An electronic grade tungsten hexafluoride purification device

Abstract

The present invention discloses an electronic-grade tungsten hexafluoride purification device, comprising: a heating tube for heating a tungsten hexafluoride mixed gas to 150°C-400°C; a buffer tank, one end of which is connected to the heating tube and the other end of which is provided with a connecting pipe; a reduction tower, the bottom of which is connected to the connecting pipe and the top of which is provided with an exhaust pipe; and a stuffing pipe, which is arranged in the reduction tower and has a breathable structure so that the tungsten hexafluoride mixed gas can only pass through the stuffing pipe and be discharged from the exhaust pipe. The stuffing pipe is filled with tungsten pellets and can automatically discharge used tungsten pellets and refill them with new tungsten pellets according to the intake volume of the tungsten hexafluoride mixed gas.

Description

Technical Field

[0001] The invention relates to the technical field of purification, in particular to an electronic-grade tungsten hexafluoride purification device. Background Art

[0002] Currently synthesized WF6 often contains a high level of impurities, which are categorized into volatile and non-volatile impurities based on their volatility. Non-volatile impurities, such as metallic impurities like potassium, sodium, and chromium, are removed by passing the produced primary WF6 through a packed distillation tower for distillation. Volatile impurities, such as gases like carbon dioxide, nitrogen, carbon monoxide, and hydrofluoric acid, can be removed based on their boiling points.

[0003] However, the current domestic WF6 industrial production has low purity and small output, which cannot meet the growing demand for high-purity WF6. Therefore, it is necessary to focus on the research and development of WF6 synthesis process and product purification technology, as well as the separation technology of difficult-to-remove Mo metal impurities, to prepare high-purity electronic-grade WF6 products.

[0004] The reason is that Mo metal impurities are the most challenging part in the WF6 production process. This is because after this type of metal ions combine with fluoride ions, the resulting compound is often MoF6, which has a melting point of 17.5°C and a boiling point of 34°C. It also has a high vapor pressure near the melting point. The melting point of WF6 is 2.3°C and the boiling point is 17.5°C. Therefore, the two are difficult to separate, and the separation treatment effect is general.

[0005] Therefore, it is necessary to provide an electronic grade tungsten hexafluoride purification device to solve the problems raised in the above background technology. Summary of the Invention

[0006] To achieve the above object, the present invention provides the following technical solution: an electronic grade tungsten hexafluoride purification device, comprising:

[0007] Heating tube, used to heat the tungsten hexafluoride mixed gas to 150℃-400℃;

[0008] a buffer tank, one end of which is connected to the heating pipe and the other end of which is provided with a connecting pipe;

[0009] a reduction tower, the bottom of which is connected to the connecting pipe and the top of which is provided with an exhaust pipe; and

[0010] A filling tube is provided in the reduction tower and has a breathable structure so that the tungsten hexafluoride mixed gas can only pass through the filling tube and be discharged from the exhaust pipe. The filling tube is filled with tungsten particles. The filling tube can automatically discharge the used tungsten particles and fill with new tungsten particles according to the intake volume of the tungsten hexafluoride mixed gas.

[0011] Furthermore, as a preference, the upper opening of the stuffing tube is connected to the stuffing supply bin by a feed pipe, the lower opening of the stuffing tube is connected to the collecting bin by a discharge pipe, an interception membrane is provided at the bottom of the collecting bin for intercepting solid particles, and the bottom of the collecting bin is connected to the reduction tower by a reflux pipe.

[0012] Furthermore, preferably, the filling tube is serpentine, comprising a plurality of nearly horizontal tube bodies and bends connected in series alternately in sequence, wherein the nearly horizontal tube body at the bottom is connected to the horizontal tube body by a bend, wherein the angle between the nearly horizontal tube body and the horizontal plane is 3°-12°.

[0013] Furthermore, preferably, an auger is rotatably provided in both the near-horizontal tube body and the horizontal tube body, and the length of the auger accounts for 1 / 6-1 / 3 of the length of the near-horizontal tube body or the horizontal tube body.

