Purification device and purification method of germanium tetrafluoride

Abstract

The invention provides a germanium tetrafluoride purification device which comprises a crude product tank, the crude product tank is connected with a first adsorption tower, the first adsorption tower is connected with a second adsorption tower, the second adsorption tower is connected with a first rectifying tower, the first rectifying tower is connected with a second rectifying tower, the first rectifying tower is connected with a first condenser, and the second rectifying tower is connected with a second condenser. The first rectifying tower is connected with a first condenser, the second rectifying tower is connected with a second condenser, a first heater is mounted on the first rectifying tower, and a second heater is mounted on the second rectifying tower. The invention relates to a purification method of germanium tetrafluoride. The purification method comprises two times of adsorption and two times of rectification. The purification mode of adsorption and rectification is adopted, high-purity germanium tetrafluoride is obtained, the purification effect is excellent, the purity of the obtained product can reach 99.99%, and the problem that the purity of the germanium tetrafluoride product is insufficient in the field of semiconductor industry is effectively solved.

Description

Technical Field

[0001] The invention relates to a germanium tetrafluoride purification device and a purification method, belonging to the technical field of chemical industry. Background Art

[0002] Germanium tetrafluoride, molecular formula is GeF4, molecular weight is 148.63, melting point is -15℃, density is 5.12g / cm 3 It solidifies immediately when cooled under normal pressure and sublimates at -36.5℃. Germanium tetrafluoride is a colorless gas, stable to heat, emits strong smoke in the air, and has a pungent odor like garlic. It is soluble in water and hydrolyzes to form GeO2 and H2GeF4.

[0003] Germanium tetrafluoride has a wide range of applications in the fields of semiconductors, optical fiber communications, etc. It can be used for doping, ion implantation, etc., and has important application value. Germanium tetrafluoride products used in the semiconductor field have very high purity. Crude germanium tetrafluoride usually contains low-boiling nitrogen, oxygen, carbon monoxide, carbon dioxide, hydrogen, carbon tetrafluoride and high-boiling hydrogen fluoride, sulfur hexafluoride, etc. These impurities seriously affect the product performance of germanium tetrafluoride and greatly affect its application effect in high-end fields.

[0004] Chinese patent CN115231609A discloses a method and system for synthesizing and purifying high-purity germanium tetrafluoride, which belongs to the technical field of high-purity gas preparation. In the present invention, a replacement reaction is carried out with excess germanium tetrachloride and fluorine gas as raw materials to obtain a crude germanium tetrafluoride product. The reaction does not bring a large amount of reaction heat, and the reaction is easy to control. In addition, the excess germanium tetrachloride can ensure that the fluorine gas reacts completely. At the same time, a defluorination and dechlorination device is also provided in the synthesis and purification system of the present invention, and the defluorination and dechlorination device is filled with high-purity germanium particles. The high-purity germanium particles react with the generated chlorine gas and the entrained fluorine gas under high temperature conditions to generate germanium tetrachloride and germanium tetrafluoride. While removing the chlorine gas and fluorine gas in the crude germanium tetrafluoride product, the generated germanium tetrachloride is refluxed to the germanium tetrafluoride synthesis furnace as a raw material for further recycling. No tail gas is generated in the whole method, and the generated by-products can be further used as raw materials, which is economical and environmentally friendly.

[0005] Chinese patent CN112546659A discloses a device and method for purifying germanium tetrafluoride, including a gas supply device, a distillation tower, a condensing device, a transfer device and a storage device. The distillation tower includes a shell and several layers of tower frames. The top and bottom of the tower frame are open. Several tower plates with a certain inclination angle are arranged in parallel in the frame. Each layer of the tower frame is connected to a condensing device pipeline through a pipeline. The transfer device is a vacuum pump or an exhaust pump, and is connected to the storage device through a pipeline. The distillation tower is connected to the transfer device through three branch pipelines. Condensing pipes and valves are respectively arranged on the pipelines. The condensing pipes are connected to the condensing device through the pipeline. The device ensures the vacuum state in the distillation tower, greatly improves the purity of germanium tetrafluoride and improves it to high purity. The device makes the distillation process simple, practical, accurate and targeted, so that the germanium tetrafluoride has higher purity and better purification effect.

