CN110416582B - Ion exchange membrane with insulating high-strength non-reaction zone and preparation method thereof - Google Patents
Ion exchange membrane with insulating high-strength non-reaction zone and preparation method thereof Download PDFInfo
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- CN110416582B CN110416582B CN201810384926.3A CN201810384926A CN110416582B CN 110416582 B CN110416582 B CN 110416582B CN 201810384926 A CN201810384926 A CN 201810384926A CN 110416582 B CN110416582 B CN 110416582B
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
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- 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
- H01M8/1051—Non-ion-conducting additives, e.g. stabilisers, SiO2 or ZrO2
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- H—ELECTRICITY
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- 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
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- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
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- 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
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Abstract
The invention relates to the field of energy storage batteries, in particular to an ion exchange membrane with an insulating high-strength non-reaction region and a preparation method thereof, and provides an effective method for improving the non-reaction region of the ion exchange membrane aiming at the problems of short service life, poor mechanical strength and poor insulativity of the ion exchange membrane of an all-vanadium flow battery. Meanwhile, the invention automatically coats the non-reaction area of the ion exchange membrane and quickly dries at normal temperature, so that the ion exchange membrane is improved, the automation of the process is realized, and the labor and the production cost are saved. Compared with the traditional ultrasonic welding and hot melt film hot melt integrated protection, the ion exchange membrane has the advantages that the mechanical strength of the coating on the surface of the non-reaction area of the ion exchange membrane is improved more obviously, the complete insulation can be realized, and the corrosion of strong acid and strong oxidizing electrolyte can be resisted more. Has good application prospect.
Description
Technical Field
The invention relates to the field of energy storage batteries, in particular to the field of all-vanadium redox flow batteries, and specifically relates to an improvement method of an ion exchange membrane non-reaction region.
Background
The all-vanadium redox flow battery is a novel large-scale energy storage battery and has the advantages of independent capacity, high power, long service life, easiness in operation and the like. The ion exchange membrane is one of the key components of the flow battery, and the performance of the ion exchange membrane directly influences the performance and the service life of the flow battery.
The main functions of ion exchange membranes for flow batteries include three aspects: 1. electrolyte solutions of the anode and the cathode of the battery are separated, so that internal short circuit of the battery is avoided; 2. a proton or ion path in the battery is constructed to form a conductive loop; 3. selectively only allowing protons or specific ions to pass through but not allowing active substances to pass through, and preventing the active substances in the positive and negative electrolyte solutions of the battery from being mixed. The better the permselectivity of the cell ion exchange membrane to a particular ion or proton, the higher the coulombic efficiency of the cell. It can be seen that the ion exchange membrane for a flow battery should satisfy the following conditions:
1) the proton or ion conductivity of ion exchange membranes for flow batteries directly affects the voltage efficiency of the cell, and the proton or ion conductivity selectivity of the separator directly affects the coulombic efficiency of the cell and the capacity stability of the cell. Ion exchange membranes are generally required to have excellent proton conductivity and selectivity for acidic electrolyte solutions, e.g., all-vanadium flow batteries typically have an aqueous solution of sulfuric acid as the solvent and protons (H) as the conductive medium+). The ion exchange membrane is required to not conduct energy storage active materials so as to improve the coulombic efficiency of the battery and the capacity retention capacity of the battery and reduce the self-discharge of the battery.
2) The flow battery generally operates under severe conditions of strong oxidation-reduction property, acidity or alkalinity, high working potential, higher temperature and the like, and the components of a membrane material and the structure of the membrane are required to be kept unchanged in the long-term operation process, namely the membrane material is required to have excellent chemical and electrochemical stability, durability and corrosion resistance.
3) The flow battery is usually used for a large-scale energy storage system, the galvanic pile is large, the pressing force and the shearing force of battery assembly and sealing are large, and the ion exchange membrane is required to have good mechanical properties, namely good tensile strength and toughness.
In practical situations, a small amount of ion exchange exists on two sides of the non-reaction area of the ion exchange membrane, and the phenomenon can cause crystals precipitated in the area to abrade the ion exchange membrane, but the ion membrane is also damaged under the action of long-time pressing force and shearing force in the non-reaction area. However, the prior art does not have an effective improvement method for the non-reaction area of the ion exchange membrane, and how to improve the mechanical strength and the insulation of the ion exchange membrane is a technical problem to be solved in the field.
