EP0095997B1 - Procédé pour la production de l'eau oxygénée et son utilisation - Google Patents

Procédé pour la production de l'eau oxygénée et son utilisation Download PDF

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Publication number
EP0095997B1
EP0095997B1 EP83710018A EP83710018A EP0095997B1 EP 0095997 B1 EP0095997 B1 EP 0095997B1 EP 83710018 A EP83710018 A EP 83710018A EP 83710018 A EP83710018 A EP 83710018A EP 0095997 B1 EP0095997 B1 EP 0095997B1
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EP
European Patent Office
Prior art keywords
oxygen
anode
water
solid electrolyte
cathode
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.)
Expired
Application number
EP83710018A
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German (de)
English (en)
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EP0095997A1 (fr
Inventor
Samuel Dr. Stucki
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BBC Brown Boveri AG Switzerland
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BBC Brown Boveri AG Switzerland
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Publication of EP0095997A1 publication Critical patent/EP0095997A1/fr
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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
    • 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
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
    • C25B9/23—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms comprising ion-exchange membranes in or on which electrode material is embedded
    • 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
    • C25B1/28—Per-compounds
    • C25B1/30—Peroxides

Definitions

  • the invention relates to a method for the electrolytic production of hydrogen peroxide according to the preamble of claim 1 and its use according to the preamble of claim 8.
  • Hydrogen peroxide is now produced either by the older peroxodisulfuric acid or the younger anthraquinone process.
  • the amount of electrical energy required in the first case is approx. 13,000 kWh and in the second case (in the case of electrolytic hydrogen production) approx. 2000 kWh per ton of hydrogen peroxide.
  • Hydrogen peroxide is produced, among other things, in electrolytic cells, provided that oxygen is present on the cathode side and the cathode is made of carbon or another material that promotes the electrochemical reduction of oxygen to H 2 0 2 .
  • the reaction equation is:
  • This harmful reaction is a particular problem in fuel cells, where it is known that oxygen is reduced to water.
  • a method and an electrolysis cell for the production of H 2 0 2 from an aqueous 0 2 emulsion (0 2 bubbles in suspension) containing an electrolyte (NaOH) are known, the liquid being a porous, made of graphite felt cross-penetrated.
  • the cathode and anode compartments are separated by a semi-permeable membrane made of plastic, among which cation exchangers (eg "Nafion 427", 152 E, 125 from Du Pont) are also mentioned.
  • the O 2 formed on the anode is returned to the cathode compartment.
  • US-A-3 856 640 describes the production of H 2 O 2 from an aqueous electrolyte in a continuous cell with a separator. “Nafion” is mentioned as a separator material. From EP-A-0 031 660 an electrolysis apparatus with plastic polymer as solid electrolyte, porous current collectors and porous film-like catalyst layers as electrodes is known, the latter being directly connected to the plastic polymer.
  • GB-A-2 071 157 describes a catalytic electrode on a polymer solid electrolyte. Pt metal oxides and [r0 2 / Ru0 2 mixtures are mentioned as electrode materials.
  • the invention has for its object to provide a production process for hydrogen peroxide H 2 0 2 , which provides a product with high economy while avoiding expensive separation and purification processes in a simple manner, which can be used as directly as possible in many fields.
