EP2937449A1 - Gasdiffusionselektrode und herstellungsverfahren dafür - Google Patents
Gasdiffusionselektrode und herstellungsverfahren dafür Download PDFInfo
- Publication number
- EP2937449A1 EP2937449A1 EP12891307.6A EP12891307A EP2937449A1 EP 2937449 A1 EP2937449 A1 EP 2937449A1 EP 12891307 A EP12891307 A EP 12891307A EP 2937449 A1 EP2937449 A1 EP 2937449A1
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- EP
- European Patent Office
- Prior art keywords
- gas diffusion
- carbon black
- layer
- diffusion electrode
- gas
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
- C25B11/032—Gas diffusion electrodes
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/042—Electrodes formed of a single material
- C25B11/043—Carbon, e.g. diamond or graphene
- C25B11/044—Impregnation of carbon
Definitions
- the present invention relates to the field of chemical engineering, particularly to a gas diffusion electrode suitable for the chlor-alkali industry and a preparation method thereof.
- chlor-alkali industry plays an important role in promoting national economic development. Meanwhile, chlor-alkali industry is an industry with high energy consumption, so how to reduce the energy consumption of chlor-alkali industry to a minimum has always been an issue focused by many countries.
- reaction equations of the traditional ion-exchange membrane brine electrolytic process with a hydrogen evolution electrode as the cathode are as follows: 2Cl - ⁇ Cl 2 +2e (1.36V) 2H 2 O+2e ⁇ 2OH - +H 2 (-0.83V) 2NaCl+2H 2 O ⁇ Cl 2 +2NaOH+H 2 (2.19V),
- electrochemical reaction equations of the ion-exchange membrane brine electrolytic process with an oxygen diffusion electrode as the cathode are as follows: 2Cl - ⁇ Cl 2 +2e (1.36V) O 2 +2H 2 O+4e ⁇ 4OH - (0.4V) 2NaCl+H 2 O+1/2O 2 ⁇ Cl 2 +2NaOH (0.96V).
- theoretic decomposition voltage thereof can be reduced by 1.23 V, the theoretic energy thereof can be saved up to 40%, and the electric energy saved will be 700KWh per ton of alkali, which make the process have very considerable application value.
- Japanese Patent Publication 2007-327092 discloses a gas diffusion electrode having high resistance of water-pressure but low speed of deterioration, which is prepared using AB-6 carbon black as hydrophobic carbon black, AB-12 carbon black as hydrophilic carbon black, and Ag powder as a catalyst.
- Japanese Patent Publication 2004-300451 discloses a gas diffusion electrode having stable performance, which is prepared with AB-6 carbon black as hydrophobic carbon black and Ag-plated metal web as a catalyst layer through the steps of dispersing the hydrophobic carbon black and an adhesive, filtering and drying, followed by hot-press molding the Ag-plated metal web, however such electrode is difficult to satisfy the requirement of large-scale industrial production of large electrode.
- Cide CN101736360A discloses a gas diffusion electrode having a structure that a Ni web plated with Ag as a support is disposed between a gas diffusion layer and a catalyst layer, however such electrode involves problems such as low mechanical strength, being liable to form cracks on the surface of the electrode during the production thereof and difficult to release during the hot pressing process, and thus cannot satisfy the requirement of industrial production.
- the present invention relates to a gas diffusion electrode comprising a current collector, a gas diffusion layer, a gas catalysis layer coated on the gas diffusion layer, and a liquid guide layer located on the gas catalysis layer; wherein the gas diffusion layer comprises highly-graphitized carbon black and polytetrafluoroethylene (PTFE), and the gas catalysis layer comprises a catalyst, acidified highly-graphitized carbon black and polytetrafluoroethylene; the highly-graphitized carbon black is the carbon black having a peak intensity ratio I D /I G between 0.3 and 1.0 in the Raman spectrum, and the degrees of graphitization in the gas diffusion layer and the gas catalysis layer may be the same or different; the current collector and the liquid guide layer are both silver-plated metal foam having a thickness of
- the mass ratio of the highly-graphitized carbon black to polytetrafluoroethylene in the gas diffusion layer is (0.01-1): (0.01-0.1).
