CN102024928A - Nafion ion exchange membrane used for enhanced vanadium redox battery and preparation method thereof - Google Patents
Nafion ion exchange membrane used for enhanced vanadium redox battery and preparation method thereof Download PDFInfo
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Abstract
本发明涉及全钒氧化还原液流电池(VRB)用离子交换膜领域，特别涉及一种增强型钒电池用全氟磺酸离子交换膜及其制备方法。由含有磺酸基团的全氟磺酸离子交换树脂为成膜树脂，树脂溶解于有机溶剂中得到成膜溶液，由成膜溶液形成全氟磺酸离子交换膜；在全氟磺酸离子交换膜中间有一层聚四氟乙烯网布作为增强材料；或者，在两层聚四氟乙烯网布中间有一层全氟磺酸离子交换膜。该膜即具有高的化学稳定性、高的电流密度，又比全氟磺酸膜机械强度高、交换容量高、成本低，可以解决现有技术中存在的全氟磺酸离子交换膜都存在交换容量高而机械强度低、机械强度高而交换容量低的问题，主要应用于全钒氧化还原液流电池(VRB)。The invention relates to the field of ion-exchange membranes for all-vanadium redox flow batteries (VRB), in particular to a perfluorosulfonic acid ion-exchange membrane for enhanced vanadium batteries and a preparation method thereof. The perfluorosulfonic acid ion exchange resin containing sulfonic acid groups is the film-forming resin, the resin is dissolved in an organic solvent to obtain a film-forming solution, and the perfluorosulfonic acid ion-exchange membrane is formed from the film-forming solution; in the perfluorosulfonic acid ion exchange There is a layer of polytetrafluoroethylene mesh in the middle of the membrane as a reinforcement material; or, there is a layer of perfluorosulfonic acid ion exchange membrane between two layers of polytetrafluoroethylene mesh. The membrane not only has high chemical stability and high current density, but also has higher mechanical strength, higher exchange capacity and lower cost than perfluorosulfonic acid membranes, and can solve the problem of perfluorosulfonic acid ion exchange membranes in the prior art. The problems of high exchange capacity and low mechanical strength, and high mechanical strength and low exchange capacity are mainly used in all-vanadium redox flow batteries (VRB).
Description
Technical Field
The invention relates to the field of ion exchange membranes for all-vanadium redox flow batteries (VRBs), in particular to a perfluorinated sulfonic acid ion exchange membrane for an enhanced vanadium battery and a preparation method thereof.
Background
With the rapid development of national economy, the contradiction between energy, resources and environmental protection is increasingly prominent, and the traditional energy system is urgently transformed into renewable energy.
The adjustment of the current electric energy structure and the development of the large-scale utilization of renewable clean energy such as wind energy, solar energy and the like become the basic national policy of the electric energy development in China. The power generation process of renewable energy sources such as wind energy, solar energy and the like has the characteristics of discontinuity and instability, and a power storage and energy storage device is required to be equipped to realize continuous and stable power output so as to avoid large-scale vicious accidents caused by impact on a local power grid. So far, among new battery technologies developed in the world, an all-vanadium Redox flow battery (Redox flow cell) is undoubtedly the most promising, and the battery has the advantages of large use scale, long service life, high energy efficiency, environmental friendliness, good current continuity and the like.
The all vanadium redox flow battery is H with V (II)/V (III) and V (IV)/V (V) redox couples2SO4The solution is used as positive and negative half-cell electrolyte respectively. H2SO4Is ionized into H+And SO4 2-Then H in the electrolyte+Sustained replacement of H in ion exchange membranes+And then enters into another electrolyte to complete the conducting process. VO in the battery positive electrolyte when discharging2 +The ions are reduced to VO2+Ion, V in negative electrode electrolyte2+The ions are oxidized to V3+Ions. When charging, the process is just reversed.
