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JPH0256213A - Low boiling point substance purification method - Google Patents

Low boiling point substance purification method

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Publication number
JPH0256213A
JPH0256213A JP1095873A JP9587389A JPH0256213A JP H0256213 A JPH0256213 A JP H0256213A JP 1095873 A JP1095873 A JP 1095873A JP 9587389 A JP9587389 A JP 9587389A JP H0256213 A JPH0256213 A JP H0256213A
Authority
JP
Japan
Prior art keywords
boiling point
raw material
adsorption tower
purified
point substance
Prior art date
Legal status (The legal status 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 status listed.)
Granted
Application number
JP1095873A
Other languages
Japanese (ja)
Other versions
JP2621975B2 (en
Inventor
Takashi Nagamura
長村　孝
Naohiko Yamashita
直彦 山下
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Teisan KK
Original Assignee
Teisan KK
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 Teisan KK filed Critical Teisan KK
Priority to JP1095873A priority Critical patent/JP2621975B2/en
Publication of JPH0256213A publication Critical patent/JPH0256213A/en
Application granted granted Critical
Publication of JP2621975B2 publication Critical patent/JP2621975B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0228—Coupling of the liquefaction unit to other units or processes, so-called integrated processes
    • F25J1/0235—Heat exchange integration
    • F25J1/0236—Heat exchange integration providing refrigeration for different processes treating not the same feed 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0005—Light or noble gases
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0005—Light or noble gases
    • F25J1/0007—Helium
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0005—Light or noble gases
    • F25J1/001—Hydrogen
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/0035—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work
    • F25J1/0037—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work of a return 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/004—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by flash gas recovery
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/0062—Light or noble gases, mixtures thereof
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/0062—Light or noble gases, mixtures thereof
    • F25J1/0065—Helium
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/0062—Light or noble gases, mixtures thereof
    • F25J1/0067—Hydrogen
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0221—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using the cold stored in an external cryogenic component in an open refrigeration loop
    • F25J1/0224—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using the cold stored in an external cryogenic component in an open refrigeration loop in combination with an internal quasi-closed refrigeration loop
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0244—Operation; Control and regulation; Instrumentation
    • F25J1/0245—Different modes, i.e. 'runs', of operation; Process control
    • F25J1/0249—Controlling refrigerant inventory, i.e. composition or quantity
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0244—Operation; Control and regulation; Instrumentation
    • F25J1/0245—Different modes, i.e. 'runs', of operation; Process control
    • F25J1/0249—Controlling refrigerant inventory, i.e. composition or quantity
    • F25J1/025—Details related to the refrigerant production or treatment, e.g. make-up supply from feed gas itself
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0257—Construction and layout of liquefaction equipments, e.g. valves, machines
    • F25J1/0275—Construction and layout of liquefaction equipments, e.g. valves, machines adapted for special use of the liquefaction unit, e.g. portable or transportable devices
    • F25J1/0276—Laboratory or other miniature devices
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • 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
    • F25J2215/32—Neon
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/02—Separating impurities in general from the feed 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
    • F25J2270/06—Internal refrigeration with work-producing gas expansion loop with multiple gas expansion loops
    • 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
    • F25J2270/912—Liquefaction cycle of a low-boiling (feed) gas in a cryocooler, i.e. in a closed-loop refrigerator

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

PURPOSE:To adsorb and remove impurities in an raw material to be refined to refine the raw material by cooling an adsorption tower packed with an adsorbent, and passing the low boiling point raw material through the adsorption tower. CONSTITUTION:Liquefied nitrogen is flushed into the closed space A between the adsorption tower 10 and a vessel 6 to gasify the liquefied nitrogen. Consequently, the atmosphere in the closed space A is cooled by the heat of vaporization to a temp. (-208 deg.C) lower than the temp. of the liquefied nitrogen, and the atmosphere in the closed space A is used as the cold source for cooling the adsorption tower 10 and the raw material. The impurities in the raw material (e.g., helium) is filtered off by a separator 7, and the raw material is then introduced into the adsorption tower 10 arranged in the vessel 6 and contg. an adsorbent such as activated carbon and a molecular sieve. Meanwhile, the impurities (e.g., air) separated by the separator 7 is discharged to the outside of the system by a conduit 9 via a heat exchanger 5.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、酸素や窒素等の不純成分を含有し且つ液体窒
素よりも低沸点である、ヘリウムや水素やネオン等の低
沸点物質の被精製原料から、前記不純成分を除去するこ
とにより、前記低沸点物質を精製する方法に関する。Detailed Description of the Invention [Field of Industrial Application] The present invention is directed to the application of low-boiling substances such as helium, hydrogen, and neon, which contain impurity components such as oxygen and nitrogen and have a lower boiling point than liquid nitrogen. The present invention relates to a method of purifying the low boiling point substance by removing the impurity components from the purified raw material.

