WO2020110527A1 - Électrode de génération d'hydrogène, son procédé de production et procédé de production d'hydrogène - Google Patents

Électrode de génération d'hydrogène, son procédé de production et procédé de production d'hydrogène Download PDF

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Publication number
WO2020110527A1
WO2020110527A1 PCT/JP2019/041653 JP2019041653W WO2020110527A1 WO 2020110527 A1 WO2020110527 A1 WO 2020110527A1 JP 2019041653 W JP2019041653 W JP 2019041653W WO 2020110527 A1 WO2020110527 A1 WO 2020110527A1
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platinum
electrode
nickel
hydrogen generation
hydrogen
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PCT/JP2019/041653
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English (en)
Japanese (ja)
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由希子 勝圓
尚平 松井
宏一 寺田
剛一 曽田
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株式会社大阪ソーダ
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Priority to JP2020558185A priority Critical patent/JPWO2020110527A1/ja
Priority to CN201980076192.5A priority patent/CN113166958A/zh
Publication of WO2020110527A1 publication Critical patent/WO2020110527A1/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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material

Definitions

  • the present invention relates to a hydrogen generating electrode, a manufacturing method thereof, and a hydrogen manufacturing method.
  • cathode in the case of the conventionally used mild steel, stainless steel, and nickel electrodes, an overvoltage of 300 to 400 mV was generated under normal operating conditions. Therefore, activation of these electrode surfaces and reduction of overvoltage have been studied, and many techniques have been developed so far. Examples of producing a highly active cathode while the electrode surface is an oxide by plasma spraying nickel oxide, Raney nickel-based plating, nickel and tin composite plating, activated carbon and oxide composite plating There is an example where it is applied to the electrode surface, and all of them are intended to be used as a cathode for hydrogen generation in caustic soda. However, in order to reduce the electrolysis voltage, it is necessary to further reduce the cathode overvoltage, and therefore various cathodes as described below have been proposed.
  • Patent Document 1 a noble metal coating made of one type of noble metal or a mixture or alloy of two types or three or more types of noble metals, and a film containing one type or two or more types of base metals such as nickel in the noble metal coating.
  • An electrode for hydrogen generation has been proposed in which is coated on a conductive base material such as nickel.
  • these hydrogen generation electrodes have a problem that they are easily poisoned by impurities such as iron in the electrolytic solution (see Patent Document 2).
  • an electrode for hydrogen generation has been proposed in which a catalyst containing platinum and ruthenium and at least one of gold and silver, or a catalyst containing particles of an organic polymer is carried on a conductive substrate (Patent Document 3).
  • the hydrogen generating electrode has an extremely small increase in overvoltage even when iron ions are present in the catholyte, and is certainly excellent in that it can reduce the amount of energy used for electrolysis of the aqueous alkali metal chloride solution.
  • platinum, ruthenium, gold, and silver are all expensive materials, and when polytetrafluoroethylene is contained therein, the cost becomes even higher. Therefore, even in this case, there is still a problem to be improved from the economical point of view.
  • Patent Document 4 an electrode for hydrogen generation using a catalyst composed of platinum and cerium oxide has been proposed (Patent Document 4).
  • the hydrogen generating electrode composed of the catalyst of platinum and cerium oxide has a low overvoltage, is suppressed from being affected by iron ions, and exhibits excellent performance as a hydrogen generating electrode for electrolysis of an aqueous solution of an alkali metal chloride.
  • a proposal has been made to provide an intermediate layer made of nickel oxide between a catalyst made of platinum and cerium oxide and a base material, and further studies are being made to further improve the cost aspect.
  • a conductive metal is heretofore coated with a cerium-platinum mixture-based electrode active substance containing at least one of cerium metal, cerium oxide or cerium hydroxide and platinum metal.
  • the composition of the electrode active material is cerium-rich with a mole fraction of platinum of 15 to 30 mol% and a cerium mole fraction of 70 to 85 mol% in terms of metal.
  • An electrode was developed (Patent Document 5). Furthermore, a platinum alloy of platinum and one kind of transition metal element selected from the group of nickel, cobalt, copper, silver and iron is supported on the conductive substrate, and the platinum content in the platinum alloy is in a molar ratio. A hydrogen generating electrode having a range of 0.40 to 0.99 has also been developed (Patent Document 6).
  • the present invention can reduce the overvoltage converted from the hydrogen generation potential of the hydrogen generation electrode, and further, the reduction of the effective surface area of the platinum catalyst due to the reverse current when the electrolysis is stopped is effective.
  • the main object of the present invention is to provide an electrode for hydrogen generation, which is suppressed physically.
  • Another object of the present invention is to provide a method for manufacturing the hydrogen generating electrode, and an electrolysis method using the hydrogen generating electrode.
  • the present inventor has diligently studied to solve the above problems.
