WO2016124346A1 - Procédé pour éliminer le fluor de gégagement gazeux contenant du fluor - Google Patents

Procédé pour éliminer le fluor de gégagement gazeux contenant du fluor Download PDF

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Publication number
WO2016124346A1
WO2016124346A1 PCT/EP2016/050102 EP2016050102W WO2016124346A1 WO 2016124346 A1 WO2016124346 A1 WO 2016124346A1 EP 2016050102 W EP2016050102 W EP 2016050102W WO 2016124346 A1 WO2016124346 A1 WO 2016124346A1
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WO
WIPO (PCT)
Prior art keywords
stage
fluorine
solution
reducing agent
washing
Prior art date
Application number
PCT/EP2016/050102
Other languages
German (de)
English (en)
Inventor
Tino TANNEBERGER
Andreas Frenzel
Matthias Förster
Stephan Trepte
Ralph Wiesenberg
Original Assignee
Das Environmental Expert Gmbh
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 Das Environmental Expert Gmbh filed Critical Das Environmental Expert Gmbh
Publication of WO2016124346A1 publication Critical patent/WO2016124346A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/75—Multi-step processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/20—Reductants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/604—Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/202—Single element halogens
    • B01D2257/2027—Fluorine
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/204—Inorganic halogen compounds
    • B01D2257/2047—Hydrofluoric acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0216—Other waste gases from CVD treatment or semi-conductor manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0241—Other waste gases from glass manufacture plants