〔従来の技術〕[Conventional technology]

従来の低沸点物質精製方法につき、ヘリウムの精製方法
を例にとって説明する。A conventional method for purifying a low-boiling point substance will be explained using a method for purifying helium as an example.

ヘリウム精製方法としては、例えば第２図に示す如く、
ヘリウムの被精製原料即ちバルブ（５１）の開栓によっ
て供給される新規の被精製原料が、乾燥器（５３）内へ
送り込まれて該乾燥器（５３）によって水分や二酸化炭
素が吸着除去された上で、冷却のため熱交換器（５５）
を経由させられた後、液体窒素（５６）中に吸着塔（５
７）が浸漬されてなる吸着装置（５８）内へ送り込まれ
て該吸着装置（５８）によって酸素や窒素等の不純成分
が吸着除去されるものがあった。なお、上述の如く不純
成分が除去されて精製されたヘリウムは、ヘリウム液化
装置へ送給されて液化され、所定の容器又は被冷却体へ
送給されるようになっている。As a helium purification method, for example, as shown in Figure 2,
The raw material to be purified of helium, that is, the new raw material to be purified supplied by opening the valve (51), was fed into the dryer (53), where moisture and carbon dioxide were adsorbed and removed. Above, a heat exchanger (55) for cooling
After passing through the adsorption tower (5) in liquid nitrogen (56),
7) is fed into an adsorption device (58) in which impurity components such as oxygen and nitrogen are adsorbed and removed by the adsorption device (58). The helium purified by removing impurities as described above is sent to a helium liquefaction device, liquefied, and delivered to a predetermined container or object to be cooled.

〔発明が解決しようとする課題〕[Problem to be solved by the invention]

かかる従来のヘリウム精製方法によってヘリウムを精製
する場合は、乾燥器（５３）による水分や二酸化炭素の
吸着除去に加え、吸着装置（５８）（実質的に吸着塔（
５７）　）によるわずかの酸素やわずかの窒素等の不純
成分の吸着除去が行われるに過ぎず、より不純成分（具
体的には空気等）の多いヘリウムを精製する必要がある
ときに対処しきれないという問題があった。When purifying helium by such a conventional helium purification method, in addition to adsorption and removal of moisture and carbon dioxide by the dryer (53), an adsorption device (58) (substantially an adsorption tower (
57) ) only adsorbs and removes a small amount of impurity components such as a small amount of oxygen and a small amount of nitrogen, and it is difficult to deal with when it is necessary to purify helium that contains more impurity components (specifically, air, etc.). The problem was that there was no.

また、前記吸着装置（５日）は吸着塔（５７）が周囲の
液体窒素（５６）によって冷却されるものであるため、
該吸着塔（５７）は前記液体窒素（５６）の温度以下に
は冷却されない。ところで、酸素や窒素等の不純成分に
対する活性炭やモレキュラーシーブ（商品名）等の吸着
剤の吸着性能は低温はど優れているので、その吸着性能
を向上させるべく前記吸着塔（５７）を例えば液体窒素
（５６）の温度以下に冷却したいときには、より高価な
寒冷源が必要になるという問題があった。In addition, in the adsorption device (5 days), the adsorption tower (57) is cooled by the surrounding liquid nitrogen (56), so
The adsorption tower (57) is not cooled below the temperature of the liquid nitrogen (56). Incidentally, the adsorption performance of adsorbents such as activated carbon and molecular sieve (trade name) for impurity components such as oxygen and nitrogen is excellent at low temperatures. There is a problem in that when it is desired to cool down to a temperature below the temperature of nitrogen (56), a more expensive cooling source is required.

また、多量の空気がヘリウムに混合している場合、この
空気をこれまでのように吸着剤に吸着させるという方法
では多量の吸着剤を必要とし、吸着装置も大型になり、
従って再生時間も長くなるという問題があった。In addition, when a large amount of air is mixed with helium, the conventional method of adsorbing this air with an adsorbent requires a large amount of adsorbent, and the adsorption equipment becomes large.
Therefore, there is a problem that the playback time becomes long.

