US20140326596A1 - Fluorine Gas Generation Apparatus - Google Patents

Fluorine Gas Generation Apparatus Download PDF

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Publication number
US20140326596A1
US20140326596A1 US14/358,630 US201214358630A US2014326596A1 US 20140326596 A1 US20140326596 A1 US 20140326596A1 US 201214358630 A US201214358630 A US 201214358630A US 2014326596 A1 US2014326596 A1 US 2014326596A1
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United States
Prior art keywords
hydrogen fluoride
vaporizer
fluorine gas
fluid level
electrolytic tank
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Abandoned
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US14/358,630
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English (en)
Inventor
Tatsuya Irie
Akifumi YAO
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Central Glass Co Ltd
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Central Glass Co Ltd
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Publication date
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Assigned to CENTRAL GLASS COMPANY, LIMITED reassignment CENTRAL GLASS COMPANY, LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: IRIE, TATSUYA, YAO, AKIFUMI
Publication of US20140326596A1 publication Critical patent/US20140326596A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/245—Fluorine; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/19—Fluorine; Hydrogen fluoride
    • C01B7/20—Fluorine
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features

Definitions

  • the present invention relates to fluorine gas generating devices of a type that is able to stably supply a fluorine gas.
  • a fluorine gas generating to device that comprises an electrolytic tank which electrolyzes hydrogen fluoride in an electrolytic bath that includes a molten salt containing therein hydrogen fluoride and which generates at an anode side thereof a main-product gas that contains as a main component fluorine gas and at a cathode side thereof a by-product gas that contains as a main component hydrogen gas (Patent Documents 1 and 2).
  • hydrogen fluoride is directly fed into the electrolytic bath through a hydrogen fluoride supply passage, from the outside of the electrolytic tank, using a hydrogen fluoride supply source such as a hydrogen fluoride cylinder bottle, a hydrogen fluoride tank or the like.
  • the fluid level of the electrolytic tank lowers since the fluid level at the anode side where fluorine gas is produced is affected by the amount of fluorine gas produced by the fluorine gas generating device.
  • Fluorine gas has a high reactivity, and thus, when the fluid level of the electrolytic tank largely changes, there is such a possibility that fluorine gas and hydrogen gas become mixed to induce a reaction therebetween. Thus, it is important to keep the fluid level of the electrolytic tank at a constant level for suppressing undesired influence to the quantity of generation of fluorine gas. Accordingly, for keeping the fluid level of the electrolytic tank at a constant level, it is necessary to stably feed a sufficient amount of hydrogen fluoride to the tank.
  • the passage through which the gaseous hydrogen fluoride flows is increased in length, so that when a large amount of gaseous hydrogen fluoride is suddenly led into the passage from the hydrogen fluoride supply source, heating of the gaseous hydrogen fluoride in the passage is not sufficiently carried out inducing a possibility of liquefaction of hydrogen fluoride, which tends to cause the liquefied hydrogen fluoride led into the electrolytic tank to make a sudden boiling thereof bringing about a fluctuation of the fluid level of the electrolytic tank.
  • the present invention is provided by taking the above-mentioned problems into consideration and aims to provide a fluorine gas generating device that is able to stably carry out feeding of hydrogen fluoride to an electrolytic tank even when a large amount of fluorine gas is produced.
  • a fluorine gas generating device that generates fluorine gas by subjecting hydrogen fluoride in a molten salt containing therein hydrogen fluoride to an electrolysis
  • the fluorine gas generating device being characterized by an electrolytic tank that generates at an anode side a main-product containing as a main component fluorine gas and at a cathode side a by-product gas containing as a main component hydrogen gas by subjecting, in an electrolytic bath, hydrogen fluoride in a molten salt containing therein hydrogen fluoride to an electrolysis, a hydrogen fluoride supply source that stores therein hydrogen fluoride that is to be fed to the electrolytic tank to fill up hydrogen fluoride, a hydrogen fluoride supply passage through which hydrogen fluoride flows from the hydrogen fluoride supply source to the electrolytic tank and a vaporizer that is connected to the hydrogen fluoride supply passage to vaporize hydrogen fluoride supplied from the hydrogen fluoride supply source.
