EP0178958B1 - Procédé d'oxydation électrolytique et ensemble d'électrolyse pour sa mise en oeuvre - Google Patents

Procédé d'oxydation électrolytique et ensemble d'électrolyse pour sa mise en oeuvre Download PDF

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Publication number
EP0178958B1
EP0178958B1 EP85401698A EP85401698A EP0178958B1 EP 0178958 B1 EP0178958 B1 EP 0178958B1 EP 85401698 A EP85401698 A EP 85401698A EP 85401698 A EP85401698 A EP 85401698A EP 0178958 B1 EP0178958 B1 EP 0178958B1
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EP
European Patent Office
Prior art keywords
solution
compartment
anode
anode compartment
abovementioned
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
EP85401698A
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German (de)
English (en)
French (fr)
Other versions
EP0178958A1 (fr
Inventor
Jean Bachot
Jean-Yves Dumousseau
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.)
Rhodia Chimie SAS
Original Assignee
Rhone Poulenc Chimie SA
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 Rhone Poulenc Chimie SA filed Critical Rhone Poulenc Chimie SA
Priority to AT85401698T priority Critical patent/ATE36010T1/de
Publication of EP0178958A1 publication Critical patent/EP0178958A1/fr
Application granted granted Critical
Publication of EP0178958B1 publication Critical patent/EP0178958B1/fr
Expired legal-status Critical Current

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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
    • 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
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • 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
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • 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
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/01—Products
    • C25B3/07—Oxygen containing compounds
    • 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
    • C25B9/70—Assemblies comprising two or more cells

Definitions

  • the present invention relates to an electrolytic oxidation process of a saline solution and an electrolysis assembly for the implementation of this process.
  • the invention applies more particularly to solutions of cerium salts.
  • the object of the invention is a method and a device ensuring better productivity with, for the device, great simplicity of structure.
  • the process of the invention for the electrolytic oxidation of a chemical species in a solution is characterized in that said solution is treated in a first anode compartment of an electrolysis cell comprising a first anode compartment and a cathode compartment separated by a first cationic membrane, the solution from the first anode compartment is then treated in a second anode compartment of the aforementioned electrolysis cell and separated from the above cathode compartment by a second cationic membrane, the solution obtained is recovered the second anode compartment which constitutes the production; an electrolyte is circulated in the aforementioned cathode compartment.
  • the method for the electrolytic oxidation of a chemical species in a solution is characterized in that in a first circulation loop, said solution is treated in the first anode compartment of a cell d electrolysis comprising a first anode compartment and a cathode compartment separated by a first cationic membrane and a first part of the treated solution is recycled in said anode compartment; in a second circulation loop, the other second part of the solution is treated in a second anode compartment of the above-mentioned electrolysis cell and separated from the above-mentioned cathode compartment by a second cationic membrane, part of the solution thus treated is recycled in the second anode compartment and the other part of the solution which constitutes the production is separated.
  • FIG. 1 An electrolysis cell 1 consisting of three compartments.
  • the compartments 2 and 3 are anode compartments, between which is located a cathode compartment 4. These compartments are separated from each other by two cationic membranes 5 and 6.
  • any suitable type of electrode can be used, for example electrodes of expanded shape and / or laminated with a titanium substrate coated with platinum, iridium or precious metal alloys for the anodes, the cathode can be platinum titanium or titanium substrate coated with palladium.
  • the anode compartments can also be provided with turbulence promoters located between the membrane and the anode.
  • turbulence promoters located between the membrane and the anode.
  • On each of the compartments 2, 3 and 4 of the cell are mounted loops or circuits for electrolyte circulation 7, 8 and 9 respectively, each equipped with pumps 10, 11 and 12 respectively.
  • the anolyte is supplied to the circuit 7 by an assembly 13 constituted in the example illustrated by a tank 14 receiving the solution to be treated, a pipe 15 connected to the circuit 7 and by a supply pump 16.
  • the circuits 7, 8 and 9 are all three equipped with tanks 17, 18 and 19 respectively with discharge by overflow, these tanks serve in particular as demister.
  • a bypass line 20 connects the circuits 7 and 8 via the tanks 17 and 18.
  • the circuit 9 is connected via a bypass line 21 to the supply assembly 13 of the circuit 7.
  • the line 21 opens into the tank 14.
  • the electrolysis assembly is supplied from the outside with solution to be treated by a line 22, and as a catholyte by the line 23 connected to the circuit 9.
  • a line 24 makes it possible to readjust the titer of the solution to be treated. In the case, for example, of a nitric solution of cerium, the necessary quantity of nitric acid can be added by 24.
  • line 25 allows the treated solution to be discharged to the outside.
  • circuit 8 the solution undergoes a second electrolytic treatment by passage through compartment 3.
  • This solution enriched again with Ce4 + is, as in circuit 7, partly recycled and partly evacuated.
  • the flow transported by line 25 constitutes production.
  • the catholyte consisting of a nitric acid solution circulates in circuit 9.
  • the nitric acid titer is readjusted via line 23.
  • Part of the catholyte is evacuated by the overflow of tank 19 and is brought back via line 21 to the tank 14. This characteristic of the system thus makes it possible to bring back into the solution to be treated the cerium ions passed through the cathode compartment.
  • FIG. 2 represents a second embodiment of the electrolysis assembly of the invention which differs from that illustrated in FIG. 1 essentially as regards the circulation loop of the catholyte. This is why the same references have been used for the parts of the assembly of FIG. 2 identical to those of FIG. 1 which will not be described again here.
  • the circulation loop of the catholyte comprises a storage tank 30 connected to the cathode compartment by a pipe 31 provided with a pump 32.
  • the circulation loop is completed by the pipe 33 connecting the tank 19 to the tank 30.
  • a bypass 34 connects the circulation loop of the catholyte to the tank 14.
  • conduits 35 and 36 supply the tank 30 with water and catholyte, for example nitric acid, respectively.
  • the method and the device of the invention can be used for the electrolytic oxidation of any chemical species. They can be applied for example to Thallium (oxidation of Thallium I to Thallium III) or to Cerium (Cerium III oxidized to Cerium IV).
  • a particularly advantageous application is that of the preparation of red solutions of IV cerium.
  • the electrolysis process of the invention makes it possible to pass directly from the cerous nitrate solution to the red solution while achieving savings in reagents, in particular nitric acid, a large excess of which must be used to redissolve the ceric hydrate.
  • the method of the invention also makes it possible to gain in productivity and security.
  • a feed solution 22 which is a cerous nitrate solution.
  • This solution may contain nitric acid.
  • cerammoniacal nitrate (Ce (N0 3 ) 4 , 2 NH 4 N0 3 ).
  • the process of the invention makes it possible to directly prepare this product from a solution of cerium III nitrate and ammonium nitrate.
  • the method and the device of the invention are implemented using as solution to be treated, entering the first circulation loop, a solution of cerous nitrate and ammonium nitrate.
  • This solution may also contain nitric acid.
  • Ammonium nitrate solution is used as the catholyte.
  • a ceriammoniacal nitrate solution After passing the solution through the anode compartment of the second cycle, a ceriammoniacal nitrate solution.
  • Another application of the process and the device of the invention is the preparation of ceric sulphate.
  • ceric sulphate solutions can be prepared by sulfuric attack of the ceric hydrate precipitated after oxidation with hydrogen peroxide. In general, the solutions obtained are not very concentrated.
  • a solution of cerous sulphate, or possibly ceric sulphate permanently resaturated with Celll is circulated in the circulation loops if it is desired to obtain a high concentration, and containing a small quantity of sulfuric acid.
  • This example illustrates the application of the invention to the oxidation of cerous nitrate for the preparation of ceric nitrate.
  • This example illustrates the same application as the previous example but under different operating conditions.
  • the productivity per active surface area of electrodes is very high (34 kg / h / m 2 ) with very low residual contents of cerous ions, which makes it possible to obtain very low oxidation costs.
  • the cell is supplied as in the previous example.
  • the first compartment works at a current density of 28 A / dm 2 .
  • the conversion rate is 80% and the “Faraday” yield is 96%.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Secondary Cells (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
EP85401698A 1984-09-13 1985-08-30 Procédé d'oxydation électrolytique et ensemble d'électrolyse pour sa mise en oeuvre Expired EP0178958B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT85401698T ATE36010T1 (de) 1984-09-13 1985-08-30 Verfahren und vorrichtung fuer elektrolytische oxydation.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8413641A FR2570087B1 (fr) 1984-09-13 1984-09-13 Procede d'oxydation electrolytique et ensemble d'electrolyse pour sa mise en oeuvre
FR8413641 1984-09-13

