EP1061158B1 - Fonctionnement en parallèle de cellules d'électrolyse à cathode de mercure et à membrane - Google Patents

Fonctionnement en parallèle de cellules d'électrolyse à cathode de mercure et à membrane Download PDF

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Publication number
EP1061158B1
EP1061158B1 EP00111000A EP00111000A EP1061158B1 EP 1061158 B1 EP1061158 B1 EP 1061158B1 EP 00111000 A EP00111000 A EP 00111000A EP 00111000 A EP00111000 A EP 00111000A EP 1061158 B1 EP1061158 B1 EP 1061158B1
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EP
European Patent Office
Prior art keywords
brine
electrolysis
amalgam
station
stream
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 - Lifetime
Application number
EP00111000A
Other languages
German (de)
English (en)
Other versions
EP1061158A3 (fr
EP1061158A2 (fr
Inventor
Fritz Dr. Gestermann
Hans-Dieter Pinter
Helmut Ziegler
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.)
Covestro Deutschland AG
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Bayer MaterialScience AG
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Publication date
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Publication of EP1061158A2 publication Critical patent/EP1061158A2/fr
Publication of EP1061158A3 publication Critical patent/EP1061158A3/fr
Application granted granted Critical
Publication of EP1061158B1 publication Critical patent/EP1061158B1/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
    • 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
    • C25B1/36—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in mercury cathode cells
    • C25B1/42—Decomposition of amalgams
    • 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
    • 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

Definitions

  • the invention relates to a method for the parallel operation of amalgam electrolyzers and membrane electrolysers with a common brine circuit below Use of an oxygen consumption cathode resistant to mercury in the Membrane electrolyzer.
  • the oxygen consumable cathode for use in NaCl electrolysis is from the literature basically known. For their operation e.g. in a pressure-compensated arrangement, as described in DE 19622744 Cl, brine is of the usual membrane cell quality used. This brine is mercury-free to protect the cathode activation held.
  • the mercury contamination for chloralkali electrolysis using the amalgam process known NaCl brine is typically from about 10 mg / l to 400 mg / l in normal operation or as a peak value after the system has come to a standstill.
  • Another aspect is the gradual changeover from amalgam electrolysis on membrane processes play an important role: if the energetically less favorable, Mercury-resistant cathode activation during the parallel operation of amalgam and membrane processes should be used, with the aim of being more complete Conversion to the optimal cathode activation, which is sensitive to mercury the entire brine and alkali cycle must be completely changed mercury-free, which causes enormous problems, especially in the Alkaline cycle that mercury can be partially in metallic form.
  • the task is therefore to provide an electrolysis process in which an amalgam electrolysis and a Membrane electrolysis, preferably using an oxygen consumable cathode, can be operated in parallel with the same brine circuit.
  • the procedure is said to Have advantages of known methods with oxygen consumption cathodes.
  • the object is achieved through the use of oxygen consumption cathodes solved in a membrane electrolysis process that against the effects of Mercury are resistant.
  • the task is also accomplished through the use of a Ca / Mg ion exchanger dissolved, the Ca / Mg content even with mercury Brine lowers to ⁇ 20 ppb, which is necessary to ensure the full life of the membranes to ensure.
  • the catalyst matrix is sintered or pressed with the support.
  • the carbon components (soot) can also be dispensed with if the catalyst density and / or the rendered hydrophobic support are set such that the majority of the catalyst particles are also contacted electrically.
  • the carbon soot can be omitted from the oxygen depletion cathode so that the electrode matrix consists only of Teflon and silver, whereby the silver takes on the function of the catalyst as well as that of electron conduction and accordingly such a high Ag loading is necessary that the particles separate touch and form conductive bridges with each other.
  • the wire mesh, a fine expanded metal as known from battery technology, as also a felt made of silver, silver-plated nickel or silver-plated alkali-resistant material, e.g. Inconnel steel. It is essential that the silver catalyst is stable behaves towards mercury.
  • sulfate content at ⁇ 5 g / l is achieved by appropriate operation, for example continuous or discontinuous discharge of the sulfate by means of precipitation or partial flow precipitation, for example with addition of CaCO 3 , BaCl 2 or BaCO 3 , or in particular in the case of very low-sulfate salts, can be adjusted by discharging a partial stream of the depleted brine.
  • Another possibility is the nanofiltration of the brine or a partial flow of the brine by means of ion-selective membranes in the feed upstream of the membrane electrolyser, or another separation process, for example by means of ion exchangers. It is important that only the partial flow to the membrane electrolyzer has to be set to the sulfate ion concentration mentioned, with the side effect that the main flow also gradually adjusts to a lower content in the circuit.
  • the SiO 2 content in the NaCl brine can easily be kept at ⁇ 5 ppm by avoiding free concrete areas in the salt store (brine bunker).
  • Peak mercury levels with a concentration of up to 400 mg Hg / l in the brine are from the oxygen consumption cathode operated behind the membrane in the sodium hydroxide solution survived easily.
  • the usual concentration of 150-200 mg / l mercury at normal peaks and ⁇ 10 mg / l mercury in normal operation is for the operation of the oxygen consumption cathode no barrier.

