Hydrogen fluoride recovery production apparatus

Abstract

The utility model belongs to fluorine chemical industry technical field especially relates to a hydrogen fluoride recovery production device, including the dehydrofluorination kettle, primary condenser, secondary condenser, hydrogen fluoride receiving tank, hydrogen fluoride dehydrofluorination kettle and tail gas absorption device that are sealed and connected in proper order through pipeline, a plurality of stirring paddles are arranged in the dehydrofluorination kettle, the dehydrofluorination kettle outside is provided with steam jacket, primary condenser is connected with the dehydrofluorination kettle top, secondary condenser is connected with primary condenser export, hydrogen fluoride receiving tank is connected with primary condenser and secondary condenser, hydrogen fluoride receiving tank outside is provided with brine jacket, hydrogen fluoride measuring tank is connected with hydrogen fluoride receiving tank, tail gas absorption device is connected with secondary condenser. The utility model makes excess HF from the organic phase volatilization, through the high -efficient liquefaction recovery of primary and secondary condenser, has improved the recovery rate, has reduced HF waste significantly, has reduced raw material unit consumption, has reduced waste acid emission from the source.

Description

Technical Field

[0001] This utility model belongs to the field of fluorochemical technology, and in particular relates to a hydrogen fluoride recovery and production device. Background Technology

[0002] Anhydrous hydrogen fluoride (HF) is an important fluorinating agent, widely used in pharmaceuticals, pesticides, and fine chemicals. It is particularly important in the fluorination of pyridine heterocyclic compounds, where an excess is required to ensure complete reaction. However, after the reaction, excess hydrogen fluoride dissolves in the organic phase. Traditional processes typically use water washing to remove residual HF, leading to the following problems:

[0003] 1. Large discharge of waste acid and wastewater: The washing process generates a large amount of wastewater containing hydrofluoric acid, which increases the difficulty and cost of environmental treatment;

[0004] 2. Serious waste of hydrogen fluoride: Excess HF is discharged as waste acid after being washed with water and is not recycled, resulting in increased raw material consumption.

[0005] 3. Poor economic efficiency: Waste acid treatment and raw material loss increase production costs and affect industry competitiveness;

[0006] Therefore, there is an urgent need to develop a hydrogen fluoride recovery device with a simple structure and high recovery efficiency to realize the recycling of HF, reduce waste acid emissions, and lower production costs. Utility Model Content

[0007] The purpose of this invention is to provide a hydrogen fluoride recovery production device to solve the problems existing in the prior art.

[0008] To achieve the above objectives, the technical solution adopted by this utility model is a hydrogen fluoride recovery production device, which includes a defluorinated hydrogen fluoride kettle, a primary condenser, a secondary condenser, a hydrogen fluoride receiving tank, a hydrogen fluoride defluorination kettle, and a tail gas absorption device that are sequentially and sealed by pipelines.

[0009] The defluorination reactor is equipped with multiple stirring paddles inside and a steam jacket outside. A primary condenser is connected to the top of the defluorination reactor, and a cold brine inlet is located on one side of the primary condenser. A secondary condenser is connected to the outlet of the primary condenser, and a cold brine inlet is located on one side of the secondary condenser. A hydrogen fluoride receiving tank is connected to the primary and secondary condensers, and a brine jacket is located on the outside of the hydrogen fluoride receiving tank for storing condensed liquid hydrogen fluoride. A hydrogen fluoride metering tank is connected to the hydrogen fluoride receiving tank for quantitatively transporting and recovering the hydrogen fluoride to the defluorination reactor. A tail gas absorption device is connected to the secondary condenser for treating uncondensed hydrogen fluoride gas.

[0010] Preferably, the defluorination reactor is made of a hydrogen fluoride-resistant Monel alloy to control the reaction temperature at 80-90℃.

[0011] Preferably, the primary condenser uses -15℃ low-temperature brine as the cooling medium to condense hydrogen fluoride gas, and the secondary condenser uses -15℃ low-temperature brine as the cooling medium to further condense residual hydrogen fluoride gas.

[0012] Preferably, the brine jacket can store brine at a temperature of -15°C.

[0013] Preferably, the condenser is made of Monel alloy.

[0014] Preferably, the hydrogen fluoride metering tank is equipped with a level sensor and a delivery pump for precise control of the amount of hydrogen fluoride recycled.