  • the object is preferably achieved by the additional features specified in claim 5.
  • Fig. 1 the basic structure of a cell suitable for H 2 0 2 production is shown in section and its mode of operation is shown schematically.
  • 1 is the H 3 0 + - based solid electrolyte ionic conduction, which is preferably present as ion exchange membrane in the form of a film - or OH.
  • a perfluorinated polymer with sulfonic acids is advantageously used as the ion-exchanging groups.
  • the solid electrolyte does not have to assume the function of gas separation, but rather only has to separate the electrodes of opposite polarity, that is to say it has to be held at a certain minimum distance to avoid short-circuits and also serves as an ion conductor, this film can be very thin . It may also be porous, ie gas permeable. As a suitable material such. B. used a Du Pont product known under the trade name “Nafion” will.
  • On the solid electrolyte 1 there is a gas-permeable, electrically conductive coating 2 acting as an anode on the positive side marked with +, and a coating 3 with similar properties acting as cathode on the negative side marked by.
  • the coating 2 acting as an anode is advantageously designed as an electrocatalyst based on platinum metals, platinum metal oxides or mixtures thereof, preferably as an IrO 2 / RuO 2 layer. In the case of an OH - -conducting electrolyte, this coating would preferably consist of NiO.
  • the coating 3, which acts as a cathode, on the other hand, must consist of a material which catalytically promotes the reduction of O 2 to H 2 0 2 , which includes, in particular, activated substances containing elemental carbon (eg carbon powder) and certain metal chelates.
  • the electron currents 2e are also indicated by arrows both on the anode and on the cathode side.
  • Fig. 2 represents the functional diagram illustrates an electrolytic cell for a first variant of the manufacturing process for H 2 0 2.
  • the reference numerals 1-4 exactly correspond to those of Fig. 1.
  • Both the like of the resulting externally supplied feed gas stream 1 ⁇ 2 O 2 on the anode side and gas stream 1 ⁇ 2 O 2 conducted around the solid electrolyte 1 and fed to the cathode side is shown by corresponding arrows.
  • the other symbols result analogously to FIG. 1.
  • FIG. 3 shows the functional diagram of an electrolytic cell for a second variant of the production process for H 2 0 2 .
  • the reference numerals 1-4 correspond exactly to those in FIG. 1.
  • the solid electrolyte 1 is designed here as a gas-permeable membrane.
  • the gas stream 1 ⁇ 2 O 2 supplied from the outside, as well as the gas stream 1 ⁇ 2 O 2 arising on the anode side and the two combined gas streams passing through the solid electrolyte 1 are drawn in the figure in the stoichiometrically correct ratio and provided with arrows. All other symbols result in the same sense as shown in Fig. 1.
  • Fig. 4 shows the schematic structure of an electrolysis device for producing H 2 0 2 in section.
  • the components corresponding to reference numerals 1-4 are identical to those of FIG. 1.
  • 7 is a pressure vessel constructed on a base plate 8 in a water-tight and gas-tight manner for receiving the electrolytic cell in the narrower sense.
  • the latter has on the positive side a space closed on all sides, the anode chamber 9, which is provided on its upper side with an overflow nozzle 10 for H 2 0 and O 2 .
  • the cathode chamber 11 which has an opening on its upper end face, the inflow support 12 for 0 2 or the oxygen-containing gas, for. B. air (0 2 + N 2 ).
  • 13 is the water supply line (feed), 15 is a circulation pump for the water.
  • a level control 16 (indicated symbolically) is provided, which is controlled by a regulating valve 14.
  • 17 is the supply line for the oxygen or the oxygen-containing gas (e.g. air), indicated by the symbol (N 2 ) +0 2 .
