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US20140246309A1 - Electrochemical cell - Google Patents

Electrochemical cell Download PDF

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Publication number
US20140246309A1
US20140246309A1 US14/191,824 US201414191824A US2014246309A1 US 20140246309 A1 US20140246309 A1 US 20140246309A1 US 201414191824 A US201414191824 A US 201414191824A US 2014246309 A1 US2014246309 A1 US 2014246309A1
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US
United States
Prior art keywords
electrochemical cell
electrolyte
gas
platinum
thiocyanate
Prior art date
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Abandoned
Application number
US14/191,824
Inventor
Christopher Frey
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.)
Compur Monitors GmbH and Co KG
Original Assignee
Compur Monitors GmbH and Co KG
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Publication of US20140246309A1 publication Critical patent/US20140246309A1/en
Assigned to COMPUR MONITORS GMBH & CO. KGR reassignment COMPUR MONITORS GMBH & CO. KGR ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: FREY, CHRISTOPHER
Assigned to ROYAL BANK OF CANADA, AS FIRST LIEN COLLATERAL AGENT reassignment ROYAL BANK OF CANADA, AS FIRST LIEN COLLATERAL AGENT SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: UNITED SORTATION SOLUTIONS LLC
Abandoned legal-status Critical Current

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Classifications

    • C25B9/06—
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0006—Calibrating gas analysers
    • 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
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • 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
    • 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
    • C25B1/22—Inorganic acids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/4163—Systems checking the operation of, or calibrating, the measuring apparatus
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/007—Arrangements to check the analyser
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/007—Arrangements to check the analyser
    • G01N33/0072—Arrangements to check the analyser by generating a test gas

