CN220845503U - Synthesis system for producing hydrazine hydrate by ketazine method - Google Patents

Synthesis system for producing hydrazine hydrate by ketazine method Download PDF

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CN220845503U
CN220845503U CN202322579144.4U CN202322579144U CN220845503U CN 220845503 U CN220845503 U CN 220845503U CN 202322579144 U CN202322579144 U CN 202322579144U CN 220845503 U CN220845503 U CN 220845503U
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synthesis system
hydrazine hydrate
inlet
ammonia
storage tank
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CN202322579144.4U
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陈尚思
罗登彦
柴进祥
谢明辉
李得银
罗浩
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Yibin Haifeng Herui Co ltd
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Yibin Haifeng Herui Co ltd
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Abstract

The utility model discloses a synthesis system for producing hydrazine hydrate by a ketazine method, which comprises a temporary storage tank, an online analyzer, a circulating pump, an ammonia absorber, a primary cooler, a mixer and a secondary cooler which are sequentially connected through pipelines, wherein the lower part of the temporary storage tank is connected with a synthesis transfer pump through a pipeline, an ammonia water inlet is arranged on the pipeline between the circulating pump and the ammonia absorber, an acetone inlet is arranged on the pipeline between the primary cooler and the mixer, a sodium hypochlorite inlet is arranged at the inlet of the mixer, and a tail gas absorber is arranged at the top of the temporary storage tank. According to the synthesis system for producing hydrazine hydrate by the ketazine method, a circulation pipeline is arranged on the temporary storage tank, so that the retention time of materials is increased by circulating the synthetic liquid in the temporary storage tank, and the reaction can be completed; meanwhile, the method is used as a carrier for reaction and a power source for ammonia absorption, so that the synthesis yield of hydrazine hydrate by a ketazine method is improved, and meanwhile, the material loss is reduced.

