Device for removing hydrogen fluoride impurity in germanium tetrafluoride

Abstract

The utility model discloses a device for removing hydrogen fluoride impurities in germanium tetrafluoride, and belongs to the technical field of inorganic chemical processes. The device comprises an adsorption tower, a microparticle filter, a pressure gauge, a thermometer and a tripod, the bottom of the adsorption tower is fixedly welded with the tripod, a feed port is formed in the top of the adsorption tower, a discharge port is formed in the bottom of the adsorption tower, and the feed port and the discharge port are connected and sealed through flanges. The microparticle filter bags are mounted on two sides of the adsorption tower through pipelines and are respectively provided with a gas outlet valve and a gas inlet valve; the pressure gauge and the thermometer are mounted on a flange of the feeding hole through pipelines and are respectively provided with a valve, and a probe rod of the thermometer extends to the bottom of the adsorption tower. The device can efficiently, simply, conveniently and safely remove hydrogen fluoride in germanium tetrafluoride, the product quality is improved, strong corrosion of hydrogen fluoride in germanium tetrafluoride to equipment such as detection equipment, valve pipelines and a rectifying tower is avoided, the problem that the pipelines and the valves are blocked is solved, and meanwhile the follow-up rectification purification pressure of germanium tetrafluoride is greatly relieved.

Description

TECHNICAL FIELD

[0001] The utility model belongs to inorganic chemical process technical field, concretely relates to a kind of hydrogen fluoride impurity removal device in germanium tetrafluoride produced by high-purity germanium metal and fluorine gas reaction. BACKGROUND

[0002] Germanium tetrafluoride (GeF4) is a germanium fluoride, and the purity of germanium tetrafluoride used in the semiconductor industry needs to reach 99.9%~99.99999%. Currently, germanium tetrafluoride is mainly prepared by the reaction of high-purity germanium metal and fluorine gas. The trace amount of hydrogen fluoride carried in the fluorine gas is the main impurity. In the process of synthesizing germanium tetrafluoride with high-purity germanium metal and pure fluorine gas, a large amount of fluorine gas is needed. The fluorine gas is mainly generated by the electrolysis of anhydrous hydrogen fluoride and obtained after purification. However, it still contains unreacted hydrogen fluoride. At the same time, after multiple nitrogen replacement and vacuumization in the germanium tetrafluoride synthesis reaction system, there is still a trace amount of moisture. The generated germanium tetrafluoride also hydrolyzes with water to produce hydrogen fluoride. As one of the main impurities in germanium tetrafluoride, hydrogen fluoride is difficult to remove in the rectification and purification process. In addition, the hydrogen fluoride impurity in germanium tetrafluoride has strong corrosiveness to the gas path pipeline, chromatographic column, and filling equipment of the gas chromatograph used for detecting the purity of germanium tetrafluoride, which easily causes damage to the precision parts such as gas chromatographic column. Moreover, hydrogen fluoride can easily cause the pipeline to be wet. After a long time of accumulation, a small amount of germanium fluoride and germanium dioxide is generated, causing the pipeline valve to be blocked. Therefore, there is an urgent need for a purification device to remove the hydrogen fluoride impurity in germanium tetrafluoride. The device can remove more than 99% of hydrogen fluoride at the front end in the preparation process of germanium tetrafluoride, improve the quality of germanium tetrafluoride products, avoid the blockage of the pipeline valve, greatly reduce the difficulty of later rectification and purification, and thus improve the protection of precision parts such as detection equipment. SUMMARY

[0003] The utility model aims to provide a kind of hydrogen fluoride's purification treatment device in germanium tetrafluoride, to improve the product quality of germanium tetrafluoride, solve the problem that pipeline valve appears blockage due to the existence of hydrogen fluoride in the production process of germanium tetrafluoride, and the problem of difficulty in later rectification and purification, and strong corrosiveness to precision parts such as detection equipment.

[0004] The application discloses a device for removing hydrogen fluoride impurities in germanium tetrafluoride, characterized by comprising an adsorption tower, a micro-particle filter, a pressure gauge, a thermometer and a tripod, the bottom of the adsorption tower is welded and fixed with the tripod, a feeding port is arranged at the top of the adsorption tower, and a discharging port is arranged at the bottom of the adsorption tower, the feeding port and the discharging port are both connected and sealed through flanges, the micro-particle filter comprises a first micro-particle filter and a second micro-particle filter, the first micro-particle filter is installed on one side of the upper portion of the adsorption tower through a pipeline and is connected with a gas outlet valve, and the second micro-particle filter is installed on the other side of the lower portion of the adsorption tower through a pipeline and is connected with a gas inlet valve; the pressure gauge and the thermometer are both installed on the flange of the feeding port through pipelines and are respectively provided with a first valve and a second valve, and the probe rod of the thermometer extends to the bottom of the adsorption tower.

