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Method for preparing hydrazine hydrate

A hydrazine hydrate and a reaction kettle technology are applied in the field of preparing hydrazine hydrate, can solve the problems of pollution and high purity of hydrazine hydrate, and achieve the effects of simple process, high purity and low cost

Active Publication Date: 2015-04-22
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

The hydrazine hydrate obtained by the method is easy to operate and has high purity, which not only solves the content requirement of hydrazine hydrate but also solves the pollution problem, and also greatly reduces the production cost and resource consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Put 130 g of benzophenone into the reactor, add 1.5 g of thorium oxide, 1.5 g of ammonium chloride and 8 g of cuprous chloride respectively, seal the reactor and evacuate it, raise the temperature to 250 ° C, and flow to the reactor at a speed of 0.5 L / min. Ammonia is continuously fed into the reactor, and oxygen is fed into the reactor at a speed of 2L / min at the same time. Under this condition, the reaction is carried out for 8 hours to obtain 65% benzophenone dinitrogen. In the reaction, the oxidation Under the catalysis of thorium and ammonium chloride, benzophenone and ammonia undergo dehydration condensation to generate dibenzylidene amine, and under the catalysis of cuprous chloride, dibenzylidene amine is further oxidatively coupled to form benzophenone diazo, After the reaction, the reaction kettle was naturally cooled to room temperature to separate the benzophenone diazo, and at the same time, the catalyst was centrifuged, washed and recovered for the next rea...

Embodiment 2

[0012] Put 260g of benzophenone into the reaction kettle, add 2g of thorium oxide, 2g of ammonium chloride and 15g of cuprous chloride respectively, seal the reaction kettle and evacuate it, raise the temperature to 250°C, and inject Feed ammonia continuously, and feed oxygen into the reactor at a speed of 2L / min simultaneously, and react under this condition for 10 hours to obtain benzophenone dinitrogen with a content of 65%. In the reaction, thorium oxide and chlorine Under the catalysis of ammonium chloride, benzophenone and ammonia undergo dehydration condensation to generate dibenzylidene amine, and under the catalysis of cuprous chloride, dibenzylidene amine is further oxidatively coupled to generate benzophenone diazo. , the reaction kettle was naturally cooled to room temperature, and the benzophenone diazoxide was separated, and the catalyst was centrifuged at the same time, and recovered after washing for the next reaction. Add 8g of polyethylene oxide and 8g of dod...

Embodiment 3

[0014] Put 650 g of benzophenone into the reaction kettle, add 8 g of thorium oxide, 8 g of ammonium chloride and 30 g of cuprous chloride respectively, seal the reaction kettle and evacuate it, raise the temperature to 250 ° C, and feed the reaction kettle at a speed of 0.5 L / min. Ammonia is continuously passed into the middle, and oxygen is passed into the reactor at a speed of 2L / min at the same time, and the reaction under this condition for 12 hours obtains benzophenone dinitrogen with a content of 60%. In the reaction, thorium oxide and Under the catalysis of ammonium chloride, benzophenone and ammonia undergo dehydration condensation to generate dibenzylidene amine, and under the catalysis of cuprous chloride, dibenzylidene amine is further oxidatively coupled to form benzophenone hydrazine, and the reaction ends Finally, the reaction kettle was cooled down to room temperature naturally, and the benzophenone diazoxide was separated. At the same time, the catalyst was cen...

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PUM

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Abstract

The invention discloses a method for preparing hydrazine hydrate. The method comprises the following steps of adding benzophenone into a reactor, vacuumizing the reactor, introducing ammonia gas into the reactor continuously at the speed of 0.5L / min, introducing oxidant oxygen into the reactor at the speed of 2L / min at the same time, carrying out reaction for 8-12 hours at the temperature of 250 DEG C to produce benzophenone-linked nitrogen, dispersing polyoxyethylene and dodecylbenzene sulfonic acid into benzophenone-linked nitrogen, mixing uniformly, feeding the mixture into an atmospheric distillation tower, hydrolyzing to obtain a finished product which is hydrazine hydrate, and recovering benzophenone at the same time, wherein thorium oxide, ammonium chloride and cuprous chloride serve as catalysts. The environment-friendly pollution-free oxygen is used as the oxidant, the process is simple, is convenient to operate and solves the problem of flooding during the hydrolysis of linked nitrogen, and the prepared hydrazine hydrate is high in purity and low in cost and is worthy of popularization.

Description

technical field [0001] The invention belongs to the field of fine chemical production, and in particular relates to a method for preparing hydrazine hydrate. Background technique [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 oxidizes ammonia gas with sodium hypochlorite to generate hydrazine hydrate. This method is also called the chloramine method because chloramine is generated in the reaction process. Since this method obtains an aqueous solution of 1 to 2% hydrazine, it needs to be evaporated and concentrated to obtain a marketable product, so the energy consumption is high, and a large amount of NaCl and NH are produced as by-products. 4 Salts such as Cl have a low yield (the total yield is 67%), so this method has basically been eliminated. The urea method is an improvement to the R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/16
Inventor 朱嘉震张敏李海存赵新远尹传祥王金才
Owner 山东斯递尔化工科技有限公司
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