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Preparation method of n,n,n-tris(n'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine

A propionate amide and hydroxyethyl technology, applied in the direction of organic chemistry, to achieve the effects of less environmental pollution, high product yield, and low cost

Active Publication Date: 2022-03-18
JIANGSU XINLU CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are few reports on the synthesis of N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine. Therefore, research and development of a N, The preparation method of N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine has very important industrial application value

Method used

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  • Preparation method of n,n,n-tris(n'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine
  • Preparation method of n,n,n-tris(n'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine

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Embodiment 1

[0015] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 30 g of methanol and 38.71 g of N,N,N-tris(3'-propionic acid methyl)-1,3,5 - Triazine, 18.3g monoethanolamine, 0.5g potassium p-toluenesulfonate, start the stirrer, when the temperature rises to 45-65°C, start timing, and the reaction time is 10h. After the reaction, cool down to 3-5°C for crystallization, filter and dry to obtain white powdery solid N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3 , 5-triazine product, the melting point is 99-102°C, and the yield of the product reaches 96.04%.

Embodiment 2

[0017] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser, and a thermometer, 70 g of isopropanol and 38.71 g of N,N,N-tris(3'-propionic acid methyl)-1,3 , 5-triazine, 24.4g monoethanolamine, 1.5g potassium p-dodecylbenzenesulfonate, start the stirrer, when the temperature rises to 45-65°C, start timing, and the reaction time is 9h. After the reaction, cool down to 3-5°C for crystallization, filter and dry to obtain white powdery solid N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3 , 5-triazine product, the melting point is 99-102°C, and the yield of the product reaches 96.34%.

Embodiment 3

[0019] In a four-necked reaction flask equipped with an electric stirrer, a reflux condenser and a thermometer, add 50 g of ethanol and 38.71 g of N,N,N-tris(3'-propionic acid methyl)-1,3,5 - Triazine, 20.2g monoethanolamine, 1.5g potassium p-toluenesulfonate, start the stirrer, when the temperature rises to 45-65°C, start timing, and the reaction time is 8.5h. After the reaction, cool down to 3-5°C for crystallization, filter and dry to obtain white powdery solid N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3 , 5-triazine product, the melting point is 99-102°C, and the yield of the product reaches 97.88%.

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Abstract

The invention provides a method for preparing a curing agent intermediate N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine, which uses N,N ,N‑tris(3'‑methyl propionate)‑1,3,5‑triazine and monoethanolamine are used as raw materials, and the curing agent intermediate N,N,N‑ Tris(N'-hydroxyethyl-3'-propionamido)-1,3,5-triazine. The present invention synthesizes curing agent intermediate N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine, the separation and purification process is simple, the reaction time is short, and the product The yield can reach more than 96%, the product has high purity, less energy consumption, less environmental pollution and low cost, and is an ideal process for realizing industrialized production.

Description

technical field [0001] The invention relates to the technical field of chemical raw materials, in particular to a preparation method of N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine. Background technique [0002] N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine is an important fine chemical raw material and organic synthesis intermediate. It can be used alone as a curing agent for powder coatings, and it can be used in conjunction with N,N,N',N'-tetra(β-hydroxyethyl)adipamide curing agent to improve the yellowing of the coating. Polarity change, even mixing with carboxy polyester powder coatings, avoiding paint foaming. The chemical name is N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine, and its molecular formula is: C 18 h 30 N 6 o 9 , molecular weight: 474.19, molecular structure formula: [0003] [0004] N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine is a white powdery solid with a me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/30
CPCC07D251/30
Inventor 丁继叶郑建王树清
Owner JIANGSU XINLU CHEM NEW MATERIAL
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