CN104124463A - Ionic liquid-polymer composite membrane for hydrogen chloride fuel cell and preparation and application thereof - Google Patents

Ionic liquid-polymer composite membrane for hydrogen chloride fuel cell and preparation and application thereof Download PDF

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Publication number
CN104124463A
CN104124463A CN201310150325.3A CN201310150325A CN104124463A CN 104124463 A CN104124463 A CN 104124463A CN 201310150325 A CN201310150325 A CN 201310150325A CN 104124463 A CN104124463 A CN 104124463A
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ionic liquid
polymer
composite membrane
fuel cell
preparation
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周利
刘飒
王鹏杰
邵志刚
衣宝廉
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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

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  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Fuel Cell (AREA)

Abstract

A preparation method of an ionic liquid-polymer composite membrane for a hydrogen chloride fuel cell comprises the following steps: a high molecular polymer substrate and an ionic liquid are dissolved in an organic solvent to prepare a membrane preparing liquid, then the ionic liquid-polymer composite membrane is prepared by a casting method, and during the method, a feed gas is in no need of humidifying. The prepared composite membrane has the advantages of high conductivity, low permeability and the like. The hydrogen chloride fuel cell prepared by use of the composite membrane can be stable in operation.

Description

Ionic liquid-composite membrane of polymer and preparation and application for hydrogen-chlorine fuel cell
Technical field
The present invention relates to a kind of feed gas does not need ionic liquid-composite membrane of polymer and preparation method thereof for hydrogen-chlorine fuel cell of humidification, is specifically related to a kind of castingization method that adopts and directly prepares the method for ionic liquid-composite membrane of polymer for hydrogen-chlorine fuel cell.
Background technology
Hydrogen-chlorine fuel cell using hydrogen as fuel, chlorine as oxidant, at anode, negative electrode place, there is electrochemical reaction respectively, the chemical energy being stored in wherein is directly changed into electric energy, generate hydrogen chloride simultaneously.Therefore need a kind of electrolyte membrance that cathode and anode is isolated.Proton exchange membrane (PEM) is one of core component of Proton Exchange Membrane Fuel Cells (PEMFC), desirable PEM should have that proton conductivity is high, gas and low, the high ion selectivity of Test Liquid Permeability of Core, sufficiently high mechanical strength, thermal stability and chemical stability, and there is suitable cost performance.
At present, the research of hydrogen-chlorine fuel cell is also in the exploratory stage, only there are 4 patent (USP4128701 both at home and abroad, CN86104831, CN1805196), and these patents are all the selection optimization about electrode materials such as battery system or catalyst, wherein electrolyte membrance adopts business Nafion film (USP4128701, JP3150803-U, CN1805196) or directly use the solution such as hydrochloric acid as electrolyte (CN86104831), do not have the research about newtype dielectric film, and the cell cathode side raw material of finding report mostly is liquid (chlorine is dissolved in hydrochloric acid), anode-side is hydrogen, this feeding manner easily causes the problems such as corrosion of material.Ionic liquid (ionic liquid) has thermal stability, chemical stability, low volatility, conductivity advantages of higher.Adopt ionic liquid as PEMFC electrolyte, can be so that battery move under humidification condition completely at middle high temperature (100-200 ° of C).
Summary of the invention
