WO2019146913A1 - Catalyseur pour réaction de dégagement d'hydrogène comprenant un promoteur de cuivre - Google Patents

Catalyseur pour réaction de dégagement d'hydrogène comprenant un promoteur de cuivre Download PDF

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WO2019146913A1
WO2019146913A1 PCT/KR2018/016087 KR2018016087W WO2019146913A1 WO 2019146913 A1 WO2019146913 A1 WO 2019146913A1 KR 2018016087 W KR2018016087 W KR 2018016087W WO 2019146913 A1 WO2019146913 A1 WO 2019146913A1
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catalyst
copper promoter
promoter
following formula
compound represented
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PCT/KR2018/016087
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English (en)
Korean (ko)
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김성웅
이규형
김예지
강세황
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성균관대학교산학협력단
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Publication of WO2019146913A1 publication Critical patent/WO2019146913A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/057—Selenium or tellurium; Compounds thereof
    • B01J27/0573—Selenium; Compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/057—Selenium or tellurium; Compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0215—Coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • 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
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • 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
    • C25B11/037—Electrodes made of particles
    • 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
    • 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
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the present invention relates to a catalyst containing a copper promoter for hydrogen generation reaction, and more particularly to a catalyst containing a copper promoter which can be used for electrolysis of water with high efficiency, resistance and homogeneity, Selenide-based or sulfide-based catalysts.
  • Water one of the easiest sources on the planet, can produce hydrogen gas through electrolysis. This method is an ideal method of hydrogen generation because it does not emit greenhouse gases from the environmental point of view and is comparable to other methods such as biomass pyrolysis and coal gasification.
  • Electronic cargo has a low work function and can be utilized as an electron emission material. Due to high magnetic entropy change, it can be used as a magnetic material (hard magnetic material, magnetic thermal material, etc.) and widely used as a catalyst material due to its high electron transfer efficiency. It is a substance that can be.
  • Electronic cargo is divided into organic and inorganic electronic cargo.
  • organic electronic cargo is unstable at room temperature and can not be applied as electronic material.
  • Inorganic electronic cargo that is stable at room temperature is C12A7 developed in 2003, namely 12CaO ⁇ 7Al2O3 (AE3N) was recently developed and patented by the Tokyo Institute of Technology, Japan (JP2014-024712, JP2012-166325).
  • the Korea Institute of Ceramic Engineering has applied for a patent for C12A7 (KR2013-0040232, etc.), but no inorganic electronic materials containing other components have been reported yet.
  • the catalyst material is at least one selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (2), and a compound represented by the following formula (1) and a compound represented by the following formula For catalyst:
  • Hf-O compound layer a layer of Hf-O compound coated on the surface of the catalyst material.
  • one or more of the Hf-Se-O compound layer, the Hf-S-O compound layer, the amorphous Hf-Se compound layer or the amorphous Hf-S compound layer coated on the surface of the catalyst material may be further included.
  • the catalyst for hydrogen generation reaction containing the copper promoter may be produced in powder or bulk form.
  • the bulk phase may be a single crystal or a sinter produced by sintering.
  • the present invention also provides an electrode comprising a catalyst for hydrogen generation reaction comprising the copper promoter according to the present invention.
  • step (b) electrodeifying the catalytic material comprising the copper promoter obtained in step (a)
  • the catalyst material is at least one selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (2), and a compound represented by the following formula (1)
  • a method of manufacturing an electrode is provided.
  • step (a) it is preferable to circulate the circulating current at least 1000 times using the circulating current method.
  • step (b) it is preferable to reduce the contact resistance by introducing an Au layer on the surface not including the proporator.
  • the present invention provides an electrode manufactured by the method for manufacturing an electrode according to the present invention.
  • the present invention also provides a hydrogen generator having a reformer in which a catalyst for hydrogen generation reaction according to the present invention is disposed.
  • the present invention provides an electrode, a counter electrode, and a hydrogen generator using the acid electrolyte or the ionizing liquid according to the present invention.
  • the catalyst for hydrogen generation reaction comprising the copper promoter provided in the present invention has a uniform catalytic property by increasing the surface area and solving the uneven problem caused by the oxide film by introducing the copper promoter on the surface of the oxide film, Can exhibit high efficiency, resistance and homogeneity for fuel production.
  • FIG. 1 is a graph showing the result of SEM measurement after introducing a Cu promoter into a selenide-based material.
  • FIG. 2 is a graph showing the result of SEM-EDS mapping showing that a Cu promoter is loaded into a selenide-based material.
  • FIG. 3 is a graph showing the results of evaluating characteristics of a catalyst for hydrogen generation reaction of a catalyst in which a Cu promoter is not introduced into a selenide-based material.
  • FIG. 4 is a graph showing the results of evaluating the characteristics of a catalyst for hydrogen generation reaction of a catalyst having a Cu promoter introduced into a selenide-based material.
  • FIG. 5 is a graph showing the result of SEM measurement after introduction of a Cu promoter on a sulfide-based material.
  • FIG. 6 is a graph showing the result of SEM-EDS mapping showing that a Cu promoter is loaded in a sulfide-based material.
  • FIG. 7 is a graph showing a result of evaluating the characteristics of a catalyst for hydrogen generation reaction of a catalyst in which a Cu promoter is not introduced into a sulfide-based material.