  • the overvoltage converted from the hydrogen generation potential of the hydrogen generating electrode It has been found that the reduction of the effective surface area of the platinum catalyst due to the reverse current when the electrolysis is stopped can be effectively suppressed.
  • the present invention has been completed by further studies based on such findings.
  • Item 1 An electrode for hydrogen generation, which has a coating film containing at least platinum, nickel oxide, and cerium oxide on a conductive substrate.
  • Item 2. Item 2. The hydrogen generating electrode according to Item 1, wherein the amount of platinum supported on the coating film is 2 g/m 2 or more.
  • Item 3. Item 3. The hydrogen generating electrode according to Item 1 or 2, wherein the conductive base material contains nickel.
  • Item 4. A method for producing an electrode for hydrogen generation, comprising a step of forming a coating film containing at least platinum, nickel oxide, and cerium oxide on a conductive base material.
  • Item 6 Use of an electrode having a coating containing at least platinum, nickel oxide, and cerium oxide on a conductive substrate for hydrogen generation.
  • the overvoltage converted from the hydrogen generation potential of the hydrogen generation electrode can be lowered, and further, the reduction of the effective surface area of the platinum catalyst due to the reverse current when the electrolysis is stopped is effectively suppressed.
  • an electrode for hydrogen generation can be provided. Further, according to the present invention, it is possible to provide a method for producing the hydrogen generating electrode and an electrolysis method using the hydrogen generating electrode.
  • the hydrogen generating electrode of the present invention includes a conductive base material and a coating film provided on the conductive base material, and the coating film contains at least platinum, nickel oxide, and cerium oxide. It is characterized by The electrode for hydrogen generation of the present invention, by having such a configuration, can reduce the overvoltage converted from the hydrogen generation potential, and further, the effectiveness of the platinum catalyst due to the reverse current when the electrolysis is stopped. The reduction in surface area is effectively suppressed.
  • the hydrogen generating electrode of the present invention, the method for producing the hydrogen generating electrode, and the electrolysis method using the hydrogen generating electrode will be described in detail.
  • the numerical value connected by “to” means a numerical value range including the numerical values before and after “to” as the lower limit value and the upper limit value.
  • any lower limit value and upper limit value can be selected and connected by "".
  • Electrode for Hydrogen Generation of the present invention comprises a conductive base material and a coating film provided on the conductive base material. Further, the coating film contains at least platinum, nickel oxide, and cerium oxide.
  • the conductive base material is not particularly limited as long as it has conductivity and functions as a base material of the coating, and a conductive base material used in a known hydrogen generating electrode is used. Can be used.
  • the conductive base material preferably contains a metal, and more preferably is composed of a metal.
  • the metal preferably includes nickel, stainless steel, iron, copper, titanium, steel and the like, and among these, nickel is preferable.
  • a conductive group The material is preferably composed of nickel.
  • As the conductive base material containing nickel in addition to the one made of nickel, for example, a stainless steel surface coated with nickel is also suitable.
  • the shape of the conductive base material is not particularly limited, and may be plate-shaped, rod-shaped, porous (expanded metal, punching metal, blind, etc.). From the viewpoint of increasing the surface area of the coating film provided on the conductive substrate, it is preferably porous.
  • the size of the conductive substrate is not particularly limited and may be appropriately set according to the scale of electrolysis, the size of the hydrogen generating electrode, etc., for example, the length is about 300 mm to 2,500 mm, and the width is 1.
  • the thickness is about 200 mm to 1,500 mm, and the thickness is about 0.1 mm to 6 mm.
  • the surface of the conductive base material may be roughened from the viewpoint of improving the adhesion of the coating.
  • the surface roughness Ra of the conductive base material can be set to, for example, about 1 to 10 ⁇ m. Examples of the method for roughening the surface of the conductive base material include blast treatment.
  • the surface of the conductive base material may be subjected to etching treatment from the viewpoint of improving the adhesion of the coating film.
  • the etching method include a method of immersing the conductive base material in an acid such as hydrochloric acid. Further, after the etching treatment, it is preferable to wash with water and dry until the surface of the conductive substrate becomes neutral.
  • the coating is formed on the conductive base material. More specifically, the coating is preferably formed on the surface of the conductive base material.
  • the coating contains platinum, nickel oxide, and cerium oxide.
  • the state of platinum is not particularly limited, but it is preferable that at least a part of platinum is contained as platinum metal, and platinum oxide, platinum hydroxide or the like may be contained.
  • at least a part of nickel is contained as nickel oxide, and nickel metal, nickel hydroxide and the like may be further contained.
  • cerium at least a part thereof is contained as a cerium oxide, and a cerium metal, a cerium hydroxide or the like may be further contained. Further, it may be in the state of an alloy of each of the above-mentioned metals or an amorphous metal.
