Adsorption device, hydrogen bromide purification system and purification method

Abstract

The invention discloses an adsorption device, a hydrogen bromide purification system and a purification method.The adsorption device of the hydrogen bromide purification system is characterized by comprising a tower body, a plurality of first sieve plates and a plurality of second sieve plates, the first sieve plates and the second sieve plates are installed in the tower body, and all the first sieve plates and all the second sieve plates are sequentially distributed at intervals in the gas flowing direction; an acid-resistant aluminum oxide adsorbent is loaded on the first sieve plate, a hydrogen type zeolite molecular sieve is loaded on the second sieve plate, and the first tower body is provided with a feed port and a discharge port through which a hydrogen bromide raw material enters. According to the adsorption device of the hydrogen bromide purification system, by arranging the two adsorbents and selecting the adsorbents, the water content of hydrogen bromide components before the hydrogen bromide components enter the rectifying tower can be lower than 1 ppm, namely, the water absorption effect meets the requirement of the purification process of hydrogen bromide, and the cost of the adsorbents can be reduced.

Description

Technical Field

[0001] This invention belongs to the field of hydrogen bromide purification technology, specifically relating to an adsorption device, a hydrogen bromide purification system, and a purification method. Background Technology

[0002] The purification process of semiconductor-grade high-purity hydrogen bromide (HBr) requires extremely stringent control over moisture and metallic impurities; even trace amounts can severely impact the yield and performance of integrated circuits. Current purification processes based on adsorption methods face significant challenges.

[0003] For water removal in the purification process of hydrogen bromide, existing technologies mostly employ specialized acid-resistant molecular sieves such as Sorbead DW. While these are reliable, their high cost limits their economic viability for large-scale applications. Other adsorbents, although cost-effective, may suffer from problems such as insufficient water removal or excessive heat release during water absorption leading to adsorbent pulverization and failure.

[0004] The information disclosed in this background section is intended only to enhance the understanding of the overall background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0005] The purpose of this invention is to provide an adsorption device, a hydrogen bromide purification system and purification method, which have the advantages of excellent water removal performance and low cost.

[0006] To achieve the above objectives, a specific embodiment of the present invention provides the following technical solution: an adsorption device for a hydrogen bromide purification system includes a tower body, a plurality of first sieve plates and a plurality of second sieve plates installed in the tower body, all the first sieve plates and second sieve plates being distributed sequentially at intervals along the gas flow direction, the first sieve plates carrying acid-resistant alumina adsorbent, the second sieve plates carrying hydrogen-type zeolite molecular sieves, and the first tower body having an inlet and an outlet for the hydrogen bromide raw material to enter.

[0007] In one or more embodiments of the present invention, the first sieve plate is disposed on one side of the inner wall of the tower body, and the second sieve plate is disposed on the inner wall of the tower body on the side opposite to the first sieve plate.

[0008] In one or more embodiments of the present invention, the hydrogen-type zeolite molecular sieve is a hydrogen-type ZSM-5 zeolite molecular sieve.

[0009] In one or more embodiments of the present invention, the mass ratio of the acid-resistant alumina adsorbent to the hydrogen-type zeolite molecular sieve is 1:5 to 5:1.

[0010] A specific embodiment of the present invention also provides a hydrogen bromide purification system, comprising: Such as the adsorption device described above; The light-light distillation column is connected to the outlet of the adsorption device; The heavy removal distillation column is connected to the light removal distillation column.

[0011] In one or more embodiments of the present invention, the hydrogen bromide purification system further includes a dust removal bag connected between the first adsorption unit and the light distillation column, the dust removal bag being used to remove particles from the gas.

[0012] In one or more embodiments of the present invention, the dust bag is a dust bag made of polytetrafluoroethylene.

[0013] In one or more embodiments of the present invention, the purification system includes two adsorption devices.

[0014] In one or more embodiments of the present invention, the hydrogen bromide purification system further includes a raw material tank for containing the hydrogen bromide raw material, the raw material tank being connected to the inlet.