[0006] The above purification device and method are relatively complex, difficult to operate, and not easy to use in industrial production. Summary of the invention

[0007] The invention provides a germanium tetrafluoride purification device and a purification method, which purifies crude germanium tetrafluoride by adsorption and distillation. The method is simple and safe, and the product has high purity.

[0008] The technical solution of the present invention:

[0009] A germanium tetrafluoride purification device comprises a crude product tank, wherein the crude product tank is connected to a first adsorption tower, the first adsorption tower is connected to a second adsorption tower, the second adsorption tower is connected to a first distillation tower, the first distillation tower is connected to a second distillation tower, the first distillation tower is connected to a first condenser, the second distillation tower is connected to a second condenser, a first heater is installed on the first distillation tower, and a second heater is installed on the second distillation tower.

[0010] Preferably, the first adsorption tower, the second adsorption tower, the first condenser and the second condenser are connected to a dry pump.

[0011] Preferably, a first control valve is installed on the pipeline between the crude product tank and the first adsorption tower, a second control valve is installed on the pipeline between the first adsorption tower and the second adsorption tower, a third control valve is installed on the pipeline between the second adsorption tower and the first distillation tower, and a fourth control valve is installed on the pipeline between the first distillation tower and the second distillation tower; a fifth control valve is installed on the pipeline between the first adsorption tower and the dry pump; a sixth control valve is installed on the pipeline between the second adsorption tower and the dry pump; a seventh control valve is installed on the pipeline between the first distillation tower and the dry pump; an eighth control valve is installed on the pipeline between the second distillation tower and the dry pump; a ninth control valve is installed on the pipeline of the first condenser; and a tenth control valve is installed on the pipeline of the second condenser.

[0012] Preferably, a porous spherical sodium fluoride or potassium fluoride filler is arranged in the first adsorption tower, a 4A grade molecular sieve is arranged in the second adsorption tower, and theta rings, ball rings or Raschig ring fillers are arranged in the first distillation tower and the second distillation tower, respectively.

[0013] Preferably, the filler diameter of the first adsorption tower is 5-20 mm, and the porosity is 0.2-0.8.

[0014] Preferably, the filler diameter of the second adsorption tower is 5-20 mm, and the porosity is 0.2-0.8.

[0015] Preferably, the first distillation tower is a packed tower, and the packing diameter is 1 to 20 mm.

[0016] Preferably, the second distillation tower is a packed tower, and the packing diameter is 1 to 20 mm.

[0017] A method for purifying germanium tetrafluoride comprises the following steps:

[0018] S1, heating the crude product tank, passing the crude germanium tetrafluoride gas in the crude product tank into the first adsorption tower, until the pressure of the first adsorption tower is 0.1-2.0Mpa, maintaining the temperature at 20-100°C, and the sodium fluoride or potassium fluoride in the first adsorption tower adsorbs hydrogen fluoride;

[0019] S2, passing the crude germanium tetrafluoride gas in the first adsorption tower into the second adsorption tower until the pressure in the second adsorption tower is 0.4-1.5Mpa, maintaining the temperature at 20-100°C, and the sodium fluoride or potassium fluoride in the second adsorption tower adsorbs hydrogen fluoride;

[0020] S3, the crude germanium tetrafluoride gas in the second adsorption tower enters the first distillation tower at a pressure of 0.3-1.5Mpa; the first heater is heated to control the kettle temperature of the first distillation tower at 0-50°C, and the top temperature control device of the first distillation tower is at 10-40°C, so that the germanium tetrafluoride gas evaporates and rises through the distillation column, and condenses and refluxes during the rising process, and further removes nitrogen, oxygen, carbon monoxide, carbon dioxide, hydrogen and carbon tetrafluoride;

[0021] S4, controlling the germanium tetrafluoride gas in the first distillation tower to enter the second distillation tower at a pressure of 0.3-1.5Mpa; heating the second heater, controlling the kettle temperature of the second distillation tower at 0-50°C, and the top temperature control device of the second distillation tower at 10-40°C, so that the germanium tetrafluoride gas evaporates and rises through the distillation column, condenses and refluxes during the rising process, and further removes sulfur hexafluoride and hydrogen fluoride;

[0022] S5, using gas chromatography analysis and infrared spectrum analysis to detect, when the impurity components in the gas at the top of the second distillation tower meet the index requirements, high-purity germanium tetrafluoride gas enters the filling system.