Definitions

  • the present invention relates to a process for the separation of fluorine from fluorine-containing gas streams, in particular from fluorine-containing exhaust gases.
  • the method according to the invention is preferably suitable for purifying exhaust gases which are produced in processes in which fluorine is used either as a process gas or as a process gas component or during the process
  • Precursor substances arises.
  • Examples of such processes are the etching of glasses, the production of photovoltaic cells, the semiconductor or chip production as well as general production processes in the field of microelectronics.
  • the prior art discloses various methods of separating fluorine or fluorine-containing compounds, e.g. OF2, described from corresponding exhaust gas streams. The aim of all these processes is, in particular, as complete as possible a depletion of the strongly oxidizing and chemically aggressive fluorine-containing substances from these exhaust gases.
  • DE 42 124 51 A1 describes the use of used titanium dioxide catalysts as absorbent
  • EP 1 201 291 A1 describes the use of Al 2 O 3
  • US Pat. No. 8,834,824 B2 describes the use of calcium or magnesium carbonate.
  • US 2004/0101460 A1 describes a two-stage process for the removal of
  • Pollutants such as fluorine
  • the gas stream is treated exclusively with water and pre-cleaned.
  • the second stage will be the remaining impurities removed, wherein in addition to various other possibilities, the use of a so-called dry scrubber medium for
  • This dry scrubber medium may be such that it contains other inorganic substances, e.g. NaOH, KOH, ammonium hydroxide or reducing agents such as sodium thiosulfate.
  • DE 10 2006 023 939 A1 relates to a two-stage process for the absorption of small amounts of chlorine from a gas containing chlorine and carbon dioxide.
  • an aqueous NaOH solution is used as the washing liquid. Due to the large carbon dioxide excess in the gas stream to be purified, the NaOH used is converted directly to sodium hydrogen carbonate at as the actually active substance.
  • This Fluorzerponentssystem is a one-stage scrubber, which with KOH solution and optionally also with a
  • Reducing agent is operated.
  • the KR 1020090097749 A describes a single-stage wet scrubber, with the
  • Reducing agent can be treated in the form of sodium or potassium thiosulfate.
  • HF or HCl-containing gas formed in a secondary reaction is separated off or neutralized in a downstream separate process step with sodium hydroxide or potassium hydroxide solution.
  • a one-stage wet scrubber process is used according to JP 2006-231 105 A, in which a basic solution of a sulfur-containing reducing agent is used as a liquid absorbent.
  • the basic medium are alkali metal or alkaline earth metal hydroxides and as
  • Sulfur-containing reducing agents sulfhydrates, sulfides and alkali metal thiosulfate.
  • the pH of the solution used is 9-10, and the content of
  • Reducing agent is relatively high and is generally 0.01 to 10%, in which
  • a disadvantage of the known methods is e.g. the high energy consumption during
  • the present invention therefore an object of the invention, a method for
  • the object is achieved in that the removal of fluorine from fluorine-containing exhaust gases is carried out in a two-stage process, in which in a first stage or a first step, the exhaust gas with a strongly basic hydroxide solution and in an adjoining second step with an aqueous solution a reducing agent, preferably a sulfur-containing reducing agent is treated.
  • the basic hydroxide solution is preferably aqueous solutions of alkali metal and / or alkaline earth metal hydroxides, wherein the alkali metal hydroxides and here sodium or potassium hydroxide are preferred according to the invention.
  • These basic solutions preferably NaOH or KOH, in particular NaOH solutions, preferably have a pH of greater than 10, in particular greater than 12 and more preferably greater than 13. This corresponds, for example, to the use of a 0.1 mol / l NaOH or KOH solution and represents an optimal compromise between economic efficiency and efficiency.
  • the gas to be treated is brought into contact with the alkaline hydroxide solution in a first stage of the process. This is preferably done in a wet scrubber, preferably in countercurrent process.
  • the residence time in this stage should preferably be at least 4 seconds.
  • the use of a packed scrubber is basically advantageous because of the larger contact area.
  • the inventively preferred reducing agents are sulfur-containing
  • Reducing agent and in particular alkali or Erdalkalithiosulfate or
  • the reducing agents according to the invention are preferably used as solutions, in particular in the form of aqueous solutions. These solutions have a concentration of reducing agent (such as sodium thiosulfate) of preferably 0.001-0.1 mol / l, more preferably 0.001-0.05 mol / l. In principle, other reducing agents are possible for which the advantage of low consumption also exists.
  • the gas discharged from the first stage is contacted with the solution of the reducing agent, preferably in a wet scrubber.
  • the scrubber of the second stage can lead to the reduction of the required installation space, the gas in cocurrent with the reducing agent.
  • the treatment duration of the gas should be but also for this second stage preferably at least 4 seconds.
  • the pH of the aqueous solution of the reducing agent in the second process stage should preferably be greater than 7 in order to avoid or minimize the discharge of undesirable by-products. Depending on the design of the wet scrubber used, however, the pH need not necessarily always be controlled or controlled. Due to the small cargo of acidic components in the gas after the first
  • washing step the amount of basic solution entrained from the first stage with the gas stream is usually sufficient to maintain the pH of the second stage in the
  • a small amount of basic solution may be pumped from the first stage to the second stage.
  • a wet scrubber can basically the scrubber described in the prior art or
  • Procedure is basically not required.
  • the wet scrubber type used in JP 2006-231 105 A which can be used according to the invention for each stage of the described two-stage process.
  • it is advantageous to use a two-stage scrubber in which the two stages are integrated in a system and controlled by a common control.
  • Proven wet scrubbers in which a packed body is wetted from above by means of a spray nozzle or in which the packing is wetted by a centrally disposed therein spray lance from the inside.
  • the exhaust gas to be treated according to the invention preferably has a fluorine content of up to 5% by volume. If the fluorine content in the exhaust gas actually occurring exceeds this value, it may be appropriate to set the exhaust gas flow to a value of less than 5% by volume, for example by metering in nitrogen.
  • the following detailed description of the method according to the invention relates to its preferred embodiment, in particular with respect to
  • the gas mixture to be treated is first washed or treated in a first stage with aqueous NaOH or KOH solution having a pH of> 12, in particular of> 13.
  • the acidic constituents contained in the exhaust gas mixture such as HF or SiF 4
  • a large part of the existing fluorine (F2) are separated.
  • a gas with a residual concentration of fluorine and possibly formed OF2 emerges from the first stage. It can be assumed that even with a very high alkali concentration, the fluorine can not be completely separated off in the first reaction stage.
  • the waste gas from the first washing or treatment stage is then subjected to a second treatment, e.g. a second wet scrubber, where it is preferably contacted with a dilute, aqueous solution of sodium thiosulfate.
  • a second treatment e.g. a second wet scrubber