[0014] Furthermore, as a preference, a power bin is provided on the inner side of the reduction tower, the shaft of the auger extends into the power bin and is fixed with a driven wheel, and a wind wheel is also rotatably provided in the reduction tower near the air outlet of the connecting pipe, and the wind wheel is driven by the gas discharged from the connecting pipe, and a rotating shaft is fixed on the wind wheel, and the rotating shaft extends into the power bin and is fixed with a driving wheel, and the driving wheel is connected to a plurality of driven wheels by a chain.

[0015] Furthermore, preferably, the driving wheel can drive the driven wheel to perform a decelerating motion.

[0016] Furthermore, preferably, the sub-horizontal tube body and the horizontal tube body are both divided into at least two sections, and elastic tubes are connected between two adjacent sub-horizontal tube body sections and between two adjacent horizontal tube body sections.

[0017] Furthermore, preferably, a knocking wheel corresponding to the elastic tube is rotatably provided in the reduction tower.

[0018] Compared with the prior art, the present invention provides an electronic grade tungsten hexafluoride purification device with the following features:

[0019] Beneficial effects:

[0020] In an embodiment of the present invention, WF6 is introduced at 150°C-400°C. Within this temperature range, WF6 is not reduced, but MoF6 is reduced to MoF3. MoF3 has a high melting point and low vapor pressure, and can be adsorbed on the surface of the tungsten particles, thereby achieving the purpose of separating MoF6. The configuration of a serpentine filler tube can ensure the continuity of the movement of the tungsten particles, ensuring that it can effectively achieve the reduction and adsorption treatment of impurities. The filler tube can automatically discharge the used tungsten particles and fill with new tungsten particles according to the intake volume of the tungsten hexafluoride mixed gas, thereby ensuring the effectiveness of the tungsten particles in reducing impurities. The serpentine filler tube can also hinder the flow of gas, thereby ensuring that the gas fully contacts and reacts with the tungsten particles. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a schematic diagram of the structure of an electronic grade tungsten hexafluoride purification device;

[0022] Figure 2 This is a schematic diagram of the structure of a reduction tower in an electronic-grade tungsten hexafluoride purification device;

[0023] In the figure: 1. Heating pipe; 2. Buffer tank; 3. Reduction tower; 4. Connecting pipe; 5. Exhaust pipe; 6. Filling pipe; 61. Nearly horizontal pipe body; 62. Bend pipe; 63. Horizontal pipe body; 7. Filling supply bin; 8. Collection bin; 9. Reflux pipe; 10. Intercepting membrane; 11. Wind wheel; 12. Rotating shaft; 13. Driving wheel; 14. Driven wheel; 15. Chain; 16. Auger; 17. Elastic tube; 19. Discharge pipe; 20. Feed pipe. DETAILED DESCRIPTION

[0024] Example: See Figures 1-2 In an embodiment of the present invention, an electronic grade tungsten hexafluoride purification device includes:

[0025] The heating tube 1 is used to heat the tungsten hexafluoride mixed gas to 150°C-400°C. It should be explained that in this embodiment, the tungsten hexafluoride mixed gas refers to tungsten hexafluoride gas containing Mo ion impurities. The Mo ions in the tungsten hexafluoride gas are often present in the form of MoF6, which has the following characteristics: a melting point of 17.5°C, a boiling point of 34°C, and a high vapor pressure near the melting point;

[0026] A buffer tank 2, one end of which is connected to the heating pipe 1 and the other end of which is provided with a connecting pipe 4;

[0027] A reduction tower 3, the bottom of which is connected to the connecting pipe 4 and the top of which is provided with an exhaust pipe 5; and

[0028] The stuffing tube 6 is arranged in the reduction tower 3 and has a breathable structure so that the tungsten hexafluoride mixed gas can only pass through the stuffing tube 6 and be discharged from the exhaust pipe 5. The stuffing tube 6 is filled with tungsten particles. The stuffing tube 6 can automatically discharge the used tungsten particles and fill them with new tungsten particles according to the intake volume of the tungsten hexafluoride mixed gas.

