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Preparation method of hydrazine hydrate

A technology of hydrazine hydrate and tubular reactors, applied in the direction of hydrazine, nitrogen and non-metallic compounds, etc., can solve the problems of large steam consumption, equipment investment and high energy consumption, avoid side reactions, improve production efficiency, and increase conversion rate and selective effects

Inactive Publication Date: 2018-11-13
重庆晶萃化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method obtains a dilute solution containing 1% to 2% of hydrazine hydrate, and the total yield is about 67%. It takes a considerable amount of heat to concentrate the hydrazine hydrate of the dilute solution. For every 1kg of hydrazine hydrate recovered, 40-110kg needs to be evaporated The water needs to consume a lot of steam, and its equipment investment and energy consumption are relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The sodium hypochlorite solution with an available chlorine content of 18% is continuously pumped into the first-stage tubular reactor after being metered by a metering pump, and liquid ammonia is also continuously added to the first-stage tubular reactor after being metered by a flow meter. The molar flow ratio of ammonia and ammonia is 1:1, the reaction temperature is controlled at 0°C to 5°C, the residence time is 60s, and then enters the second-stage tubular reactor; the liquid ammonia is continuously added to the second stage after being metered by a flow meter In the tubular reactor, the molar flow ratio of liquid ammonia and sodium hypochlorite pumped into the first-stage tubular reactor is 1.5:1, the reaction temperature is controlled at 30°C to 40°C, the residence time is 75s, and the hydrazine hydrate at the reactor outlet is The content is 10.6%, and the reaction yield is 92.2%.

Embodiment 2

[0024] The sodium hypochlorite solution with an available chlorine content of 18% is continuously pumped into the first-stage tubular reactor after being metered by a metering pump, and ammonia gas is also continuously added to the first-stage tubular reactor after being metered by a flow meter. The molar flow ratio of ammonia and ammonia is 1:1, the reaction temperature is controlled at 5°C to 10°C, the residence time is 45s, and then enters the second-stage tubular reactor; liquid ammonia is continuously added to the second stage after being measured by a flow meter In the tubular reactor, the molar flow ratio of liquid ammonia and sodium hypochlorite pumped into the first-stage tubular reactor is 2:1, the reaction temperature is controlled at 40°C to 50°C, the residence time is 60s, and the hydrazine hydrate at the reactor outlet is The content is 10.3%, and the reaction yield is 91.3%.

Embodiment 3

[0026]The sodium hypochlorite solution with an available chlorine content of 18% is continuously pumped into the first-stage tubular reactor after being metered by a metering pump, and ammonia gas is also continuously added to the first-stage tubular reactor after being metered by a flow meter. The molar flow ratio of ammonia and ammonia is 1:1, the reaction temperature is controlled at 10°C to 15°C, the residence time is 30s, and then enters the second-stage tubular reactor; the ammonia gas is continuously added to the second stage after being metered by a flow meter In the tubular reactor, the molar flow ratio of ammonia gas and sodium hypochlorite pumped into the first section of the tubular reactor is 1.75:1, the reaction temperature is controlled at 35°C to 45°C, the residence time is 90s, and the hydrazine hydrate at the reactor outlet is The content is 10.5%, and the reaction yield is 92.5%.

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Abstract

The invention provides a preparation method of hydrazine hydrate. The preparation method is used for significantly improving the production technology of Raschig process. The preparation method is characterized in that a sodium hypochlorite solution and liquid ammonia or ammonia gas are used as the raw materials, and a tubular reaction device is used for preparing the hydrazine hydrate; the tubular reaction device comprises a first tubular reactor and a second tubular reactor in series, the two steps of reaction are performed by sections according to different reaction temperatures, the side effect is effectively avoided, and the yield rate of the hydrazine hydrate reaches 90% or above; the mass concentration of the generated hydrazine hydrate is greater than 10%, and is greater than the mass concentration of Raschig process and urea process, the energy consumption in the hydrazine hydrate concentrating and recycling process is greatly decreased, the production efficiency is improved,and the production cost is reduced; compared with the ketazine method, the ketazine hydrolysis procedure with high energy consumption is not needed, the equipment investment is reduced, the high-salinity organic wastewater which has high COD (chemical oxygen demand) content and is difficult to treat is not produced, and the production is more energy-saving and environment-friendly.

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 is a chemical product with a wide range of uses. It is an important raw material for the production of foaming agents, pesticides, medicines, dyes, developers and reducing agents. It is also used in the manufacture of high-purity metals, synthetic fibers and rare elements. Deoxygenation, production of rocket fuel and explosives, etc. [0003] At present, there are three main production methods of hydrazine hydrate in China: Raschig method, urea method and ketazine method. Among them, the urea method uses urea and hypochlorite to react in an alkaline solution to obtain hydrazine hydrate. Since the reactant NaClO is a strong oxidizing agent, the product hydrazine hydrate is a strong reducing agent. During the reaction, hydrazine hydrate is oxidized by NaClO. The side ...

Claims

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Application Information

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IPC IPC(8): C01B21/16
CPCC01B21/16
Inventor 不公告发明人
Owner 重庆晶萃化工科技有限公司
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