CN117695801A - 9N ultra-pure low-temperature hydrogen purification device and purification method - Google Patents
9N ultra-pure low-temperature hydrogen purification device and purification method Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 67
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 67
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000746 purification Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims description 30
- 239000007789 gas Substances 0.000 claims abstract description 259
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 116
- 239000002994 raw material Substances 0.000 claims abstract description 89
- 238000001179 sorption measurement Methods 0.000 claims abstract description 88
- 230000008929 regeneration Effects 0.000 claims abstract description 64
- 238000011069 regeneration method Methods 0.000 claims abstract description 64
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 58
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 239000003463 adsorbent Substances 0.000 claims abstract description 42
- 239000011229 interlayer Substances 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000000945 filler Substances 0.000 claims abstract description 24
- 238000010926 purge Methods 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010457 zeolite Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 11
- 238000005192 partition Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 description 96
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000002912 waste gas Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000012264 purified product Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 2
- -1 methane hydrocarbons Chemical class 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
- F28D7/16—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being arranged in parallel spaced relation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/25—Coated, impregnated or composite adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/042—Purification by adsorption on solids
- C01B2203/043—Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/047—Composition of the impurity the impurity being carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0475—Composition of the impurity the impurity being carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/048—Composition of the impurity the impurity being an organic compound
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0495—Composition of the impurity the impurity being water
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention discloses a 9N ultra-pure low-temperature hydrogen purification device, which comprises a standby low-temperature adsorption reactor, a raw material gas input pipeline, a product gas output pipeline, a liquid nitrogen input pipeline, a nitrogen purging pipeline, an exhaust gas discharge pipeline, a corresponding switching valve and a control system, wherein a bypass of the product gas output pipeline is connected with a regenerated gas input pipeline which is communicated with a regeneration tower, and a heater is arranged on the regenerated gas input pipeline; the low-temperature adsorption reactor comprises an inner cylinder, an interlayer surrounding the circumference of the inner cylinder, a filler reaction tube arranged in the inner cylinder, and a heat exchange system, wherein the interlayer is communicated with a liquid nitrogen input pipeline, an adsorbent is arranged in the filler reaction tube, and the adsorbent is formed by mixing activated carbon, alumina and zeolite; the heat exchange system is used for cooling the raw material gas and heating the product gas. The invention discloses a 9N ultra-pure low-temperature hydrogen purification device, which is used for removing impurities contained in raw material 5N grade hydrogen and outputting 9N grade product gas.
Description
Technical Field
The invention relates to the technical field of hydrogen purification, in particular to a 9N ultra-pure low-temperature hydrogen purification device and a purification method.
Background
The ultra-pure hydrogen is widely applied to strategic emerging industries such as electronics, semiconductors and LEDs, hydrogen in industrial gas manufacturing links used in the industries mainly comprises two manufacturing methods, namely water electrolysis and coal pyrolysis hydrogen production, and the hydrogen manufactured by the two manufacturing methods contains more impurities, and after primary filtration of manufacturers, the hydrogen also contains impurities such as nitrogen, argon, oxygen, water, carbon monoxide, carbon dioxide and non-methane hydrocarbons with ppm-ppb level, and if the hydrogen is directly applied to the field of semiconductor industrial manufacturing, the product quality is directly influenced, so that the removal of the impurities is very critical.
At present, the method for preparing high-purity hydrogen with the purity of more than 99.999 percent by adsorption separation, cryogenic separation, palladium alloy diffusion separation and the like cannot meet new requirements, and along with the rapid development of the semiconductor industry and the microelectronics industry, the method has higher requirements on the quality, the purity and other indexes of ultra-high-purity gas.
In order to further improve the quality and purity of ultra-high purity gas, researchers at present mainly finish the purification of hydrogen raw material by means of getter and deoxidization adsorption method, in the process, firstly, the hydrogen raw material is pretreated by deoxidization adsorption method, and then impurity adsorption and removal are carried out by means of the getter, so as to remove the impurity in the hydrogen raw material to 10 -9 Stage, can obtain ultrapure hydrogen with purity of more than 8N, but because the hydrogen also contains inert gas argon, the current stage is requiredThe impurity such as argon cannot be removed well by using a purification gas method, so that the removal of the impurity in the hydrogen presents a certain limitation.