[0023] Preferably, in step S2, the gas flow rate of germanium tetrafluoride is 0.5 to 5 L / min, and the gas residence time is 1 to 30 min;

[0024] Preferably, the distillation method is continuous distillation; the index of each impurity component is that the total content of each impurity component is below 0.01%.

[0025] The beneficial effects of the present invention are:

[0026] 1. The present invention adopts a purification method of adsorption and distillation to obtain high-purity germanium tetrafluoride, and its purification effect is excellent. The purity of the obtained product can reach 99.99%, which effectively solves the problem of insufficient purity of germanium tetrafluoride products in the semiconductor industry.

[0027] 2. The method described in the present invention has simple operation steps, optimizes the purification process through parameter control, and improves production efficiency.

[0028] 3. The method of the present invention is highly operable, and the obtained germanium tetrafluoride product has high purity and can be used for large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a schematic diagram of the overall structure of the device of the present invention.

[0030] 1. Crude product tank; 2. First adsorption tower; 3. Second adsorption tower; 4. First distillation tower; 5. Second distillation tower; 6. First condenser; 7. Second condenser; 8. First heater; 9. Second heater; 10. Dry pump;

[0031] V1, first control valve; V2, second control valve; V3, third control valve; V4, fourth control valve; V5, fifth control valve; V6, sixth control valve; V7, seventh control valve; V8, eighth control valve; V9, ninth control valve; V10, tenth control valve. DETAILED DESCRIPTION

[0032] Combine the following Figure 1 The present invention and the embodiments of the present invention provide a clear and complete description of the technical solutions of the present invention. The described embodiments are only part of the embodiments of the present invention, not all. Based on the embodiments of the present invention, other embodiments obtained by other persons in the art without creative work are within the scope of protection of the present invention. Among them, the methods are conventional methods unless otherwise specified, and the raw materials can be obtained from public commercial channels unless otherwise specified.

[0033] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present application. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprising" and / or "including" are used in this specification, it indicates the presence of features, steps, devices, components and / or their combinations.

[0034] Device Embodiment

[0035] like Figure 1 As shown, a germanium tetrafluoride purification device includes a crude product tank 1, the crude product tank 1 is connected to a first adsorption tower 2, the first adsorption tower 2 is connected to a second adsorption tower 3, the second adsorption tower 3 is connected to a first distillation tower 4, the first distillation tower 4 is connected to a second distillation tower 5, the first distillation tower 4 is connected to a first condenser 6, the second distillation tower 5 is connected to a second condenser 7, the first distillation tower 4 is equipped with a first heater 8, the second distillation tower 5 is equipped with a second heater 9, the first adsorption tower 2, the second adsorption tower 3, the first condenser 6 and the second condenser 7 are connected to a dry pump 10. A porous spherical sodium fluoride or potassium fluoride filler is arranged in the first adsorption tower 2, the filler diameter is 5 to 20 mm, and the porosity is 0.2-0.8; a 4A-grade molecular sieve is arranged in the second adsorption tower 3, the diameter is 5 to 20 mm, and the porosity is 0.2-0.8; the first distillation tower 4 and the second distillation tower 5 are respectively equipped with θ rings, ball rings or Raschig ring fillers, and the filler diameter is 1 to 20 mm.

[0036] A first control valve V1 is installed on the pipeline between the crude product tank 1 and the first adsorption tower 2, a second control valve V2 is installed on the pipeline between the first adsorption tower 2 and the second adsorption tower 3, a third control valve V3 is installed on the pipeline between the second adsorption tower 3 and the first distillation tower 4, and a fourth control valve V4 is installed on the pipeline between the first distillation tower 4 and the second distillation tower 5; a fifth control valve V5 is installed on the pipeline between the first adsorption tower 2 and the dry pump 10; a sixth control valve V6 is installed on the pipeline between the second adsorption tower 3 and the dry pump 10; a seventh control valve V7 is installed on the pipeline between the first distillation tower 4 and the dry pump 10; an eighth control valve V8 is installed on the pipeline between the second distillation tower 5 and the dry pump 10; a ninth control valve V9 is installed on the pipeline of the first condenser 6; and a tenth control valve V10 is installed on the pipeline of the second condenser 7.

