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Preparation method of mixed adipic acid alcohol amide curing agent

A kind of technology of adipic acid alcohol amide and curing agent, which is applied in the direction of coating, powder coating, polyester coating, etc., can solve the problems of uneven mixing of powder coating, easy yellowing, easy foaming of coating, etc., and achieve environmental pollution Small size, high product yield and low cost

Inactive Publication Date: 2020-04-28
JIANGSU XINLU CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Mixed adipamides include N,N,N',N'-tetrakis(β-hydroxyethyl)adipamide, N,N'-bis(β-hydroxyethyl)adipamide and N,N- Two (β-hydroxyethyl)-N'-(β-hydroxyethyl) adipamide three compounds, of which N, N, N', N'-tetrakis (β-hydroxyethyl) adipamide is mainly used It is used as a curing agent for powder coatings, but due to the high melting point of this compound, it is prone to yellowing, and it is unevenly mixed with carboxylated polyester powder coatings, and the coating is easy to foam. If mixed with N,N'-bis(β-hydroxyethyl base) adipamide and N,N-bis(β-hydroxyethyl)-N'-(β-hydroxyethyl)adipamide can improve the shortcomings of traditional curing agents for powder coatings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 500mL reaction bottle equipped with a thermometer, add 22.6g of diethanolamine, 13.9g of ethanolamine, and 0.8g of composite catalyst, install a condenser, start the agitator, and when the temperature rises to 90°C, start to add dimethyl adipate dropwise 34.8g, added dropwise within 1 hour, and kept warm for 6 hours (monitored the reaction by gas chromatography). After the reaction, cool down to 45°C, add 35g of a mixed solvent, decolorize the organic phase with activated carbon, filter out the catalyst and activated carbon, cool down, crystallize, and filter to obtain mixed adipamide, with a product yield of 95.35%.

Embodiment 2

[0029] In a 500mL reaction bottle equipped with a thermometer, add 22.6g of diethanolamine, 13.9g of ethanolamine, and 1.2g of composite catalyst, install a condenser, start the agitator, and when the temperature rises to 95°C, start to add dimethyl adipate dropwise 34.8g, added dropwise within 1h, and then kept warm for 8h (reaction monitored by gas chromatography). After the reaction, the temperature was lowered to 45°C, 45g of mixed solvent was added, and the organic phase was decolorized by activated carbon. After the catalyst and activated carbon were filtered out, the temperature was cooled, crystallized, and mixed adipamide was obtained by filtration. The product yield was 96.04%.

Embodiment 3

[0031] In a 500mL reaction flask equipped with a thermometer, add 24.8g of diethanolamine, 14.2g of ethanolamine, and 0.8g of composite catalyst, install a condenser, start the agitator, and start adding dimethyl adipate dropwise when the temperature rises to 100°C 34.8g, added dropwise within 1h, and then kept warm for 10h (reaction monitored by gas chromatography). After the reaction, the temperature was lowered to 45°C, 55g of mixed solvent was added, and the organic phase was decolorized with activated carbon. After the catalyst and activated carbon were filtered out, the temperature was cooled, crystallized, and mixed adipamide was obtained by filtration. The product yield was 95.12%.

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PUM

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Abstract

The invention provides a preparation method of a mixed adipic acid alcohol amide curing agent, and the method comprises the following steps: mixing diethanolamine, ethanolamine and a composite catalyst, and dropwisely adding dimethyl adipate; after the reaction is finished, adding a mixed solvent, then adding a decolorizing agent for decolorizing, and filtering out the decolorizing agent and the composite catalyst; cooling the obtained organic phase, crystallizing, and finally filtering to obtain the mixed adipic acid alcohol amide curing agent. According to the invention, the dimethyl adipate, the diethanolamine and the ethanolamine are used as raw materials to synthesize mixed adipic acid alcohol amide; by adopting the mixed catalyst, the separation and purification process is simple, the reaction time is short, the product yield is high and can reach more than 95%, the product purity is high, the energy consumption is reduced, the environmental pollution is small, the cost is low, and the method is an ideal process for realizing industrial preparation.

Description

technical field [0001] The invention relates to a preparation method of a mixed adipate alcohol amide curing agent. Background technique [0002] Mixed adipamides include N,N,N',N'-tetrakis(β-hydroxyethyl)adipamide, N,N'-bis(β-hydroxyethyl)adipamide and N,N- Two (β-hydroxyethyl)-N'-(β-hydroxyethyl) adipamide three compounds, of which N, N, N', N'-tetrakis (β-hydroxyethyl) adipamide is mainly used It is used as a curing agent for powder coatings, but due to the high melting point of this compound, it is prone to yellowing, and it is unevenly mixed with carboxylated polyester powder coatings, and the coating is prone to foaming. If mixed with N,N'-bis(β-hydroxyethyl Base) adipamide and N,N-bis(β-hydroxyethyl)-N'-(β-hydroxyethyl)adipamide can improve the shortcomings of traditional curing agents for powder coatings. Contents of the invention [0003] For addressing above-mentioned defective, the object of the present invention is to provide a kind of preparation method of t...

Claims

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Application Information

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IPC IPC(8): C09D5/03C09D7/63C09D167/00
CPCC09D5/033C09D167/00
Inventor 郑建王树清丁继叶
Owner JIANGSU XINLU CHEM NEW MATERIAL
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