  • the fluorine gas generating device may have such a feature that the vaporizer comprises a hollow vessel that is equipped with a temperature adjuster and has therein a vaporizing chamber, a hydrogen fluoride inlet portion that introduces thereinto liquefied hydrogen fluoride from the hydrogen fluoride supply source, and a hydrogen fluoride outlet portion that discharges gaseous hydrogen fluoride from the vaporizing chamber.
  • the fluorine gas generating device may further comprise a flow rate control valve that controls a flow rate of hydrogen fluoride led into the vaporizer, a fluid level detecting means that detects a fluid level of hydrogen fluoride contained in the vaporizer and a control means that, in accordance with a detected output from the fluid level detecting means, controls an open degree of the flow rate control valve in such a manner as to cause the fluid level of hydrogen fluoride in the vaporizer to take a given level.
  • a flow rate control valve that controls a flow rate of hydrogen fluoride led into the vaporizer
  • a fluid level detecting means that detects a fluid level of hydrogen fluoride contained in the vaporizer
  • a control means that, in accordance with a detected output from the fluid level detecting means, controls an open degree of the flow rate control valve in such a manner as to cause the fluid level of hydrogen fluoride in the vaporizer to take a given level.
  • controlling of the fluid level of hydrogen fluoride in the vaporizer is facilitated and thus, supplying of hydrogen fluoride is much stably carried out.
  • supplying of hydrogen fluoride from the hydrogen fluoride supply source may be so made that the fluid level of hydrogen fluoride in the vaporizer keeps a given level constantly.
  • a vaporizer is connected to a hydrogen fluoride supply passage for vaporizing liquefied hydrogen fluoride and the amount of hydrogen fluoride received in the vaporizer is adjusted. Accordingly, even when, due to a large generation of fluorine gas by the electrolytic tank, it becomes needed to feed the electrolytic tank with a large amount of hydrogen fluoride, it never occurs that the amount of hydrogen fluoride fed to the tank shows a shortage. Accordingly, feeding of hydrogen fluoride to the tank is stable and thus undesired fluctuation of the fluid level is suppressed, which brings about a stable supply of fluorine gas.
  • FIG. 1 is a system diagram of a fluorine gas generating device that embodies the present invention.
  • FIG. 2 is a schematic view of a vaporizer used in the invention.
  • FIG. 3 is a drawing showing one example of a fluorine gas generating device that mounts both a vaporizer and an electrolytic tank in a common housing.
  • a fluorine gas generating device 100 of an embodiment of the present invention will be described with the aid of FIG. 1 .
  • the fluorine gas generating device 100 is a device that generates fluorine gas by subjecting a molten salt containing therein hydrogen fluoride to an electrolysis and supplies fluorine gas thus generated to an external device.
  • the external device is a semiconductor production device is exemplified. In such case, fluorine gas supplied is used as a cleaning gas in a semiconductor production process.
  • the fluorine gas generating device 100 comprises an electrolytic tank 1 that produces fluorine gas with the aid of electrolysis, a fluorine gas feeding system 2 that feeds fluorine gas produced by electrolytic tank to an external device 4 and a by-product gas treatment system that treats a by-product gas produced together with fluorine gas.
  • the electrolytic tank 1 Within the electrolytic tank 1 , there is stored a molten salt that contains therein hydrogen fluoride (HF).
  • HF hydrogen fluoride
  • the composition of fluorine compound gas produced by the electrolytic tank 1 can be suitably changed.
  • KF ⁇ nHF nitrogen trifluoride
  • NF 3 nitrogen trifluoride
  • NK 4 F ⁇ KF ⁇ HF molten salt mixture of F 2 and NF 3 is obtained.
  • an embodiment of the present invention will be described in case of casing a mixed molten salt (KF ⁇ 2HF) of hydrogen fluoride and potassium fluoride as the molten salt.
  • An interior of the electrolytic tank 1 is partitioned into an anode chamber 11 and a cathode chamber 12 by a partition wall 6 immersed in the molten salt.
  • anode and cathode chambers 11 and 12 there are respectively arranged anode and cathode 7 and 8 that are immersed in the molten salt.
  • a current between the anode and cathode 7 and 8 from an electric power source there are produced at the anode 7 a main-product gas that contains as a main component fluorine gas (F 2 ) and at the cathode 8 a by-product that contains as a main component hydrogen gas (H 2 ).
  • the anode 7 there is used for is example a carbon electrode
  • the cathode 8 there is used for example soft-iron, Monel or nickel.
  • a first gas chamber 11 a into which fluorine gas produced at the anode 7 is led and a second gas chamber 12 a into which hydrogen gas produced at the cathode 8 is led, the two gas chambers being isolated from each other by the partition wall 6 so that the two chambers don't permit gas transfer therebetween.
  • the first and second gas chambers 11 a and 12 a are completely separated by the partition wall 6 . While, the molten salt contained in the anode chamber 11 and the molten salt contained in the cathode chamber 12 are connected to each other below the partition wall 6 .
