Method for synthesizing methyl ethyl ketazine through air oxidation method

A technology of butanone azine and air oxidation, which is applied in the directions of organic chemistry, hydrazone preparation, etc., can solve the problems of low benzophenone azine content, many side reactions and high reaction temperature, and achieves reduction of reaction temperature and energy consumption, The effect of improving yield and content and wide source of raw materials

Active Publication Date: 2015-10-07
杭州圣捷菲科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of the prior art are: benzophenone is a solid at normal temperature, has a high boiling point, and requires high energy consumption for hydrolysis and recovery of hydrazine; the reaction temperature is high (about 200 ° C), and the safety hazard is large. The generated benzophenone azine will be oxidized and decomposed by air in the reaction system, with many side reactions, low yield (70-80%), low content of benzophenone azine (50-60%), The actual production cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 288g of butanone, PdCl 2 / CuCl 2 Catalyst 6.2g, formamide 95g, sodium bromide 17g, water 160mL, after stirring and dissolving, feed ammonia gas to saturation (the liquid surface has gas overflow), then change to slow feed, heat up to 41°C, start to feed air , the volume of air per minute is 1500ml, the reaction temperature is controlled at 40~45°C, and the reaction time is 7h. After feeding air for 40min, the upper layer reaction solution was started to be sucked into the liquid-liquid separator, and the volume of the upper layer reaction solution pumped into the liquid-liquid separator per hour was 1100ml, and the reaction solution was in the liquid-liquid separator It is separated into an organic phase and an aqueous phase, the organic phase is sent to the butanone azine storage tank, and the aqueous phase is sent back to the reactor to continue to participate in the reaction. After the reaction, the organic phase and the aqueous phase were weighed and analyzed,...

Embodiment 2

[0020] Add 432g of methyl ethyl ketone, PdCl 2 / CuCl 2 Catalyst 17.5g, formamide 173g, sodium bromide 35g, water 240mL, after stirring and dissolving, feed ammonia gas to saturation (the liquid surface has gas overflow), then change to slow feed, heat up to 43°C, start to feed air , the volume of air per minute is 3000ml, the reaction temperature is controlled at 40~45°C, and the reaction time is 9h. After feeding air for 50min, start to draw the upper layer reaction solution into the liquid-liquid separator, the volume of the upper layer reaction solution drawn into the liquid-liquid separator per hour is 2400ml, and the reaction solution is in the liquid-liquid separator It is separated into an organic phase and an aqueous phase, the organic phase is sent to the butanone azine storage tank, and the aqueous phase is sent back to the reactor to continue to participate in the reaction. After the reaction, the organic phase and the aqueous phase were weighed and analyzed, and ...

Embodiment 3

[0022] Add 576g of methyl ethyl ketone, PdCl 2 / CuCl 2 Catalyst 28.8g, formamide 230g, sodium bromide 46g, water 350mL, after stirring and dissolving, feed ammonia gas to saturation (the liquid surface has gas overflow), then change to slow feed, heat up to 42°C, start to feed air , the volume of air per minute is 5500ml, the reaction temperature is controlled at 40~45°C, and the reaction time is 8h. After feeding air for 30min, begin to pump the upper layer reaction solution into the liquid-liquid separator, the volume of the upper layer reaction solution pumped into the liquid-liquid separator per hour is 3500ml, and the reaction solution is in the liquid-liquid separator It is separated into an organic phase and an aqueous phase, the organic phase is sent to the butanone azine storage tank, and the aqueous phase is sent back to the reactor to continue to participate in the reaction. After the reaction, the organic phase and the aqueous phase were weighed and analyzed, and...

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PUM

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Abstract

The invention discloses a method for synthesizing methyl ethyl ketazine through an air oxidation method. The methyl ethyl ketazine is synthesized by taking butanone and ammonia as raw materials, taking air as an oxidizing agent and using PdCl2 / CuCl2 as a catalyst and formamide and sodium bromide as cocatalysts. The method disclosed by the invention is wide in raw material source by taking the air as the oxidizing agent, thereby being low in cost; the method disclosed by the invention enables the synthetic reaction of ketazine to be carried out in a water phase by taking the butanone and ammonia as the raw materials and using the PdCl2 / CuCl2 as the catalyst and the formamide and sodium bromide as the cocatalysts, thereby reducing the reaction temperature and the energy consumption; the method disclosed by the invention can be used for separating the methyl ethyl ketazine from a reaction system in time by adopting a liquid-liquid separator, thereby reducing the generation of side reaction and the generation of a by-product, and increasing the yield and content of the ketazine. According to the method, the yield of the methyl ethyl ketazine is more than 90% in terms of the addition amount of ammonia, and the content of the methyl ethyl ketazine is about 95%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing butanazine by an air oxidation method. Background technique [0002] Ketazine is an intermediate for preparing hydrazine hydrate, and ketazine can be hydrolyzed to produce hydrazine hydrate. Hydrazine hydrate is an important chemical raw material and a widely used chemical product. It is an important raw material for the production of foaming agents, pesticides, medicines, dyes, developers and reducing agents. It is also used to manufacture high-purity metals, synthetic fibers and rare elements. Separation, deoxygenation of large boiler feed water, production of rocket fuel and explosives, etc. [0003] As everyone knows, the production method of hydrazine hydrate mainly contains four kinds, is respectively the Rasching (Rasching) method, the ketazine method of Bayer company, the urea method and the hydrogen peroxide method of PC...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07C251/88C07C249/16
Inventor李亚杉
Owner杭州圣捷菲科技有限公司