CN113871673B - Composite proton exchange membrane and preparation method thereof - Google Patents
Composite proton exchange membrane and preparation method thereof Download PDFInfo
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- CN113871673B CN113871673B CN202111045776.1A CN202111045776A CN113871673B CN 113871673 B CN113871673 B CN 113871673B CN 202111045776 A CN202111045776 A CN 202111045776A CN 113871673 B CN113871673 B CN 113871673B
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- proton exchange
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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
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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- 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
Abstract
The invention discloses a preparation method of a composite proton exchange membrane, which comprises the following steps: a. dissolving resin in a solvent, mixing and stirring to obtain resin slurry, wherein the solvent is at least two solvents selected from methanol, ethanol, isopropanol, n-propanol, n-hexane, cyclohexane, acetone and water, and the solvent is not a mixed solvent formed by two or three of acetone, cyclohexane and n-hexane; b. and c, coating the resin slurry obtained in the step a on two sides of polytetrafluoroethylene, and drying to obtain the composite proton exchange membrane. According to the preparation method, the low-boiling point solvent is adopted, so that the resin can be filled into the pores of the ePTFE to a greater extent, the selectivity of the composite proton exchange membrane is improved, the interface between the resin layer and the enhancement layer is well combined, the contact resistance of the composite proton exchange membrane is reduced, and the chemical property and the mechanical property of the composite proton exchange membrane are improved.
Description
Technical Field
The invention belongs to the technical field of proton exchange membranes, in particular to a composite proton exchange membrane, and particularly relates to a preparation method of the composite proton exchange membrane.
Background
The proton exchange membrane fuel cell has the advantages of low working temperature, quick start, high specific power, simple structure, convenient operation and the like, and is recognized as the first choice energy source of electric automobiles, fixed power stations and the like. In the fuel cell, the proton exchange membrane provides a channel for migration and transportation of protons, so that the protons pass through the membrane to reach the cathode from the anode to form a loop with the electron transfer of an external circuit, and current is provided to the outside, therefore, the performance of the proton exchange membrane plays a very important role in the performance of the fuel cell, and the service life of the fuel cell is directly influenced by the quality of the proton exchange membrane.
The proton exchange membrane is a core component of the proton exchange membrane fuel cell and plays a key role in the performance of the cell. Therefore, in order to improve the performance of proton exchange membranes, researchers have continuously studied improvements of proton exchange membranes.
Disclosure of Invention
The present invention has been made based on the findings and knowledge of the inventors regarding the following facts and problems: at present, proton exchange membranes are prepared by a plurality of methods, but high-boiling point solvents are mostly adopted in the preparation process. CN105762392a proposes a preparation method of a composite proton exchange membrane, firstly preparing hyperbranched sulfonated polyarylether, then doping polytetrafluoroethylene with the hyperbranched sulfonated polyarylether, and preparing the composite hyperbranched sulfonated polyarylether/polytetrafluoroethylene proton exchange membrane. In the method, the preparation steps are complex, the slurry components are more, the high-boiling-point organic solvent is introduced, the high-boiling-point organic solvent is difficult to remove in the preparation process of the composite membrane, and the high-boiling-point organic solvent is likely to influence the structure of the composite membrane.
The present invention aims to solve at least one of the technical problems in the related art to some extent. Therefore, the embodiment of the invention provides a preparation method of the composite proton exchange membrane, which adopts a low-boiling point solvent, so that the resin can be filled into the pores of the ePTFE to a greater extent, the selectivity of the composite proton exchange membrane is improved, the interface between the resin layer and the enhancement layer is well combined, the contact resistance of the composite proton exchange membrane is reduced, and the chemical property and the mechanical property of the composite proton exchange membrane are improved.
The preparation method of the composite proton exchange membrane according to the embodiment of the invention comprises the following steps:
a. dissolving resin in a solvent, mixing and stirring to obtain resin slurry, wherein the solvent is at least two solvents selected from methanol, ethanol, isopropanol, n-propanol, n-hexane, cyclohexane, acetone and water, and the solvent is not a mixed solvent formed by two or three of acetone, cyclohexane and n-hexane;
b. and c, coating the resin slurry obtained in the step a on two sides of polytetrafluoroethylene, and drying to obtain the composite proton exchange membrane.