Disclosure of Invention
The invention discloses a 9N ultra-pure low-temperature hydrogen purification device, which aims to overcome the defect that the removal of argon cannot be realized in the existing purification method, thereby influencing the quality and purity of ultra-pure gas.
In order to achieve the above object, the technical scheme of the present invention is as follows: the 9N ultra-pure low-temperature hydrogen purification device comprises a standby low-temperature adsorption reactor, a raw material gas input pipeline, a product gas output pipeline, a liquid nitrogen input pipeline, a nitrogen purging pipeline, a waste gas discharge pipeline, corresponding switching valves and a control system, wherein the standby low-temperature adsorption reactor is respectively in a purification stage and a regeneration stage, the low-temperature adsorption reactor in the purification stage is used as a working tower, the low-temperature adsorption reactor in the regeneration stage is used as a regeneration tower, a bypass of the product gas output pipeline is connected with a regeneration gas input pipeline, the regeneration gas input pipeline is communicated with the regeneration tower, and a heater is arranged on the regeneration gas input pipeline; the low-temperature adsorption reactor comprises an inner cylinder, an interlayer surrounding the circumferential side wall of the inner cylinder, a filler reaction tube arranged in the inner cylinder, and a heat exchange system arranged at the upper end and the lower end of the inner cylinder, wherein the interlayer is communicated with a liquid nitrogen input pipeline, an adsorbent is arranged in the filler reaction tube, and the adsorbent is formed by mixing activated carbon, alumina and zeolite; the heat exchange system is used for cooling the raw material gas and heating the product gas.
Further, the heat exchange system comprises a raw material gas heat exchange pipe and a product gas heat exchange pipe, two ends of the inner cylinder are respectively provided with a cavity, two partition plates are arranged in the cavities, the cavities are divided into a raw material gas heat exchange cavity and a product gas heat exchange cavity by the partition plates, the raw material gas heat exchange pipe is communicated with the upper raw material gas heat exchange cavity and the lower raw material gas heat exchange cavity, the product gas heat exchange pipe is communicated with the upper product gas heat exchange cavity and the lower product gas heat exchange cavity, the upper raw material gas heat exchange cavity and the lower product gas heat exchange cavity are communicated with a filler reaction pipe, the lower raw material gas heat exchange cavity is communicated with a raw material gas input pipeline, and the upper product gas heat exchange cavity is communicated with a product gas output pipeline.
Further, one end of the raw material gas heat exchange pipe is communicated with the lower raw material gas heat exchange cavity, and the other end of the raw material gas heat exchange pipe penetrates through the interlayer and is communicated with the upper raw material gas heat exchange cavity; one end of the product gas heat exchange tube is communicated with the lower product gas heat exchange cavity, and the other end of the product gas heat exchange tube penetrates through the interlayer and is communicated with the upper product gas heat exchange cavity.
Further, the mass ratio of the active carbon to the alumina to the zeolite is 1:1:1.
Further, the product gas output pipeline is provided with a carbon dioxide remover, and the product gas is adsorbed at normal temperature through the carbon dioxide remover to remove a small amount of impurities contained in the product gas again, and then directly enters the next working procedure or enters the regenerated gas input pipeline.
Further, a bypass of the product gas output pipeline is connected with a product gas detection pipeline, the product gas detection pipeline is communicated with the waste gas discharge pipeline, and Ar index in the product gas can be less than 1ppb.
Further, a pressure relief pipeline is communicated with the low-temperature adsorption reactor, a safety valve and a pressure sensor are arranged on the pressure relief pipeline, and when the safety valve is tripped, a high pressure alarm is given.
Further, a liquid level meter for monitoring the liquid level of the liquid nitrogen in the interlayer is arranged on the low-temperature adsorption reactor, and the liquid level of the liquid nitrogen in the interlayer is controlled to be 50-80% of the height of the interlayer.
Further, the product gas output pipeline and the raw material gas input pipeline are respectively provided with a pressure sensor, whether the adsorbent has caking phenomenon or not can be judged by comparing the pressure drop of the inlet and the outlet, and whether the adsorbent fails or not can be judged, and when the pressure drop is more than 2barg (0.2 MPa), the adsorbent needs to be replaced.
