EP0126490A1 - Diaphragme à base d'oxyde de nickel et procédé pour sa fabrication - Google Patents
Diaphragme à base d'oxyde de nickel et procédé pour sa fabrication Download PDFInfo
- Publication number
- EP0126490A1 EP0126490A1 EP84105869A EP84105869A EP0126490A1 EP 0126490 A1 EP0126490 A1 EP 0126490A1 EP 84105869 A EP84105869 A EP 84105869A EP 84105869 A EP84105869 A EP 84105869A EP 0126490 A1 EP0126490 A1 EP 0126490A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- titanium
- nickel
- oxide
- diaphragm
- weight
- 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.)
- Granted
Links
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 238000000034 method Methods 0.000 title abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000010936 titanium Substances 0.000 claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 238000010292 electrical insulation Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000000843 powder Substances 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000010425 asbestos Substances 0.000 description 4
- 229910052895 riebeckite Inorganic materials 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- -1 Zr0 2 Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
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
- C25B13/00—Diaphragms; Spacing elements
- C25B13/04—Diaphragms; Spacing elements characterised by the material
Definitions
- the invention relates to a diaphragm based on nickel oxide for alkaline water electrolysis and to a method for producing the same.
- the alkaline water electrolysis generally takes place at relatively low temperatures (below 90 ° C.), which must be chosen in hot KOH because of the low chemical resistance of the asbestos diaphragms usually used. These low temperatures are both thermodynamically and kinetically disadvantageous an unnecessarily high electrolysis voltage is required, and the whole process appears uneconomical for energy reasons.
- Potassium silicate was added to the KOH electrolyte to reduce asbestos solubility in KOH (RLVic et al in Hydrogen Energy Progress IV, 4th WHE Conference, June 13-17, 1982, California, pp. 129-140). It is clear that this measure is not ultimately satisfactory can be viewed.
- Porous metallic diaphragms made of sintered nickel have also been proposed (P. Perroud, G. Terrier: "Hydrogen Energy System", Proc. 2nd WHE Conference, Zurich 1978, p. 241). These have a very low electrical resistance and are also mechanically stable and inexpensive.
- the major disadvantage, however, is that this diaphragm, like the electrodes, is also electron-conductive and there is too great a risk of short-circuiting in a compact design.
- porous nickel oxide diaphragms have been developed by the applicant (DE-OSes 29 27 566 and 30 31 064), which are produced by oxidation of sintered metal at elevated temperature (DE-OS 29 27 566) or more simply by oxidizing firing a carrier pressed nickel powder layer can be obtained (DE-OS 30 31 064).
- These NiO diaphragms have excellent properties as separators for alkaline water electrolysis.
- Such a reductive attack by hydrogen is not subject to ceramic diaphragms made of thermodynamically stable oxide compounds, such as Zr0 2 , BaTiO 3 , K 2 Ti 6 0 13 etc. (see above), but the manufacture of such diaphragms has the disadvantages mentioned above, in particular very high manufacturing temperatures, and they are attacked in 10 N KOH at elevated temperature with time.
- the "in situ" NiO diaphragm according to DE-OS 30 31 064 is alkali-resistant and its manufacture not only starts from a cheap starting material, but also offers the decisive technological advantage that the exothermic reaction 2 Ni + 0 2 ⁇ 2 Ni0 only expires when the diaphragm is manufactured. This results in a considerable temperature increase locally and the external manufacturing temperature can only be 1000 ° C., which is advantageous. Due to the manufacturing process (oxidizing sintering), there is also no need to maintain an inert atmosphere, which is also a significant relief.
- the invention is therefore based on the object, the reduction stability of the nickel oxide diaphragms to improve under the conditions of alkaline water electrolysis.
- the nickel oxide-based diaphragm according to the invention developed for this purpose is characterized by a content of 0.5 to 10% by weight of titanium (in oxidized form; based on the oxide mass).
- NiO 2 was added to the nickel powder in the preparation of the diaphragm in amounts of 1 to 20% by weight (based on the sum of metallic nickel and titanium dioxide) .
- the grain size of the admixed powder should be approximately comparable or smaller than that of the nickel powder in order to ensure a uniform distribution of the titanium over the oxide mass.
- titanium powder can also be admixed to the nickel powder mass in the manufacture of the diaphragm, or else as a compound, which transform into titanium oxide during the oxidizing sintering treatment. If necessary, a nickel oxide diaphragm which has already been produced can also be impregnated with a titanium compound which is converted into oxidized form by afterburning.
