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WO2017151003A1 - Matériau composite pour des éléments combustibles basse température et procédé de fabrication - Google Patents

Matériau composite pour des éléments combustibles basse température et procédé de fabrication Download PDF

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Publication number
WO2017151003A1
WO2017151003A1 PCT/RU2016/000111 RU2016000111W WO2017151003A1 WO 2017151003 A1 WO2017151003 A1 WO 2017151003A1 RU 2016000111 W RU2016000111 W RU 2016000111W WO 2017151003 A1 WO2017151003 A1 WO 2017151003A1
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Prior art keywords
membrane
platinum
acid
membranes
composite material
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PCT/RU2016/000111
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English (en)
Russian (ru)
Inventor
Евгений Александрович САНГИНОВ
Екатерина Викторовна ЗОЛОТУХИНА
Юрий Анатольевич ДОБРОВОЛЬСКИЙ
Сергей Иванович НЕФЕДКИН
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At Energy LLC
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At Energy LLC
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Priority to PCT/RU2016/000111 priority Critical patent/WO2017151003A1/fr
Publication of WO2017151003A1 publication Critical patent/WO2017151003A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • H01M8/1018—Polymeric electrolyte materials
    • H01M8/102—Polymeric electrolyte materials characterised by the chemical structure of the main chain of the ion-conducting polymer
    • H01M8/103—Polymeric electrolyte materials characterised by the chemical structure of the main chain of the ion-conducting polymer having nitrogen, e.g. sulfonated polybenzimidazoles [S-PBI], polybenzimidazoles with phosphoric acid, sulfonated polyamides [S-PA] or sulfonated polyphosphazenes [S-PPh]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • H01M8/1018—Polymeric electrolyte materials
    • H01M8/1041—Polymer electrolyte composites, mixtures or blends
    • H01M8/1046—Mixtures of at least one polymer and at least one additive
    • H01M8/1048—Ion-conducting additives, e.g. ion-conducting particles, heteropolyacids, metal phosphate or polybenzimidazole with phosphoric acid
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • H01M8/1018—Polymeric electrolyte materials
    • H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
    • 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
    • Y02E60/50—Fuel cells
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to composite polymer membranes based on perfluorinated sulfation cation exchange membranes modified with inorganic inclusion particles to increase the moisture content and self-humidification of the membrane, as well as to methods for producing modified polymer membranes intended for use in low-temperature solid polymer fuel cells.
  • POMs proton exchange membranes
  • FCs fuel cells
  • electrochemical sensors [Nagarale RK, Gohil GS, Shahi VK Advances In Colloid And Interface Science, 1 19 (2006) 97; Yaroslavtsev A.B., Dobrovolsky Yu.A., Shaglaeva HC, Frolova L.A., Gerasimova E.V., Sanginov E.A. Advances in Chemistry, 81 (2012), 191].
  • POM performs three Role: it provides proton transport from the anode region to the cathode region, separation of reacting gases, plays the role of an electronic insulator, which defines a wide range of requirements for such membranes: high proton conductivity, thermal and chemical resistance, high mechanical strength, low permeability of methanol and hydrogen.
  • POMs perforated sulfonation cation exchange membranes of the Nafion type from Du Pont, as described, for example, in US Pat. No. 4,330,654 and representing a copolymer of tetrafluoroethylene and perforated ether with a sulfo group.
  • the main advantages of such membranes are chemical and thermal stability due to the perforated structure, high proton conductivity achieved at high moisture content, and strength characteristics.
  • a number of disadvantages such as the unsatisfactory characteristics of proton transport during low moisture content and high values of membrane permeability for fuel (hydrogen and methanol) limit their practical application.
  • the drying of the membrane during the operation of the FC is the most critical, since in addition to the deterioration of power characteristics, it leads to chemical and mechanical destruction of the membrane.
  • the reactant gases are humidified before they enter the cell (for example, US Pat. No. 6,403,249) or with water produced during reactions in the fuel cell (US Pat. No. 6,207,312 )
  • the external humidification system significantly complicates the design of the fuel cell, increases the cost and reduces its energy efficiency.
  • inorganic additives which are most often used as oxide and salt systems that firmly retain adsorbed water (oxides of silicon, titanium, zirconium, aluminum, zeolites, etc.) and inorganic solid proton-conducting electrolytes (most often heteropoly acids and their salts, zirconium phosphates, cesium hydrosulfate) [for example, Thiam HS, Daud WRW, Kamarudin SK et al. Int. J.
  • Hydrogen Energy 36 (201 1) 3187, Yaroslavtsev A.B., Dobrovolsky Yu.A., Shaglaeva H.C., Frolova L.A., Gerasimova E.V., Sanginov E.A. Advances in Chemistry 81 (2012) 191, EP 0926754, US 20050175880, US 5.523, 181, US 6.902.839, US 2005/0053821, RF 2,352,384, RF 2,400,294] or polymer inclusions with additional polar centers (for example, polyaniline, polyvinyl alcohol, sulfosallicylic acid ) [RF 2,400,294, RF 2,428,767].
