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Preparation method of curing agent intermediate N, N, N-tri(3'-methyl propionate)-1, 3, 5-triazine

A technology of methyl propionate and methyl acrylate, which is applied in the field of preparation of curing agent intermediate N,N,N-tri-1,3,5-triazine, which achieves low environmental pollution, simple separation and purification process, and high product quality The effect of high purity

Active Publication Date: 2021-05-14
JIANGSU XINLU CHEM NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] N,N,N-tris(3'-methylpropionate)-1,3,5-triazine is a white solid powder, currently, about N,N,N-tris(3'-methylpropionate) )-1,3,5-triazine synthesis is rarely reported, therefore, research and development of a N,N,N-tri(3'-propionate methyl)-1,3,5-triazine The preparation method has very important industrial application value

Method used

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  • Preparation method of curing agent intermediate N, N, N-tri(3'-methyl propionate)-1, 3, 5-triazine
  • Preparation method of curing agent intermediate N, N, N-tri(3'-methyl propionate)-1, 3, 5-triazine

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Experimental program
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Effect test

Embodiment 1

[0016] In a 500mL four-neck flask equipped with a thermometer and a condenser tube, add 30g of xylene, 12.9g of cyanuric acid, 25.9g of methyl acrylate, 0.4g of tetrabutylammonium bromide, and 0.2g of hydroquinone, and heat up When the temperature reaches 110-115°C, the reaction time is 10h (monitor the reaction with liquid chromatography). After the reaction, the temperature of the organic phase was lowered to 5-8°C, the crystallization was complete, and it was filtered to obtain the N,N,N-tris(3'-propionic acid methyl)-1,3,5-triazine product. The rate is 95.03%.

Embodiment 2

[0018] In a 500mL four-necked flask equipped with a thermometer and a condenser tube, add 30g of toluene, 12.9g of cyanuric acid, 34.4g of methyl acrylate, 5.0g of tetraisopropylammonium bromide, and 3.0g of hydroquinone, and heat up When the temperature reaches 110-115°C, the reaction time is 9h (monitor the reaction by liquid chromatography). After the reaction, the temperature of the organic phase was lowered to 5-8°C, the crystallization was complete, and it was filtered to obtain the N,N,N-tris(3'-propionic acid methyl)-1,3,5-triazine product. The rate is 97.62%.

Embodiment 3

[0020] In a 500mL four-necked flask equipped with a thermometer and a condenser, add 50g of toluene, 12.9g of cyanuric acid, 31.0g of methyl acrylate, 1.5g of tetrabutylammonium bromide, and 1.0g of hydroquinone, and heat up to At 110-115°C, the reaction time is 11h (monitor the reaction by liquid chromatography). After the reaction, the temperature of the organic phase was lowered to 5-8°C, the crystallization was complete, and it was filtered to obtain the N,N,N-tris(3'-propionic acid methyl)-1,3,5-triazine product. The rate is 97.07%.

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Abstract

The invention provides a preparation method of a curing agent intermediate N, N, N-tri(3'-methyl propionate)-1, 3, 5-triazine, cyanuric acid and methyl acrylate are used as raw materials, and the target product curing agent intermediate N, N, N-tri (3'-methyl propionate)-1, 3, 5-triazine is prepared by reaction in the presence of a catalyst, a polymerization inhibitor and a solvent. According to the method, cyanuric acid and methyl acrylate are adopted as raw materials to synthesize N, N, N-tri (3'-methyl propionate)-1, 3, 5-triazine, the separation and purification process is simple, the reaction time is short, the product yield can reach 95% or above, the product purity is high, the energy consumption is low, the environmental pollution is small, the cost is low, and the method is an ideal process for achieving industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical raw materials, in particular to a method for preparing a curing agent intermediate N,N,N-tris(3'-methyl propionate)-1,3,5-triazine. Background technique [0002] N,N,N-tris(3'-propionic acid methyl)-1,3,5-triazine is an important fine chemical raw material and organic synthesis intermediate. It is mainly used in the synthesis of curing agent N,N,N-tris(N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine and the synthesis of curing agent N,N,N-tris( N'-hydroxyethyl-3'-propionic acid amido)-1,3,5-triazine can be matched with N,N,N',N'-tetra(β-hydroxyethyl)adipamide curing agent Using it can improve the yellowing phenomenon of the paint. Due to the change of the polarity of the compound curing agent, it can be evenly mixed with the carboxyl polyester powder paint to avoid foaming of the paint. Its molecular formula is C 15 h 21 N 3 o 9 , molecular weight: 387.35, molecular structure formul...

Claims

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Application Information

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IPC IPC(8): C07D251/34
CPCC07D251/34
Inventor 王树清郑建丁继叶
Owner JIANGSU XINLU CHEM NEW MATERIAL
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