[0015] Compared with the prior art, the advantages and positive effects of this utility model are as follows:

[0016] This invention utilizes a defluorination reactor to heat excess HF, causing it to volatilize from the organic phase. The HF is then efficiently liquefied and recovered via primary and secondary condensers, improving the recovery rate, significantly reducing HF waste, lowering raw material consumption, and avoiding the large amounts of HF-containing wastewater generated by traditional water washing processes. This reduces waste acid emissions at the source, lowers environmental treatment costs, and meets green chemical requirements. The recovered liquid HF can be directly recycled for fluorination reactions, reducing the cost of purchasing new HF. A tail gas absorption device treats residual HF gas, ensuring emissions meet standards and guaranteeing production safety. The device is compact, stable in operation, and suitable for fine chemical industries such as pharmaceuticals and pesticides. It particularly solves the problem of recovering excess HF in fluorination processes of pyridine compounds, offering both economic and environmental benefits. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of this utility model, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of a hydrogen fluoride recovery and production device.

[0019] In the above diagrams, 1. Dehydrogenation reactor, 2. Primary condenser, 3. Secondary condenser, 4. Hydrogen fluoride receiving tank, 5. Hydrogen fluoride metering tank, 6. Hydrogen fluoride defluorination reactor, 7. Tail gas absorption device, 8. Liquid level sensor, and 9. Transfer pump. Detailed Implementation

[0020] To better understand the above-mentioned objectives, features, and advantages of this utility model, the present utility model will be further described below with reference to the accompanying drawings and embodiments. It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other.

[0021] Many specific details are set forth in the following description in order to provide a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Therefore, the present invention is not limited to the specific embodiments disclosed in the following specification.

[0022] Example 1, as Figure 1 As shown, the specific design of the key components mentioned above is described below: A hydrogen fluoride recovery production device includes a defluorination reactor 1, a primary condenser 2, a secondary condenser 3, a hydrogen fluoride receiving tank 4, a hydrogen fluoride defluorination reactor 6, and a tail gas absorption device 7, which are sequentially and sealed together by pipelines. The defluorination reactor 1 is equipped with multiple stirring paddles inside and a steam jacket outside. The primary condenser 2 is connected to the top of the defluorination reactor 1, and a cold brine inlet is located on one side of the primary condenser 2. The secondary condenser 3 is connected to the outlet of the primary condenser 2, and a cold brine inlet is located on one side of the secondary condenser 3. The hydrogen fluoride receiving tank 4 is connected to the primary condenser 2 and the secondary condenser 3, and a brine jacket is located outside the hydrogen fluoride receiving tank 4 for storing condensed liquid hydrogen fluoride. A hydrogen fluoride metering tank 5 is connected to the hydrogen fluoride receiving tank 4 for quantitatively transporting the recovered hydrogen fluoride to the defluorination reactor 6. The tail gas absorption device 7 is connected to the secondary condenser 3 for treating uncondensed hydrogen fluoride gas. After the fluorination reaction, the material containing excess HF is cooled to 80°C and then transferred to the defluorination reactor 1. The defluorination reactor 1 is made of corrosion-resistant Monel alloy, and the jacket is vented with steam to control the temperature at 80-90°C. Multiple agitators enhance the separation of HF from the organic phase, causing HF to vaporize and escape, while preventing excessive temperature from causing side reactions. The primary condenser 2 condenses most of the HF gas into liquid, which flows directly into the hydrogen fluoride receiving tank 4. The secondary condenser 3 collects the residual HF gas from the primary condenser 2, further improving the recovery rate. The condensate is returned to the hydrogen fluoride receiving tank 4, and the uncondensed trace amounts of HF gas enter the tail gas absorption device 7 to ensure that the emissions meet the standards. The liquid HF in the hydrogen fluoride receiving tank 4 is quantitatively transported to the hydrogen fluoride defluorination reactor 6 via the hydrogen fluoride metering tank 5, and then reused for the next batch of reaction, forming a closed-loop production. The two-stage condensation system improves the HF recovery rate, reduces raw material waste, lowers production costs, and avoids the large amount of HF-containing wastewater generated by traditional water washing processes. It solves the waste acid treatment problem from the source and is both economical and environmentally friendly.

