A high-purity electronic-grade hydrogen bromide metal ion impurity control device and control method
By introducing adsorption devices, bag filters, and distillation units into the hydrogen bromide production process, and by setting spike structures in key areas, the problem of removing metal impurities from high-purity electronic-grade hydrogen bromide has been solved, achieving efficient and low-cost removal of metal particles and improving product purity.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SUZHOU JINHONG GAS CO LTD
- Filing Date
- 2024-01-08
- Publication Date
- 2026-06-05
AI Technical Summary
In existing technologies, it is difficult to effectively remove metal impurities, especially solid metal particles, during the preparation of high-purity electronic-grade hydrogen bromide, resulting in substandard product purity and affecting the quality of semiconductor manufacturing.
A high-purity electronic-grade hydrogen bromide metal ion impurity control device is adopted, including an adsorption device, a bag filter, and a distillation device. By designing the first and second impurity removal mechanisms on the adsorption column and the distillation column, and setting the thorn structure on the flow channel of the bag filter, the efficient removal of gaseous and liquid phase metal impurities is achieved.
It significantly improves the removal efficiency and effect of metal particles, ensures the production of high-purity hydrogen bromide to meet the needs of semiconductor manufacturing, and has the advantages of simple process, low cost and good environmental performance.
Smart Images
Figure CN117815823B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of high-purity hydrogen bromide production technology, specifically to a device and method for controlling metal ion impurities in high-purity electronic-grade hydrogen bromide. Background Technology
[0002] Hydrogen bromide, also known as hydrobromic acid (HBr), is a binary compound with strong corrosive properties. It can react with some active metal powders and is a basic raw material for manufacturing various inorganic bromides and certain alkyl bromides. In semiconductor manufacturing, electronic specialty gases are crucial throughout the entire semiconductor process. Plasma etching technology using hydrogen bromide as a specialty electronic gas enables highly selective polysilicon etching in 8-inch and 12-inch chip manufacturing processes, making it one of the core gases in advanced chip manufacturing. Therefore, high-purity electronic-grade hydrogen bromide has become a core product for evaluating semiconductor technology. In existing technologies, plasma hydrogen bromide etching technology can precisely control etching depth and perpendicularity without damaging the ozone layer or producing greenhouse gases, making it a good alternative to fluorocarbon etching gases. With the development of the semiconductor industry, higher requirements have been placed on the purity of electronic-grade hydrogen bromide used in the main etching processes. During the process, contamination by impurities can easily damage the circuitry within the wafer, causing integrated circuit failure and affecting the formation of geometric features. Therefore, high-purity hydrogen bromide gas is required.
[0003] High-purity electronic-grade hydrogen bromide has become a core gas for etching phosphorus-doped N-type polycrystalline silicon, phosphorus-doped monocrystalline silicon, and two-dimensional semiconductors due to its high etching selectivity and precise control over etching morphology and angle. Therefore, developing high-purity hydrogen bromide is of significant practical importance to the future development of my country's electronics industry. The most challenging aspect of hydrogen bromide gas purification is removing moisture. High moisture content is highly corrosive to metal materials and also generates metal ion impurities, severely impacting product purity and applications. This has become a technological bottleneck in the purification of high-purity electronic-grade hydrogen bromide.
[0004] In the prior art, patent 202210500438.0 provides a method for purifying electronic-grade hydrogen bromide, patent 202110681411.1 provides a method for preparing high-purity hydrogen bromide, patent 202310298595.2 discloses a distillation apparatus and its production process for hydrogen bromide gas, and patent 202122409841.6 provides an apparatus for producing high-purity hydrogen bromide using ammonia heat pump distillation. Based on the above patents and production practice, it can be found that the existing disclosed technologies are mainly limited to the combination of distillation and adsorption processes, on which trace amounts of water and light and heavy component impurities in hydrogen bromide are removed. In production practice, the levels of metallic impurities are seriously exceeded, resulting in a discrepancy with expectations. The main reasons are:
[0005] There is a lack of technology for removing metal impurities. This is because hydrogen bromide is extremely corrosive to water, and existing processes mainly focus on distillation and adsorption to remove water and gaseous impurities, neglecting the removal of metal impurities.
