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Beta-hydroxyalkylamide curing agent as well as preparation method and application thereof

A technology of hydroxyalkylamide and curing agent, which is applied in the field of β-hydroxyalkylamide curing agent and its preparation, which can solve the problems of complex preparation method and easy corrosion, and achieve the effects of small dosage, increased yield and uniform dispersion

Pending Publication Date: 2020-12-04
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention provides a kind of preparation method of β-hydroxyalkylamide curing agent in order to overcome the defects of complex preparation method and easy-to-corrosion reaction equipment described in the above-mentioned prior art

Method used

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  • Beta-hydroxyalkylamide curing agent as well as preparation method and application thereof
  • Beta-hydroxyalkylamide curing agent as well as preparation method and application thereof
  • Beta-hydroxyalkylamide curing agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 provides a kind of β-hydroxyalkylamide curing agent, the preparation method of this β-hydroxyalkylamide curing agent comprises the steps:

[0043] Add diethanolamine 18.92g (1.8mol) and 40%KOH / XL 552 solid base catalyst 0.158g (0.8wt% of total material) in four-necked flask, under inert gas N 2 The temperature was raised to 80°C under atmosphere. After pumping out the gas in the reaction flask to a pressure of -0.065 MPa, 17.42 g (1.0 mol) of dimethyl adipate was evenly added dropwise within 1.5 h, and at the same time, the alcohol continuously produced in the ammonolysis reaction was removed by vacuum distillation. After the ammonolysis reaction was continued for 4 hours, the temperature was raised to 119°C, and the raw materials and by-products that did not participate in the reaction were removed by vacuum distillation at a pressure of -0.09MPa, and the state of the reactants was observed. When a white solid product was obtained, the reaction ended.

[...

Embodiment 2

[0047] Embodiment 2 provides a kind of β-hydroxyalkylamide curing agent, the difference of the preparation method of this β-hydroxyalkylamide curing agent and embodiment 1 is: the addition amount of diethanolamine is 26.28g (2.5mol), 40% The addition amount of KOH / XL552 solid base catalyst is 0.657g (2.5wt% of total material).

[0048]The β-hydroxyalkylamide curing agent prepared in this example: N,N,N',N'-tetrakis(β-hydroxyethyl)adipamide totaled 40.8g, and the yield was 92.0%.

Embodiment 3

[0050] Embodiment 3 provides a kind of β-hydroxyalkylamide curing agent, the difference of the preparation method of this β-hydroxyalkylamide curing agent and embodiment 1 is: the addition amount of diethanolamine is 22.66g (2.15mol), 40% The addition amount of KOH / XL552 solid base catalyst is 0.485g (1.2wt% of total material).

[0051] The β-hydroxyalkylamide curing agent prepared in this example: N,N,N',N'-tetrakis(β-hydroxyethyl)adipamide totaled 38.37g, and the yield was 94.58%.

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Abstract

The invention discloses a beta-hydroxyalkylamide curing agent as well as a preparation method and application thereof. The preparation method of the beta-hydroxyalkylamide curing agent comprises the following steps: S1, mixing alkanolamine and a supported solid base catalyst, heating, reducing pressure, dropwise adding carboxylic acid alkyl ester, simultaneously carrying out reduced pressure distillation to remove byproduct alcohol, and carrying out ammonolysis reaction to obtain a white solid product; S2, adding the white solid product into methanol for recrystallization, and performing post-treatment to obtain the white powdery beta-hydroxyalkylamide curing agent; wherein in the supported solid base catalyst, the base serving as a precursor is one of sodium hydroxide, potassium hydroxideand potassium carbonate, and the carrier is N, N, N ', N'-tetra (beta hydroxyethyl) adipamide. The preparation method provided by the invention is efficient and environment-friendly, the product yield is high, the preparation conditions are mild, and reaction equipment is not damaged.

Description

technical field [0001] The invention relates to the field of organic synthesis, more specifically, to a β-hydroxyalkylamide curing agent and its preparation method and application. Background technique [0002] Powder coating has the characteristics of energy saving, low pollution and high efficiency, and has become a recognized coating product that is eco-friendly, economical, high production efficiency and excellent coating performance. As people's awareness of environmental protection increases year by year, powder coatings are widely used in fields such as home appliances, furniture, automobile bodies and building materials. Powder coating is composed of resin and additives. The resin determines the structure, type and quality of the powder coating, while the additives, especially the curing agent, determine the aggregation state of the coating and play a vital role in the performance of the coating. . [0003] Triglycidyl isocyanurate (TGIC) is currently the most impo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/18C09D7/63C09D5/03
CPCC07C231/02C09D5/033C07C233/18
Inventor 易国斌苏秋萍王韶顺刘杰鸣何嘉健林霄峰林文静俎喜红
Owner GUANGDONG UNIV OF TECH