According to the preparation method of the composite proton exchange membrane, 1, in the method of the embodiment of the invention, the low-boiling-point organic composite solvent is adopted to disperse the resin, so that the problem that the high-boiling-point solvent is difficult to remove is avoided; 2. according to the method provided by the embodiment of the invention, the resin is dispersed by adopting the low-boiling point composite solvent, the obtained resin slurry can be filled into the pores of the enhancement layer polytetrafluoroethylene to a greater extent, the selectivity of the composite proton exchange membrane is provided, the interface between the resin layer and the enhancement layer is well combined, and the composite proton exchange membrane is reducedThe contact resistance improves the chemical property and the mechanical property of the composite proton exchange membrane, effectively reduces the swelling rate of the composite membrane, and has the advantages of difficult rupture of the membrane structure and excellent stability; 3. the method of the embodiment of the invention is simple and easy to implement and easy to apply, can prepare the composite proton exchange membrane with compact structure, and the surface density of the composite proton exchange membrane with the thickness of 12 micrometers can be up to 2.5mg/cm 2 The mechanical strength can reach 55Mpa, the longitudinal swelling rate can be as low as 2.0%, and the transverse swelling rate can be as low as 5.1%.
In some embodiments, in the step a, the solvent comprises a first component, a second component and a third component, wherein the first component is at least one of n-propanol and isopropanol, the second component is at least one of methanol, ethanol, n-hexane and cyclohexane, the third component is at least one of water and acetone, and the mass ratio of the first component, the second component and the third component is (0-1): (0.5-5): (0-6).
In some embodiments, in step a, the mass ratio of the first component, the second component, and the third component is 1: (0.5-5): (0-6).
In some embodiments, in step a, the mass ratio of the first component, the second component, and the third component is 1: (0.5-5): (0.5-6).
In some embodiments, in the step a, the mass ratio of the first component, the second component, and the third component is 0: (1-5): (0.5-3).
In some embodiments, in step a, the resin is a perfluorosulfonic acid resin.
In some embodiments, in step a, the resulting resin syrup has a solids content of 10-50%.
In some embodiments, in the step b, the thickness of the resin layer in the prepared composite proton exchange membrane is 2-15 micrometers, and the thickness of the polytetrafluoroethylene membrane is 4-12 micrometers.
In some embodiments, in step b, the resulting composite proton exchange membrane has a thickness of 8-40 μm.
The embodiment of the invention also provides a composite proton exchange membrane, which is prepared by the method of the embodiment of the invention. The composite proton exchange membrane provided by the embodiment of the invention is easy to remove because a low-boiling-point solvent is adopted in the preparation process, and the influence caused by high-boiling-point solvent residues is avoided in the subsequent application.
Detailed Description
The following detailed description of embodiments of the invention, examples of which are illustrative and intended to be used to illustrate the invention and not to be construed as limiting the invention.
The preparation method of the composite proton exchange membrane according to the embodiment of the invention comprises the following steps:
a. dissolving resin in a solvent, mixing and stirring to obtain resin slurry, wherein the solvent is at least two solvents selected from methanol, ethanol, isopropanol, n-propanol, n-hexane, cyclohexane, acetone and water, and the solvent is not a mixed solvent formed by two or three of acetone, cyclohexane and n-hexane;
b. and c, coating the resin slurry obtained in the step a on two sides of polytetrafluoroethylene, and drying to obtain the composite proton exchange membrane.
According to the composite proton exchange membrane provided by the embodiment of the invention, the resin is dispersed by adopting the low-boiling-point organic composite solvent, so that the problem that the high-boiling-point solvent is difficult to remove is avoided; according to the method provided by the embodiment of the invention, the resin is dispersed by adopting the low-boiling point composite solvent, the obtained resin slurry can be filled into the pores of the enhancement layer polytetrafluoroethylene to a greater extent, the selectivity of the composite proton exchange membrane is provided, the interface between the resin layer and the enhancement layer is well combined, the contact resistance of the composite proton exchange membrane is reduced, the chemical property and the mechanical property of the composite proton exchange membrane are improved, the swelling rate of the composite membrane is effectively reduced, the structure of the membrane is not easy to break, and the membrane has excellent stability; the method of the embodiment of the invention is simple and easy to implement and easy to apply, can prepare the composite proton exchange membrane with compact structure, and the surface density of the composite proton exchange membrane with the thickness of 12 micrometers can be up to 2.5mg/cm 2 The mechanical strength can reach 55Mpa, the longitudinal swelling rate can be as low as 2.0%, and the transverse swelling rate can be as low as 5.1%.