  • FIG. 8 is a graph showing the results of evaluating the characteristics of a catalyst for hydrogen generation reaction of a catalyst having a Cu promoter introduced into a sulfide-based material.
  • the invention Hf 2 + x Se (0 ⁇ x ⁇ 0.4) , Hf 2 Se 1 -y (0 ⁇ y ⁇ 0.1), Hf 2 + x Se (0 ⁇ x ⁇ 0.4) and Hf 2 Se 1-y ( complex of 0 ⁇ y ⁇ 0.1), Hf 2 + x S (0 ⁇ x ⁇ 0.4), Hf 2 S 1 -y (0 ⁇ y ⁇ 0.1), or Hf 2 + x S (0 ⁇ x ⁇ 0.4) and A copper promoter is introduced into the surface of an oxide film serving as a protective layer of Hf 2 S 1 -y (0 ⁇ y ? 0.1), thereby widening the surface area of the catalyst, exhibiting uniform catalytic properties, A catalyst for hydrogen generation reaction comprising a copper promoter having a hydrogen atom and a hydrogen atom.
  • 'promoter' is a substance to be added to increase the activity of the catalyst, itself having no catalytic activity or less activity. Therefore, although it is not a catalyst used in the hydrogen generation reaction, copper promoting the activity of the catalyst can be referred to as a promoter.
  • the present invention provides
  • a catalytic material and a copper promoter wherein the catalytic material is selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (2), and a complex of a compound represented by the following formula Or more of the total amount of the catalyst.
  • Hf-O compound layer a layer of Hf-O compound coated on the surface of the catalyst material.
  • one or more of the Hf-Se-O compound layer, the Hf-S-O compound layer, the amorphous Hf-Se compound layer or the amorphous Hf-S compound layer coated on the surface of the catalyst material may be further included.
  • the stabilization degree of the material itself can be further enhanced.
  • the complex catalyst for hydrogen generation reaction may be prepared in powder or bulk form.
  • the bulk phase may be a single crystal or a sinter produced by sintering.
  • the present invention also provides an electrode comprising a catalyst for hydrogen evolution reaction.
  • the hydrogen generating reaction may be performed using the electrode, the counter electrode, and the acid electrolyte or the ionizing liquid.
  • the electrolyte may be nitric acid, hydrochloric acid, sulfuric acid, etc.
  • the counter electrode may be a wire, a mesh, various types of metal electrodes such as a coil may be used.
  • the catalyst material is at least one selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (2), and a compound represented by the following formula (1)
  • a method for producing an electrode for hydrogen generation reaction is provided.
  • the introduction of the copper promoter by the circulating current method in the step (a) preferably maintains a cycle of at least 100 times, preferably up to 3000 times.
  • the step (b) preferably introduces a gold layer on the surface of the electrode not including the promoter.
  • the present invention provides an electrode manufactured by the method for manufacturing an electrode according to the present invention.
  • a general acid type electrolyte nitric acid, hydrochloric acid, sulfuric acid, etc.
  • an ionic liquid may be used.
  • various types of metal electrodes such as a wire, a mesh, and a coil may be used.
  • the present invention also provides a hydrogen generator having a reformer in which a catalyst for hydrogen generation reaction according to the present invention is disposed.
  • the present invention provides a hydrogen generator including the electrode, the electrolyte, the acid electrolyte or the ionizing liquid, and the counter electrode according to the present invention.
  • Hf and Se powders are mixed at a ratio of 2: 1, pelletized, sealed in a silica tube, and then placed in a furnace and sintered at 450-500 ° C for 50-70 hours.
  • the heat-treated mixture is placed in an arc melting facility chamber and an inert gas atmosphere such as argon is formed at a level capable of arc driving after forming a vacuum atmosphere. After the arc is applied, the heat-treated mixture is melted and solidified to synthesize an electrode material.
  • the synthesized electrode material is polished in a flat shape, connected to the cathode of the circulating current system together with copper metal, and then a copper promoter is introduced through a voltage sweep.
  • Hf and Se powder were mixed at a ratio of 2.1: 1 to prepare a sample as in Example 1.
  • Example 3 Preparation of electrode including Hf 2 Se 0 .9 and copper promoter
  • Hf and Se powder were mixed at a ratio of 2: 0.9 to prepare a sample as in Example 1.
  • Hf and S powder are mixed in a ratio of 2: 1, pelletized, vacuum-sealed in a silica tube, sintered at 450-500 ° C for 50-70 hours in a furnace.
  • the heat-treated mixture is placed in an arc melting facility chamber and an inert gas atmosphere such as argon is formed at a level capable of arc driving after forming a vacuum atmosphere. After the arc is applied, the heat-treated mixture is melted and solidified to synthesize an electrode material.
  • the synthesized electrode material is polished in a flat shape, connected to a cathode of a circulating current system together with copper metal, and then a copper promoter is introduced through a voltage sweep
  • Hf and S powder were mixed at a ratio of 2.1: 1 to prepare a sample as in Example 4.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne un catalyseur pour une réaction de dégagement d'hydrogène, le catalyseur comprenant : un matériau catalyseur contenant l'un quelconque parmi Hf et Se ou S ; et un promoteur de cuivre. Plus particulièrement, la présente invention concerne un catalyseur pour une réaction de dégagement d'hydrogène, le catalyseur comprenant : <formule chimique 1> Hf2 + xA (A étant Se ou S, x étant 0 ou un nombre premier et 0 ≤ x ≤ 0,4), <formule chimique 2> Hf2A1 - y (A étant Se ou S, y étant un nombre premier et 0 < y ≤ 0,1), ou un complexe associé ; et un promoteur de cuivre. Le catalyseur pour une réaction de dégagement d'hydrogène, selon la présente invention, a un promoteur de cuivre introduit sur une surface ayant un film d'oxyde, et peut ainsi permettre de résoudre des problèmes de contact dus au film d'oxyde, peut contribuer à l'amélioration de performance en ayant la surface du catalyseur agrandie, peut présenter des propriétés catalytiques uniformes et peut présenter une efficacité, une résistance et une homogénéité élevées dans la fabrication de combustible à base d'hydrogène.
PCT/KR2018/016087 2017-11-15 2018-12-18 Catalyseur pour réaction de dégagement d'hydrogène comprenant un promoteur de cuivre WO2019146913A1 (fr)