[0005] Further, the hydrogen fluoride adsorption tower is made of 316L material, the inside of the hydrogen fluoride adsorption tower is mirror-polished, the height of the hydrogen fluoride adsorption tower is 1500mm-1800mm, the pipe opening diameter of the hydrogen fluoride adsorption tower is 200mm-300mm, and the wall thickness of the hydrogen fluoride adsorption tower is 3mm-5mm, and the use pressure range of the hydrogen fluoride adsorption tower is-0.1Mpa-1Mpa.

[0006] Further, the first micro-particle filter and the second micro-particle filter and the pipelines connected with the first micro-particle filter and the second micro-particle filter are made of corrosion-resistant materials, the size of the micro-particle filter is 80mm*100mm, the thickness of the micro-particle filter is 2mm-3mm, the filter core diameter of the micro-particle filter is less than 0.5μm, and the material of the micro-particle filter is a 316L microporous filter core.

[0007] Further, the pressure gauge is a 316L stainless steel diaphragm pressure gauge, and the pressure range of the pressure gauge is-0.1MPa-2.4MPa.

[0008] Further, the thermometer and the pipelines connected with the thermometer are made of corrosion-resistant materials, the probe rod is made of 316L material, the length of a single probe rod is 1200mm-1500mm, and the application range of the thermometer is-70℃-200℃.

[0009] Further, the diameter of the feeding port is 200mm-300mm, and the diameter of the discharging port is 150mm-180mm.

[0010] The device has the advantages that the hydrogen fluoride in germanium tetrafluoride can be efficiently, simply and safely removed according to the particularity of germanium tetrafluoride and the chemical properties of hydrogen fluoride, the product quality is improved, the strong corrosion of hydrogen fluoride in germanium tetrafluoride on detection equipment, valve pipelines and rectifying towers and other equipment is avoided, the problem of pipeline valve blockage is solved, and the subsequent rectification and purification pressure of germanium tetrafluoride is greatly reduced. ACCURACY OF DRAWINGS

[0011] Figure 1 It is a device for removing hydrogen fluoride impurities in germanium tetrafluoride.

[0012] Wherein: 1-adsorption tower, 2-feed inlet, 3-discharge outlet, 4-tripod, 5-pressure gauge, 6-thermometer, 71-first valve, 72-second valve, 8-inlet valve, 9-outlet valve, 10-first micro-particle filter, 11-second micro-particle filter. DETAILED DESCRIPTION

[0013] In the embodiment, the device for removing hydrogen fluoride impurities in germanium tetrafluoride includes an adsorption tower 1, a micro-particle filter, a pressure gauge 5, a thermometer 6 and a tripod 4. The adsorption tower 1 is made of 316L material and has a mirror-polished inner surface. The height of the adsorption tower 1 is 1500mm-1800mm, the pipe opening diameter is 200mm-300mm, the wall thickness is 3mm-5mm, the use pressure range is -0.1Mpa-1Mpa, and the adsorption tower 1 has corrosion resistance. The adsorption tower 1 is welded and fixed to the tripod 4 at the bottom. The adsorption tower 1 is provided with a feed inlet 2 at the top and a discharge outlet 3 at the bottom. The feed inlet 2 and the discharge outlet 3 are both connected and sealed by flanges. The pressure gauge 5 and the thermometer 6 are both installed on the flange of the feed inlet 2 through pipes and are respectively provided with a first valve 71 and a second valve 72. The probe rod of the thermometer 6 extends to the bottom of the adsorption tower 1. The pressure gauge 5 is a 316L stainless steel diaphragm pressure gauge with a pressure range of -0.1MPa-2.4MPa, which is used to measure and monitor the pressure of the adsorption tower 1, can provide high-precision pressure measurement, and can avoid the influence of high pressure in the adsorption tower 1 on the adsorption efficiency of hydrogen fluoride. The thermometer 6 and the pipes connected thereto are made of corrosion-resistant material, the probe rod is made of 316L material, the length of a single probe rod is 1200mm-1500mm, the application range is -70℃-200℃, and the thermometer 6 is used to monitor the temperature in the adsorption tower 1. When the temperature is higher than a certain value, it indicates that the adsorption capacity of the adsorbent 1 has reached saturation, and the hydrogen fluoride adsorbent needs to be replaced in time, otherwise the adsorption efficiency of hydrogen fluoride in germanium tetrafluoride will be affected. The micro-particle filter includes a first micro-particle filter 10 and a second micro-particle filter 11. The first micro-particle filter 10 is installed on one side of the upper part of the adsorption tower 1 through a pipe and is connected to an outlet valve 9. The second micro-particle filter 11 is installed on the other side of the lower part of the adsorption tower 1 through a pipe and is connected to an inlet valve 8. The first micro-particle filter 10, the second micro-particle filter 11 and the pipes connected thereto are made of corrosion-resistant material. The size of the micro-particle filter is 80mm*100mm, the thickness is 2mm-3mm, the filter core diameter is less than 0.5μm, the material is 316L microporous filter core, and the two micro-particle filters are used to filter the hydrogen fluoride adsorbent particles in the adsorption tower 1 to prevent the particles from entering the front-end fluorination reactor pipeline and the rear-end germanium tetrafluoride compression charging system and rectification system.