[0015] A specific embodiment of the present invention also provides a method for purifying hydrogen bromide, applied to the hydrogen bromide purification system described above, the purification method comprising the following steps: The hydrogen bromide feedstock was dehydrated using an adsorption device to obtain a dehydrated product. The dehydration product was purified using a light-light distillation column to obtain a dehydrogenated and impurity-removed product. The dehydrogenation and impurity removal products were purified using a de-heavy distillation column to obtain purified hydrogen bromide.

[0016] Compared with the prior art, the adsorption device, hydrogen bromide purification system and purification method of the present invention, by setting two adsorbents and selecting the adsorbents, can not only meet the requirement that the water content of the hydrogen bromide component before entering the distillation column is less than 1 ppm, that is, the water absorption effect meets the requirements of the hydrogen bromide purification process, but also reduce the cost of the adsorbent. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of a hydrogen bromide purification system in one embodiment of the present invention.

[0019] Explanation of key figure labels: 1. Adsorption device; 11. Tower body; 12. First sieve plate; 13. Second sieve plate; 2. Dust collector bag; 3. Light weight removal distillation tower; 4. Heavy weight removal distillation tower; 5. Raw material tank. Detailed Implementation

[0020] To enable those skilled in the art to better understand the technical solutions in this disclosure, the technical solutions in the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this disclosure, and not all embodiments. Based on the embodiments in this disclosure, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this disclosure.

[0021] like Figure 1 As shown, the adsorption device 1 in one example of the present invention includes a tower body 11, a plurality of first sieve plates 12 and a plurality of second sieve plates 13 installed in the tower body 11. Along the gas flow direction, all the first sieve plates 12 and second sieve plates 13 are distributed in sequence at intervals. The first sieve plates 12 carry acid-resistant alumina adsorbent, and the second sieve plates 13 carry hydrogen-type zeolite molecular sieves. The first tower body 11 has an inlet for the hydrogen bromide raw material to enter and an outlet for the material to be discharged.

[0022] It is understood that the adsorption device 1 of the present invention is part of the hydrogen bromide purification system. By setting two adsorbents at intervals in the column body 11 and selecting the two adsorbents, it can not only meet the requirement that the water content of the hydrogen bromide component before entering the distillation column (light distillation column 3) is less than 1 ppm, that is, the water absorption effect meets the requirements of the hydrogen bromide purification process, but also reduce the cost of the adsorbent.

[0023] While conventional alumina molecular sieves possess some water-holding capacity, they struggle to reduce moisture levels to extremely low levels, typically only reaching around 100 ppm. Furthermore, hydrogen bromide and water molecules can form HBr·H₂O, causing the alumina molecular sieve to pulverize. This can lead to structural collapse, agglomeration, and excessive dust reaching downstream pipes and filters, potentially resulting in high levels of Na, Ca, Al, and Mg ions, thus impacting product quality. Hydrogen-form ZSM-5 zeolite molecular sieves exhibit high adsorption heat. Since the moisture content in raw materials is generally greater than 100 ppm, using hydrogen-form ZSM-5 zeolite molecular sieves alone can cause the adsorbent temperature to rise rapidly above 100°C, leading to pulverization and failure of the hydrogen-form ZSM-5 zeolite molecular sieve.

[0024] In this example, the hydrogen-form zeolite molecular sieve is a hydrogen-form ZSM-5 zeolite molecular sieve; the acid-resistant alumina adsorbent is AW-300 alumina. Using AW-300 alumina reduces the moisture content of the raw material to approximately 20 ppm; the hydrogen-form ZSM-5 zeolite molecular sieve is responsible for deep dehydration, ensuring that the water content of the hydrogen bromide intermediate entering the distillation column is below 1 ppm. Because AW-300 alumina significantly reduces the moisture content of the raw material, the hydrogen-form ZSM-5 zeolite molecular sieve requires less water removal during deep dehydration, avoiding the problem of excessively high temperatures during dehydration.