- the assembly was sintered in air at 1050 ° C for about 20 minutes.
- the chemical stability was, however, greatly improved, as can be seen from FIGS. 1 and 2:
- the decrease in oxygen in a pure hydrogen atmosphere at 140 to 170 ° C. can no longer be measured during the first 2000 h, which indicates an enormously increased reduction stability.
- a diaphragm made of pure NiO loses 7% of the oxygen in 2000 hours and even a diaphragm stabilized with A1 2 0 3 additive still loses about 1.5% of the oxygen content in the same time.
- the already excellent chemical stability in hot KOH is further increased: As FIG. 2 shows, the total weight loss after 2000 hours in 10 N KOH at 120 ° C. is only 0.3%.
- a pure NiO diaphragm loses 0.8%, a BaTi0 3 diaphragm 2% and a diaphragm mixed with 5% Al 2 O 3 8% of the total weight, which is attributable to A1 2 0 3 .
- Example 1 Before the slurrying step, 8% by weight of metallic Ti (based on the powder mixture) of approximately the same grain size as Ni was added to the Ni powder. The subsequent production steps were the same as in Example 1. After the oxidizing sintering, both nickel and titanium were present in oxidic form. This diaphragm had the same properties as that of Example 1 with respect to the reducibility in H 2 atmosphere.
- Example 1 50% TiO 2 was added to the Ni powder before slurrying. Otherwise, the preparation corresponded to that of Example 1.
- the diaphragm produced in this way showed a weight loss of 10% after only 500 hours in 10 N KOH at 120 ° C.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Electrolytic Production Of Metals (AREA)
- Saccharide Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Diaphragms For Electromechanical Transducers (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Magnetic Ceramics (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT84105869T ATE31432T1 (de) | 1983-05-24 | 1984-05-23 | Diaphragma auf nickeloxidbasis und verfahren zur herstellung desselben. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3318758 | 1983-05-24 | ||
DE3318758A DE3318758C2 (de) | 1983-05-24 | 1983-05-24 | Diaphragma auf Nickeloxidbasis und Verfahren zur Herstellung desselben |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0126490A1 true EP0126490A1 (fr) | 1984-11-28 |
EP0126490B1 EP0126490B1 (fr) | 1987-12-16 |
Family
ID=6199718
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP84105869A Expired EP0126490B1 (fr) | 1983-05-24 | 1984-05-23 | Diaphragme à base d'oxyde de nickel et procédé pour sa fabrication |
Country Status (9)
Country | Link |
---|---|
US (1) | US4559124A (fr) |
EP (1) | EP0126490B1 (fr) |
JP (1) | JPS59229489A (fr) |
AT (1) | ATE31432T1 (fr) |
BR (1) | BR8402480A (fr) |
CA (1) | CA1254857A (fr) |
DE (2) | DE3318758C2 (fr) |
NO (1) | NO161628C (fr) |
ZA (1) | ZA843921B (fr) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0339728A1 (fr) * | 1988-04-23 | 1989-11-02 | Metallgesellschaft Ag | Procédé et dispositif de fabrication de diaphragmes |
WO2021043578A1 (fr) | 2019-09-05 | 2021-03-11 | Thyssenkrupp Uhde Chlorine Engineers Gmbh | Électrolyse de l'eau à flux croisé |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3424203A1 (de) * | 1984-06-30 | 1986-01-16 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | Diaphragma fuer alkalische elektrolysen und verfahren zur herstellung desselben |
DE8517106U1 (de) * | 1985-06-12 | 1985-08-01 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | Diaphragma für alkalische Elektrolysen |
US7329332B2 (en) * | 2004-08-25 | 2008-02-12 | Ppg Industries Ohio, Inc. | Diaphragm for electrolytic cell |
US7618527B2 (en) * | 2005-08-31 | 2009-11-17 | Ppg Industries Ohio, Inc. | Method of operating a diaphragm electrolytic cell |
US8460536B2 (en) * | 2006-01-19 | 2013-06-11 | Eagle Controlled 2 Ohio Spinco, Inc. | Diaphragm for electrolytic cell |