Object of the present invention, except providing a kind of hydrogen-chlorine fuel cell with ionic liquid-composite membrane of polymer, is also to provide a kind of casting method that adopts directly to prepare the preparation method of ionic liquid-composite membrane of polymer for hydrogen-chlorine fuel cell.
For achieving the above object, the technical solution used in the present invention can realize as follows: a kind of ionic liquid-composite membrane of polymer for hydrogen-chlorine fuel cell, and it is by high molecular polymer substrate and has composite proton conductive membranes prepared by the ionic liquid filler of proton conduction carrier; Ionic liquid mass fraction in polymeric substrates is 30-90wt.%.
High molecular polymer used is hydrogen chloride or chlorine to be had to poly-inclined to one side tetrafluoroethene (PVDF), Kynoar-hexafluoropropylene copolymer (PVDF-HFP) or the polybenzimidazoles (PBI) etc. of well tolerable property, and molecular weight is 10000-100000g mol -1;
Polysulfones is polysulfones or polyether sulfone etc., and molecular weight is 10000-100000g mol -1;
High boiling solvent used is the good solvent of high molecular polymer, is DMSO, DMF, DMAC or NMP;
Ionic liquid is mainly imidazoles or amine ionic liquid, as 1-ethyl-3-methylimidazole tetrafluoroborate ([EMIm] BF 4), 1-butyl-3-methylimidazole hexafluorophosphate ([BMIm] PF 6), 1-methyl-3-butyl sulfonic acid imidazole bisulfate ([BMIm] HSO 3hSO 4), Trimethylamine phosphoric acid hydrogen disalt ([tma] H 2pO 4), diethylmethyl amine trifluoromethyl sulfonic acid ([dema] TfO), Trimethylamine trifluoromethyl sulfonic acid ([tma] TfO) etc.
Described ionic liquid-composite membrane of polymer is even compact film, and ionic liquid is uniformly distributed.The preparation method of described composite membrane: high molecular polymer substrate and the ionic liquid filler with proton conduction carrier are dissolved in high boiling organic solvent, adopt casting method to prepare composite proton conductive membranes.Be specially:
A. prepare casting solution, wherein polymeric substrates mass fraction is that 1-30wt.% and high boiling solvent are 70-99wt.%, and both mass fraction sums are 100%, in this casting solution, also will add the ionic liquid that is equivalent to polymeric substrates quality 30-90wt.%;
B. above-mentioned casting solution stirs 0.5-20h under temperature 20-100 ° C, makes final casting solution;
C. a certain amount of casting solution is poured in glass mold, casting film under 60-120 ° of C, the film thickness making is 25-250 μ m.
The polymer that the present invention adopts for the preparation of ionic liquid for hydrogen-chlorine fuel cell-composite membrane of polymer can be hydrogen chloride or chlorine to be had to poly-inclined to one side tetrafluoroethene (PVDF), Kynoar-hexafluoropropylene copolymer (PVDF-HFP), Nafion, polybenzimidazoles (PBI) or the polysulfones etc. of well tolerable property.Proton-conductive films prepared by the present invention has high conductance, not in humidification situation, can reach 0.03S/cm completely.
Tool of the present invention has the following advantages:
1. method of operation is simple, easily goes, and ionic liquid-composite membrane of polymer thickness, the ionic liquid doping of making is easy to control, and intensity is good, and conductivity is high, and cost is low, environmental friendliness, safe and reliable, is suitable for large-scale production.
2. because the ionic liquid-composite membrane of polymer of this invention is processed without humidification, can directly take dry chlorine gas as raw material, avoid chlorine water suction to become hydrochloric acid and hypochlorous acid, and then cause that battery performance reduces and the corrosion to battery material etc.There is novelty.
3. the hydrogen-chlorine fuel cell that the composite membrane that adopts the present invention to prepare is assembled can move under middle high temperature (100-200 ° of C) condition.
Accompanying drawing explanation
