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Method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine

A technology of dimethoxyl and methoxylization, which is applied in the direction of organic chemistry, can solve the problems of large loss of organic solvents and complicated process, and achieve the effect of reducing production costs

Inactive Publication Date: 2016-11-23
ANHUI SHINDO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine in the preparation process with complex process flow, numerous operation steps and large organic solvent loss. - Chloro-4, the method of 6-dimethoxy-1,3,5-triazine, this method drops into methanol in the reactor, sodium bicarbonate, slowly drops into cyanuric chloride in batches, then heats up to Reflux methanol, recover most of the methanol by distillation, put the distillation residue into the water analysis kettle for crystallization, suction filtration, add water to the solid phase for washing, suction filtration, and dry to obtain the crude product, add heptane to the crude product for recrystallization, filter, and dry the solid phase to obtain the finished product 2-Chloro-4,6-dimethoxy-1,3,5-triazine

Method used

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  • Method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine
  • Method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine

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Embodiment 1

[0021] A method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine, comprising the following steps:

[0022] 1) Methoxylation reaction: 900 kg of methanol and 240 kg of sodium bicarbonate were put into the reactor, and 260 kg of cyanuric chloride was slowly added in batches under stirring, and then the temperature was raised to reflux of methanol in stages, and the reaction was carried out for 5 hours;

[0023] 2) Distillation: After the methoxylation reaction, most of the methanol is distilled to recover 750kg; the methanol distillation recovery is carried out in the reactor, and the distillation is condensed by water cooling and freezing brine;

[0024] 3) Dilute crystallization: 516kg of distillation residue is put into the water analysis kettle, and 1010kg of crystallization is diluted with water;

[0025] 4) Suction filtration / washing, drying: adding water to the crystalline solid phase, washing with suction, and drying to obtain 240 kg of crude product;

[0026] 5) Rec...

Embodiment 2

[0029] A method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine, comprising the following steps:

[0030] 1) Methoxylation reaction: 900 kg of methanol and 180 kg of sodium bicarbonate were put into the reaction kettle, and 225 kg of cyanuric chloride was slowly added in batches under stirring, and then the temperature was raised to methanol reflux in stages, and the reaction was carried out for 4 hours;

[0031] 2) Distillation: After the methoxylation reaction, most of the methanol is distilled to recover 770kg; the methanol distillation recovery is carried out in the reactor, and the distillation is condensed by water cooling and freezing brine;

[0032] 3) Dilute crystallization: Distill 480kg of residue into the water analysis kettle and add water to dilute crystallization 1010kg;

[0033] 4) Suction filtration / washing, drying: add water to the crystalline solid phase, wash with suction, and dry to obtain 215 kg of crude product;

[0034] 5) Recrystallization, filtra...

Embodiment 3

[0037] A method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine, comprising the following steps:

[0038] 1) Methoxylation reaction: 900 kg of methanol and 270 kg of sodium bicarbonate were put into the reactor, and 315 kg of cyanuric chloride was slowly added in batches under stirring, and then the temperature was raised to reflux of methanol in stages, and the reaction was carried out for 6 hours;

[0039] 2) Distillation: After the methoxylation reaction, most of the methanol is distilled to recover 730kg; the methanol distillation recovery is carried out in the reactor, and the distillation is condensed by water cooling and freezing brine;

[0040] 3) Dilute crystallization: 545kg of distillation residue is put into the water analysis kettle and dilutes 1150kg of crystallization with water;

[0041] 4) Suction filtration / washing, drying: add water to the crystalline solid phase, wash with suction, and dry to obtain 275 kg of crude product;

[0042] 5) Recrystallizatio...

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Abstract

The invention discloses a method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine. The method includes the steps of methoxylation, distillation, dilution and crystallization, suction filtration / washing, drying, recrystallization, filtering and drying. According to the method for preparing 2-chloro-4,6-dimethoxy-1,3,5-triazine, methyl alcohol and sodium bicarbonate are put in a reaction kettle, cyanuric chloride is slowly put in batches, then heating is carried out in a phased mode till methyl alcohol flows back, most of methyl alcohol is recovered in a distillation mode, distillation residues are put in an elutriation kettle to be subjected to crystallization and suction filtration, water is added into solid phases for washing, suction filtration and drying are carried out, and a crude product is obtained; heptanes is added into the crude product for recrystallization, filtering and solid-phase drying are carried out, and the finished product is obtained. According to the process, a methyl alcohol solvent is stored in a middle vessel after being recovered, and only a small amount of disorderly waste gas is exhausted; the methyl alcohol solvent is recovered in the reaction kettle and can be reused, and the production cost is reduced for enterprises.

Description

technical field [0001] The invention relates to the technical field of production and processing of 2-chloro-4,6-dimethoxy-1,3,5-triazine, in particular to a method for preparing 2-chloro-4,6-dimethoxy-1, 3,5-triazine method. Background technique [0002] Cyanuric chloride is also called cyanuric chloride, 2,4,6-trichloro-1,3,5-triazine, commonly known as cyanuric chloride. Cyanuric chloride has a special structure, has a lively step-by-step reaction performance, and can be connected with different groups respectively. It is one of the few heterocyclic compounds with an annual output of more than 100 thousand tons in the world. About two-thirds of cyanuric chloride is used in the manufacture of pesticides and herbicides, one-third is used in the manufacture of dyes and fluorescent whitening agents, and a small amount is used in the manufacture of rubber accelerators, medicines, anti-ultraviolet agents, polymers and textile assistants. agent etc. In medicine, 2-chloro-4,6-...

Claims

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Application Information

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IPC IPC(8): C07D251/26
CPCC07D251/26
Inventor 郑华忠
Owner ANHUI SHINDO CHEM
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