An apparatus for producing iridium hexafluoride

Abstract

The application relates to a preparation device of iridium hexafluoride, which comprises a reactor, the reactor comprises a first cylinder body and an electric heating jacket outside the wall of the first cylinder body, the outlet of the first cylinder body is connected with the inlet of a first-stage condensation collector through a pipeline, the outlet of the first-stage condensation collector is connected with the inlet of a product collection tank through a pipeline, the outlet of the product collection tank is connected with the inlet of a tail gas absorption tower, a filter is arranged on the pipeline between the reactor and the first-stage condensation collector, pipeline heating devices are arranged on the outer walls of the pipeline between the reactor and the first-stage condensation collector and the pipeline between the first-stage condensation collector and the product collection tank, the first-stage condensation collector and the product collection tank all comprise a second cylinder body and a temperature-adjusting jacket. Two baffles are arranged in the first-stage condensation collector and the product collection tank along the axial direction of the second cylinder body, so that the gas moves along a V-shaped route. The device improves the yield of the product. Meanwhile, the process is simple, the operation is convenient, and the cost is saved to a certain extent.

Description

Technical Field

[0001] This invention relates to the field of chemical engineering technology, specifically to an apparatus for preparing iridium hexafluoride. Background Technology

[0002] Iridium hexafluoride is commonly used as a catalyst in organic synthesis, especially in fluorination reactions, where it promotes the fluorination of various organic compounds. Furthermore, due to its excellent conductivity and stability, iridium hexafluoride can be used to manufacture key components in electronic devices and integrated circuits. However, iridium hexafluoride is a yellow crystalline solid at room temperature, is volatile, and has strong oxidizing and hygroscopic properties, readily absorbing moisture from the air and undergoing hydrolysis.

[0003] The preparation of iridium hexafluoride by reacting metallic iridium powder with fluorine gas often requires an excess of fluorine gas in the initial reaction to avoid the formation of low-fluoride compounds and thus improve product purity. However, in actual industrial production, an excess of fluorine gas in the initial reaction results in high reactor pressure, which is difficult to implement and poses significant safety risks. Using a continuous flow of pure fluorine gas easily leads to the formation of low-fluoride compounds. Therefore, using fluorinated nitrogen as a fluorine source is considered, but the presence of nitrogen carries away small floating particles, resulting in a very low yield. Furthermore, there is a risk of hydrolysis upon contact with water during the collection and transfer of iridium hexafluoride.

[0004] T. Chemnitz et al. prepared iridium hexafluoride by using nitrogen trifluoride as a fluorine source and argon as a carrier gas to dilute and react with iridium powder. However, nitrogen trifluoride needs to be ionized by a plasma source (RPS) to generate fluorine radicals before reacting with iridium powder to form iridium hexafluoride. This process is complex and difficult to implement for industrial production. Summary of the Invention

[0005] To address the aforementioned problems, the present invention aims to provide an apparatus for preparing iridium hexafluoride. This apparatus enables the industrial production of iridium hexafluoride using fluorine and nitrogen gas, improving yield, reducing the risk of hydrolysis during transfer, achieving high-yield preparation and collection of iridium hexafluoride, and avoiding the risk of deterioration due to contact with air during transfer.

[0006] An apparatus for preparing iridium hexafluoride includes a reactor. The reactor includes a first cylindrical body and an electrically heated jacket disposed on the outer wall of the first cylindrical body. The outlet of the first cylindrical body is connected to the inlet of a primary condenser via a pipe. The outlet of the primary condenser is connected to the inlet of a product collection tank via a pipe. The outlet of the product collection tank, located at the top, is connected to the inlet of a tail gas absorption tower. A filter is installed on the pipe between the reactor and the primary condenser. Pipe heating devices are installed on the outer wall of the pipe between the filter and the primary condenser, and on the outer wall of the pipe between the primary condenser and the product collection tank. Both the collector and the product collection tank include a second cylinder and a jacket for adjusting the temperature of the corresponding second cylinder. The jacket is connected to the corresponding second cylinder, and each jacket is provided with a refrigerant inlet and a refrigerant outlet. The first-stage condenser collector and the product collection tank are both provided with two baffles along the axial direction of the second cylinder. The length of the baffle is less than the height of the second cylinder. The two baffles in the same second cylinder are arranged facing each other. One baffle faces the inlet and is connected to the top of the second cylinder, and the other baffle is connected to the bottom of the second cylinder, so that the gas moves in the second cylinder in a roughly "V" shaped path.