Fig. 1 is polybenzimidazoles (PBI)/diethylmethyl amine trifluoromethyl sulfonic acid ([dema] TfO) photo of composite membrane section under scanning electron microscopy of embodiment 1 preparation;
Fig. 2 is the conductivity under polybenzimidazoles (PBI)/diethylmethyl amine trifluoromethyl sulfonic acid ([dema] TfO) composite membrane different temperatures of embodiment 1 preparation;
Fig. 3 is the battery performance curve chart of embodiment 1;
Fig. 4 is polyether sulfone (PES)/1-ethyl-3-methylimidazole tetrafluoroborate ([EMIm] BF of embodiment 2 preparations 4) photo of composite membrane section under scanning electron microscopy;
Fig. 5 is polyether sulfone (PES)/1-ethyl-3-methylimidazole tetrafluoroborate ([EMIm] BF of embodiment 2 preparations 4) conductivity under composite membrane different temperatures;
Fig. 6 is Nafion/1-methyl-3-butyl sulfonic acid imidazole bisulfate ([BMIm] HSO of embodiment 3 preparations 3hSO 4) photo of composite membrane section under scanning electron microscopy;
Fig. 7 is Nafion/1-methyl-3-butyl sulfonic acid imidazole bisulfate ([BMIm] HSO of embodiment 3 preparations 3hSO 4) conductivity under composite membrane different temperatures.
Embodiment
Embodiment 1: by the highly purified polybenzimidazoles of 0.25g (PBI, molecular weight M w=58000), the analytically pure DMF of 30g mixes, room temperature lower magnetic force stirs 5h, Filter paper filtering, add the ultrasonic mixing 1h of 1.25g diethylmethyl amine trifluoromethyl sulfonic acid ([dema] TfO), 5h, static 2h deaeration under room temperature, film forming in 80 ° of C baking ovens are stirred in 80 ° of C oil baths.Film thickness is 60 μ m.Gained film has compact texture (film section electromicroscopic photograph is shown in accompanying drawing 1), adopts AC impedence method (EIS) to test conductivity under its different temperatures (completely not humidification, see accompanying drawing 2), and fracture strength is 20MPa.
Adopt method described in patent CN02127802.4 to prepare electrode (binding agent is PBI, and catalyst is 70%Pt/C), in electrode, catalyst Pt carrying capacity is 0.4mg cm -2.For guaranteeing that electrode and the effective of film contact, reduce the contact resistance between electrode and film, negative electrode and anode are placed in respectively to prepared film both sides, in hydraulic press, under 140 ° of C and 0.1MP, suppress 1min, take out rapidly coolingly, obtain membrane electrode three-in-one (MEA).
Gained MEA is assembled into fuel cell, test battery performance on monocell evaluating apparatus.Test performance curve is shown in accompanying drawing 3.Battery-operated condition is as follows: battery temperature is 120 ° of C, and hydrogen, chlorine flow velocity are respectively 10ml min -1, 20ml min -1, without humidification, normal pressure.
Embodiment 2: by 0.3g polyether sulfone (PES, M w=60000), 30g NMP mixes, and under room temperature, stirs 1h, adds 1g1-ethyl-3-methylimidazole tetrafluoroborate ([EMIm] BF 4), ultrasonic mixing 0.5h, 3h, static 1h deaeration afterwards, film forming in 80 ° of C baking ovens are stirred in 90 ° of C oil baths.Film thickness is 125 μ m.Gained film has compact texture (film section electromicroscopic photograph is shown in accompanying drawing 4), adopts four probe method to test conductivity under its different temperatures (completely not humidification, see accompanying drawing 5), and fracture strength is 15MPa.
Embodiment 3: by 10g Nafion solution, (E.I.Du Pont Company 5wt.%), the ultrasonic mixing of 10g DMAC 3h, adds 1g1-methyl-3-butyl sulfonic acid imidazoles hydrogen sulfate ([BMIm] HSO 3hSO 4), under room temperature, stir 5h, static 3h deaeration afterwards, casting film in 60 ° of C baking ovens.Film thickness is 100 μ m.Gained film has compact texture (film section electromicroscopic photograph is shown in accompanying drawing 6), adopts four probe method to test conductivity under its different temperatures (completely not humidification, see accompanying drawing 7), and fracture strength is 30MPa.