Description

Synthesis system for producing hydrazine hydrate by ketazine method
Technical Field
The utility model relates to the technical field of hydrazine hydrate production, in particular to a synthesis system for producing hydrazine hydrate by a ketazine method.
Background
Hydrazine hydrate, also known as: hydrazine hydrate with a chemical formula of N 2H4·H2 O is a strong reducing agent, and the industrial production method of the hydrazine hydrate is carried out according to the Laxi (Rashing) method, the Bayer (Bayer) method or the hydrogen peroxide method by using the method for preparing the hydrazine hydrate by CN99118158.1 which is an important chemical raw material. The ketazine method is actually Bei Erfa, and is a method for preparing hydrazine hydrate by oxidizing ammonia with sodium hypochlorite in the presence of ketone to obtain ketazine and then hydrolyzing. CN99118158.1 considers Bei Erfa as another form of raschig, which shifts the chemical equilibrium by the formation of ketazine by the absorption of hydrazine by acetone, obtaining higher yields than that of raschig, presumably by the following chemical reaction equation:
NH3+NaOCl→NH2Cl+NaOH
NH2Cl+NH3+NaOH+2(CH3)2C=O→(CH3)2C=N-N=C(CH3)2+NaCl+3H2O
(CH3)2C=N-N=C(CH3)2+3H2O→NH2-NH2·H2O+2(CH3)2C=O
In the Laxi method, sodium hypochlorite is used as an oxidant, the generated hydrazine hydrate is used as a reducing agent, the yield of the hydrazine hydrate is not high, and ketazine which is not easy to oxidize is generated by a ketazine method, so that the high yield can be maintained. Many factors affecting the yield of ketazine synthesis, such as the ratio of acetone to ammonia, the concentration of sodium hypochlorite, the reaction temperature, and the inhibition of side reactions, make it difficult to obtain high yields stably for a long period of time. Relatively high reactant concentrations increase reaction rate and yield, but excessive amounts of reactants result in losses and increased recovery energy consumption.
Disclosure of utility model
The utility model aims to provide a synthesis system for producing hydrazine hydrate by a ketazine method, which reduces recovery energy consumption and improves yield.
The technical scheme adopted for solving the technical problems is as follows: the utility model provides a synthesizing system of ketazine method production hydrazine hydrate, ketazine method production hydrazine hydrate's synthesizing system includes the temporary storage tank, online analysis appearance, circulating pump, ammonia absorber, one-level cooler, blender, the second grade cooler that loop through the pipe connection in proper order, wherein the lower part of temporary storage tank has synthetic material transfer pump through the pipe connection the pipeline between circulating pump and the ammonia absorber is equipped with the aqueous ammonia import, be equipped with the acetone import on the pipeline between one-level cooler and the blender import is equipped with the sodium hypochlorite import, be equipped with the recovery gaseous phase ammonia import on the ammonia absorber, establish gaseous acetone import on the temporary storage tank, the top is equipped with the tail gas absorber.
Furthermore, the temporary storage tank is a normal pressure container.
Further, the sodium chlorate inlet is connected with a sodium hypochlorite inlet pipeline, and the sodium hypochlorite inlet pipeline is provided with an ORP meter.
Further, the ammonia absorber is a venturi structure, and gaseous ammonia is sucked in through a high-speed fluid.
Further, the mixer is a static mixer.
Further, the online analyzer is a near infrared analyzer, and can detect the contents of ketazine, acetone and ammonia in the synthetic liquid.
The synthesis system for producing hydrazine hydrate by the ketazine method is simple to operate and reduces equipment investment, and the synthesis is carried out under normal pressure; the tubular reactor can make the materials fully contacted, further reduce the equipment scale and reduce the occupied area and investment. The concentration of the raw material sodium hypochlorite is monitored by ORP, and according to the on-line monitoring of the concentration of the target product, the accurate control and the automatic control can be realized by means of an automatic instrument. The acetone concentration is detected on line, and whether the acetone amount needs to be regulated or not can be automatically judged according to the concentration of a product and the concentration condition of the acetone, and the regulation is carried out, so that the high yield and the stable control are ensured. The ammonia concentration is detected on line, whether the ammonia water amount needs to be regulated or not can be automatically judged according to the concentration of the product and the ammonia concentration condition, and the regulation is carried out, so that the high yield and the stable control are ensured. The two-stage control is carried out on the temperature, after the synthetic solution is absorbed into ammonia, the solution heat is released due to the dissolution of the ammonia, if the control is not carried out, the initial temperature is excessively high when sodium hypochlorite is mixed, and the sodium hypochlorite is decomposed to influence the synthetic yield; after the sodium hypochlorite is mixed for reaction, the synthetic solution is cooled, so that the volatilization loss of ammonia and acetone is reduced by controlling the temperature, or the energy consumption is increased due to secondary absorption; and can also prevent ammonia and acetone from gasifying at the impeller of the pump due to high temperature, thereby causing cavitation damage.
The beneficial effects of the utility model are as follows: according to the synthesis system for producing hydrazine hydrate by the ketazine method, a circulation pipeline is arranged on the temporary storage tank, so that the retention time of materials is increased by circulating the synthetic liquid in the temporary storage tank, and the reaction can be completed; meanwhile, the method is used as a carrier for reaction and a power source for ammonia absorption, so that the synthesis yield of hydrazine hydrate by a ketazine method is improved, and meanwhile, the material loss is reduced.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present utility model;
Marked in the figure as: 1-temporary storage tank, 2-online analyzer, 3-circulating pump, 4-ammonia absorber, 5-primary cooler, 6-mixer, 7-ORP, 8-secondary cooler, 9-tail gas absorber, 10-synthetic transfer pump.
Detailed Description
The utility model will be further described with reference to the drawings and examples.
As shown in figure 1, the synthesis system for producing hydrazine hydrate by a ketazine method comprises a temporary storage tank 1, an online analyzer 2, a circulating pump 3, an ammonia absorber 4, a primary cooler 5, a mixer 6 and a secondary cooler 8 which are sequentially connected through pipelines, wherein the lower part of the temporary storage tank 1 is connected with a synthesis transfer pump 10 through a pipeline, an ammonia water inlet is arranged on the pipeline between the circulating pump 3 and the ammonia absorber 4, an acetone inlet is arranged on the pipeline between the primary cooler 5 and the mixer 6, a sodium hypochlorite inlet is arranged on the inlet of the mixer 6, the ammonia absorber 4 is provided with a gas phase ammonia inlet, the pipeline for separating and recovering gas phase ammonia and acetone in a ketazine separation process is connected with the ammonia absorber 4, the temporary storage tank 1 is provided with a gaseous acetone inlet, the top is provided with a tail gas absorber 9, the sodium chlorate inlet is connected with a sodium hypochlorite inlet pipeline, and the sodium hypochlorite inlet pipeline is provided with an ORP 7. The ammonia absorber 4 is a venturi structure that sucks in gaseous ammonia through a high-velocity fluid. The mixer 6 is a static mixer. The online analyzer 2 is a near infrared analyzer, and can detect the contents of ketazine, acetone and ammonia in the synthetic liquid.
The utility model relates to a synthesis system for producing hydrazine hydrate by a ketazine method, which comprises the following operation processes:
When the device is started for the first time, the synthesis is carried out in a temporary storage tank 1 of a normal pressure container, ammonia water and acetone are firstly added into the temporary storage tank 1, after the ammonia and acetone content reaches the requirement, a circulating pump 3 is started for circulation, sodium hypochlorite with a certain flow is added for synthesis reaction, when the liquid level in the temporary storage tank 1 reaches 50% of the liquid level, a synthesis transfer pump 10 is started for conveying materials to a ketazine separation process, and gas phase ammonia and gas phase acetone separated and recovered in the ketazine separation process are returned to a synthesis system;
The synthetic liquid in the temporary storage tank 1 enters a primary cooler 5 through a circulating pump 3 to be cooled, and meanwhile, the recovered gas-phase ammonia and acetone are sucked and dissolved in the synthetic liquid through an ammonia absorber 4 and a tail gas absorber 9 to enter the primary cooler 5 together to be cooled, ammonia and acetone required by reaction are supplemented, sodium hypochlorite enters a mixer 6 to be uniformly mixed in a pipeline mixer 6, and then enters a secondary cooler 8 together with the synthetic liquid to be cooled and then enters the temporary storage tank 1 to be reacted; at the moment, according to the set acetone and ammonia content, the flow rates of ammonia water and acetone are automatically regulated to meet the process requirements, and at the moment, the synthesis yield can be automatically calculated according to the synthesis liquid conversion flow rate, the ketazine concentration, the raw material sodium hypochlorite addition amount and the concentration.
Examples:
As shown in figure 1, the synthesis system for producing hydrazine hydrate by a ketazine method comprises a temporary storage tank 1, an online analyzer 2, a circulating pump 3, an ammonia absorber 4, a primary cooler 5, a mixer 6 and a secondary cooler 8 which are sequentially connected through pipelines, wherein the lower part of the temporary storage tank 1 is connected with a synthesis transfer pump 10 through a pipeline, an ammonia water inlet is arranged on the pipeline between the circulating pump 3 and the ammonia absorber 4, an acetone inlet is arranged on the pipeline between the primary cooler 5 and the mixer 6, a sodium hypochlorite inlet is arranged on the inlet of the mixer 6, a gas-phase ammonia inlet is arranged on the ammonia absorber 4, the pipeline for separating and recovering gas-phase ammonia and acetone in the ketazine separation process is connected with the ammonia absorber 4, the temporary storage tank 1 is provided with a gas-phase acetone inlet, and the top is provided with a tail gas absorber 9. The sodium chlorate inlet is connected with a sodium hypochlorite inlet pipeline, and the sodium hypochlorite inlet pipeline is provided with an ORP meter 7.
The specific operation process is as follows:
Monitoring the concentration of raw material sodium hypochlorite through ORP, and controlling the effective chlorine in the sodium hypochlorite to be about 5%; detecting the concentration of acetone in the synthetic liquid on line to keep the concentration at 2-4%; detecting the ammonia concentration in the synthetic liquid on line to keep the ammonia concentration at 6-10%; the temperature is controlled in two stages by the primary cooler 5 and the secondary cooler 8, the temperature of the primary stage is controlled to be 20-25 ℃, and the temperature of the secondary stage is controlled to be 40-45 ℃.
Sodium hypochlorite with 5.0% available chlorine content was added at 5m 3/h, the measured ketazine content (calculated as hydrazine) was 2.55%, at this time the acetone content was 2.33%, the ammonia content was 13.6%, the temperature was 42 ℃, and the synthetic yield calculated as sodium hypochlorite was 95.55%.
Sodium hypochlorite with 5.2% available chlorine content was added at a flow rate of 5m 3/h, the measured ketazine content (calculated as hydrazine) was 2.58%, at this time the acetone content was 2.47%, the ammonia content was 13.40%, the temperature was 44 ℃, and the synthetic yield calculated as sodium hypochlorite was 95.60%.

