WO2005092786A1 - Methode de purification d'acide hydrofluorique et appareil de purification - Google Patents

Methode de purification d'acide hydrofluorique et appareil de purification Download PDF

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Publication number
WO2005092786A1
WO2005092786A1 PCT/JP2005/005575 JP2005005575W WO2005092786A1 WO 2005092786 A1 WO2005092786 A1 WO 2005092786A1 JP 2005005575 W JP2005005575 W JP 2005005575W WO 2005092786 A1 WO2005092786 A1 WO 2005092786A1
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WO
WIPO (PCT)
Prior art keywords
hydrofluoric acid
gas
fluorine gas
fluorine
arsenic compound
Prior art date
Application number
PCT/JP2005/005575
Other languages
English (en)
Japanese (ja)
Inventor
Hiroto Izumi
Yuji Imafuku
Kenichi Ishizaki
Original Assignee
Stella Chemifa Corporation
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 Stella Chemifa Corporation filed Critical Stella Chemifa Corporation
Publication of WO2005092786A1 publication Critical patent/WO2005092786A1/fr

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Classifications

    • 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
    • C01B7/191—Hydrogen fluoride
    • C01B7/195—Separation; Purification
    • C01B7/196—Separation; Purification by distillation

Definitions

  • the present invention relates to a method and an apparatus for dissolving fluorine gas in hydrofluoric acid to remove arsenic compounds contained in hydrofluoric acid.
  • hydrofluoric acid used for this purpose is required to be a high-purity product with extremely few impurities, and not only hydrofluoric acid but also chemicals used in semiconductor manufacturing are being highly purified year by year. .
  • the required metal impurity concentration in chemicals has reached the order of ppm to ppb, and the order of tens of ppt to several ppt. Requires a level of 5ppt or less, and there is an urgent need to develop a method for removing metal impurities.
  • Patent Document 1 there is a method using an oxidizing agent such as potassium permanganate.
  • an oxidizing agent such as potassium permanganate.
  • manganese and chromium contained in the oxidizing agent are distilled off and the purified hydrofluoric acid is contaminated, a divalent iron salt must be used in combination, and further contamination occurs.
  • Patent Document 2 water is added to anhydrous hydrofluoric acid, hydrofluoric acid is introduced into an electrolytic device having a nickel electrode, and electrolysis is performed to reduce the arsenic concentration in hydrofluoric acid. Lowering is exemplified. It is obvious that the electrode force composed of metal dissolves in metal hydrofluoric acid as well as the metal impurity, and cannot be used as a chemical for semiconductor manufacturing. Patent Document 3 discloses a method for removing arsenic impurities in hydrofluoric acid.
  • This method involves dissolving fluorine gas in hydrofluoric acid, reacting it with the arsenic compound contained in hydrofluoric acid, and purifying it by distillation. If this method is used, hydrofluoric acid that does not dissolve metal impurities can be used. It is a very good method that can be purified. However, according to Patent Document 3, the concentration of arsenic compounds in purified hydrofluoric acid is about 100ppt. Cannot meet the demands of the semiconductor manufacturing industry.
  • Patent Document 1 Japanese Patent Publication No. 47-16407
  • Patent Document 2 JP-A-6-263406
  • Patent Document 3 JP-A-61-151002
  • hydrofluoric acid containing an arsenic compound after adding a fluorine gas or a mixed gas of a fluorine gas and an inert gas to hydrofluoric acid containing an arsenic compound, the mixture is allowed to stay for a certain time, and then hydrofluoric acid is added.
  • a method for purifying hydrofluoric acid, which is characterized by distillation, is obtained.
  • a fluorine gas or a mixed gas of a fluorine gas and an inert gas is added to hydrofluoric acid containing an arsenic compound. After the addition, the solution is kept for 5 minutes or more, and the hydrofluoric acid is distilled off, thereby obtaining a hydrofluoric acid purification method.
  • a method for purifying hydrofluoric acid comprising adding a fluorine gas or a mixed gas of a fluorine gas and an inert gas after reducing the content of an arsenic compound to 100 ppb or less. Is obtained.
  • an apparatus for adding a fluorine gas or a mixed gas of a fluorine gas and an inert gas to hydrofluoric acid containing an arsenic compound, an apparatus for adding fluorine, and a distillation apparatus An apparatus for purifying hydrofluoric acid, characterized in that a retaining section for hydrofluoric acid is provided between them, is obtained.
  • the purification target of the present invention is hydrofluoric acid, more specifically hydrofluoric acid containing an arsenic compound.
  • hydrofluoric acid means hydrofluoric acid containing at least 3% or less of water.
  • the arsenic compound contained as an impurity in the hydrofluoric acid of the present invention is not particularly limited to any particular type, and any arsenic compound is effectively removed.
  • any arsenic compound is effectively removed.
  • AsF and AsF can be mentioned. It also exists in forms other than arsenic itself or fluoride.
  • Arsenic compounds can also be effectively removed.
  • the amount of the arsenic compound present as an impurity is 100 ppb or less, preferably 50 ppb or less, and more preferably 100 ppb or less.
  • the content of arsenic compound Hydrofluoric acid greater than this may be removed by a known method in advance, and then the purification of the present invention may be used.
  • the arsenic concentration is reduced to 5 ppt or less by applying the method of the present invention after the arsenic compound is once reduced to 100 ppb or less. When lOOppb or more is contained, the residence time of the method of the invention may be long.
  • fluorine gas is added to hydrofluoric acid containing the above impurities.
  • the fluorine gas used may be a single gas or a mixed gas with another inert gas.
  • the inert gas include helium, argon, and nitrogen.
  • the added fluorine gas is at least 50 ppm, preferably at least 60 ppm, more preferably at least 70 ppm, based on hydrofluoric acid.
  • the effect saturates even at 80 ppm or more, so the upper limit is preferably set to 80 ppm from an economic viewpoint!
  • the concentration of the impurities be 5% or less because the removal efficiency is increased. It is more preferable to be 1% or less!
  • the residence time is at least 5 minutes, preferably at least 5 minutes and 30 seconds, more preferably at least 6 minutes.
  • the above operation is preferably carried out at a temperature lower than the boiling point of hydrofluoric acid, that is, at 0 to 20 ° C.
  • the present invention it is possible to reduce the arsenic content to 5 ppt or less, and it becomes possible to produce ultrapure chemicals.
  • the refining device of the present invention includes a device for adding a fluorine gas, that is, a portion for blowing a fluorine gas through a pipe or a vessel equipped with a gas blowing nozzle and then retaining the fluorine gas for a certain period of time before moving to a distillation step.
  • the stagnation section may be a container, or may be a simple pipe.
  • a baffle plate or the like may be provided inside the container so that the reaction between the fluorine gas and the arsenic compound proceeds. Iron, stainless steel, fluorinated resin, etc. can be used for the contact portion with hydrofluoric acid.
  • distillation method a batch distillation purification method, a continuous distillation purification method, or other distillation methods can be appropriately used.
  • the raw hydrofluoric acid (99.9%, arsenic 15ppb) was continuously supplied to a rectification unit having a tetrafluoroethylene cooler and a tetrafluoroethylene packed tower at lOOKgZ.
  • a rectification unit having a tetrafluoroethylene cooler and a tetrafluoroethylene packed tower at lOOKgZ.
  • the water was continuously added so that the fluorine gas concentration became 50 ppm.
  • a stagnant section was provided so that hydrofluoric acid to which the fluorine gas was added reached the rectifier after 5 minutes, and rectification was performed.
  • the arsenic content of the purified hydrofluoric acid obtained by continuous operation for 10 hours was measured by this method and found to be 5 ppt.
  • the present invention after adding fluorine gas to hydrofluoric acid containing an arsenic compound and allowing it to stay for a certain period of time, by performing rectification, it is possible to obtain ultrapure hydrofluoric acid of 5 ppt or less. it can.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Une méthode de purification d'acide hydrofluorique par laquelle un acide hydrofluorique ayant une pureté aussi élevée que 5 ppt ou moins peut être obtenu. La méthode est caractérisée par l'ajout de gaz de fluorine ou d'un mélange gazeux de gaz de fluorine et d'un gaz inerte avec de l'acide hydrofluorique contenant un composé d'arsenic, faisant reposer le mélange résultant pour une certaine durée, puis distillant l'acide hydrofluorique.
PCT/JP2005/005575 2004-03-29 2005-03-25 Methode de purification d'acide hydrofluorique et appareil de purification WO2005092786A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004096278A JP2005281048A (ja) 2004-03-29 2004-03-29 フッ化水素酸の精製法及び精製装置
JP2004-096278 2004-03-29

