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Preparation method of azodiisobutyronitrile

A technology for the reaction of azobisisobutyronitrile, which is applied in the field of preparation of organic compound azobisisobutyronitrile, can solve the problems of low yield and no condensation waste water.

Active Publication Date: 2006-06-14
SHANGHAI NO 4 REAGENT & H V CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Because the waste acid of condensation waste water and oxidation reaction has been applied mechanically, the discharge of waste water has been reduced, but the optimal value of adjusting the pH value of condensation waste water has not been pointed out in this report, so the total yield of the reaction can only reach 68-72%. Between, the yield is not high

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  • Preparation method of azodiisobutyronitrile
  • Preparation method of azodiisobutyronitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0020] The preparation of embodiment 1 azobisisobutyronitrile

[0021] Preparation of diisobutyronitrile hydrazine: add 100g (1.153mol) of 98% acetone cyanohydrin and 150g (8.3mol) of condensation waste water in a 500ml three-necked flask, and control the pH value of condensation waste water at 4.8. Carry out condensation reaction, control reaction temperature between 51~60 ℃, reaction time is 3 hours. Then the feed solution was cooled to 10°C, crystallized, and filtered to obtain diisobutyronitrile hydrazine.

[0022] respectively in 1 # ,2 # Add the obtained diisobutyronitrile hydrazine into a 1000ml three-neck flask to dilute with water, the amount of water added is 400ml, and the mixed solution is cooled to 10°C, and then oxidized by passing chlorine gas. 1 # The residual chlorine produced during the chlorine oxidation process in the bottle is within 2 # Absorb in the bottle, control the chlorine flow rate during the chlorine flow process to 0.025-0.030mol / min, 2 # T...

Embodiment 2

[0027] Embodiment 2 Preparation of azobisisobutyronitrile

[0028] Preparation of diisobutyronitrile hydrazine: add 200g (2.306mol) of 98% acetone cyanohydrin and 380g (21.1mol) of condensation waste water in a 1000ml three-necked flask, and control the pH value of condensation waste water at 4.4. For the condensation reaction, the reaction temperature is controlled to be stable between 51°C and 60°C, and the reaction time is 3.5 hours. Then the reaction solution was cooled to 10°C, crystallized, and filtered to obtain diisobutyronitrile hydrazine.

[0029] respectively in 1 # ,2 # Add the obtained diisobutyronitrile hydrazine into a 2000ml three-neck flask to dilute with water, the amount of water added is 850ml, and the mixed solution is cooled to 8°C, and then oxidized by passing chlorine gas. 1 # The residual chlorine generated during the chlorine oxidation process in the bottle is within 2 # Absorb in the bottle, control the speed of chlorine flow at 0.021 ~ 0.025mol...

Embodiment 3

[0031] Embodiment 3 control experiment

[0032] 100g (1.153mol) of 98% acetone cyanohydrin and 270g (15mol) of condensation wastewater controlled at a pH of 6.5 were added into a 500ml three-necked flask to react with 36.5g (0.584mol) of 80% hydrazine hydrate. The condensation reaction temperature is controlled to be between 50-60° C., and the reaction time is controlled to be 3.5 hours. Then the feed solution was cooled to 10°C, crystallized, and filtered to obtain diisobutyronitrile hydrazine. The obtained diisobutyronitrile hydrazine was diluted with water, the amount of water added was 400ml, and the mixture was cooled to 10°C. Then carry out the oxidation reaction in a single oxidation device with chlorine gas, and use 10% sodium hypobromite solution titration to control the oxidation reaction end point according to the routine operation. It is the end point that no white precipitate occurs in the titration, and consumes 40g of chlorine gas to obtain azobisisobutyl The ...

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Abstract

The present invention relates to method for preparing azobisisobutyronitrile. It is an improvement on two-step reaction process including the procedures of utilizing acetone cyanohydrin and hydrazine hydrate to form diisobutyronitrile, using mixed waste water in the reaction and introducing chlorine gas to make oxidation and form azobisisobutyronitrile. Said improvement includes the following several contents: controlling pH value of condensed water used in first-step reaction and making said pH value be 4-5; in second-step reaction adopting two sets of oxidation devices to alternatively make chlorine gas introduction reaction and negative pressure absorption of released residual chlorine gas and its circular comprehensive utilization; and using 10% hypobromite solution to control end point of oxidation reaction. Said method can raise total yield to above 82%, and the utilization rate of chlorine gas can be raised to about 81-86%.

Description

technical field [0001] The present invention relates to the preparation method of organic compound azobisisobutyronitrile. Background technique [0002] Azobisisobutyronitrile belongs to the chemical products of organic initiators. It is widely used in initiators and foaming agents. It can be used as polyvinyl chloride, polyvinyl acetate, polyacrylonitrile, polystyrene, polysiloxane, etc. Initiator of high molecular polymer and organic free radical reaction, also can be used as foaming agent of plastic, rubber, etc. [0003] For the preparation method of azobisisobutyronitrile, there are many studies at home and abroad, mainly the following preparation methods of azobisisobutyronitrile. [0004] In "Fine Organic Chemical Raw Materials and Intermediates" published by Chemical Industry Press in June 1998, there is: the acetone azine method uses acetone as a raw material. The first step reaction is the reaction of acetone and hydrazine hydrate to generate acetonazine, the sec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C245/04
Inventor 顾云飞沈忠华杜维杰孙兆琪
Owner SHANGHAI NO 4 REAGENT & H V CHEM
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