  • additional polar centers for example, polyaniline, polyvinyl alcohol, sulfosallicylic acid
  • 2012 / 0052407A1 describes Nafion-based composite membranes doped with a catalyst (Ag, Pd, Ru, and combinations thereof) promoting the decomposition of hydrogen peroxide and oxides (Ti, Zr, Nb, Ru).
  • a catalyst Al, Pd, Ru, and combinations thereof
  • a self-moistening membrane described in U.S. Pat. No. 7,993,791 B2 and comprising a proton conductive polymer, including perfluorinated sulfonic acids, a catalyst promoting a hydrogen oxidation reaction and a hygroscopic substance (including, for example, zinc chloride, calcium chloride or calcium bromide, chloride or acetate or magnesium sulfate, lithium chloride, bisphosphate or acetate or silicate potassium, acetate or sodium silicate, cobalt chloride, silica gel, etc.).
  • a proton conductive polymer including perfluorinated sulfonic acids, a catalyst promoting a hydrogen oxidation reaction and a hygroscopic substance (including, for example, zinc chloride, calcium chloride or calcium bromide, chloride or acetate or magnesium sulfate, lithium chloride, bisphosphate or acetate or silicate potassium, acetate or sodium silicate, cobalt chloride, silica
  • the membrane may contain solid inorganic acids selected from the series: zirconium and titanium oxophosphates, zirconium and titanium sulfates, boron phosphate, silica with grafted acid groups and mixtures based on them.
  • the disadvantage of the prototype is the presence of hygroscopic salts, the cations of which are easily exchanged with sulfocationic groups and can lead to blocking of proton transport.
  • the above solid inorganic acids in comparison with heteropoly compounds, have no or low catalytic activity in electrochemical processes.
  • heteropoly acids in particular phosphor tungsten and phosphoform molybdenum acids, are record holders among solid proton conductivity electrolytes at room temperature.
  • a method for the synthesis of composite membranes consists in mixing solutions or suspensions of POM and the added additives, followed by watering, which leads to a low technological process and deterioration of the stability of swollen membranes (up to dissolution), since it requires the preparation and use of an aqueous dispersion of sulfocationite ionomer.
  • the general objective of the proposed group of inventions is the development of new membranes and a method for their preparation, namely, an in situ method for the modification of solid perfluorinated sulfation cation exchange membranes of the National type by particles of inorganic inclusions (platinum and heteropoly acid) by chemical deposition to obtain a hybrid membrane (composite) material with improved moisture content, specific proton conductivity and thermal stability, the ability to self-humidify in a hydrogen-air fuel cell.
  • the overall technical result achieved by the implementation of the group of inventions is to increase the specific proton conductivity of a polyelectrolyte membrane, which significantly exceeds the conductivity of membranes containing only platinum and only polyacid, increasing its thermal stability at relatively low humidity, the ability to self-humidify in a hydrogen-air fuel cell .
  • the novelty of this solution is the joint use of platinum and heteropoly acid particles in a solid membrane, which leads to a synergistic effect in proton conductivity under the conditions of operation of a fuel cell.
  • the sequence and set of operations for producing a composite membrane are new.
  • the thermal stability of the modified membrane is increased compared to unmodified.
  • a membrane modified by this method retains the ability to proton conductivity due to the synergy of the effects of self-humidification in the presence of particles of platinum and heteropoly acid. Besides Moreover, the additional electrocatalytic activity of heteropoly compounds leads to an additional increase in conductivity.
  • the modification procedure consists of two main parts: the modification of the membrane with platinum and the subsequent modification of the resulting platinum-containing membrane with a heteropoly acid.
  • This order of introducing the components is due to the fact that to reduce platinum it is required to use a reducing agent with an alkaline reaction of the medium in the solution of which the heteropoly acid will be unstable.
  • a Nafion-211 membrane is used as a starting membrane for producing a composite material.
  • the introduction of platinum in the Nafion-211 membrane is carried out by chemical precipitation, which includes saturation of the membrane with a platinum precursor and subsequent reduction to metal particles.
  • the saturation of the membrane with a solution of platinum tetraammonium dichloride dichloride (II) is carried out under stationary conditions during the day to complete ion exchange at room temperature.
  • the reduction is carried out in a 10-fold excess of NaBH 4 relative to the total exchange capacity of the membrane at the doubly charged cation until gas evolution ceases. Saturation and reduction alternate with washing the membrane with distilled water from an irreplaceably absorbed electrolyte and recovery by-products.
  • the finished modified membrane is transferred to the initial H + form with 0.1 M sulfuric acid and then the membrane is repeatedly washed with water.
