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Process for preparing hydrazine hydrate by air oxidation method

A technology of air oxidation and hydrazine hydrate, applied in the direction of nitrogen and non-metallic compounds, hydrazine, etc., to meet the content requirements, high product purity, and low pollution effects

Inactive Publication Date: 2012-01-25
山东斯递尔化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the early 1980s, the Liming Chemical Research Institute of the Ministry of Chemical Industry had a research report on the preparation of hydrazine hydrate by the ketazine method. In the mid-1980s, the Southwest Chemical Industry Research Institute of the Ministry of Chemical Industry successfully tested the hydrogen peroxide and methyl ethyl ketone method to produce hydrazine hydrate. Not pilot

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Put 200g of benzophenone and two kinds of catalysts (2g and 8g of zinc-based, copper-nickel-based respectively) at 170-220°C into 0.3-0.5 liters / min ammonia gas and 1.0-1.5 liters / min The air, reacted under this condition for 4 ~ 10 hours to obtain a content of 50% benzophenone diazo. Add 4g of dodecylbenzenesulfonic acid, 40g of hydrochloric acid, and 200mL of water to carry out hydrolysis and alkali neutralization at 70-100°C to obtain hydrazine hydrate.

Embodiment 2

[0016] Put 400g of benzophenone and two kinds of catalysts (4g and 16g of zinc-based, copper-nickel-based respectively) at 170-220°C into 0.5-0.7 liters / min ammonia gas and 1.5-2 liters / min The air, reacted under this condition for 4 ~ 10 hours to obtain a content of 55% benzophenone diazo. Add 8g of stearic acid, 80g of hydrochloric acid, and 400mL of water to carry out hydrolysis and neutralization with alkali at 70-100°C to obtain hydrazine hydrate.

Embodiment 3

[0018] Put 1000g of benzophenone and two kinds of catalysts (8g and 30g of zinc-based, copper-nickel based) at 170-220°C and feed 1-1.8 liters / minute of ammonia gas and 2.5-5 liters / minute of air , Under this condition, react for 4 to 10 hours to obtain benzophenone diazoxide with a content of 60%. Add 10g of dodecylbenzenesulfonic acid, 100g of hydrochloric acid, and 1000mL of water to carry out hydrolysis and neutralization with alkali at 70-100°C to obtain hydrazine hydrate.

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PUM

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Abstract

The invention belongs to the field of fine chemical industry production and in particular discloses a process for preparing hydrazine hydrate by an air oxidation method. In the process, benzophenone serves as a raw material. The method is characterized by comprising the following steps of: in the presence of a catalyst, putting the benzophenone into a reactor; stirring uniformly; introducing ammonia and air stably and continuously; adding dodecylbenzene sulfonic acid and water under the strongly acidic condition; and hydrolyzing and neutralizing by adding alkali to obtain the hydrazine hydrate. The method is simple in operation, light in pollution and high in product purity. By the method, the requirement for the content of the hydrazine hydrate is met, the problem of pollution is solved, and production cost and resource consumption are greatly reduced.

Description

(1) Technical field [0001] The invention belongs to the field of fine chemical production, in particular to a process for preparing hydrazine hydrate by an air oxidation method. (2) Background technology [0002] At present, the industrial production methods of hydrazine hydrate mainly include Raschig method, urea method, ketazine method and hydrogen peroxide method. The Raschig method uses ammonia as the nitrogen source and uses sodium hypochlorite to oxidize ammonia gas to generate hydrazine hydrate. This method is also called the chloramine method because chloramine is generated during the reaction process. Because this method obtains 1-2% hydrazine Aqueous solution needs to be evaporated and concentrated to obtain marketable products, so the energy consumption is high, and a large amount of NaCl and NH are produced by-products 4 Cl and other salts have a low yield (total yield is 67%), so this method has basically been eliminated; the urea method is an improvement t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/16
Inventor 朱嘉震朱运宏马远忠尹传祥刘帅王颖李海存孙华杨鹏
Owner 山东斯递尔化工科技有限公司
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