Definitions

  • the present invention relates to an electrochemical cell for generating hydrogen cyanide gas using a generator electrode and a counter electrode.
  • a platinum electrode completely submerged in an aqueous electrolyte is flushed by nitrogen, so as to transport the generated hydrogen cyanide gas outward.
  • the object is accomplished by an electrochemical cell of the type mentioned above, wherein the electrolyte comprises at least one ionic liquid and includes thiocyanate ions for generating hydrogen cyanide gas.
  • ionic liquids Due to its high electrochemical stability with respect to oxidation and reduction, the use of ionic liquids makes it possible to provide electrochemical cells for generating hydrogen cyanide gas, e.g. to check gas analysing devices, whereby the electrochemical cells generate stable amounts of hydrogen cyanide gas without failing over a long life time and also at changing temperatures and environmental conditions.
  • the use of ionic liquid as electrolyte makes it possible to have long storage periods for such gas generators without impacting their function in later use.
  • the electrolyte comprises a mixture of at least two ionic liquids, thus allowing to easily select and set the melting point and water absorption capacity of the electrolyte by an appropriate choice of ionic liquids and/or their appropriate mixing ratio.
  • the electrolyte preferably comprises at least one ionic liquid of the group of 1-butyl-3-methylimidazoliurn trifluoromethanesulfonate (hereinafter abbreviated as BMIM OTf), 1-ethyl-3-methylimidazolium trifluoromethanesulfonate (hereinafter abbreviated as EMIM OTf) and 1-ethyl-3-methylimidazolium thiocyanate (hereinafter abbreviated as EMIM SCN).
  • BMIM OTf 1-butyl-3-methylimidazoliurn trifluoromethanesulfonate
  • EMIM OTf 1-ethyl-3-methylimidazolium trifluoromethanesulfonate
  • EMIM SCN 1-ethyl-3-methylimidazolium thiocyanate
  • the use of the mentioned ionic liquids and optionally of further additional substances results in reductions in the electroyte's melting point, which allows operation until far below the melting points of the individual ionic liquids and thus within the operating temperature range of the electrochemical cell, such as between ⁇ 30° C. and +60° C.
  • Thiocyanate salt is preferably used as gas generating substance, and it is particularly advantageous to select it from the group NaSCN, KSCN, LiSCN, NH 4 SCN, NBu 4 SCN.
  • thiocyanate can also be itself the anion of an ionic liquid.
  • At least one noble metal as generator electrode, in particular one of the group of gold, rhodium, iridium, palladium or platinum, wherein platinum is particularly advantageous.
  • the generator electrode is preferably formed as a platinum wire mesh or as a polytetrafluorethylene (in the following abbreviated as PTFE) gas diffusion membrane coated with the noble metal.
  • the container for the ionic liquid in the electrochemical cell is sealed to the outside by a PTFE gas diffusion membrane, which is permeable for the generated hydrogen cyanide gas.
  • the generated hydrogen cyanide gas is discharged to the outside via this PTFE gas diffusion membrane.
  • the counter electrode is preferably a PTFE support which is coated with platinum or platinum black, which is preferably porous.
  • An electrochemical cell 1 comprises a cell housing or container 2 at its bottom side above of which a counter electrode 3 is disposed on which ionic liquid 4 is provided.
  • a generator electrode 5 is disposed on the side of the ionic liquid opposing the counter electrode 3 .
  • the generator electrode 5 acting as an anode and the counter electrode 3 acting as a cathode are connected to a constant current source 6 .
  • generator electrode 5 On the outer side of generator electrode 5 , which is formed for example as a wire mesh or as a gas diffusion membrane, another gas diffusion membrane is possibly provided, through which the generated hydrogen cyanide by diffusion passes out of the cell to the outside.
  • the gas diffusion membrane 7 is additionally stabilized by a PTFE support grid 8 .
  • the interior of the cell housing 2 containing the ionic liquid 4 preferably comprises glass fiber layers impregnated with ionic liquid containing thiocyanate ions.
  • the ionic liquid is selected in particular with regard of the melting point and the water absorbing capacity.
  • BMIM OTf, EMIM OTf and EMIM SCN are of particular advantage.
  • the ionic liquids can be used as a basis for the cell's electrolyte, either in its pure forms or as mixtures. It is preferred to have a proportion of 30-25 vol % of EMIM SCN in the mixture with EMIM OTf or BMIM OTf.
  • Typically 0.2-0.4 mol/l lithium thiocyanate, potassium thiocyanate, sodium thiocyanate, ammonium thiocyanate or tetrabutylammonium thiocyanate are added to BMIM OTf.
  • a proportion of 5-20% H 2 O is required as a reactant in all cases. It is also used to optimize the solubility of thiocyanate salts and the reaction products.
  • the generator electrode consists of a platinum wire mesh or a coating of noble metal and preferably of platinum on the inner side of PTFE gas diffusion membrane 7 .
  • the counter electrode is a 0.25 mm PTFE gore membrane coated with platinum black.
  • the electrochemical cell operates galvanostatically with current densities preferably between 0.5 and 1.5 mA/cm 2 . With a generator electrode having a diameter of 20 mm the optimum operating current is 2 to 3 mA.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Molecular Biology (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

An electrochemical cell is described, which provides a reliable gas generation even under unfavorable environmental conditions and with significant changes in temperature and environment. Furthermore the cell has a long life time. The electrolyte of this electrochemical cell comprises at least one ionic liquid containing thiocyanate ions for the generation of hydrogen cyanide gas. Preferred substances for the composition of the electrolyte and for the provision of thiocyanate ions in the electrolyte are specified.

Description

    FIELD OF THE INVENTION
  • The present invention relates to an electrochemical cell for generating hydrogen cyanide gas using a generator electrode and a counter electrode.
    • BACKGROUND OF THE INVENTION
  • Electrochemical cells for generating test gases for gas analysis devices are known, e.g. from German patent specification 26 21 677, for various gases, but not for hydrogen cyanide gas.
  • From document Z. Tocksteinová, F. Opekar, “The Electrochemical Generation of Small Amounts of Hydrogen Cyanide”, Talanta, 1986, vol. 33, no. 8, pages 688-690 a method for generating hydrogen cyanide gas using an electrochemical cell is known, wherein hydrogen cyanide gas is generated by oxidation of thiocyanate ions. The gas is generated via controlled oxidation of thiocyanate in aqueous solution according to reaction