[0006] Incomplete moisture removal. Because hydrogen bromide readily absorbs water, some areas are not completely dehydrated, leading to the formation of metallic impurities.
[0007] Therefore, the rational design and development of a high-purity electronic-grade hydrogen bromide metal ion impurity control device and method to effectively remove metal ion impurities to meet semiconductor requirements is obviously of practical significance. Summary of the Invention
[0008] The purpose of this invention is to provide a high-purity electronic-grade hydrogen bromide metal ion impurity control device and method, which removes metal ion impurities by adding a bag filter and improving the structure of the adsorption device and distillation device.
[0009] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a high-purity electronic-grade hydrogen bromide metal ion impurity control device, comprising an adsorption device, a bag filter, and a distillation device, wherein the bag filter is located between the adsorption device and the distillation device; the adsorption device includes at least one adsorption column, the distillation device includes at least one distillation column, a first product outlet is provided at the upper end of the adsorption column and the top of the distillation column, a first impurity removal mechanism is provided at each of the first product outlets for removing gaseous metal impurities, and a second impurity removal mechanism is provided at the bottom of the distillation column for removing liquid-phase metal impurities; the bag filter includes a flow channel, a frame, and a dust collection bag, wherein the dust collection bag is fitted outside the frame and disposed inside the flow channel, the flow channel extends from the outside of the dust collection bag to the inside of the dust collection bag, and a third impurity removal mechanism is provided on the flow channel.
[0010] In the above text, the applicant found through extensive experimental research that the metal impurities are composed of solid metal particles, including solid metal bromides or oxides, such as iron oxide, iron bromide, nickel oxide, nickel bromide, chromium oxide, and chromium bromide, rather than metal cations dissolved in the liquid phase.
[0011] Preferably, the first impurity removal mechanism includes a first cover and a second cover. The first cover is located outside the second cover. The second cover covers the first product outlet and has a gap between it and the first product outlet. Both ends of the first cover are connected to an adsorption column or a distillation column. The second product outlet is located in the middle of the first cover.
[0012] Preferably, the first cover and the second cover are concentric arc-shaped covers, the two ends of the first cover extend to connect with the outer shell of the adsorption column, the two ends of the second cover extend to cover the first product outlet, and the two ends of the second cover are provided with a gap between the upper end of the adsorption column and the top of the distillation column.
[0013] In the above text, when hydrogen bromide enters the first impurity removal mechanism, it enters from the first product outlet, is diverted by the second shroud, and flows down into the flow channel formed by the first and second shrouds, and finally flows out from the second product outlet in the middle of the second shroud.
[0014] Preferably, in the first impurity removal mechanism, the flow rate of hydrogen bromide is 2-10 kg / h.
[0015] Preferably, the adsorption column is provided with a first protrusion structure on the side of the upper end of the adsorption column near the first cover, the top of the distillation column near the first cover, the inner side of the first cover, and the inner side of the second cover.
[0016] Preferably, the first spike structure includes a plurality of upward-curving spikes to remove metal impurity particles in the gas phase. The spikes are evenly distributed on the side of the adsorption column near the first cover, the side of the distillation column top near the first cover, the inner side of the first cover, and the inner side of the second cover. Each spike has the same length and angle, and the spacing between each spike is the same. The upward angle of the spikes in the first spike structure is 15°~75°, more preferably 30°~60°, and most preferably 45°~60°. The ratio of the gap between the spikes to the spike length (D / R) in the first spike structure is 1:5~10, more preferably 1:8~10.
[0017] Preferably, the length of the spikes in the first spike structure is 20-50 mm.
[0018] As mentioned above, hydrogen bromide readily forms hydrates with water, and metal oxides react with these hydrates, causing changes in the particle size of the metal ions. Therefore, to effectively remove metal impurities at the top of the adsorption column and the top of the distillation column, the flow rate of hydrogen bromide gas must be controlled at 2-10 kg / h to ensure sufficient settling time for the metal particles. During the Stokes motion of the metal particles, a slight disturbance from the airflow is required. If the gaps between the spikes are too large, the disturbance will be insufficient, making it difficult to trap the metal particles. If the gaps are too small, the disturbance will be too intense, disturbing the boundary layer of the spikes in the first spike structure and carrying away the metal particles, thus reducing the impurity removal effect. Therefore, it is necessary to control the length and spacing of the spikes in the first spike structure.
