WO2013034055A1 - 一种离子膜的生产方法 - Google Patents

一种离子膜的生产方法 Download PDF

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WO2013034055A1
WO2013034055A1 PCT/CN2012/080508 CN2012080508W WO2013034055A1 WO 2013034055 A1 WO2013034055 A1 WO 2013034055A1 CN 2012080508 W CN2012080508 W CN 2012080508W WO 2013034055 A1 WO2013034055 A1 WO 2013034055A1
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producing
constant temperature
ionic membrane
ion membrane
drying
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PCT/CN2012/080508
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French (fr)
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郑东冬
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深圳市金钒能源科技有限公司
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    • 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
    • C08J5/20—Manufacture of shaped structures of ion-exchange resins
    • C08J5/22—Films, membranes or diaphragms
    • C08J5/2206—Films, membranes or diaphragms based on organic and/or inorganic macromolecular compounds
    • C08J5/2218—Synthetic macromolecular compounds
    • C08J5/2256—Synthetic macromolecular compounds based on macromolecular compounds obtained by reactions other than those involving carbon-to-carbon bonds, e.g. obtained by polycondensation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
    • H01B1/122—Ionic conductors
    • 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
    • H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
    • H01M8/184—Regeneration by electrochemical means
    • H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
    • 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
    • H01M8/22—Fuel cells in which the fuel is based on materials comprising carbon or oxygen or hydrogen and other elements; Fuel cells in which the fuel is based on materials comprising only elements other than carbon, oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0082—Organic polymers
    • 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
    • Y02E60/10—Energy storage using batteries
    • 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

Definitions

  • the invention belongs to the field of vanadium flow batteries, and particularly relates to an ion membrane production method applied in a vanadium flow battery.
  • the surface of the ion-exchange membrane produced by the ionic membrane production method involved in the conventional technology may have fine wrinkles, form a water-grain surface, and the surface of the ion-exchange membrane is not flat enough.
  • the ionic membrane tends to accumulate impurities during the use of the ionic membrane. The formation of impurities will reduce the service life of the ion membrane, and will also affect the normal use of the vanadium flow reactor, and reduce the working efficiency of the vanadium flow reactor.
  • the present invention provides a novel method of producing an ion film.
  • the technical solution adopted by the present invention to solve the problems of the prior art is to provide an ion membrane production method, and the method for producing the ion membrane comprises the steps of:
  • the precipitated filtrate is poured into a drying device, and dried at a constant temperature of 120 ° C for 90 minutes, and vacuum-treated at the same time as the constant temperature drying;
  • the step A is specifically: mixing a sulfonic acid resin and dimethylformamide into a stainless steel container, and treating at a constant temperature of 230 ° C and an environment of 0.3 MPa to 0.4 MPa. For one hour, the mixture was agitated at a speed of 60 to 100 rpm while being processed.
  • the sulfonic acid resin is a perfluorosulfonic acid resin.
  • the filtering process in the step B is performed using a filter made of titanium.
  • the step C is specifically: placing the filtrate in a plastic container and allowing to stand at a constant temperature of 25 ° C for 20 days.
  • the plastic container is transparent or white.
  • the step D is specifically: pouring the precipitated filtrate onto a flat table in a drying device, drying at a constant temperature of 120 ° C for 90 minutes, and drying at a constant temperature. At the same time, vacuuming is performed, and the drying device is an electronic pulse infrared heater.
  • the step E is specifically to take out the dried and formed ion film and place it on a flat cooling table for room temperature cooling treatment.
  • the surface of the ion membrane produced by the disclosed technical solution is very flat, and the toughness and airtightness of the ion membrane are very good, and the service life of the ion membrane is greatly increased, thereby increasing the service life of the vanadium flow reactor and improving The working efficiency of the vanadium flow reactor.
  • Figure 1 is a flow chart showing the production method of the ion film of the present invention.
  • FIG. 1 a flow chart of the ion membrane production method of the present invention.
  • a flow chart of the ion membrane production method As shown in Figure 1, a flow chart of the ion membrane production method.
  • the present invention provides an ion film production method, and the method for producing the ion film comprises the steps of:
  • the precipitated filtrate is poured into a drying device, and dried at a constant temperature of 120 ° C for 90 minutes, and vacuum-treated at the same time as the constant temperature drying;
  • the step A is specifically: mixing the sulfonic acid resin and the dimethylformamide into a stainless steel container, and treating at a constant temperature of 230 ° C and an environment of 0.3 MPa to 0.4 MPa. In the hour, the mixture is agitated at a speed of 60 to 100 rpm while being processed.
  • the sulfonic acid resin is preferably a perfluorosulfonic acid resin.
  • the treatment temperature and pressure selected in the step A of the present invention are the optimum values obtained by the inventors through a large number of experiments, and are not randomly selected values according to common sense.
  • the filtration treatment uses a filter made of titanium.
  • the filter of too material is selected, mainly considering that the chemical composition of the titanium material is relatively stable, and it is difficult to chemically react with the filtrate.
  • the step C is specifically that the filtrate is placed in a plastic container and allowed to stand at a constant temperature of 25 ° C for 20 days.
  • the plastic container is transparent or white, and a transparent or white plastic container is mainly used.
  • the purpose is to facilitate the observation of the precipitation of the filtrate in the container at any time, so as to facilitate timely detection of problems occurring during the precipitation process. Drying on a flat table in a dry device at a constant temperature of 120 ° C for 90 minutes, vacuuming at the same time as the constant temperature drying, and drawing the working chamber of the drying device into a negative pressure, the drying In the step E, the dried and formed ion film is taken out and placed on a flat cooling table for room temperature cooling treatment.
  • the surface of the ion membrane produced by the disclosed technical solution is very flat, and the toughness and airtightness of the ion membrane are very good, and the service life of the ion membrane is greatly increased, thereby increasing the service life of the vanadium flow reactor and improving The working efficiency of the vanadium flow reactor.

