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Method for preparing atrazine

A technology of atrazine and cyanuric chloride, which is applied in the field of herbicides, can solve problems such as the dissolution and hydrolysis of cyanuric chloride, low product yield and purity, reduced content and yield, etc. Uniformity, quality and yield improvement, smooth and stable reaction

Active Publication Date: 2015-04-01
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, water production is difficult to solve the problem of dissolving and hydrolyzing cyanuric chloride in water, resulting in low product yield and purity
Therefore, the solvent method using toluene or acetone as a solvent is mostly used in domestic and foreign production, but when toluene or acetone is used as a solvent, the solubility of atrazine is small during synthesis, and atrazine forms a suspension in toluene during synthesis, which is not conducive to mass transfer. The process makes the reaction uneven and reduces the content and yield

Method used

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  • Method for preparing atrazine

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Embodiment 1

[0030] The method for synthesizing atrazine of the present invention, the steps are as follows: (1) 4473L methyl ethyl ketone is added in the reactor, feeds frozen brine in the jacket, cools down to 10 ℃, adds 600Kg cyanuric chloride, continues to stir and cool down; (2) When the temperature reaches 1°C, add 275Kg of 70% isopropylamine to the reaction kettle, the dropwise addition time is 70 minutes, the dropping temperature is controlled at 1-11°C, after the dropwise addition is completed, the temperature is controlled at 11-15°C and the stirring is continued for 10 minutes (3) Add dropwise 468Kg32% sodium hydroxide solution to the reaction kettle, control the temperature at 20-25°C, and add the time for 50 minutes, control the temperature at 20-25°C and continue to stir for 30 minutes after the dropwise addition Leave the upper organic phase; (4) dropwise add 216Kg68% monoethylamine to the reaction kettle, control the temperature at 20-30°C, and add the time for 62 minutes. A...

Embodiment 2

[0032] The method for synthesizing atrazine of the present invention, the steps are as follows: (1) 3727L methyl ethyl ketone is added in the reactor, feeds frozen brine in the jacket, cools down to 9 ℃, adds 600Kg cyanuric chloride, continues to stir and cool down; (2) When the temperature reaches 0°C, add 296Kg65% isopropylamine to the reaction kettle, the dropwise addition time is 80 minutes, the dropping temperature is controlled at 0-15°C, after the dropwise addition is completed, the temperature is controlled at 15-25°C and continued to stir for 10 minutes (3) Add 483Kg31% sodium hydroxide solution dropwise to the reaction kettle, control the temperature at 6-18°C, and add the time for 56 minutes. After the dropwise addition, control the temperature at 18-22°C and continue stirring for 30 minutes before separating Leave the upper organic phase; (4) dropwise add 210Kg70% monoethylamine to the reactor, control the temperature at 20-30°C, and add the time for 68 minutes. Aft...

Embodiment 3

[0034] The method for synthesizing atrazine of the present invention, the steps are as follows: (1) 2982L methyl ethyl ketone is added in the reactor, feeds frozen brine in the jacket, cools down to 4 ℃, adds 600Kg cyanuric chloride, continues to stir and cool down; (2) When the temperature reaches 3°C, add 283Kg68% isopropylamine to the reaction kettle, the dropwise addition time is 120 minutes, the dropping temperature is controlled at 3-10°C, after the dropwise addition is completed, the temperature is controlled at 10-15°C and the stirring is continued for 10 minutes (3) Add dropwise 499Kg30% sodium hydroxide solution to the reaction kettle, control the temperature at 15-20°C, and add the time for 60 minutes. After the dropwise addition, control the temperature at 20-25°C and continue stirring for 30 minutes before separating Leave the upper organic phase; (4) dropwise add 210Kg70% monoethylamine to the reactor, control the temperature at 30-40°C, and add the time for 70 mi...

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Abstract

The invention discloses a method for preparing atrazine. In the method, cyanuric chloride, iso-propylamine and mono ethyl amine are used as raw materials, and an organic solvent is used for synthesizing atrazine. The method is characterized in that methyl ethyl ketone is used as an organic solvent. According to the invention, the organic solvent is changed to be methyl ethyl ketone, so that the raw materials are homogeneous; the reaction is slow and steady; the resultant atrazine can be completely dissolved in the solvent; aftertreatment is simple; and the content and the yield of atrazine are effectively improved.

Description

technical field [0001] The invention relates to a method for preparing atrazine, in particular to a method for synthesizing atrazine by using methyl ethyl ketone as a solvent, and belongs to the technical field of herbicides. Background technique [0002] The chemical name of atrazine is 2-chloro-4-ethylamino-6-isopropylamino-1,3,5-triazine, also known as atrazine, and its physical and chemical properties are: white crystalline powder with a melting point of 173- The solubility in water is 33mg / L at 175°C and 25°C. It is easily soluble in organic solvents, such as 1.8% in methanol and 5.2% in chloroform. It is relatively stable in weak acids and weak bases. Alkali and inorganic acids can be used at higher temperatures. It is hydrolyzed into herbicidally active hydroxyl derivatives. Atrazine is a special herbicide for corn, sugarcane, sorghum, etc. It can control annual grass weeds, especially for broad-leaved weeds. It can be compounded with a variety of amide herbicides to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/50
Inventor 孙国庆侯永生迟志龙李志清沈婕刘元强刘强袁良国孙国冉陈琦宋吉奎
Owner SHANDONG WEIFANG RAINBOW CHEM
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