CN219469703U - Purification device of electronic grade hydrogen bromide - Google Patents
Purification device of electronic grade hydrogen bromide Download PDFInfo
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- CN219469703U CN219469703U CN202223613008.4U CN202223613008U CN219469703U CN 219469703 U CN219469703 U CN 219469703U CN 202223613008 U CN202223613008 U CN 202223613008U CN 219469703 U CN219469703 U CN 219469703U
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Abstract
The utility model discloses a purifying device of electronic grade hydrogen bromide, which comprises a secondary adsorption tower, a heavy-removal rectifying tower, a light-removal rectifying tower, a tertiary adsorption tower and a finished product storage tank; the two-stage adsorption towers are connected in series, a discharge hole of the two-stage adsorption tower is connected with the lower part of the body of the heavy removal rectifying tower, a discharge hole of the top of the heavy removal rectifying tower is connected with the middle part of the light removal rectifying tower, the bottom of the light removal rectifying tower is connected with the upper part of the three-stage adsorption tower, the lower part of the three-stage adsorption tower is connected with a finished product storage tank, and the finished product storage tank is connected with a steel cylinder through a filling pump; the first-stage adsorption tower is filled with a mixture of active carbon and molecular sieve, and the second-stage adsorption tower is filled with molecular sieve; the heavy-removal rectifying tower and the light-removal rectifying tower are filler rectifying towers; the three-stage adsorption tower is filled with modified activated carbon or molecular sieve, wherein the modified activated carbon or molecular sieve refers to activated carbon or molecular sieve prepared by impregnating with metal salt solution. The purification device solves the problem that sulfide impurities are difficult to deeply remove in the hydrogen bromide purification process, and purifies the hydrogen bromide to more than 99.9999 percent.
Description
Technical Field
The utility model relates to a preparation device of hydrogen bromide, in particular to a purification device of electronic grade hydrogen bromide.
Background
The electronic grade hydrogen bromide (HBr) gas is mainly used for etching of semiconductor phosphorus-doped n-type polycrystalline silicon, phosphorus-doped monocrystalline silicon or two-dimensional semiconductors in the chip manufacturing process, and is an indispensable raw material in the semiconductor field. The plasma etching technology using electronic grade hydrogen bromide as etching gas can accurately control the vertical etching of the etched object or the taper etching process with a set taper angle through temperature control, has the characteristics of high selectivity, etching anisotropy and the like, and is one of core gases of the chip advanced process. The electronic grade hydrogen bromide gas has corrosiveness and extremely strong hydrophilicity, and the corrosiveness of the hydrogen bromide is greatly enhanced along with the increase of moisture, so that most metal materials are strongly corroded, and more impurities are generated in the contact corrosion process. Therefore, the removal of moisture during the purification of electronic grade hydrogen bromide becomes a major point and difficulty in the overall purification process.
The hydrogen bromide purifying process mainly comprises adsorption, rectification and other modes. The rectification method has the problems of high requirement on corrosion resistance of equipment, insufficient water removal depth and the like in the water removal process; the adsorption method has simple operation and good removal effect, and is the first choice process for dehydrating electronic grade hydrogen bromide. In the existing hydrogen bromide purification process, part of sulfide impurities are difficult to remove through a conventional adsorption or rectification process, so that the currently disclosed patent and method generally defaults to be free of sulfide impurities, namely the content of sulfide impurities in the obtained product is considered to be zero, and the problem that the purity of the actual product is lower than that described exists; meanwhile, the regeneration, activation, recovery and replacement processes of the adsorbent in the adsorption and dehydration process can cause production stop and influence production efficiency, and the problems and the technical difficulties are the main problems for limiting the application of the hydrogen bromide adsorption and dehydration process.
Disclosure of Invention
The utility model aims to provide an electronic grade hydrogen bromide purifying device, which solves the problem that sulfide impurities are difficult to deeply remove in a hydrogen bromide purifying process, purifies hydrogen bromide to more than 99.9999%, improves the production efficiency, and meets the requirement of large-scale industrial production.