本発明はかかる事情に鑑みてなされたものであり、上述
した如き問題を解消し得る低沸点物質精製方法、即ち、
より不純成分の多い低沸点物質を精製し得る低沸点物質
精製方法及び該低沸点物質を高効率にて精製し得る低沸
点物質精製方法を提供することを目的とする。The present invention has been made in view of the above circumstances, and provides a method for purifying a low boiling point substance that can solve the above-mentioned problems, that is,
It is an object of the present invention to provide a method for purifying a low-boiling point substance that can purify a low-boiling point substance containing more impure components, and a method for purifying a low-boiling point substance that can purify the low-boiling point substance with high efficiency.

〔課題を解決するための手段〕[Means to solve the problem]

本発明に係る低沸点物質精製方法は、吸着剤が充填され
た吸着塔を冷却し、該吸着塔内へ前記低沸点物質の被精
製原料を送給して該吸着塔内を経由させることにより、
前記被精製原料中の不純成分を吸着除去して前記被精製
原料を精製する低沸点物質精製方法であって、前記被精
製原料を吸着塔内へ送給する前に、前記被精製原料を冷
却してその不純成分を凝縮液化させ、該不純成分を液化
除去する点に特徴を有している。The low boiling point substance purification method according to the present invention cools an adsorption tower filled with an adsorbent, and feeds the raw material of the low boiling point substance to be purified into the adsorption tower to pass through the adsorption tower. ,
A method for purifying a low-boiling point substance in which the raw material to be purified is purified by adsorbing and removing impurity components in the raw material to be purified, the raw material being cooled before being fed into an adsorption tower. It is characterized in that the impure components are condensed and liquefied, and the impure components are removed by liquefaction.

なお、前記低沸点物質としては、ヘリウム、水素、ネオ
ン等が挙げられる。Note that examples of the low boiling point substance include helium, hydrogen, neon, and the like.

そして、かかる方法を実施するに際しては、前記吸着塔
の周υ■に、真空吸引されて減圧された閉空間を形成す
ると共に、該閉空間内へ液体窒素をフラッシュさせるこ
とにより、該閉空間の雰囲気を前記液体窒素の温度より
も低温に冷却し、該閉空間の雰囲気を、前記吸着塔の冷
却用及び前記吸着塔内へ送給する前の前記被精製原料の
冷却用の寒冷源として兼用することが好ましい。When carrying out such a method, a closed space is formed around the adsorption tower by vacuum suction and reduced pressure, and liquid nitrogen is flushed into the closed space. The atmosphere is cooled to a temperature lower than the temperature of the liquid nitrogen, and the atmosphere in the closed space is used as a cold source for cooling the adsorption tower and for cooling the raw material to be purified before being fed into the adsorption tower. It is preferable to do so.

〔作　用〕[For production]

かかる本発明方法によれば、前記被精製原料が吸着塔内
へ送給される前に、該被精製原料を冷却してその中に含
有される酸素や窒素等の不純成分を凝縮液化させること
としているため、その冷却された被精製原料を例えばセ
パレータにかけることによって前記不純成分を濾過除去
することができる結果、前記不純成分の含有量を減少さ
せた状態で被精製原料を吸着塔内の送給することができ
る。According to the method of the present invention, before the raw material to be purified is fed into the adsorption tower, the raw material to be purified is cooled to condense and liquefy impurity components such as oxygen and nitrogen contained therein. As a result, the impure components can be filtered out by passing the cooled raw material to be purified through a separator, for example, and the raw material to be purified can be transferred into the adsorption tower with the content of the impure components reduced. can be sent.

〔発明の効果〕〔Effect of the invention〕

従って、例えば凝縮器やセパレータによる予備的な精製
処理を行わないまま被精製原料を吸着塔へ送給して酸素
や窒素等の不純成分の吸着除去を行う従来方法に比し、
本発明方法による場合は、上述の如く酸素や窒素等の不
純成分を液化分離した上で被精製原料を吸着塔内へ送給
し、該吸着塔内で更に前記不純成分を吸着除去すること
ができるので、低沸点物質を短時間で精製することがで
きる。従って、より不純成分（具体的には空気等）の多
い低沸点物質も効率よく精製することができる。Therefore, compared to the conventional method in which the raw material to be purified is sent to an adsorption tower without performing preliminary purification treatment using a condenser or separator, impurity components such as oxygen and nitrogen are adsorbed and removed.
In the case of the method of the present invention, the raw material to be purified is fed into an adsorption tower after impurity components such as oxygen and nitrogen are liquefied and separated as described above, and the impurity components are further removed by adsorption within the adsorption tower. Therefore, low-boiling substances can be purified in a short time. Therefore, even low-boiling substances containing more impure components (specifically, air, etc.) can be efficiently purified.