  • SCN−+4 H2O→6 e −+SO4 2−+HCN+7 H+
  • A platinum electrode completely submerged in an aqueous electrolyte is flushed by nitrogen, so as to transport the generated hydrogen cyanide gas outward.
  • Besides the fact that the use of such a gas generator is only possible under laboratory conditions, this gas generator is unfavorable in particular due to the electrolyte which is an aqueous solution. Thus in practical applications for example climatic influences will cause loss of electrolyte, which does not allow for a reliable generation of hydrogen cyanide gas in controllable and constant amounts or might even cause a complete functional failure of such a generator.
    • SUMMARY OF THE INVENTION
  • Thus it is an object of the invention to provide an electrochemical cell which makes a reliable hydrogen cyanide gas generation with a long life possible even under unfavorable and substantially changing environmental conditions, such as significant changes in temperature and environment.
  • According to the invention the object is accomplished by an electrochemical cell of the type mentioned above, wherein the electrolyte comprises at least one ionic liquid and includes thiocyanate ions for generating hydrogen cyanide gas.
  • Due to its high electrochemical stability with respect to oxidation and reduction, the use of ionic liquids makes it possible to provide electrochemical cells for generating hydrogen cyanide gas, e.g. to check gas analysing devices, whereby the electrochemical cells generate stable amounts of hydrogen cyanide gas without failing over a long life time and also at changing temperatures and environmental conditions. The use of ionic liquid as electrolyte makes it possible to have long storage periods for such gas generators without impacting their function in later use.
  • According to a preferred embodiment of the invention, the electrolyte comprises a mixture of at least two ionic liquids, thus allowing to easily select and set the melting point and water absorption capacity of the electrolyte by an appropriate choice of ionic liquids and/or their appropriate mixing ratio. The electrolyte preferably comprises at least one ionic liquid of the group of 1-butyl-3-methylimidazoliurn trifluoromethanesulfonate (hereinafter abbreviated as BMIM OTf), 1-ethyl-3-methylimidazolium trifluoromethanesulfonate (hereinafter abbreviated as EMIM OTf) and 1-ethyl-3-methylimidazolium thiocyanate (hereinafter abbreviated as EMIM SCN). These ionic liquids have been found to be particularly advantageous especially in view of the setting and adjusting options with respect to melting point and water absorption. In particular, the use of the mentioned ionic liquids and optionally of further additional substances results in reductions in the electroyte's melting point, which allows operation until far below the melting points of the individual ionic liquids and thus within the operating temperature range of the electrochemical cell, such as between −30° C. and +60° C.
  • Thiocyanate salt is preferably used as gas generating substance, and it is particularly advantageous to select it from the group NaSCN, KSCN, LiSCN, NH4SCN, NBu4SCN. However, thiocyanate can also be itself the anion of an ionic liquid.
  • It is particularly advantageous to have at least one noble metal as generator electrode, in particular one of the group of gold, rhodium, iridium, palladium or platinum, wherein platinum is particularly advantageous. The generator electrode is preferably formed as a platinum wire mesh or as a polytetrafluorethylene (in the following abbreviated as PTFE) gas diffusion membrane coated with the noble metal.
  • The container for the ionic liquid in the electrochemical cell is sealed to the outside by a PTFE gas diffusion membrane, which is permeable for the generated hydrogen cyanide gas. The generated hydrogen cyanide gas is discharged to the outside via this PTFE gas diffusion membrane.
  • It is advantageous to provide layers of glass fiber between the generator electrode and the counter electrode, the glass fiber being impregnated with the ionic liquid or with a mixture of ionic liquids, whereby these liquids comprise thiocyanate ions.
  • The counter electrode is preferably a PTFE support which is coated with platinum or platinum black, which is preferably porous.
    • DETAILED DESCRIPTION OF THE INVENTION
  • The present invention and preferred embodiments will be discussed below further with reference to the single drawing schematically showing an electrochemical cell according to the present invention.
  • An electrochemical cell 1 comprises a cell housing or container 2 at its bottom side above of which a counter electrode 3 is disposed on which ionic liquid 4 is provided. A generator electrode 5 is disposed on the side of the ionic liquid opposing the counter electrode 3. The generator electrode 5 acting as an anode and the counter electrode 3 acting as a cathode are connected to a constant current source 6.
  • On the outer side of generator electrode 5, which is formed for example as a wire mesh or as a gas diffusion membrane, another gas diffusion membrane is possibly provided, through which the generated hydrogen cyanide by diffusion passes out of the cell to the outside. The gas diffusion membrane 7 is additionally stabilized by a PTFE support grid 8.
  • The interior of the cell housing 2 containing the ionic liquid 4 preferably comprises glass fiber layers impregnated with ionic liquid containing thiocyanate ions.
  • The ionic liquid is selected in particular with regard of the melting point and the water absorbing capacity. BMIM OTf, EMIM OTf and EMIM SCN are of particular advantage. The ionic liquids can be used as a basis for the cell's electrolyte, either in its pure forms or as mixtures. It is preferred to have a proportion of 30-25 vol % of EMIM SCN in the mixture with EMIM OTf or BMIM OTf. Typically 0.2-0.4 mol/l lithium thiocyanate, potassium thiocyanate, sodium thiocyanate, ammonium thiocyanate or tetrabutylammonium thiocyanate are added to BMIM OTf. A proportion of 5-20% H2O is required as a reactant in all cases. It is also used to optimize the solubility of thiocyanate salts and the reaction products.
  • Current densities of the current provided by the constant power source 6 and flowing through ionic electrolyte 4 are typically between 0.3 1.5 mA/cm3. The generated hydrogen cyanide gas passes through the PTFE gas diffusion membrane 7 by diffusion out of the cell to the outside. For a performance test of hydrogen cyanide detectors a generator electrode area of preferably 3.8 cm2 and an operating current of about 2 mA with a power-on time of 30 s is advantageous, in order to generate hydrogen cyanide concentrations greater than 20 ppm in front of the outlet opening of the cell.
  • In the present embodiment the generator electrode consists of a platinum wire mesh or a coating of noble metal and preferably of platinum on the inner side of PTFE gas diffusion membrane 7. The counter electrode is a 0.25 mm PTFE gore membrane coated with platinum black. The electrochemical cell operates galvanostatically with current densities preferably between 0.5 and 1.5 mA/cm2. With a generator electrode having a diameter of 20 mm the optimum operating current is 2 to 3 mA.
  • The invention has been described with reference to preferred embodiments. However, a person skilled in the art is capable of further embodiments or modifications without departing from the scope of the invention.