In order to achieve the above purpose, the technical scheme of the utility model is as follows: an electronic grade hydrogen bromide purifying device comprises a secondary adsorption tower, a heavy removal rectifying tower, a light removal rectifying tower, a tertiary adsorption tower and a finished product storage tank; 1. the two-stage adsorption towers are connected in series, a discharge hole of the two-stage adsorption tower is connected with the lower part of the body of the heavy removal rectifying tower, a discharge hole of the top of the heavy removal rectifying tower is connected with the middle part of the body of the light removal rectifying tower, the bottom of the light removal rectifying tower is connected with the upper part of the three-stage adsorption tower, the lower part of the three-stage adsorption tower is connected with a finished product storage tank, and the finished product storage tank is connected with a steel cylinder through a filling pump; the first-stage adsorption tower is filled with a mixture of active carbon and molecular sieve, the second-stage adsorption tower is filled with molecular sieve, and the molecular sieve in the second-stage adsorption tower is preferably a high silica alumina acid resistant molecular sieve; the heavy-removal rectifying tower and the light-removal rectifying tower are filler rectifying towers, wherein the filler is respectively and independently one of pall rings, ladder rings, saddle rings, raschig rings or structured filler, the diameters of the filler are respectively and independently 2-20 mm, and the surface roughness of the inner walls of the heavy-removal rectifying tower and the light-removal rectifying tower is 0.1-0.9 mu m; the three-stage adsorption tower is filled with modified activated carbon or molecular sieve, wherein the modified activated carbon or molecular sieve refers to activated carbon or molecular sieve prepared by impregnating with metal salt solution.
The metal salt solution is one of aqueous solution or alcoholic solution of metal salt, preferably metal salt alcoholic solution, the activated carbon or molecular sieve is immersed in the metal salt solution, soaked for 4-48 h at 20-60 ℃, and dried in the air, thus obtaining the modified activated carbon or molecular sieve. The mass concentration of the metal salt solution is preferably 5% -30%.
The metal salt is selected from one or more of calcium bromide, magnesium bromide, manganese bromide, copper bromide, ferrous bromide, zinc bromide and the like.
The activated carbon is selected from one or more of wood activated carbon, coal activated carbon, fruit shell activated carbon, coconut shell activated carbon and the like; the molecular sieve is preferably a 5A molecular sieve, ZSM-5 molecular sieve, or the like.
Preferably, the mixing mass ratio of the active carbon to the molecular sieve in the first-stage adsorption tower is one of 1:1, 1.5:1, 2:1, 3:1 and 4:1.
Preferably, the primary adsorption tower, the rectifying tower, the tertiary adsorption tower and the finished product storage tank are connected to the tail gas catcher through pipelines, and hydrogen bromide consumed in the production process can be collected and treated through the tail gas catcher.
Preferably, the absorption tower body is provided with a circulating water cooling device, and the corrosion aggravation risk and the hydrogen bromide pyrolysis hidden trouble caused by heat release in the absorption process are reduced through the circulating water cooling device.
Preferably, the adsorption towers are connected in parallel to realize one-by-one continuous production. The adsorbent can be switched during regeneration or replacement, so that continuous operation of equipment is ensured, and production efficiency is improved.
Preferably, a filter is arranged on the pipeline from the rear of the secondary adsorption tower to the sample inlet of the rectifying tower, and the pipeline from the rear of the tertiary adsorption tower to the finished product storage tank and the filling pipeline at the rear end of the filling pump. The pore diameter of the filter is independently 0.003-10 mu m.
Preferably, the tower bottom and the tower top of the rectifying tower are respectively provided with a heat exchanger, and the heat exchangers are respectively and independently preferably one of an inner coil type heat exchanger and a tubular type heat exchanger.
