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Production technology of beta-hydroxyalkylamide

A technology of hydroxyalkylamide and production process, applied in the field of production technology of β-hydroxyalkylamide, can solve the problems of ineffective slurry sedimentation and low melting point, and achieves improved application performance, high purity, and reduced side reactions Effect

Active Publication Date: 2010-05-12
六安捷通达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the β-hydroxyalkylamide target product (such as β-hydroxypropylamide) has a low melting point and cannot settle out of the molten system, the slurry sedimentation method cannot be effective

Method used

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  • Production technology of beta-hydroxyalkylamide
  • Production technology of beta-hydroxyalkylamide
  • Production technology of beta-hydroxyalkylamide

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Put 150.7kg (1.2kmol) of diethanolamine and 1.74kg of sodium methoxide into a reaction kettle with a gas dispersion device at the bottom, and heat it to 110°C under the protection of nitrogen. After the gas in the kettle is pumped out until the pressure in the kettle reaches 0.03MPa, at 1.5 Add 174.0kg (1kmol) dimethyl adipate dropwise within 2h, stir the reaction constantly, and simultaneously steam the methanol released during the reaction. After 1h of reaction, add 2.0kg of acetic acid to the reaction mixture, stir and mix thoroughly Afterwards, the temperature of the reaction system was raised to 180°C and kept warm, and the reaction system was filled with nitrogen gas bubbling through the gas dispersion device at the bottom of the reactor at a pressure of 0.5 MPa for 5 minutes and stirred continuously, and then the nitrogen flow was stopped. Evaporate excess diethanolamine under reduced pressure until the pressure of the kettle reaches 0.003MPa and continue vacuumin...

Embodiment 2

[0044] Put 266.2kg (2kmol) of diisopropanolamine and 3.0kg of potassium hydroxide mixture into a reaction kettle with a gas dispersion device at the bottom, and heat to 100°C under nitrogen protection. After the gas in the kettle was pumped out until the pressure inside the kettle reached 0.05MPa, 174.0kg (1kmol) dimethyl adipate was added dropwise within 2 hours, the reaction was continuously stirred, and the methanol released during the reaction was distilled synchronously. After another 1 hour of reaction, add 5.0kg of propionic acid to the reaction mixture, stir and mix thoroughly, then raise the temperature of the reaction system to 150°C, and pass through the gas dispersion device at the bottom of the reaction kettle at a pressure of 0.3MPa for 5 minutes. Bubble nitrogen into the molten reaction system and keep stirring, then stop nitrogen, distill off excess diisopropanolamine under reduced pressure until the pressure of the kettle reaches 0.004MPa and continue vacuuming...

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Abstract

The invention discloses a production technology of beta-hydroxyalkylamide. The method comprises the following steps: taking carboxylic acid alkyl ester and excessive beta-alkanolamine as raw materials, conducting aminolysis reaction while heating and stirring, then adding volatile acid to break alkali catalyst, further raising temperature, constantly removing byproducts and the unreacted beta-alkanolamine by adopting the combination of bubbling and sweeping by inert gas and the reduced pressure distillation process, and then emptying, cooling and grinding to directly obtain a high-purity beta-hydroxyalkylamide powder product. The production technology purifies products by replacing the traditional organic solvent crystallization technology with the combination of bubbling and sweeping by the inert gas and the reduced pressure distillation process, needs not to add acetone, methanol and other organic solvents and can not only obtain the high-purity beta-hydroxyalkylamide product, but also avoid the consumption of crystallized solvent and the pollution thereof to the environment, thus being a novel production technology with low material consumption and low pollution.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a production process of β-hydroxyalkylamides, in particular to a production process of β-hydroxyalkylamides that can be used as curing agents for powder coatings. Background technique [0002] β-hydroxyalkylamide is a kind of substance with 2-4 functionality β-hydroxyl, its highly reactive β-hydroxyl can cross-link with the carboxyl group in the resin molecule, so it can be used as a curing agent for carboxyl functional group resin Agents are used in coatings, especially in the field of powder coatings. As a new type of powder coating curing agent, β-hydroxyalkylamide can not only provide excellent weather resistance, heat resistance, corrosion resistance and other application properties, but also has the advantages of non-toxic, non-irritating and low-temperature curing, so it is highly regarded Researchers in the field of powder coatings are concerned. [0003] At present, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/18C09D5/03
Inventor 鲍远志翁世兵
Owner 六安捷通达新材料有限公司
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