[0037] Before the experiment, the fifth control valve V5, the sixth control valve V6, the seventh control valve V7, the eighth control valve V8 and the ninth control valve V9 were opened to replace the equipment. After the replacement, the fifth control valve V5, the sixth control valve V6, the seventh control valve V7, the eighth control valve V8 and the ninth control valve V9 were closed.

[0038] In the distillation stage of germanium tetrafluoride, the flow rate of germanium tetrafluoride entering the first adsorption tower 2 is regulated by adjusting the first control valve V1. When the pressure of the first adsorption tower 2 reaches the requirement, the second control valve V2 is opened to allow the material to enter the second adsorption tower 3. After the pressure of the second adsorption tower 3 reaches the requirement and passes the test, the third control valve V3 is opened to control the appropriate flow rate so that the material enters the first distillation tower 4 for collection, and the pressure drop of the first distillation tower 4 is controlled by adjusting the opening of the ninth control valve V9. After the target impurities are removed by distillation, the fourth control valve V4 is opened to control the appropriate flow rate so that the material enters the second distillation tower 5 for collection, and the pressure drop of the second distillation tower 5 is controlled by adjusting the opening of the tenth control valve V10.

[0039] Examples 1-3 employ the apparatus of the device example.

[0040] Example 1

[0041] A method for purifying high-purity germanium tetrafluoride, which comprises starting a dry pump 10, passing impure germanium tetrafluoride gas in a crude product tank 1 into the bottom of a first adsorption tower 2 which is filled with porous spherical sodium fluoride or potassium fluoride fillers, wherein the temperature of the first adsorption tower 2 is 20°C and the pressure is 0.5 MPa, and most of the hydrogen fluoride impurities can be removed; wherein the filler diameter of the first adsorption tower 2 is 5 mm and the porosity is 0.3; the germanium tetrafluoride gas passes through the first adsorption tower 2 and enters the bottom of a second adsorption tower 3 which is filled with 4A molecular sieves The temperature of the second adsorption tower 3 is 20°C and the pressure is 0.5Mpa, which can remove most of the hydrogen fluoride impurities; the filler diameter of the second adsorption tower 3 is 5mm and the porosity is 0.3; the germanium tetrafluoride gas passes through the adsorption tower and its pipeline into the first distillation tower 4 for collection, the flow rate of germanium tetrafluoride is 2L / min, the gas residence time is 10min, the temperature of the first distillation tower 4 in the collection stage is -10°C, the tower top temperature is 5°C, and the pressure of the distillation tower 4 is 0.4Mpa.

[0042] The first heater 8 heats and the first condenser 6 condenses, the kettle temperature of the first distillation tower 4 is controlled at 10°C, the top temperature is controlled at 15°C, the vapor is passed through the distillation column and rises, and gradually condenses and refluxes during the rising process, further removing nitrogen, oxygen, carbon monoxide, carbon dioxide, hydrogen, and carbon tetrafluoride.

[0043] The germanium tetrafluoride gas in the first distillation tower 4 enters the second distillation tower 5 through a flow meter, the germanium tetrafluoride flow rate is 2L / min, the gas residence time is 10min, the temperature of the second distillation tower 5 in the collection stage is -10°C, the top temperature is 5°C, and the pressure of the distillation tower 4 is 0.4Mpa. The second heater 9 heats, the second condenser 7 condenses, the kettle temperature of the second distillation tower 5 is controlled at 10°C, the top temperature is controlled at 15°C, the vaporization passes through the distillation column and rises, and gradually condenses and refluxes during the rising process, and further removes impurities such as sulfur hexafluoride and hydrogen fluoride.

[0044] Using gas chromatography and infrared spectrum analysis, when the impurity content of germanium tetrafluoride in the gas at the top of the distillation tower reaches the index requirements, the high-purity germanium tetrafluoride gas enters the collection device system.

[0045] The germanium tetrafluoride gas coming out from the top of the distillation tower has been tested and its purity has reached 99.9%. The impurity indicators are shown in Table 1.