[0023] The primary condenser 2 uses -15℃ low-temperature brine as the cooling medium to condense hydrogen fluoride gas. The secondary condenser 3 uses -15℃ low-temperature brine as the cooling medium to further condense residual hydrogen fluoride gas. The brine jacket can store -15℃ low-temperature brine. The interior of the condenser is made of Monel alloy, which has excellent corrosion resistance to anhydrous HF and medium-to-low concentration hydrofluoric acid. It is cheaper than Hastelloy, has a long service life, low maintenance cost, and low permeability, making it suitable for HF-organic phase mixed systems. It is an ideal material for HF recovery devices. The hydrogen fluoride metering tank 5 is equipped with a level sensor 8 and a transfer pump 9 for precise control of the amount of hydrogen fluoride recycled. Both the primary condenser 2 and the secondary condenser 3 use -15℃ low-temperature brine. Since hydrogen fluoride has a boiling point of 19.5℃, forced cooling with -15℃ brine allows for rapid liquefaction of HF gas. The primary condenser 2 handles the main HF gas flow, while the secondary condenser 3 captures residual gas, forming a gradient condensation process that improves recovery efficiency, ensures complete HF liquefaction, and reduces exhaust emissions. The use of brine at the same -15℃ temperature simplifies the refrigeration system and reduces energy consumption. The hydrogen fluoride receiving... Tank 4 has an external brine jacket to continuously provide a low-temperature environment, preventing the vaporization and evaporation of liquid HF. This avoids HF loss or pressure increase due to temperature fluctuations, reduces the need for tank depressurization, and lowers the risk of leakage. Liquid level sensor 8 monitors the HF level in real time, and transfer pump 9 delivers the HF to the hydrogen fluoride defluorination reactor 6 as needed, avoiding human error, ensuring stable reaction ratios, reducing personnel contact with HF, improving safety, and efficiently recovering and reducing waste acid emissions. It is suitable for HF recycling in fine chemicals such as pharmaceuticals and pesticides, and is especially suitable for production lines that are sensitive to recovery efficiency and cost.

[0024] The contents not described in detail in this specification are existing technologies known to those skilled in the art.

[0025] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any other way. Any person skilled in the art may make changes or modifications to the above-disclosed technical content to create equivalent embodiments for application in other fields. However, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present utility model without departing from the technical solution of the present utility model shall still fall within the protection scope of the technical solution of the present utility model.

Claims

1. A hydrogen fluoride recovery and production apparatus, characterized in that, It includes a hydrogen defluorination reactor, a primary condenser, a secondary condenser, a hydrogen fluoride receiving tank, a hydrogen fluoride defluorination reactor, and a tail gas absorption device, which are sequentially and sealed together by pipelines. The defluorination reactor is equipped with multiple stirring paddles inside and a steam jacket outside. A primary condenser is connected to the top of the defluorination reactor, and a cold brine inlet is located on one side of the primary condenser. A secondary condenser is connected to the outlet of the primary condenser, and a cold brine inlet is located on one side of the secondary condenser. A hydrogen fluoride receiving tank is connected to the primary and secondary condensers, and a brine jacket is located on the outside of the hydrogen fluoride receiving tank for storing condensed liquid hydrogen fluoride. A hydrogen fluoride metering tank is connected to the hydrogen fluoride receiving tank for quantitatively transporting and recovering the hydrogen fluoride to the defluorination reactor. A tail gas absorption device is connected to the secondary condenser for treating uncondensed hydrogen fluoride gas.

2. The hydrogen fluoride recovery production apparatus according to claim 1, characterized in that, The defluorination reactor is made of Monel alloy, which is resistant to hydrogen fluoride, and is used to control the reaction temperature at 80-90℃.

3. The hydrogen fluoride recovery production apparatus according to claim 2, characterized in that, The primary condenser uses -15℃ low-temperature brine as the cooling medium to condense hydrogen fluoride gas, and the secondary condenser uses -15℃ low-temperature brine as the cooling medium to further condense residual hydrogen fluoride gas.

4. The hydrogen fluoride recovery production apparatus according to claim 3, characterized in that, The brine jacket can store brine at a temperature of -15°C.

5. The hydrogen fluoride recovery production apparatus according to claim 4, characterized in that, The condenser is made of Monel alloy.

6. The hydrogen fluoride recovery production apparatus according to claim 5, characterized in that, The hydrogen fluoride metering tank is equipped with a level sensor and a delivery pump to precisely control the amount of hydrogen fluoride recycled.

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