Disclosure of Invention
In order to make up for the blank of the prior art, the invention provides an insulating high-strength ion exchange membrane non-reaction area and a preparation method thereof, namely, chemical/physical spraying is adopted to coat the insulating high-strength coating on the ion exchange membrane non-reaction area, so that the mechanical strength and the chemical stability of the area of the ion exchange membrane are greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
an insulating high strength ion exchange membrane non-reactive zone coated with an insulating resin composition comprising: 20-65wt% of nano-scale ceramic powder, 35-80wt% of epoxy resin mixture, 1-5wt% of active dispersant and 2-5wt% of polyamine curing agent.
Wherein the nano-scale ceramic powder is prepared from AL with particle size of 5-50nm2O3、SiC、Si3N4And MgO. Preferably, Al is used2O3SiC two-component ratio of nano-ceramic powder, wherein Al2O3Accounting for 25-50wt% of the total mass of the nano-scale ceramic powder, and accounting for 25-50wt% of the total mass of the nano-scale ceramic powder
The epoxy resin mixture is composed of two or more of bisphenol A type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin or glycidyl ester type epoxy resin, preferably, the mass ratio of the epoxy resin mixture to the epoxy resin mixture is 1: 0.1 to 1: 1 bisphenol a epoxy resin and aliphatic glycidyl ether epoxy resin.
The active dispersant is one or more of polyacrylamide, polyacrylic acid and sodium salt thereof, hydroxymethyl cellulose and polyvinyl alcohol.
The polyamine curing agent mixture is composed of two or more of diethylenetriamine, tetramethylenediamine, diaminocyclohexane and methylene dicyclohexylamine. Preferably, the polyamine curing agent mixture consists of diethylenetriamine, tetramethylenediamine and methylenedicyclohexylamine, wherein the diethylenetriamine accounts for 20-50 wt% of the total mass of the polyamine curing agent mixture, the tetramethylenediamine accounts for 20-50 wt% of the total mass of the polyamine curing agent mixture, and the methylenedicyclohexylamine accounts for 5-15 wt% of the total mass of the polyamine curing agent mixture.
The second object of the present invention is to protect the above insulating resin composition preparation method, comprising the steps of:
s1, weighing epoxy resin according to a proportion, and uniformly stirring and mixing to obtain an epoxy resin mixture;
s2, weighing nano-scale ceramic powder according to a proportion, adding the nano-scale ceramic powder into the epoxy resin mixture and uniformly stirring the mixture;
s3, weighing the active dispersing agent according to the proportion, adding the active dispersing agent into the component obtained in the step S2, and stirring while adding the active dispersing agent until the active dispersing agent is uniformly stirred;
s4, weighing the polyamine curing agent in proportion, adding the polyamine curing agent into the component in the step S3, and stirring while adding until the stirring is uniform, so as to obtain an insulating resin mixture.
The third objective of the present invention is to provide a method for preparing an insulating high-strength ion exchange membrane non-reaction area, wherein the insulating resin mixture obtained in the step S4 is added into a full-automatic coating machine to coat the ion exchange membrane non-reaction area, and the coating conditions are as follows: the air source is nitrogen, the air pressure is 0.05-0.5MPa, the distance between the spray head and the surface of the ion exchange membrane is 0.1-10cm, the running speed of the spray head is 0.1-50cm/s, and the coated ion exchange membrane is dried at normal temperature to obtain the ion exchange membrane with the insulating high-strength non-reaction zone.
The invention provides an effective method for improving a non-reaction area of an ion exchange membrane, aiming at the problems of short service life, poor mechanical strength and poor insulativity of the ion exchange membrane of an all-vanadium redox flow battery in a high-potential, strong-acid and strong-oxidizing-property environment when the ion exchange membrane is used. Meanwhile, the invention automatically coats the non-reaction area of the ion exchange membrane and quickly dries at normal temperature, so that the ion exchange membrane is improved, the automation of the process is realized, and the labor and the production cost are saved. Compared with the traditional ultrasonic welding and hot melt film hot melt integrated protection, the ion exchange membrane has the advantages that the mechanical strength of the coating on the surface of the non-reaction area of the ion exchange membrane is improved more obviously, the complete insulation can be realized, and the corrosion of strong acid and strong oxidizing electrolyte can be resisted more. Has good application prospect.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources.
In the following examples, the premix formulation shown in Table 1 and the coating conditions shown in Table 2 were used.
Table 1 premix formula
TABLE 2 coating conditions
Examples
S1, weighing epoxy resin according to a proportion, and uniformly stirring and mixing to obtain an epoxy resin mixture;
s2, weighing nano-scale ceramic powder according to a proportion, adding the nano-scale ceramic powder into the epoxy resin mixture and uniformly stirring the mixture;
s3, weighing the active dispersing agent according to the proportion, adding the active dispersing agent into the component obtained in the step S2, and stirring while adding the active dispersing agent until the active dispersing agent is uniformly stirred;
s4, weighing the polyamine curing agent in proportion, adding the polyamine curing agent into the component in the step S3, and stirring while adding until the stirring is uniform, so as to obtain an insulating resin mixture.