Publications (1)

Publication Number Publication Date
WO2005092786A1 true WO2005092786A1 (fr) 2005-10-06

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Family Applications (1)

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PCT/JP2005/005575 WO2005092786A1 (fr) 2004-03-29 2005-03-25 Methode de purification d'acide hydrofluorique et appareil de purification

Country Status (3)

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JP (1) JP2005281048A (fr)
TW (1) TW200536780A (fr)
WO (1) WO2005092786A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114180526A (zh) * 2021-12-16 2022-03-15 浙江博瑞电子科技有限公司 一种超声耦合微电流除氟化氢中砷制备电子级氟化氢与电子级氢氟酸的方法

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5188064B2 (ja) * 2006-12-15 2013-04-24 ステラケミファ株式会社 フッ酸及び塩酸の回収方法
MX357878B (es) 2014-12-18 2018-07-27 Mexichem Fluor Sa De Capital Variable Proceso para la purificación del ácido fluorhídrico incluyendo la obtención del subproducto ácido arsenioso.
KR102256840B1 (ko) * 2020-12-23 2021-05-27 (주)후성 초고순도 불화수소 제조 중 불화수소 내 비소화합물의 제거 및 처리방법
KR102310763B1 (ko) * 2021-06-03 2021-10-08 램테크놀러지 주식회사 초고순도 불화수소의 정제방법 및 장치

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61151002A (ja) * 1984-12-25 1986-07-09 Hashimoto Kasei Kogyo Kk フツ化水素酸の精製法
JPS61191502A (ja) * 1985-02-20 1986-08-26 Hashimoto Kasei Kogyo Kk フツ化水素酸の精製法
JPH11507001A (ja) * 1995-06-05 1999-06-22 スターテック・ベンチャーズ・インコーポレーテッド 半導体処理用超高純度弗化水素酸の現場での製造

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61151002A (ja) * 1984-12-25 1986-07-09 Hashimoto Kasei Kogyo Kk フツ化水素酸の精製法
JPS61191502A (ja) * 1985-02-20 1986-08-26 Hashimoto Kasei Kogyo Kk フツ化水素酸の精製法
JPH11507001A (ja) * 1995-06-05 1999-06-22 スターテック・ベンチャーズ・インコーポレーテッド 半導体処理用超高純度弗化水素酸の現場での製造

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114180526A (zh) * 2021-12-16 2022-03-15 浙江博瑞电子科技有限公司 一种超声耦合微电流除氟化氢中砷制备电子级氟化氢与电子级氢氟酸的方法

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Publication number Publication date
TW200536780A (en) 2005-11-16
JP2005281048A (ja) 2005-10-13

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