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Preparation process of azodicarbonamide

A technology of azodicarbonamide and preparation process, applied in organic chemistry and other directions, can solve problems such as waste of resources, environmental pollution, environmental pollution, etc., and achieve the effect of reducing consumption

Inactive Publication Date: 2014-04-30
GUANGXI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (5) Air Oxidation Air Oxidation is currently the most advanced method of hydrazine production, the basic raw materials are only ammonia and air, other raw materials such as diphenylmethane Ketones, cuprous chloride, etc. can be recycled in the synthesis process, and are all readily available chemicals, but this method is difficult to achieve industrial production
[0012] 2. Crude hydrazine refining process
The hydrochloric acid contains a large amount of inorganic salts and organic amines and azo substances, which is difficult to handle
This process is low in cost and is adopted by most manufacturers in the world, but waste acid is generated and unreacted chlorine gas escapes, polluting the environment
In my country, chlorine gas is often used in the preparation of foaming agent ADC by oxidized biurea, which produces a large amount of hydrochloric acid by-products, causing serious pollution to the environment and wasting resources.

Method used

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  • Preparation process of azodicarbonamide

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Effect test

Embodiment 1

[0055] The preparation process of azodicarbonamide, the process flow see figure 1 ,Proceed as follows:

[0056] 1) Sodium hypochlorite, sodium hydroxide lye with a mass concentration of 11% and a prepared urea solution with a mass concentration of 4% are mixed at a urine-to-chlorine ratio of 1:1 . 189 (mass ratio), chlor-alkali ratio of 1:1.162 (mass ratio) is pumped to the standpipe reactor, and the mass ratio of the amount of catalyst added to the urea used in the reaction is 1 : 83 . Hydrazine hydrate is produced under the action of 33% magnesium sulfate, and the reaction temperature of the pipeline reactor is controlled at 110-114°C to obtain hydrazine hydrate solution (crude product).

[0057] 2) The generated hydrazine hydrate solution is cooled down to -5°C by freezing, and sodium carbonate is precipitated in the form of solid crystallized sodium carbonate decahydrate, which is sent to a centrifuge for solid-liquid separation to remove salts, and the refined hydrazine...

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Abstract

The invention discloses a preparation process of azodicarbonamide. The process comprises the steps: 1) synthesizing a hydrazine hydrate crude product by a urea method; 2) refining hydrazine hydrate by a freeze separation method; 3) preparing biurea by alkaline condensation; and 4) obtaining the azodicarbonamide by a hydrogen peroxide oxidation method. According to the preparation process, different procedure production methods are analyzed and compared, the hydrazine hydrate is synthesized by selecting the urea method; refined hydrazine is obtained from crude hydrazine by the freeze separation method, biurea is prepared in a continuous condensation manner by an alkaline process, and finally, the azodicarbonamide is generated by the biurea oxidized by the hydrogen peroxide. Thus, the traditional acid condensation is changed into alkaline condensation to synthesize the biurea, consumption of raw materials and environmental pollution are reduced, hydrogen peroxide is selected as an oxidant in the oxidation process of the biurea, just by-product water is generated in the reaction, the environment is not polluted, and a green chemical pathway is taken.

Description

Technical field [0001] The invention relates to a preparation process of azodicarbonamide. Background technique [0002] The production process of azodicarbonamide is divided into four parts: hydrazine hydrate synthesis, crude hydrazine refining, condensation reaction and biuret oxidation. Most manufacturers use chlorine-based oxidants when preparing hydrazine raw materials using the urea method, and chlorine is also used as the oxidant when using biuret to prepare ADC. Unreacted chlorine is discharged into the atmosphere, polluting the environment. As the country and society pay more and more attention to environmental protection, there will be increasing pressure and restrictions on the use of chlorine. To this end, existing processes should be improved, such as using ketazine as raw material and hydrogen peroxide instead of chlorine. Oxidants, etc. [0003] 1. At present, there are five main hydrazine hydrate production processes at home and abroad: the traditional Ras...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/20
Inventor 罗建平余颖思
Owner GUANGXI UNIVERSITY OF TECHNOLOGY
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