EP1061158B1 - Parallel Betrieb von Amalgamelektrolyseuren und Membranelektrolyseuren - Google Patents
Parallel Betrieb von Amalgamelektrolyseuren und Membranelektrolyseuren Download PDFInfo
- 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
- Authority
- 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
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Classifications
-
- 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)
- Organic Chemistry (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)
- Electrolytic Production Of Metals (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)
- Secondary Cells (AREA)
Description
Vorbehandeln des Teilstroms der Sole durch Entfernen von freiem Chlor in einer Entchlorungsstation, Ausfällen von insbesondere Al-, Fe- und Mg-Ionen in einer Hydroxidfällungsstatio und Abtrennen von Calzium- und Magnesiumionen aus der Sole bis zu einem Gehalt von < 20 ppb in der Station, insbesondere einem Ionenaustauscher,
anschließend Elektrolysieren des Teilstroms der Sole in einem Membranelektrolyseur, wobei ein Membranelektrolyseur mit einer quecksilberresistenten Sauerstoffverzehrkathode, wenigstens enthaltend einen Silber-Katalysator, verwendet wird, und
Der metallische Träger zur Verteilung der Elektronen besteht aus Gewebe aus Silberdraht oder versilbertem Nickeldraht oder einer anderen laugefesten Legierung, z.B. Inconel, die zur Vermeidung von schlecht leitenden Oxid- oder Hydroxidschichten ebenfalls versilbert oder anders veredelt sein sollten. Besonders vorteilhaft ist die Verwendung eines tiefstrukturierten Trägers wie z.B. Filz aus feinen Fasern des oben genannten Gewebematerials. Die Katalysatormatrix besteht aus dem bekannten Gemisch aus Teflon zur Einstellung der Hydrophobie und der Porosität für die Gasdiffusion, einem elektrisch leitfähigen Träger, z.B. Vulkanruß oder Acetylenruß, und dem darin fein verteilten Katalysatormaterial selbst, das in Form von katalytisch aktiven Silberpartikeln untergemischt ist. Die Katalysatormatrix ist mit dem Träger versintert oder verpresst. Alternativ kann auch auf die Kohlenstoffanteile (Ruß) verzichtet werden, wenn die Katalysatordichte und/oder der leitfähig gemachte hydrophobe Träger so eingestellt sind, dass die überwiegende Menge der Katalysatorpartikel auch elektrisch kontaktiert werden.
Der Silber-Katalysator in der vorliegenden Matrix aus Ruß und Teflon der vorzugsweise verwendeten Sauerstoffverzehrkathode ist offenkundig völlig unempfindlich gegenüber Quecksilber.
Fe | ∼ 0,12 mg/l |
Al | ∼ 0,25 mg/l |
Ca | ∼ 4,5 mg/l |
Mg | ∼ 0,15 mg/l |
SO4 2- | ∼ 7-10 g/l |
Es wurde eine für das Gesamtverfahren geeignete Elektrode unter Laborbedingungen getestet.
Claims (7)
- Verfahren zur Elektrolyse Natriumchlorid-haltiger Sole mit einem parallelen Betrieb von Amalgamelektrolyseuren (5) und Membranelektrolyseuren (4) mit Sauerstoffverzehrkathode mit einem gemeinsamen Solekreislauf, mit den Schritten:Zuführen der Sole (9) von einer Salzlösestation (1) zu einer Fäll- und Filterstation (2) und grobes Abtrennen von Sulfat-, Calzium- und Magnesiumionen aus der Sole (9) in der Fäll- und Filterstation (2),Aufteilen der Sole in einen Hauptstrom (10) und einen Teilstrom (11), Elektrolysieren des Hauptstroms (10) der Sole in einem Amalgamelektrolyseur (5),Vorbehandeln des Teilstroms (11) der Sole durch Entfernen von freiem Chlor in einer Entchlorungsstation (7), Ausfällen von insbesondere Al-, Fe- und Mg-Ionen in einer Hydroxidfällungsstation (6) und Abtrennen von Calziumund Magnesiumionen aus der Sole (11) bis zu einem Gehalt von < 20 ppb in der Station (3), insbesondere einem Ionenaustauscher,anschließend Elektrolysieren des Teilstroms (11) der Sole in einem Membranelektrolyseur (4), wobei ein Membranelektrolyseur (4) mit einer quecksilberresistenten Sauerstoffverzehrkathode, wenigstens enthaltend einen Silber-Katalysator, verwendet wird, undZusammenführen der Anolytströme des Membranelektrolyseurs (4) und des Amalgamelektrolyseur (5) in einen gemeinsamen Anolytstrom (14).
- Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass eine Sauerstoffverzehrkathode, bestehend wenigstens aus einem elektrisch leitenden metallischen, laugefesten Träger, bevorzugt einem Gewebe, Streckmetall oder Filz aus Silberdraht oder versilbertem Nickel- oder Inconel-Draht und einer mit dem Träger versinterten oder verpressten Katalysatormatrix aus Teflon, elektrisch leitfähigem Matrixmaterial, bevorzugt Ruß, und Katalysatormaterial aus katalytisch aktiven Silberpartikeln oder anderen quecksilberverträglichen Katalysatorpartikeln, verwendet wird.
- Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass der Gehalt an Sulfationen in der Fäll- und Filterstation (2), insbesondere durch Fällung mit CaCO3, BaCl2 oder BaCO3 oder durch Nanofiltration auf <5 g/l eingestellt wird.
- Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass vor dem Elektrolysieren des Teilstroms (11) der Sole im Membranelektrolyseur (4) Calzium- und Magnesiumionen aus der Sole (11) in einem Ca/Mg-Ionenaustauscher (3) abgetrennt werden.
- Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass der Ca/Mg-Ionenaustauscher (3) ein quecksilberresistenter Ionenaustauscher ist.
- Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass der gemeinsame Anolytstrom (14) von Amalgamelektrolyseur (5) und Membranelektrolyseur (4) in die Salzlösestation (1) zurückgeführt wird.
- Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass der SiO2-Gehalt der Sole vor der Elektrolyse auf <5 ppm gehalten wird.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19926887 | 1999-06-12 | ||
DE19926887A DE19926887A1 (de) | 1999-06-12 | 1999-06-12 | Elektrolyseverfahren |
Publications (3)
Publication Number | Publication Date |
---|---|
EP1061158A2 EP1061158A2 (de) | 2000-12-20 |
EP1061158A3 EP1061158A3 (de) | 2000-12-27 |
EP1061158B1 true EP1061158B1 (de) | 2004-04-14 |
Family
ID=7911060
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00111000A Expired - Lifetime EP1061158B1 (de) | 1999-06-12 | 2000-05-30 | Parallel Betrieb von Amalgamelektrolyseuren und Membranelektrolyseuren |
Country Status (14)
Country | Link |
---|---|
US (1) | US6224740B1 (de) |
EP (1) | EP1061158B1 (de) |
JP (1) | JP2001029956A (de) |
KR (1) | KR20010049521A (de) |
CN (1) | CN1277269A (de) |
AT (1) | ATE264412T1 (de) |
BR (1) | BR0002624A (de) |
CA (1) | CA2311042A1 (de) |
DE (2) | DE19926887A1 (de) |
ES (1) | ES2219223T3 (de) |
NO (1) | NO20002992L (de) |
SG (1) | SG87894A1 (de) |
TW (1) | TW539774B (de) |
ZA (1) | ZA200002914B (de) |
Cited By (1)
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)
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 |
US7341667B2 (en) * | 2003-10-31 | 2008-03-11 | Mar Systems, Llc | Process for reduction of inorganic contaminants from waste streams |
US8322909B2 (en) * | 2004-09-22 | 2012-12-04 | 3M Deutschland Gmbh | Mixer for multi-component pastes, kit, and method of mixing paste components |
EP1640060A1 (de) | 2004-09-22 | 2006-03-29 | 3M Espe Ag | Mischer für Mehrkomponentenpasten, Bausatz, und Verfahren zum Mischen von Pasten |
JP2008223115A (ja) * | 2007-03-15 | 2008-09-25 | Asahi Kasei Chemicals Corp | 塩水の処理方法 |
WO2011005742A1 (en) | 2009-07-06 | 2011-01-13 | Mar Systems, Llc | Media for removal of contaminants from fluid streams and method of making and using same |
Family Cites Families (4)
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 |
-
1999
- 1999-06-12 DE DE19926887A patent/DE19926887A1/de not_active Withdrawn
-
2000
- 2000-05-24 SG SG200003281A patent/SG87894A1/en unknown
- 2000-05-30 AT AT00111000T patent/ATE264412T1/de not_active IP Right Cessation
- 2000-05-30 DE DE50006039T patent/DE50006039D1/de not_active Expired - Fee Related
- 2000-05-30 ES ES00111000T patent/ES2219223T3/es not_active Expired - Lifetime
- 2000-05-30 EP EP00111000A patent/EP1061158B1/de not_active Expired - Lifetime
- 2000-06-05 TW TW089110922A patent/TW539774B/zh not_active IP Right Cessation
- 2000-06-05 US US09/587,309 patent/US6224740B1/en not_active Expired - Fee Related
- 2000-06-09 JP JP2000174114A patent/JP2001029956A/ja active Pending
- 2000-06-09 ZA ZA200002914A patent/ZA200002914B/xx unknown
- 2000-06-09 CA CA002311042A patent/CA2311042A1/en not_active Abandoned
- 2000-06-09 NO NO20002992A patent/NO20002992L/no not_active Application Discontinuation
- 2000-06-10 KR KR1020000031930A patent/KR20010049521A/ko not_active Application Discontinuation
- 2000-06-12 BR BR0002624-7A patent/BR0002624A/pt not_active IP Right Cessation
- 2000-06-12 CN CN00118182A patent/CN1277269A/zh active Pending
Cited By (1)
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 |
---|---|
ES2219223T3 (es) | 2004-12-01 |
JP2001029956A (ja) | 2001-02-06 |
DE50006039D1 (de) | 2004-05-19 |
CA2311042A1 (en) | 2000-12-12 |
ZA200002914B (en) | 2000-12-12 |
NO20002992D0 (no) | 2000-06-09 |
EP1061158A2 (de) | 2000-12-20 |
NO20002992L (no) | 2000-12-13 |
US6224740B1 (en) | 2001-05-01 |
SG87894A1 (en) | 2002-04-16 |
EP1061158A3 (de) | 2000-12-27 |
DE19926887A1 (de) | 2000-12-14 |
ATE264412T1 (de) | 2004-04-15 |
CN1277269A (zh) | 2000-12-20 |
KR20010049521A (ko) | 2001-06-15 |
BR0002624A (pt) | 2001-01-02 |
TW539774B (en) | 2003-07-01 |
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