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Method for preparing azodicarbonamide by oxygen oxidation

An azodicarbonamide and oxygen oxidation technology, applied in the direction of organic chemistry, can solve the problems of high equipment requirements, corrosion equipment, and high equipment requirements, and achieve the effects of new preparation technology, less product impurities, and uniform particle size.

Inactive Publication Date: 2016-10-12
JIANGSU SOPO CHEM +2
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  • Claims
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Problems solved by technology

The chlorine oxidation method is highly toxic and highly corrosive, so it has high requirements on equipment, and this method will produce a large amount of hydrogen chloride-containing wastewater, which will bring huge pressure to environmental protection issues under such severe environmental protection conditions today; the hydrogen peroxide method The co-catalyst used is either expensive or difficult to handle, and the cost is relatively high. The use of hydrogen peroxide with too high a concentration is likely to cause an explosion accident; during the chlorate process, highly toxic chemical impurities that are difficult to get out will be produced, which seriously affect the "ADC" development. The quality of the foaming agent is not suitable for industrial production, and there is also the problem of corrosion of equipment, and the requirements for equipment are relatively high

Method used

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  • Method for preparing azodicarbonamide by oxygen oxidation

Examples

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Embodiment 1

[0014] Embodiment 1: choose cobalt-manganese catalyst 15g that is made up of cobalt chloride and manganese nitrate, cobalt-manganese ion ratio is 1:1 in the catalyst, take biurea 100g, add 500ml deionized water to dissolve and form solution, solution is heated to 70 ℃, and continue to feed oxygen to keep the pH of the solution at 7. After 6 hours of reaction, the reaction is terminated. After filtration, the filter cake is washed three times with 100ml distilled water, and vacuum-dried at 90°C to obtain 91.5g of the product. After IR, IH-NMR and ESI-MS analysis confirmed that its structure is azodicarbonamide with a yield of 93.1% and a content of more than 99.5%. The detection method refers to HG2097-2008.

Embodiment 2

[0015] Example 2: Select 20g of a cobalt-manganese catalyst composed of cobalt sulfate and manganese sulfate, the ratio of cobalt-manganese ions in the catalyst is 2:1, take 100g of biurea, add 500ml of deionized water to dissolve and form a solution, and heat the solution to 70°C , and continue to feed oxygen to keep the pH of the solution at 7. After 6 hours of reaction, the reaction is terminated. After filtration, the filter cake is washed three times with 100ml distilled water, and vacuum-dried at 90°C to obtain 93.4g of the product. After IR, IH-NMR and ESI -MS analysis confirms that its structure is azodicarbonamide, the yield rate is 95.1%, and the content is greater than 99.5%. The detection method refers to HG2097-2008.

Embodiment 3

[0016] Example 3: Select 15g of cobalt-manganese catalyst composed of cobalt acetate and manganese acetate, the ratio of cobalt-manganese ions in the catalyst is 3:1, take 100g of biurea, add 500ml of deionized water to dissolve and form a solution, and heat the solution to 80°C , and continue to feed oxygen to keep the pH of the solution at 7. After 7 hours of reaction, the reaction is terminated. After filtration, the filter cake is washed three times with 100ml distilled water, and vacuum-dried at 90°C to obtain 91.5g of the product. After IR, IH-NMR and ESI -MS analysis confirms that its structure is azodicarbonamide, the yield rate is 93.1%, and the content is greater than 99.5%. The detection method refers to HG2097-2008.

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Abstract

The invention relates to a method for preparing azodicarbonamide by oxygen oxidation. The method comprises the following steps: taking biurea as a raw material; dissolving the biurea in a solvent to form a solution; adding a cobalt manganese catalyst in the solution; feeding oxygen under joint catalysis of the cobalt manganese catalyst and under the neutrality condition that the temperature of the solution is kept at 60-100 DEG C and carrying out oxidation reaction; after reaction is conducted for 6-8 hours, purifying to obtain the azodicarbonamide with uniform grain size. By the method for preparing the azodicarbonamide by oxygen oxidation, a preparation process is simple, requirements to equipment are low, and the prepared product is high in purity and uniform in grain size.

Description

technical field [0001] The invention relates to a method for preparing azodicarbonamide by an oxygen oxidation method. Background technique [0002] Biurea: Its chemical formula is C2H6N4O2, its English name is 1,2-Hydrazinedicarboxamide, and its structural formula is Azodicarbonamide, its chemical formula is C2H4N4O2, its English name is azodicarbonamide, and its structural formula is: Azodicarbonamide, commonly known as "ADC" foaming agent, is currently the chemical foaming agent with the most modified varieties, the largest production and consumption, and the widest application fields in the world. Because of its non-toxicity, moderate decomposition temperature, and colorless decomposition products Odorless can be used in products such as EVA, PVC, PE, PB, polyamide 11, neoprene, acetonitrile rubber, butyl rubber, styrene-butadiene rubber and silicone rubber. It is also the development with the fastest growth rate in recent years. foaming agent. It can be seen from t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/20
CPCC07C281/20
Inventor 张园园邵守言朱桂生郭如涛凌晨刘玲唐丽
Owner JIANGSU SOPO CHEM
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