  • 18 represents a valve for keeping the pressure constant (p o ) in the pressure vessel 7, 19 the H 2 0 2 discharge (removal), which also carries the solvent H 2 0 and the excess oxygen-containing gas (N 2 ) +0 2 .
  • the flow directions are shown by arrows.
  • 1 ⁇ 2 O 2 must therefore additionally be supplied to the outside of the cell, which is symbolically indicated in FIG. 1 by an arrow pointing obliquely downwards on the cathode side.
  • the other half amount of oxygen corresponding to 1 ⁇ 2 O 2 comes from electrolysis from the anode (arrow pointing vertically upwards) and must also be brought to the cathode side in some way.
  • the electrolytic cell used to carry out the method had, as solid electrolyte 1, a membrane made of a perfluorinated polymer with sulfonic acids with the trade name “Nafion 120” from Du Pont.
  • This Nafion film was provided on the positive side with a gas-permeable coating 2 made of a noble metal mixed oxide acting as an anode, in this case according to the formula (Ru o , 5 Ir 0.5 ) O 2 .
  • the negative side carried the gas-permeable coating 3 acting as a cathode in the form of a graphite coating.
  • the current was supplied via the current collectors 4, a film made of porous sintered titanium being used on the anode side and a mesh (wire mesh) made of nickel being used on the cathode side.
  • the cell was closed and held together by a frame made of titanium, forming the anode chamber 9 and the cathode chamber 11.
  • an opening was provided in each frame on the lower and the upper end.
  • the upper part of the anode chamber 9 had an overflow connection 10 for H 2 0 and O 2 and the cathode chamber 11 had an inflow connection 12 for O 2 or O 2 + N 2 .
  • the anode chamber 9 was fed via the water supply line 13 (feed) and the regulating valve 14 with demineralized water of 80 ° C.
  • the cathode chamber 11 was supplied with a humidified 0 2 stream of approximately 1 l / h via the connector 12. Now a direct current source 5 has been connected to the current collectors 4 of the cell.
  • the voltage U was gradually increased. At a voltage of approx. 1 V, the current rose. At the voltage of 1.4 V, a current density of 10 mA / cm 2 was established .
  • the water transported by the current flow through the solid electrolyte 1 was collected in the cathode chamber 11 and examined for its H 2 O 2 content. This was done by means of a decolorization reaction of a permanganate solution. An H 2 0 2 concentration of 3% by weight in water can generally be expected.
  • a cell designed according to Example I was installed in a gas-tight pressure vessel 7 closed at the bottom by a base plate 8.
  • the openings made on the lower end faces of the anode chamber 9 and the cathode chamber 11 were passed through the base plate 8 and connected to the water supply line 13 and the H 2 O 2 discharge line 19 (removal).
  • the pressure vessel 7 was now filled by feeding water through the water supply line 13 and the regulating valve 14 up to the level control 16 mark.
  • the entire pressure vessel 7 was then placed under a pressure p o of 10 MPa on both the gas and water side.
  • the valve 18 for keeping the pressure constant (p " ) ensured that this pressure was maintained. It goes without saying that the oxygen-containing gas fed in via the feed line 17 (in this case compressed air N 2 + O 2 ) and the feed via the feed line 13 The device was then put into operation by connecting a power source (see FIG. 5 in FIG. 1) to the current collectors 4 and switching on the circulation pump 15. At a direct voltage of 1.4 V. and a regulated supply of compressed air of 0.5 l / h, a current density of 100 mA / cm 2 was achieved The H 2 0 2 content of the aqueous solution taken off was on average 3% by weight.
  • the invention is not restricted to the exemplary embodiments.
  • the process can also be carried out with tap water of up to 5 g / l salinity.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Claims (8)

