WO2000060293A1 - Procede et dispositif de production d'un gaz ultra pur - Google Patents

Procede et dispositif de production d'un gaz ultra pur Download PDF

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Publication number
WO2000060293A1
WO2000060293A1 PCT/JP2000/002194 JP0002194W WO0060293A1 WO 2000060293 A1 WO2000060293 A1 WO 2000060293A1 JP 0002194 W JP0002194 W JP 0002194W WO 0060293 A1 WO0060293 A1 WO 0060293A1
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WO
WIPO (PCT)
Prior art keywords
gas
rectification column
rectification
column
purity
Prior art date
Application number
PCT/JP2000/002194
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English (en)
Japanese (ja)
Inventor
Naohiko Yamashita
Original Assignee
Air Liquide Japan, Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Air Liquide Japan, Ltd. filed Critical Air Liquide Japan, Ltd.
Publication of WO2000060293A1 publication Critical patent/WO2000060293A1/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146—Multiple effect distillation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/30—Processes or apparatus using separation by rectification using a side column in a single pressure column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/58—Argon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

Definitions

  • the present invention provides a method for producing an ultra-high-purity gas by purifying a preliminarily purified raw material fluid in a first rectification column, guiding the obtained high-purity fluid to a second rectification column, and performing further purification. And an apparatus for producing the same, which is particularly useful for producing ultra-high purity argon. Background art
  • Separation and purification of various gases using a rectification column is used for technologies for separating low-temperature components from air and technologies for recovering useful gases with high purity from exhaust gases from various industrial equipment.
  • the basic principle of the rectification column is to use a phenomenon in which the composition of gas and liquid in vapor-liquid equilibrium is different to separate the reflux liquid flowing down the rectification section inside the column and the vapor rising up the rectification section.
  • high-boiling components are concentrated below the rectification section and low-boiling components are concentrated above.
  • a condenser and a reboiler are usually provided at the top and the bottom of the rectification column.
  • the raw material fluid is purified in the first rectification column, and the obtained high-purity gas or the like is guided to the second rectification column. Further purification methods are often employed. Accordingly, many methods for producing various types of high-purity gas using a plurality of rectification columns have been filed.
  • Japanese Patent No. 2594604 discloses that a raw material fluid is guided to a first rectification column to extract a purified bottom liquid, which is then passed through a middle stage of a second rectification column. And a method for recovering ultra-high-purity gas from the top of the tower is described. At that time, Each of the 1st and 2nd rectification towers is equipped with a condenser and a reboiler. It is configured so that rectification conditions suitable for recovery of each rectification column can be adjusted for each rectification column.
  • Japanese Patent Publication No. 7-8577 61 discloses that while a part of the gas at the bottom of the first rectification tower is supplied to the bottom of the second rectification tower, It describes a method for recovering ultrapure substances from the top of the second rectification column while returning the liquid extracted from the bottom to the bottom of the first rectification column. In addition, there is described a method in which a part of the reflux liquid generated by the condenser of the first rectification column is led to the top of the second rectification column to make the reflux liquid of the second rectification column. .
  • the device configuration is simplified in a type in which gas and liquid are supplied in both directions between the first rectification column and the bottom of the second rectification column to omit the repoiler.
  • the purity of the product gas is easily reduced when the raw material composition changes due to the small flexibility of control to enable the recovery of ultra-high purity fluid. there were.
  • the amount of reflux and the amount of reboil need to be finely adjusted independently, since the reboiler does not exist in the second rectification column, the adjustment becomes difficult, and it becomes difficult to maintain the product purity.
  • an object of the present invention is to provide a method for producing an ultra-high-purity gas, which has a simple apparatus configuration, is advantageous in cost, and can maintain a high purity of the ultra-high-purity gas, and an apparatus therefor. is there. Disclosure of the invention
  • the ultra-high-purity process has a process in which the pre-purified raw material fluid is purified in the first rectification column, the resulting high-purity fluid is guided to the second rectification column, and further purified to produce ultra-high-purity gas.
  • the gas production method a part of the reflux liquid on the top side of the first rectification column from the supply section of the raw material fluid is guided to the top section of the second rectification column while adjusting the flow rate, and the reflux liquid
  • the method is characterized in that ultrahigh-purity substances are recovered from the rectification section or the bottom of the second rectification column while returning the gas at the column top to the column top side of the first rectification column.
  • the “ultra-high-purity gas” refers to a gas having a higher purity than a gas purified by one rectification column, and has only a relative meaning.
  • the condenser of the second rectification column can be eliminated.
  • the reflux liquid was allocated by adjusting the capacity of the condenser of each column, but in the present invention, the allocation can be easily performed by adjusting the flow rate of the reflux liquid supplied to the second rectification column. Can be.