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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)
  • Automation & Control Theory (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Secondary Cells (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)

Claims (7)

  1. Procédé pour l'électrolyse de saumures (lessives de chlorure de sodium) avec fonctionnement parallèle d'électrolyseurs à amalgame (5) et d'électrolyseurs à membrane (4) avec cathode à consommation d'oxygène et circuit commun de saumure, comportant les stades opératoires suivants :
    envoi de la saumure (9) provenant d'une station de dissolution du chlorure de sodium (1) vers une station de précipitation et de filtration (2) et séparation grossière des ions sulfate, calcium et magnésium contenus dans la saumure (9) à la station de précipitation et de filtration (2),
    partage de la saumure entre un courant principal (10) et un courant partiel (11), électrolyse du courant principal (10) de saumure dans un électrolyseur à amalgame (5),
    traitement préalable du courant partiel (11) de la saumure par élimination du chlore libre dans une station de déchlorage (7), précipitation plus spécialement des ions Al, Fe et Mg dans une station de précipitation des hydroxydes (6) et séparation des ions calcium et magnésium contenus dans la saumure (11) jusqu'à une teneur résiduelle inférieure à 20 ppb dans la station (3), plus particulièrement un échangeur d'ions,
    puis électrolyse du courant partiel (11) de la saumure dans un électrolyseur à membrane (4), avec utilisation d'un électrolyseur à membrane (4) à cathode à consommation d'oxygène résistant au mercure, contenant au moins un catalyseur à base d'argent, et
    réunion des courants d'anolyte de l'électrolyseur à membrane (4) et de l'électrolyseur à amalgame (5) en un courant d'anolyte commun (14).
  2. Procédé selon la revendication 1, caractérisé en ce que l'on utilise une cathode à consommation d'oxygène consistant en au moins un support métallique conducteur de l'électricité et résistant aux lessives alcalines, de préférence une toile, un métal étiré ou un feutre de fils d'argent ou de fils de nickel ou d'Inconel argenté et une gangue de catalyseur frittée ou comprimée avec le support et consistant elle-même en Téflon, une matière de gangue conductrice de l'électricité, de préférence du noir de carbone, et une matière catalytique consistant en particules d'argent possédant l'activité catalytique ou d'autres particules de catalyseur résistant au mercure.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on règle la teneur en ions sulfate à moins de 5 g/l dans la station de précipitation et de filtration (2), plus spécialement par précipitation à l'aide de CaCO3, de BaCl2 ou de BaCO3 ou par nanofiltration.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que, avant l'électrolyse du courant partiel (11) de saumure dans l'électrolyseur à membrane (4), on sépare les ions calcium et magnésium de la saumure (11) dans un échangeur d'ions Ca/Mg (3).
  5. Procédé selon la revendication 4, caractérisé en ce que l'échangeur d'ions Ca/Mg (3) est un échangeur d'ions résistant au mercure.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que le courant commun d'anolyte (14) provenant de l'électrolyseur à amalgame (5) et de l'électrolyseur à membrane (4) est recyclé à la station de dissolution du chlorure de sodium (1).
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que la teneur en SiO2 de la saumure est maintenue à moins de 5 ppm avant l'électrolyse.
EP00111000A 1999-06-12 2000-05-30 Fonctionnement en parallèle de cellules d'électrolyse à cathode de mercure et à membrane Expired - Lifetime EP1061158B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19926887A DE19926887A1 (de) 1999-06-12 1999-06-12 Elektrolyseverfahren
DE19926887 1999-06-12