- the mass ratio of the catalyst, the acidified highly-graphitized carbon black and polytetrafluoroethylene in the gas catalysis layer is (0.1-1): (0.1-1): (0.1-1).
- the metal of the silver-plated metal foam is selected from nickel, titanium, tungsten, cobalt, or alloys thereof.
- the catalyst in the gas catalysis layer is selected from silver powder or Ag/C composite catalyst; preferably, the catalyst has a particle size between 0.01 and 5 ⁇ m.
- the diffusion electrode is applied as a gas diffusion electrode in chlor-alkali industry.
- the gas diffusion layer is prepared from raw materials comprising highly-graphitized carbon black, water, Triton, polytetrafluoroethylene emulsion and isopropanol in a mass ratio of (0.01-1): (0.1-1): (0.01-0.1): (0.01-0.1): 1, wherein the aqueous isopropanol solution of Triton is used as a dispersion medium.
- the gas catalysis layer is prepared from raw materials comprising a catalyst, acidified highly-graphitized carbon black, water, Triton, polytetrafluoroethylene solution and isopropanol in a mass ratio of (0.1-1): (0.1-1): (1-10): (0.1-1): (0.1-1) : 1, wherein the aqueous solution of Triton is used as a dispersion medium.
- the preparation method of the gas diffusion layer comprises the following steps: (1) dispersing the highly-graphitized carbon black in the aqueous isopropanol solution comprising surfactant Triton, so as to obtain the slurry of the gas diffusion layer; dispersing this slurry by ultrasonic shear for 10 to 200 min; then adding 40 to 80 mass% of polytetrafluoroethylene emulsion, further dispersing by shear for 10 to 150 min; controlling the temperature during the dispersion of the gas diffusion layer slurry between 10 and 100°C, and the powder in the gas diffusion layer slurry having an average particle size between 0.2 and 10 ⁇ m after dispersion; setting the gas diffusion layer slurry for 5 to 100 h after dispersion; and controlling the solid content of the gas diffusion layer slurry between 5 and 40 wt%; and (2) coating the gas diffusion layer slurry evenly on the silver-plated metal foam of the current collector; after coating of the gas
- the preparation method of the gas catalysis layer comprises the following steps: (1) dispersing the catalyst, the acidified graphitized carbon black in the aqueous isopropanol solution comprising surfactant Triton, so as to obtain the catalysis layer slurry; dispersing this slurry by ultrasonic shear for 10-200 min; then adding 40-80 mass% of polytetrafluoroethylene emulsion, further dispersing by shear for 10-150 min; and controlling the temperature during the dispersion of the catalysis layer slurry between 10-100°C and the powder in the catalysis layer slurry having an average particle size between 0.2-10 ⁇ m after dispersion; and (2) coating the catalysis layer slurry evenly on the gas diffusion layer of the assembly of the gas diffusion layer and the current collector; drying it at 40-120°C for 0.5-1 h after coating of the catalysis layer slurry; after the coating and drying of the catalysis layer
- the silver-plated metal foam is prepared by plating Ag on the metal foam using electroplating, chemical plating, and replacement plating methods.
- the catalyst used in the present invention includes Ag powder and Ag/C composite catalyst (the preparation thereof please refer to CN 101745390A ), and the Ag/C composite catalysts mentioned in the context are all those prepared according to patent publication CN 101745390A .
- the present invention has the following advantageous effects.
- a gas diffusion layer which has not only good electrical conductivity and gas permeability capability but also excellent resistance to water pressure, can be prepared by the processes of dispersing highly-graphitized carbon black in the aqueous isopropanol solution comprising a certain surfactant using ultrasonic shear and standing, so as to obtain a uniformly dispersed gas diffusion layer slurry; coating the gas diffusion layer slurry evenly on the silver-plated metal foam; and performing cold-pressing after drying the slurry.
