WO2018097069A1 - Électrode destinée à l'électrolyse - Google Patents

Électrode destinée à l'électrolyse Download PDF

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Publication number
WO2018097069A1
WO2018097069A1 PCT/JP2017/041559 JP2017041559W WO2018097069A1 WO 2018097069 A1 WO2018097069 A1 WO 2018097069A1 JP 2017041559 W JP2017041559 W JP 2017041559W WO 2018097069 A1 WO2018097069 A1 WO 2018097069A1
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WIPO (PCT)
Prior art keywords
electrolysis
electrode
catalyst layer
ruthenium
mol
Prior art date
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PCT/JP2017/041559
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English (en)
Japanese (ja)
Inventor
豊光 宮阪
誠 西澤
佳典 角
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旭化成株式会社
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Filing date
Publication date
Application filed by 旭化成株式会社 filed Critical 旭化成株式会社
Priority to KR1020197013662A priority Critical patent/KR102272749B1/ko
Priority to ES17873862T priority patent/ES2850501T3/es
Priority to RU2019115501A priority patent/RU2720309C1/ru
Priority to US16/462,367 priority patent/US20190338429A1/en
Priority to CN201780066562.8A priority patent/CN109891002B/zh
Priority to JP2018552551A priority patent/JP6670948B2/ja
Priority to BR112019010219A priority patent/BR112019010219A2/pt
Priority to EP17873862.1A priority patent/EP3546619B1/fr
Publication of WO2018097069A1 publication Critical patent/WO2018097069A1/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
    • 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
    • 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
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • 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
    • C25B11/093—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 at least one noble metal or noble metal oxide and at least one non-noble metal oxide
    • 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
    • C25B11/097—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 comprising two or more noble metals or noble metal alloys
    • 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
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • 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
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • 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
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
    • 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
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
    • C25B9/23—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms comprising ion-exchange membranes in or on which electrode material is embedded