1. Procédé pour la génération électrochimique d'eau oxygénée, H202 à partir d'eau et d'oxygène dans une cellule électrolytique, caractérisé en ce que l'on met en oeuvre en tant qu'électrolyte un corps électrolytique solide (1) conducteur des ions H30+- ou OH--sous forme d'une membrane échangeuse d'ions qui présente sur ses faces latérales des couches poreuses, perméables au gaz, conductrices de l'électricité (2, 3), faisant fonction d'anode et de cathode, et en ce que l'on fait passer de l'eau pure ou de l'eau du réseau avec une teneur en sels pouvant aller jusqu'à 5 g/I sur le côté anode du corps électrolytique solide (1) et un gaz contenant de l'oxygène ou de l'oxygène pur sur le côté cathode et en ce que l'on prélève du côté cathode l'H202 obtenue.
2. Procédé selon la revendication 1, caractérisé en ce que l'eau du réseau que l'on amène au corps électrolytique solide (1) est dépourvue de cations polyvalents.
3. Procédé selon la revendication 1, caractérisé en ce que l'on alimente le corps électrolytique solide (1) en eau pure entièrement désionisée.
4. Procédé selon la revendication 1, caractérisé en ce que l'on met en ceuvre une membrane échangeuse d'ions en tant que corps électrolyte solide (1), sous forme d'un film du type polymère perfluoré avec des acides sulfoniques en tant que groupes échangeurs d'ions, lequel porte d'un côté une couche perméable aux gaz (2) à base de IrO2/RuO2, jouant le rôle d'anode et de l'autre côté une couche perméable aux gaz (3) à base de poudre de charbon, jouant le rôle de cathode, et en ce que l'on prévoit en tant qu'alimentation de courant, au moins du côté de la cathode, un collecteur de courant (4) de type grille ou de type toile.
5. Procédé selon la revendication 1, caractérisé en ce qu'aussi bien l'oxygène amené de l'extérieur que l'oxygène engendré à l'anode sont amenés à la cathode du côté ne faisant pas face au corps électrolyte solide.
6. Procédé selon la revendication 1, caractérisé en ce que l'on met en oeuvre en tant que corps électrolytique solide (1) une membrane échangeuse d'ions poreuse, perméable au gaz oxygène, et en ce que l'on amène l'oxygène venant de l'extérieur ainsi que l'eau du côté anode de la cellule, et qu'on les fait passer avec l'oxygène obtenu à l'anode à l'aide d'une surpression, à travers le corps électrolytique solide poreux (1) pour atteindre le côté cathode.
7. Procédé selon la revendication 1, caractérisé en ce que l'on amène l'eau par une conduite d'eau (13) à une cellule électrolytique qui se trouve dans un récipient pressurisé (7) placé sous la pression po avec une plaque de base étanche (8), constituée d'un corps électrolyte solide (1), de couches perméables aux gaz (2, 3) et de collecteurs de courant (4) et possédant une chambre anodique (9) avec un déversoir (10) pour l'eau et l'oxygène, de même qu'une chambre cathodique (11) avec un moyen d'entrée (12) pour l'oxygène ou pour un gaz contenant de l'oxygène, sur le côté de la chambre anodique (9) et qu'on la maintient en circulation permanente au moyen d'une pompe de circulation (15), en ce que l'on amène l'oxygène ou le gaz contenant de l'oxygène, introduit de l'extérieur, par une conduite d'amenée (17) dans l'espace humidifié ou non-humidifié du récipient pressurisé (7) et en ce que l'on introduit l'oxygène obtenu dans la chambre anodique (9) par le déversoir (10) dans l'espace supérieur, non-humidifié du récipient pressurisé (7) et en ce que l'on comprime tout l'oxygène sur ledit espace non-humidifié dans la chambre cathodique (11) de la cellule, où l'on maintient la même pression du côté de l'anode et du côté de la cathode, et en ce que l'on maintient en outre le niveau d'eau dans le récipient pressurisé (7) dans des limites extrêmement étroites, par l'intermédiaire d'un contrôleur de niveau (16) qui actionne une vanne régulatrice (14) dans la conduite d'amenée d'eau (13) et en ce que l'on prélève finalement de la cellule, en tant que produit, une solution aqueuse d'eau oxygénée, qui peut contenir encore des composants d'oxygène et/ou d'azote atmosphérique, par l'intermédiaire d'une conduite de retrait (19) munie d'une vanne (18) prévue pour le maintien d'une pression constante.
8. Mise en oeuvre du procédé selon la revendication 1 pour la fabrication d'une solution aqueuse d'H202, pour la stérilisation et l'épuration directes de l'eau, et pour sa décoloration, aussi bien seul qu'en combinaison avec une irradiation ultraviolette.
EP83710018A 1982-05-28 1983-04-11 Procédé pour la production de l'eau oxygénée et son utilisation Expired EP0095997B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH329482 1982-05-28
CH3294/82 1982-05-28

