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Method for preparing N,N,N',N'-tetra(beta-hydroxypropyl) adipamide

A technology of adipamide and hydroxypropyl, which is applied in the field of preparing N,N,N',N'-tetraadipamide, which can solve the problem of low separation efficiency of diisopropanolamine, high energy cost and product chromaticity uncontrollable issues

Pending Publication Date: 2021-11-26
南京安科迩环保新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing separation method mainly adopts crystallization separation or distillation to separate diisopropanolamine in the synthetic product. The disadvantage of the crystallization separation method is that the yield is low, and the remaining materials and products after separation are difficult to recycle at the same time, so the production cost is high and the defect of the method of distillation separation is that diisopropanol is a heat-sensitive substance, and the product chromaticity in the separation process is difficult to control, and the separation efficiency of diisopropanolamine is also low, and the purity is low, and compared with the crystallization separation method, its Energy costs are relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 166.3g of diisopropanolamine and 1.15g of potassium hydroxide into a glass reactor, stir and heat to a reaction temperature of 100°C, and drop 87.0g of dimethyl adipate into the reaction vessel under a vacuum condition of -0.099MPa. In the kettle, after the feed was completed, the stirring reaction was continued for 2 hours.

[0020] After the reaction was completed, the temperature of the material was lowered to 60 ° C, and under the condition of -0.099 MPa, 25.0 g of concentrated sulfuric acid was added dropwise. After stirring and crystallizing, diisopropanolamine sulfate was separated by filtration, and the filtrate was distilled to remove the ethanol solvent to obtain 169.7g of N,N,N',N'-tetrakis(β-hydroxypropyl)adipamide product, product yield It is 90.3%, and the product purity is 96.2%.

Embodiment 2

[0022] Add 199.5g of diisopropanolamine and 1.15g of potassium hydroxide into the glass reaction kettle, stir and heat to the reaction temperature of 100°C, and drop 87.0g of dimethyl adipate into the reaction under the vacuum condition of -0.099MPa In the kettle, after the feed was completed, the reaction was continued under reduced pressure and stirred for 2 hours.

[0023] After the reaction was completed, the temperature of the material was lowered to 80°C. Under the condition of vacuum -0.090, 50.0g of concentrated sulfuric acid was added dropwise. After the dropwise addition, the stirring was continued for 1 hour under this condition. After stirring and crystallizing, diisopropanolamine sulfate was separated by filtration, and the filtrate was distilled to remove the ethanol solvent to obtain 173.0g of N,N,N',N'-tetrakis(β-hydroxypropyl)adipamide product, the product yield It is 92.0%, and the product purity is 97.7%.

Embodiment 3

[0025] Add 266.0g of diisopropanolamine and 1.15g of potassium hydroxide into the glass reactor, stir and heat to the reaction temperature of 100°C, and drop 87.0g of dimethyl adipate into the reaction vessel under the vacuum condition of -0.099MPa In the kettle, after the feed was completed, the reaction was continued under reduced pressure and stirred for 2 hours.

[0026] After the reaction is completed, the temperature of the material is lowered to 80°C. Under the condition of -0.099MPa, 100g of concentrated sulfuric acid is added dropwise. After the dropwise addition, the stirring is continued for 1 hour under this condition, and then 700.0g of n-propanol is added, and the temperature is lowered to 25°C. After stirring and crystallizing, diisopropanolamine sulfate was separated by filtration, and the filtrate was removed by distillation to remove the n-propanol solvent to obtain 180.8g of N, N, N', N'-tetrakis (β-hydroxypropyl) adipamide product, The product yield is 96.2...

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Abstract

The invention discloses a method for preparing N,N,N',N'-tetra(beta-hydroxypropyl) adipamide, which comprises the following steps: (1) adding excessive diisopropanolamine and a basic catalyst into a reaction kettle, and then dropwise adding dimethyl adipate to prepare a crude product of N,N,N',N'-tetra(beta-hydroxypropyl) adipamide; (2) lowering the temperature in the reaction kettle to a set temperature, dropwise adding or adding neutralizing acid into the reaction kettle in batches under a vacuum condition so as to neutralize the excessive diisopropanolamine, and dehydrating at the same time; (3) after the neutralization is finished, adding a solvent into the reaction kettle, stirring and crystallizing, then filtering, and separating out diisopropanolamine sulfate, and subjecting the filtrate to distillation to separate the solvent so as to obtain the N,N,N',N'-tetra(beta-hydroxypropyl) adipamide product with high purity. According to the method, the unreacted diisopropanolamine raw material is separated by utilizing the high-amine ester, so that the preparation process is simple in flow and low in energy consumption, and the separated diisopropanolamine salt can be recycled as an industrial raw material.

Description

technical field [0001] The invention relates to a method for preparing N,N,N',N'-tetrakis(β-hydroxypropyl)adipamide. Background technique [0002] β-Hydroxyalkylamide is a thermosetting polyester powder coating curing agent, the main varieties are tetrakis-(β-hydroxyethyl)adipamide, tetrakis-(β-hydroxypropyl)adipamide, etc. The four-functional low-toxicity thermosetting polyester powder coating curing agent has the advantage of low toxicity compared with the traditional TGIC type curing agent. It is currently the best TGIC substitute for application performance and has a great application prospect. [0003] At present, the preparation methods of β-hydroxyalkylamide generally use alkanolamine and dialkyl dicarboxylate as raw materials, and they are synthesized and prepared under alkaline conditions. Alkanolamine conditions, and this synthetic reaction condition will increase the probability of side reactions, reducing the selectivity of the synthetic reaction, especially whe...

Claims

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Application Information

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IPC IPC(8): C07C233/18C07C231/02C07C231/24
CPCC07C231/02C07C231/24C07C233/18
Inventor 汪少平田秀娟江忠义
Owner 南京安科迩环保新材料有限公司
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