Preferably, the heat exchange areas of the tower kettle reboiler and the tower top condenser of the heavy and light removal rectifying tower and the light removal rectifying tower are respectively and independently 1-20 m 2 。
The inside coil pipe that sets up of finished product storage tank for guarantee that hydrogen bromide in the storage tank is liquid, the lower part is installed and is weighed the module, is used for monitoring the material weight in the jar.
Preferably, the filling pump is a diaphragm pump.
Preferably, the tail gas trap may re-enter the collected hydrogen bromide into the sample line via a playback system.
Preferably, the adsorption tower, the rectifying tower, the desulfurization adsorption tower, the finished product storage tank and the tail gas catcher are respectively and independently selected from one of 304, 304L, 316 and 316L, nickel-plated stainless steel and polytetrafluoroethylene lining stainless steel.
Preferably, the hydrogen bromide main material pipeline, the analysis pipeline, the replacement pipeline and the connecting pipeline use one of BA-level or EP-level clean pipes.
Preferably, the main process pipeline valve uses a pneumatic valve, is connected with a DCS or a PLC system, and realizes remote program control.
Compared with the prior art, the electronic grade hydrogen bromide gas purifying device has the following components
The beneficial effects are that:
(1) The device adopts a secondary adsorption tower, takes the mixture of the activated carbon and the molecular sieve with low cost and high stability as the adsorbent to carry out primary pre-adsorption, greatly prolongs the service life of deep dehydration of the adsorbent in the secondary adsorption process, prolongs the period of regeneration and replacement of the adsorbent, and improves the production efficiency.
(2) The device removes sulfide impurities which are difficult to remove in the rectification and adsorption processes through the three-stage adsorption towers, and improves the quality of hydrogen bromide products.
(3) The device adopts two groups of adsorption systems to be connected in parallel, one is used for one preparation, and the regeneration or replacement process of the adsorbent can be switched to the other group for production, so that production stagnation is avoided.
(4) The device adopts high-purity helium gas to replace in the filling system, ensures the stability of the quality of the hydrogen bromide product in the refilling process, and improves the filling safety by adopting a low-temperature liquid filling technology.
(5) The rectification tower and the finished product storage tank of the device adopt refrigerant heat exchange, and meanwhile, liquid nitrogen used by the tail gas catcher enters the refrigerant storage tank for heat exchange, so that the use of the liquid nitrogen is reduced, the utilization rate of the liquid nitrogen is improved, and the energy consumption is greatly reduced.
(6) The device purifies hydrogen bromide collected by the tail gas catcher by re-entering the production system through the playback system, thereby greatly reducing the loss of crude hydrogen bromide and improving the yield.
(7) The main process pipelines of the device all adopt pneumatic valves, can be remotely controlled by a program, reduces the possibility of misoperation of personnel, and improves the production efficiency and the safety.
Drawings
FIG. 1 is a schematic diagram of an electronic grade hydrogen bromide purification device according to the present utility model.
11, a first-stage adsorption tower; 21. a second-stage adsorption tower; 31. a condenser at the top of the heavy-duty removal tower; 32. a weight removing tower body; 33. a reboiler at the tower bottom of the heavy-removal tower; 41. a condenser at the top of the light component removing tower; 42. a light component removing tower body; 43. a reboiler at the bottom of the light component removing tower; 51. a third-stage adsorption tower; 6. a finished product storage tank; 7. filling a pump; 8. an exhaust gas trap; 91. steel cylinder
Detailed Description
The utility model is further described below with reference to the drawings and examples.