[0007] Furthermore, a first valve is installed on the pipe between the reactor and the filter.

[0008] Furthermore, a nitrogen pipeline is connected between the reactor and the filter, and a second valve is installed on the nitrogen pipeline.

[0009] Furthermore, the nitrogen inlet pipe and the fluorine-nitrogen inlet pipe are respectively connected to the inlet of the first cylinder in the reactor.

[0010] Furthermore, the reactor is equipped with a reaction boat and a thermometer, with the thermometer located in the central area of ​​the reactor; a pressure gauge is also installed on the reactor.

[0011] Furthermore, pressure gauges are installed on both the primary condenser collector and the product collection tank.

[0012] Furthermore, the first cylinder of the reactor is made of Monel or nickel, while the second cylinder of the primary condenser and product collection tank is made of nickel.

[0013] Furthermore, the pipeline heating device includes an insulation strip, with insulation cotton and a temperature probe installed on the outside of the insulation strip, and the pipeline is heated by electricity.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] This study solves the problem of low yield in the preparation of iridium hexafluoride using fluorine nitrogen gas in industrial production, improving both product purity and yield, and holds promise for industrial-scale production. Converting the refrigerant to a heat transfer medium enables product transfer, reducing the risk of hydrolysis due to air contact during the transfer process. Furthermore, the process is simple, the process conditions are easy to meet, and the operation is convenient, resulting in cost savings to some extent. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the apparatus for preparing iridium hexafluoride according to the present invention.

[0017] Figure Labels

[0018] 1-Reactor, 2-First-stage condenser, 3-Product collection tank, 4-Filter, 5-Pipeline heating device, 6-Tail gas absorption tower. Detailed Implementation

[0019] To further illustrate the technical means and effects adopted by this utility model to achieve its intended purpose, the following will describe in detail the specific implementation, structure, features and effects of an iridium hexafluoride preparation apparatus proposed according to this utility model, in conjunction with preferred embodiments and accompanying drawings.

[0020] In the description of this utility model, it should be understood that the terms "center", "upper", "lower", "front", "rear", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0021] An embodiment of an apparatus for preparing iridium hexafluoride, such as... Figure 1 As shown, the reactor includes a reactor 1, which includes a first cylinder and an electric heating jacket disposed on the outer wall of the first cylinder. The outlet of the first cylinder is connected to the inlet of a primary condenser 2 via a pipe. The outlet of the primary condenser 2 is connected to the inlet of a product collection tank 3 via a pipe. The outlet of the product collection tank 3 located at the top is connected to the inlet of a tail gas absorption tower 6. A filter 4 is provided on the pipe between the reactor 1 and the primary condenser 2. Pipe heating devices are provided on the outer wall of the pipe between the filter 4 and the primary condenser 2, and on the outer wall of the pipe between the primary condenser 2 and the product collection tank 3. The primary condenser and the product collection tank each include a second cylinder and a jacket for adjusting the temperature of the corresponding second cylinder. The jacket is connected to the corresponding second cylinder, and each jacket has a refrigerant inlet and a refrigerant outlet. The inlet and outlet of the primary condenser and the product collection tank are located on the upper part of the side of the corresponding second cylinder.

[0022] Both the primary condenser collector 2 and the product collection tank 3 have two baffles arranged along the axial direction of the second cylinder. The length of each baffle is less than the height of the second cylinder. The two baffles in the same second cylinder are arranged facing each other. One baffle faces the inlet and is connected to the top of the second cylinder, while the other baffle is connected to the bottom of the second cylinder, so that the gas moves roughly along a "V" shaped path in the second cylinder.