In some embodiments, in the step a, the solvent comprises a first component, a second component and a third component, wherein the first component is at least one of n-propanol and isopropanol, the second component is at least one of methanol, ethanol, n-hexane and cyclohexane, the third component is at least one of water and acetone, and the mass ratio of the first component, the second component and the third component is (0-1): (0.5-5): (0-6). Preferably, the mass ratio of the first component, the second component and the third component is 1: (0.5-5): (0-6), further preferably, the mass ratio of the first component, the second component and the third component is 1: (0.5-5): (0.5-6). Alternatively, preferably, the mass ratio of the first component, the second component and the third component is 0: (1-5): (0.5-3). . In the method of the embodiment of the invention, the polymer resin can be filled into the porous structure of the polytetrafluoroethylene to the greatest extent by adopting the low-boiling-point solvent with specific composition, so that the surface density and the mechanical strength of the proton exchange membrane are improved, and the resin and the polytetrafluoroethylene can form good combination at the interface, thereby realizing high proton selectivity, further improving the conductivity of the proton exchange membrane, effectively reducing the swelling rate of the composite proton exchange membrane and improving the stability of the composite proton exchange membrane.
In some embodiments, in the step a, the resin is a perfluorosulfonic acid resin, preferably, the obtained resin slurry has a solid content of 10-50%, and the solid content refers to the percentage of the mass of the solid in the slurry to the mass of the slurry. The resin in the embodiments of the present invention may be dissolved in a low boiling point solvent using resin particles or resin dispersion.
In some embodiments, in the step b, the thickness of the resin layer in the prepared composite proton exchange membrane is 2-15 micrometers, and the thickness of the polytetrafluoroethylene membrane is 4-12 micrometers; the thickness of the prepared composite proton exchange membrane is 8-40 mu m. The method of the embodiment of the invention can prepare the composite proton exchange membranes with different thicknesses and has wide application range.
The embodiment of the invention also provides a composite proton exchange membrane, which is prepared by the method of the embodiment of the invention. The composite proton exchange membrane provided by the embodiment of the invention is easy to remove because a low-boiling-point solvent is adopted in the preparation process, and the influence caused by high-boiling-point solvent residues is avoided in the subsequent application.
The present invention will be described in detail with reference to examples.
Example 1
Isopropanol, ethanol, water were mixed according to 1:1: mixing the mixture at a mass ratio of 0.5 to obtain a low boiling point mixed solvent, mixing the low boiling point mixed solvent with perfluorosulfonic acid resin particles, and stirring for 6 hours to prepare a resin slurry with a solid content of 15 wt%.
The resin slurry is uniformly coated on a high polymer substrate, then a polytetrafluoroethylene (ePTFE) porous membrane with the thickness of 5 micrometers is coated on the resin slurry, and then the resin slurry is coated on the ePTFE porous membrane to form the composite membrane.
And (3) placing the composite membrane in a drying oven at 60 ℃ for 30min, and then drying the composite membrane in the drying oven at 160 ℃ for 30min to obtain the composite proton exchange membrane with the thickness of 12 microns.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.5mg/cm 2 Conductivity of 0.10Scm -1 The mechanical strength reaches 55MPa. The swelling ratio was 2.0% (machine direction ), 5.1% (transverse direction, transverse Direction). The conductivity test conditions in the invention are that the test is carried out under the constant temperature and humidity environment with the relative humidity of 50% +/-5% at 25+/-2 ℃ according to GB/T20042.3-2009; the swelling ratio was measured under the conditions of 80℃for 8 hours.
Example 2
Ethanol and water were mixed according to 4:2, mixing the mixture to obtain a low boiling point solvent, mixing the low boiling point solvent with perfluorosulfonic acid resin particles, and stirring for 6 hours to prepare a slurry with a solid content of 20 wt%.
The resin slurry is uniformly coated on a high polymer substrate, then an ePTFE porous membrane with the thickness of 5 micrometers is coated on the resin slurry, and then the resin slurry is coated on the ePTFE porous membrane to form the composite membrane.