[0019] Preferably, the second impurity removal mechanism includes a built-in vessel disposed within the distillation column, and the built-in vessel is provided with a second spike structure.
[0020] Preferably, the second spike structure includes a plurality of upward-curving spikes to intercept metal particles. The spikes are evenly distributed on the side of the built-in vessel near the top of the distillation column, and each spike has the same length and angle, and the spacing between each spike is the same. The upward angle of the spikes in the second spike structure is 15°~75°, more preferably 30°~60°, and most preferably 45°~60°. The ratio of the gap between the spikes to the spike length D / R in the second spike structure is 1:5~10, more preferably 1:8~10.
[0021] Preferably, the length of the spikes in the second spike structure is 20-50 mm.
[0022] In the above text, the main functions of the spikes in the first and second spike structures are:
[0023] a) The intermittent splinters trap metal impurity particles, forming a trapping space. A larger intermittent spacing can provide more space for metal ions to be trapped.
[0024] b) The spikes enhance gas turbulence. Solid particles are subjected to drag, while gas is subjected to resistance. The density difference between the two and the difference in flow velocity after turbulence enhance the flow of gas, which can promote the separation of metal particles from the gas. Therefore, the spikes cannot be too short and must have a certain length.
[0025] c) A boundary layer will form at the edges of spikes and intermittents. The laminar sublayer of the boundary layer near the wall is mainly composed of metal particles, which are in a stagnant state. The intermittents should not be too short to prevent the airflow from blowing away the trapped metal particles.
[0026] d) The upward angle of the spikes is to catch particles entering the intermittent and prevent metal particles from falling to the bottom of the main equipment.
[0027] Preferably, a baffle 43 is provided at the bottom of the distillation column. The baffle is located above the built-in vessel. One end of the baffle is connected to the wall of the distillation column, and the other end is inclined downward to extend into the built-in vessel, but there is a gap between the baffle and the built-in vessel.
[0028] Preferably, the built-in vessel is an arc-shaped vessel, and the radius of the built-in vessel is 1 / 2 to 3 / 4 of the radius of the distillation column. The distillation column is equipped with a bundle tube, and the distance between the built-in vessel and the bundle tube is 50mm to 500mm. The bottom of the distillation column is provided with a third product outlet, and there is a distance between the third product outlet and the bottom of the distillation column, and the distance is 50 to 300mm.
[0029] In the above text, hydrogen bromide is converted into liquid hydrogen bromide after being distilled in the distillation column. The liquid hydrogen bromide flows out from the bundle tube, flows into the built-in vessel in the second impurity removal mechanism through the downward-sloping baffle, overflows into the distillation column through the built-in vessel, and flows out through the third product outlet at the bottom of the distillation column.
[0030] As mentioned above, the third product outlet is not located at the bottom of the distillation column to prevent metal particles from leaving with the liquid hydrogen bromide. The distance between the third product outlet and the bottom of the column is crucial. Specifically, if the distance between the third product outlet and the bottom is too large, a large amount of heavy hydrogen bromide impurities will remain, especially water-bound hydrogen bromide hydrates and metal bromide hydrates, which will severely corrode the bottom of the equipment, posing a safety hazard. Even with bottom valve discharge, a large amount of hydrogen bromide product will be wasted. If the distance is too short, metal bromide hydrates will enter the product storage tank with the fluid. Therefore, the distance between the third product outlet and the bottom of the distillation column needs to be controlled at 50-300 mm, more preferably 100-200 mm.
[0031] Preferably, the third impurity removal mechanism includes a third spike structure disposed on the flow channel. The third spike structure, the first spike structure, and the second spike structure are all upward-curving spikes. The upward angle of the spikes is 15° to 75°, and the ratio of the gap between the spikes to the length of the spikes, D / R, is 1:5 to 10.
[0032] Preferably, the third spike structure includes a plurality of spikes evenly distributed on the flow channel, wherein the spacing between the spikes is the same, the length of each spike is the same, and the upward angle of each spike is the same; the upward angle of the spikes in the third spike structure is 15°~75°, more preferably 30°~60°, and most preferably 45°~60°; the ratio of the gap between the spikes to the length of the spikes in the third spike structure, D / R, is 1:5~10, more preferably 1:8~10.