  • the amount of reboil in each column can be adjusted independently, the amount of recirculation and the amount of reboil are adjusted when the amount of product fluid recovered is adjusted so that product purity does not decrease when the raw material composition changes. It can be finely adjusted independently, and the purity of ultra-high-purity gas can be kept high.
  • the flow of the reflux liquid and the gas between the first rectification column and the second rectification column can be performed by using various types of propulsion, but the reflux from the first rectification column
  • the flow rate of the reflux liquid is adjusted by opening a valve provided in the path while flowing the reflux liquid using a height difference.
  • the gas may be caused to flow using the pressure difference between the two towers. preferable.
  • additional equipment The recirculation liquid can be easily allocated by the valve opening while securing the propulsion necessary for the flow while minimizing the flow rate.
  • various types of reboil systems can be adopted, but after mixing the bottom solution of the first rectification column and the bottom solution of the second rectification column, the pressure is reduced to reduce the pressure of the first rectification column.
  • the gas vaporized in the refrigerant storage part is compressed by the compressor, and then distributed by the valves provided in each of the branched paths, and reboiled to the bottom of each column as reboil gas.
  • the ultrapure substance is recovered from the middle of the rectification section of the second rectification column together with the supply. In this case, the reboil amount allocation can be easily adjusted.
  • the raw material fluid may be preliminarily purified so as not to hinder rectification, but the raw material fluid is argon having a purity of 95% by volume or more and a substance having a lower boiling point. And a substance having a higher boiling point as impurities.
  • the higher boiling substances can be almost completely removed in the first rectification column, so that ultra-high purity argon is produced by removing the lower boiling substances in the second rectification column. can do.
  • the production apparatus of the present invention has a rectification section having a supply section for the raw material fluid in the middle, and a gas condenser from the rectification section that is liquefied and partially supplied as a reflux liquid.
  • a reflux liquid supply pipe that guides the gas to the top of the second rectification column through a valve whose opening can be adjusted; and A gas supply pipe leading to the side, and a bottom liquid of the first rectification column and a bottom liquid of the second rectification column are mixed, and then the pressure is reduced and the mixture is introduced into the refrigerant storage section of the condenser.
  • the gas vaporized in the refrigerant storage unit is compressed by the compressor, the gas is distributed by valves provided in each of the branched paths, and a recycle path is supplied to the bottom of each of the towers as reboil gas. It is a thing.
  • the apparatus configuration is simple and advantageous in terms of cost, and the purity of the ultrahigh-purity gas can be kept high.
  • Refrigerant supply to vessel, each tower Can be adjusted.
  • FIG. 1 is a schematic configuration diagram illustrating an example of an apparatus used in the manufacturing method according to the first embodiment of the present invention.
  • FIG. 2 is a schematic configuration diagram illustrating an example of an apparatus used in the manufacturing method according to the second embodiment.
  • FIG. 3 is a schematic configuration diagram illustrating an example of an apparatus used in the manufacturing method according to the third embodiment.
  • FIG. 4 is a schematic configuration diagram illustrating an example of an argon recovery facility using the third embodiment.
  • 10 is the first rectification column
  • 11 is the rectification section
  • 12 is the rectification section
  • 13 is the condenser
  • 16 is the expansion valve
  • 20 is the second rectification tower
  • 21 Is a rectification section
  • 31 is a valve
  • 39 is a compressor
  • L8 is a reflux liquid supply pipe
  • L9 is a gas supply pipe.
  • FIG. 1 As the first embodiment of the present invention, the simplest embodiment as shown in FIG. 1 will be exemplified.
  • the raw material fluid is supplied to the first rectification column 10 from the line L1.
  • preliminarily refining, cooling, compression and the like are usually performed by equipment not shown.
  • components that are difficult to remove in the rectification column impurities such as solid components such as dust are removed, and a purification operation is performed to make the raw material of the pellets to a considerably high purity.
  • Cooling and compression are performed to bring the temperature and pressure of the raw material fluid to a range suitable for feeding to the rectification column 10, and are usually slightly higher than the feed section of the first rectification column 10. It is compressed to pressure and cooled to near the liquefaction temperature at that pressure.
  • a rectification section 12 (enrichment section) is provided on the top side (upper side) of the raw material fluid supply section inside the first rectification column 10, and a bottom side (lower side) of the supply section. Is equipped with a rectification section 1 1 (recovery section).
  • the types of the rectifying sections 11 and 12 include a tray type and a filling type, and any type can be adopted.
  • the rectification sections 1 1 and 1 2 the descending reflux liquid and By repeating vaporization and condensation while the vapor ascending is in gas-liquid contact, high-boiling impurities are concentrated below the rectification sections 11 and 12, and products and low-boiling impurities are concentrated above.
  • An external reboiler 14 is provided at the bottom of the first rectification column 10, and the bottom liquid is withdrawn from a route L2 at the bottom of the column and evaporated to be reboiled from a route L3. To the bottom of the tower. Part of it is discharged from L4 as effluent.
  • the type and heat source of the reboiler 14 may be any.
  • an external condenser 13 is provided at the top of the first rectification column 10, and the top gas is extracted from the line L5 at the top of the column, and a part of the gas is liquefied. As a result, the reflux liquid is returned to the top of the tower from line L6. At that time, the concentrated low-boiling component gas is discharged from 7 as an exhaust gas.