- a pre-molded gas diffusion electrode can be prepared by dispersing the catalyst and the acidified highly-graphitized carbon black in the aqueous isopropanol solution comprising a certain surfactant using ultrasonic shear so as to obtain a uniformly dispersed catalysis layer slurry; coating the catalysis layer slurry evenly on the gas diffusion layer; and performing cold-pressing after drying the slurry.
- the catalysis layer obtained in this way not only has suitable hydrophilic and hydrophobic capacity which is beneficial to the gas-liquid-solid three-phase reaction, but also has anti-etching capacity and the capacity of preventing the occurrence of side reaction producing hydrogen peroxide, thus facilitating the long-term and stable operation of the electrode.
- the pre-molded gas diffusion electrode is subjected to high-temperature baking in order to thoroughly remove the residual surfactant in the interior of the electrode, thereby facilitating the uniform of the pore structure during the hot-press molding process.
- a gas diffusion electrode having a sandwich structure is formed by hot-pressing the silver-plated metal foam on the surface of the catalysis layer during the hot-pressing process, thus not only being beneficial to the progression of the three-phase reaction in the catalysis process, but also being capable of improving the electro-catalysis capacity of the electrode in a basic solution and the mechanical strength of the electrode itself due to the silver-plated metal foam. Therefore, the gas diffusion electrode provided by the present invention has good corrosion resistance and good electrical conductivity, and runs stably in a basic solution; thus it is suitable for the electrolysis reaction in chlor-alkali industry.
- the highly-graphitized carbon black used in this example is prepared by graphitizing carbon black (Vulcan XC-72) in a high-temperature graphitization furnace at 2700°C for 6-10 h, and a Raman Spectrogram for measuring the graphitization degree thereof is shown in Figure 2 with I D /I G of 0.67.
- the silver-plated nickel foam is prepared by electroplating, wherein the nickel foam is commercially available from Heze Tianyu Technical Developing Lt. Corp.
- the acidified highly-graphitized carbon black is prepared by refluxing the graphitized carbon black in nitric acid solution (68 mass%) at 120°C for 6 to 10 h. Specifically,
- the highly-graphitized carbon black used in this example is prepared by graphitizing carbon black (Vulcan XC-72) at 2600°C for 2-15 h, and has a Raman Spectrogram with I D /I G of 0.7-1.0.
- the silver-plated nickel foam is prepared by electroplating, wherein the nickel foam is commercially available from Heze Tianyu Technical Developing Lt. Corp.
- the acidified highly-graphitized carbon black is prepared by refluxing the graphitized carbon black in nitric acid solution (68 mass%) at 140°C for 6 to 10 h. Specifically,
- the highly-graphitized carbon black used in this example is prepared by graphitizing carbon black (Vulcan XC-72) in a high-temperature graphitization furnace at 2900°C for 2-15 h, and has a Raman Spectrogram with I D /I G of 0.3-0.6.
- the silver-plated nickel foam is prepared by electroplating, wherein the nickel foam is commercially available from Heze Tianyu Technical Developing Lt. Corp.
- the acidified highly-graphitized carbon black is prepared by refluxing the graphitized carbon black in nitric acid solution (68 mass%) at 160°C for 6 to 10 h. Specifically,
- the highly-graphitized carbon black used herein is prepared by graphitizing carbon black (Vulcan XC-72) in a high-temperature graphitization furnace at 2700°C for 6-10 h, and a Raman Spectrogram for measuring the graphitization degree thereof is shown in Figure 2 with I D /I G of 0.67.
- the silver-plated nickel foam is prepared by electroplating, wherein the nickel foam is commercially available from Heze Tianyu Technical Developing Lt. Corp.