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

一种离子膜的生产方法，其包括步骤：将磺酸树脂与二甲基甲酰胺进行混合处理，并进行搅拌；对混合液进行过滤处理；将滤液放置在塑料容器中进行沉淀处理；将经沉淀处理的滤液倒入烘干装置内，在120°C的恒温下进行烘干处理90分钟，在恒温烘干的同时进行抽真空处理；将烘干成型的离子膜取出进行冷却处理。根据本发明所公开的技术方案所生产的离子膜表面非常平整，而且离子膜的韧性和气密性非常好，离子膜的使用寿命大大增加，从而也增加了钒液流电堆的使用寿命，提高了钒液流电堆的工作效率。

Description

一种离子膜的生产方法 技术领域
本发明属于钒液流电池领域， 具体涉及钒液流电池中应用的离子膜生 产方法。
背景技术
应用传统技术中涉及的离子膜生产方法生产出的离子膜表面会出现细 微的褶皱， 形成水纹面， 离子膜表面不够平整， 这种离子膜在使用过程中， 其褶皱处容易积存杂质， 这种杂质的生成会使离子膜的使用寿命降低， 而 且也会影响钒液流电堆的正常使用， 降低钒液流电堆的工作效率。
发明内容
为了解决现有技术中存在的技术问题， 本发明提供了一种新的离子膜 的生产方法。
本发明解决现有技术问题所采用的技术方案为提供了一种离子膜生产 方法， 所述离子膜的生产方法包括步骤：
A:将磺酸树脂与二甲基甲酰胺进行混合处理， 并进行搅拌；
B:对所述步骤 A中所得到的混合液进行过滤处理；
C:将滤液放置在塑料容器中进行沉淀处理；
D:将经沉淀处理的滤液倒入烘干装置内， 在 120°C的恒温下进行烘干 处理 90分钟， 在恒温烘干的同时进行抽真空处理；
E:将烘干成型的离子膜取出进行冷却处理。
根据本发明的优选技术方案： 所述步骤 A具体为将磺酸树脂与二甲基 甲酰胺放入不锈钢材质容器内进行混合， 并在 230°C的恒温、 0.3MPa ~ 0.4 MPa的环境下处理一小时，在处理的同时以 60 ~ 100转 /分的转速进行搅拌 处理。
根据本发明的优选技术方案： 所述磺酸树脂为全氟磺酸树脂。
根据本发明的优选技术方案： 所述步骤 B中过滤处理采用钛材质的过 滤器。
根据本发明的优选技术方案： 所述步骤 C具体为将滤液放置在塑料容 器中， 在 25 °C的恒温下静置 20天。 根据本发明的优选技术方案： 所述塑料容器为透明或白色。 根据本发明的优选技术方案： 所述步骤 D具体为将经沉淀处理的滤液 倒入烘干装置内的平板工作台上，在 120°C的恒温下进行烘干处理 90分钟， 在恒温烘干的同时进行抽真空处理， 所述烘干装置为电子脉沖红外线加热 器。
根据本发明的优选技术方案： 所述步骤 E具体为将烘干成型的离子膜 取出放置在平整的冷却台上进行室温冷却处理。
根据本发明所公开的技术方案所生产的离子膜表面非常平整， 而且离 子膜的韧性和气密性非常好， 离子膜的使用寿命大大增加， 从而也增加了 钒液流电堆的使用寿命， 提高了钒液流电堆的工作效率。
附图说明
图 1本发明离子膜生产方法流程图。
具体实施方式
以下结合附图对本发明技术方案进行详细说明：
请参阅图 1本发明离子膜生产方法流程图。 如图 1所示， 离子膜生产 方法流程图。 如图中所示， 本发明提供了一种离子膜生产方法， 所述离子 膜的生产方法包括步骤：
A:将磺酸树脂与二甲基甲酰胺进行混合处理， 并进行搅拌；
B:对所述步骤 A中所得到的混合液进行过滤处理；
C:将滤液放置在塑料容器中进行沉淀处理；
D:将经沉淀处理的滤液倒入烘干装置内， 在 120°C的恒温下进行烘干 处理 90分钟， 在恒温烘干的同时进行抽真空处理；
E:将烘干成型的离子膜取出进行冷却处理。
在本发明的技术方案中所述步骤 A具体为将磺酸树脂与二甲基甲酰胺 放入不锈钢材质容器内进行混合， 并在 230 °C的恒温、 0.3MPa ~ 0.4 MPa 的环境下处理一小时， 在处理的同时以 60 ~ 100转 /分的转速进行搅拌处 理。 所述磺酸树脂优选全氟磺酸树脂， 本发明步骤 A中所选定的处理温度 和压力是发明人经过大量实验得到的最佳数值， 并不是根据常识随机选取 的数值。 经过发明人的实验发现处理温度设置在恒温 230°C恒温， 压力设 定在 0.3MPa ~ 0.4 MPa对离子膜最终的质量好坏具有很大的影响。 所述步骤 B中过滤处理采用钛材质的过滤器。 选用太材质的过滤器， 主要是考虑钛材料的化学成分比较稳定， 不易与滤液发生化学反应。
在本发明的技术方案中所述步骤 C具体为将滤液放置在塑料容器中， 在 25 °C的恒温下静置 20天， 所述塑料容器为透明或白色， 选用透明或白 色的塑料容器主要目的在于可以方便随时观察容器内滤液的沉淀情况， 便 于及时发现沉淀过程中出现的问题。 干装置内的平板工作台上， 在 120°C的恒温下进行烘干处理 90分钟， 在恒 温烘干的同时进行抽真空处理， 将烘干装置的工作腔抽成负压， 所述烘干 所述步骤 E具体为将烘干成型的离子膜取出放置在平整的冷却台上进 行室温冷却处理。
根据本发明所公开的技术方案所生产的离子膜表面非常平整， 而且离 子膜的韧性和气密性非常好， 离子膜的使用寿命大大增加， 从而也增加了 钒液流电堆的使用寿命， 提高了钒液流电堆的工作效率。
以上内容是结合具体的优选技术方案对本发明所作的进一步详细说 明， 不能认定本发明的具体实施只局限于这些说明。 对于本发明所属技术 领域的普通技术人员来说， 在不脱离本发明构思的前提下， 还可以做出若 干筒单推演或替换， 都应当视为属于本发明的保护范围。