The composite film was dried in an oven at 60℃for 30min, followed by drying in an oven at 160℃for 30min. And preparing the composite proton exchange membrane with the thickness of 12 microns.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.1mg/cm 2 Conductivity of 0.08Scm -1 The mechanical strength reaches 48MPa. The swelling ratio was 2.1% (Machine Direction), 5.5% (Transverse Direction).
Example 3
N-propanol, cyclohexane, water according to 3:3:3, mixing the mixture to obtain a low-boiling point mixed solvent, mixing the low-boiling point mixed solvent with perfluorosulfonic acid resin particles, and stirring for 12 hours to prepare a slurry with a solid content of 40 wt%.
The resin slurry is uniformly coated on a high polymer substrate, then an ePTFE porous membrane with the thickness of 8 micrometers is coated on the resin slurry, and then the resin slurry is coated on the ePTFE porous membrane to form the composite membrane.
And (3) placing the composite membrane in a drying oven at 60 ℃ for 30min, and then drying the composite membrane in the drying oven at 160 ℃ for 30min to obtain the composite proton exchange membrane with the thickness of 25 microns.
The surface density of the composite proton exchange membrane prepared in the embodiment is 4.8mg/cm 2 Mechanical strength 48; conductivity of 0.08Scm -1 The swelling ratio was 2.2% (Machine Direction), 5.6% (Transverse Direction).
Example 4
The same procedure as in example 1 was followed except that isopropanol, ethanol, water were used in an amount of 1:5:2 mass ratio.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.4mg/cm 2 Conductivity of 0.09Scm -1 The mechanical strength reaches 54MPa, and the swelling ratio is 2.0 percent (Machine Direction) and 5.3 percent (Transverse Direction).
Example 5
The same procedure as in example 1 was followed except that isopropanol, ethanol, water were used in an amount of 1:4:6 mass ratio.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.4mg/cm 2 Conductivity of 0.07Scm -1 The mechanical strength reaches 50MPa, the swelling ratio is 2.4 percent (Machine Direction)，5.4％(Transverse Direction)。
Example 6
The same procedure as in example 1 is followed except that the low boiling solvent is prepared from isopropanol and ethanol according to 1: mixing at a mass ratio of 0.5.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.3mg/cm 2 Conductivity of 0.08Scm -1 The mechanical strength reaches 51MPa, and the swelling ratio is 2.1 percent (Machine Direction) and 5.3 percent (Transverse Direction).
Example 7
The same procedure as in example 1 was followed except that the low boiling point mixed solvent was mixed with water and acetone in a mass ratio of 1:3.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.3mg/cm 2 Conductivity of 0.07Scm -1 The mechanical strength reaches 47MPa, and the swelling ratio is 3.2 percent (Machine Direction) and 6.3 percent (Transverse Direction).
Example 8
The same procedure as in example 1 was followed except that the low boiling point mixed solvent was mixed with methanol and acetone in a mass ratio of 5:1.
The surface density of the composite proton exchange membrane prepared in the embodiment is 2.2mg/cm 2 Conductivity of 0.08Scm -1 The mechanical strength reaches 47MPa, and the swelling ratio is 2.4 percent (Machine Direction) and 5.6 percent (Transverse Direction).
Comparative example 1
The same method as in example 1 is different in that the low boiling point mixed solvent is mixed with three solvents of isopropanol, ethanol and water in a mass ratio of 1:7:7.
The surface density of the composite proton exchange membrane prepared in comparative example 1 is 2.0mg/cm 2 Conductivity of 0.08Scm -1 The mechanical strength was 46MPa, the swelling ratio was 3.9% (Machine Direction), 8.1% (Transverse Direction).
Comparative example 2
The same procedure as in example 1 was followed except that the low boiling point mixed solvent was prepared from ethanol and water according to 15:1 by mass ratio.
The surface density of the composite proton exchange membrane prepared in comparative example 2 is 1.9mg/cm 2 Conductivity of 0.08Scm -1 The mechanical strength was 42MPa, the swelling ratio was 4.1% (Machine Direction), 8.5% (Transverse Direction).
Comparative example 3
The same procedure as in example 1 was followed except that the low boiling point solvent was n-propanol.
The surface density of the composite proton exchange membrane prepared in comparative example 3 is 1.6mg/cm 2 Conductivity of 0.05Scm -1 The mechanical strength was 32MPa, the swelling ratio was 6.7% (Machine Direction), 8.4% (Transverse Direction).