Claims (11)

1. An electrochemical cell (1) having an electrolyte (4), a generator electrode (5) and a counter electrode (3), wherein the electrolyte (4) comprises at least one ionic liquid and contains thiocyanate ions for generating hydrogen cyanide gas.
2. An electrochemical cell (1) according to claim 1, wherein the electrolyte (4) comprises a mixture of at least two ionic fluids preferably from the group of 1-butyl-3-methylimidazolium trifluoromethanesulfonate, 1-ethyl-3-methylimidazolium trifluoromethanesulfonate and 1-ethyl-3-methylimidazolium thiocyanate.
3. An electrochemical cell (1) according to claim 1, wherein the gas generating substance is a thiocyanate salt.
4. An electrochemical cell (1) according to claim 3, wherein the thiocyanate salt is at least one of the group of NaSCN, KSCN, LiSCN, NH4SCN, NBu4SCN.
5. An electrochemical cell (1) according to claim 1, wherein the generator electrode (5) consists of a noble metal, preferably of one of the group of gold, rhodium, iridium, palladium and platinum.
6. An electrochemical cell (1) according to claim 5, wherein the generator electrode (5) is a noble metal wire mesh and preferably a platinum wire mesh.
7. An electrochemical cell (1) according to claim 5, wherein the generator electrode (5) is a PTFE gas diffusion membrane coated on one side with a noble metal.
8. An electrochemical cell (1) according to claim 1, wherein it is sealed to the outside by a PTFE gas diffusion membrane (7), which is permeable to the generated hydrogen cyanide gas.
9. An electrochemical cell (1) according to claim 1, wherein the ionic liquid (4) is provided in a housing or container (2) comprising glass fiber layers.
10. An electrochemical cell (1) according to claim 1, wherein the counter electrode (3) essentially consists of platinum.
11. An electrochemical cell (1) according to claim 10, wherein the counter electrode (2) is a PTFE coated with platinum.
US14/191,824 2013-03-01 2014-02-27 Electrochemical cell Abandoned US20140246309A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102013003559.7A DE102013003559B4 (en) 2013-03-01 2013-03-01 Process for producing hydrogen cyanide gas in an electrochemical cell
DE102013003559.7 2013-03-01