[0033] Preferably, the length of the spikes in the third spike structure is 20-50 mm.
[0034] Preferably, the dust bag has a mesh size of 2000-5000, and the frame has several channels with a diameter of 10-40mm.
[0035] As mentioned above, hydrogen bromide is highly polar and, upon absorbing water, forms hydrates with metal bromide ions. The metal particles form a core with high surface energy, easily absorbing metal bromide hydrates. This leads to a colloidal state during the gas phase process. Extensive production experience has shown that the size and volume of these colloidal metal impurity particles range from 6 to 10 micrometers. Controlling the mesh size of the filter bag to 2000-5000 mesh (corresponding to 2.6-6.5 micrometers) effectively traps metal particles, a feat unattainable with conventional filter bags. The upward-curving spikes arranged within the hydrogen bromide flow channel serve two purposes: First, they enhance the flow state and promote turbulence, allowing metal particles to be smoothly intercepted without excessively disturbing the boundary layer, thus carrying away the intercepted particles. This is similar to the function of spikes (first and second impurity removal mechanisms) in adsorption columns and distillation towers. The second purpose is the most important. Because hydrogen bromide is a low-pressure liquefied gas, excessive resistance would cause the flow channel pressure to become too high, leading to liquefaction. Baghouse dust collectors are only effective for the gas phase and cannot separate particulate matter from liquid hydrogen bromide. Therefore, to ensure sufficient mass transfer driving pressure for metal particle interception without excessive resistance, channels are also provided inside the baghouse dust collector's frame, and the spikes are spaced sufficiently to prevent excessive resistance.
[0036] This application also claims a method for controlling high-purity electronic-grade hydrogen bromide metal ion impurities, which uses the high-purity electronic-grade hydrogen bromide metal ion impurity control device described above. Hydrogen bromide is passed sequentially through an adsorption device, a bag filter, and a distillation device, and then flows into a filling system connected to the high-purity electronic-grade hydrogen bromide metal ion impurity control device.
[0037] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:
[0038] 1. This invention increases the removal efficiency and effect of metal particles by adding a metal ion dust collector to an existing process system and designing its structure to enable solid-liquid separation of liquids to retain metal particles.
[0039] 2. This invention designs the structure of the adsorption equipment and the distillation equipment, and designs a first impurity removal mechanism at the upper end of the adsorption column and the distillation column to remove gaseous metal impurities, and designs a second impurity removal mechanism at the bottom of the distillation column to remove liquid metal impurities, thereby increasing the removal efficiency and effect of metal particles.
[0040] 3. This invention, from a structural design perspective, aims to achieve efficient removal of impurities from hydrogen bromide. The designed structure is simple, the removal method is simple and feasible, the cost is low, and it is more environmentally friendly, thus solving the technical defects of existing technologies, such as complex processes and a large number of impurities. Attached Figure Description
[0041] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, some of the drawings in the following description are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0042] Figure 1 This is a schematic diagram of the first impurity removal mechanism in Embodiment 1 of the present invention;
[0043] Figure 2 This is a schematic diagram of the second impurity removal mechanism in Embodiment 1 of the present invention;
[0044] Figure 3 This is a schematic diagram of the structure of the bag filter in Embodiment 1 of the present invention;
[0045] Figure 4 This is a schematic diagram of the overall structure of Embodiment 2 of the present invention.