- the acidified highly-graphitized carbon black is prepared by refluxing the graphitized carbon black in nitric acid solution (68 mass%) at 120°C for 6 to 10 h. Specifically,
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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)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Inert Electrodes (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2012/001722 WO2014100912A1 (zh) | 2012-12-24 | 2012-12-24 | 一种气体扩散电极及其制备方法 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP2937449A1 true EP2937449A1 (de) | 2015-10-28 |
| EP2937449A4 EP2937449A4 (de) | 2016-08-17 |
| EP2937449B1 EP2937449B1 (de) | 2017-07-12 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP12891307.6A Active EP2937449B1 (de) | 2012-12-24 | 2012-12-24 | Gasdiffusionselektrode und herstellungsverfahren dafür |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP2937449B1 (de) |
| JP (1) | JP6128709B2 (de) |
| CN (1) | CN104603331B (de) |
| WO (1) | WO2014100912A1 (de) |
Cited By (2)
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|---|---|---|---|---|
| CN111058055A (zh) * | 2019-12-20 | 2020-04-24 | 江苏安凯特科技股份有限公司 | 一种离子膜电解槽的阴极结构 |
| JPWO2019106879A1 (ja) * | 2017-11-29 | 2020-10-01 | 住友電気工業株式会社 | 金属多孔体、燃料電池及び金属多孔体の製造方法 |
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| CN106894042B (zh) * | 2017-02-28 | 2018-08-17 | 天津大学 | 一种酸处理石墨颗粒电极的制备及应用 |
| CN110565112B (zh) * | 2019-08-19 | 2021-10-26 | 天津大学 | 一种通过调控亲疏水性改变阴极氧还原活性的方法 |
| CN113149142A (zh) * | 2020-01-22 | 2021-07-23 | 中国科学院大连化学物理研究所 | 气体扩散电极及其制备方法和应用 |
| CN111733426B (zh) * | 2020-07-31 | 2022-08-30 | 北京化工大学 | 一种基于气体扩散电极电化学制备高铁酸盐的方法及装置 |
| CN111893502A (zh) * | 2020-07-31 | 2020-11-06 | 北京化工大学 | 一种用非贵金属催化的气体扩散电极电解制备高铁酸盐的方法 |
| CN113371799B (zh) * | 2021-06-22 | 2022-10-04 | 哈尔滨工业大学 | 基于单线态氧的电化学消毒方法 |
| CN116040751A (zh) * | 2021-10-28 | 2023-05-02 | 中国石油化工股份有限公司 | 一种改性氮掺杂炭电极及其制备方法和应用 |
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| CN115478286B (zh) * | 2022-09-22 | 2026-03-24 | 盐城工学院 | 一种气体扩散电极及其制备方法 |
| CN116235962B (zh) * | 2022-11-25 | 2026-01-23 | 珠海格力电器股份有限公司 | 电解装置、电极制备方法及清洗设备 |
| CN116334659B (zh) * | 2023-04-16 | 2024-06-21 | 深圳中科翎碳生物科技有限公司 | Sn基气体扩散电极、制备方法、相应电催化装置及应用 |
| CN118825310A (zh) * | 2024-06-28 | 2024-10-22 | 深圳市贝特瑞新能源技术研究院有限公司 | 一种微孔层水性浆料及其制备方法和气体扩散层 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3068641D1 (de) * | 1979-02-27 | 1984-08-30 | Asahi Glass Co Ltd | Gas diffusion electrode |
| JP3625520B2 (ja) * | 1995-04-13 | 2005-03-02 | ペルメレック電極株式会社 | ガス拡散電極 |