Claims

权 利 要求 书
1.一种离子膜的生产方法， 其特征在于： 所述离子膜的生产方法包括 步骤：
A:将磺酸树脂与二甲基甲酰胺进行混合处理， 并进行搅拌；
B:对所述步骤 A中所得到的混合液进行过滤处理；
C:将滤液放置在塑料容器中进行沉淀处理；
D:将经沉淀处理的滤液倒入烘干装置内， 在 120°C的恒温下进行烘干 处理 90分钟， 在恒温烘干的同时进行抽真空处理；
E:将烘干成型的离子膜取出进行冷却处理。
2.根据权利要求 1所述离子膜的生产方法， 其特征在于：
所述步骤 A具体为将磺酸树脂与二甲基甲酰胺放入不锈钢材质容器内 进行混合， 并在 230°C的恒温、 0.3MPa ~ 0.4 MPa的环境下处理一小时， 在处理的同时以 60 ~ 100转 /分的转速进行搅拌处理。
3.根据权利要求 2所述离子膜的生产方法， 其特征在于： 所述磺酸树 脂为全氟磺酸树脂。
4.根据权利要求 1所述离子膜的生产方法， 其特征在于： 所述步骤 B 中过滤处理采用钛材质的过滤器。
5.根据权利要求 1所述离子膜的生产方法， 其特征在于： 所述步骤 C 具体为将滤液放置在塑料容器中， 在 25 °C的恒温下静置 20天。
6.根据权利要求 5所述离子膜的生产方法， 其特征在于： 所述塑料容 器为透明或白色。
7.根据权利要求 1所述离子膜的生产方法， 其特征在于： 所述步骤 D 具体为将经沉淀处理的滤液倒入烘干装置内的平板工作台上， 在 120°C的 恒温下进行烘干处理 90分钟，在恒温烘干的同时进行抽真空处理，所述烘 干装置为电子脉沖红外线加热器。
8.根据权利要求 1所述离子膜的生产方法， 其特征在于： 所述步骤 E 具体为将烘干成型的离子膜取出放置在平整的冷却台上进行室温冷却处 理。
PCT/CN2012/080508 2011-09-09 2012-08-23 一种离子膜的生产方法 WO2013034055A1 (zh)

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CN101367903A (zh) * 2008-08-07 2009-02-18 同济大学 一种基于半互穿网络的增强型复合质子交换膜及其制备方法
CN101759865A (zh) * 2008-11-14 2010-06-30 杨玉生 一种液面流延法制备全氟磺酸质子交换膜的方法
CN102344578A (zh) * 2011-09-09 2012-02-08 深圳市金钒能源科技有限公司 一种离子膜的生产方法

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