  • concentration of saturation solutions of platinum tetraammonium dichloride dichloride (II) was selected to achieve a platinum metal content in the membrane of 0.01-2%.
  • the optimal platinum content in the Nafion-21 1 membrane was 0.2 wt.%, Achieved by immersing it in a solution of 0.026 mM platinum (II) tetraammonium dichloride. An increase in the platinum content in the membrane is impractical because of its mechanical embrittlement.
  • heteropoly acids into the modified platinum membrane is as follows.
  • the membrane is placed in a water-alcohol solution of heteropoly acid and incubated for two days.
  • the nature of alcohol from Some methanol, ethanol, isopropanol practically do not affect the degree of heteropoly acid incorporation.
  • the optimal solvent composition water - ethanol in a ratio of 1: 1 for irrigation membranes and pure ethanol for extrusion membranes.
  • As the heteropoly acid it is most optimal to use phosphoric tungsten, phosphoromolybdenum and silicotungsten acids, with a concentration of 2 g per 10 ml of solvent.
  • the membrane is thoroughly crimped with filter paper and dried.
  • the membrane is pre-incubated in an atmosphere of air with a humidity of 75% rel. and placed in a desiccator with P2O5.
  • the effect of the composition of the Nafion-211 composite membrane on the specific proton conductivity of the membrane was determined by measuring the impedance spectra in a cell of ElectroChem, Inc.
  • the active area of the cell was 1 cm 2 , gas flows were supplied from both sides: air (7.2 l / h), hydrogen (7.2 l / h).
  • As the electrodes Toray TGP-H-060T porous carbon paper (Toray Industries, Inc.) was used, the conductivity of which in the direction perpendicular to the plane is 12.5 S / cm.
  • the impedance spectra were measured in the frequency range 3 MHz - 100 Hz (impedance meter Z-3000, LLC "Eline", Russia) with an open circuit potential of 100-800 mV and at zero potential.
  • a number of samples were selected with different contents of the modifying component: 0.01, 0.05, 0.2 and 1, 2, 3% wt.% Pt and 0.01, 0.05, 0.5 and 3, 6, 8 wt.% Phosphoric tungsten acid.
  • the Nafion-2 1 proton exchange membrane was used for the manufacture of a composite membrane.
  • I prepared a series of membranes with different amounts of additives.
  • the initial proton exchange membrane was treated with a solution of platinum (II) tetraammonia for 2 hours.
  • the concentration of the solution was calculated in such a way as to obtain membranes with a platinum content of 0.01, 0.05, 0.2, and 1, 2, 3 wt.% Of the mass of the original membrane.
  • platinum (II) tetraammonium After saturation of the initial membrane with platinum (II) tetraammonium, it was reduced with sodium borohydride to platinum metal.
  • the resulting membrane doped with platinum particles was converted into a proton-conducting form by treatment with sulfuric acid, after which it was treated with a 2 molar aqueous-alcoholic solution of phosphoric tungsten acid, so as to obtain membranes containing 0.01, 0.05, 0.2, and 1, 2, 3% wt.% heteropoly acids by weight original membrane. After saturation of the membrane with phosphoric tungsten acid, it was dried in a dry heat oven at a temperature of 60 ° C.
  • membranes modified only with platinum or only heteropoly acid were prepared.
  • the methods described above were used for the synthesis.
  • GPS more than 6% and platinum more than 2% practically does not lead to a further increase in membrane conductivity.
  • the content of both GPS and platinum is less than 0.01%; such low amounts of modifying components do not increase the membrane conductivity.
  • the platinum content in the membrane is more than 0.2%, its embrittlement is observed. With a platinum content of more than 2%, the use of a membrane for practical use becomes impossible due to its high fragility.
  • the most optimal contents of the modifying components for the modification of sulfocationic membranes are: heteropoly acid: 0.01-6 mass. % and platinum: 0.01-2%.
  • the specific proton conductivity of a composite membrane containing both heteropoly acid and platinum is 7.8 times higher than the unmodified conductivity, while the specific proton conductivity of composite membranes containing only platinum or heteropoly acid is only 2.2 and 2.9 times higher than unmodified conductivity, respectively.
  • the synergistic effect is explained, inter alia, by the sequence of the introduction of additives into the membrane.
  • the introduction of heteropoly acids after the introduction of platinum provides an increased concentration of heteropoly acids near platinum nanoparticles.
  • This combination of platinum and heteropolyacids provides water to platinum particles during the reaction of hydrogen with oxygen and the retention of the resulting water at a heteropoly acid.
  • the conductivity and mechanical integrity of the modified Nation platinum and heteropoly acid membrane is maintained at a relative humidity of 32% to a temperature of 80 ° C, while for an unmodified Nafion-211 membrane at 60 ° C, breakdown occurs due to mechanical degradation.
  • the new composite membrane material obtained by chemical modification of a perfluorinated sulfocationic membrane which is a copolymer of tetrafluoroethylene and perfluorinated ether with a sulfo group, metal particles (platinum) and heteropoly acid, has improved proton conductivity, thermal stability and the ability to self-humidify in dry flow conditions hydrogen and air.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Fuel Cell (AREA)