[0025] Both the first sieve plate 12 and the second sieve plate 13 have porous structures, primarily serving to fix the adsorbent. The acid-resistant alumina adsorbent and the hydrogen-form zeolite molecular sieve are respectively placed on the first sieve plate 12 and the second sieve plate 13, which not only allows for better differentiation between the two adsorbents but also enables layering of the adsorbents. Furthermore, the first sieve plate 12 and the second sieve plate 13 also serve to support and fix the acid-resistant alumina adsorbent and the hydrogen-form zeolite molecular sieve. For example, water-containing HBr can cause the alumina adsorbent to pulverize; without sieve plates, the powder is more likely to gradually settle and clump at the bottom, causing blockage.

[0026] Preferably, the mass ratio of the acid-resistant alumina adsorbent to the hydrogen-type zeolite molecular sieve is 1:5 to 5:1.

[0027] like Figure 1 As shown, a specific example of the present invention also provides a hydrogen bromide purification system, including an adsorption device 1, a light distillation column 3 and a heavy distillation column 4; the adsorption device 1 is connected to the light distillation column 3; the heavy distillation column 4 is connected to the light distillation column 3.

[0028] It should be noted that the light-weight removal distillation column 3 and the heavy-weight removal distillation column 4 are existing light-weight removal distillation columns 3 and 4 in hydrogen bromide purification systems. This invention primarily focuses on improving the adsorption device 1, which has an adsorption and dehydration function. By spaced two adsorbents within the column body 11 and by selecting the appropriate adsorbents, the water content of the hydrogen bromide component before entering the distillation column (light-weight removal distillation column 3) can be kept below 1 ppm, meaning the water absorption effect meets the requirements of the hydrogen bromide purification process. This also reduces the cost of the adsorbents. The hydrogen bromide raw material used in this invention is an industrial-grade hydrogen bromide product.

[0029] Preferably, the purification system of this example includes two adsorption devices 1 arranged in series. The downstream adsorption device 1 is connected to the light distillation column 3. This arrangement can improve the water removal effect and avoid the individual adsorption device 1 being too tall and occupying too much space.

[0030] Furthermore, the adsorption device 1 also includes a dust collection bag 2 connected between the second adsorption mechanism and the light-duty distillation column 3. The dust collection bag 2 is used to remove particles from the gas brought in by the first and second adsorption mechanisms. That is, the dust collection bag 2 can filter particles brought in by the trace pulverization of the adsorbent, effectively reducing the particulate matter entering the subsequent pipelines and distillation column. Specifically, the dust collection bag 2 is made of polytetrafluoroethylene (PTFE).

[0031] The hydrogen bromide purification system also includes a raw material tank 5 for containing the hydrogen bromide raw material, the raw material tank 5 being connected to the inlet.

[0032] It is understandable that the raw material tank 5, the two adsorption devices 1 set in series, the dust removal bag 2, the light distillation column 3 and the heavy distillation column 4 can be connected by pipelines, and valves can be installed on the pipelines.

[0033] A specific example of the present invention also provides a method for purifying hydrogen bromide, comprising the following steps: S1. Use an adsorption device to dehydrate the hydrogen bromide raw material to obtain a dehydrated product; S2. The dehydration product is purified using a light-light distillation column to obtain a dehydrogenated and impurity-removed product; S3. The dehydrogenation and impurity removal product is purified using a de-heavy distillation column to obtain purified hydrogen bromide.

[0034] The hydrogen bromide raw material is an industrial-grade hydrogen bromide product.

[0035] The purification system and method for hydrogen bromide of the present invention will be described in detail below with reference to specific embodiments and comparative examples.

[0036] Example 1

[0037] Building such Figure 1 The hydrogen bromide purification system shown.

[0038] First, flush all pipelines and pressure vessels with nitrogen and evacuate the system beforehand. Each adsorption unit is then sequentially filled with acid-resistant desiccant AW-300 (1.71 kg) and hydrogen-form ZSM-5 zeolite molecular sieve HZSM-5 (silicon-to-aluminum ratio of 220) (2.03 kg). Temperature sensors are installed in the upper, middle, and lower parts of the first adsorption unit, respectively.