  • the remaining residual concentration of fluorine is at least so far removed that the fluorine content is lowered below tolerated limits.
  • Also contained in the gas stream OF2 is washed out in this second stage and reduced by the thiosulfate to fluoride.
  • Washing liquid) in the first washing stage is recycled through the washing stage pumped. Due to the absorption of the acid gases, the alkaline washing solution used in the first stage, eg NaOH, is progressively neutralized and lye must be replenished again and again. Upon reaching a maximum amount of metered lye in the reservoir of the scrubber, a portion of the solution is pumped off and replaced with fresh water and a corresponding amount of concentrated liquor. When the temperature falls below the preferred pH ranges for the washing solution, lye is added again until the maximum amount possible is reached again. With good knowledge of the incoming amount of fluorine from the upstream process, it may alternatively be sufficient to meter the lye used for the reaction stoichiometrically to the amount of fluorine contained in the input stream at defined intervals.
  • the alkaline washing solution used in the first stage eg NaOH
  • the washing solution or the reducing agent of the second washing stage is also slowly consumed by chemical reaction.
  • the content of unused thiosulphate or, in general, reducing agent in the washing solution of the second process stage can be determined using a redox electrode.
  • the measuring method has proven to be less robust and reliable in practice, since the measured value is strongly pH-dependent and the measurement itself is very sluggish. Since in most process plants, in which scrubbers are provided for the exhaust gas purification, always run the same specified processes and thus also produces a narrowly fluctuating exhaust gas, it is possible, for example. a signal from the
  • the second stage wash solution is then supplemented with an addition of fresh thiosulfate solution.
  • the washing solution is (partly) pumped off and replenished with fresh water and thiosulphate solution or completely replaced.
  • the process is preferably implemented so that the washing liquid always remains alkaline in the second stage.
  • the exhaust gas can be monitored after the second washing stage with a gas sensor and when a warning value is exceeded, a dosage of reducing agent is triggered.
  • the consumption of reducing agent preferably thiosulfate and Na2S203 here, compared to the methods of the prior art can be kept very low. This is among other things of importance because at the production sites usually caustic soda is available via a piping system, while thiosulphate solutions must be provided in storage tanks.
  • the wet scrubbers used at moderate fluorine concentrations in the gas to be treated preferably less than 5 vol .-%, largely from inexpensive plastics. Only in the area of the gas inlet into the first scrubbing stage are particularly resistant materials, eg PVDF, necessary or at least advantageous.
  • the process according to the invention may also be part of a more complex purification process comprising further process stages, in which e.g. In addition to the fluorine-containing substances, other gaseous compounds or even particles or droplets are removed from a gas stream.
  • the process is carried out by way of example in a two-stage wet scrubber according to FIG. 1.
  • Two washing stages are integrated in one system and are controlled by a common electronic control system. In order to build the system as compact as possible, the two washing stages are in opposite
  • Ambient temperature in the range of 0-40 ° C operated.
  • a mixture of 0.5 to 2% by volume of fluorine in 50 to 800 slm (standard liter per minute) of nitrogen is used.
  • the gas to be treated is passed via the inlet region 1 and the free volume in the first washing liquid container 2 to the lower end of the first washing stage 3.
  • This first washing stage 3 consists of a packed column with a
  • Wash liquid container 2 a flow of 25 to 50 l / min of the first washing liquid, which in this case is an aqueous sodium hydroxide solution, in the cycle over the packed
  • the first washing stage 3 is in
  • an electronic control 10 By means of an electronic control 10, when the pH falls below a defined value, in the example pH 12, a predetermined amount of concentrated sodium hydroxide solution is metered in via a feed 5 for concentrated lye in the first washing liquid container 2.
  • the amount of liquor supplied to the washing liquid container 2 is determined by the electronic controller 10 either via a metering pump or a sensor. Upon reaching a total metered amount of alkali, theoretically in the reaction with fluorine in the washing liquid to a concentration of
  • washing liquid exchange is triggered.
  • a part, at least half, of the washing solution is pumped out of the first washing liquid container 2 and the corresponding volume refilled with fresh water and alkali, so that a predetermined in the control NaOH Concentration in the washing liquid tank, typically from 0.01 to 0.15 mol / l, is reached again.
  • a predetermined in the control NaOH Concentration in the washing liquid tank typically from 0.01 to 0.15 mol / l
  • Washing liquid circuit on the washing line 3 is not interrupted.
  • the gas treated in the first washing stage from the upper end of the washing stage 3 is passed into the upper end of the second washing stage 7, the absorption column of which is the same or similar to that of the first.
  • the second washing stage 7 is operated according to the direct-current principle, with gas and washing liquid to be cleaned flowing in the same direction, from top to bottom, through a packed body.
  • a flow of 25 to 50 l / min washing solution from the second washing liquid container 6 by means of the pump 8 is circulated.
  • the washing solution used is 0.01 to 0.1 mol / l sodium thiosulfate solution having a pH of greater than pH 7.
  • the pH of the second washing liquid container 6 is typically slightly alkaline, but as a rule it is not measured or regulated.
  • a small partial stream of the washing liquid of the first washing stage can be conducted to the second washing stage in a makeshift manner.
  • the treated gas is passed through the free volume in the washing liquid container 6 and a mist eliminator 12 and mixed with air at the end of the wet scrubber. The admixture of air, sucked
  • Ambient air or dry compressed air reduces the relative humidity of the discharged gas and prevents condensation.
  • a measurement of the residual fluorine content can then be carried out with the aid of a gas sensor 11.
  • a predetermined amount for example 10 ml, of a 1 M sodium thiosulfate solution via a feed 9 for
  • the electronic controller 10 can estimate the amount of fluoride supplied to disposal via communication with the upstream process and thus determine it empirically
  • the dosage of the reducing agent takes place after a fixed time.
  • the concentration of fluorine in the exhaust gas is monitored after the second washing stage with a gas sensor 11 and when exceeding a
  • Warning value of, e.g., 10 ppm fluorine continuously e.g. 5 ml / min reductant added until the warning value falls below again.
  • the electronic control calculates the total metered amount of reducing agent and triggers after reaching a predetermined maximum amount of a washing liquid exchange. In this case, one part, at least half, of the washing solution from the second
  • Wash liquid tank 6 pumped and filled the corresponding volume again with fresh water and dosed a predetermined amount of reducing agent.
  • the washing liquid circuit is not interrupted via the washing section 7.
  • a concentration of less than 10 ppm fluorine in the exhaust gas can be achieved after the treatment, with a consumption of less than 70 ml / h of Na 2 S 2 O 3 solution per 1 slm of fluorine.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treating Waste Gases (AREA)