The method for purifying the hydrogen by using the 9N ultra-pure low-temperature hydrogen purification device removes impurities contained in 5N grade hydrogen as a raw material to produce 9N grade product gas output, and comprises the following steps:
purification stage: after the raw material gas enters a working tower, the raw material gas at normal temperature is cooled to a low-temperature adsorption temperature under the action of a heat exchange system, purified hydrogen is obtained through the purification effect of the filler in the raw material gas, the purified hydrogen is taken as product gas, the product gas is output when the temperature of the product gas is raised to 10 ℃ lower than the room temperature under the action of the heat exchange system, and the output product gas enters the next working procedure through a product gas outlet;
regeneration: purging liquid nitrogen contained in the interlayer of the regeneration tower by adopting nitrogen so as to enable the low-temperature adsorption reactor to return to a room temperature state; and then introducing part of product gas to raise the temperature of the regeneration tower to above 300 ℃, and removing saturated impurities adsorbed in the adsorbent filler at high temperature to recover the adsorption capacity of the adsorbent.
Still further, the method further comprises the steps of,
the purification procedure was as follows: after passing through a raw material gas inlet and a raw material gas inlet hand valve, detecting that the pressure and flow conditions of the raw material gas meet the basic purification requirements after passing through a raw material gas pressure sensor and a raw material gas flowmeter, entering a low-temperature adsorption reactor after passing through a reactor inlet pneumatic valve, and providing a cold environment because the interlayer of the low-temperature adsorption reactor is filled with liquid nitrogen, all raw material 5N hydrogen is subjected to low-temperature adsorption by a special adsorbent, so that impurities such as nitrogen, argon, oxygen, water, carbon monoxide, carbon dioxide and non-methane in the raw material 5N hydrogen are adsorbed and removed. After passing through the product gas outlet valve and the CRU15, the required high-purity 9N-level hydrogen is reached, then passes through the product gas pressure sensor and the product gas outlet hand valve, and finally the high-purity 9N-level hydrogen is delivered out through the product gas outlet.
The regeneration flow is as follows: the product gas is regenerated by the product gas, and firstly, the product gas enters the heater through the regeneration pipeline, passes through the regeneration valve and the regeneration inlet valve, so that the temperature of the gas is raised to above 300 ℃, and enters the low-temperature adsorption reactor, the temperature of the reaction bed layer is raised, and then saturated impurities adsorbed in the adsorbent filler are subjected to high Wen Tuochu, so that the adsorption capacity of the adsorbent is recovered again. And then the regenerated gas is subjected to emptying treatment or recycling and reutilization through a regeneration outlet valve and a regeneration discharge valve.
Because the reaction conditions, the regeneration conditions and the properties of metals are determined, the liquid nitrogen contained in the low-temperature adsorption reactor needs to be purged before regeneration, nitrogen needs to be injected from a nitrogen purging inlet at the moment, enters the interlayer of the reactor through a nitrogen purging inlet valve, is purged with the liquid nitrogen for a period of time, and returns the temperature of the low-temperature adsorption reactor to the room temperature state, so that the regeneration flow of the low-temperature adsorption reactor is started.
In summary, the invention has the following beneficial effects:
1. the method adopts activated carbon, alumina and zeolite filler to form the adsorbent, and adopts a heat exchange system to cool the raw material gas before the raw material gas contacts with the adsorbent filler, so that the raw material gas and the adsorbent are adsorbed at low temperature, and the adsorption capacity of the adsorbent can reach 30mL/g in a low-temperature state through measurement; meanwhile, the adsorbent has good adsorption effect on Ar, can better adsorb and remove impurities contained in hydrogen, produce high-purity hydrogen with the purity of 9N, and can solve the technical problem of argon removal in the current high-purity hydrogen, so that Ar index in product gas can be less than 1ppb.