  • the type, the cooling medium, and the like of the condenser 13 may be any.
  • the obtained high-purity fluid is guided to the second rectification column 20 for further purification.
  • a part of the reflux liquid at the top of the first rectification column 10 was withdrawn from the feed section of the raw material fluid, and was led to the top of the second rectification column 20 to be used as the reflux liquid.
  • the gas at the top is returned to the top of the first rectification column 10.
  • a reflux liquid supply pipe L8 in which a valve 31 is interposed between the first rectification column 10 and the second rectification column 20 is provided, and the reflux liquid flows using the height difference.
  • the amount of reflux liquid introduced can be adjusted by the opening of the valve 31.
  • the gas at the top of the second rectification column 20 flows through the gas supply pipe L9 due to the pressure difference between the two columns, and is returned to the top of the first rectification column 10.
  • the introduced reflux liquid evaporates while descending through the rectification section 21 in the second rectification column 20 while making gas-liquid contact with the rising steam.
  • the product is in a state in which the lower the rectifying section 21 is, the lower the boiling point impurities are concentrated in the upper side. For this reason, an ultra-high-purity product fluid (product gas) can be recovered from the space above the bottom of the second rectification column 20 in the channel L10.
  • An external reboiler 22 is provided at the bottom of the second rectification column 20, and the bottom liquid is extracted from a path L 11 at the bottom of the column and evaporated to obtain a liquid from the line L 12. It is returned to the bottom of the tower as reboil gas. If the product fluid is in the middle of the rectification section 21 Can also be recovered.
  • the type and heat source of the reboiler 22 may be any.
  • the control method of the rectification operation in the above device is as follows.
  • the rectification operation of the first rectification column 10 and the second rectification column 20 is controlled by ⁇ ; adjusting the capacity of the condenser 13 and distributing the generated reflux liquid to each column by the valve 31 This is done by adjusting the balance.
  • the balance is adjusted by adjusting the flow rate of the reflux liquid supplied to the second rectification column 20, and the second rectification tower 20 adjusts the capacity of the reboiler 22 and the product in accordance with the flow rate of the reflux liquid.
  • the gas recovery amount is adjusted, and as a result, the rectification operation of the second rectification column 20 can be optimally controlled.
  • a first rectification column 10 of the first embodiment further having a rectification section 15 added thereto is exemplified. Note that the other parts are the same as in the first embodiment, and therefore only different parts will be described.
  • the rectifying section 15 is located above the rectifying section 12 (to the top of the tower) and above the connection between the reflux liquid supply pipe L 8 and the gas supply pipe L 9 (to the top of the tower). Is provided.
  • the reflux liquid returned to the tower top from the condenser 13 is directly drawn out of the reflux liquid supply pipe L8, whereas in the second embodiment, the reflux liquid is discharged from the condenser 13 While the reflux liquid returned to the top of the column descends through the rectification section 15, low-boiling-point impurities are further removed, and then are withdrawn through the reflux liquid supply pipe L8. As a result, the removal of low-boiling impurities in the second rectification column 20 is facilitated.
  • FIG. 3 an embodiment in which a recycling path, a heat exchanger, and the like are added to the first embodiment to improve heat efficiency and effectively use exhaust gas and the like is illustrated. . Since the basic parts are the same as in the first embodiment, only the added parts will be described.
  • the present embodiment is characterized in that a recycle path having a function of supplying a refrigerant to the condenser 13 is provided in place of the reboilers 14 and 22 of the first embodiment.
  • this recycling path first, the bottom liquid of the first rectification column 10 and the bottom liquid of the second rectification column 20 are mixed. Transfer the liquid to the bottom of the first rectification column 10 This is done by flowing down the road L11.
  • the mixed bottom liquid of the first rectification column 10 flows to the expansion valve 16 and is subjected to JE through the expansion valve 16 to be introduced into the refrigerant storage section of the heat sink 13 to be cooled by the cooling source.
  • the insufficient cold is supplied from the cold source via the valve L13 via the valve 17 as necessary.
  • the bottom liquid vaporized in the refrigerant storage section is heated by the heat exchanger 32 and then compressed by the compressor 39.
  • a small amount of the bottom liquid is compressed by the compressor 3 so that the high-boiling components are not concentrated in the recycling path. It is discharged from the upstream side of 9 through a valve 38.
  • the path is bifurcated, and the flow is adjusted and distributed by valves 36 and 37 provided in each path L14 and L15. Then, after being cooled in the heat exchanger 32, it is supplied as reboil gas to the bottom of each tower from the lines L12 and L3.
  • a type (aluminum / plate fin condenser) in which a liquid refrigerant is stored and a part of the liquid refrigerant is evaporated to cool and compress the gas at the top of the column is used.
  • a discharge path may be provided (not shown), and a part of the liquid refrigerant may be extracted, vaporized, and then discharged.
  • the raw material fluid is flow-regulated by the valve 34, cooled by the heat exchanger 32, and then supplied from the path L1 to the first rectification column 10 to perform the same rectification operation as in the first embodiment. It is done.
  • the gas that has not been condensed and liquefied is discharged through a path L7, while the liquefied gas is returned to the top of the tower as a reflux liquid.