[0023] In this embodiment, the pipeline heating device includes an insulation strip, with insulation cotton and a temperature probe on the outside of the insulation strip. The insulation cotton provides insulation, and the temperature probe controls the temperature. The insulation strip is electrically heated to ensure the pipeline temperature is between 60 and 100°C, preventing iridium hexafluoride from solidifying in the pipeline and reducing the yield.

[0024] A first valve is installed on the pipe between reactor 1 and filter 4.

[0025] A nitrogen pipeline is connected between reactor 1 and filter 4, and a second valve is installed on the nitrogen pipeline.

[0026] Filter 4 can filter solid particles, thus ensuring that the collected iridium hexafluoride product has a high purity.

[0027] The nitrogen inlet pipe and the fluorine-nitrogen inlet pipe are respectively connected to the inlet of the first cylinder in reactor 1, and the nitrogen inlet pipe and the fluorine-nitrogen inlet pipe are respectively equipped with inlet valves.

[0028] Reactor 1 is also equipped with a reaction boat and a thermometer. The thermometer is located in the central area of ​​the reactor, allowing for precise measurement of the reaction temperature, which is beneficial for temperature control. A pressure gauge is also installed on reactor 1.

[0029] The first cylinder of reactor 1 is made of Monel or nickel, and the second cylinder of the primary condenser and product collection tank is made of nickel.

[0030] Pressure gauges are installed on both the primary condenser collector 2 and the product collection tank 3.

[0031] When using the above-mentioned iridium hexafluoride preparation apparatus, the first cylinder of the reactor is cleaned and dried. Then, iridium powder is placed in the reaction boat, and the reaction boat is placed in the reactor. A pressure holding test is performed. If the pressure fluctuates within 1 kPa within 1 hour, it is considered to have good airtightness. After that, the reactor is evacuated and heated to 120-150°C and held for 2-4 hours to further dry the raw material iridium powder and the reactor. Then, the valve on the nitrogen inlet pipe at the front end of the reactor is opened to introduce nitrogen into the equipment and pipes. The system is evacuated and purged three times. After that, the reactor is heated again, and fluorine-nitrogen gas is introduced into reactor 1 to allow the reactor to react under the temperature and pressure conditions required by the process. Once the reaction time required by the process is met and the reactor pressure remains stable, the reaction ends. After the reaction is complete, the pipeline heating device is used to heat the pipeline between filter 4 and primary condenser 2, and the pipeline between primary condenser 2 and product collection tank 3, to 60-80°C. The first valve is then opened, allowing the gas in the reactor to pass sequentially through filter 4 and primary condenser 2 before entering product collection tank 3. After each equilibrium is reached (if the pressure in the reactor and the pressure in the primary condenser are stable, i.e., fluctuating within 1 kPa for 1 hour), the outlet of the first cylinder of the reactor and the inlet and outlet of the primary condenser are closed. This allows the reacted gas to solidify and settle in the primary condenser. After condensation for 4-6 hours, the outlet of the primary condenser, the inlet and outlet of the product collection tank are opened, allowing the product collection tank to collect any product not collected by the primary condenser. Next, the first valve is closed, the second valve is opened, and nitrogen gas is introduced to purge the gas in the pipeline between the reactor and the primary condenser into the primary condenser and then into the product collection tank. Iridium hexafluoride is collected in the primary condenser and the product collection tank, while other gases are discharged from the upper outlet of the product collection tank and enter the tail gas absorption tower. After tail gas absorption, the gas is vented. Finally, the nitrogen inlet pipeline at the reactor inlet is opened to purge the reactor. The gas passes sequentially through the reactor, the primary condenser, and the product collection tank, collecting any remaining product.