2. According to the method, the heat exchange system is arranged in the low-temperature adsorption reactor, so that the raw material gas which can pass through the normal temperature can be cooled to the low-temperature adsorption temperature after passing through the heat exchange system, and meanwhile, the purified product gas exchanges heat with the raw material gas to be heated, so that the temperature is restored to be 10 ℃ lower than the room temperature, and the raw material gas can be directly conveyed to a rear-end production line without additional secondary heating;
3. the method adopts the product gas as the regeneration gas, can be regenerated on site, does not need to return to factories for regeneration, and saves a great amount of time cost for semiconductor manufacturers.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments or the description of the prior art will be briefly described below, it will be obvious that the drawings in the following description are some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic flow chart of a 9N ultra-pure low-temperature hydrogen purification device disclosed by the invention;
FIG. 2 is a schematic diagram of a cryogenic adsorption reactor of the present disclosure;
in the figure: 1. a feed gas inlet; 2. a feed gas inlet hand valve; 3. a raw material air pressure sensor; 4. a feed gas flow meter; 5. a reactor inlet pneumatic valve; 6. a low temperature adsorption reactor; 6A, an interlayer; 6B, a filler reaction tube; 6C, a raw material gas heat exchange tube; 6D, a product gas heat exchange tube; 6E, a partition plate; 7. a liquid level gauge; 8. a liquid nitrogen inlet; 8A, a liquid nitrogen inlet valve; 9. a nitrogen inlet; 9A, purging a nitrogen inlet valve; 10. a nitrogen outlet; 11. a low temperature adsorption reactor pressure sensor; 12. a low temperature adsorption reactor safety valve; 13. a safety vent; 14. a product gas outlet valve; 15. a carbon dioxide remover; 16. a product air pressure sensor; 17. a product gas outlet hand valve; 18. a product gas outlet; 19. a product gas vent valve; 20. a regeneration valve; 21. a regeneration inlet valve; 22. a heater; 23. a regeneration outlet valve; 24. a regeneration vent valve; 25. a product gas purge valve; 26. an exhaust gas discharge port.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, a 9N ultra-pure low-temperature hydrogen purification device consists of a pipeline system, a low-temperature adsorption reactor 6 and a heater 22; the 5N-level hydrogen at the inlet is used as raw material gas, and the raw material gas is subjected to low-temperature adsorption by a special adsorbent after passing through a pipeline system and a low-temperature adsorption purifier, so that the purity of the product gas can reach 9N-level high-purity hydrogen. Meanwhile, the application also relates to a regeneration flow after the adsorption saturation of the reactor, mainly through the high-purity 9N hydrogen of a product, a regeneration pipeline system and a heater 22, the temperature of the gas is raised, the temperature of the reactor bed is raised to be higher than 300 ℃, and then the impurities adsorbed and saturated in the adsorbent filler are subjected to high Wen Tuochu, so that the adsorption capacity of the adsorbent is recovered again.
In a specific embodiment, the 9N ultra-pure low-temperature hydrogen purification device comprises a standby two low-temperature adsorption reactors 6, a raw material gas input pipeline, a product gas output pipeline, a liquid nitrogen input pipeline, a nitrogen purging pipeline, an exhaust gas discharge pipeline, a corresponding switching valve and a control system, wherein the control system is a PLC full-automatic control system, and the PLC full-automatic control system can control the standby two low-temperature adsorption reactors 6, the corresponding valves and the corresponding pipelines to work or close. The process selects a double-tower structure with a low-temperature adsorption reactor 6 in a purification stage and a regeneration stage respectively, wherein the low-temperature adsorption reactor 6 in the purification stage is used as a working tower, and the low-temperature adsorption reactor 6 in the regeneration stage is used as a regeneration tower.
The air inlet of the working tower is connected with the raw material gas inlet 1 through a connecting pipeline, a raw material gas input auxiliary pipeline, an inlet pneumatic valve, a raw material gas input pipeline and a raw material gas inlet 1 hand valve. A raw material gas pressure sensor 3 and a raw material gas flow meter 4 are sequentially arranged on a raw material gas input pipeline along the input direction of raw material gas, the pressure and flow conditions of the raw material gas are detected by the raw material gas pressure sensor 3 and the raw material gas flow meter 4, and after the pressure and the flow meet the basic purification requirements, the raw material gas enters a low-temperature adsorption reactor 6 through opening a corresponding inlet pneumatic valve to carry out purification work.
The gas outlet of the working tower is connected with a product gas outlet 18 through a product gas output auxiliary pipeline, a product gas outlet valve 14, a product gas output pipeline and a product gas outlet hand valve 17. The carbon dioxide remover 15 is arranged on the product gas output pipeline, and the product gas is adsorbed at normal temperature by the carbon dioxide remover (CRU) to remove a small amount of impurities contained in the product gas again, so that the purity of the product gas is improved.