[0046] Among them, 1. Baghouse dust collector; 2. First product outlet; 3. First impurity removal mechanism; 4. Second impurity removal mechanism; 5. Third impurity removal mechanism; 6. Second product outlet;
[0047] 11. Flow channel; 12. Keel frame; 13. Dust collection bag; 14. Channel; 15. Third spike structure;
[0048] 31. First cover; 32. Second cover; 33. First spike structure;
[0049] 41. Internal vessel body; 42. Second spike structure; 43. Third product outlet; 44. Baffle. Detailed Implementation
[0050] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0051] Example 1
[0052] like Figure 1-3 As shown, this embodiment relates to a high-purity electronic-grade hydrogen bromide metal ion impurity control device:
[0053] A high-purity electronic-grade hydrogen bromide metal ion impurity control device includes an adsorption device, a bag filter 1, and a distillation device, wherein the bag filter is located between the adsorption device and the distillation device; the adsorption device includes at least one adsorption column, and the distillation device includes at least one distillation column, wherein a first product outlet 2 is provided at the upper end of the adsorption column and the top of the distillation column, and a first impurity removal mechanism 3 is provided at the first product outlet to remove gaseous metal impurities; a second impurity removal mechanism 4 is provided at the bottom of the distillation column to remove liquid-phase metal impurities; the bag filter includes a flow channel 11, a frame 12, and a dust collection bag 13, wherein the dust collection bag is fitted outside the frame and disposed inside the flow channel, the flow channel extends from the outside of the dust collection bag to the inside of the dust collection bag, and a third impurity removal mechanism 5 is provided on the flow channel.
[0054] In the above text, the applicant found through extensive experimental research that the metal impurities are composed of solid metal particles, including solid metal bromides or oxides, such as iron oxide, iron bromide, nickel oxide, nickel bromide, chromium oxide, and chromium bromide, rather than metal cations dissolved in the liquid phase.
[0055] Preferably, the first impurity removal mechanism includes a first cover 31 and a second cover 32. The first cover is located outside the second cover, and the second cover is placed over the first product outlet and has a gap between it and the first product outlet. Both ends of the first cover are connected to an adsorption column or a distillation column, and the middle part of the first cover has a second product outlet 6.
[0056] Preferably, the first cover and the second cover are concentric arc-shaped covers, the two ends of the first cover extend to connect with the outer shell of the adsorption column, the two ends of the second cover extend to cover the first product outlet, and the two ends of the second cover are provided with a gap between the upper end of the adsorption column and the top of the distillation column.
[0057] In the above text, when hydrogen bromide enters the first impurity removal mechanism, it enters from the first product outlet, is diverted by the second shroud, and flows down into the flow channel formed by the first and second shrouds, and finally flows out from the second product outlet in the middle of the second shroud.
[0058] Preferably, in the first impurity removal mechanism, the flow rate of hydrogen bromide is 2-10 kg / h.
[0059] Preferably, a first spike structure 33 is provided on the side of the adsorption column near the first cover, the side of the distillation column top near the first cover, the inner side of the first cover, and the inner side of the second cover.
[0060] Preferably, the first spike structure includes a plurality of upward-curving spikes to remove metal impurity particles in the gas phase. The spikes are evenly distributed on the side of the adsorption column near the first cover, the side of the distillation column top near the first cover, the inner side of the first cover, and the inner side of the second cover. Each spike has the same length and angle, and the spacing between each spike is the same. The upward angle of the spikes in the first spike structure is 15°~75°, more preferably 30°~60°, and most preferably 45°~60°. The ratio of the gap between the spikes to the spike length (D / R) in the first spike structure is 1:5~10, more preferably 1:8~10.
[0061] Preferably, the length of the spikes in the first spike structure is 20-50 mm.
[0062] Preferably, the second product outlet is also evenly distributed with spikes.
[0063] As mentioned above, hydrogen bromide readily forms hydrates with water, and metal oxides react with these hydrates, causing changes in the particle size of the metal ions. Therefore, to effectively remove metal impurities at the top of the adsorption column and the top of the distillation column, the flow rate of hydrogen bromide gas must be controlled at 2-10 kg / h to ensure sufficient settling time for the metal particles. During the Stokes motion of the metal particles, a slight disturbance from the airflow is required. If the gaps between the spikes are too large, the disturbance will be insufficient, making it difficult to trap the metal particles. If the gaps are too small, the disturbance will be too intense, disturbing the boundary layer of the spikes in the first spike structure and carrying away the metal particles, thus reducing the impurity removal effect. Therefore, it is necessary to control the length and spacing of the spikes in the first spike structure.
[0064] Preferably, the second impurity removal mechanism includes an internal vessel 41 disposed within the distillation column, and the internal vessel is provided with a second spike structure 42.
[0065] Preferably, a baffle 43 is provided at the bottom of the distillation column. The baffle is located above the built-in vessel. One end of the baffle is connected to the wall of the distillation column, and the other end is inclined downward to extend into the built-in vessel, but there is a gap between the baffle and the built-in vessel.