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EP0095997B1 true EP0095997B1 (fr) 1987-04-01

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EP (1) EP0095997B1 (fr)
JP (1) JPS58213885A (fr)
DE (1) DE3370657D1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107317051A (zh) * 2017-06-05 2017-11-03 南京大学 一种以过氧化氢为添加剂的锂‑氧气电池电解液的制备方法

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JP2574678B2 (ja) * 1987-08-07 1997-01-22 工業技術院長 過酸化物を含有する水溶液の製造装置
JP2558042B2 (ja) * 1992-09-03 1996-11-27 本州製紙株式会社 過酸化水素の製造方法
DE4317349C1 (de) * 1993-05-25 1994-10-13 Metallgesellschaft Ag Verfahren zur Herstellung von Alkaliperoxid/Percarbonat-Lösungen
US5645700A (en) * 1994-12-28 1997-07-08 Eltron Research, Inc. Polymer membrane based electrolytic cell and process for the direct generation of hydrogen peroxide in liquid streams
BR9610837A (pt) * 1995-10-06 1999-07-13 Dow Chemical Co Membrana composta reator e método para a sintese de peróxido de hidrogênio
US6255009B1 (en) 1998-03-28 2001-07-03 The United States Of America As Represented By The Secretary Of The Navy Combined cycle power generation using controlled hydrogen peroxide decomposition
US6316653B1 (en) * 1998-07-06 2001-11-13 The Trustees Of Princeton University Mn4O4-cubane type catalysts
FR2784979B1 (fr) * 1998-10-26 2001-09-28 Cie Ind Pour Le Traitement De Procede electrochimique de desinfection des eaux par electroperoxydation et dispositif pour la mise en oeuvre d'un tel procede
WO2001010215A1 (fr) 1999-08-05 2001-02-15 Steris Inc. Synthese electrolytique de l'acide peracetique
EP1170259A1 (fr) * 2000-07-05 2002-01-09 Sony International (Europe) GmbH Dispositif électrochimique et procödé de purification de fluids
DE10054082A1 (de) * 2000-10-31 2002-05-16 Forschungszentrum Juelich Gmbh Verfahren zur enzymatischen Oxidation von Substraten mit H2O2
ITMI20061799A1 (it) * 2006-09-21 2008-03-22 Industrie De Nora Spa Cella di elettrolisi per la produzione di acqua ossigenata e metodo di utilizzazione
US7754064B2 (en) * 2006-09-29 2010-07-13 Eltron Research & Development Methods and apparatus for the on-site production of hydrogen peroxide
WO2011036633A2 (fr) 2009-09-23 2011-03-31 Ecolab Usa Inc. Système de nettoyage in situ
US8937037B2 (en) 2011-03-02 2015-01-20 Ecolab Usa Inc. Electrochemical enhancement of detergent alkalinity
CA2960965A1 (fr) 2014-08-15 2016-02-18 Global Oil EOR Systems, Ltd. Generateur de vapeur de peroxyde d'hydrogene pour des applications petroliferes
EP3378999B1 (fr) 2015-08-24 2021-05-05 Kohler Co. Toilette avec un levier de chasse d'eau, comprenant un distributeur de produits chimiques
CN106939427B (zh) * 2017-02-23 2018-08-28 清华大学 一种利用自供氧双阴极装置同时产生双氧水和氢气的方法
CN108545804A (zh) * 2018-05-08 2018-09-18 凡邸（天津）环保科技有限公司 一种基于生物电化学、高级氧化耦合体系杀灭细菌的方法
JP7126654B2 (ja) * 2018-09-05 2022-08-29 富士電機株式会社 電気分解ユニット
CN113774409B (zh) * 2021-09-24 2023-12-19 浙江清越科技有限公司 一种静置式平板过氧化氢电化学发生器

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Publication number Priority date Publication date Assignee Title
CN107317051A (zh) * 2017-06-05 2017-11-03 南京大学 一种以过氧化氢为添加剂的锂‑氧气电池电解液的制备方法

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DE3370657D1 (en) 1987-05-07
EP0095997A1 (fr) 1983-12-07
JPS58213885A (ja) 1983-12-12
US4455203A (en) 1984-06-19

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