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DE (1) DE102013003559B4 (en)
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4256548A (en) * 1978-11-11 1981-03-17 International Business Machines Corporation Elimination of anode hydrogen cyanide formation in trivalent chromium plating
US4526662A (en) * 1982-09-09 1985-07-02 Byerley John J Processes for the recovery of cyanide from aqueous thiocyanate solutions and detoxication of aqueous thiocyanate solutions
US20030030963A1 (en) * 1996-05-15 2003-02-13 Howard Tennent Graphitic nanofibers in electrochemical capacitors
US20120028868A1 (en) * 2009-04-16 2012-02-02 Basf Se Removal of metal salt-comprising ionic liquids from workpieces and recycling of such liquids
US20120067745A1 (en) * 2009-03-10 2012-03-22 Senova Systems, Inc. Device for providing a means for internal calibration in an electrochemical sensor
US20120257357A1 (en) * 2009-10-05 2012-10-11 Taiyo Yuden Co., Ltd. Electrochemical capacitor

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2621677A1 (en) 1976-05-15 1977-11-24 Bayer Ag PROCEDURE FOR CHECKING GAS ANALYZERS
GB9302838D0 (en) * 1993-02-12 1993-03-31 City Tech Gas generating apparatus
EP1512460A1 (en) * 2003-09-05 2005-03-09 Solvent Innovation GmbH Preparation and use of ionic liquids having thiocyanat as anion
DE102010003496A1 (en) * 2009-04-08 2010-12-16 Basf Se Producing chlorine and simultaneously separating metal comprising e.g. aluminum, comprises providing electrolysis device, and separating chlorine at anode and metal at cathode from an ionic liquid containing ions of metal to be separated

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4256548A (en) * 1978-11-11 1981-03-17 International Business Machines Corporation Elimination of anode hydrogen cyanide formation in trivalent chromium plating
US4526662A (en) * 1982-09-09 1985-07-02 Byerley John J Processes for the recovery of cyanide from aqueous thiocyanate solutions and detoxication of aqueous thiocyanate solutions
US20030030963A1 (en) * 1996-05-15 2003-02-13 Howard Tennent Graphitic nanofibers in electrochemical capacitors
US20120067745A1 (en) * 2009-03-10 2012-03-22 Senova Systems, Inc. Device for providing a means for internal calibration in an electrochemical sensor
US20120028868A1 (en) * 2009-04-16 2012-02-02 Basf Se Removal of metal salt-comprising ionic liquids from workpieces and recycling of such liquids
US20120257357A1 (en) * 2009-10-05 2012-10-11 Taiyo Yuden Co., Ltd. Electrochemical capacitor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Bhattacharya et al, A nanoporous TiO2 electrode and new ionic liquid doped solid polymer electrolyte for dye sensitized solar cell application, Nanotechnology, Vol. 18, No. 48, November 2007, pp. 1-4 *
Sun et al, Application of 1-ethyl-3-methylimidazolium thiocyanate to the electrolyte of electrochemical double layer capacitors, Jounral of Power Sources, Vol. 162, No. 2, November 2006, pp. 1444-1450 *

Also Published As

Publication number Publication date
GB201403608D0 (en) 2014-04-16
GB2513459A (en) 2014-10-29
DE102013003559B4 (en) 2014-12-11
DE102013003559A1 (en) 2014-09-04

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