  • the molar ratio of platinum element, nickel element, and cerium element (Pt/Ni/Ce) contained in the coating film is not particularly limited, but the nickel element is preferably 0.05 to 5 moles per 1 mole of platinum. The amount is more preferably about 0.5 to 2 mol. Further, the amount of cerium element is preferably about 0.05 to 10 mol, and more preferably about 0.5 to 2 mol with respect to 1 mol of platinum.
  • the platinum content in the coating is , Preferably 2 g/m 2 or more, more preferably 3 g/m 2 or more, still more preferably 4 g/m 2 or more.
  • the upper limit of the amount of platinum catalyst supported is, for example, 20 g/m 2 .
  • the thickness of the coating film is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, and further 1 ⁇ m or more.
  • the upper limit of the thickness of the coating is, for example, 20 ⁇ m.
  • the method for forming a coating film on a conductive substrate is not particularly limited, but as described below, for example, a solution containing a platinum compound, a nickel compound, and a cerium compound is applied onto the conductive substrate, It can be suitably formed by a method of firing the formed coating film to thermally decompose these compounds.
  • the coating may contain other metals different from platinum, nickel, and cerium.
  • other metals include lanthanum, zirconium, niobium, molybdenum, and the like.
  • the content thereof is preferably 5 mol% or less, more preferably 1 mol% or less, further preferably 0.5 mol% or less.
  • the metal contained in the coating is preferably 95 mol% or more in total of platinum, nickel, and cerium, more preferably 99 mol% or more, and 99.5 mol. % Or more, 99.9 mol% or more, and further 100 mol% (that is, substantially no other metal is contained) is also preferable.
  • the electrode for hydrogen generation of the present invention is an electrode for a known electrolysis method of a solution containing water (for example, water, an aqueous solution of an alkali metal chloride such as sodium chloride, an aqueous solution of an alkali metal hydroxide such as sodium hydroxide). It is preferably used to generate hydrogen from the electrode. That is, the hydrogen generating electrode of the present invention is suitable as a cathode in a method of electrolyzing a solution containing water.
  • the method for producing a hydrogen generation electrode of the present invention includes at least a step of forming a coating film containing platinum, nickel oxide, and cerium oxide.
  • the method for forming the coating is not particularly limited, and includes pyrolysis method, powder sintering method, electroplating method, dispersion plating method, thermal spraying method, arc ion plating method, platinum, nickel oxide, and cerium oxide.
  • a known method can be employed in which a coating film containing is formed on the conductive substrate.
  • the thermal decomposition method for example, a step of applying a solution containing at least a platinum compound, a nickel compound, and a cerium compound on a conductive base material to form a coating film of the solution on the conductive base material, Firing the coating film on the conductive base material to form a coating film containing at least platinum, nickel oxide, and cerium oxide on the conductive base material.
  • the platinum compound is not particularly limited as long as it contains platinum in the coating by thermally decomposing by firing of the coating film, for example, dinitrodiammine platinum, chloroplatinic acid, tetraammine platinum nitrate, hexaammine platinum hydroxide, Examples include bis(acetylacetonato)platinum.
  • the platinum compound may be one kind or two or more kinds.
  • the nickel compound is not particularly limited as long as it is thermally decomposed by firing of the coating film and contains nickel oxide in the coating film, and examples thereof include nickel nitrate, nickel sulfate, nickel carbonate, nickel chloride and nickel acetate. Is mentioned.
  • the nickel compound may be one kind or two or more kinds.
  • cerium compound is not particularly limited as long as it is pyrolyzed by firing the coating film and contains cerium oxide in the coating film, for example, cerium nitrate, cerium sulfate, cerium carbonate, cerium chloride, cerium acetate, etc. Is mentioned.
  • cerium compound may be one kind or two or more kinds.
  • the molar ratio (Pt/Ni/Ce) of platinum element, nickel element, and cerium element contained in the solution is not particularly limited, and it can be adjusted so as to be the molar ratio in the above-mentioned coating.
  • the solvent contained in the solution is not particularly limited, but those capable of dissolving the platinum compound, nickel compound and cerium compound are preferable.
  • Specific examples of the solvent include water, inorganic acids such as nitric acid, hydrochloric acid, sulfuric acid and acetic acid, lower alcohols such as methanol, ethanol, propanol and butanol, and mixed solutions containing at least two of these.
  • a pH adjusting agent or the like may be added to the solution, and from the viewpoint of complexing platinum, nickel, and cerium to increase the surface area, lysine , Citric acid, etc. may be added.
  • the total concentration of platinum, nickel, and cerium in the solution is not particularly limited, but preferably 2% from the viewpoint of suitably forming the coating so that the amount of the platinum catalyst contained in the coating becomes a predetermined amount. As mentioned above, more preferably about 3 to 30%, further preferably about 4 to 20%.
  • a solution containing at least a platinum compound, a solution containing at least a nickel compound, and a solution containing at least a cerium compound are prepared, and each solution is applied onto a conductive base material. Then, a coating film may be formed.