Definitions

  • Ion exchange membrane method salt electrolysis is a method for producing caustic soda, chlorine, and hydrogen by electrolyzing (electrolyzing) salt water using an electrode for electrolysis.
  • a technique capable of maintaining a low electrolysis voltage over a long period of time is required in order to reduce power consumption.
  • a breakdown of the breakdown of the electrolysis voltage reveals that, in addition to the theoretically required electrolysis voltage, the voltage resulting from the resistance of the ion exchange membrane and the structure resistance of the electrolytic cell, the overvoltage of the anode and cathode as electrolysis electrodes, the anode and cathode It has been clarified that a voltage or the like due to the distance between is included. Further, when electrolysis is continued for a long period of time, a voltage increase or the like caused by various causes such as impurities in salt water may occur.
  • the first transition metal element includes at least one metal element selected from the group consisting of vanadium, cobalt, copper, and zinc.
  • the content of the first transition metal element with respect to all the metal elements contained in the catalyst layer is 10 mol% or more and 30 mol% or less.
  • the catalyst layer of the present embodiment includes the first transition metal element together with the above-described ruthenium element, iridium element, and titanium element.
  • the presence form of the first transition metal element is not particularly limited.
  • the first transition metal element may be in the form of an oxide, a simple metal, or an alloy, as long as it is contained in the catalyst layer.
  • the first transition metal element preferably forms a solid solution with a solid solution of ruthenium oxide, iridium oxide, and titanium oxide.
  • the formation of such a solid solution can be confirmed by, for example, XRD.
  • said solid solution can be formed by adjusting the calcination temperature at the time of forming a catalyst layer, the addition amount of a 1st transition metal element, etc. to an appropriate range.
  • the first transition metal element preferably contains a metal element selected from the group consisting of vanadium, cobalt, copper, and zinc from the viewpoint of compatibility between the voltage and durability of the catalyst layer. More preferably, the metal element contains a vanadium element.
  • Example a Electrode for Electrolysis with V / Ti Charge Ratio of 0.11
  • the element ratio (molar ratio) of ruthenium, iridium, titanium, and vanadium was 23.75: 23.75: 47.5: 5, respectively.
  • the electrode for electrolysis obtained by the method similar to Example 1 mentioned later except having applied to the electroconductive base material using the coating liquid a prepared so that it might become.
  • the D value as an index of the electric double layer capacity is a value calculated using the concept of electric double layer capacity, and the surface area of the electrode (that is, the specific surface area of the catalyst layer on the electrode) is large.
  • the value is expected to increase.
  • the D value can be set to the above-described range by adjusting the content of the first transition metal element to the above-described preferable range.
  • the D value tends to increase by increasing the content of the first transition metal element.
  • the D value tends to decrease by increasing the firing temperature (post-bake temperature) when forming the catalyst layer.
  • the thickness of the catalyst layer is preferably 0.1 to 5 ⁇ m, and more preferably 0.5 to 3 ⁇ m.
  • a preferred aspect of the method for producing an electrode for electrolysis according to the present embodiment includes a step of preparing a coating liquid containing a ruthenium compound, an iridium compound, a titanium compound, and a compound containing a first transition metal element; It is preferable to have a step of coating the liquid on at least one surface of the conductive substrate to form a coating film; and a step of baking the coating film in an oxygen-containing atmosphere to form a catalyst layer.
  • the ruthenium compound, the iridium compound, the titanium compound, and the compound containing the first transition metal element correspond to the precursor containing the metal element contained in the catalyst layer in the present embodiment.
  • the ruthenium compound, the iridium compound, and the titanium compound may be oxides, but are not necessarily oxides.
  • a metal salt or the like may be used.
  • these metal salts include, but are not limited to, any one selected from the group consisting of chloride salts, nitrates, dinitrodiammine complexes, nitrosyl nitrates, sulfates, acetates, and metal alkoxides.
  • the metal salt of the ruthenium compound is not limited to the following, and examples thereof include ruthenium chloride and ruthenium nitrate.
  • the metal salt of the iridium compound examples include, but are not limited to, iridium chloride and iridium nitrate. Although it does not limit to the following as a metal salt of a titanium compound, For example, titanium tetrachloride etc. are mentioned.
  • the compound containing the first transition metal element may be an oxide, but is not necessarily an oxide.
  • the oxo acid of vanadium and the salt thereof; vanadium chloride; and one or more selected from the group consisting of vanadium nitrate are preferable.
  • Examples of the counter cation in the oxo acid salt include, but are not limited to, Na + , K + , Ca 2+ and the like.
  • Such compounds include oxoacids or salts thereof such as sodium metavanadate, sodium orthovanadate, potassium orthovanadate and the like; chlorides such as vanadium chloride and the like; , Vanadium nitrate, and the like.
  • the above compounds are appropriately selected and used according to the desired metal element ratio in the catalyst layer.
  • the coating liquid may further contain a compound other than the compounds contained in the above-described compound. Examples of other compounds include, but are not limited to, metal compounds containing metal elements such as tantalum, niobium, tin, platinum, and rhodium; organics containing metal elements such as tantalum, niobium, tin, platinum, and rhodium Compounds and the like.
  • the coating liquid is preferably a liquid composition in which the above compound group is dissolved or dispersed in an appropriate solvent.
  • the solvent for the coating solution used here can be selected according to the type of the compound. For example, water; alcohols such as butanol can be used.
  • the total compound concentration in the coating solution is not particularly limited, but is preferably 10 to 150 g / L from the viewpoint of appropriately controlling the thickness of the catalyst layer.