[0014] The device selects high-purity sodium fluoride particles as hydrogen fluoride adsorbent, which is in the form of particles with a diameter of Φ5 mm and a purity of >99%. Sodium fluoride particles have good adsorption capacity for hydrogen fluoride, and the adsorption rate can reach 99.9%. Fluoride ions (F-) in sodium fluoride have strong electrophilicity. At room temperature, hydrogen fluoride (HF) reacts with sodium fluoride (NaF) to adsorb hydrogen fluoride and generate sodium bifluoride (NaHF2). This adsorption reaction can be represented as: NaF + HF → NaHF2. In this process, sodium fluoride has no adsorption for germanium tetrafluoride, and the hydrogen fluoride in it is adsorbed and converted into a more stable compound, so that the hydrogen fluoride in germanium tetrafluoride gas can be adsorbed and removed.

[0015] In specific use, first prepare the raw materials, tighten the discharge port 3 flange to close, open the adsorption tower 1 feed port 2 flange, put high-purity sodium fluoride particles into the adsorption tower 1, ensure the dosage for this use, tighten the first valve 71 and the second valve 72 after completion, close the inlet valve 8 and the outlet valve 9, vacuum the whole device several times, open the first valve 71 and the second valve 72, check whether the pressure gauge 5 and the thermometer 6 are normal, check no error, open the inlet valve 8 to pass in nitrogen, pressurize the whole device, test whether it leaks, wait for 30 min to observe the pressure gauge 5, if the pressure gauge 5 value remains unchanged, then finally vacuum the whole device.

[0016] When in use, open the inlet valve 8 and the outlet valve 9 to pass germanium tetrafluoride into the adsorption tower 1, and through online detection data, the hydrogen fluoride removal rate can be as high as 99.9% or more. After several tests of passing in germanium tetrafluoride with different hydrogen fluoride contents, the hydrogen fluoride removal rate is as high as 99.9% or more.

Claims

1. A device for removing hydrogen fluoride impurities from germanium tetrafluoride, characterized in that: The adsorption tower, the micro-particle filter, the pressure gauge, the thermometer and the tripod are included, the bottom of the adsorption tower is welded and fixed with the tripod, the top of the adsorption tower is provided with a feeding port, the bottom is provided with a discharging port, the feeding port and the discharging port are both connected and sealed through flanges, the micro-particle filter includes a first micro-particle filter and a second micro-particle filter, the first micro-particle filter is installed on the upper side of the adsorption tower through a pipeline and is connected with a gas outlet valve, the second micro-particle filter is installed on the lower side of the adsorption tower through a pipeline and is connected with a gas inlet valve; the pressure gauge and the thermometer are both installed on the flange of the feeding port through a pipeline and are respectively provided with a first valve and a second valve, the probe rod of the thermometer extends to the bottom of the adsorption tower.

2. A device for removing hydrogen fluoride impurities from germanium tetrafluoride as claimed in claim 1, wherein The adsorption tower is made of 316L material, the inside is mirror-polished, the height is 1500mm-1800mm, the pipe diameter is 200mm-300mm, the wall thickness is 3mm-5mm, and the use pressure range is-0.1Mpa-1Mpa.

3. A device for removing hydrogen fluoride impurities from germanium tetrafluoride as claimed in claim 1, wherein The first micro-particle filter and the second micro-particle filter and the pipeline connected therewith are made of corrosion-resistant material, the size of the micro-particle filter is 80mm*100mm, the thickness is 2mm-3mm, the filter core diameter is less than 0.5μm, and the material is 316L microporous filter core.

4. A device for removing hydrogen fluoride impurities from germanium tetrafluoride as claimed in claim 1, wherein The pressure gauge is a 316L stainless steel diaphragm pressure gauge, and the pressure range is-0.1MPa-2.4MPa.

5. A device for removing hydrogen fluoride impurities from germanium tetrafluoride as claimed in claim 1, wherein The thermometer and the pipeline connected therewith are made of corrosion-resistant material, the probe rod is made of 316L material, the length of a single probe rod is 1200mm-1500mm, and the application range is-70℃-200℃.

6. A device for removing hydrogen fluoride impurities from germanium tetrafluoride as claimed in claim 1, wherein The diameter of the feeding port is 200mm-300mm, and the diameter of the discharging port is 150mm-180mm.

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