Claims (8)

1. ionic liquid-composite membrane of polymer for hydrogen-chlorine fuel cell, is characterized in that:
It is the composite proton conductive membranes of being prepared by high molecular polymer substrate and ionic liquid, and ionic liquid is uniformly distributed in polymeric substrates; Ionic liquid mass fraction in composite membrane is 30-90wt.%.
2. according to ionic liquid-composite membrane of polymer claimed in claim 1, it is characterized in that:
High molecular polymer used is that hydrogen chloride or chlorine are had to one or more blends in poly-inclined to one side tetrafluoroethene (PVDF), Kynoar-hexafluoropropylene copolymer (PVDF-HFP), polysulfones-like polymer, Nafion or the polybenzimidazoles (PBI) of well tolerable property;
Ionic liquid is mainly imidazoles or amine ionic liquid, as 1-ethyl-3-methylimidazole tetrafluoroborate ([EMIm] BF 4), 1-butyl-3-methylimidazole hexafluorophosphate ([BMIm] PF 6), 1-methyl-3-butyl sulfonic acid imidazole bisulfate ([BMIm] HSO 3hSO 4), Trimethylamine phosphoric acid hydrogen disalt ([tma] H 2pO 4), a kind of in diethylmethyl amine trifluoromethyl sulfonic acid ([dema] TfO), Trimethylamine trifluoromethyl sulfonic acid ([tma] TfO).
3. according to the ionic liquid-composite membrane of polymer described in claim 1 or 2, it is characterized in that:
The molecular weight of described poly-inclined to one side tetrafluoroethene (PVDF), Kynoar-hexafluoropropylene copolymer (PVDF-HFP) or polybenzimidazoles (PBI) is 10000-100000g mol -1;
Polysulfones-like polymer is polysulfones or polyether sulfone, and molecular weight is 10000-100000g mol -1.
4. according to ionic liquid-composite membrane of polymer claimed in claim 1, it is characterized in that:
Described ionic liquid-composite membrane of polymer is even compact film, and ionic liquid is uniformly distributed.
5. a preparation method for ionic liquid-composite membrane of polymer described in claim 1, is characterized in that:
High molecular polymer and ionic liquid filler are dissolved in high boiling organic solvent, adopt casting method to prepare ionic liquid-composite membrane of polymer.
6. according to preparation method claimed in claim 5, it is characterized in that:
A. prepare casting solution, wherein polymeric substrates mass fraction is 1-30wt.%, and high boiling solvent is 70-99wt.%, and both mass fraction sums are 100%, in this casting solution, also will add the ionic liquid that is equivalent to polymeric substrates quality 30-90wt.%;
B. above-mentioned casting solution stirs 0.5-20h under temperature 20-100 ° C, makes final casting solution;
C. casting solution is poured in glass mold, casting film under 60-120 ° of C, the film thickness making is 25-250 μ m.
7. according to preparation method claimed in claim 6, it is characterized in that:
High boiling solvent used is good solvent DMSO, DMF, DMAC or the NMP of high molecular polymer.
8. an application for ionic liquid-composite membrane of polymer described in claim 1, is characterized in that:
Described ionic liquid-composite membrane of polymer can be used as electrolyte membrance does not need the hydrogen-chlorine fuel cell of humidification for feed gas.
CN201310150325.3A 2013-04-26 2013-04-26 Ionic liquid-polymer composite membrane for hydrogen chloride fuel cell and preparation and application thereof Pending CN104124463A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105789659A (en) * 2016-04-27 2016-07-20 北京化工大学 Alkaline membrane containing cobaltocenium-benzimidazole polymer and preparation method thereof
CN106750441A (en) * 2016-12-07 2017-05-31 黄河科技学院 A kind of poly- triazole ionic liquid of cross-linking type/polybenzimidazoles high temperature proton exchange film and preparation method thereof
CN109592756A (en) * 2018-12-28 2019-04-09 中国科学院青岛生物能源与过程研究所 A kind of polymer overmold film that NdFeB permanent magnets are excellent and its preparation and the application in electrodialysis recycling concentrating waste acid
CN110896150A (en) * 2018-09-12 2020-03-20 中国科学院大连化学物理研究所 Method for preparing anion exchange membrane by polymerizing ionic liquid monomer
CN111969232A (en) * 2020-08-27 2020-11-20 盐城工学院 Preparation method of fuel cell diaphragm material
CN116253817A (en) * 2023-03-13 2023-06-13 浙江聚合储能科技有限公司 Fluorine ion exchange membrane and preparation method thereof

