Preparation method of chloramine

A chlorinated amine and hydroxylamine salt technology, applied in the field of organic synthesis, can solve the problems of long reaction period, high temperature, increased risk factor, etc., and achieve the effects of low cost, improved yield and purity, and increased safety factor

Pending Publication Date: 2022-03-01
山东科加工业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has high conversion rate and yield, but the reaction cycle is long, the temperature is high, and the risk factor increases

Method used

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  • Preparation method of chloramine

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Embodiment 1

[0073] The preparation method of present embodiment chlorinated amine, comprises the following steps:

[0074] Hydroxylamine sulfate, acetate and 27% liquid caustic soda are entered in continuous flow reactor 1 with continuous feed pump respectively, and the feed rate of hydroxylamine salt is 15.92ml / min, and the feed rate of acetate is 7.7ml / min , the feed rate of liquid caustic soda is 7.8ml / min, the temperature of the integrated machine is controlled at 28°C, and the residence time is 164.05s to obtain the intermediate product A.

[0075] Intermediate product A is added 0.3% EDTA as catalyst to obtain mixture B, mixture B and 1,3-dichloropropene enter continuous flow reactor 2 at a certain flow rate, mixture B is 30ml / min, 1,3-dichloropropene The feed rate of the product was 5.88ml / min, the temperature of the integrated machine was controlled at 80°C, and the residence time was 164.05s to obtain the intermediate product C.

[0076] The intermediate product C and hydrochlor...

Embodiment 2

[0081] The preparation method of present embodiment chlorinated amine, comprises the following steps:

[0082] Hydroxylamine hydrochloride, acetate and 25% liquid caustic soda are entered in continuous flow reactor 1 respectively with continuous feed pump, and the feed rate of hydroxylamine salt is 15.92ml / min, and the feed rate of acetate is 7.7ml / min , the feed rate of liquid caustic soda is 7.8ml / min, the temperature of the integrated machine is controlled at 28°C, and the residence time is 164.05s to obtain the intermediate product A.

[0083] Intermediate product A is added 0.3% EDTA as catalyst, obtains mixture B, mixture B and 1,3-dichloropropene enter continuous flow reactor 2 at a certain flow rate, mixture B is 20ml / min, 1,3-dichloropropene The feed rate is 8.89ml / min, the temperature of the integrated machine is controlled at 80°C, and the residence time is 182.76s to obtain the intermediate product C.

[0084] The intermediate product C and hydrochloric acid are u...

Embodiment 3

[0089] The preparation method of present embodiment chlorinated amine, comprises the following steps:

[0090] Hydroxylamine sulfate, acetate and 30% liquid caustic soda are entered in continuous flow reactor 1 respectively with continuous feed pump, and the feed rate of hydroxylamine salt is 15.92ml / min, and the feed rate of acetate is 7.7ml / min , the feed rate of liquid caustic soda is 7.8ml / min, the temperature of the integrated machine is controlled at 28°C, and the residence time is 164.05s to obtain the intermediate product A.

[0091] Intermediate product A is added 0.3% EDTA as catalyst, obtains mixture B, mixture B and 1,3-dichloropropene enter continuous flow reactor 2 at a certain flow rate, mixture B is 20ml / min, 1,3-dichloropropene The feed rate was 8.89ml / min, the temperature of the integrated machine was controlled at 80°C, and the residence time was 182.76s to obtain the intermediate product C.

[0092] The intermediate product C and hydrochloric acid are used...

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Abstract

The invention belongs to the field of organic synthesis, and relates to a preparation method of chloramine, which comprises the following steps: reacting hydroxylamine salt, carboxylic acid ester and an acid-binding agent in a continuous flow reactor to obtain an intermediate product A; mixing the intermediate product A with a catalyst to obtain a mixture B, and reacting the mixture B with 1, 3-dichloropropene in a continuous flow reactor to obtain an intermediate product C; reacting the intermediate product C with hydrochloric acid in a continuous flow reactor to obtain an intermediate product D; uniformly mixing dichloromethane and the intermediate product D, and extracting to obtain an oil phase E and a water phase F; reacting the F with alkali in a continuous flow reactor to obtain an intermediate product H; uniformly mixing dichloromethane and the intermediate product H, and extracting to obtain an oil phase I and a water phase J; and I, performing continuous distillation by using a continuous distillation device, and continuously applying the recovered dichloromethane to obtain chloramine. The yield and the purity of the product are improved, the safety coefficient is increased, the cost is reduced, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method and equipment for preparing chlorinated amines through a microchannel reactor. Background technique [0002] Chloramines are important pesticides and pharmaceutical intermediates, and are widely used in cyclohexenone herbicides. This type of herbicide is an important class of ACCase inhibitors, mainly used in broadleaf crop fields to control grass weeds, and has special effects on most annual and perennial grass weeds. [0003] The existing process often uses ethyl acetate and hydroxylamine hydrochloride as raw materials, acetohydroxamic acid is obtained through acetamidation reaction, and then alkylated with 1,3-dichloropropene, and finally the alkylated product is hydrolyzed with hydrochloric acid to obtain chlorine Substituted amines. This method takes a long time, and the bottle experiment is very dangerous; the activity of trans-propylene is ...

Claims

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Application Information

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IPC IPC(8): C07C239/10
CPCC07C239/10
Inventor 褚国忠刘慧敏赵传孝任义仙郑欣欣张献张鸿飞
Owner 山东科加工业技术研究院有限公司
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