In the specific embodiment, the raw material gas input pipelines are all provided with raw material gas pressure sensors 3, the product gas output pipelines are provided with product gas pressure sensors 16, and when the pressure drop is greater than 0.2MPa through comparison of inlet and outlet pressure drops, the packing in the low-temperature adsorption reactor 6 is proved to be agglomerated or pulverized, and the packing needs to be replaced at the moment.
In a specific embodiment, a bypass of the product gas output pipeline is connected with a regenerated gas input pipeline, the regenerated gas input pipeline is communicated with a regenerated gas input auxiliary pipeline through a regeneration valve 20, a regeneration inlet valve 21 and a heater 22 are sequentially arranged on the regenerated gas input auxiliary pipeline along the gas flowing direction, purified product gas enters the regeneration tower after being heated through the regenerated gas input pipeline and the heater 22, the temperature of a reaction bed layer in the regeneration tower is further raised to be higher than 300 ℃, and then saturated impurities adsorbed in the adsorbent filler are subjected to high Wen Tuochu, so that the adsorption capacity of the adsorbent is recovered again. The regenerated gas output pipeline is communicated with the waste gas outlet through a regenerated gas outlet valve and a regenerated gas discharge valve.
In a specific embodiment, a product gas detection pipeline is connected to a bypass of the product gas output pipeline, the product gas detection pipeline is communicated with the waste gas discharge pipeline through a product gas blow-off valve 19, and when Ar index in detected product gas is less than 1ppb, a product gas outlet hand valve 17 is opened to convey the product gas to the next process.
In a specific embodiment, referring to fig. 2, the low-temperature adsorption reactor 6 comprises an inner cylinder, an interlayer 6A surrounding the circumferential side wall of the inner cylinder, a filler reaction tube 6B arranged inside the inner cylinder, and a heat exchange system arranged at the upper end and the lower end of the inner cylinder; the interlayer 6A is communicated with a liquid nitrogen input pipeline, an adsorbent is arranged in the filler reaction tube 6B, and the adsorbent is formed by mixing activated carbon, alumina and zeolite according to a mass ratio of 1:1:1; the adsorption capacity of the adsorbent is far smaller than that of the adsorbent in a low-temperature state at normal temperature, and the adsorption capacity of the adsorbent can reach 30mL/g in the low-temperature state. Filling liquid nitrogen into the interlayer 6A, wherein the liquid level of the liquid nitrogen in the interlayer 6A is 50-80% of the height of the interlayer 6A; because the low temperature adsorption reactor 6 intermediate layer 6A is filled with liquid nitrogen, provide cold energy environment, all raw materials 5N hydrogen carries out low temperature absorption through the adsorbent, adsorb impurity such as nitrogen in the raw materials 5N hydrogen, argon, oxygen, water, carbon monoxide, carbon dioxide and non-methane hydrocarbon, it is about-180 behind the product gas purification, if directly supply air to the rear end production line, can lead to rear end product gas pipeline dewfall, can have certain corruption to the pipeline, cause the loss of rear end production line, in order to avoid the influence of low temperature product gas to the rear end pipeline, this application utilizes the temperature of raw materials gas to heat up the product gas through heat transfer system, utilize the low temperature of product gas to cool down the raw materials gas simultaneously, realize the heat conduction between raw materials gas and the product gas, specifically:
the heat exchange system comprises a raw material gas heat exchange pipe 6C arranged in the interlayer 6A and a product gas heat exchange pipe 6D arranged in the interlayer 6A, wherein the upper end and the lower end of the low-temperature adsorption reactor 6 are respectively provided with a cavity, a partition plate 6E is fixedly arranged in the cavity, the partition plate 6E divides the corresponding cavity into a raw material gas heat exchange cavity and a product gas heat exchange cavity, and the raw material gas heat exchange cavity positioned at the upper end of the low-temperature adsorption reactor 6 is used as an upper raw material gas heat exchange cavity and the raw material gas heat exchange cavity positioned at the lower end is used as a lower raw material gas heat exchange cavity along the conveying direction of raw material gas; the product gas heat exchange cavity at the upper end is used as an upper product gas heat exchange cavity, the product gas heat exchange cavity at the lower end is used as a lower product gas heat exchange cavity, the upper product gas heat exchange cavity and the lower product gas heat exchange cavity are communicated with the filler reaction tube 6B, normal-temperature raw material gas sequentially passes through a raw material gas input pipeline and the upper raw material gas heat exchange cavity to enter the filler reaction tube 6B, purified hydrogen is obtained after the raw material gas passes through the purification effect of the filler inside the filler reaction tube 6B, and the purified hydrogen sequentially passes through the lower product gas heat exchange cavity, the product gas heat exchange tube 6D and the upper product gas heat exchange cavity to enter the product gas output pipeline. This application establishes ties heat transfer system and filler reaction tube 6B, ensures that the raw materials gas that can normal atmospheric temperature can cool down to low temperature adsorption temperature after heat transfer system, and the product gas after the purification exchanges heat with it simultaneously, heats up, resumes to the state 10 ℃ below than room temperature, can directly carry the rear end production line, does not need extra secondary to heat up.