また、被精製原料を吸着塔内へ送給する前に上述の如く
被精製原料を冷却してその中に含有される酸素や窒素等
の不純成分を凝縮液化させるには、何らかの凝縮器が必
要となるが、前記吸着塔を冷却するためにその周囲に、
真空吸引されて減圧された閉空間を形成すると共に、該
閉空間内へ液体窒素をフラッシュさせることにより、該
液体窒素を気化させてその気化熱によって該液体窒素の
温度よりも低温にまで冷却した前記閉空間の雰囲気を、
上述の如く、前記吸着塔内へ送給する前の被精製原料の
冷却用寒冷源としても兼用することとすれば、これが前
記凝縮器として作用することとなって新たに凝縮器を設
ける必要がなくなり、効率的である。なお、前記閉空間
の雰囲気は本来的には前記吸着塔を冷却するのに用いら
れるものであるが、該雰囲気は供給される液体窒素の温
度よりも低温にまで冷却されているため、吸着塔を液体
窒素中に浸漬してこれを冷却する従来方法に比し、より
低温に吸着塔が冷却され、該吸着塔による前記不純成分
の吸着性能も向上する。In addition, some kind of condenser is required to cool the raw material to be purified and condense and liquefy impurity components such as oxygen and nitrogen contained therein as described above before feeding the raw material to be purified into the adsorption tower. However, in order to cool the adsorption tower, around it,
By creating a closed space with reduced pressure by vacuum suction and flashing liquid nitrogen into the closed space, the liquid nitrogen was vaporized and cooled to a temperature lower than the temperature of the liquid nitrogen by the heat of vaporization. The atmosphere of the closed space,
As mentioned above, if it is also used as a cold source for cooling the raw material to be purified before being fed into the adsorption tower, this will act as the condenser and it will be necessary to provide a new condenser. It is efficient. Note that the atmosphere in the closed space is originally used to cool the adsorption tower, but since the atmosphere is cooled to a temperature lower than the temperature of the liquid nitrogen supplied, the adsorption tower Compared to the conventional method in which the adsorption tower is cooled by immersing it in liquid nitrogen, the adsorption tower is cooled to a lower temperature, and the adsorption performance of the impurity components by the adsorption tower is also improved.

〔実施例〕〔Example〕

以下、本発明の実施例を図面に基づいて説明する。 Embodiments of the present invention will be described below based on the drawings.

第１図において、（１）は液体窒素（沸点ニー１９６°
Ｃ）よりも低沸点である低沸点物質の一例たるヘリウム
（沸点ニー２６９°Ｃ）の被精製原料を収納するボンベ
であり、該ボンベ（１）内の被精製原料は、導管（２）
によって乾燥器（３）内へ導かれ、該乾燥器（３）を通
過する間に水分や二酸化炭素が乾燥除去された上で、導
管（４）によって熱交換器（５）内及び空間（６）内を
経由させら゛れた後、セパレータ（７）内へ送給される
ようになっている。In Figure 1, (1) is liquid nitrogen (boiling point knee 196°
This cylinder stores a raw material to be purified of helium (boiling point knee 269°C), which is an example of a low-boiling point substance that has a lower boiling point than C), and the raw material to be purified in the cylinder (1) is connected to a conduit (2).
is introduced into the dryer (3), and while passing through the dryer (3), moisture and carbon dioxide are dried and removed, and then the inside of the heat exchanger (5) and the space (6 ) and then fed into the separator (7).