[0039] Hydrogen bromide feedstock is introduced, and the gaseous product discharged from the dust collection bag is collected.

[0040] Comparative Example 1 Building such Figure 1 The hydrogen bromide purification system shown is basically the same as that in Example 1, except that each adsorption device is filled with only 3.35 kg of acid-resistant water absorbent AW-300.

[0041] Hydrogen bromide feedstock is introduced, and the gaseous product discharged from the dust collection bag is collected.

[0042] Comparative Example 2 Building such Figure 1 The hydrogen bromide purification system shown is basically the same as that in Example 1, except that each adsorption device is filled with only 3.73 kg of hydrogen-type ZSM-5 zeolite molecular sieve (silicon-to-aluminum ratio of 220).

[0043] Hydrogen bromide feedstock is introduced, and the gaseous product discharged from the dust collection bag is collected.

[0044] The sensor temperature and moisture content of the gas product discharged from the dust collection bag in the first adsorption device of Example 1, Comparative Example 1 and Comparative Example 2 were recorded, and the data are shown in the table below.

[0045]

[0046] Note: The specific moisture content of the raw materials varied slightly in each experiment, but all met the raw material specifications.

[0047] As can be seen from the moisture data of the gas product in Example 1, the adsorption device of the present invention can effectively reduce the moisture in the hydrogen bromide raw material to below 1 ppm.

[0048] It will be apparent to those skilled in the art that this disclosure is not limited to the details of the exemplary embodiments described above, and that this disclosure can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of this disclosure is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this disclosure. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0049] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An adsorption device for a hydrogen bromide purification system, characterized in that, The system includes a tower body, multiple first sieve plates and multiple second sieve plates installed inside the tower body. All the first sieve plates and second sieve plates are distributed sequentially and alternately along the gas flow direction. The first sieve plates are loaded with acid-resistant alumina adsorbent, and the second sieve plates are loaded with hydrogen-type zeolite molecular sieves. The first tower body has an inlet and an outlet for hydrogen bromide raw materials to enter.

2. The adsorption device of the hydrogen bromide purification system according to claim 1, characterized in that, The first sieve plate is located on one side of the inner wall of the tower, and the second sieve plate is located on the inner wall of the tower on the side opposite to the first sieve plate.

3. The adsorption device of the hydrogen bromide purification system according to claim 1, characterized in that, The hydrogen-type zeolite molecular sieve is a hydrogen-type ZSM-5 zeolite molecular sieve.

4. The adsorption device of the hydrogen bromide purification system according to claim 1, characterized in that, The mass ratio of the acid-resistant alumina adsorbent to the hydrogen-type zeolite molecular sieve is 1:5 to 5:

1.

5. A hydrogen bromide purification system, characterized in that, include: The adsorption device as described in any one of claims 1 to 4; The light-light distillation column is connected to the outlet of the adsorption device; The heavy removal distillation column is connected to the light removal distillation column.

6. The hydrogen bromide purification system according to claim 5, characterized in that, The hydrogen bromide purification system also includes a dust removal bag connected between the first adsorption unit and the light distillation column, the dust removal bag being used to remove particles from the gas.

7. The hydrogen bromide purification system according to claim 6, characterized in that, The dust collection bag is made of polytetrafluoroethylene.

8. The hydrogen bromide purification system according to claim 5, characterized in that, The purification system includes two adsorption devices.

9. The hydrogen bromide purification system according to claim 5, characterized in that, The hydrogen bromide purification system also includes a raw material tank for containing the hydrogen bromide feedstock, the raw material tank being connected to the inlet.

10. A method for purifying hydrogen bromide, applied to the hydrogen bromide purification system as described above, characterized in that, The purification method includes the following steps: The hydrogen bromide feedstock was dehydrated using an adsorption device to obtain a dehydrated product. The dehydration product was purified using a light-light distillation column to obtain a dehydrogenated and impurity-removed product. The dehydrogenation and impurity removal products were purified using a de-heavy distillation column to obtain purified hydrogen bromide.

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