In a specific embodiment, referring to fig. 1 and 2, a liquid level meter 7 for monitoring the liquid level of liquid nitrogen in an interlayer 6A is arranged on a low-temperature adsorption reactor 6, the liquid level condition is monitored through a control system, and the liquid nitrogen is injected into the interlayer 6A of the low-temperature adsorption reactor 6 from a liquid nitrogen inlet 8 valve, so that the cold energy environment of the liquid nitrogen is constantly maintained; the gasified liquid nitrogen is discharged through the nitrogen outlet 10, so that the safety problem cannot occur due to overpressure inside the security interlayer 6A.
In the specific embodiment, a nitrogen purging pipeline is arranged on the low-temperature adsorption reactor 6, and a purging nitrogen inlet 9 is communicated with the interlayer 6A through a nitrogen purging pipeline and a purging nitrogen inlet 9 valve; the purge nitrogen outlet 10 communicates with the off-gas discharge port 26 through a product gas purge valve 25.
In a specific embodiment, the low-temperature adsorption reactor 6 is communicated with a pressure relief pipeline, a safety valve is installed on the pressure relief pipeline at the bottom of the low-temperature adsorption reactor 6 to prevent the increase of pressure in the cylinder caused by the volume expansion of gas due to temperature rise in the cylinder, and a pressure sensor of the low-temperature adsorption reactor 6 is additionally arranged at the front end of the pressure relief pipeline to ensure that when the safety valve is tripped, a high pressure alarm is given, and the low-temperature adsorption reactor 6 is communicated with the safety relief port 13 through the pressure sensor of the low-temperature adsorption reactor 6.
Example 2
A method for purifying hydrogen using the purification apparatus disclosed in example 1, comprising the steps of:
s1: purification stage
(1) Preparation before purification: the working tower is activated and regenerated, and the adsorbent is deactivated for one time under the condition of first starting, so that the adsorbent recovers the adsorption capacity again, and impurities contained in the raw material gas can be adsorbed and removed normally.
The step is one of key steps for ensuring the purity of the product gas to be 9N hydrogen, and is used for blowing off impurities contained in a pipeline system, so that the reduction of adsorption time and the economic waste caused by the over high concentration of the impurities contained in the pipeline are prevented; meanwhile, the purifier is a hydrogen purifier, so that the purity in the tank cannot be guaranteed in the transportation process, and the adsorbent is in the air for a long time and is already adsorbed and saturated, so that the adsorbent needs to be regenerated and activated, the adsorption capacity of the adsorbent is recovered again, and the gas production is guaranteed to be 9N hydrogen with high purity. Avoiding unnecessary economic cost waste caused by the earlier stage.
(2) Pre-cooling preparation: because the whole purification condition needs low temperature, the valve is opened through the liquid nitrogen inlet 8, the low-temperature adsorption reactor 6 is filled with liquid nitrogen, the temperature of the whole reaction container is reduced, and the working tower needs to be subjected to deep precooling after the regeneration is finished, so that one condition of the adsorption reaction is ensured.
The step is one of key steps for ensuring the purity of the product gas to be 9N hydrogen, and because the whole adsorption environment is an extremely low-temperature reaction environment, the whole working tower is required to be cooled before the whole purification is started, and a temperature condition capable of carrying out low-temperature adsorption reaction is reached, so that the low-temperature adsorption capacity is maximized, and the raw material 5N hydrogen is purified into high-purity 9N hydrogen.
