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Beta-hydroxyalkyl amide synthesis process

A technology of hydroxyalkylamide and synthesis process, which is applied in the field of β-hydroxyalkylamide synthesis technology, can solve the problems of low product yield, unreasonable structure of β-hydroxyalkylamide synthesis equipment, low purity, etc., and achieve reduction Energy consumption, good practical value, and the effect of speeding up the response

Inactive Publication Date: 2014-03-26
HUBEI JIANGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a synthesis process of β-hydroxyalkylamides, which is used to solve the technical problems of existing β-hydroxyalkylamide synthesis equipment such as unreasonable structure, low product yield and low purity.

Method used

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  • Beta-hydroxyalkyl amide synthesis process

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: a kind of β-hydroxyalkylamide synthetic technique comprises the following steps:

[0021] A. Put 90 parts (100 grams per part, the same below) of diethanolamine and 0.5 parts of white carbon black into the β-hydroxyalkylamide synthesis reactor, add 1.85 parts of multi-component composite catalyst to the reactor, and the multi-component composite catalyst It is made by mixing 60% sodium methoxide, 29% potassium hydroxide, 5% sodium carbonate, 5% sodium sulfite and 1% sodium citrate;

[0022] B. After the feeding is completed, first pass through the argon gas for replacement three times, then pump out the gas in the kettle, control the temperature of the material in the kettle to 80°C, and the stirring speed to 90 rpm, and then add 135.83 parts of dimethyl adipate dropwise to the reaction kettle Esters were added dropwise in 1 hour;

[0023] C. After the addition of dimethyl adipate is completed, control the temperature in the heating tank to 110°C, stir at...

Embodiment 2

[0024] Embodiment 2: a kind of β-hydroxyalkylamide synthetic technique comprises the following steps:

[0025] A. 100 parts of diethanolamine and 0.5 part of white carbon black are dropped into the β-hydroxyalkylamide synthesis reactor, and 2.05 parts of multi-component composite catalysts are added in the reactor. The multi-component composite catalyst is composed of 70% sodium methylate, 16% Potassium hydroxide, 6% sodium carbonate, 6% sodium sulfite, 2% sodium citrate are mixed;

[0026] B. After the feeding is completed, first replace it with argon for three times, then pump out the gas in the kettle, control the temperature of the material in the kettle to 85°C, and the stirring speed to 90 rpm, and then add 150.92 parts of dimethyl adipate dropwise to the reaction kettle Esters were added dropwise in 1.5 hours;

[0027] C. After the addition of dimethyl adipate is completed, control the temperature in the heating tank to 115°C, the stirring speed is 45 rpm, react for 2....

Embodiment 3

[0028] Embodiment 3: a kind of β-hydroxyalkylamide synthetic technique comprises the following steps:

[0029] A. 110 parts of diethanolamine and 0.5 part of white carbon black are dropped into the β-hydroxyalkylamide synthesis reactor, and 2.26 parts of multi-component composite catalysts are added in the reactor. The multi-component composite catalyst is composed of 74% sodium methylate, 10% Potassium hydroxide, 7% sodium carbonate, 7% sodium sulfite, and 2% sodium citrate are mixed;

[0030] B. After the feeding is completed, first replace it with argon for three times, then pump out the gas in the kettle, control the temperature of the material in the kettle to 90°C, and the stirring speed at 90 rpm, and then add 166.01 parts of dimethyl adipate dropwise to the reaction kettle Ester, added dropwise in 2 hours;

[0031] C. After the addition of dimethyl adipate is completed, control the temperature in the heating tank to 120°C, the stirring speed is 50 rpm, react for 3 hou...

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Abstract

The invention relates to a beta-hydroxyalkyl amide synthesis process, which comprises the steps of inputting diethanol amine and silica into a reaction kettle, adding a multi-component composite catalyst into the reaction kettle, introducing argon gas for three times for gas replacement, extracting gas in the reaction kettle until the pressure reaches negative pressure, stirring and dripping dimethyl adipate into the reaction kettle, heating for two times and constantly stirring and introducing argon gas at the same time, and obtaining the finished product beta-hydroxyalkyl amide after the product cools down naturally. The beta-hydroxyalkyl amide synthesis process has the advantages of reasonable process, reliable performance and the like; under the catalytic action of the multi-component composite catalyst, ammonolysis of dimethyl adipate is realized through diethanol amine, ,and the beta-hydroxyalkyl amide is obtained, besides, sodium carbonate can accelerate the reaction, and sodium sulfite and sodium citrate have efficacy of xanthochromia resistance. The structure of the reaction kettle body for beta-hydroxyalkyl amide synthesis is reasonable, and temperature control and stirring effect are good; as reaction is performed under segmented temperature in the reaction kettle, mass production requirement can be satisfied.

Description

technical field [0001] The invention relates to a paint curing agent, in particular to a synthesis process of β-hydroxyalkylamide. Background technique [0002] N,N,N',N'-Tetrakis[β-Hydroxyethyl]adipamide (HAA for short), is a hydroxyalkylamide curing agent, suitable for curing polyester powder coatings containing carboxyl groups and acid anhydrides . It uses the hydroxyalkyl group on the β position to perform esterification and dehydration reaction with the carboxyl group on the resin. The coating film cured by HAA has good stability, corrosion resistance, impact resistance and durability. The traditional triglycidyl isocyanurate (TGIC) curing agent has certain toxicity. With the strengthening of occupational health awareness, β-hydroxyalkylamide curing agent has gradually replaced TGIC to become the largest type of curing agent. [0003] At present, there are more and more domestic manufacturers producing HAA, but the product yield and purity vary greatly. The synthesis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/18C07C231/02B01J31/26B01J19/18
Inventor 胡四军刘银彩余佳
Owner HUBEI JIANGDA CHEM
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