The vanadium battery electrode reaction is as follows:
and (3) positive electrode:E0＝1.00V
negative electrode:
E0＝-0.26V
the vanadium battery is developed to the present day, and reaches a more advanced level, but still has many key problems to be solved urgently, wherein the key material diaphragm is one of the two, the diaphragm in the vanadium battery has the functions of isolating positive and negative electrode electrolyte solutions and preventing the vanadium ions with different valence states from mutually permeating, the cross contamination of the positive and negative electrode electrolyte solutions is prevented, the ion selectivity is improved, protons can freely pass through, and the vanadium with different valence states has high selectivity. A large number of tests prove that the perfluorosulfonic acid ion exchange membrane has high chemical stability, high current density and small ion conduction resistance. Among them, Nafion117 membranes produced by dupont have the best performance in all respects among many membranes, but the membranes are expensive to manufacture; the domestic diaphragm has low cost, but the performance is inferior to that of the Nafion117 membrane. At present, perfluorosulfonic acid ion exchange membranes all have the problems of high exchange capacity, low mechanical strength, high mechanical strength and low exchange capacity. In addition, when large-area batteries are assembled in a large scale by using wind energy and solar energy in practical application, the requirements on the mechanical strength and the service life of the diaphragm are quite high, and question is raised about whether the existing perfluorinated sulfonic acid ion exchange membrane can meet the requirements.
The invention content is as follows:
the invention aims to provide a perfluorinated sulfonic acid ion exchange membrane for an enhanced vanadium battery and a preparation method thereof, and solves the problems that the perfluorinated sulfonic acid ion exchange membranes in the prior art are high in exchange capacity, low in mechanical strength, high in mechanical strength and low in exchange capacity. The enhanced perfluorinated sulfonic acid ion exchange membrane is a membrane applied to a vanadium redox flow battery (VRB), has high chemical stability and high current density, and can meet the requirements of high mechanical strength and high exchange capacity and reduce cost compared with the existing perfluorinated sulfonic acid ion exchange membrane.
The technical scheme of the invention is as follows:
a perfluorinated sulfonic acid ion exchange membrane for an enhanced vanadium battery is prepared by taking perfluorinated sulfonic acid ion exchange resin containing sulfonic acid groups as membrane forming resin, dissolving the resin in an organic solvent to obtain a membrane forming solution, and forming the perfluorinated sulfonic acid ion exchange membrane by the membrane forming solution; a layer of Polytetrafluoroethylene (PTFE) mesh cloth is arranged in the middle of the perfluorinated sulfonic acid ion exchange membrane to be used as a reinforcing material; or, a layer of perfluorinated sulfonic acid ion exchange membrane is arranged between two layers of Polytetrafluoroethylene (PTFE) mesh cloth.
The film forming solution of the perfluorinated sulfonic acid ion exchange resin is firmly combined with the reinforcing net by smearing and heating.
The Polytetrafluoroethylene (PTFE) mesh fabric is a reticular base fabric woven by taking glass fiber as a base material, and then is coated with polytetrafluoroethylene resin; the mesh of the mesh cloth is 0.3mm-10 mm and the thickness is 0.01mm-1.2 mm. Wherein,
polytetrafluoroethylene is a polymer of tetrafluoroethylene. The basic structure is as follows:
-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-。
the structure of the perfluorosulfonic acid ion exchange resin is as follows:
wherein X is more than or equal to 1, Y is more than or equal to 0, Z is 0-3, n is more than or equal to 1, and the exchange capacity of the perfluorosulfonic acid ion exchange resin is IEC 0.67-1.3 mmol/g.
The preparation method of the perfluorinated sulfonic acid ion exchange membrane for the enhanced vanadium battery comprises the following specific steps:
(1) dissolving perfluorosulfonic acid ion exchange resin (with exchange capacity IEC of 0.67-1.3mmol/g) into an organic solvent according to the mass ratio w of 5-30%, heating a reaction kettle to 110-250 ℃, and preserving heat for 1-4h to dissolve the resin to obtain a uniform and clear film forming solution.
Wherein the organic solvent is xylene, N-dimethylformamide, N-dimethylformamide, dimethyl sulfoxide or N-methylpyrrolidone.
(2) The prepared film forming solution is vibrated in an ultrasonic oscillator for 30min-60min, so that the solution is refined and tiny bubbles in the solution are removed.
(3) And (2) taking a certain amount of film forming solution to be cast on a clean mould, heating to 100-120 ℃, keeping the temperature for 1-2 hours, then flatly placing a Polytetrafluoroethylene (PTFE) mesh on the film forming solution, finally coating the remaining film forming solution on the Polytetrafluoroethylene (PTFE) mesh, evaporating and cooling a solvent to room temperature by heating to 120-180 ℃ and keeping the temperature for 1-4 hours, cleaning the obtained film with distilled water, and drying at 50-70 ℃ to obtain the enhanced perfluorinated sulfonic acid ion exchange membrane for the vanadium battery.