As shown in fig. 1, the purification device of the electronic grade hydrogen bromide comprises a two-stage adsorption tower, a heavy-removal rectifying tower, a light-removal rectifying tower, a three-stage adsorption tower and a finished product storage tank; 1. the two-stage adsorption towers are connected in series, a discharge hole of the two-stage adsorption tower is connected with the lower part of the body of the heavy removal rectifying tower, a discharge hole of the top of the heavy removal rectifying tower is connected with the middle part of the body of the light removal rectifying tower, the bottom of the light removal rectifying tower is connected with the upper part of the desulfurization adsorption column, the lower part of the three-stage adsorption tower is connected with a finished product storage tank, and the finished product storage tank is connected with a steel cylinder through a filling pump; the first-stage adsorption tower is filled with a mixture of active carbon and molecular sieve, the second-stage adsorption tower is filled with molecular sieve, and the molecular sieve in the second-stage adsorption tower uses high silica alumina ratio acid-resistant molecular sieve; the heavy-removal rectifying tower and the light-removal rectifying tower are filler rectifying towers, wherein the filler is respectively and independently one of pall rings, ladder rings, saddle rings, raschig rings or structured filler, the diameters of the filler are respectively and independently 2-20 mm, and the surface roughness of the inner walls of the heavy-removal rectifying tower and the light-removal rectifying tower is 0.1-0.9 mu m; the three-stage adsorption tower is filled with modified activated carbon or molecular sieve, wherein the modified activated carbon or molecular sieve is prepared by impregnating with metal salt solution. The adsorption tower, the rectifying tower, the desulfurization adsorption tower and the finished product storage tank are connected to the tail gas catcher through pipelines. The absorption tower body is provided with a circulating water cooling device. The adsorption towers are connected in parallel to realize one-by-one continuous production. The heights of the adsorption towers are respectively and independently 1-8 m, and the tower diameters are respectively and independently 0.05-0.6 m. And a filter is arranged on the pipeline from the rear of the second-stage adsorption tower to the sample inlet of the rectifying tower, and the pipeline from the rear of the third-stage adsorption tower to the rear end of the finished product storage tank and the filling pipe at the rear end of the filling pump, wherein the pore diameter of the filter is respectively and independently 0.003-10 mu m. The heavy-removal rectifying tower and the light-removal rectifying towerThe tower heights are respectively and independently 5-15 m, and the tower diameters are respectively and independently 0.05-0.7 m. The tower bottom and the tower top of the rectifying tower are respectively provided with a heat exchanger, and the heat exchangers are respectively and independently preferably one of an inner coil type heat exchanger and a tubular type heat exchanger. The heat exchange areas of a tower kettle reboiler and a tower top condenser of the heavy and light removal rectifying towers are respectively and independently 1-20 m 2 . The interior of the finished product storage tank is provided with a cold liquid inner coil pipe. The filling pump is a diaphragm pump. The tail gas catcher reenters the collected hydrogen bromide into the sample injection pipeline through the playback system. The adsorption tower, the rectifying tower, the desulfurization adsorption tower, the finished product storage tank and the tail gas catcher are respectively and independently selected from one of 304, 304L, 316 and 316L, nickel-plated stainless steel and polytetrafluoroethylene lining stainless steel. The main material pipeline, the analysis pipeline, the replacement pipeline and the connecting pipeline of the hydrogen bromide are one of BA-level or EP-level clean pipes. The main process pipeline valve uses a pneumatic valve, is connected with a DCS or a PLC system, and realizes remote program control.
1. The second-stage adsorption towers are connected in series, the first-stage adsorption towers pre-remove the water in the hydrogen bromide, and the second-stage adsorption towers deeply remove the water; the discharge port of the second-stage adsorption tower is connected with the lower part of the tower body of the heavy-removal rectifying tower through a pipeline provided with a filter, the heavy-removal rectifying tower and the light-removal rectifying tower are composed of a tower kettle reboiler, a tower body and a tower top condenser, the tower kettle is provided with a heating device and a sewage outlet, and the tower top is provided with a condensing reflux device; one path of the discharge port of the tower kettle of the light component removal rectifying tower is directly connected to a finished product storage tank through a filter, and the other path of the discharge port of the tower kettle of the light component removal rectifying tower enters a three-stage adsorption tower and enters the finished product storage tank through the filter from the outlet of the three-stage adsorption tower; the finished product storage tank is provided with a heat exchange system for cooling and liquefying materials, and a discharge hole is arranged at the bottom of the finished product storage tank and connected to a filling pump.
