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Novel synthesis method of 2,4,6-tri(aminocaproate)-1,3,5-triazine

A synthesis method, the technology of aminocaproic acid, applied in the field of synthesis of 2,4,6-tri-1,3,5-triazine, to achieve the effects of less product loss, lessen the environmental protection pressure of enterprises, and high yield

Inactive Publication Date: 2018-08-03
DAFENG YUELONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of this invention is to provide a kind of new 2,4,6-three (amino caproic acid base)-1,3,5-triazine that solves from the source the problem of producing a large amount of high ammonia nitrogen and high COD wastewater problems resolve resolution

Method used

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  • Novel synthesis method of 2,4,6-tri(aminocaproate)-1,3,5-triazine
  • Novel synthesis method of 2,4,6-tri(aminocaproate)-1,3,5-triazine

Examples

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Effect test

example 1

[0023] Add 339g caprolactam, 450g cesium hydroxide and 1500g solvent xylene into the bottle. 54g of water was added dropwise with stirring, the reaction exothermed, and the temperature was controlled not to exceed 90°C. The reaction was kept at 80-90°C for 3 hours, and gas chromatography (GC) analysis showed that the caprolactam conversion rate was greater than 99.5%, and the reaction was completed. The temperature was lowered to 40°C, 126g of melamine was added, and the mixture was stirred and heated. When the temperature rises to 90-100°C, gaseous ammonia is released, absorbed by water, and the gas release is not obvious, continue to heat up to 110-120°C, gaseous ammonia is released, absorbed by water, and the gas release is not obvious, continue to heat up to At 135-145°C, gaseous ammonia is released, absorbed by water, and kept at 135-145°C to react until the raw material melamine and intermediates disappeared by high performance liquid chromatography (HPLC) analysis, the ...

example 2

[0026] Add 339g caprolactam, 224g potassium hydroxide and 1000g solvent dichlorobenzene into the bottle. 54g of water was added dropwise with stirring, the reaction exothermed, and the temperature was controlled not to exceed 90°C. The reaction was kept at 80-90°C for 3 hours. GC analysis showed that the conversion rate of caprolactam was greater than 99.5%, and the reaction was completed. The temperature was lowered to 40°C, 126g of melamine was added, and the mixture was stirred and heated. When the temperature rises to 90-100°C, gaseous ammonia is released, absorbed by water, and the gas release is not obvious, continue to heat up to 110-120°C, gaseous ammonia is released, absorbed by water, and the gas release is not obvious, continue to heat up to At 135-145°C, gaseous ammonia is released, absorbed by water, and reacted at 135-145°C at 135-145°C until the raw material melamine and intermediates disappeared as analyzed by HPLC, the reaction ends. Cool down to below 40°C, ...

example 3

[0028] Add 339 g caprolactam, 200 g sodium hydroxide and 800 g solvent xylene into the bottle. 54g of water was added dropwise with stirring, the reaction exothermed, and the temperature was controlled not to exceed 90°C. The reaction was kept at 80-90°C for 3 hours. GC analysis showed that the conversion rate of caprolactam was greater than 99.5%, and the reaction was completed. The temperature was lowered to 40°C, 126g of melamine was added, and the mixture was stirred and heated. When the temperature rises to 90-100°C, gaseous ammonia is released, absorbed by water, and the gas release is not obvious, continue to heat up to 110-120°C, gaseous ammonia is released, absorbed by water, and the gas release is not obvious, continue to heat up to At 135-145°C, gaseous ammonia is released, absorbed by water, and reacted at 135-145°C at 135-145°C until the raw material melamine and intermediates disappeared as analyzed by HPLC, the reaction ends. Cool down to below 40°C, stir slowl...

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Abstract

The invention provides a novel synthesis method of 2,4,6-tri(aminocaproate)-1,3,5-triazine. The novel synthesis method comprises the following steps: taking caprolactam, alkali and water to react, soas to generate a first intermediate; taking the first intermediate and melamine to react to generate a second intermediate; adding sulfuric acid and the second intermediate and stirring materials to obtain particles with a certain size; under the protection of nitrogen gas, centrifuging the materials. The invention provides a novel synthesis route; an organic solvent is used as a reaction system and the water quantity is greatly reduced; a product has certain solubility in water, so that compared with a water system of an existing technology, the loss of the product is less and the yield is higher.

Description

Technical field [0001] The invention belongs to a synthetic method, and more specifically relates to a new synthetic method of 2,4,6-tris(aminohexanoic acid)-1,3,5-triazine. Background technique [0002] The first step of the prior art process is to mix the caprolactam with water and liquid caustic soda, and then heat up the reaction to generate a 6-aminocaproate sodium salt solution; the second step is to react the 6-aminocaproate sodium salt solution with cyanuric chloride , Generate 2,4,6-tris(aminohexanoic acid)-1,3,5-triazine trisodium salt solution; the third step is 2,4,6-tris(aminohexanoic acid)-1,3, Acidification of 5-triazine trisodium salt solution to produce 2,4,6-tris(aminohexanoic acid)-1,3,5-triazine. As a rust remover and cutting fluid, the product has very high requirements on the chloride ion content, and the product in the prior art has a relatively high chloride ion content and is difficult to control. The prior art uses a large amount of distilled water to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/70
CPCC07D251/70
Inventor 江以桦何福春李逸超李艳军杨一飞范鹏
Owner DAFENG YUELONG CHEM
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