WO2014204332A1 - Cellule modulaire électrochimique pour le traitement de solutions d'électrolytes - Google Patents

Cellule modulaire électrochimique pour le traitement de solutions d'électrolytes Download PDF

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Publication number
WO2014204332A1
WO2014204332A1 PCT/RU2013/000501 RU2013000501W WO2014204332A1 WO 2014204332 A1 WO2014204332 A1 WO 2014204332A1 RU 2013000501 W RU2013000501 W RU 2013000501W WO 2014204332 A1 WO2014204332 A1 WO 2014204332A1
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Prior art keywords
cathode
cell
anodes
anode
devices
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PCT/RU2013/000501
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English (en)
Russian (ru)
Inventor
Витольд Михайлович БАХИР
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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
    • C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
    • C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
    • 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

Definitions

  • the invention relates to the field of chemical technology, in particular to devices for electrochemical processing of electrolyte solutions, and can be used in the processes of electrochemical production of various chemical products by electrolysis of aqueous solutions, in particular, in the process of producing a mixture of oxidants in the electrolysis of an aqueous solution of alkali or alkaline earth metal chlorides .
  • a mixture of oxidants can be used in water purification and disinfection processes, in processes related to the electrochemical regulation of acid-base, redox properties and catalytic activity of water and / or aqueous solutions, as well as in the processes of obtaining various chemical products.
  • flow diaphragm electrolyzers of various designs are used, containing both flat electrodes with a flat diaphragm installed between them, and coaxially arranged cylindrical electrodes with coaxially placed between them aperture.
  • Such electrolyzers are usually designed with a fixed capacity for the target products.
  • modular electrolyzers which achieve the required performance by connecting the required number of electrochemical modular cells, which reduces the cost of designing and manufacturing electrolyzers of fixed capacity, unify parts and assemblies, and reduce the time of installation and repair of such electrolyzers.
  • design of the electrochemical cell is essential, which determines all the advantages and disadvantages of a modular electrolyzer.
  • electrochemical modular cell containing a main electrode mounted 5 vertically, a cylindrical counter electrode also mounted vertically, a ceramic diaphragm placed coaxially with the main electrode and dividing the interelectrode space into sealed anode and cathode chambers, lower and upper sealing devices, devices for supplying processed liquids to the cathode and anode chambers and devices for I drain liquids and gases from the anode and cathode chambers (see US Patent N 5635040, C 02 F 1/461, 06/03/97).
  • the electrolyte or water solution is treated with a single or multiple (using an external circulation circuit) flow 15 of the treated solution through the electrode chambers of the cell from the bottom up.
  • Devices of the required performance are made of the required number of electrochemical modular cells.
  • the electrodes and the diaphragm are cylindrical and 25 are fixed in special dielectric bushings and heads, the latter being mounted for rotation.
  • the bushings and heads channels are made for supplying and discharging the treated aqueous solution from the electrode chambers.
  • preferred cell sizes are indicated. Such an implementation is relatively complicated, requires pairing a large number of parts, while there are requirements for maintaining the tightness of the cell, which requires the use of a significant number of sealing parts.
  • the known cell can be made in a narrow range of sizes, and, as a result, has a relatively small performance.
  • a disadvantage of the known cell is the fact that it works mainly with a fixed connection of the electrodes in such a way that the main electrode located inside the diaphragm is the anode and the external counter electrode is the cathode. This is due to the fact that there are significant difficulties in applying anodic electrocatalytic coatings to the inner surface of tubular electrodes.
  • a well-known electrochemical cell operating at a current strength of 8 - 10 A and on concentrated (more than 10 g / l) chloride solutions, it is impossible to control the composition and properties of catholyte, as well as its purity (amount of chlorides entering the catholyte). Due to the intense gas evolution in the anode chamber, the tightness of the cell chambers can be violated over time, which leads to a deterioration in the performance of the reactor based on electrochemical modular cells.
  • the technical result achieved by using the invention is to provide the possibility of increasing cell productivity by anode products, while simplifying the design of the cell, and making it possible to arrange the required number of cells in a smaller space, simplifying the fixation nodes of the cell elements while improving reliability, simplifying the design of high power reactors due to reducing auxiliary communications, as well as expanding the functionality of the cell, which is achieved at the expense of providing opportunities regulating the properties of catholyte and anolyte; and increasing the purity of the resulting products.
  • an electrochemical module cell for processing electrolyte solutions containing a cylindrical main electrode mounted vertically, a cylindrical counter electrode also mounted vertically, a ceramic diaphragm placed coaxially with the main electrode and dividing the interelectrode space into sealed anode and cathode chambers, the lower and top sealing devices, devices for supplying processed fluids to the cathode and anode chambers , devices for draining liquids and gases from the anode and cathode chambers, the upper and lower sealing devices are made in the form of plugs, and the cell contains one or more main vertical electrodes and more than one counter electrode (with respect to each main electrode), and the main electrodes are cathodes and counter electrodes — by anodes.