[0066] Preferably, the second spike structure includes a plurality of upward-curving spikes to intercept metal particles. The spikes are evenly distributed on the side of the built-in vessel near the top of the distillation column, and each spike has the same length and angle, and the spacing between each spike is the same. The upward angle of the spikes in the second spike structure is 15°~75°, more preferably 30°~60°, and most preferably 45°~60°. The ratio of the gap between the spikes to the spike length D / R in the second spike structure is 1:5~10, more preferably 1:8~10.
[0067] Preferably, the length of the spikes in the second spike structure is 20-50 mm.
[0068] Preferably, the built-in vessel is an arc-shaped vessel, and the radius of the built-in vessel is 1 / 2 to 3 / 4 of the radius of the distillation column. The distillation column is provided with a bundle tube, and the distance between the built-in vessel and the bundle tube is 50mm to 500mm. The bottom of the distillation column is provided with a third product outlet 43, and there is a distance between the third product outlet and the bottom of the distillation column, and the distance is 50 to 300mm.
[0069] In the above text, hydrogen bromide is converted into liquid hydrogen bromide after being distilled in the distillation column. The liquid hydrogen bromide flows out from the bundle tube, flows into the built-in vessel in the second impurity removal mechanism through the downward-sloping baffle, overflows into the distillation column through the built-in vessel, and flows out through the third product outlet at the bottom of the distillation column.
[0070] As mentioned above, the third product outlet is not located at the bottom of the distillation column to prevent metal particles from leaving with the liquid hydrogen bromide. The distance between the third product outlet and the bottom of the column is crucial. Specifically, if the distance between the third product outlet and the bottom is too large, a large amount of heavy hydrogen bromide impurities will remain, especially water-bound hydrogen bromide hydrates and metal bromide hydrates, which will severely corrode the bottom of the equipment, posing a safety hazard. Even with bottom valve discharge, a large amount of hydrogen bromide product will be wasted. If the distance is too short, metal bromide hydrates will enter the product storage tank with the fluid. Therefore, the distance between the third product outlet and the bottom of the distillation column needs to be controlled at 50-300 mm, more preferably 100-200 mm.
[0071] Preferably, the third impurity removal mechanism includes a third spike structure 15 disposed on the flow channel. The third spike structure, the first spike structure, and the second spike structure are all upward-curving spikes. The upward angle of the spikes is 15° to 75°, and the ratio of the gap between the spikes to the length of the spikes, D / R, is 1:5 to 10.
[0072] Preferably, the third spike structure includes a plurality of spikes evenly distributed on the flow channel, wherein the spacing between the spikes is the same, the length of each spike is the same, and the upward angle of each spike is the same; the upward angle of the spikes in the third spike structure is 15°~75°, more preferably 30°~60°, and most preferably 45°~60°; the ratio of the gap between the spikes to the length of the spikes in the third spike structure, D / R, is 1:5~10, more preferably 1:8~10.
[0073] Preferably, the length of the spikes in the third spike structure is 20-50 mm.
[0074] Preferably, the dust bag has a mesh size of 2000-5000 mesh, and the keel frame is provided with a plurality of channels 14, the diameter of which is 10-40mm.
[0075] As mentioned above, hydrogen bromide is highly polar and, upon absorbing water, forms hydrates with metal bromide ions. The metal particles form a core with high surface energy, easily absorbing metal bromide hydrates. This leads to a colloidal state during the gas phase process. Extensive production experience has shown that the size and volume of these colloidal metal impurity particles range from 6 to 10 micrometers. Controlling the mesh size of the filter bag to 2000-5000 mesh (corresponding to 2.6-6.5 micrometers) effectively traps metal particles, a feat unattainable with conventional filter bags. The upward-curving spikes arranged within the hydrogen bromide flow channel serve two purposes: First, they enhance the flow state and promote turbulence, allowing metal particles to be smoothly intercepted without excessively disturbing the boundary layer, thus carrying away the intercepted particles. This is similar to the function of spikes (first and second impurity removal mechanisms) in adsorption columns and distillation towers. The second purpose is the most important. Because hydrogen bromide is a low-pressure liquefied gas, excessive resistance would cause the flow channel pressure to become too high, leading to liquefaction. Baghouse dust collectors are only effective for the gas phase and cannot separate particulate matter from liquid hydrogen bromide. Therefore, to ensure sufficient mass transfer driving pressure for metal particle interception without excessive resistance, channels are also provided inside the baghouse dust collector's frame, and the spikes are spaced sufficiently to prevent excessive resistance.