[0046] Table 1

[0047] Test items Component content (volume fraction) <![CDATA[GeF4]]> ＞99.99％ <![CDATA[N2]]> 0.84 <![CDATA[O2]]> 1.52 <![CDATA[CO2]]> 0.43 CO 3.42 <![CDATA[H2]]> 7.58 <![CDATA[CF4]]> 3.47 HF 6.72 <![CDATA[SF6]]> 0.97

[0048] Example 2

[0049] A method for purifying high-purity germanium tetrafluoride, which comprises starting a dry pump 10, passing impure germanium tetrafluoride gas in a crude product tank 1 into the bottom of a first adsorption tower 2 which is filled with porous spherical sodium fluoride or potassium fluoride fillers, wherein the temperature of the first adsorption tower 2 is 50° C. and the pressure is 1.0 MPa, and most of the hydrogen fluoride impurities can be removed; wherein the filler diameter of the first adsorption tower 2 is 10 mm and the porosity is 0.5; the germanium tetrafluoride gas passes through the first adsorption tower 2 and enters a second adsorption tower 3 which is filled with 4A molecular sieves. At the bottom, the temperature of the second adsorption tower 3 is 50°C and the pressure is 0.8Mpa, which can remove most of the hydrogen fluoride impurities; the filler diameter of the second adsorption tower 3 is 10mm and the porosity is 0.5; the germanium tetrafluoride gas passes through the adsorption tower and its pipeline into the first distillation tower 4 for collection, the flow rate of germanium tetrafluoride is 3L / min, the gas residence time is 15min, the temperature of the distillation tower 4 in the collection stage is -7°C, the top temperature is 7°C, and the pressure of the distillation tower 4 is 0.7Mpa.

[0050] The first heater 8 heats and the first condenser 6 condenses, the kettle temperature of the first distillation tower 4 is controlled at 20°C, the top temperature is controlled at 25°C, the vapor is passed through the distillation column and rises, and gradually condenses and refluxes during the rising process, and nitrogen, oxygen, carbon monoxide, carbon dioxide, hydrogen, and carbon tetrafluoride are further removed.

[0051] The germanium tetrafluoride gas in the first distillation tower 4 enters the second distillation tower 5 through a flow meter, the germanium tetrafluoride flow rate is 2L / min, the gas residence time is 15min, the temperature of the second distillation tower 5 in the collection stage is -8°C, the top temperature is 8°C, and the pressure of the second distillation tower 5 is 0.7Mpa. The second heater 9 heats, the second condenser 7 condenses, the kettle temperature of the second distillation tower 5 is controlled at 20°C, the top temperature is controlled at 25°C, the vaporization passes through the distillation column and rises, and gradually condenses and refluxes during the rising process, and further removes impurities such as sulfur hexafluoride and hydrogen fluoride.

[0052] Using gas chromatography and infrared spectrum analysis, when the impurity content of germanium tetrafluoride in the gas at the top of the distillation tower reaches the index requirements, the high-purity germanium tetrafluoride gas enters the collection device system.

[0053] The germanium tetrafluoride gas coming out from the top of the distillation tower has been tested and its purity has reached 99.9%. The impurity indicators are shown in Table 2.

[0054] Table 2

[0055] Test items Component content (volume fraction) <![CDATA[GeF4]]> ＞99.99％ <![CDATA[N2]]> 1.88 <![CDATA[O2]]> 2.42 <![CDATA[CO2]]> 1.24 CO 0.91 <![CDATA[H2]]> 4.26 <![CDATA[CF4]]> 3.11 HF 5.27 <![CDATA[SF6]]> 0.88

[0056] Example 3

[0057] A method for purifying high-purity germanium tetrafluoride, which comprises starting a dry pump 10, passing impure germanium tetrafluoride gas in a crude product tank 1 into the bottom of a first adsorption tower 2 which is filled with porous spherical sodium fluoride or potassium fluoride fillers, wherein the temperature of the first adsorption tower 2 is 100° C. and the pressure is 2.0 MPa, and most of the hydrogen fluoride impurities can be removed; wherein the filler diameter of the first adsorption tower 2 is 20 mm and the porosity is 0.8; the germanium tetrafluoride gas passes through the first adsorption tower 2 and enters a second adsorption tower 3 which is filled with 4A molecular sieves At the bottom, the temperature of the second adsorption tower 3 is 40°C and the pressure is 1.5Mpa, which can remove most of the hydrogen fluoride impurities; the filler diameter of the second adsorption tower 3 is 20mm and the porosity is 0.8; the germanium tetrafluoride gas passes through the adsorption tower and its pipeline into the first distillation tower 4 for collection, the flow rate of germanium tetrafluoride is 4L / min, the gas residence time is 20min, the temperature of the first distillation tower 4 in the collection stage is -5°C, the top temperature is 5°C, and the pressure of the distillation tower 4 is 1.5Mpa.