Abstract

L'invention se rapporte au domaine des membranes polymères composites à base de membranes perfluorées à échange de cations de soufre modifiées à l'aide de particules à inclusion inorganique pour augmenter le contenu en humidité et l'auto-humidification de la membrane, ainsi que des procédés de production de membranes polymères modifiées utilisées dans des éléments combustibles basse température en polymères solides. Ce matériau composite pour des éléments combustibles basse température se compose d'une membrane à échange de protons comprenant une membrane perforée à échange de cations de soufre perfluorée qui consiste en un copolymère de tétrafluoroéthylène et un éther perfluoré avec un groupe sulfure comprenant du latine dans une quantité de 0,01-2 en % poids et un hétéropolyacide dans une quantité de 0,01-6 en % poids, dans lequel on utilise de préférence en qualité d'hétéropolyacides un acide phosphorique de tungstène, un acide phosphorique de molybdène, un acide silicique de tungstène ou une quelconque de leur combinaisons possibles. Ce matériau composite est obtenu grâce à un procédé dans lequel on effectue successivement les étapes suivantes: on dépose le platine sur une membrane solide par introduction par échange d'ions de tétra-ammoniac de platine (II) dans la membrane, suivi de la réduction du platine en particules métalliques avec de tetrahydruroborate de sodium, on fait passer la membrane sous une forme Н+, on maintient la membrane dans une solution eau-alcool d'hétéropolyacide et on procède au séchage.
PCT/RU2016/000111 2016-03-02 2016-03-02 Matériau composite pour des éléments combustibles basse température et procédé de fabrication Ceased WO2017151003A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110137470A (zh) * 2019-05-15 2019-08-16 华南理工大学 一种氟基离子液体表面修饰锂离子电池三元正极材料的方法
CN113823819A (zh) * 2021-06-26 2021-12-21 中国科学院深圳先进技术研究院 全氟磺酸/耦合磷钨酸木质素涂膜液、离子交换膜及制备方法
RU2851589C1 (ru) * 2024-12-18 2025-11-25 Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) Полимерный протонпроводящий композит и способ его получения

Citations (4)

* Cited by examiner, † Cited by third party
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US7993791B2 (en) * 2005-10-26 2011-08-09 Nanotek Instruments, Inc. Self-humidifying proton exchange membrane, membrane-electrode assembly, and fuel cell
CN103887536A (zh) * 2014-03-13 2014-06-25 清华大学 一种无机材料杂化的聚苯并咪唑质子交换膜的制备方法
CN104701560A (zh) * 2015-02-05 2015-06-10 成都新柯力化工科技有限公司 一种燃料电池质子交换膜及其制备方法
CN105355939A (zh) * 2015-11-26 2016-02-24 辽宁科技大学 一种用于燃料电池的质子交换膜及其制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7993791B2 (en) * 2005-10-26 2011-08-09 Nanotek Instruments, Inc. Self-humidifying proton exchange membrane, membrane-electrode assembly, and fuel cell
CN103887536A (zh) * 2014-03-13 2014-06-25 清华大学 一种无机材料杂化的聚苯并咪唑质子交换膜的制备方法
CN104701560A (zh) * 2015-02-05 2015-06-10 成都新柯力化工科技有限公司 一种燃料电池质子交换膜及其制备方法
CN105355939A (zh) * 2015-11-26 2016-02-24 辽宁科技大学 一种用于燃料电池的质子交换膜及其制备方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110137470A (zh) * 2019-05-15 2019-08-16 华南理工大学 一种氟基离子液体表面修饰锂离子电池三元正极材料的方法
CN113823819A (zh) * 2021-06-26 2021-12-21 中国科学院深圳先进技术研究院 全氟磺酸/耦合磷钨酸木质素涂膜液、离子交换膜及制备方法
RU2851589C1 (ru) * 2024-12-18 2025-11-25 Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) Полимерный протонпроводящий композит и способ его получения
RU2852054C1 (ru) * 2024-12-18 2025-12-02 Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) Протонпроводящий гетерогенный полимерный композит и способ его получения
RU2852053C1 (ru) * 2024-12-18 2025-12-02 Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) Гетерогенная протонпроводящая полимерная композиция и способ ее получения

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