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Production method of pesticide intermediate 1,2,3,6-tetrahydrophthalimide

A technology of tetrahydrophthalimide and tetrahydrophthalic anhydride, which is applied in the field of organic chemical synthesis and achieves the effects of good development prospects, great potential safety hazards, and mild and easy-to-control reaction conditions

Inactive Publication Date: 2018-09-04
濮阳惠成新材料产业技术研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After centrifugation, the solid was directly dried in a microwave dryer

Method used

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  • Production method of pesticide intermediate 1,2,3,6-tetrahydrophthalimide

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Add 235Kg of ammonia water with a mass fraction of 20% in a 500L reactor, and cool the jacket to 20% with cooling water. o C, 299Kg of 1,2,3,6-tetrahydrophthalic anhydride was dropped in batches under stirring, and the temperature of the control material was not more than 60 o c. After the feeding is completed, close the feeding port, release the jacket cooling water and slowly inject steam to start heating until the material temperature is 100 o At about C, water is evaporated, and after condensation, it enters the buffer tank and reacts while steaming water. As the amount of steamed water approaches the theoretical value, the temperature of the material gradually rises to 145 o C, keep the reaction temperature and continue the reaction until the central control sampling detects that the raw material 1,2,3,6-tetrahydrophthalic anhydride is 98.5%, stop heating, cool down to material temperature 70 o At about C, inject distilled water with nitrogen pressure from the fe...

Embodiment 2

[0017] Add 1417Kg of ammonia water with a mass fraction of 19.5% in a 3000L reactor, and cool the jacket to 20 with cooling water. o C, 1650Kg of 1,2,3,6-tetrahydrophthalic anhydride was dropped in batches under stirring, and the temperature of the control material was not more than 60 o c. After the feeding is completed, close the feeding port, release the jacket cooling water and slowly inject steam to start heating, and heat to the material temperature of 105 o At about C, water is evaporated, and after condensation, it enters the buffer tank and reacts while steaming water. As the amount of steamed water approaches the theoretical value, the temperature of the material gradually rises to 145 o C, keep the reaction temperature and continue the reaction until the central control sampling detects that the raw material 1,2,3,6-tetrahydrophthalic anhydride is 98.5%, stop heating, cool down to material temperature 70 o At about C, inject distilled water with nitrogen pressure ...

Embodiment 3

[0020] Add 2107Kg of ammonia water with a mass fraction of 20% in a 5000L reactor, and cool the jacket to 20% with cooling water. o C, put 2500Kg of 1,2,3,6-tetrahydrophthalic anhydride in batches under stirring, and control the material temperature not to exceed 60 o c. After the feeding is completed, close the feeding port, release the jacket cooling water and slowly inject steam to start heating until the material temperature is 110 o At about C, water is evaporated, and after condensation, it enters the buffer tank and reacts while steaming water. As the amount of steamed water approaches the theoretical value, the temperature of the material gradually rises to 145 o C, keep the reaction temperature and continue the reaction until the central control sampling detects that the raw material 1,2,3,6-tetrahydrophthalic anhydride is 98.5%, stop heating, cool down to material temperature 70 o At about C, inject distilled water with nitrogen pressure from the feed port, and the...

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Abstract

The invention discloses a production method of 1,2,3,6-tetrahydrophthalimide, and belongs to the field of organic chemical synthesis. According to the method, 1,2,3,6-tetrahydrophthalic anhydride andammonia water are used as raw materials, excess water is distilled out while reacting at a certain raw material ratio and reaction temperature, and after the reaction is finished, the reaction solution is recrystallized by using distilled water. A crude product obtained by recrystallization is then centrifuged and dried to obtain a finished product of 1,2,3,6-tetrahydrophthalimide. The method hasthe advantages of mild reaction condition, easy control, high raw material conversion rate, and high product yield reaching 86% or more. The obtained product is a white needle crystal with high purityreaching 99.5% or more. The production method avoids the defects of large potential safety hazard and more waste gas generated in the traditional process, is more green and environment-friendly, hasa simple preparation process and a lower cost, is favorable for large-scale production, and has a good development prospect.

Description

technical field [0001] The invention relates to a production method of a pesticide intermediate 1,2,3,6-tetrahydrophthalimide, belonging to the field of organic chemical synthesis. Background technique [0002] 1,2,3,6-tetrahydrophthalimide, also known as tetrahydrophthalimide, cis-1,2,3,6-tetrahydrophenamine, the appearance is light yellow or white needles It is an intermediate of pesticides captafol and captan. Captan and Captan are broad-spectrum protective organosulfur fungicides, which mainly control scab, downy mildew, powdery mildew, gray mold, etc. on fruit trees, vegetables, flowers and other economic crops, and can also be used on soil Treatment, prevention and treatment of root diseases, low toxicity to humans and animals. 1,2,3,6-Tetrahydrophthalimide is an intermediate of captafol and captan, and the development of its production process is of great significance to the economic development of crops. [0003] At present, the main industrial production method o...

Claims

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Application Information

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IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 刘二畅赵尚董栋张国阳王晓莺
Owner 濮阳惠成新材料产业技术研究院有限公司
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