[0058] The first heater 8 heats and the first condenser 6 condenses, the kettle temperature of the first distillation tower 4 is controlled at 50°C, the top temperature is controlled at 40°C, the vapor is passed through the distillation column and rises, and gradually condenses and refluxes during the rising process, and nitrogen, oxygen, carbon monoxide, carbon dioxide, hydrogen, and carbon tetrafluoride are further removed.

[0059] The germanium tetrafluoride gas in the first distillation tower 4 enters the second distillation tower 5 through a flow meter, the germanium tetrafluoride flow rate is 5L / min, the gas residence time is 20min, the temperature of the second distillation tower 5 in the collection stage is -5°C, the top temperature is 5°C, and the pressure of the second distillation tower 5 is 1.5Mpa. The second heater 9 heats, the second condenser 7 condenses, the kettle temperature of the second distillation tower 5 is controlled at 50°C, the top temperature is controlled at 40°C, the vaporization passes through the distillation column and rises, and gradually condenses and refluxes during the rising process, and further removes impurities such as sulfur hexafluoride and hydrogen fluoride.

[0060] Using gas chromatography and infrared spectrum analysis, when the impurity content of germanium tetrafluoride in the gas at the top of the distillation tower reaches the index requirements, the high-purity germanium tetrafluoride gas enters the collection device system.

[0061] The germanium tetrafluoride gas coming out from the top of the distillation tower was tested and its purity reached 99.9%. The impurity indicators are shown in Table 3.

[0062] Table 3

[0063]

[0064]

[0065] As shown in Table 1, Table 2 and Table 3, the test results are basically consistent. According to the test results of Table 1, Table 2 and Table 3, the purity of germanium tetrafluoride in Implementation Examples 1 to 3 can be obtained. The test results can illustrate that high-purity germanium tetrafluoride is prepared by the purification method of the present invention through adsorption and distillation, and the purity of the final product reaches 99.99%, which effectively solves the problem of insufficient purity of germanium tetrafluoride products in the semiconductor field.

[0066] The method described in the invention has simple steps, optimizes the purification process through parameter control, and improves production efficiency; the invention has strong operability, and the germanium tetrafluoride product obtained by purification has high purity and stability, and can be used for large-scale production.

[0067] The above-mentioned embodiments are preferred embodiments of the present invention, but not an exhaustive list of feasible experiments of the present invention. For those skilled in the art, various improvements made without departing from the spirit and essence of the present invention should be considered to be included in the protection scope of the present invention.

Claims

1. A germanium tetrafluoride purification device, characterized in that: The invention comprises a crude product tank (1), wherein the crude product tank (1) is connected to a first adsorption tower (2), the first adsorption tower (2) is connected to a second adsorption tower (3), the second adsorption tower (3) is connected to a first rectification tower (4), the first rectification tower (4) is connected to a second rectification tower (5), the first rectification tower (4) is connected to a first condenser (6), the second rectification tower (5) is connected to a second condenser (7), the first rectification tower (4) is provided with a first heater (8), and the second rectification tower (5) is provided with a second heater (9).

2. A germanium tetrafluoride purification device according to claim 1, characterized in that: The first adsorption tower (2), the second adsorption tower (3), the first condenser (6) and the second condenser (7) are connected to a dry pump (10).

