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Method for synthesizing ketazine by hydrogen peroxide oxidation method

A hydrogen peroxide, ketazine technology, applied in the directions of organic chemistry, hydrazone preparation, etc., can solve the problems of high energy consumption, large emission, low product yield, etc., achieve high product yield, reduce side reactions, and yield reduced effect

Inactive Publication Date: 2010-12-22
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method avoids the circulation of a large amount of ammonia, but due to the oxidative decomposition of hydrazine, the product yield is low (about 70% in terms of NaClO), the energy consumption is high, and the shortcomings such as a large amount of ammonia nitrogen compounds are discharged in the production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 72.4g of acetamide, 40.9g of ammonium acetate, 60mL of water, 73.2mL of methyl ethyl ketone, 30mL of cyclohexane, and 2 HPO 4 0.25g, EDTA 0.19g, stir to dissolve and start to heat, pass ammonia gas at the same time, change to slowly pass in after reaching saturation, slowly add 25mL of 47.5% hydrogen peroxide dropwise when the temperature rises to 45°C, drop it in 5 minutes, and control the temperature at Reaction at 54°C for 6h. After the reaction, cool down and discharge the material, let it stand for stratification, take the samples of the methyl ethyl ketazine layer and the working solution layer and weigh them for analysis. The yield of methyl ethyl ketazine is 94.3% and the selectivity of hydrogen peroxide is 98.9% through chemical analysis.

Embodiment 2

[0027] Into the reactor equipped with stirring, temperature display, ammonia gas introduction tube and reflux condenser, add acetamide 87g, ammonium acetate 49g, water 65mL, methyl ethyl ketone 80mL, cyclohexane 300mL, Na2 HPO 4 0.32g, EDTA 0.22, stir to dissolve and start heating, and pass through ammonia gas at the same time, and then slowly pass through after reaching saturation, slowly add 25mL of 49% hydrogen peroxide dropwise when the temperature rises to 46°C, drop it in 2 minutes, and control the temperature at 54°C ℃ reaction 3h. After the reaction was completed, the temperature was lowered and the material was discharged, and the layers were allowed to stand for stratification. The samples of the ketazine layer and the working liquid layer were weighed and analyzed respectively. The yield of methyl ethyl ketazine was 93.1% and the selectivity of hydrogen peroxide was 98.5% through chemical analysis.

Embodiment 3

[0029] The extractant was 20 mL of n-hexane and 20 mL of cyclohexane, and the rest of the experimental conditions and operating methods were the same as in Example 2. The obtained results showed that the yield of methyl ethyl ketazine was 95.3%, and the selectivity of hydrogen peroxide was 99.4%.

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PUM

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Abstract

The invention discloses a method for synthesizing ketazine by a hydrogen peroxide oxidation method. The ketazine is synthesized by using ketone and ammonia as raw materials, hydrogen peroxide as an oxidant and acetamide-ammonium acetate-Na2HPO4 as a catalyst. The method is characterized in that: an extracting agent is added into a reaction system, wherein the extracting agent is an organic solvent which is soluble in the ketazine and insoluble in water, such as alkane of cyclohexane, n-hexane, n-heptane and the like, and halogenated hydrocarbon of chloroform, 1,2-dichloroethane, 1,1,1-trichloro ethane, carbone tetrachloride and the like; and one or more of the alkane and the halogenated hydrocarbon can be added. The method has high yield of products and the extracting agent can be recycled.

Description

technical field [0001] The invention relates to a method for preparing ketazine, in particular to a process for synthesizing ketazine by oxidation with hydrogen peroxide, and belongs to the technical field of fine chemicals. Background technique [0002] Hydrazine hydrate is an important chemical raw material and a widely used chemical product. It can be obtained by hydrolyzing and refining ketazine. It is an important raw material for the production of foaming agents, pesticides, medicines, dyes, developers and reducing agents. Separation of pure metals, synthetic fibers and rare elements, deoxygenation of large boiler feed water, production of rocket fuel and explosives, etc. [0003] As we all know, there are mainly four methods for the industrial production of hydrazine hydrate, namely the Rasching method, the ketazine method of Bayer Company, the urea method and the hydrogen peroxide oxidation method of PCUK Company. Among them, the Raschig method uses sodium hypochlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/88C07C249/16
Inventor 娄风雷王琴马俊红张晓斌刘明郭晓冉
Owner LIMING RES INST OF CHEM IND
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