該セパレータ（７）は、前記被精製原料中の酸素や窒素
等の不純成分を凝縮液化した状態で濾過除去するための
フィルタを備えている。そして該セパレータ（７）から
は２本の導管（８）　、　（９）が引き出されており、
そのうちの一方の導管（８）はセパレータ（７）にて前
記不純成分を濾過除去した被精製原料を前記容器（６）
内に配され活性炭やモレキュラーシーブ等の吸着剤を内
蔵する吸着塔（１０）内へ導く一方、他方の導管（９）
はセパレータ（７）にて濾過除去した前記不純成分（具
体的には空気）を前記熱交換器（５）経由で系外へ導く
ようになっている。The separator (7) is equipped with a filter for filtering and removing impurity components such as oxygen and nitrogen in the raw material to be purified in a condensed and liquefied state. Two conduits (8) and (9) are drawn out from the separator (7),
One of the conduits (8) carries the raw material to be purified, after the impurity components have been filtered out through the separator (7), into the container (6).
One conduit (9) leads to the adsorption tower (10) which contains an adsorbent such as activated carbon or molecular sieve.
The impurity component (specifically, air) filtered out by the separator (7) is guided out of the system via the heat exchanger (5).

さて、前記容器（６）内には前述の如き吸着塔（１０）
が配されているが、容器（６）内であって吸着塔（１０
）の周囲には閉空間（Ａ）が形成されている。そして該
閉空間（Ａ）内の雰囲気は導管（１３）経由で真空ポン
プ（１４）による真空吸引が行われて減圧される一方で
、該閉空間（Ａ）内へは液体窒素容器（１１）内に収納
された液体窒素（温度ニー１９６°Ｃ）が導管（１２）
経由でフラッシュされつつ供給されるようになっている
。なお該液体窒素の一部は後述するヘリウム液化サイク
ル（１６）の寒冷源としても用いられる。Now, inside the container (6) is an adsorption tower (10) as described above.
is placed inside the container (6) and the adsorption tower (10
) A closed space (A) is formed around it. The atmosphere in the closed space (A) is depressurized by vacuum suction by the vacuum pump (14) via the conduit (13), while the liquid nitrogen container (11) is injected into the closed space (A). The liquid nitrogen (temperature: 196°C) stored in the conduit (12)
It is designed to be supplied while being flushed via. A portion of the liquid nitrogen is also used as a cooling source for a helium liquefaction cycle (16), which will be described later.

また、前記吸着塔（１０）を経由することによって酸素
や窒素等の不純成分が吸着除去された被精製原料、即ち
精製済みのヘリウムガスは導管（１５）経由でヘリウム
液化サイクル（１６）へ送給されるようになっている。Further, the raw material to be purified, that is, the purified helium gas, from which impurity components such as oxygen and nitrogen have been adsorbed and removed by passing through the adsorption tower (10), is sent to the helium liquefaction cycle (16) via the conduit (15). They are now being paid.

そして該精製済みのヘリウムガスは前記ヘリウム液化サ
イクル（１６）によって液化され、これによって得られ
る液体ヘリウムは導管（１７）を経由した後、バルブ（
１８）。The purified helium gas is liquefied by the helium liquefaction cycle (16), and the resulting liquid helium passes through the conduit (17) and then passes through the valve (
18).

（１９）の開閉に基づいて被冷却体（２０）又は液体ヘ
リウム容２Ｂ（２１）内へ供給されるようになっζいる
。Based on the opening and closing of (19), the liquid helium is supplied to the object to be cooled (20) or into the liquid helium container 2B (21).

なお、前記ヘリウム液化サイクル（１６）に付設された
バッファタンク（２２）は、前記乾燥器（３）やセパレ
ータ（７）や吸着塔（１０）等を用いて被精製原料が精
製されて得られる前記ヘリウムガスを貯溜しておくもの
であり、前記ボンベ（１）の交換や精製部（乾燥器（３
）や吸着塔（１０）等）の再生等に起因して前記ヘリウ
ムガスの前記ヘリウム液化サイクル（１６）への供給が
不足するときには該バッファタンク（２２）から前記ヘ
リウムガスを供給し、液体ヘリウムを連続的に得ること
ができる結果、例えば前記被冷却体（２０）を連続的に
冷却することができるようになっている。In addition, the buffer tank (22) attached to the helium liquefaction cycle (16) is used to purify the raw material to be purified using the dryer (3), separator (7), adsorption tower (10), etc. It is used to store the helium gas, and is used to replace the cylinder (1) and the purification section (dryer (3).
), adsorption tower (10), etc.), when the supply of helium gas to the helium liquefaction cycle (16) is insufficient, the helium gas is supplied from the buffer tank (22), and liquid helium is As a result, for example, the object to be cooled (20) can be continuously cooled.