  • the gas discharged in the route L7 is collected by the heat exchanger 32 in the cold state and then discharged through the valve 33.
  • a rectification section 23 is further provided below the rectification section 21 of the second rectification tower 20 (to the bottom of the tower), and the product gas is recovered by a route L10 connected therebetween. Do. If the above-described recycling route is configured, the purity at the bottom of the second rectification column 20 is likely to decrease, but such a rectification section 23 is provided, and By collecting the product, impurities at the bottom of the tower can be prevented from mixing into the product gas.
  • the product gas recovered from the second rectification column 20 is cold-recovered in the heat exchanger 32 and then discharged through the valve 35. (Argon recovery equipment)
  • FIG. 4 shows an example of a flow sheet of an argon recovery facility using the production method of the third embodiment.
  • This equipment consists of a single-crystal silicon pulling device 1, a pre-purification unit 6, a cooling unit 40, a decarburization drying unit 50, a low-If unit 60, and a high-purity argon tank 90.
  • the apparatus shown in FIG. 3 is employed as the low-temperature purification section 60.
  • the single crystal silicon pulling apparatus 1 is supplied with high-purity argon gas (boiling point: 186 ° C) as a shielding gas from the pipe P1.
  • Monocrystalline silicon pulling apparatus 1 is discharged by the vacuum bomb 2 gas (hereinafter, referred to as "argon exhaust gas") into the other dust, H 2, N 2, 0 2, CO, C 0 2, Hydrocarbons are contained as impurities. Hydrocarbons are primarily CH 4 below 5 0 vo 1 PPM. In Fig. 4, it is simple! Although only one single-crystal silicon pulling device 1 and one vacuum pump 2 are shown in FIG. 1 for the sake of a dagger, a plurality of devices are actually arranged in parallel. The amount of the argon exhaust gas discharged from the single-crystal silicon lifting device 1 varies depending on the number of operating single-crystal silicon lifting devices 1 and the like, and is therefore temporarily stored in the gas holder 3.
  • the argon exhaust gas stored in the gas holder 3 is introduced into the pre-purification unit 6 by the compressor 5 via the suction filter unit 4. At this time, the dust is removed from the argon exhaust gas by the suction fill unit 4. Further, in order to supplement the amount of oxygen required in the subsequent oxidation step, a small amount of air is added to the argon exhaust gas discharged from the suction filter unit 4 via the pipe P31.
  • the argon exhaust gas is boosted by the compressor 5 to a pressure of about 3.5 to 9.0 kg / cm 2 G. The value of this pressure is set according to the optimum operating conditions in the subsequent decarburization drying process or the argon product pressure.
  • the argon exhaust gas leaving the compressor 5 is introduced into the pre-refining unit 6.
  • the pre-refining unit 6 includes a carbon monoxide oxidizing tower 7 and a deoxo tower 8, and H 2 for deoxidation is supplied to the deoxo tower 7 from a hydrogen gas source outside the system via a pipe p32.
  • Argon gas is first introduced into a carbon monoxide oxidation tower 7, changes are oxidized by connexion CO to P d catalyst C 0 2. Then, after H 2 is added, Introduced into tower 8. In Dokiso column 8, reaction of the 0 2 and H z by Pd catalyst is accelerated, 0 2 is changed to the H 2 0.
  • the flow rate of H 2 added in the deoxo tower 8 to remove O 2 almost completely is set excessively to the theoretically required amount.
  • Argon gas (hereinafter referred to as “doxo argon gas j”) leaving the pre-refining facility 6 is introduced into the cooling unit 40.
  • the cooling unit 40 includes a water-cooled heat exchanger 41 and a separator 43. It comprises a heat exchanger 45 equipped with a refrigerator 46 and a water separator 47.
  • Deoxo argon gas is first introduced into the heat exchanger 41 and cooled to about 40 ° C.
  • the obtained deoxo argon gas is introduced into the separator 43 to separate the condensed water, and then the deoxo argon gas is cooled to about 10 ° C. in the heat exchanger 45.
  • Deoxo argon gas is introduced into the water separator 47, where the condensed water is further separated.
  • the deoxo argon gas exiting the cooling unit 40 is introduced into the decarburization drying unit 50.
  • the decarburization drying unit 50 includes a pair of adsorption towers 51 and 52 used alternately.
  • the B ⁇ tower 51 and 52 for adsorbing H 2 0 and C0 2, filler such as alumina and molecular sieves are filled. Since the pair of adsorption towers 51 and 52 are operated using the principle of pressure swing adsorption (PSA) or temperature swing adsorption (TSA), a pipe P 50 for supplying nitrogen gas is used for regeneration of the adsorbent.
  • PSA pressure swing adsorption
  • TSA temperature swing adsorption
  • the deoxo argon gas leaving the decarburization drying unit 50 is introduced into the heat exchanger 32 of the low-temperature purification section 60 at a temperature of about 10 ° C and a pressure of about 6.4 kg / cm 2 G.
  • the composition at that time for example, N 2: 2. 0vo l%, CH 4: 0. 005vo l%, H 2: in 0. 5 vo 1%, the remainder being argon.
  • the rectification operation as in the third embodiment described above is performed, and ultra-high-purity argon gas (purity of 99.999% or more) is recovered as a product gas.
  • high-purity liquid argon is supplied from the tank 90 as a cold source.
  • the product gas is introduced into the product filter facility 70 through the pipe P15, and after the dust is removed to the level of cleanliness required for the introduction of the single crystal silicon lifting device 1, it is returned to the single crystal silicon lifting device 1 again. Supplied. Initially or as a shortage, pull up single-crystal silicon.
  • the high-purity argon gas supplied to the apparatus 1 is introduced into the evaporator 95 from the tank 90 via the valve V8 and gasified.
  • the manufacturing method and manufacturing apparatus of the ultrapure gas of the present invention have a simple apparatus configuration and are advantageous in terms of cost, and can maintain a high purity of the ultrapure gas. Therefore, it can be used for the production of various ultra-high-purity gases, and is particularly useful for producing ultra-high-purity argon.