Publications (2)

Publication Number Publication Date
EP0178958A1 EP0178958A1 (fr) 1986-04-23
EP0178958B1 true EP0178958B1 (fr) 1988-07-27

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP85401698A Expired EP0178958B1 (fr) 1984-09-13 1985-08-30 Procédé d'oxydation électrolytique et ensemble d'électrolyse pour sa mise en oeuvre

Country Status (11)

Country Link
US (2) US4657644A (enrdf_load_stackoverflow)
EP (1) EP0178958B1 (enrdf_load_stackoverflow)
JP (1) JPS6187886A (enrdf_load_stackoverflow)
KR (1) KR900002492B1 (enrdf_load_stackoverflow)
AT (1) ATE36010T1 (enrdf_load_stackoverflow)
AU (1) AU576263B2 (enrdf_load_stackoverflow)
CA (1) CA1254170A (enrdf_load_stackoverflow)
DE (1) DE3563986D1 (enrdf_load_stackoverflow)
FR (1) FR2570087B1 (enrdf_load_stackoverflow)
NO (1) NO853542L (enrdf_load_stackoverflow)
ZA (1) ZA856991B (enrdf_load_stackoverflow)

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Also Published As

Publication number Publication date
US4749462A (en) 1988-06-07
CA1254170A (fr) 1989-05-16
DE3563986D1 (en) 1988-09-01
AU4737285A (en) 1986-03-20
ATE36010T1 (de) 1988-08-15
NO853542L (no) 1986-03-14
EP0178958A1 (fr) 1986-04-23
JPS6187886A (ja) 1986-05-06
AU576263B2 (en) 1988-08-18
JPS6342709B2 (enrdf_load_stackoverflow) 1988-08-25
US4657644A (en) 1987-04-14
ZA856991B (en) 1986-05-28
KR860002595A (ko) 1986-04-28
KR900002492B1 (ko) 1990-04-16
FR2570087B1 (fr) 1986-11-21
FR2570087A1 (fr) 1986-03-14

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