The adsorption towers are provided with a heating device, a temperature display and remote control device and a safety release device, the two-stage adsorption towers share one set of gas purging vacuum displacement system, a group of identical adsorption systems are arranged at the sides and are connected in parallel for standby, and the adsorption towers can be switched to another adsorption system in the regeneration or replacement process of the adsorbent. The bottom discharge port of the second-stage adsorption tower is connected with the feed port of the heavy-removal rectifying tower body 32 through a pipeline provided with a multi-stage filter, the discharge port of the top condenser 31 of the heavy-removal rectifying tower is connected with the feed port of the bottom 42 of the heavy-removal rectifying tower, and the rectifying tower is provided with a heating and condensing heat exchange device, a temperature and pressure sensor, a remote transmission device and a safety discharge device. A group of pipelines of the discharge port of the reboiler 43 of the light-removal tower kettle are connected with the finished product storage tank 6, a group of pipelines of the reboiler 43 of the light-removal tower kettle are connected with the feed port of the three-stage adsorption tower 51, the direct sample injection finished product storage tank 6 can be selected according to the analysis result of the hydrogen bromide impurity in the reboiler 43 of the light-removal rectification tower kettle, and the two groups of three-stage adsorption towers are connected in parallel and can be switched to use according to the use requirement. The discharge port of the finished product storage tank 6 is connected with the inlet of the filling pump 7, and the outlet of the filling pump 7 is connected with two groups of filling steel cylinders. The dehydration adsorption system, the rectification system, the finished product storage tank 6 and the filling system are all provided with pipelines which are connected to a tail gas catcher 8, and two discharge ports of the tail gas catcher 8 are respectively connected to a tail gas treatment system and a playback system.
The composition of the crude hydrogen bromide is shown in Table 1.
TABLE 1 composition of crude hydrogen bromide
| Composition of components | Detection value (ppmv) |
| Hydrogen gas | 1910 |
| Nitrogen gas | 920 |
| Oxygen + argon | 70 |
| Sulfide gas | 870 |
| Carbon monoxide | 120 |
| Carbon dioxide | 460 |
| Acetylene (acetylene) | 580 |
| Methane | 60 |
| Water and its preparation method | 14 |
| Purity of Hydrogen bromide | 99.5％ |
Example 1
The crude product of hydrogen bromide enters a purification device through a sample injection pipeline, the purity of the hydrogen bromide after rectification reaches 99.9996% through analysis of a tower kettle of a light component removal tower, the moisture is less than 0.3ppmv, wherein the total content of sulfide gas impurities is 2.9ppmv, the finished product of hydrogen bromide enters a three-stage adsorption tower, the purity of the hydrogen bromide reaches 99.9999% through detection, and the content of sulfide impurities is less than 0.4ppmv.
Example 2
The crude product of hydrogen bromide enters a purification device through a sample injection pipeline, the purity of the hydrogen bromide reaches 99.9995% after rectification through analysis of a tower kettle of a light component removal tower, the moisture is less than 0.2ppmv, wherein the total content of sulfide gas impurities is 4.3ppmv, the finished product of hydrogen bromide enters a three-stage adsorption tower, the purity of the hydrogen bromide reaches 99.9999% after detection, and the content of sulfide impurities is less than 0.3ppmv.
Example 3
The crude product of hydrogen bromide enters a purification device through a sample injection pipeline, the purity of the hydrogen bromide reaches 99.9991 percent after rectification through analysis of a tower kettle of a light component removal tower, the moisture is less than 0.5ppmv, wherein the total content of sulfide gas impurities is 7.7ppmv, the finished product of hydrogen bromide enters a three-stage adsorption tower, the purity of the hydrogen bromide reaches 99.9999 percent after detection, and the content of sulfide impurities is less than 0.3ppmv.
