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Preparation method of hydrazine hydrate

A technology of hydrazine hydrate and hydrazine salt, which is applied in the directions of hydrazine, nitrogen and non-metallic compounds, can solve the problems of reducing the yield of hydrazine hydrate, affecting the quality of hydrazine hydrate, and high equipment requirements, so as to save the refining process and equipment investment, The production process is safe and stable, and the effect of improving purity and quality

Inactive Publication Date: 2015-04-29
重庆锦杉科技有限公司
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although this method does not produce saline waste water and has no environmental pollution problems, the hydrolysis process of butanazine will produce more organic impurities. The existence of these organic impurities will reduce the yield of hydrazine hydrate and also affect the quality of hydrazine hydrate.
In order to remove these organic impurities from hydrazine hydrate, it is necessary to install a set of special hydrazine hydrate refining device. In addition, because the property of butanazine is very stable, its hydrolysis reaction must be carried out at relatively high temperature and pressure. The equipment requirements are high, the investment is large, and the steam energy consumption required for hydrolysis is also high

Method used

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  • Preparation method of hydrazine hydrate

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Effect test

Embodiment 1

[0040] refer to figure 1 process for production. 108g of butanone, 34g of formamide and 170g of mass fraction of 20% ammonia are packed into a four-necked flask with a reflux condenser, a thermometer, a dropping funnel and stirring, and a mass fraction of 30% peroxide is added in the dropping funnel. Hydrogen 56.7 g (0.5 mol). Heat in a water bath to raise the temperature of the solution to 45°C, start adding hydrogen peroxide dropwise, control the reaction temperature to 45°C, and complete the dropwise in 3 to 4 hours. After the dropwise addition, the temperature was raised to 50° C. and kept at 50° C. to continue the reaction for 2 hours. After completion of the reaction, stop heating and stirring, and transfer the reaction liquid into a separatory funnel after cooling, and separate the water phase and the oil phase, the content of butanazine in the oil phase is 69.2%. The aqueous phase is distilled and concentrated to recover ammonia, methyl ethyl ketone and catalyst. T...

Embodiment 2

[0042] 1100g butanone, 350g formamide and 1360g mass fraction of 28% ammonia water are charged into a jacketed reactor with stirring and reflux condenser, and there is a refrigerant for controlling the reaction temperature in the jacket. The temperature of the solution was raised to 40°C, and 566.7g of hydrogen peroxide (30%) was added dropwise, the refrigerant was turned on, the reaction temperature was controlled to be 40°C, and the dripping was completed in 3 to 4 hours. After the dropwise addition, the temperature was raised to 45°C, and the reaction was continued at 45°C for 2.5 hours. After completion of the reaction, stop heating and stirring, transfer the reaction solution into a separatory funnel, separate the water phase and the oil phase, and the content of butanazine in the oil phase is 67.7%. The aqueous phase is distilled and concentrated to recover ammonia, methyl ethyl ketone and catalyst. The oil phase is transferred to a jacketed reactor with stirring and dist...

Embodiment 3

[0044] 150g butanone, 52g ammonium acetate, 63g acetamide and 156g mass percent concentration are 25% ammoniacal liquor to pack in the four-neck flask that band reflux condenser, thermometer, dropping funnel and stir, add mass fraction in dropping funnel. 37.8g (1mol) of 90% hydrogen peroxide. Heat in a water bath to raise the temperature of the solution to 30°C, start adding hydrogen peroxide dropwise, control the reaction temperature to 30°C, and complete the dropwise in 3 to 4 hours. After the dropwise addition, the temperature was raised to 45° C. and kept at 45° C. to continue the reaction for 3 hours. After the reaction, stop heating and stirring, transfer the reaction solution into a separatory funnel, separate the water phase and the oil phase, and the content of butanazine in the oil phase is 95.5%. The aqueous phase is distilled and concentrated to recover ammonia, methyl ethyl ketone and catalyst. Transfer the oil phase into a four-neck flask with distillation con...

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Abstract

The invention belongs to the technical field of chemical synthesis, particularly relates to a preparation method of hydrazine hydrate and aims at improving production process of a hydrogen peroxide method and provides a hydrazine hydrate preparation method which is low in energy consumption, high in yield and free of pollution. The hydrazine hydrate preparation method provided by the invention comprises the following steps: carrying out reaction on ammonia, hydrogen peroxide and butanone in the presence of a catalyst to generate methyl ethyl azine; separating the methyl ethyl azine -containing upper oil phase from the catalyst-containing water phase; concentrating the catalyst-containing water phase to reuse; acid decomposing the methyl ethyl azine into hydrazonium salt and butanone, recycling the butanone, neutralizing the hydrazonium salt into hydrazine hydrate by alkali and distilling and recovering to obtain a hydrazine hydrate solution. The method can be used for preparing hydrazine hydrate and is high in yield and free of pollution.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of hydrazine hydrate. Background technique [0002] Hydrazine hydrate, also known as hydrazine hydrate, is the monohydrate of hydrazine (N 2 h 4 ·H 2 O), the appearance is a colorless transparent liquid, which can be mixed with water and alcohol arbitrarily, and is insoluble in ether and chloroform. Hydrazine hydrate is an important fine chemical intermediate, which is widely used in the synthesis of pesticides, medicines, water treatment agents, foaming agents, initiators and curing agents, etc., and has broad prospects for development and utilization. [0003] At present, most domestic methods of producing hydrazine hydrate are produced by the urea method, and some are produced by the ketazine method. Wherein, the urea method is to adopt urea and hypochlorite to react in alkaline solution to obtain hydrazine hydrate, and the hydra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/16
Inventor 李亚杉
Owner 重庆锦杉科技有限公司
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