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Preparation method of azodiisobutyronitrile

A technology for dichlorination of azobisisobutyronitrile and acetone cyanamide, which is applied in the field of preparation of azobisisobutyronitrile, can solve the problems that the reaction end point is not easy to control, the by-products are not easily separated, and the production cost is high, and the production process is achieved. Green environmental protection, easy control of the reaction end point, and reduced production costs

Inactive Publication Date: 2013-10-02
ZIBO HUIGANGCHUAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of the above two production methods: expensive and dangerous hydrazine hydrate must be used, and it must be carried out in two steps (determined by different reaction mother liquors), the reaction process of the chlorine flow method is unstable, and the reaction end point is not easy to control. The method should be stable, but it cannot solve the problem of the accumulation of waste acid in the reaction mother liquor and the final discharge
[0003] Using the hydrazine hydrate chlorine method, it is easy to produce more by-products, and the by-products are not easy to separate from the product. Later, the hydrogen peroxide method is also to avoid this, but the hydrogen peroxide method must also use hydrazine hydrate, the production cost is high, and all The acidic system is used as a solvent, and the amount of acidic water and wastewater is large, which is contrary to the purpose of today's green and environmentally friendly production

Method used

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  • Preparation method of azodiisobutyronitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of acetone cyanamide dichloride: Add 260 grams of pure water and 85 grams of 99% acetone cyanamide in a 1000ml three-neck flask, pass chlorine gas under stirring, observe the situation of chlorine gas bubbles being absorbed, judge the end point of the reaction, pass 0.5 hours After completion, the reaction temperature is controlled at 15°C during the process of chlorine flow. The final amount of chlorine flow is obtained by weighing the weight of the material in the three-necked flask, and the controlled amount of chlorine flow is 149±7 grams. Add 260 grams of pure water and 85 grams of acetone cyanamide), add 30% liquid caustic soda dropwise, control the dropping temperature at 15°C during the dropping process, and finish dropping in 0.5 hours. Use a pH meter to track and detect to ensure that the pH value is 7.

[0026] The preparation of azobisisobutyronitrile: in the above-mentioned three-necked flask, dropwise add 80 grams of acetone cyanamide and 30% li...

Embodiment 2

[0029] Preparation of acetone cyanamide dichloride: Add 255 grams of pure water and 85 grams of 99% acetone cyanamide in a 1000ml three-neck flask, pass chlorine gas under stirring, observe the situation of chlorine gas bubbles being absorbed, judge the end point of the reaction, pass 1 hour After completion, the reaction temperature is controlled at 30°C during the chlorine flow process. The final chlorine flow rate is obtained by weighing the material weight in the three-necked flask. The controlled chlorine flow rate is 160±3 grams. Add 255 grams of water and 85 grams of acetone cyanamide), add dropwise 30% liquid caustic soda, control the dropwise addition temperature at 25°C during the dropwise addition, and finish dropping in 1 hour. Use a pH meter to track and detect to ensure that the pH value is 8.

[0030] Preparation of azobisisobutyronitrile: Add 80 grams of acetone cyanamide and 30% liquid caustic dropwise to the above-mentioned three-necked bottle at the same time...

Embodiment 3

[0033] Preparation of acetone cyanamide dichloride: add 340 grams of pure water and 85 grams of 99% acetone cyanamide to a 1000ml three-neck flask, pass chlorine gas under stirring, observe the situation of chlorine gas bubbles being absorbed, judge the reaction end point, pass through in 0.8 hours, During the process of chlorine flow, the reaction temperature is controlled at 20°C. The final amount of chlorine flow is obtained by weighing the weight of the material in the three-necked flask. The controlled amount of chlorine flow is 167±3 grams. gram of water and 85 grams of acetone cyanamide) was added dropwise with 30% liquid caustic soda, the dropping temperature was controlled at 20°C during the dropping process, the dropping was completed in 0.9 hours, and the pH meter was used to track and detect to ensure that the pH value was 7.5.

[0034] The preparation of azobisisobutyronitrile: in the above-mentioned three-necked flask, dropwise add 80 grams of acetone cyanamide an...

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a preparation method of azodiisobutyronitrile. The method comprises the steps of chloro reaction and condensation reaction, wherein the chloro reaction is that acetone cyanamide, chlorine and a solvent react to form an acetone cyanamide dichlorinated product; and the condensation reaction is that the acetone cyanamide dichlorinated product and acetone cyanamide react to form azodiisobutyronitrile. The method avoids the conventional expensive and dangerous hydrazine hydrate synthesis technology, and the reaction end point is very easy to control, so that the production cost is lowered greatly; and waste water is brine waste, and can serve as a chlorine solvent after salt is separated out, so that no waste water is achieved basically, a production technology is green and environment-friendly, and the operation is simple.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of azobisisobutyronitrile. Background technique [0002] At present, the production method of azobisisobutyronitrile mainly adopts acetone cyanohydrin plus hydrazine hydrate to obtain diisobutyronitrile hydrazine, and then uses diisobutyronitrile hydrazine to prepare azobisisobutyronitrile through chlorine or hydrogen peroxide oxidation. The disadvantages of the above two production methods: expensive and dangerous hydrazine hydrate must be used, and it must be carried out in two steps (determined by different reaction mother liquors), the reaction process of the chlorine flow method is unstable, and the reaction end point is not easy to control. The method should be stable, but it cannot solve the problem of the accumulation of waste acid in the reaction mother liquor and the final discharge. [0003] Using the hydrazine hydrate chlorine method,...

Claims

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Application Information

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IPC IPC(8): C07C255/65C07C253/30
Inventor 张杰
Owner ZIBO HUIGANGCHUAN CHEM TECH
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