CN102400139A (zh) * | 2010-09-15 | 2012-04-04 | 鸿富锦精密工业(深圳)有限公司 | 镀膜件及其制作方法 |
ITMI20131804A1 (it) * | 2013-10-30 | 2015-05-01 | Intecna S R L | Processo e apparato per la produzione in continuo di ferrati alcalini, in particolare di ferrato di sodio |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AT343146B (de) * | 1974-05-24 | 1978-05-10 | Ici Ltd | Elektrochemische diaphragmazelle und verfahren zu ihrer herstellung |
DE2927566A1 (de) * | 1979-07-07 | 1981-01-08 | Kernforschungsanlage Juelich | Diaphragma fuer alkalische wasserelektrolysen und verfahren zur herstellung desselben sowie dessen verwendung |
DE3031064A1 (de) * | 1980-08-16 | 1982-03-04 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | Poroeses oxiddiaphragma fuer alkalische elektrolysen, dessen herstellung und verwendung |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
IT1002909B (it) * | 1973-02-17 | 1976-05-20 | Deutsche Automobilgesellsch | Membrana per la separazione di idro geno da miscele di gas contenenti idrogeno |
IT1115372B (it) * | 1977-07-15 | 1986-02-03 | Oronzio De Nora Impianti | Membrane ceramiche a due fasi per celle elettrolitiche |
US4394224A (en) * | 1980-04-24 | 1983-07-19 | British Aerospace Public Limited Company | Treatment of titanium prior to bonding |
DE3108255C2 (de) * | 1981-03-05 | 1986-05-07 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | Baueinheit für Elektrolysezellen für die alkalische Wasserelektrolyse und Verfahren zur Herstellung derselben |
DE3109183C2 (de) * | 1981-03-11 | 1983-05-11 | BOMIN Bochumer Mineralöl GmbH & Co, 4630 Bochum | Aus Nickelpulver heißgepreßte hochporöse Elektrode für alkalische Wasserelektrolyseure |
-
1983
- 1983-05-24 DE DE3318758A patent/DE3318758C2/de not_active Expired
-
1984
- 1984-05-23 AT AT84105869T patent/ATE31432T1/de not_active IP Right Cessation
- 1984-05-23 EP EP84105869A patent/EP0126490B1/fr not_active Expired
- 1984-05-23 DE DE8484105869T patent/DE3468129D1/de not_active Expired
- 1984-05-23 BR BR8402480A patent/BR8402480A/pt not_active IP Right Cessation
- 1984-05-23 CA CA000454981A patent/CA1254857A/fr not_active Expired
- 1984-05-23 NO NO842048A patent/NO161628C/no unknown
- 1984-05-24 ZA ZA843921A patent/ZA843921B/xx unknown
- 1984-05-24 US US06/613,877 patent/US4559124A/en not_active Expired - Fee Related
- 1984-05-24 JP JP59103772A patent/JPS59229489A/ja active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AT343146B (de) * | 1974-05-24 | 1978-05-10 | Ici Ltd | Elektrochemische diaphragmazelle und verfahren zu ihrer herstellung |
DE2927566A1 (de) * | 1979-07-07 | 1981-01-08 | Kernforschungsanlage Juelich | Diaphragma fuer alkalische wasserelektrolysen und verfahren zur herstellung desselben sowie dessen verwendung |
DE3031064A1 (de) * | 1980-08-16 | 1982-03-04 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | Poroeses oxiddiaphragma fuer alkalische elektrolysen, dessen herstellung und verwendung |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0339728A1 (fr) * | 1988-04-23 | 1989-11-02 | Metallgesellschaft Ag | Procédé et dispositif de fabrication de diaphragmes |
DE3813743A1 (de) * | 1988-04-23 | 1989-11-02 | Metallgesellschaft Ag | Verfahren und vorrichtung zur herstellung von diaphragmen |
WO2021043578A1 (fr) | 2019-09-05 | 2021-03-11 | Thyssenkrupp Uhde Chlorine Engineers Gmbh | Électrolyse de l'eau à flux croisé |
Also Published As
Publication number | Publication date |
---|---|
US4559124A (en) | 1985-12-17 |
DE3318758A1 (de) | 1984-11-29 |
EP0126490B1 (fr) | 1987-12-16 |
ZA843921B (en) | 1986-01-29 |
ATE31432T1 (de) | 1988-01-15 |
NO842048L (no) | 1984-11-26 |
NO161628B (no) | 1989-05-29 |
DE3318758C2 (de) | 1985-06-13 |
NO161628C (no) | 1989-09-06 |
DE3468129D1 (en) | 1988-01-28 |
CA1254857A (fr) | 1989-05-30 |
BR8402480A (pt) | 1985-04-02 |
JPS59229489A (ja) | 1984-12-22 |
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