  • the anodes in the cell are fixed in the upper and lower plugs, the diaphragms are mounted either on the plugs or on the cathodes, and the cell is equipped with a housing on which the plugs are installed on the upper and lower parts.
  • the electrodes In the inner space of the casing there are electrodes that are installed at the vertices and center of one or more regular polygons inscribed in the plane of the cross section of the casing.
  • a cathode and a diaphragm are installed at the center of each regular polygon, and anodes at the vertices of the polygon.
  • the anodes can be made hollow and equipped with devices for supplying and removing coolant, which are connected respectively to the lower and upper ends of the anodes.
  • the cathode in the cell can be made of metal or graphite.
  • the cathode can be made tubular, and additionally contain devices for supplying and removing coolant, respectively connected to the ends of the cathode.
  • perforations can be made on the surface of the cathode, and devices for supplying the liquid to be processed into the cathode chamber, and devices for removing liquids and gases from the cathode chamber, can be connected to the lower and upper ends of the cathode, respectively.
  • the plugs and the cell body can be made of a dielectric acid-base material or of metal, while the inner surface of the metal parts is coated with a layer of a dielectric acid-base material.
  • One regular polygon with the number of vertices 3 - 12, or several close-packed regular polygons, each of which is either an equilateral triangle or a square or hexagon, can be inscribed in the plane of the cross section of the body.
  • the cell diaphragm must be made of acid-alkali-resistant nanostructured ultrafiltration ceramics.
  • an electrochemical modular cell for processing electrolyte solutions containing a main electrode mounted vertically, a cylindrical counter electrode also mounted vertically, a ceramic diaphragm placed coaxially with the main electrode and dividing the interelectrode space into sealed anode and cathode chambers, lower and upper sealing devices made in the form of plugs and the cell contains one or more main vertical electrodes and more than one prot of the electrode (with respect to each main electrode), with the main electrodes being the cathodes and the counter electrode as the anodes, it becomes possible to increase the cell performance of the anode products and place more electrodes in a smaller space, which also leads to a reduction in the number and length of auxiliary communications when combined cells in the reactors.
  • the anodes in the cell are fixed in the upper and lower plugs and the diaphragms are fixed either on the plugs or on the cathodes. This simplifies the manufacturing process of the cell.
  • the fact that the cell is equipped with a housing with plugs on its upper and lower parts allows to increase the safety of the cell, since in this case, unlike the prototype, the outer surface of the cell is not an electrode.
  • the electrodes are located in the interior of the housing, and are installed at the vertices and center of one or more regular polygons inscribed in the plane of the cross section of the housing.
  • a cathode and a diaphragm are installed at the center of each regular polygon, and anodes at the vertices of the polygon.
  • This implementation allows for constancy the distance between the electrodes and the diaphragm at any possible pressure drops, maintain the stability of the cell. Moreover, the fact that the number of anodes exceeds the number of cathodes allows one to directionally change the properties of solutions obtained by electrolysis, and, in particular, to increase the concentration of catholyte at
  • the heat removal system from the anode chamber can be constructed differently, for example, in the form of hollow tubes located in the anode chamber connected to means for supplying and removing heat carrier, or supplying a cooling case
  • the coolant can be directed by direct flow or countercurrent with respect to the movement of the electrolyte processed in the anode chamber.
  • the 20 cathode chambers can be installed both on sealing devices and on the side surfaces of the housing.
  • the choice of constructive execution is determined by the required performance and spatial limitations of the placement of cells.
  • the cathode in the cell can be made of metal or graphite.
  • the choice of 25 cathode material is determined by the conditions of the problem being solved, that is, the requirements for optimizing the ongoing electrochemical process, and depends both on the composition of the electrolyte and on the requirements for the type and quality of the products obtained.
  • the cathode can also be performed in various ways.
  • the cathode may be tubular, and further comprise devices for supplying and discharging the coolant, connected respectively to the ends of the cathode. This allows you to intensify the electrolysis process due to the removal of excess heat generated at the cathode.
  • the coolant can be directed by direct flow or countercurrent with respect to the movement of the electrolyte processed in the cathode chamber.
  • various methods of supplying the processed electrolyte to the cathode chamber can be applied.
  • the cathode is tubular, perforations can be made on the surface of the cathode, while devices for supplying the liquid to be processed into the cathode chamber, and devices for removing liquids and gases from the cathode chamber, can be connected to the lower and upper ends of the cathode, respectively.