Or smearing the film-forming solution on a layer of polytetrafluoroethylene mesh cloth, covering the film-forming solution with a layer of polytetrafluoroethylene mesh cloth, heating to 120-180 ℃, keeping the temperature for 1-4h to evaporate the solvent, cooling to room temperature, washing the obtained film with distilled water, and drying at 50-70 ℃ to obtain the enhanced perfluorosulfonic acid ion exchange membrane for the vanadium battery.
The mould material is glass plate, aluminum plate, stainless steel plate, polytetrafluoroethylene board or polyvinyl chloride material.
In the present invention, 20ml of a 10% by mass film-forming solution was prepared to have a thickness of 70 μm and an area of 165mm2The thickness of the membrane and Polytetrafluoroethylene (PTFE) net cloth is the total thickness of the perfluorinated sulfonic acid ion exchange membrane.
The invention has the advantages that:
1. the invention uses Polytetrafluoroethylene (PTFE) mesh as the reinforcing material of the perfluorinated sulfonic acid ion exchange membrane, and can obviously improve the mechanical strength of the perfluorinated sulfonic acid ion exchange membrane, thereby ensuring that the mechanical strength and the service life which are quite high in requirements are ensured when the wind energy and the solar energy are utilized to assemble the large-area all-vanadium redox flow battery in a large scale in practical application, and avoiding the phenomenon that the diaphragm is broken because of insufficient mechanical strength of the diaphragm during the process of assembling the battery or after the battery is operated for a period of time, damaging the operation of the whole battery, further improving the maintenance work of the battery, namely improving the cost of the battery.
2. At present, the perfluorosulfonic acid ion exchange membrane has the problems of high mechanical strength and low exchange capacity. Therefore, because the Polytetrafluoroethylene (PTFE) mesh is used as the reinforcing material of the perfluorinated sulfonic acid ion exchange membrane, the perfluorinated sulfonic acid ion exchange resin with high exchange capacity can be used for preparing the membrane forming solution, so that the diaphragm has high mechanical strength and high exchange capacity, and the performance of the all-vanadium redox flow battery is improved.
3. The invention uses Polytetrafluoroethylene (PTFE) mesh as the reinforcing material of the perfluorinated sulfonic acid ion exchange membrane, reduces the dosage of perfluorinated sulfonic acid ion exchange resin under the condition of meeting the electrochemical performance of the membrane, and greatly reduces the cost for preparing the membrane.
Drawings
FIG. 1 is a schematic structural diagram of a perfluorinated sulfonic acid ion exchange membrane for an enhanced vanadium battery.
FIG. 2 is another schematic structural diagram of the perfluorinated sulfonic acid ion exchange membrane for the enhanced vanadium battery.
In the figure, 1 film; 2 Polytetrafluoroethylene (PTFE) scrim.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific embodiments and with reference to the accompanying drawings.
Example 1
1.89g of perfluorosulfonic acid ion exchange resin (exchange capacity IEC ═ 0.7mmol/g) was dissolved in 20ml of N, N2Heating the mixture in Dimethylformamide (DMF) to 140 ℃ in a reaction kettle, and keeping the temperature for 3 hours to dissolve the resin, thereby obtaining a uniform and clear film forming solution which is used as a film forming solution.
Firstly, the prepared film forming solution is vibrated for 1 hour in an ultrasonic oscillator, so that the solution is refined and tiny bubbles in the solution are removed. Then, 10ml of film forming solution is taken to be cast on a clean mould, the temperature is heated to 100 ℃, the temperature is kept for 1h, and then Polytetrafluoroethylene (PTFE) mesh cloth 2 is flatly placed on the film forming solution. And finally, coating the remaining 10ml of film forming solution on a Polytetrafluoroethylene (PTFE) mesh fabric 2, heating to 140 ℃, keeping the temperature for 2h, naturally cooling to room temperature, respectively forming a film 1 on two surfaces of the Polytetrafluoroethylene (PTFE) mesh fabric 2, cleaning the obtained film with distilled water, and drying at 60 ℃ to obtain the enhanced perfluorosulfonic acid ion exchange membrane for the vanadium battery (figure 1).