3. A germanium tetrafluoride purification device according to claim 1, characterized in that: A first control valve (V1) is installed on the pipeline between the crude product tank (1) and the first adsorption tower (2); a second control valve (V2) is installed on the pipeline between the first adsorption tower (2) and the second adsorption tower (3); a third control valve (V3) is installed on the pipeline between the second adsorption tower (3) and the first rectification tower (4); and a fourth control valve (V4) is installed on the pipeline between the first rectification tower (4) and the second rectification tower (5); a fifth control valve (V5) is installed on the pipeline between the first adsorption tower (2) and the dry pump (10); a sixth control valve (V6) is installed on the pipeline between the second adsorption tower (3) and the dry pump (10); a seventh control valve (V7) is installed on the pipeline between the first rectification tower (4) and the dry pump (10); an eighth control valve (V8) is installed on the pipeline between the second rectification tower (5) and the dry pump (10); a ninth control valve (V9) is installed on the pipeline of the first condenser (6); and a tenth control valve (V10) is installed on the pipeline of the second condenser (7).

4. A germanium tetrafluoride purification device according to claim 1, characterized in that: A porous spherical sodium fluoride or potassium fluoride filler is arranged in the first adsorption tower (2), a 4A-grade molecular sieve is arranged in the second adsorption tower (3), and the first distillation tower (4) and the second distillation tower (5) are respectively provided with θ-ring, Pall ring or Raschig ring fillers.

5. A germanium tetrafluoride purification device according to claim 4, characterized in that: The filler of the first adsorption tower (2) has a diameter of 5 to 20 mm and a porosity of 0.2 to 0.8; The filler of the second adsorption tower (3) has a diameter of 5 to 20 mm and a porosity of 0.2 to 0.

8.

6. A germanium tetrafluoride purification device according to claim 1, characterized in that: The first distillation tower (4) is a packed tower, and the packing diameter is 1 to 20 mm.

7. A germanium tetrafluoride purification device according to claim 1, characterized in that: The second distillation tower (5) is a packed tower, and the packing diameter is 1 to 20 mm.

8. A method for purifying germanium tetrafluoride, using a germanium tetrafluoride purification device according to any one of claims 1 to 7, characterized in that: Take the following steps: S1, heating the crude product tank (1), passing the crude germanium tetrafluoride gas in the crude product tank (1) into the first adsorption tower (2), until the pressure of the first adsorption tower (2) is 0.1-2.0 MPa, maintaining the temperature at 20-100° C., and the sodium fluoride or potassium fluoride in the first adsorption tower (2) adsorbs hydrogen fluoride; S2, passing the crude germanium tetrafluoride gas in the first adsorption tower (2) into the interior of the second adsorption tower (3), until the pressure of the second adsorption tower (3) is 0.4-1.5Mpa, and the temperature is maintained at 20-100° C., and the sodium fluoride or potassium fluoride in the second adsorption tower (3) adsorbs hydrogen fluoride; S3, the crude germanium tetrafluoride gas in the second adsorption tower (3) enters the first distillation tower (4) at a pressure of 0.3-1.5Mpa; the first heater (8) is heated to control the kettle temperature of the first distillation tower (4) at 0-50°C, and the top temperature control device of the first distillation tower (4) is at 10-40°C, so that the germanium tetrafluoride gas evaporates and rises through the distillation column, condenses and refluxes during the rising process, and further removes nitrogen, oxygen, carbon monoxide, carbon dioxide, hydrogen and carbon tetrafluoride; S4, controlling the germanium tetrafluoride gas in the first distillation tower (4) to enter the second distillation tower (5) at a pressure of 0.3-1.5 MPa; heating the second heater (9), controlling the kettle temperature of the second distillation tower (5) at 0-50° C., and the top temperature control device of the second distillation tower (5) at 10-40° C., so that the germanium tetrafluoride gas evaporates and rises through the distillation column, condenses and refluxes during the rising process, and further removes sulfur hexafluoride and hydrogen fluoride; S5, using gas chromatography analysis and infrared spectrum analysis to detect, when the impurity components in the gas at the top of the second distillation tower (5) meet the index requirements, the high-purity germanium tetrafluoride gas enters the filling system.

9. The method for purifying germanium tetrafluoride according to claim 8, characterized in that: In step S2, the gas flow rate of germanium tetrafluoride is 0.5-5 L / min, and the gas residence time is 1-30 min.

10. The method for purifying germanium tetrafluoride according to claim 8, characterized in that: The distillation method is continuous distillation; The index of each impurity component is that the total content of each impurity component is less than 0.01%.

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