Preparation method for composite terminated waterborne epoxy resin curing agent

A technology of water-based epoxy resin and curing agent, which is applied in the direction of organic chemistry and can solve the problems of unseen reports and patents

Inactive Publication Date: 2015-05-13
SICHUAN VOCATIONAL & TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method for composite terminated waterborne epoxy resin curing agent
  • Preparation method for composite terminated waterborne epoxy resin curing agent
  • Preparation method for composite terminated waterborne epoxy resin curing agent

Examples

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Example Embodiment

[0026] Example 1

[0027] In the present embodiment, a kind of preparation method of composite end-blocking water-based epoxy resin curing agent, its process step is as follows in order:

[0028] (1) After dissolving 20.2g of N-(4-aminophenyl)maleimide and 0.25g of phase transfer catalyst benzyltriethylammonium chloride with 300ml of absolute ethanol, under the condition of nitrogen protection, the temperature was raised to 65°C, and then dropwise added 24.9 g of epichlorohydrin, and after the dropwise addition, the temperature was lowered to 55°C and reacted for 5 hours.

[0029] (2) Cool the reaction system to 30-40° C. and add 8.6 g of solid sodium hydroxide, then raise the temperature to 50° C. for 3 hours for ring closure reaction.

[0030] (3) After the reaction, cool down to room temperature, filter with suction, extract the filtrate with 3000ml of ethyl acetate, wash with deionized water for 3 times, and remove the ethyl acetate by rotary evaporation at 45°C to obtain...

Example Embodiment

[0031] Example 2

[0032] In the present embodiment, a kind of preparation method of composite end-blocking water-based epoxy resin curing agent, its process step is as follows in order:

[0033] (1) After dissolving 20.2g of N-(4-aminophenyl)maleimide and 0.25g of phase transfer catalyst tetrabutylammonium chloride in 300ml of propanol, the temperature was raised to 65°C under nitrogen protection , and then 24.9 g of epichlorohydrin was added dropwise, and after the dropwise addition, the temperature was lowered to 55° C. and reacted for 4 hours.

[0034] (2) Cool the reaction system to 30-40°C and add 8.6g of solid sodium hydroxide, then raise the temperature to 50°C to carry out the ring-closing reaction for 4 hours.

[0035] (3) After the reaction, cool down to room temperature, filter with suction, extract the filtrate with 4200ml of ethyl acetate, wash with deionized water for 3 times, and remove the ethyl acetate by rotary evaporation at 45°C to obtain the brown viscous ...

Example Embodiment

[0036] Example 3

[0037] In the present embodiment, a kind of preparation method of composite end-blocking water-based epoxy resin curing agent, its process step is as follows in order:

[0038] (1) After dissolving 20.2g of N-(4-aminophenyl)maleimide, 0.25g of phase transfer catalyst benzyltriethylammonium chloride with 360ml of absolute ethanol, under the condition of nitrogen protection, the temperature was raised to 65°C, then 29.9 g of epichlorohydrin was added dropwise, and after the dropwise addition, the temperature was lowered to 55°C and reacted for 6 hours.

[0039] (2) The temperature of the reaction system was lowered to 30-40° C. and 8.6 g of solid potassium hydroxide was added, and then the temperature was raised to 50° C. for 2 hours of ring closure reaction.

[0040] (3) After the reaction, cool down to room temperature, filter with suction, extract the filtrate with 3000ml of ethyl acetate, wash with deionized water for 3 times, and remove the ethyl acetate...

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Abstract

The invention discloses a preparation method for a benzoxazine intermediate containing a maleimide biphenyl diphenol structure. The preparation method comprises the following steps: (1) producing a synthesis reaction 1, namely adding an aldehyde compound and a solvent into a reaction container and mixing uniformly under the normal pressure at a normal temperature, adding an amine compound into the container while stirring, and reacting for at least 10 hours at 0-100 DEG C under the normal pressure; after reacting, pouring reaction liquor into washing liquor for washing, filtering, collecting solid matters, and drying at 30-100 DEG C to obtain an intermediate containing a triazine structure; (2) producing a synthesis reaction 2, namely adding the solid matters (triazine), the aldehyde compound, biphenyl diphenol and 1,4-dioxane into the reaction container in sequence, mixing uniformly, heating to 110 DEG C, performing reflux reaction for 30 hours to obtain reaction liquor containing earthy yellow deposits, pouring the obtained reaction liquor into de-ionized water, fully stirring, depositing, performing suction filtration, washing with the de-ionized water and ethanol for multiple times, and drying in a drying oven to obtain an earthy yellow powdery solid target product.

Description

Technical field: [0001] The invention belongs to the field of preparation of epoxy resin curing agent, in particular to a preparation method of composite end-capped water-based epoxy resin curing agent. Background technique: [0002] Epoxy resin coatings have the characteristics of high hardness, good wear resistance, high adhesion and excellent chemical resistance, and are widely used in the field of coating. In recent years, with the continuous improvement of people's awareness of environmental protection, many countries have promulgated environmental regulations to limit volatile organic solvents (VOC), and water-based coatings have become an important trend in the development of coatings. At present, the water-based technology of epoxy resin at home and abroad is mainly divided into two categories: emulsification method and salt-forming method. The emulsification method refers to direct emulsification of epoxy resin, self-emulsification without external emulsifier or em...

Claims

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Application Information

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IPC IPC(8): C07D405/14C08G59/50
CPCC07D405/14C08G59/506
Inventor 陶果陈自然徐友辉王碧曾琪成诚
Owner SICHUAN VOCATIONAL & TECHN COLLEGE
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