なお、前記被冷却体（２０）及び／又は液体ヘリウム容
器（２１）から排出される低温ヘリウムは、バルブ（２
３）　、　（２４）の開閉に基づいて導管（２５）内へ
送給され、更に該導管（２５）、ウオーマ（２Ｇ）　、
回収コンプレッサ（２８）　、油除去装！　（２９）等
を経由して再生用の被精製原料として前記導管（２）へ
戻されると共に、その一部は前記ヘリウム液化サイクル
（１６）の寒冷源として用いられる。なお回収コンプレ
ッサ（２８）の上流側に付設されているホルダ（２７）
は、回収コンプレッサ（２８）にて処理しきれないヘリ
ウムを一旦貯溜するためのものである。Note that the low temperature helium discharged from the object to be cooled (20) and/or the liquid helium container (21) is discharged through the valve (2
3), is fed into the conduit (25) based on the opening/closing of (24), and is further fed into the conduit (25), the warmer (2G),
Recovery compressor (28), oil removal equipment! (29) etc., it is returned to the conduit (2) as a raw material to be purified for regeneration, and a part of it is used as a cold source for the helium liquefaction cycle (16). Note that the holder (27) attached to the upstream side of the recovery compressor (28)
is for temporarily storing helium that cannot be processed by the recovery compressor (28).

かかる構成の設備を用いて本発明方法を実施する場合は
、吸着塔（１０）と容器（６）との間の閉空間（Ａ）内
へ液体窒素をフラッシュさせることにより、該液体窒素
を気化させてその気化熱によって閉空間（＾）の雰囲気
を前記液体窒素の温度よりも低温（具体的には一２０８
°Ｃ）に冷却し、該閉空間（Ａ）の雰囲気を、前記吸着
塔（１０）の冷却用及び前記吸着塔（１０）内へ送給す
る前の前記被精製原料の冷却用の寒冷源として兼用する
ことができる。When carrying out the method of the present invention using equipment with such a configuration, the liquid nitrogen is vaporized by flashing it into the closed space (A) between the adsorption tower (10) and the container (6). The heat of vaporization lowers the atmosphere in the closed space (^) to a temperature lower than the temperature of the liquid nitrogen (specifically, -208
°C), and the atmosphere in the closed space (A) is a cold source for cooling the adsorption tower (10) and for cooling the raw material to be purified before being fed into the adsorption tower (10). It can also be used as

そして、該閉空間（Ａ）の雰囲気で前記吸着等（１０）
を冷却することにより、吸着塔を液体窒素中に浸漬して
これを冷却する従来方法に比し、より低温に吸着塔（１
０）が冷却され、該吸着塔（１０）による前記不純物の
吸着性能が向上する。Then, the adsorption, etc. (10) is carried out in the atmosphere of the closed space (A).
By cooling the adsorption tower (1
0) is cooled, and the adsorption performance of the impurity by the adsorption tower (10) is improved.

また、前記閉空間（＾）の雰囲気で前記被精製原料を吸
着塔（１０）内の送給前に冷却することにより、その中
に含有される酸素や窒素等の不純成分を凝縮液化させ、
その冷却された被精製原料をセパレータ（７）にかける
ことによっ、て前記不純成分を濾過除去することができ
る結果、前記不純成分の含有量を減少させた状態で被精
製原料を吸着塔（１０）内へ送給することができる。Further, by cooling the raw material to be purified in the atmosphere of the closed space (^) before feeding it into the adsorption tower (10), impurity components such as oxygen and nitrogen contained therein are condensed and liquefied,
By applying the cooled raw material to be purified to the separator (7), the impure components can be filtered out. As a result, the raw material to be purified can be passed through the adsorption tower ( 10) Can be delivered to the inside.

また、かかる設備を用いる場合は、被冷却体（２０）を
経ることによって空気が混合したヘリウムガスを捨てる
ことなく回収することができ、高価なヘリウムの有効利
用を図ることができる。Furthermore, when such equipment is used, the helium gas mixed with air can be recovered without being thrown away by passing through the object to be cooled (20), and expensive helium can be used effectively.