[0076] Example 2
[0077] This embodiment is based on the first embodiment described above, and the similarities with the first embodiment will not be repeated.
[0078] like Figure 4 As shown, this embodiment relates to a high-purity electronic-grade hydrogen bromide metal ion impurity control device. The adsorption device includes an adsorption column A and an adsorption column B, with the adsorption column B located between the adsorption column A and the bag filter. The distillation device includes a distillation column A and a distillation column B, with the distillation column A located between the distillation column B and the bag filter.
[0079] Preferably, distillation column A is a heavy-weight removal distillation column, and distillation column B is a light-weight removal distillation column.
[0080] In this embodiment, the first product outlet of adsorption column A is connected to the inlet of adsorption column B, and the first product outlet of adsorption column B is connected to the inlet of a bag filter. Both adsorption column A and adsorption column B have a first impurity removal mechanism at their first product outlets. The outlet of the bag filter is connected to the inlet of distillation column A, and the first product outlet at the top of distillation column A is connected to the inlet of distillation column B. The first product outlet at the top of distillation column A has a first impurity removal mechanism. The bottom of distillation column A is used to discharge tail gas from distillation column A. The top outlet of distillation column B is used to discharge tail gas from distillation column B, and the bottom of distillation column B has a second impurity removal mechanism. The bottom of distillation column B is connected to a filling system.
[0081] Example 3
[0082] This embodiment is based on the above embodiment one.
[0083] This embodiment relates to a method for controlling high-purity electronic-grade hydrogen bromide metal ion impurities. The method uses the high-purity electronic-grade hydrogen bromide metal ion impurity control device described above. Hydrogen bromide is passed sequentially through an adsorption device, a bag filter, and a distillation device, and then flows into a filling system connected to the high-purity electronic-grade hydrogen bromide metal ion impurity control device.
[0084] Example 4
[0085] This embodiment is based on any one of the above embodiments one to three, and the similarities with the above embodiments will not be repeated.
[0086] In this embodiment, the upward angle of the spikes in the first spike structure, the second spike structure, and the third spike structure is 45°, and the ratio of the gap between the spikes to the length of the spikes (D / R) is 1:4.
[0087] Example 5
[0088] This embodiment is based on any one of the above embodiments one to three, and the similarities with the above embodiments will not be repeated.
[0089] In this embodiment, the upward angle of the spikes in the first spike structure, the second spike structure, and the third spike structure is 45°, and the ratio of the gap between the spikes to the length of the spikes (D / R) is 1:9.
[0090] Example 6
[0091] This embodiment is based on any one of the above embodiments one to three, and the similarities with the above embodiments will not be repeated.
[0092] In this embodiment, the upward angle of the spikes in the first spike structure, the second spike structure, and the third spike structure is 45°, and the ratio of the gap between the spikes to the length of the spikes (D / R) is 1:12.
[0093] Example 7
[0094] This embodiment is based on any one of the above embodiments one to three, and the similarities with the above embodiments will not be repeated.
[0095] In this embodiment, the upward angle of the spikes in the first spike structure, the second spike structure, and the third spike structure is 60°, and the ratio of the gap between the spikes to the length of the spikes (D / R) is 1:9.
[0096] Example 8
[0097] This embodiment is based on any one of the above embodiments one to three, and the similarities with the above embodiments will not be repeated.
[0098] In this embodiment, the upward angle of the spikes in the first spike structure, the second spike structure, and the third spike structure is 30°, and the ratio of the gap between the spikes to the length of the spikes (D / R) is 1:9.
[0099] Example 9
[0100] This embodiment is based on any one of the above embodiments one to three, and the similarities with the above embodiments will not be repeated.
[0101] In this embodiment, the upward angle of the spikes in the first spike structure, the second spike structure, and the third spike structure is 10°, and the ratio of the gap between the spikes to the length of the spikes (D / R) is 1:9.