  • the method of coating the coating liquid on the surface of the conductive substrate is not limited to the following, but, for example, a dipping method in which the conductive substrate is immersed in the coating liquid, or coating on the surface of the conductive substrate.
  • An electrocoating method or the like can be used.
  • the roll method and the electrostatic coating method are preferable from the viewpoint of excellent industrial productivity.
  • a coating film of the coating liquid can be formed on at least one surface of the conductive substrate.
  • the firing temperature can be appropriately selected depending on the composition of the coating liquid and the solvent type.
  • the firing temperature is preferably 300 to 650 ° C.
  • the precursor such as ruthenium compound is not sufficiently decomposed, and a catalyst layer containing ruthenium oxide or the like may not be obtained.
  • the firing temperature exceeds 650 ° C., the conductive base material may be oxidized, so that the adhesion at the interface between the catalyst layer and the base material may be lowered. This tendency should be emphasized particularly when a titanium substrate is used as the conductive substrate. A longer firing time is preferred.
  • the above-mentioned steps of coating, drying and firing the catalyst layer can be repeated a plurality of times to form the catalyst layer in a desired thickness.
  • firing can be performed for a longer time if necessary to further improve the stability of the catalyst layer that is extremely chemically, physically and thermally stable.
  • the conditions for the long-term firing are preferably about 30 minutes to 4 hours at 400 to 650 ° C.
  • the electrode for electrolysis of this embodiment has a low overvoltage even in the initial stage of electrolysis, and can be electrolyzed with a low voltage and low power consumption over a long period. Therefore, it can be used for various electrolysis.
  • it is preferably used as an anode for chlorine generation, and more preferably used as an anode for salt electrolysis in the ion exchange membrane method.
  • FIG. 1 shows a schematic sectional view according to an example of the electrolytic cell of the present embodiment.
  • an aqueous alkali chloride solution such as a 2.5 to 5.5 N (N) aqueous sodium chloride solution (saline solution) or an aqueous potassium chloride solution is provided.
  • aqueous alkali hydroxide aqueous solution for example, sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, etc.
  • water can be used.
  • the structure of the electrolytic cell of this embodiment is not specifically limited, A monopolar type or a bipolar type may be sufficient.
  • the material constituting the electrolytic cell is not particularly limited.
  • the material for the anode chamber is preferably titanium or the like resistant to alkali chloride and chlorine; the material for the cathode chamber is resistant to alkali hydroxide and hydrogen. Nickel or the like is preferred.
  • the electrode for electrolysis (anode 230) of the present embodiment may be disposed with an appropriate interval between the electrode and the ion exchange membrane 250, or even if it is disposed in contact with the ion exchange membrane 250, there is no problem.
  • the cathode 240 may be arranged with an appropriate interval from the ion exchange membrane 250, or even if it is a contact type electrolytic cell (zero gap type electrolytic cell) with no gap between the ion exchange membrane 250, Can be used without any problems.
  • the electrolysis conditions of the electrolytic cell of the present embodiment are not particularly limited, and can be operated under known conditions. For example, it is preferable to perform electrolysis by adjusting the electrolysis temperature to 50 to 120 ° C. and the current density to 0.5 to 10 kA / m 2 .
  • an electrolytic cell comprising an anode cell having an anode chamber and a cathode cell having a cathode chamber was prepared.
  • a nickel wire mesh base material coated with a ruthenium oxide catalyst was used as the cathode.
  • an expanded base material made of metallic nickel as a current collector was cut out and welded at the same size as the anode, and then a cushion mat knitted with nickel wire was placed on it.
  • a cathode was placed.
  • a rubber gasket made of EPDM (ethylene propylene diene) was used as the gasket, and an ion exchange membrane was sandwiched between the anode cell and the cathode cell.
  • a cation exchange membrane “Aciplex” (registered trademark) F6801 (manufactured by Asahi Kasei Co., Ltd.) for salt electrolysis was used.
  • the overvoltage and the electrolysis voltage were measured after 7 days from the start of electrolysis.
  • the electrolysis conditions were a current density of 6 kA / m 2 , a salt water concentration of 205 g / L in the anode cell, a NaOH concentration of 32% by mass in the cathode cell, and a temperature of 90 ° C.
  • PAD36-100LA manufactured by Kikusui Electronics Co., Ltd.
  • aqueous iridium chloride solution manufactured by Tanaka Kikinzoku Co., Ltd., iridium concentration 100 g / L
  • Vanadium chloride (III) manufactured by Kishida Chemical Co., Ltd.
  • the above-mentioned cycle comprising roll coating, drying and firing is repeated 3 times by raising the firing temperature to 450 ° C., and finally by further firing for 1 hour at 520 ° C.
  • a black-brown catalyst layer was formed thereon to produce an electrode for electrolysis.
  • Example 8 The use of an aqueous ruthenium chloride solution (manufactured by Tanaka Kikinzoku Co., Ltd., ruthenium concentration 100 g / L) instead of an aqueous ruthenium nitrate solution, and an element ratio (molar ratio) of ruthenium, iridium, titanium, and vanadium of 19.6: 20.2: 47 .09: 13.11
  • the coating liquid A8 prepared so as to be 1311. 11 was applied to the conductive substrate, and the cycle consisting of roll coating, drying, and firing was performed from the first to the eighth firing.
  • An electrode for electrolysis was produced in the same manner as in Example 1 except that the temperature was set to 393 ° C. and then baking was performed at 485 ° C. for 1 hour.
  • Example 9 Use of ruthenium chloride aqueous solution (Tanaka Kikinzoku Co., Ltd., ruthenium concentration 100 g / L) instead of ruthenium nitrate aqueous solution, and cobalt (II) chloride hexahydrate (manufactured by Wako Pure Chemical Industries) instead of vanadium (III) chloride Coating the conductive substrate using the coating liquid A9 prepared so that the elemental ratio (molar ratio) of ruthenium, iridium, titanium and cobalt is 50: 3: 30: 17; and The cycle consisting of roll coating, drying and firing was carried out at a first firing temperature of 440 ° C., then heated to 475 ° C. and repeated three more times, and finally fired at 520 ° C. for 1 hour. Except for this, an electrode for electrolysis was produced in the same manner as in Example 1.