なお、上述の実施例においては、前記被精製原料を吸着
塔（１０）内への送給前に冷却してその中に含有される
不純成分を凝縮液化させるのに、前記被精製原料を導管
（４）を用いて容器（６）内へ導き、該容器（６）内の
閉空間（Δ）の雰囲気で冷却することとしたが、導管（
４）の中途に別の凝縮器を設け、該凝縮器にて前記被精
製原料を冷却することも考えられる。In the above embodiment, in order to cool the raw material to be purified and condense and liquefy the impurity components contained therein before feeding the raw material to the adsorption tower (10), the raw material to be purified is passed through the conduit. (4) into the container (6) and cooled in the atmosphere of the closed space (Δ) inside the container (6), but the conduit (
It is also conceivable to provide another condenser in the middle of step 4) and cool the raw material to be purified in this condenser.

〔別実施例〕[Another example]

上述の実施例は、前記低沸点物質がヘリウムである場合
について言及したが、前記低沸点物質がヘリウム以外の
物質、例えば水素（沸点ニー２５３℃）又はネオン（沸
点ニー２４６℃）である場合においても、本発明方法は
上述の実施例と同様にして適用することができる。In the above embodiments, the low boiling point substance is helium, but in the case where the low boiling point substance is a substance other than helium, such as hydrogen (boiling point knee 253°C) or neon (boiling point knee 246°C) The method of the present invention can also be applied in the same manner as in the above embodiments.

また、前記低沸点物質が、ヘリウム、水素及びネオンの
少なくとも二つを含む混合ガスである場合においても、
本発明方法は上述の実施例と同様にして適用することが
できる。Further, even when the low boiling point substance is a mixed gas containing at least two of helium, hydrogen and neon,
The method of the invention can be applied in the same manner as in the embodiments described above.

なお、特許請求の範囲の項に図面との対照を便利にする
為に符号を記すが、該記入により本発明は添付図面にて
示される方法に限定されるものではない。Note that although reference numerals are written in the claims section for convenient comparison with the drawings, the present invention is not limited to the method shown in the accompanying drawings.

【図面の簡単な説明】[Brief explanation of the drawing]

第１図は本発明に係る低沸点物質精製方法の実施状態を
示す模式的説明図、第２図は従来方法の実施状態を示す
模式的説明図である。 （１０）・・・・・・吸着塔、（Ａ）・・・・・・閉空
間。FIG. 1 is a schematic explanatory diagram showing the implementation state of the low boiling point substance purification method according to the present invention, and FIG. 2 is a typical explanatory diagram showing the implementation state of the conventional method. (10)...Adsorption tower, (A)...Closed space.

Claims (1)

【特許請求の範囲】 １、吸着剤が充填された吸着塔（１０）を液体窒素を用
いて冷却し、該吸着塔（１０）内へ液体窒素よりも低沸
点である低沸点物質の被精製原料を送給して該吸着塔（
１０）内を経由させることにより、前記被精製原料中の
不純成分を吸着除去して前記被精製原料を精製する低沸
点物質精製方法であって、前記被精製原料を吸着塔（１
０）内へ送給する前に、前記被精製原料を液体窒素を用
いて冷却してその不純成分を凝縮液化させ、該不純成分
を液化除去する低沸点物質精製方法。 ２、前記低沸点物質がヘリウムである請求項１記載の低
沸点物質精製方法。 ３、前記低沸点物質が水素である請求項１記載の低沸点
物質精製方法。 ４、前記低沸点物質がネオンである請求項１記載の低沸
点物質精製方法。 ５、前記低沸点物質がヘリウム、水素及びネオンの少な
くとも二つを含む混合ガスである請求項１記載の低沸点
物質精製方法。 ６、前記吸着塔（１０）の周囲に、真空吸引されて減圧
された閉空間（Ａ）を形成すると共に、該閉空間（Ａ）
内へ液体窒素をフラッシュさせることにより、該閉空間
（Ａ）の雰囲気を前記液体窒素の温度よりも低温に冷却
し、該閉空間（Ａ）の雰囲気を、前記吸着塔（１０）の
冷却用及び前記吸着塔（１０）内へ給送する前の前記被
精製原料の冷却用の寒冷源として兼用する請求項１記載
の低沸点物質精製方法。[Claims] 1. An adsorption tower (10) filled with an adsorbent is cooled using liquid nitrogen, and a low-boiling substance to be purified having a boiling point lower than that of liquid nitrogen is introduced into the adsorption tower (10). The raw material is fed to the adsorption tower (
10) A low boiling point substance purification method for purifying the raw material to be purified by adsorbing and removing impurity components in the raw material to be purified by passing the raw material to be purified through an adsorption column (10).
0) A method for purifying a low-boiling point substance, in which the raw material to be purified is cooled using liquid nitrogen to condense and liquefy impure components, and the impure components are removed by liquefaction. 2. The method for purifying a low boiling point substance according to claim 1, wherein the low boiling point substance is helium. 3. The method for purifying a low-boiling point substance according to claim 1, wherein the low-boiling point substance is hydrogen. 4. The method for purifying a low-boiling point substance according to claim 1, wherein the low-boiling point substance is neon. 5. The method for purifying a low boiling point substance according to claim 1, wherein the low boiling point substance is a mixed gas containing at least two of helium, hydrogen, and neon. 6. Forming a closed space (A) around the adsorption tower (10), which is vacuum-suctioned and depressurized, and the closed space (A)
By flashing liquid nitrogen into the closed space (A), the atmosphere in the closed space (A) is cooled to a temperature lower than the temperature of the liquid nitrogen, and the atmosphere in the closed space (A) is used for cooling the adsorption tower (10). 2. The method for purifying a low boiling point substance according to claim 1, wherein the cold source also serves as a cold source for cooling the raw material to be purified before being fed into the adsorption tower (10).
JP1095873A 1988-04-15 1989-04-15 Purification method for low-boiling substances Expired - Fee Related JP2621975B2 (en)