  • the melting point of KF ⁇ 2HF is 71.7° C. and thus it is preferable to control the temperature of the molten salt in the range of 91 to 93° C.
  • hydrogen fluoride from the molten salt by an amount corresponding to a vapor pressure of it.
  • fluorine gas produced at the anode 7 and led into the first gas chamber 11 a and hydrogen gas produced at the cathode 8 and led into the second gas chamber 12 a contain hydrogen fluoride gas therein respectively.
  • a first pump 17 by which fluorine gas is led from the first gas chamber 11 a for its conveyance.
  • a volume-type pump such as bellows pump, diaphragm pump or the like is used.
  • a refining device 20 that collects hydrogen fluoride mixed with fluorine gas to refine fluorine gas.
  • a second pump 31 by which hydrogen gas is led from the second gas chamber 12 a for its conveyance.
  • a harmful matter remover 34 To the second main passage 30 at a position downstream of the second pump 31 , there is connected a harmful matter remover 34 , so that hydrogen gas conveyed by the second pump 31 is subjected, at the harmful matter remover 34 , to an adsorption removing of hydrogen fluoride to be rendered harmless and discharged to the outside.
  • the fluorine gas generating device 100 has further a material supply system 5 that, for supplementation, feeds the molten salt in the electrolytic tank 1 with hydrogen fluoride as a material of fluorine gas to be produced.
  • the material supply system 5 will be described.
  • the electrolytic tank 1 is connected through a material supply passage 41 to a hydrogen fluoride supply source 40 that stores hydrogen fluoride for supplementation of hydrogen fluoride in the tank.
  • the hydrogen fluoride stored in the hydrogen fluoride supply source 40 is fed to the molten salt in the electrolytic tank 1 through the material supply passage 41 .
  • the material supply passage 41 may be provided with a flow rate control valve 71 that controls a feeding flow rate of is hydrogen fluoride.
  • To the material supply passage 41 there is connected a vaporizer 60 that vaporizes liquid hydrogen fluoride fed from the hydrogen fluoride supply source 40 . Hydrogen fluoride gas discharged from the vaporizer 60 is kept in a gaseous state by a heating means (not shown) such as heater or the like connected to the material supply passage 41 .
  • the vaporizer 60 will be described in detail hereinafter.
  • a carrier gas supply passage 46 through which a carrier gas supplied by a carrier gas supply source 45 is led into the material supply passage 41 .
  • the carrier gas is a gas used for guiding hydrogen fluoride from the hydrogen fluoride supply source 40 into the molten salt, and thus, as the carrier gas, nitrogen gas that is an inert gas is used.
  • the nitrogen gas is fed together with hydrogen fluoride to the molten salt in the cathode chamber 12 , but the nitrogen gas hardly dissolves in the molten salt and the gas is discharged from the second gas chamber 12 a through the second main passage 30 .
  • the vaporizer 60 is a device that receives and vaporizes the liquid hydrogen fluoride fed from the hydrogen fluoride supply source 40 and discharge the gaseous hydrogen fluoride to a given portion.
  • the vaporizer 60 will be described in detail. It is however to be noted that the vaporizer 60 used in the invention is not limited to a vaporizer that will be described in the following.
  • the vaporizer 60 is equipped with a temperature adjusting device 64 such as a heater or the like, and comprises a hollow vessel 61 that forms therein a vaporizing chamber 65 , a hydrogen fluoride inlet portion 62 that introduces thereinto liquefied hydrogen fluoride from the hydrogen fluoride supply source 40 , and hydrogen fluoride outlet portion 63 that discharges gaseous hydrogen fluoride from the vaporizing chamber.
  • a temperature adjusting device 64 such as a heater or the like
  • the vaporizing chamber 65 is provided, on its inner wall, with a plurality of projections 66 such as fins or the like for the purpose of achieving an effective heat transmission from the temperature adjusting device 64 to the chamber 65 .
  • the shape of the projections 66 has no limitation, it is preferable that as is shown in FIG. 2 , the projections are shaped like plates and projected at right angles from the wall surface toward the vaporizing chamber 65 throughout the entire surface of the wall. Furthermore, preferably, the projections are placed in the vicinity of the hydrogen fluoride inlet portion 62 .
  • a fluid level detecting means that detects the fluid level of the liquefied hydrogen fluoride received in the vaporizing chamber 65 .
  • a pressure detecting device 68 that detects the pressure in the vaporizing chamber 65
  • a fluid level detecting device 69 that detects the fluid level of the liquefied hydrogen fluoride received in the vaporizing chamber 65 are usable.
  • a level indicator for general purpose use is usable. In this case, the level indicator is inserted in an inserting tube 67 for its purpose.