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KR20170152648 2017-11-15
KR20170152647 2017-11-15
KR1020180010599A KR102080027B1 (ko) 2017-11-15 2018-01-29 구리 프로모터를 포함하는 수소발생 반응용 촉매
KR10-2018-0010599 2018-01-29

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KR102497165B1 (ko) 2020-10-06 2023-02-09 한국과학기술원 전이금속 붕화물 복합체, 이의 제조방법 및 상기 전이금속 붕화물 복합체를 포함하는 수소발생반응용 촉매

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KR20090012525A (ko) * 2007-07-30 2009-02-04 삼성에스디아이 주식회사 전자 방출원, 전자 방출 소자 및 전자 방출원의 제조 방법
US20170226040A1 (en) * 2014-08-06 2017-08-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method for producing an adsorbent from organometallic framework structures (mof)
KR20160047045A (ko) * 2014-10-21 2016-05-02 서울대학교산학협력단 산소 발생 촉매, 전극 및 전기화학반응 시스템
KR20170055082A (ko) * 2015-11-10 2017-05-19 성균관대학교산학협력단 전자방출 물질 및 이의 제조방법
KR20170055622A (ko) * 2015-11-11 2017-05-22 성균관대학교산학협력단 전도성 고분자로 안정화된 전자화물 및 그 제조방법

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