Priority Applications (1)

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JP1095873A JP2621975B2 (en) 1988-04-15 1989-04-15 Purification method for low-boiling substances

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Application Number Priority Date Filing Date Title
JP63-94289 1988-04-15
JP9428988 1988-04-15
JP1095873A JP2621975B2 (en) 1988-04-15 1989-04-15 Purification method for low-boiling substances

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JPH0256213A true JPH0256213A (en) 1990-02-26
JP2621975B2 JP2621975B2 (en) 1997-06-18

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004070296A1 (en) * 2003-02-03 2004-08-19 Japan Science And Technology Agency Circulation-type liquid helium reliquefaction apparatus with contaminant discharge function, method of discharging contaminant from the apparatus, and refiner and transfer tube both of which are used for the apparatus
FR2970563A1 (en) * 2011-01-19 2012-07-20 Air Liquide INSTALLATION AND PROCESS FOR PRODUCTION OF LIQUID HELIUM

Families Citing this family (1)

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Publication number Priority date Publication date Assignee Title
KR101236713B1 (en) 2012-02-28 2013-03-25 (주)원익머트리얼즈 Purifying method for pentafluoroethyl iodide

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Publication number Priority date Publication date Assignee Title
JPS59193516U (en) * 1983-06-08 1984-12-22 株式会社日立製作所 low temperature purifier
JPS60169078A (en) * 1984-12-21 1985-09-02 株式会社日立製作所 low temperature purifier

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59193516U (en) * 1983-06-08 1984-12-22 株式会社日立製作所 low temperature purifier
JPS60169078A (en) * 1984-12-21 1985-09-02 株式会社日立製作所 low temperature purifier

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004070296A1 (en) * 2003-02-03 2004-08-19 Japan Science And Technology Agency Circulation-type liquid helium reliquefaction apparatus with contaminant discharge function, method of discharging contaminant from the apparatus, and refiner and transfer tube both of which are used for the apparatus
US7565809B2 (en) 2003-02-03 2009-07-28 Japan Science And Technology Agency Circulation-type liquid helium reliquefaction apparatus with contaminant discharge function, method of discharging contaminant from the apparatus, and refiner and transfer tube both of which are used for the apparatus
FR2970563A1 (en) * 2011-01-19 2012-07-20 Air Liquide INSTALLATION AND PROCESS FOR PRODUCTION OF LIQUID HELIUM
WO2012098326A3 (en) * 2011-01-19 2013-08-29 L'air Liquide,Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Installation and method for producing liquid helium
RU2578508C2 (en) * 2011-01-19 2016-03-27 Л'Эр Ликид, Сосьете Аноним Пур Л'Этюд Э Л'Эксплуатасьон Де Проседе Жорж Клод Unit and method of producing liquid helium
AU2012208462B2 (en) * 2011-01-19 2016-11-10 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Installation and method for producing liquid helium
US9657986B2 (en) 2011-01-19 2017-05-23 L'Air Liquide Société Anonyme Pour L'Étude Et L'Exploitation Des Procedes Georges Claude Installation and method for producing liquid helium

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