  • the solution containing at least a platinum compound may further contain at least one of a nickel compound and a cerium compound, or the solution containing at least a nickel compound may further contain at least one of a platinum compound and a cerium compound.
  • a solution containing at least a cerium compound may further contain at least one of a platinum compound and a nickel compound.
  • drying and firing described later may be performed to form a coating film having a multi-layer structure having different compositions.
  • the method of applying the solution onto the conductive base material is not particularly limited, and known methods such as a brush application method, a spray method and a dip coating method can be adopted.
  • the surface of the conductive base material may be roughened or may be subjected to treatments such as etching, washing with water and drying.
  • the coating film After coating the solution on the conductive base material, it is preferable to dry the coating film before firing the coating film.
  • the drying may be carried out under the condition that the solvent evaporates, for example, at a temperature of 200° C. or lower for about 5 to 60 minutes, and preferably at a temperature of 150° C. or lower.
  • the obtained coating film is fired to form a coating film containing at least platinum, nickel oxide, and cerium oxide on the conductive base material to obtain a hydrogen generating electrode.
  • the calcination can be performed, for example, in an oxidizing atmosphere such as air (for example, in the air).
  • Calcination may be carried out under the condition that the platinum compound, nickel compound and cerium compound in the coating film are thermally decomposed and the resulting coating film contains platinum, nickel oxide and cerium oxide.
  • the firing temperature is preferably about 200 to 700°C, more preferably about 350 to 550°C.
  • the firing time is preferably about 5 to 60 minutes, more preferably about 10 to 30 minutes.
  • the above-mentioned series of steps of coating, drying, and firing are repeated once or more, preferably a plurality of times to form a film on the conductive substrate.
  • the number of times of the series of steps is not particularly limited, and it is preferable to repeat until the amount of platinum catalyst supported reaches a predetermined amount.
  • the composition of the solution to be applied may be the same or different, but usually the same.
  • the hydrogen generating electrode of the present invention can be suitably manufactured.
  • the electrolysis method of the present invention is a method for electrolyzing a solution containing water (for example, water, an aqueous solution of an alkali metal chloride such as sodium chloride, an aqueous solution of an alkali metal hydroxide such as sodium hydroxide). It is a method using the hydrogen generating electrode of the invention. Specifically, in a known electrolysis method of a solution containing water, the hydrogen generating electrode of the present invention is used as the hydrogen generating electrode.
  • the temperature of the electrolyte at the start of use is about 70 to 90° C.
  • the concentration of the electrolyte in the cathode chamber (sodium hydroxide). can be about 20 to 40% by mass, and the current density can be about 0.1 to 10 kA/m 2 .
  • Electrolyte solution 32 wt% sodium hydroxide aqueous solution (capacity about 300 mL) Liquid temperature: 80°C
  • Working electrode each hydrogen generating electrode of Examples 1 to 4 and Comparative example 1
  • Counter electrode Platinum plate (25 mm x 25 mm)
  • Reference electrode mercury/mercury oxide electrode (Hg/HgO) (immersed in 32 wt% sodium hydroxide aqueous solution (25° C.))
  • ⁇ Reverse current resistance test> A reverse current resistance test was conducted using the hydrogen generating electrodes of Examples 1 to 4. Specifically, each hydrogen generating electrode was used as a working electrode, and a cell as shown in the schematic view of FIG. 1 was assembled. Next, a negative polarization electrolysis was performed at 10 kA/m 2 for 60 minutes to prepare a sample before the test (current is in a direction usually used). Then, 1 kA/m 2 for 45 minutes of anodic polarization electrolysis (current is in the opposite direction to that normally used) and 9 kA/m 2 for 15 minutes of negative polarization electrolysis (current is normally used). Direction) is set as one cycle, and a cycle test (see the cycle diagram of FIG.
  • Example 1 is represented by Ex1
  • Example 2 is represented by Ex2
  • Example 3 is represented by Ex3
  • Example 4 is represented by Ex4.
  • Example 3 As shown in Table 1, when comparing the effective surface areas of the platinum catalysts before and after the reverse current resistance test, the reduction rate of Example 3 was suppressed about three times that of Comparative Example 1. This shows that the platinum catalyst functions more effectively in Comparative Example 1 after the load of reverse current is applied, and Example 3 has resistance to reverse current. Can be said. Further, as shown in FIG. 3, the absolute value of the initial hydrogen generation potential was lower than that of Comparative Example 1 (Rf1) in all Examples (Ex1 to Ex4), and a decrease in overvoltage was observed. In addition, as shown in FIG. 4, this low overvoltage continued even after the reverse current load.
  • the hydrogen generation electrode of the present invention can reduce the overvoltage converted from the hydrogen generation potential, and further, the reduction of the effective surface area of the platinum catalyst due to the reverse current when the electrolysis is stopped is effectively suppressed. It is shown in Table 1 and FIGS. 3 and 4 that it has resistance to reverse current.