Claims (6)

1. A synthesis system for producing hydrazine hydrate by a ketazine method is characterized in that: the synthesis system for producing hydrazine hydrate by the ketone-to-nitrogen method comprises a temporary storage tank, an online analyzer, a circulating pump, an ammonia absorber, a primary cooler, a mixer and a secondary cooler which are sequentially connected through pipelines, wherein the lower part of the temporary storage tank is connected with a synthesis transfer pump through a pipeline, an ammonia water inlet is formed in the pipeline between the circulating pump and the ammonia absorber, an acetone inlet is formed in the pipeline between the primary cooler and the mixer, a sodium hypochlorite inlet is formed in the inlet of the mixer, a recovered gas phase ammonia inlet is formed in the ammonia absorber, a gaseous acetone inlet is formed in the temporary storage tank, and a tail gas absorber is arranged at the top of the temporary storage tank.
2. The synthesis system for producing hydrazine hydrate by a ketazine method according to claim 1, wherein the synthesis system is characterized in that: the temporary storage tank is a normal pressure container.
3. The synthesis system for producing hydrazine hydrate by a ketazine method according to claim 1, wherein the synthesis system is characterized in that: the sodium chlorate inlet is connected with a sodium hypochlorite inlet pipeline, and the sodium hypochlorite inlet pipeline is provided with an ORP meter.
4. The synthesis system for producing hydrazine hydrate by a ketazine method according to claim 1, wherein the synthesis system is characterized in that: the ammonia absorber is of a venturi structure.
5. The synthesis system for producing hydrazine hydrate by a ketazine method according to claim 1, wherein the synthesis system is characterized in that: the mixer is a static mixer.
6. The synthesis system for producing hydrazine hydrate by a ketazine method according to claim 1, wherein the synthesis system is characterized in that: the online analyzer is a near infrared analyzer.
CN202322579144.4U 2023-09-21 2023-09-21 Synthesis system for producing hydrazine hydrate by ketazine method Active CN220845503U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202322579144.4U CN220845503U (en) 2023-09-21 2023-09-21 Synthesis system for producing hydrazine hydrate by ketazine method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202322579144.4U CN220845503U (en) 2023-09-21 2023-09-21 Synthesis system for producing hydrazine hydrate by ketazine method

Publications (1)

Publication Number Publication Date
CN220845503U true CN220845503U (en) 2024-04-26

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