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Beta-hydroxyalkylamide curing agent preparation method

A technology of hydroxyalkylamide and curing agent, which is applied in the field of preparation of β-hydroxyalkylamide curing agent, can solve the problems of increased solvent consumption and post-processing steps, large equipment investment, and low total yield, and achieve strong industry Effects of utilization and popularization, simple operation unit, and low investment in equipment

Pending Publication Date: 2020-01-03
甘肃青宇新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Using methanol etc. as a solvent not only increases solvent consumption and post-processing steps, but also the volatilization of the crystallization solvent will cause environmental pollution
[0005] 2. The high-temperature melting reaction is easy to make the material turn yellow, and recrystallization is required to decolorize
[0006] 3. The total yield is low
This synthesis method requires a relatively large investment in equipment, and it is difficult to grasp the control point in actual operation.

Method used

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  • Beta-hydroxyalkylamide curing agent preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A preparation method of β-hydroxyalkylamide curing agent, comprising the following preparation steps:

[0029] (1) Get four-necked bottle, device mechanical stirring, condenser tube and thermometer, take by weighing dimethyl adipate, diethanolamine and catalyst (diethanolamine and dimethyl adipate mol ratio are 2.5, catalyst and product A weight ratio is 0.14%), added to the reaction flask, heated up to 65°C for reaction under reduced pressure, stirred for 2 hours, evaporated methanol as a volatile component, and obtained tetrahydroxyethyl adipamide solution, which was product A;

[0030] (2) The product A was solidified in a tray for 10 hours, crushed into powder and dried at 85°C. Crushed and dried to obtain white powder solid tetrahydroxyethyl adipamide curing agent.

Embodiment 2

[0032] A preparation method of β-hydroxyalkylamide curing agent, comprising the following preparation steps:

[0033] (1) Get four-necked bottle, device mechanical stirring, condenser tube and thermometer, take by weighing dimethyl adipate, diethanolamine and catalyst (diethanolamine and dimethyl adipate mol ratio are 2.4, catalyst and product A weight ratio of 0.14%), added to the reaction flask, heated to 80 ° C and reacted under reduced pressure, stirred for 2 hours, evaporated the volatile methanol, and obtained tetrahydroxyethyl adipamide solution, which was product A;

[0034] (2) The product A was cured in a tray for 9 hours, broken into powder and dried at 95°C. Crushed and dried to obtain white powder solid tetrahydroxyethyl adipamide curing agent.

Embodiment 3

[0036] A preparation method of β-hydroxyalkylamide curing agent, comprising the following preparation steps:

[0037] (1) Get four-necked bottle, device mechanical stirring, condenser tube and thermometer, take diethyl adipate, diethanolamine and catalyst (diethanolamine and dimethyl adipate mol ratio are 2.0, catalyst and product A weight ratio is 0.12%), added to the reaction flask, heated up to 75°C for reaction under reduced pressure, stirred for 2 hours, evaporated the volatile component ethanol, and obtained tetrahydroxyethyl adipamide solution, which was product A;

[0038] (2) The product A was cured in a tray for 8 hours, broken into powder and dried at 100°C. Crushed and dried to obtain white powder solid tetrahydroxyethyl adipamide curing agent.

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PUM

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Abstract

The invention discloses a beta-hydroxyalkylamide curing agent preparation method, which comprises: (1) mixing dimethyl adipate or diethyl adipate and diethanol amine, adding a catalyst, heating, and carrying out pressure reducing distillation to remove volatile components to obtain a tetrahydroxyethyl adipamide solution, i.e., a product A, wherein the reaction equation formula is defined in the specification; and (2) curing the product A, breaking, and drying to obtain a white powder solid, ie., the qualified tetrahydroxyethyl adipamide (beta-hydroxyalkylamide). The method of the invention hasadvantages of high yield, no generation of wastewater, waste liquid and waste solid during preparation, environmental protection, less equipment investment and simple operation.

Description

technical field [0001] The invention relates to the technical field of coatings, in particular to a preparation method of a β-hydroxyalkylamide curing agent. Background technique [0002] β-Hydroxyalkylamide is a kind of substance with β-hydroxyl group of multi-hydroxyalkyl functional group. Since the hydroxyl group is in the β position, it can undergo cross-linking reaction with the carboxyl group in the resin molecule under the influence of the N atom, so it can be used as Used as a curing agent for polyester resin powder coatings. As a new type of powder coating curing agent, β-hydroxyalkylamide not only has the advantages of low toxicity, no irritation, no mutagenesis, etc., but also has good application properties such as weather resistance, heat resistance, and corrosion resistance, and has good Leveling and excellent impact resistance. Therefore, it has attracted the attention of researchers in the field of powder coatings. [0003] At present, the method for produ...

Claims

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Application Information

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IPC IPC(8): C07C235/74C07C231/02C09D5/03C09D167/00
CPCC07C231/02C08K2003/2241C09D5/033C09D167/00C07C235/74C08K3/22
Inventor 刘旭亮李振勇周幸旺寇成龙赵萍蕊
Owner 甘肃青宇新材料有限公司
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