| JP3628756B2 (ja) * | 1995-04-28 | 2005-03-16 | ペルメレック電極株式会社 | ガス拡散電極 |
| JP3002974B2 (ja) * | 1998-05-20 | 2000-01-24 | 長一 古屋 | ガス拡散電極の製造方法 |
| JP2946328B1 (ja) * | 1998-08-25 | 1999-09-06 | 長一 古屋 | 食塩電解方法及び電解槽 |
| EP1029946A3 (de) * | 1999-02-16 | 2007-11-14 | Nagakazu Furuya | Gasdiffusionselektrodenanordnungen und Verfahren zu ihrer Herstellung |
| EP1076115A1 (de) * | 1999-02-25 | 2001-02-14 | Toagosei Co., Ltd. | Gasdiffusionselektrode und elektrolytisches bohrlaugenbad |
| JP4290454B2 (ja) | 2003-03-28 | 2009-07-08 | 三井化学株式会社 | ガス拡散電極の製造方法、電解槽及び電解方法 |
| JP4715842B2 (ja) * | 2005-02-21 | 2011-07-06 | 日産自動車株式会社 | 電極触媒の製造方法、膜電極接合体の製造方法、および固体高分子型燃料電池の製造方法 |
| DE102005023615A1 (de) * | 2005-05-21 | 2006-11-23 | Bayer Materialscience Ag | Verfahren zur Herstellung von Gasdiffusionselektroden |
| JP4868949B2 (ja) | 2006-06-07 | 2012-02-01 | ペルメレック電極株式会社 | ガス拡散電極とその製造方法 |
| JP5222056B2 (ja) * | 2008-07-29 | 2013-06-26 | 三菱重工業株式会社 | 料金収受機、料金収受方法及びプログラム |
| CN101736360B (zh) | 2009-11-27 | 2011-06-01 | 北京化工大学 | 一种气体扩散电极及其制备方法 |
| CA2782274A1 (en) * | 2009-12-09 | 2011-06-16 | Nisshinbo Holdings Inc. | Flexible carbon fiber nonwoven fabric |
| CN101745390B (zh) | 2010-01-29 | 2011-11-16 | 北京化工大学 | 一种用于食盐电解的负载型银碳催化剂及其制备方法 |
| CN101774666B (zh) * | 2010-01-29 | 2011-12-21 | 北京化工大学 | 一种2-乙基蒽醌改性气体扩散电极及其制备方法 |
| JP5648785B2 (ja) * | 2010-07-29 | 2015-01-07 | 日清紡ホールディングス株式会社 | 燃料電池用電極 |
| CN102517602B (zh) * | 2011-12-29 | 2014-10-29 | 北京化工大学 | 一种气体扩散电极的明胶造孔方法 |
-
2012
- 2012-12-24 JP JP2015548134A patent/JP6128709B2/ja active Active
- 2012-12-24 CN CN201280074539.0A patent/CN104603331B/zh active Active
- 2012-12-24 WO PCT/CN2012/001722 patent/WO2014100912A1/zh not_active Ceased
- 2012-12-24 EP EP12891307.6A patent/EP2937449B1/de active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2019106879A1 (ja) * | 2017-11-29 | 2020-10-01 | 住友電気工業株式会社 | 金属多孔体、燃料電池及び金属多孔体の製造方法 |
| JP7076693B2 (ja) | 2017-11-29 | 2022-05-30 | 住友電気工業株式会社 | 金属多孔体、燃料電池及び金属多孔体の製造方法 |
| CN111058055A (zh) * | 2019-12-20 | 2020-04-24 | 江苏安凯特科技股份有限公司 | 一种离子膜电解槽的阴极结构 |
| CN111058055B (zh) * | 2019-12-20 | 2021-01-15 | 江苏安凯特科技股份有限公司 | 一种离子膜电解槽的阴极结构 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104603331A (zh) | 2015-05-06 |
| CN104603331B (zh) | 2017-04-05 |
| EP2937449A4 (de) | 2016-08-17 |
| JP2016505716A (ja) | 2016-02-25 |
| JP6128709B2 (ja) | 2017-05-17 |
| WO2014100912A1 (zh) | 2014-07-03 |
| EP2937449B1 (de) | 2017-07-12 |
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