Abstract

L'invention concerne un procédé de production d'un gaz ultra pur consistant à raffiner une matière brute préraffinée fluide dans une première colonne de raffinage (10) et à guider le fluide très pur ainsi obtenu vers une seconde colonne de raffinage (20) en vue d'un raffinage ultérieur. Ce procédé est caractérisé en ce que cette partie d'un liquide refluant plus proche du haut de la colonne que de la section d'alimentation de la matière brute de la première colonne de raffinage (10) est guidée vers le haut de la colonne de la seconde colonne de raffinage (20) alors que son débit est régulé pour former un liquide refluant et alors que le gaz dans le haut de la colonne est renvoyé vers le haut de la colonne de la première colonne de raffinage (10), et en ce qu'une substance ultra pure est recouverte depuis la section de raffinage (20). L'invention concerne aussi un dispositif associé, facile à construire et peu coûteux, conçu pour préserver la pureté d'un gaz ultra pur à son plus haut niveau.
PCT/JP2000/002194 1999-04-05 2000-04-05 Procede et dispositif de production d'un gaz ultra pur WO2000060293A1 (fr)

Applications Claiming Priority (2)

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JP11/97142 1999-04-05
JP09714299A JP4242507B2 (ja) 1999-04-05 1999-04-05 超高純度ガスの製造方法及び製造装置

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KR (1) KR100680921B1 (fr)
TW (1) TW449495B (fr)
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CN110508022A (zh) * 2019-10-11 2019-11-29 唐山三孚电子材料有限公司 不利用不凝气体控制精馏塔塔压的装置及方法

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