  • This embodiment is advisable to apply in conditions when it is necessary to organize the effective circulation of catholyte in the cathode chamber of the cell due to gas lift.
  • the holes can be equipped with visors located in the upper part of the holes along the course of the solution in the chamber.
  • the plugs and the cell body can be made of various materials. They can be made of a dielectric acid-base material, for example glass, ceramics, fluoroplastic, polyvinyl chloride, polypropylene. They can also be made of metal, while the inner surface of the housing parts and plugs must be coated with a layer of dielectric acid-base material.
  • the material for the manufacture of body parts and plugs is determined by the conditions of the problem. The use of dielectrics is advisable in the design of cells containing a relatively small number of electrodes, for example, one cathode and three to six, in some cases (when using electrodes of relatively small diameters) up to twelve anodes.
  • One regular polygon with the number of vertices 3 - 12, or several close-packed regular polygons, each of which is either an equilateral triangle or a square or hexagon, can be inscribed in the plane of the cross section of the body.
  • the number of electrodes, their size (and, accordingly, the choice of the pattern by which they are placed inside the housing) is also determined by the conditions of the problem being solved.
  • the number of anodes can be
  • the number of anodes cannot be less than three, since otherwise it is impossible to ensure comparative uniformity of the electric field (and the characteristics of the electrolysis process).
  • the number of anodes is impractical to increase over twelve, as this will require either an increase in the outer diameter of the cell, which in turn will lead to an increase in the interelectrode distance, possible violations of the hydraulic regime of electrolyte movement, or the placement of anodes with small gaps between them, which will lead to uneven density distribution current on the surface of the anodes.
  • the number of anodes will be determined by the choice of the pattern of their placement. In this case, the electrodes
  • the 20 can provide close packing of polygons in a plane.
  • the type of polygons - an equilateral triangle, square or equilateral hexagon - is selected depending on the selected cross-sectional shape of the casing and the conditions of the problem being solved - the requirements for the electrolysis process and the requirements for the materials of the casing and flange plugs.
  • the cell diaphragm must be made of acid-alkali-resistant nanostructured ultrafiltration ceramics.
  • the diaphragm may be made of ceramic based on metal oxides, in particular, based on aluminum oxide, and may contain various additives, including additives of oxides of zirconium, yttrium, niobium, tantalum, titanium, gadolinium and hafnium. In this case, the aperture is performed by ultrafiltration.
  • FIG. 1 shows the upper part of the cell containing one cathode and four anodes.
  • FIG. Figure 2 shows the cross section of the cell body containing cathodes and anodes distributed in the cell cross section, respectively, at the centers and vertices of close-packed regular hexagons inscribed in the cross section of the cell.
  • FIG. 3 shows a diagram of an apparatus for producing a mixture of oxidants, in accordance with which comparative tests of the cells of the present invention and the cells of the prototype were performed.
  • the electrochemical modular cell for processing aqueous solutions contains a vertical cylindrical inner hollow cathode 1 and four anodes 2.
  • the cathode 1 and anodes 2 are located respectively in the center and at the tops of the square inscribed in the cross section of the housing 3.
  • a sealing plug 4 is installed at the upper end of the housing 3 .
  • a cathode 1, anodes 2 and a diaphragm 5 are fixed on the sealing plug 4.
  • the diaphragm 5 divides the interelectrode space into the anode 6 and the cathode 7 of the chamber.
  • a device for removing liquids and gases from the anode chamber is also located on the upper plug; devices for removing liquids and gases from the cathode chamber are connected to the cavity of the cathode 1 (not shown in the drawing).
  • a plug is installed, made similar to the upper plug, on which the cathode 1, anodes 2, diaphragm 5, and a device for supplying the processed fluids to the anode chamber 6 and a device for supplying the processed fluids to the cathode chamber 7 connected to the cavity of the cathode 1 are fixed (on not shown).
  • the cathode 1 is made with perforations 8, providing the flow of the processed fluid into the space between the outer surface of the cathode 1 and the inner surface of the diaphragm 5.
  • the cell works as follows.
  • the processed liquid enters, and through a device for supplying the processed liquids to the anode chamber 6, placed on the lower sealing plug (not shown in the drawing), the processed liquid enters - for example, a solution of sodium chloride.
  • water fills the cavity of the cathode 1 and through the holes 9 enters the space between the diaphragm 5 and the outer surface of the cathode 1, that is, into the cathode chamber 7.
  • the flow of water into the cathode chamber 7 is stopped after it is filled.
  • gas hydrogen gas
  • gas bubbles trap the catholyte (liquid in the cathode chamber) up.
  • the catholyte enters the space between the diaphragm 5 and the outer surface of the cathode 1, and through the upper holes 8 it is discharged into the inner cavity of the cathode 1 and is removed from the cell. Since electrolysis does not occur on the inner surface, the catholyte simply fills the inner space of the hollow electrode and, since it is less saturated with gas bubbles and has a greater apparent density, a slow catholyte circulation occurs in the hollow cathode chamber 1.