(3) The purification process comprises the following steps: after the preparation of the two steps (1) and (2), the raw material gas can be introduced into a pipeline system, the raw material gas is input into a low-temperature adsorption reactor 6 through a reactor inlet pneumatic valve 5, impurities contained in the raw material gas are removed by utilizing adsorbents contained in a working tower, meanwhile, a user needs to monitor the product gas index output by a purifier at an outlet, and the purified product gas can be output for production after reaching standards.
The step is a step of starting purification of the working tower, and because the working tower is fully immersed in a liquid nitrogen environment, the main conditions of the low-temperature adsorption reaction are ensured, so that the raw material hydrogen starts to undergo the low-temperature adsorption reaction after passing through a special adsorbent, and impurities such as nitrogen, argon, oxygen, water, carbon monoxide, carbon dioxide, non-methane and the like contained in the raw material 5N-level hydrogen are adsorbed and removed, and further the high-purity 9N-level hydrogen is produced, thereby meeting the gas purity required in the semiconductor production process.
S2: regeneration phase
(1) Preparation before regeneration: because the regeneration process is in a high-temperature regeneration state, the normally adsorbed low-temperature adsorption reactor 6 is in an extremely low-temperature state, so that the liquid nitrogen contained in the interlayer 6A needs to be purged, normal-temperature nitrogen is introduced through the purging nitrogen inlet 9, is injected into the interlayer 6A of the low-temperature adsorption reactor 6 through the valve of the purging nitrogen inlet 9, and is purged to the normal-temperature state through a period of liquid nitrogen purging process.
This step is an important step to ensure safe regeneration of the device. Since the normal low-temperature adsorption process is extremely low-temperature and the regeneration process is high-temperature, if the whole reactor is restored to room temperature at the beginning of regeneration, the inside of the reactor is cracked, and the low-temperature adsorption reactor 6 is damaged, so that the liquid nitrogen in the interlayer 6A inside the low-temperature adsorption reactor 6 needs to be purged before the beginning of regeneration.
(2) The regeneration process comprises the following steps: the purified product gas is utilized, and the temperature of the regenerated product gas is raised to be higher than 300 ℃ through a regeneration pipeline, a regeneration valve 20, a regeneration inlet valve 21 and a heater 22, so that the temperature of a regeneration tower bed layer is raised, the adsorption capacity of the bed layer adsorbent is restored again, the adsorption capacity can be normally reached, and then the regenerated product gas is discharged through a waste gas discharge port 26 through a regeneration outlet valve 23 and a regeneration discharge valve 24.
The method has the advantages that the product gas is utilized for regeneration, so that the purity of the pipeline can be ensured; and meanwhile, reverse regeneration is utilized to prevent the regenerated waste gas from being in gas communication with a product gas pipeline, so that the purity of the product gas is polluted.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. The 9N ultra-pure low-temperature hydrogen purification device comprises a standby low-temperature adsorption reactor (6), a raw material gas input pipeline, a product gas output pipeline, a liquid nitrogen input pipeline, a nitrogen purging pipeline, an exhaust gas discharge pipeline, a corresponding switching valve and a control system, wherein the standby low-temperature adsorption reactor (6) is respectively in a purification stage and a regeneration stage, the low-temperature adsorption reactor (6) in the purification stage is used as a working tower, the low-temperature adsorption reactor (6) in the regeneration stage is used as a regeneration tower, a bypass of the product gas output pipeline is connected with a regeneration gas input pipeline, the regeneration gas input pipeline is communicated with the regeneration tower, and a heater (22) is arranged on the regeneration gas input pipeline; the low-temperature adsorption reactor is characterized in that the low-temperature adsorption reactor (6) comprises an inner cylinder, an interlayer (6A) encircling the circumferential side wall of the inner cylinder, a filler reaction tube (6B) arranged in the inner cylinder, and a heat exchange system arranged at the upper end and the lower end of the inner cylinder, wherein the interlayer (6A) is communicated with a liquid nitrogen input pipeline, an adsorbent is arranged in the filler reaction tube (6B), and the adsorbent is formed by mixing activated carbon, alumina and zeolite; the heat exchange system is used for cooling the raw material gas and heating the product gas.