Publications (3)

Publication Number Publication Date
EP1061158A2 EP1061158A2 (fr) 2000-12-20
EP1061158A3 EP1061158A3 (fr) 2000-12-27
EP1061158B1 true EP1061158B1 (fr) 2004-04-14

Family

ID=7911060

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00111000A Expired - Lifetime EP1061158B1 (fr) 1999-06-12 2000-05-30 Fonctionnement en parallèle de cellules d'électrolyse à cathode de mercure et à membrane

Country Status (14)

Country Link
US (1) US6224740B1 (fr)
EP (1) EP1061158B1 (fr)
JP (1) JP2001029956A (fr)
KR (1) KR20010049521A (fr)
CN (1) CN1277269A (fr)
AT (1) ATE264412T1 (fr)
BR (1) BR0002624A (fr)
CA (1) CA2311042A1 (fr)
DE (2) DE19926887A1 (fr)
ES (1) ES2219223T3 (fr)
NO (1) NO20002992L (fr)
SG (1) SG87894A1 (fr)
TW (1) TW539774B (fr)
ZA (1) ZA200002914B (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106216360A (zh) * 2016-08-16 2016-12-14 南京格洛特环境工程股份有限公司 一种副产品盐的精制及资源化利用方法

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10149779A1 (de) * 2001-10-09 2003-04-10 Bayer Ag Verfahren zur Rückführung von Prozessgas in elektrochemischen Prozessen
CN1901982B (zh) * 2003-10-31 2010-04-21 金属合金回收公司 从废弃物流减少无机污染物的方法
US8322909B2 (en) * 2004-09-22 2012-12-04 3M Deutschland Gmbh Mixer for multi-component pastes, kit, and method of mixing paste components
EP1640060A1 (fr) 2004-09-22 2006-03-29 3M Espe Ag Mélangeur pour pâtes multi-composants, kit, et méthode pour mélanger des pâtes
JP2008223115A (ja) * 2007-03-15 2008-09-25 Asahi Kasei Chemicals Corp 塩水の処理方法
WO2011005742A1 (fr) * 2009-07-06 2011-01-13 Mar Systems, Llc Milieux pour l'élimination de contaminants à partir de courants de fluides et procédé de fabrication et d'utilisation de ceux-ci

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3037818C2 (de) * 1980-10-07 1985-08-14 Hoechst Ag, 6230 Frankfurt Verfahren zur Herstellung von Natriumbisulfat
DE3543379A1 (de) * 1985-12-07 1987-06-11 Metallgesellschaft Ag Verfahren zur elektrolytischen herstellung von alkalimetallhydroxid, chlor und wasserstoff
US5028302A (en) * 1989-11-16 1991-07-02 Texas Brine Corporation Purification of chlor-alkali membrane cell brine
JPH08283978A (ja) * 1995-04-10 1996-10-29 Permelec Electrode Ltd ガス拡散電極の製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106216360A (zh) * 2016-08-16 2016-12-14 南京格洛特环境工程股份有限公司 一种副产品盐的精制及资源化利用方法

Also Published As

Publication number Publication date
NO20002992L (no) 2000-12-13
EP1061158A3 (fr) 2000-12-27
CA2311042A1 (fr) 2000-12-12
BR0002624A (pt) 2001-01-02
EP1061158A2 (fr) 2000-12-20
DE19926887A1 (de) 2000-12-14
ES2219223T3 (es) 2004-12-01
TW539774B (en) 2003-07-01
US6224740B1 (en) 2001-05-01
ZA200002914B (en) 2000-12-12
ATE264412T1 (de) 2004-04-15
SG87894A1 (en) 2002-04-16
CN1277269A (zh) 2000-12-20
DE50006039D1 (de) 2004-05-19
JP2001029956A (ja) 2001-02-06
KR20010049521A (ko) 2001-06-15
NO20002992D0 (no) 2000-06-09

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