  • the perforation holes 8 are located along a helical line along of the entire surface of the cathode 1, then part of the hydrogen bubbles from the space between the outer surface of the cathode 1 and the inner surface of the diaphragm 5 penetrates into the inner cavity of the cathode 1, where x coalescence, accompanied by a significant acceleration of circulation in the internal cavity of the cathode 1 due to the separation of the gas and liquid phases.
  • the hydrogen bubbles move up while the liquid freed from the gas phase moves down and enters the working space of the electrode 1 through the lower perforation holes.
  • an electrolyte for example, a solution of sodium chloride enters the treatment through a device for supplying the processed liquids to the anode chamber located on the lower sealing plug (not shown in the drawing), and, passing the anode chamber 6 from the bottom up, it is discharged through device for draining liquids and gases from the anode chamber 6.
  • the electrolyte is circulated in the anode chamber 6 due to the convective movement of the electrolyte under the action of gases released at the anodes 2, in particular chlorine and in small lichestvah - oxygen.
  • metal ions in particular, sodium
  • a cell containing 7 cathodes and 24 anodes which are installed in accordance with the following rule: 7 regular hexagons are inscribed in the cross section of the cell body made of CPVC pipe with an inner diameter of 200 mm, cathodes made of steel pipe are installed at their centers 12X18H10T, with an external diameter of 16 mm and a wall thickness of 1.5 mm, surrounded by a diaphragm with a thickness of 2.5 mm, with an external diameter of 28 mm made of ceramic based on aluminum oxide (A1 2 0z).
  • the anodes are made of titanium tube grade VT 1-00 with an electrocatalytic coating ORTA deposited on its surface.
  • the interelectrode distance is 12 mm, while the outer diameter of the anode is 16 mm with a pipe wall thickness of 1 mm.
  • a coolant — water — was supplied to the internal cavities of the anodes at a rate of 20 liters per hour through each anode.
  • the heat carrier was supplied by direct flow in relation to the electrolyte solution being treated.
  • the housing and sealing plugs are made of chlorinated polyvinyl chloride (CPVC).
  • Devices for supplying the processed electrolytes to the cathode and anode chambers and devices for removing liquid and gaseous electrolysis products from the anode and cathode chambers (fittings) are installed on sealing plugs.
  • Installation for producing a mixture of oxidants contains a reactor 9 made of modular cells or cells.
  • Cells or cell contain anode 6 and cathode 7 cameras.
  • the installation also contains a container with a processed solution 10, a pump 11, a circulation loop of the cathode chamber 7 with a separation tank 12, a line for supplying the processed solution 13 to the anode chamber 6, a discharge line for catholyte 14, an output line for the mixture of oxylants 15 with a regulator installed on it pressure "to yourself" 16, the discharge line of the gas-liquid mixture (hydrogen and catholyte) 17 with a primary separator 18 installed on it.
  • the gas-liquid mixture — hydrogen and catholyte — is removed from the cathode chamber 7 through a line 17.
  • hydrogen is separated from the catholyte, after which hydrogen is removed from the system, and the catholyte enters the circulation tank 12. Excess catholyte is discharged from tank 12
  • the installation with a cell according to the invention consumed 2.94 liters of saline per hour, while the installation with 16 cells according to the prototype consumed 3.5 liters per hour.
  • the concentration of sodium hydroxide in catholyte from the installation with a cell according to the invention was 194 g / l, and from the installation with 16 cells according to the prototype it was 163 g / l, which indicates a more complete use of salt in the installation with a cell according to the invention.
  • the voltage on the electrochemical cell of the reactor of the installation with the cell according to the invention was 4.3 V during operation, while the voltage on the cells of the prototype in the installation was 4.7 V. Therefore, the electric power consumed to produce an equal amount of chlorine in installation with 16 cells of the prototype with the investigated operating mode is 8% more than in the installation with a cell according to the invention.
  • the current strength was 400 amperes
  • the voltage at the terminals of the current source was 4.3 V
  • the installation's chlorine gas productivity was 500 g / h.
  • the parameters of the installation with 16 cells according to the prototype were as follows: the current strength in a circuit of four groups of electrically parallel connected cells, where in each group four cells are electrically connected in series, was 100 amperes at a voltage of 22.5 volts against 18.8 volts at the beginning comparative tests. Therefore, the electric power spent on the production of chlorine after 60 hours of continuous operation increased by 16% in the installation with 16 cells of the prototype and remained unchanged in the installation with a cell according to the invention.
  • the voltage on the unit cell with the cell according to the invention increased to 4.8 volts.
  • the electrolyte temperature in the cell increased by 1 degree in comparison with the temperature at a current of 400 A equal to 34 ° ⁇ and, having reached 35 ° ⁇ , remained at this level during the duration of the comparative tests that lasted 48
  • EFFECT makes it possible to increase cell productivity by anode products, while simplifying cell design and providing the possibility of arranging the required number of cells in a smaller space, to simplify fixation units of cell elements while increasing reliability, to simplify the creation of high power reactors by reducing auxiliary communications, and expand the functionality of the cell by providing the ability to control the properties of catholyte and anolyte and Improving the purity of the resulting products.