Abstract

Procédé pour éliminer le fluor de courants gazeux contenant du fluor, comprenant les deux étapes suivantes : au cours d'une première étape le courant gazeux contenant du fluor est traité avec une solution d'hydroxyde alcalin (par exemple NaOH) et au cours d'une deuxième étape le courant gazeux issu de cette première étape est traité avec une solution d'un agent réducteur (par exemple du thiosulfate de sodium).
PCT/EP2016/050102 2015-02-06 2016-01-06 Procédé pour éliminer le fluor de gégagement gazeux contenant du fluor WO2016124346A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015101728.8A DE102015101728A1 (de) 2015-02-06 2015-02-06 Verfahren zum Entfernen von Fluor aus fluorhaltigen Abgasen
DE102015101728.8 2015-02-06

Publications (1)

Publication Number Publication Date
WO2016124346A1 true WO2016124346A1 (fr) 2016-08-11

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DE (1) DE102015101728A1 (fr)
WO (1) WO2016124346A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI708635B (zh) * 2018-11-02 2020-11-01 德商達斯環境專家有限責任公司 用於溼式清潔氣流之裝置及方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108176205B (zh) * 2018-01-03 2020-07-17 泉州台商投资区中栓机械技术有限公司 一种次氯酸钙生产中氯气处理装置

