for extraction three times, 200ml each time, the extracts were combined, concentrated un...

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Abstract

The invention discloses a preparation method of high-modulus heterocyclic epoxy resin. The preparation method comprises the following steps of: reacting benzenetriol with allyl chloride to generate 1-allyl benzenetriol, carrying out high-temperature transposition and cyclization to obtain heterocyclic bisphenol, reacting the heterocyclic bisphenol with epoxy chloropropane under the catalytic action of liquid caustic soda, and carrying out solvent refining to obtain the heterocyclic epoxy resin. After being cured, the heterocyclic epoxy resin has very high modulus, adhesion and weather resistance, has very good compatibility when being mixed with common epoxy resin, and can improve the overall performance of the epoxy resin.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to a preparation method of a high modulus heterocyclic epoxy resin. Background technique [0002] Epoxy resin refers to the general term for a class of polymers containing two or more epoxy groups in the molecule. Epoxy resins can cross-link with amine or acid anhydride curing agents to form insoluble and infusible polymers with a three-dimensional network structure. The excellent physical, mechanical and electrical insulation properties of epoxy resin, the bonding performance with various materials, and the flexibility of its use process are not available in other thermosetting plastics. Therefore, it can be made into coatings, composite materials, casting materials, adhesives, molding materials and injection molding materials, and is widely used in various fields of the national economy. [0003] Epoxy resin has excellent mechanical properties and adhesive properties, but it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/26C07D407/14
CPCC08G59/26C07D407/14
Inventor 李文泉李冉李文峰
Owner 山东天茂新材料科技股份有限公司
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