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Beta-hydroxyalkylamide and preparation method thereof

A technology of hydroxyalkylamide and alkyl, which is applied in the field of curing agent and its preparation, can solve the problems of harsh synthesis conditions and low yield, and achieve the effects of low production cost, simple synthesis and strong reactivity

Active Publication Date: 2016-05-04
NANJING JINHAO MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis conditions of this product are harsh and the yield is low
[0005] China Ningbo Nanhai Chemical Co., Ltd. has developed T105 and T105M series products, but the main component is still N,N,N',N'-tetrakis(β-hydroxyethyl)adipamide, which fails to solve the problem fundamentally

Method used

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  • Beta-hydroxyalkylamide and preparation method thereof
  • Beta-hydroxyalkylamide and preparation method thereof
  • Beta-hydroxyalkylamide and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Preparation of N,N'-bis(β-hydroxyethyl)adipamide

[0035] Place 0.5mol dimethyl adipate and 1mol ethanolamine in a four-necked flask, then add 0.6g potassium hydroxide as a catalyst, under N 2 Under protection, the reaction was heated and refluxed, and the reaction temperature was controlled at about 90°C with a temperature-controlled water bath until no methanol distilled out, and the reaction was terminated. The obtained product crystallized immediately after standing at room temperature to obtain a pale yellow solid. The light yellow solid was recrystallized with methanol and acetone to obtain a white solid, which was placed in a vacuum oven and dried.

Embodiment 2

[0037] Preparation of N,N'-bis(β-hydroxyethyl)-N,N'-bis(β-hydroxypropyl)adipamide 0.88gN,N'-bis(β-hydroxyethyl)adipamide Dissolve in 3.7g dimethylformamide, slowly add 0.44g propylene oxide dropwise at 60°C, after the dropwise addition is completed, heat up and reflux for 2 hours; cool down to room temperature, wash the product with 20% NaOH, distill the solvent, white The residue is refined with ethanol to obtain the target product with a content greater than 99%.

Embodiment 3

[0039] Preparation of N,N'-bis(β-hydroxyethyl)adipamide Place 0.5mol dimethyl adipate and 1mol ethanolamine in a four-necked flask, then add 2.6g n-butyl titanate as a catalyst, N 2 Under protection, the reaction was heated and refluxed, and the reaction temperature was controlled at about 90°C with a temperature-controlled water bath until no methanol distilled out, and the reaction was terminated. The obtained product crystallized immediately after standing at room temperature to obtain a white transparent solid. The white solid was dried in a vacuum oven.

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Abstract

The invention discloses beta-hydroxyalkylamide and a preparation method thereof, relates to a curing agent and a preparation method thereof and provides a preparation method of N,N'-bis(beta-hydroxyethyl)-N,N'bis(beta-hydroxypropyl) adipamide. Dimethyl adipate, ethanolamine and propylene oxide are taken as raw materials for synthesis of N,N'-bis(beta-hydroxyethyl)-N,N'bis(beta-hydroxypropyl) adipamide. The synthetic method of N,N'-bis(beta-hydroxyethyl)-N,N'bis(beta-hydroxypropyl) adipamide comprises two steps: (1) synthesis of N,N'-bis(beta-hydroxyethyl) adipamide; (2) addition reaction. A product obtained with the method has high purity and good performance, and an obtained intermediate product is an important organic intermediate. The method has the advantages that the molecular reaction activity is reduced, the reaction speed is reduced, so that the viscosity of a coating film is improved, and an anti-pinhole effect is enhanced; the synthesis is simple, severe conditions such as high pressure, high vacuum and the like are avoided, the production cost is lower, and industrialization is facilitated.

Description

technical field [0001] The invention relates to a curing agent and a preparation method thereof, in particular to a β-hydroxyalkylamide and a preparation method thereof. Background technique [0002] β-Hydroxyalkylamide (HAA) is a new type of curing agent, which is widely used in the fields of daily chemicals, surfactants and coatings. It can not only be used as a cross-linking agent for water-based and solvent-based coatings, but especially for powder coatings. It is a new type of solid agent that is less toxic than the traditional weather-resistant powder special curing agent TGIC. It is a low-toxic and environmentally friendly type compound, which has the characteristics of strong reactivity and stable storage, and its application in Europe and America is on the rise. With the development of the economy, countries and regions are becoming more and more aware of environmental protection, which makes HAA have greater development space and application prospects. [0003] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/18C07C231/12C09D167/00C09D7/12C09D5/03
CPCC07C231/02C07C231/12C08K5/20C09D5/033C09D167/00C07C233/18
Inventor 孔祥文顾春玲王欢张静
Owner NANJING JINHAO MEDICAL TECH CO LTD
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