Abstract

L'invention concerne une électrode destinée à l'électrolyse équipée d'un matériau de base conducteur et d'une couche de catalyseur qui est formée sur la surface du matériau de base conducteur. La couche de catalyseur contient du ruthénium élémentaire, de l'iridium élémentaire, du titane élémentaire et au moins un premier élément métal de transition choisi dans le groupe constitué du Sc, du V, du Cr, du Fe, du Co, du Ni, du Cu et du Zn ; le rapport de teneur du premier élément métal de transition contenu dans la couche de catalyseur par rapport à 1 mole du titane élémentaire est supérieur ou égal à 0,25 % en mole, mais est inférieur à 3,4 % en mole ; et la valeur D servant d'indice de la capacité électrique double couche de cette électrode destinée à l'électrolyse est comprise entre 120 C/m2 et 420 C/m2 (inclus).
PCT/JP2017/041559 2016-11-22 2017-11-17 Électrode destinée à l'électrolyse WO2018097069A1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
KR1020197013662A KR102272749B1 (ko) 2016-11-22 2017-11-17 전해용 전극
ES17873862T ES2850501T3 (es) 2016-11-22 2017-11-17 Electrodo para electrólisis
RU2019115501A RU2720309C1 (ru) 2016-11-22 2017-11-17 Электрод для электролиза
US16/462,367 US20190338429A1 (en) 2016-11-22 2017-11-17 Electrode for electrolysis
CN201780066562.8A CN109891002B (zh) 2016-11-22 2017-11-17 电解用电极
JP2018552551A JP6670948B2 (ja) 2016-11-22 2017-11-17 電解用電極
BR112019010219A BR112019010219A2 (pt) 2016-11-22 2017-11-17 eletrodo para eletrólise, método para produzir o eletrodo para eletrólise, e, eletrolisador.
EP17873862.1A EP3546619B1 (fr) 2016-11-22 2017-11-17 Électrode destinée à l'électrolyse

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2016-227066 2016-11-22
JP2016227066 2016-11-22

Publications (1)

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WO2018097069A1 true WO2018097069A1 (fr) 2018-05-31

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US (1) US20190338429A1 (fr)
EP (1) EP3546619B1 (fr)
JP (1) JP6670948B2 (fr)
KR (1) KR102272749B1 (fr)
CN (1) CN109891002B (fr)
BR (1) BR112019010219A2 (fr)
ES (1) ES2850501T3 (fr)
RU (1) RU2720309C1 (fr)
TW (1) TWI661091B (fr)
WO (1) WO2018097069A1 (fr)

Cited By (2)

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WO2023249011A1 (fr) * 2022-06-20 2023-12-28 旭化成株式会社 Électrode d'électrolyse et réservoir d'électrolyse
JP7434828B2 (ja) 2019-11-21 2024-02-21 中国電力株式会社 水素含有水生成装置、及び電極交換時期の予測方法

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KR102017567B1 (ko) * 2018-11-27 2019-09-03 주식회사 웨스코일렉트로드 전해 제련용 전극 조립체
CN110438527A (zh) * 2019-08-05 2019-11-12 上海氯碱化工股份有限公司 过渡金属掺杂的含钌涂层阳极的制备方法
WO2021108461A1 (fr) * 2019-11-25 2021-06-03 The Regents Of The University Of California Électrocatalyseur amorphe à base d'iridium et synthèse dudit électrocatalyseur
KR102424607B1 (ko) * 2020-08-11 2022-07-25 울산과학기술원 금속 복합체 및 이의 제조방법
CN112195482B (zh) * 2020-10-15 2023-05-16 昆明冶金研究院有限公司 一种复合钛阳极板及其制备方法
CN112458495B (zh) * 2020-11-27 2022-05-10 浙江大学衢州研究院 一种钌基过渡金属氧化物固溶体的电催化剂及其制备方法和应用

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US20190338429A1 (en) 2019-11-07
EP3546619A1 (fr) 2019-10-02
TW201819687A (zh) 2018-06-01
CN109891002A (zh) 2019-06-14
BR112019010219A2 (pt) 2019-08-27
TWI661091B (zh) 2019-06-01
JP6670948B2 (ja) 2020-03-25
CN109891002B (zh) 2021-03-12
KR102272749B1 (ko) 2021-07-06
RU2720309C1 (ru) 2020-04-28
JPWO2018097069A1 (ja) 2019-07-25
KR20190067859A (ko) 2019-06-17
EP3546619A4 (fr) 2019-12-25
EP3546619B1 (fr) 2021-01-06

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