[0029] The melting point of MoF6 is close to the boiling point of WF6, and MoF6 has a higher vapor pressure near its melting point, making it difficult to separate from WF6. In this embodiment, WF6 is introduced at a temperature of 150°C-400°C. Within this temperature range, WF6 is not reduced, while MoF6 is reduced to MoF3. Since MoF3 has a high melting point and low vapor pressure, it can be adsorbed on the surface of the tungsten particles, thus achieving the purpose of separating MoF6.

[0030] More specifically, the upper opening of the stuffing tube 6 is connected to the stuffing supply bin 7 via a feed pipe 20, and the lower opening of the stuffing tube 6 is connected to the collecting bin 8 via a discharge pipe 19. The bottom of the collecting bin 8 is provided with an interception membrane 10 for intercepting solid particles. The bottom of the collecting bin 8 is connected to the reduction tower 3 via a reflux pipe 9. New tungsten particles can be continuously supplied through the feed bin 7, while the collecting bin 8 can continuously collect used tungsten particles, thereby achieving uninterrupted renewal of tungsten particles and ensuring that it can effectively achieve reduction and adsorption treatment of impurities. In addition, the stuffing tube 6 is serpentine, comprising a plurality of nearly horizontal tube bodies 61 and bends 62 alternately connected in series. The nearly horizontal tube body 61 at the bottom is connected to the horizontal tube body 63 via a bend, wherein the angle between the nearly horizontal tube body 61 and the horizontal plane is 3°-12°.

[0031] It should be noted that, since the packing tube 6 is serpentine, the tungsten hexafluoride mixed gas can be discharged from the exhaust pipe 5 only after being processed layer by layer by the packing tube 6. That is to say, configuring the packing tube 6 as a serpentine is beneficial to ensuring the continuity of the packing tube 6 and the continuous replacement of the tungsten particles on the one hand, and is beneficial to hindering the flow of the gas on the other hand, ensuring that the gas can fully contact with the tungsten particles and ensuring the contact time, thereby making the impurities in the gas react more fully.

[0032] As a preferred embodiment, an auger 16 is rotatably provided in both the near-horizontal tube body 61 and the horizontal tube body 63 , and the length of the auger 16 accounts for 1 / 6-1 / 3 of the length of the near-horizontal tube body 61 or the horizontal tube body 63 .

[0033] Among them, by configuring the auger 16, active control of the tungsten particles can be achieved so that they are discharged at a certain speed.

[0034] In order to further realize that the filling tube 6 can automatically discharge the used tungsten particles and fill them with new tungsten particles according to the intake volume of the tungsten hexafluoride mixed gas, a power bin is provided on the inner side of the reduction tower 3, the shaft of the auger extends into the power bin and is fixed with a driven wheel 14, and the reduction tower 3 also rotates a wind wheel 11 close to the air outlet of the connecting pipe 4. The wind wheel 11 is driven by the gas discharged from the connecting pipe 4, and a rotating shaft 12 is fixed on the wind wheel 11. The rotating shaft 12 extends into the power bin and is fixed with a driving wheel 13, and the driving wheel 13 is connected to a plurality of driven wheels 14 by a chain 15.

[0035] That is to say, the greater the intake volume of the tungsten hexafluoride mixture, the faster the rotation speed of the wind wheel 11, thereby driving the rotation speed of the auger to increase. By configuring the auger 16, active control of the tungsten particles can be achieved so that they are discharged at a certain speed. Therefore, in this embodiment, the used tungsten particles can be automatically discharged and filled with new tungsten particles according to the intake volume of the tungsten hexafluoride mixture.

[0036] As a preferred embodiment, the driving wheel 13 can drive the driven wheel 14 to perform deceleration motion.

[0037] In this embodiment, the sub-horizontal tube body 61 and the horizontal tube body 63 are both divided into at least two sections, and an elastic tube 17 is connected between two adjacent sections of the sub-horizontal tube body 61 and between two adjacent sections of the horizontal tube body 63.

[0038] In addition, a knocking wheel (not shown in the figure) corresponding to the elastic tube 17 is rotatably provided in the reduction tower 3 .

[0039] Among them, the elastic tube is a soft and flexible tubular structure made of elastic material. It consists of an inner tube wall, a reinforcement layer (such as fiber braiding or metal wire) and an outer protective layer.