[0102] The hydrogen bromide to be tested was introduced into Examples 4 and 5 above. After passing through an adsorption device, a bag filter, and a distillation device in sequence, the hydrogen bromide flowed into the detection system. The concentration of metal ions in the hydrogen bromide after the impurity removal process was detected, and the detection results are shown in Table 1 below.
[0103] Table 1
[0104]
[0105] As can be clearly seen from the table above, choosing the appropriate angle, interval, and length of the spikes is a comprehensive result.
[0106] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A high-purity electronic-grade hydrogen bromide metal ion impurity control device, characterized in that, The device includes an adsorption unit, a bag filter, and a distillation unit, with the bag filter located between the adsorption unit and the distillation unit. The adsorption unit includes at least one adsorption column, and the distillation unit includes at least one distillation column. A first product outlet is provided at the upper end of the adsorption column and at the top of the distillation column. A first impurity removal mechanism is provided at each of the first product outlets to remove gaseous metal impurities. A second impurity removal mechanism is provided at the bottom of the distillation column to remove liquid-phase metal impurities. The bag filter includes a flow channel, a frame, and a dust collection bag. The dust collection bag is fitted outside the frame and located inside the flow channel, which extends from the outside of the dust collection bag to its interior. A third impurity removal mechanism is provided on the flow channel. The first impurity removal mechanism includes a first cover and a second cover. The first cover is located outside the second cover. The second cover covers the first product outlet and has a gap between it and the first product outlet. Both ends of the first cover are connected to an adsorption column or a distillation column. The second product outlet is located in the middle of the first cover. The adsorption column is provided with a first protrusion structure on the side of the upper end of the adsorption column near the first cover, the top of the distillation column is provided with a first cover, the inner side of the first cover and the inner side of the second cover; The second impurity removal mechanism includes an internal vessel set inside a distillation column, the internal vessel being provided with a second protruding structure; a baffle is also provided at the bottom of the distillation column, the baffle being located above the internal vessel, one end of the baffle being connected to the distillation column wall, and the other end being inclined downward to extend into the internal vessel but with a gap between it and the internal vessel; The third impurity removal mechanism includes a third spike structure disposed on the flow channel, and the dragon skeleton is provided with a number of channels; The third, first, and second spike structures are all upward-curving spikes, with an upward angle of 15° to 75°. The ratio of the gap between the spikes to the spike length (D / R) is 1:5 to 10.
2. The high-purity electronic-grade hydrogen bromide metal ion impurity control device according to claim 1, characterized in that, The first cover and the second cover are concentric arc-shaped covers. The two ends of the first cover extend to connect with the outer shell of the adsorption column, and the two ends of the second cover extend to cover the first product outlet. The two ends of the second cover are provided with a gap between them and the upper end of the adsorption column and the top of the distillation column.
3. The high-purity electronic-grade hydrogen bromide metal ion impurity control device according to claim 1, characterized in that, In the first impurity removal mechanism, the flow rate of hydrogen bromide is 2-10 kg / h.
4. The high-purity electronic-grade hydrogen bromide metal ion impurity control device according to claim 1, characterized in that, The built-in vessel is an arc-shaped vessel with a radius of 1 / 2 to 3 / 4 of the radius of the distillation column. The distillation column is equipped with a bundle tube, and the distance between the built-in vessel and the bundle tube is 50mm to 500mm. The bottom of the distillation column is equipped with a third product outlet, and there is a distance of 50 to 300mm between the third product outlet and the bottom of the distillation column.
5. The high-purity electronic-grade hydrogen bromide metal ion impurity control device according to claim 1, characterized in that, The dust collector bag has a mesh size of 2000-5000 mesh, and the diameter of the pores is 10-40mm.
6. A method for controlling high-purity electronic-grade hydrogen bromide metal ion impurities, characterized in that, Using the high-purity electronic-grade hydrogen bromide metal ion impurity control device according to any one of claims 1-5, hydrogen bromide is sequentially passed through an adsorption device, a bag filter, and a distillation device, and then flows into a filling system connected to the high-purity electronic-grade hydrogen bromide metal ion impurity control device.