2. The 9N ultra-pure low-temperature hydrogen purification device according to claim 1, wherein the heat exchange system comprises a raw gas heat exchange tube (6C) and a product gas heat exchange tube (6D), cavities are respectively arranged at two ends of the inner cylinder, a partition plate (6E) is arranged in each cavity, the partition plate (6E) divides the cavities into a raw gas heat exchange cavity and a product gas heat exchange cavity, the raw gas heat exchange tube (6C) is communicated with an upper raw gas heat exchange cavity and a lower raw gas heat exchange cavity, the product gas heat exchange tube (6D) is communicated with an upper product gas heat exchange cavity and a lower product gas heat exchange cavity, the upper raw gas heat exchange cavity and the lower product gas heat exchange cavity are both communicated with a filler reaction tube (6B), the lower raw gas heat exchange cavity is communicated with a raw gas input pipeline, and the upper product gas heat exchange cavity is communicated with a product gas output pipeline.
3. The 9N ultra-pure low-temperature hydrogen purification device according to claim 2, wherein one end of the raw material gas heat exchange tube (6C) is communicated with the lower raw material gas heat exchange cavity, and the other end penetrates through the interlayer (6A) and is communicated with the upper raw material gas heat exchange cavity; one end of the product gas heat exchange tube (6D) is communicated with the lower product gas heat exchange cavity, and the other end of the product gas heat exchange tube penetrates through the interlayer (6A) and is communicated with the upper product gas heat exchange cavity.
4. A 9N ultra-pure cryogenic hydrogen purification device according to claim 1, wherein the mass ratio of activated carbon, alumina and zeolite is 1:1:1.
5. The 9N ultra-pure low-temperature hydrogen purification device according to claim 1, wherein the product gas output pipeline is provided with a carbon dioxide remover (15), and the product gas is adsorbed at normal temperature by the carbon dioxide remover to remove a small amount of impurities contained in the product gas again, and then directly enters the next working procedure or enters the regenerated gas input pipeline.
6. The 9N ultra-pure low temperature hydrogen purification device according to claim 1, wherein a bypass of the product gas output pipeline is connected with a product gas detection pipeline, the product gas detection pipeline is communicated with an exhaust gas discharge pipeline, and an Ar index in the product gas can be less than 1ppb.
7. The 9N ultra-pure low temperature hydrogen purification device according to any one of claims 1-6, wherein the low temperature adsorption reactor (6) is communicated with a pressure relief pipeline, the pressure relief pipeline is provided with a safety valve and a pressure sensor, and when the safety valve is tripped, a high pressure alarm is given.
8. The 9N ultra-pure low-temperature hydrogen purification device according to claim 1, wherein a liquid level meter (7) for monitoring the liquid level of liquid nitrogen in the interlayer (6A) is arranged on the low-temperature adsorption reactor (6), and the liquid level of the liquid nitrogen in the interlayer (6A) is controlled to be 50-80% of the height of the interlayer (6A).
9. The apparatus according to claim 1, wherein the product gas output line and the raw gas input line are each provided with a pressure sensor, and the adsorbent is agglomerated or pulverized when the pressure drop is greater than 0.2MPa by comparing the inlet-outlet pressure drop, and then the adsorbent is replaced.
10. A method for purifying hydrogen using a 9N ultra-pure cryogenic hydrogen purification apparatus according to any one of claims 1-9, wherein impurities contained in raw 5N grade hydrogen are removed to yield a 9N grade product gas output, comprising the steps of:
purification stage: after the raw material gas enters a working tower, the raw material gas at normal temperature is cooled to a low-temperature adsorption temperature under the action of a heat exchange system, purified hydrogen is obtained through the purification effect of the filler in the raw material gas, the purified hydrogen is taken as product gas, the product gas is output when the temperature of the product gas is raised to 10 ℃ lower than the room temperature under the action of the heat exchange system, and the output product gas enters the next working procedure through a product gas outlet;
regeneration: liquid nitrogen contained in the interlayer (6A) of the regeneration tower is purged by adopting nitrogen, so that the regeneration tower is restored to a room temperature state; and then introducing part of product gas to raise the temperature of the regeneration tower to above 300 ℃, and removing the saturated impurities adsorbed in the adsorbent at high temperature to recover the adsorption capacity of the adsorbent.
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