[0032] When it is necessary to transfer the product from the product collection tank, the refrigerant in the jacket outside the second cylinder of the primary condenser is replaced with a heating medium. Specifically, the heating medium is introduced through the refrigerant inlet and then discharged through the refrigerant outlet. The product collection tank is cooled using refrigerant, while the primary condenser is heated to 80–100°C, resulting in a product collection tank temperature of -60–-70°C. After the product collection tank has cooled to -60–-70°C and maintained at this temperature for 2–4 hours, it is evacuated. The product can then be transferred using the pressure difference. This reduces the risk of hydrolysis due to product contact with air during the transfer process. Furthermore, the process is simple, easy to operate, and saves costs to some extent.

[0033] The gas produced by the reactor passes through pipes and filters before entering the primary condenser. A pipe heating device on the outer wall of the pipes prevents iridium hexafluoride in the gas from liquefying or solidifying before entering the primary condenser, reducing losses. Once the gas containing iridium hexafluoride enters the primary condenser, internal baffles further disperse the gas, significantly improving heat transfer efficiency and allowing for better condensation of the iridium hexafluoride. A jacket is installed outside the primary condenser, allowing the introduced refrigerant to rapidly cool the gas and maintain a consistently low temperature. This reduces the likelihood of iridium hexafluoride decomposition. Furthermore, a product collection tank further enhances the complete capture of iridium hexafluoride, improving collection efficiency and purity. Pressure gauges display the pressure in the primary condenser and product collection tank, enabling the calculation of the iridium hexafluoride weight. When needed, the refrigerant in the jacket can be replaced with a heat source to heat the iridium hexafluoride, converting it into a gaseous state for transfer.

[0034] 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 way. Any simple modifications, equivalent changes, and alterations made by those skilled in the art to the above embodiments based on the technical essence of the present utility model without departing from the scope of the present utility model's technical solution shall still fall within the scope of the present utility model's technical solution.

Claims

1. An apparatus for preparing iridium hexafluoride, characterized in that, The system includes a reactor, which comprises a first cylindrical body and an electric heating jacket disposed on the outer wall of the first cylindrical body. The outlet of the first cylindrical body is connected to the inlet of a primary condenser collector via a pipe. The outlet of the primary condenser collector is connected to the inlet of a product collection tank via a pipe. The outlet of the product collection tank, located at the top, is connected to the inlet of a tail gas absorption tower. A filter is installed on the pipe between the reactor and the primary condenser collector. Pipe heating devices are installed on the outer walls of the pipe between the filter and the primary condenser collector, and on the outer walls of the pipe between the primary condenser collector and the product collection tank. Both the primary condenser collector and the product collection tank include a second cylindrical body and a jacket for adjusting the temperature of the corresponding second cylindrical body. The jacket is connected to the corresponding second cylindrical body, and each jacket has a refrigerant inlet and a refrigerant outlet. Inside both the primary condenser collector and the product collection tank, two baffles are arranged along the axial direction of the second cylindrical body. The length of the baffles is less than the height of the second cylindrical body. The two baffles inside the same second cylindrical body are arranged facing each other, with one baffle facing the inlet and connected to the top of the second cylindrical body, and the other baffle connected to the bottom of the second cylindrical body.

2. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, A first valve is installed on the pipe between the reactor and the filter.

3. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, A nitrogen pipeline is connected between the reactor and the filter, and a second valve is installed on the nitrogen pipeline.

4. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, The nitrogen inlet pipe and the fluorine-nitrogen inlet pipe are respectively connected to the inlet of the first cylinder in the reactor.

5. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, The reactor's first cylinder contains a reaction boat and a thermometer; the reactor is also equipped with a pressure gauge.

6. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, Pressure gauges are installed on both the primary condenser and the product collection tank.

7. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, The pipeline heating device includes an insulation strip, and the outside of the insulation strip is equipped with insulation cotton and a temperature probe.

8. The apparatus for preparing iridium hexafluoride as described in claim 1, characterized in that, The first cylinder of the reactor is made of Monel or nickel, while the second cylinder of the primary condenser and product collection tank is made of nickel.

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