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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)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

L'invention concerne une électrode de génération d'hydrogène selon laquelle il est possible de réduire une surtension, qui est convertie à partir du potentiel de génération d'hydrogène de l'électrode de génération d'hydrogène, et selon laquelle des réductions de surface effective de catalyseur de platine, provoquées par un courant inverse lorsqu'une électrolyse est arrêtée, peuvent être efficacement empêchées.　L'électrode de génération d'hydrogène comprend un revêtement contenant au moins du platine, de l'oxyde de nickel et de l'oxyde de cérium sur un matériau de base électroconducteur.
PCT/JP2019/041653 2018-11-27 2019-10-24 Électrode de génération d'hydrogène, son procédé de production et procédé de production d'hydrogène WO2020110527A1 (fr)

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JP2020558185A JPWO2020110527A1 (ja) 2018-11-27 2019-10-24 水素発生用電極、その製造方法、及び水素の製造方法
CN201980076192.5A CN113166958A (zh) 2018-11-27 2019-10-24 氢产生用电极、其制造方法、以及氢的制造方法

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20220135481A (ko) * 2021-03-30 2022-10-07 전남대학교산학협력단 수소 발생 반응 촉매 전극, 이의 제조방법, 및 이를 이용한 수소 제조 방법

Citations (4)

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JPH0633492B2 (ja) * 1987-06-29 1994-05-02 ペルメレック電極株式会社 電解用陰極及びその製造方法
JP2000239882A (ja) * 1999-02-24 2000-09-05 Permelec Electrode Ltd 活性化陰極及びその製造方法
WO2015098058A1 (fr) * 2013-12-26 2015-07-02 東ソー株式会社 Électrode pour la production d'hydrogène, procédé pour la production de celle-ci et procédé d'électrolyse utilisant celle-ci
CN107687002A (zh) * 2017-08-17 2018-02-13 沈阳中科惠友科技发展有限责任公司 一种掺杂石墨烯的活性阴极及其制备方法

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CN1012970B (zh) * 1987-06-29 1991-06-26 耐用电极株式会社 用于电解的阴极及其制备方法

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
JPH0633492B2 (ja) * 1987-06-29 1994-05-02 ペルメレック電極株式会社 電解用陰極及びその製造方法
JP2000239882A (ja) * 1999-02-24 2000-09-05 Permelec Electrode Ltd 活性化陰極及びその製造方法
WO2015098058A1 (fr) * 2013-12-26 2015-07-02 東ソー株式会社 Électrode pour la production d'hydrogène, procédé pour la production de celle-ci et procédé d'électrolyse utilisant celle-ci
CN107687002A (zh) * 2017-08-17 2018-02-13 沈阳中科惠友科技发展有限责任公司 一种掺杂石墨烯的活性阴极及其制备方法

Cited By (2)

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Publication number Priority date Publication date Assignee Title
KR20220135481A (ko) * 2021-03-30 2022-10-07 전남대학교산학협력단 수소 발생 반응 촉매 전극, 이의 제조방법, 및 이를 이용한 수소 제조 방법
KR102577725B1 (ko) * 2021-03-30 2023-09-12 전남대학교산학협력단 수소 발생 반응 촉매 전극, 이의 제조방법, 및 이를 이용한 수소 제조 방법

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