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Publication number Priority date Publication date Assignee Title
US4128701A (en) * 1977-12-23 1978-12-05 United Technologies Corp. Hydrogen/chlorine regenerative fuel cell
US7282295B2 (en) * 2004-02-06 2007-10-16 Polyplus Battery Company Protected active metal electrode and battery cell structures with non-aqueous interlayer architecture
JP3150803U (en) * 2009-02-24 2009-06-04 俊一郎 森 A set-type fuel cell that circulates and uses hydrogen gas and chlorine gas
CN101935398A (en) * 2010-06-24 2011-01-05 中国科学院宁波材料技术与工程研究所 High-electric conductivity aromatic polymer ionic liquid diaphragm material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4128701A (en) * 1977-12-23 1978-12-05 United Technologies Corp. Hydrogen/chlorine regenerative fuel cell
US7282295B2 (en) * 2004-02-06 2007-10-16 Polyplus Battery Company Protected active metal electrode and battery cell structures with non-aqueous interlayer architecture
JP3150803U (en) * 2009-02-24 2009-06-04 俊一郎 森 A set-type fuel cell that circulates and uses hydrogen gas and chlorine gas
CN101935398A (en) * 2010-06-24 2011-01-05 中国科学院宁波材料技术与工程研究所 High-electric conductivity aromatic polymer ionic liquid diaphragm material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
S.S. SEKHON ET AL: "Proton conducting membrane containing room temperature ionic liquid", 《ELECTROCHIMICA ACTA》, vol. 52, no. 2006, 7 July 2006 (2006-07-07), pages 1639 - 1644 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105789659A (en) * 2016-04-27 2016-07-20 北京化工大学 Alkaline membrane containing cobaltocenium-benzimidazole polymer and preparation method thereof
CN105789659B (en) * 2016-04-27 2018-05-25 北京化工大学 Alkaline membrane of cation containing cobaltocene-benzimidazole polymer and preparation method thereof
CN106750441A (en) * 2016-12-07 2017-05-31 黄河科技学院 A kind of poly- triazole ionic liquid of cross-linking type/polybenzimidazoles high temperature proton exchange film and preparation method thereof
CN106750441B (en) * 2016-12-07 2019-06-21 中科院大连化学物理研究所张家港产业技术研究院有限公司 A kind of poly- triazole ionic liquid of cross-linking type/polybenzimidazoles high temperature proton exchange film and preparation method thereof
CN110896150A (en) * 2018-09-12 2020-03-20 中国科学院大连化学物理研究所 Method for preparing anion exchange membrane by polymerizing ionic liquid monomer
CN110896150B (en) * 2018-09-12 2020-10-27 中国科学院大连化学物理研究所 Method for preparing anion exchange membrane by polymerizing ionic liquid monomer
CN109592756A (en) * 2018-12-28 2019-04-09 中国科学院青岛生物能源与过程研究所 A kind of polymer overmold film that NdFeB permanent magnets are excellent and its preparation and the application in electrodialysis recycling concentrating waste acid
CN111969232A (en) * 2020-08-27 2020-11-20 盐城工学院 Preparation method of fuel cell diaphragm material
CN111969232B (en) * 2020-08-27 2021-11-16 盐城工学院 Preparation method of fuel cell diaphragm material
CN116253817A (en) * 2023-03-13 2023-06-13 浙江聚合储能科技有限公司 Fluorine ion exchange membrane and preparation method thereof

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Application publication date: 20141029