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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)

Abstract

La présente invention se rapporte au domaine de l'électrotechnique, concerne notamment un dispositif pour le traitement électrochimique de solutions aqueuses, et peut être utilisée par exemple lors de l'électrolyse de solutions aqueuses de de chlorures de métaux alcalins ou alcalino-terreux. Cette cellule modulaire électrochimique pour le traitement des solutions susmentionnées comprend une ou plusieurs électrodes cylindriques principales verticales consistant en des cathodes, un diaphragme céramique disposé coaxialement par rapport à l'électrode principale et séparant l'espace entre les électrodes en des chambres hermétiques d'anode et de cathode, des équipements d'étanchéité inférieur et supérieur sous forme de bouchons, des équipements pour l'alimentation en fluides à traiter dans les chambre, et des équipements pour évacuer les liquides et les gaz des chambres d'anode et de cathode. La cellule comprend plus d'une contre-électrode cylindrique ou anode. La cellule modulaire comprend un corps sur les parties supérieure et inférieure duquel sont installés les bouchons, les anodes de la cellule étant fixées sur les bouchons supérieur et inférieur. Les diaphragmes sont fixés sur les bouchons ou sur les cathodes. Les électrodes de la cellule sont disposées dans les sommets et les centres de polygones droits étroitement serrés inscrits dans le plan de la section transversale du corps. L'invention permet d'augmenter la productivité de la cellule électrochimique modulaire du point de vue des produits anodiques et de simplifier l'assemblage de la structure.
PCT/RU2013/000501 2013-06-17 2013-06-17 Cellule modulaire électrochimique pour le traitement de solutions d'électrolytes Ceased WO2014204332A1 (fr)

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PCT/RU2013/000501 WO2014204332A1 (fr) 2013-06-17 2013-06-17 Cellule modulaire électrochimique pour le traitement de solutions d'électrolytes

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PCT/RU2013/000501 WO2014204332A1 (fr) 2013-06-17 2013-06-17 Cellule modulaire électrochimique pour le traitement de solutions d'électrolytes

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5635040A (en) * 1996-03-11 1997-06-03 Rscecat, Usa, Inc. Electrochemical cell
JP3141995B1 (ja) * 1999-12-03 2001-03-07 株式会社荏原電産 アルカリ過マンガン酸塩溶液電解再生装置
US20110226615A1 (en) * 2008-12-03 2011-09-22 Vitold Mikhailovich Bakhir Electrochemical modular cell for processing electrolyte solutions

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5635040A (en) * 1996-03-11 1997-06-03 Rscecat, Usa, Inc. Electrochemical cell
JP3141995B1 (ja) * 1999-12-03 2001-03-07 株式会社荏原電産 アルカリ過マンガン酸塩溶液電解再生装置
US20110226615A1 (en) * 2008-12-03 2011-09-22 Vitold Mikhailovich Bakhir Electrochemical modular cell for processing electrolyte solutions

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