  • a thermometer may be connected to the vaporizer 60 for measuring the temperature of the vaporizing chamber 65 .
  • the fluid level of the liquefied hydrogen fluoride in the to vaporizing chamber 65 is so adjusted that the hydrogen fluoride in the chamber keeps an amount in a given range.
  • the fluorine gas generating device 100 of the present invention generates, at the electrolytic tank, a large amount of fluorine gas, and even when it becomes needed to supply a large amount of hydrogen fluoride to the tank, a needed amount of hydrogen fluoride can be instantly supplied to the tank from the hydrogen fluoride supply source 40 , and thus, shortage of amount of hydrogen fluoride to be supplied to the tank never occurs.
  • some methods are used, one being a method (viz., batch method) in which at first, upper and lower limits of the fluid level are set and when the fluid level of hydrogen fluoride comes to the lower limit, hydraulic fluoride is intermittently fed to the tank, the other being a method (viz., continuous method) in which hydrogen fluoride is continuously fed to the tank in such a manner as to constantly keep the fluid level at a given level.
  • the fluid level of hydrogen fluoride For keeping the fluid level of hydrogen fluoride within a given range, it is preferable to adjust the fluid level of hydrogen fluoride in the vaporizing chamber 60 based on the results of detection by the fluid level detecting means.
  • the pressure detecting device 68 As the fluid level detecting means, it is preferable to use the pressure detecting device 68 . To the pressure detecting device 68 , there is connected a controller 70 (control means), so that detecting results of the pressure detecting device 68 are fed to the controller 70 . For allowing the internal pressure of the vaporizing chamber 65 to take a predetermined value, the controller 70 controls an open/close degree of the flow rate control valve 71 mounted to the material supply passage 41 thereby controlling a to supply rate of hydrogen fluoride in such a manner that the internal pressure of the vaporizing chamber 65 shows a value within a given range. Like this, the fluid level of hydrogen fluoride is controlled in a given range.
  • a feeding stability of hydrogen fluoride to the electrolytic tank 1 is easily affected by the internal pressure of the vaporizer 60 . Accordingly, usage of the continuous method is preferable because it can keep the internal pressure of the vaporizer 60 at a given level and can continuously feed hydrogen fluoride to the tank while keeping the fluid level at a given level.
  • a control means such as controller or the like is connected to the fluid level detecting means, and for the purpose of adjusting the amount of hydrogen fluoride supplied to the tank, with the aid of detected results of the fluid level detecting means, the open/close degree of the flow rate control valve 71 is controlled in such a manner that the fluid level of hydrogen fluoride in the vaporizer 60 is kept at a constant level.
  • a fluid level detecting means that detects the fluid level of hydrogen fluoride in the vaporizer, and based on the detected results of the fluid level detecting means, the fluid level of hydrogen fluoride in the vaporizer 60 can be kept within a given range. Accordingly, controlling the fluid level of hydrogen fluoride in the vaporizer is facilitated, and thus, much stable feeding in amount of hydrogen fluoride to the electrolytic tank is to achieved.
  • the electrolytic tank when, due to generation of a large amount of fluorine gas in the electrolytic tank, it becomes necessary to supply the electrolytic tank with a large amount of hydrogen fluoride, the difference between the internal pressure of the hydrogen fluoride supply source and that of the electrolytic tank does not induce a sudden fluctuation of the fluid level of the molten salt in the electrolytic tank and thus the electrolytic tank can supply fluorine gas stably.
  • the present invention has the other embodiment.
  • the vaporizer 60 and the electrolytic tank 1 are installed in a common housing 80 .
  • down-sizing has been required in the field of fluorine gas generating devices, and thus down-sizing is needed by facilities and equipments that are used for constituting the fluorine gas generating device.
  • the fluorine gas generating device 100 can be reduced in size. Since, in this embodiment, the vaporizer 60 is received in the housing 80 , the passage for feeding gaseous hydrogen fluoride can be reduced in length as compared with a passage used in a conventional fluorine gas generating device, and thus, liquefaction of hydrogen fluoride does not easily occur. Furthermore, since leakage of gaseous hydrogen fluoride to the outside can be suppressed, the device is assessed with an eye to its safety.
  • controller 70 (control means) is connected to the pressure detecting device 68 and a method for keeping the fluid level of hydrogen fluoride within a given range is described, it is of course possible to keep the fluid level of hydrogen fluoride within a given range by connecting a similar controller to the fluid level detecting device 69 .