In addition, 20ml of film forming solution can be firstly smeared on a layer of Polytetrafluoroethylene (PTFE) mesh cloth 2, then a layer of Polytetrafluoroethylene (PTFE) mesh cloth 2 is covered on the film forming solution, the membrane is cleaned by distilled water and dried at 60 ℃ after being heated to 140 ℃ and kept at a constant temperature for 2 hours and naturally cooled to room temperature, and the enhanced perfluorosulfonic acid ion exchange membrane for the vanadium battery is obtained (figure 2).
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 0.3 multiplied by 0.3mm, and the thickness is 0.03 mm.
Example 2
Essentially the same as in example 1, except that 0.63g of perfluorosulfonic acid ion exchange resin was dissolved in 6.67ml of N, N2-Dimethylformamide (DMF) as film formationAnd (3) solution.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 0.5 multiplied by 0.5mm, and the thickness is 0.05 mm.
Example 3
Essentially the same as in example 1, except that 2.83g of perfluorosulfonic acid ion exchange resin was dissolved in 30ml of N, N2-Dimethylformamide (DMF), as a film forming solution.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 1 multiplied by 1mm, and the thickness is 0.1 mm.
Example 4
Essentially the same as in example 1, except that 5.67g of perfluorosulfonic acid ion exchange resin was dissolved in 60ml of N, N2-Dimethylformamide (DMF), as a film forming solution.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the screen cloth is 2 multiplied by 2mm, and the thickness is 0.2 mm.
Example 5
Essentially the same as in example 1, except that 1.89g of perfluorosulfonic acid ion exchange resin was dissolved in 10ml of N, N2-Dimethylformamide (DMF), as a film forming solution.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 0.3 multiplied by 0.3mm, and the thickness is 0.03 mm.
Example 6
Essentially the same as in example 1, except that 1.89g of perfluorosulfonic acidThe acid ion exchange resin was dissolved in 30ml of N, N2-Dimethylformamide (DMF), as a film forming solution.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 1 multiplied by 1mm, and the thickness is 0.1 mm.
Example 7
Essentially the same as in example 1, except that 1.89g of perfluorosulfonic acid ion exchange resin was dissolved in 50ml of N, N2-Dimethylformamide (DMF), as a film forming solution.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the screen cloth is 2 multiplied by 2mm, and the thickness is 0.2 mm.
Example 8
Essentially the same as example 1, except that the perfluorosulfonic acid ion exchange resin had an exchange capacity IEC of 0.9 mmol/g.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 0.3 multiplied by 0.3mm, and the thickness is 0.03 mm.
Example 9
Essentially the same as example 1 except that the perfluorosulfonic acid ion exchange resin had an exchange capacity IEC of 1.1 mmol/g.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the mesh cloth is 1 multiplied by 1mm, and the thickness is 0.1 mm.
Example 10
Essentially the same as example 1 except that the perfluorosulfonic acid ion exchange resin had an exchange capacity IEC of 1.3 mmol/g.
In this embodiment, the reinforcing mesh is a Polytetrafluoroethylene (PTFE) mesh fabric, which is woven from glass fibers as a base material, and then coated with PTFE resin. The mesh of the screen cloth is 2 multiplied by 2mm, and the thickness is 0.2 mm.
The result shows that the invention has a layer of Polytetrafluoroethylene (PTFE) mesh cloth as a reinforcing material in the middle of the perfluorinated sulfonic acid ion exchange membrane or a layer of perfluorinated sulfonic acid ion exchange membrane in the middle of two layers of Polytetrafluoroethylene (PTFE) mesh cloth, so that the ion exchange membrane has high chemical stability, high current density, high mechanical strength, high exchange capacity and low cost, and can be applied to vanadium redox flow batteries (VRB).
Claims (8)
1. A perfluorinated sulfonic acid ion exchange membrane for an enhanced vanadium battery is characterized in that: the method comprises the following steps of (1) taking perfluorosulfonic acid ion exchange resin containing sulfonic acid groups as film-forming resin, dissolving the resin in an organic solvent to obtain a film-forming solution, and forming the perfluorosulfonic acid ion exchange membrane from the film-forming solution; a layer of polytetrafluoroethylene mesh cloth is arranged in the middle of the perfluorinated sulfonic acid ion exchange membrane as a reinforcing material; or, a layer of perfluorinated sulfonic acid ion exchange membrane is arranged between the two layers of polytetrafluoroethylene mesh cloth.