Comparative example 4
The same procedure as in example 1 was followed except that the low boiling solvent was isopropanol.
The surface density of the composite proton exchange membrane prepared in comparative example 4 is 1.5mg/cm 2 Conductivity of 0.06Scm -1 The mechanical strength was 31MPa, the swelling ratio was 6.5% (Machine Direction) and 7.9% (Transverse Direction).
Comparative example 5
The same procedure as in example 1 was followed except that the low boiling solvent was acetone.
The low boiling point solvent used in comparative example 5 did not dissolve the perfluorosulfonic acid resin. The acetone in the solvent system has the function of being used as an additive to enhance the wettability of the resin solution and polytetrafluoroethylene, but the acetone cannot be used as a solvent of the perfluorinated sulfonic acid resin.
Comparative example 6
The same procedure as in example 1 was followed except that the low boiling point solvent was water.
The resin slurry prepared from the low boiling point solvent adopted in comparative example 6 has poor film forming property, poor wettability with polytetrafluoroethylene, and the composite proton exchange membrane prepared in comparative example 6 is uneven and cannot be tested for areal density, conductivity and mechanical strength.
Comparative example 7
The same procedure as in example 1 was followed except that the low boiling solvent was methanol.
The surface density of the composite proton exchange membrane prepared in comparative example 7 is 1.8mg/cm 2 Conductivity of 0.08Scm -1 The mechanical strength was 40MPa, the swelling ratio was 5.2% (Machine Direction) and 9.6% (Transverse Direction).
Comparative example 8
The same procedure as in example 1 was followed except that the low boiling point solvent was n-hexane.
The low boiling point solvent used in comparative example 8 was not capable of dissolving the perfluorosulfonic acid resin, and the role of n-hexane in the solvent system was to enhance the wettability of the resin solution with polytetrafluoroethylene as an additive, but n-hexane itself was not capable of acting as a solvent for the perfluorosulfonic acid resin.
Comparative example 9
The same procedure as in example 1 was followed except that the low boiling point solvent was cyclohexane.
The low boiling point solvent used in comparative example 9 was not capable of dissolving the perfluorosulfonic acid resin, and cyclohexane in the solvent system was effective as an additive to enhance the wettability of the resin solution with polytetrafluoroethylene, but cyclohexane itself was not capable of acting as a solvent for the perfluorosulfonic acid resin.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (9)
1. The preparation method of the composite proton exchange membrane is characterized by comprising the following steps:
a. dissolving resin in a solvent, mixing and stirring to obtain resin slurry, wherein the solvent comprises a first component, a second component and a third component, wherein the first component is at least one of n-propanol and isopropanol, the second component is at least one of methanol, n-hexane and cyclohexane, the third component is at least one of water and acetone, and the mass ratio of the first component to the second component to the third component is (0-1): (0.5-5): (0-6), and the solvent is not a mixed solvent formed by two or three of acetone, cyclohexane or n-hexane;
b. and c, coating the resin slurry obtained in the step a on two sides of polytetrafluoroethylene, and drying to obtain the composite proton exchange membrane.
2. The method for preparing a composite proton exchange membrane according to claim 1, wherein in the step a, the mass ratio of the first component, the second component and the third component is 1: (0.5-5): (0-6).
3. The method for preparing a composite proton exchange membrane according to claim 2, wherein in the step a, the mass ratio of the first component, the second component and the third component is 1: (0.5-5): (0.5-6).
4. The method for preparing a composite proton exchange membrane according to claim 1, wherein in the step a, the mass ratio of the first component, the second component and the third component is 0: (1-5): (0.5-3).
5. The method for preparing a composite proton exchange membrane according to claim 1, wherein in the step a, the resin is a perfluorosulfonic acid resin.
6. The method for preparing a composite proton exchange membrane according to claim 1, wherein in the step a, the solid content of the obtained resin slurry is 10-50%.
7. The method for preparing a composite proton exchange membrane according to claim 1, wherein in the step b, the thickness of the resin layer in the prepared composite proton exchange membrane is 2-15 micrometers, and the thickness of the polytetrafluoroethylene membrane is 4-12 micrometers.
8. The method for preparing a composite proton exchange membrane according to claim 1, wherein in the step b, the thickness of the prepared composite proton exchange membrane is 8-40 μm.
9. A composite proton exchange membrane prepared by the method of any one of claims 1-8.
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