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4212451A1 (de) 1992-04-14 1993-10-21 Huels Chemische Werke Ag Verfahren zur Entfernung von Fluor und/oder anorganischen Fluorverbindungen aus Gasen sowie die Verwendung von gebrauchten Katalysatoren auf Basis von Titandioxid hierzu
FR2813205A1 (fr) * 2000-08-24 2002-03-01 Picosil Procede d'epuration des effluents gazeux fluores
EP1201291A1 (fr) 2000-10-31 2002-05-02 Air Products And Chemicals, Inc. Elimination de fluor de gaz d'échappement du traitement de semi-conducteurs
WO2003082444A1 (fr) 2002-03-27 2003-10-09 The Boc Group Plc Traitement d'effluents gazeux
US20040101460A1 (en) 1997-05-16 2004-05-27 Arno Jose I. Apparatus and method for point-of-use treatment of effluent gas streams
JP2006231105A (ja) 2005-02-22 2006-09-07 Fujitsu Ltd 酸化性ガスの除去方法
DE102006023939A1 (de) 2006-05-19 2007-11-22 Bayer Materialscience Ag Verfahren zur Absorption von Chlor aus einem Chlor- und Kohlendioxid-enthaltenden Gas
KR20090097749A (ko) 2008-03-12 2009-09-16 엔텍이앤씨 주식회사 악취 가스 제거 방법
WO2012035000A1 (fr) * 2010-09-15 2012-03-22 Solvay Sa Procédé pour l'élimination de f2 et/ou of2 d'un gaz
DE212011100142U1 (de) 2010-09-16 2013-04-24 Solvay Sa Fluorgasanlage
US20130175161A1 (en) * 2010-09-15 2013-07-11 Solvay Sa Plant for fluorine production and a process using it
US8834824B2 (en) 2005-10-07 2014-09-16 Edwards Limited Method of treating a gas stream

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4212451A1 (de) 1992-04-14 1993-10-21 Huels Chemische Werke Ag Verfahren zur Entfernung von Fluor und/oder anorganischen Fluorverbindungen aus Gasen sowie die Verwendung von gebrauchten Katalysatoren auf Basis von Titandioxid hierzu
US20040101460A1 (en) 1997-05-16 2004-05-27 Arno Jose I. Apparatus and method for point-of-use treatment of effluent gas streams
FR2813205A1 (fr) * 2000-08-24 2002-03-01 Picosil Procede d'epuration des effluents gazeux fluores
EP1201291A1 (fr) 2000-10-31 2002-05-02 Air Products And Chemicals, Inc. Elimination de fluor de gaz d'échappement du traitement de semi-conducteurs
WO2003082444A1 (fr) 2002-03-27 2003-10-09 The Boc Group Plc Traitement d'effluents gazeux
JP2006231105A (ja) 2005-02-22 2006-09-07 Fujitsu Ltd 酸化性ガスの除去方法
US8834824B2 (en) 2005-10-07 2014-09-16 Edwards Limited Method of treating a gas stream
DE102006023939A1 (de) 2006-05-19 2007-11-22 Bayer Materialscience Ag Verfahren zur Absorption von Chlor aus einem Chlor- und Kohlendioxid-enthaltenden Gas
KR20090097749A (ko) 2008-03-12 2009-09-16 엔텍이앤씨 주식회사 악취 가스 제거 방법
WO2012035000A1 (fr) * 2010-09-15 2012-03-22 Solvay Sa Procédé pour l'élimination de f2 et/ou of2 d'un gaz
US20130175161A1 (en) * 2010-09-15 2013-07-11 Solvay Sa Plant for fluorine production and a process using it
DE212011100142U1 (de) 2010-09-16 2013-04-24 Solvay Sa Fluorgasanlage

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI708635B (zh) * 2018-11-02 2020-11-01 德商達斯環境專家有限責任公司 用於溼式清潔氣流之裝置及方法
US11504670B2 (en) 2018-11-02 2022-11-22 Das Environmental Expert Gmbh Apparatus and method for wet cleaning a gas stream

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