[0040] The inner tube wall is the inner wall of the elastic tube that contacts the medium being transported. Therefore, it is necessary to select a material with corrosion resistance, high temperature resistance, and pressure resistance. Different inner tube materials can be selected according to the type of medium and temperature requirements.

[0041] To increase the strength and pressure resistance of elastic tubes, reinforcement layers are often added to the inner tube wall. These layers can take the form of fiber braiding, spirally wound steel wire, or wire mesh. These reinforcements resist internal pressure and prevent deformation or rupture of the elastic tube.

[0042] To protect the flexible tube from external physical or chemical damage, an outer protective layer is often added to the outer layer of the reinforcement. This layer is usually made of wear-resistant and corrosion-resistant materials, and the outer protective layer provides additional strength and durability.

[0043] The elastic tube has good flexibility and bending performance, can adapt to various complex layout and installation requirements, and can be bent to a certain angle without affecting the conveying of the material.

[0044] By configuring the knocking wheel, the elastic tube 17 can be knocked, thereby reducing the occurrence of tungsten particle blockage in the filling tube 6.

[0045] The above is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with this technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solutions and inventive concepts of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. An electronic grade tungsten hexafluoride purification device, characterized by: include: A heating tube (1) is used to heat the tungsten hexafluoride mixed gas to 150° C.-400° C.; A buffer tank (2), one end of which is connected to the heating pipe (1) and the other end of which is provided with a connecting pipe (4); a reduction tower (3), the bottom of which is connected to the connecting pipe (4) and the top of which is provided with an exhaust pipe (5); and A stuffing tube (6) is provided in the reduction tower (3) and has a breathable structure so that the tungsten hexafluoride mixed gas can only pass through the stuffing tube (6) and be discharged from the exhaust pipe (5). The stuffing tube (6) is filled with tungsten particles. The stuffing tube (6) can automatically discharge the used tungsten particles and fill them with new tungsten particles according to the intake volume of the tungsten hexafluoride mixed gas; The filling tube (6) is serpentine and comprises a plurality of nearly horizontal tubes (61) and curved tubes (62) alternately connected in series. The nearly horizontal tube (61) at the bottom is connected to the horizontal tube (63) by a curved tube, wherein the angle between the nearly horizontal tube (61) and the horizontal plane is 3°-12°. The sub-horizontal tube body (61) and the horizontal tube body (63) are both divided into at least two sections, and an elastic tube (17) is connected between two adjacent sections of the sub-horizontal tube body (61) and between two adjacent sections of the horizontal tube body (63); A screw auger (16) is rotatably provided in both the near-horizontal tube body (61) and the horizontal tube body (63). A power bin is provided on the inner side of the reduction tower (3). The shaft of the screw auger extends into the power bin and is fixed with a driven wheel (14). A wind wheel (11) close to the air outlet of the connecting pipe (4) is also rotatably provided in the reduction tower (3). The wind wheel (11) is driven by the gas discharged from the connecting pipe (4). A rotating shaft (12) is fixed on the wind wheel (11). The rotating shaft (12) extends into the power bin and is fixed with a driving wheel (13). The driving wheel (13) is connected to a plurality of driven wheels (14) by a chain (15).

2. The electronic grade tungsten hexafluoride purification device according to claim 1, characterized in that: The upper opening of the stuffing tube (6) is connected to the stuffing supply bin (7) via a feed pipe (20), and the lower opening of the stuffing tube (6) is connected to the collecting bin (8) via a discharge pipe (19). The bottom of the collecting bin (8) is provided with an interception membrane (10) for intercepting solid particles. The bottom of the collecting bin (8) is connected to the reduction tower (3) via a reflux pipe (9).

3. The electronic grade tungsten hexafluoride purification device according to claim 1, characterized in that: The length of the auger (16) is 1 / 6 to 1 / 3 of the length of the near-horizontal tube (61) or the horizontal tube (63).

4. The electronic grade tungsten hexafluoride purification device according to claim 1, characterized in that: The driving wheel (13) can drive the driven wheel (14) to perform deceleration motion.

5. The electronic grade tungsten hexafluoride purification device according to claim 1, characterized in that: A knocking wheel corresponding to the elastic tube (17) is rotatably provided in the reduction tower (3).

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