2. The enhanced perfluorinated sulfonic acid ion exchange membrane for the vanadium redox battery as claimed in claim 1, wherein: the film forming solution of the perfluorinated sulfonic acid ion exchange resin is firmly combined with the reinforcing net by smearing and heating.
3. The enhanced perfluorinated sulfonic acid ion exchange membrane for the vanadium redox battery as claimed in claim 1, wherein: the polytetrafluoroethylene mesh cloth is woven by taking glass fiber as a base material to form a mesh-shaped base cloth, and then polytetrafluoroethylene resin is coated on the mesh-shaped base cloth; the mesh of the mesh cloth is 0.3mm-10 mm and the thickness is 0.01mm-1.2 mm.
4. The enhanced perfluorinated sulfonic acid ion exchange membrane for the vanadium redox battery as claimed in claim 1, wherein: the polytetrafluoroethylene is a polymer of tetrafluoroethylene, and has the following basic structure:
-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-。
5. the enhanced perfluorinated sulfonic acid ion exchange membrane for the vanadium redox battery as claimed in claim 1, wherein: the structure of the perfluorinated sulfonic acid ion exchange resin is as follows:
wherein X is more than or equal to 1, Y is more than or equal to 0, Z is 0-3, and n is more than or equal to 1.
6. The enhanced perfluorinated sulfonic acid ion exchange membrane for the vanadium redox battery as claimed in claim 1, wherein: the exchange capacity of the perfluorosulfonic acid ion exchange resin is 0.67 to 1.3 mmol/g.
7. The preparation method of the perfluorinated sulfonic acid ion exchange membrane for the enhanced vanadium redox battery according to claim 1, which is characterized by comprising the following specific steps:
(1) dissolving perfluorosulfonic acid ion exchange resin into an organic solvent according to the mass ratio w of 5-30%, heating a reaction kettle to 110-250 ℃, and keeping the temperature for 1-4h to dissolve the resin to obtain a uniform and clear film forming solution;
(2) oscillating the prepared film forming solution in an ultrasonic oscillator for 30-60 min to thin the solution and remove micro bubbles in the solution;
(3) and (2) casting the film forming solution on a clean mould, heating to 80-120 ℃, keeping the temperature for 1-2h, then flatly placing a polytetrafluoroethylene mesh on the film forming solution, finally coating the remaining film forming solution on the polytetrafluoroethylene mesh, evaporating and cooling the solvent to room temperature by heating to 120-180 ℃ and keeping the temperature for 1-4h, cleaning the obtained film with distilled water, and drying at 50-70 ℃ to obtain the enhanced perfluorosulfonic acid ion exchange membrane for the vanadium battery.
8. The preparation method of the perfluorinated sulfonic acid ion exchange membrane for the enhanced vanadium redox battery according to claim 1, which is characterized by comprising the following specific steps:
(1) dissolving perfluorosulfonic acid ion exchange resin into an organic solvent according to the mass ratio w of 5-30%, heating a reaction kettle to 110-250 ℃, and keeping the temperature for 1-4h to dissolve the resin to obtain a uniform and clear film forming solution;
(2) oscillating the prepared film forming solution in an ultrasonic oscillator for 30-60 min to thin the solution and remove micro bubbles in the solution;
(3) and (3) coating the film forming solution on a layer of polytetrafluoroethylene mesh cloth, then covering the film forming solution with a layer of polytetrafluoroethylene mesh cloth, heating to 120-180 ℃, keeping the temperature for 1-4h to evaporate the solvent, cooling to room temperature, cleaning the obtained film with distilled water, and drying at 50-70 ℃ to obtain the enhanced perfluorosulfonic acid ion exchange membrane for the vanadium battery.
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| WO2018214843A1 (en) * | 2017-05-22 | 2018-11-29 | 大连理工大学 | Crosslinked porous membrane resulting from hydrolysis of ester group side chain and preparation method therefor |
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Application publication date: 20110420 |