The above description is only of the preferred embodiments of the present patent, and is not intended to limit the present patent. Various modifications to the embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the disclosure. Thus, the present patent is not intended 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 (9)
1. The purifying device of electronic grade hydrogen bromide is characterized by comprising a second-level adsorption tower, a heavy-removal rectifying tower, a light-removal rectifying tower, a third-level adsorption tower and a finished product storage tank; 1. the two-stage adsorption towers are connected in series, a discharge hole of the two-stage adsorption tower is connected with the lower part of the body of the heavy removal rectifying tower, a discharge hole of the top of the heavy removal rectifying tower is connected with the middle part of the body of the light removal rectifying tower, the bottom of the light removal rectifying tower is connected with the upper part of the three-stage adsorption tower, the lower part of the three-stage adsorption tower is connected with a finished product storage tank, and the finished product storage tank is connected with a steel cylinder through a filling pump; the first-stage adsorption tower is filled with a mixture of active carbon and molecular sieve, and the second-stage adsorption tower is filled with molecular sieve; the heavy-removal rectifying tower and the light-removal rectifying tower are filler rectifying towers, wherein the filler is respectively and independently one of pall rings, ladder rings, saddle rings, raschig rings or structured filler, the diameters of the filler are respectively and independently 2-20 mm, and the surface roughness of the inner walls of the heavy-removal rectifying tower and the light-removal rectifying tower is 0.1-0.9 mu m; the three-stage adsorption tower is filled with modified activated carbon or molecular sieve, wherein the modified activated carbon or molecular sieve refers to activated carbon or molecular sieve prepared by impregnating with metal salt solution.
2. The purification apparatus of claim 1, wherein the molecular sieve in the secondary adsorption column is a high silica alumina acid resistant molecular sieve.
3. The purification device according to claim 1, wherein the secondary adsorption tower, the rectifying tower, the tertiary adsorption tower and the finished product storage tank are connected to the tail gas catcher through pipelines.
4. The purification device according to claim 1, wherein two groups of two-stage adsorption towers are connected in parallel to realize one-by-one continuous production.
5. The purification device according to claim 1, wherein a filter is arranged in a filling pipe line from the rear of the two-stage adsorption tower to the inlet pipe line of the rectifying tower to the rear of the finished product storage tank pipe line and the rear end of the filling pump, and the pore diameter of the filter is independently 0.003-10 μm.
6. The purifying device according to claim 1, wherein the absorption tower body is provided with a circulating water cooling device; the tower bottom and the tower top of the rectifying tower are respectively provided with a heat exchanger, and the heat exchangers are respectively and independently one of an inner coil type heat exchanger and a tubular type heat exchanger.
7. The purifying device according to claim 1, wherein the cold liquid inner coil is arranged in the finished product storage tank, and the weighing module is arranged at the lower part; the filling pump is a diaphragm pump.
8. The purification device according to claim 3, wherein the adsorption tower, the rectification tower, the desulfurization adsorption tower, the finished product storage tank and the tail gas catcher are respectively and independently selected from one of 304, 304L, 316 and 316L, nickel-plated stainless steel and polytetrafluoroethylene lining stainless steel; the main material pipeline, the analysis pipeline, the replacement pipeline and the connecting pipeline of the hydrogen bromide are one of BA-level or EP-level clean pipes.
9. The purification device of claim 1, wherein the process line valve is pneumatically operated to access a DCS or PLC system for remote program control.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202223613008.4U CN219469703U (en) | 2022-12-29 | 2022-12-29 | Purification device of electronic grade hydrogen bromide |
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| CN202223613008.4U CN219469703U (en) | 2022-12-29 | 2022-12-29 | Purification device of electronic grade hydrogen bromide |
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