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
US14/358,630 2012-01-05 2012-10-31 Fluorine Gas Generation Apparatus Abandoned US20140326596A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2012000408A JP5906742B2 (ja) 2012-01-05 2012-01-05 フッ素ガス生成装置
JP2012-000408 2012-01-05
PCT/JP2012/078114 WO2013103042A1 (ja) 2012-01-05 2012-10-31 フッ素ガス生成装置

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JP (1) JP5906742B2 (ja)
KR (1) KR20140101407A (ja)
TW (1) TW201331419A (ja)
WO (1) WO2013103042A1 (ja)

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US20220228272A1 (en) * 2019-12-27 2022-07-21 Showa Denko K.K. Method for producing fluorine gas and device for producing fluorine gas
CN113430542A (zh) * 2021-07-08 2021-09-24 中核四0四有限公司 一种制氟电解槽液态氟化氢集中供料装置
CN113430543A (zh) * 2021-07-08 2021-09-24 中核四0四有限公司 一种制氟电解槽液态氟化氢集中供料方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050224366A1 (en) * 2002-07-19 2005-10-13 Graham Hodgson Apparatus and method for fluorine production
US20070181703A1 (en) * 2006-02-07 2007-08-09 Daryl Buchanan System and method for producing and delivering vapor

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JPH08128596A (ja) * 1994-10-28 1996-05-21 Fujitsu Ltd ガス蒸発装置及びガス供給方法
JP2003160869A (ja) * 2001-11-27 2003-06-06 Japan Science & Technology Corp 液体気化器、液体気化供給システム及び液体気化制御方法
KR100712345B1 (ko) * 2001-12-17 2007-05-02 도요탄소 가부시키가이샤 Ｆ2 가스발생장치, ｆ2 가스발생방법 및 ｆ2 가스
JP4999605B2 (ja) * 2007-08-23 2012-08-15 日本エア・リキード株式会社 液化ガスの気化方法、気化装置およびこれを用いた液化ガス供給装置
JP5584904B2 (ja) * 2008-03-11 2014-09-10 東洋炭素株式会社 フッ素ガス発生装置
JP5461786B2 (ja) * 2008-04-01 2014-04-02 株式会社フジキン 気化器を備えたガス供給装置
JP5388538B2 (ja) * 2008-10-27 2014-01-15 東洋炭素株式会社 気体発生装置
JP2011058015A (ja) * 2009-09-07 2011-03-24 Toyo Tanso Kk 電解装置
JP5375673B2 (ja) * 2010-03-01 2013-12-25 セントラル硝子株式会社 フッ素ガス生成装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050224366A1 (en) * 2002-07-19 2005-10-13 Graham Hodgson Apparatus and method for fluorine production
US20070181703A1 (en) * 2006-02-07 2007-08-09 Daryl Buchanan System and method for producing and delivering vapor

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WO2013103042A1 (ja) 2013-07-11
KR20140101407A (ko) 2014-08-19
TW201331419A (zh) 2013-08-01
JP5906742B2 (ja) 2016-04-20
JP2013139606A (ja) 2013-07-18

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