S5, adding the insulating resin mixture obtained in the step S4 into a full-automatic coating machine, uncoiling the coiled untreated ion exchange membrane, cutting the coiled untreated ion exchange membrane into a required shape, and coating the non-reaction area of the ion exchange membrane on two sides when passing through the full-automatic coating machine, wherein the coating conditions are as follows: the air source is nitrogen, the air pressure is 0.05-0.5MPa, the distance between the spray head and the surface of the ion exchange membrane is 0.1-10cm, the running speed of the spray head is 0.1-50cm/s, and the coated ion exchange membrane is dried at normal temperature to obtain the ion exchange membrane with the insulating high-strength non-reaction zone.
By controlling the raw material proportion and the coating conditions, the thickness, the required drying time, the mechanical strength and the cost of the coating of the non-reaction area of the ion exchange membrane can be controlled, so that the design of the all-vanadium redox flow battery with different requirements is adapted.
Table 3 examples 1-18 respective coating mixture formulations and coating methods
| Examples | Ceramic 1 | Ceramic 2 | Ceramic 3 | Resin 1 | Resin composition2 | Resin 3 | Dispersing agent | Curing agent | Coating conditions |
| 1 | 620 | 0 | 0 | 319 | 0 | 0 | 42 | 19 | Condition 1 |
| 2 | 525 | 0 | 0 | 413 | 0 | 0 | 37 | 25 | Condition 1 |
| 3 | 410 | 0 | 0 | 0 | 528 | 0 | 30 | 32 | Condition 1 |
| 4 | 325 | 0 | 0 | 0 | 615 | 0 | 24 | 36 | Condition 1 |
| 5 | 260 | 0 | 0 | 0 | 0 | 677 | 19 | 44 | Condition 1 |
| 6 | 220 | 0 | 0 | 0 | 0 | 719 | 11 | 50 | Condition 1 |
| 7 | 0 | 620 | 0 | 0 | 0 | 319 | 42 | 19 | Condition 2 |
| 8 | 0 | 525 | 0 | 0 | 0 | 413 | 37 | 25 | Condition 2 |
| 9 | 0 | 410 | 0 | 0 | 528 | 0 | 30 | 32 | Condition 2 |
| 10 | 0 | 325 | 0 | 0 | 615 | 0 | 24 | 36 | Condition 2 |
| 11 | 0 | 260 | 0 | 677 | 0 | 0 | 19 | 44 | Condition 2 |
| 12 | 0 | 220 | 0 | 719 | 0 | 0 | 11 | 50 | Condition 2 |
| 13 | 0 | 0 | 620 | 319 | 0 | 0 | 42 | 19 | Condition 3 |
| 14 | 0 | 0 | 525 | 413 | 0 | 0 | 37 | 25 | Condition 3 |
| 15 | 0 | 0 | 410 | 0 | 528 | 0 | 30 | 32 | Condition 3 |
| 16 | 0 | 0 | 325 | 0 | 615 | 0 | 24 | 36 | Condition 3 |
| 17 | 0 | 0 | 260 | 0 | 0 | 677 | 19 | 44 | Condition 3 |
| 18 | 0 | 0 | 220 | 0 | 0 | 719 | 11 | 50 | Condition 3 |
The performance tests and comparisons of the ion exchange membrane raw membrane NR212 of all-vanadium redox flow batteries produced by examples 1 to 18 and dupont of the present invention are performed, and the test results are shown in table 4.
TABLE 4 comparison of coating Properties of examples and comparative examples
Note: the comparative example is a raw ion exchange membrane without any pretreatment.
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (4)
1. An insulating high strength ion exchange membrane non-reactive zone coated with an insulating resin composition comprising: 20-65wt% of nano-scale ceramic powder, 35-80wt% of epoxy resin mixture, 1-5wt% of active dispersant and 2-5wt% of polyamine curing agent;
wherein the nano-scale ceramic powder is prepared from Al with the particle size of 5-50nm2O3SiC two-component ratio of nano-ceramic powder, wherein Al2O3Accounting for 25-50wt% of the total mass of the nano-scale ceramic powder, and accounting for 25-50wt% of the total mass of the nano-scale ceramic powder;
the epoxy resin mixture is prepared by the following raw materials in a mass ratio of 1: 0.1 to 1: 1 bisphenol A epoxy resin and aliphatic glycidyl ether epoxy resin;
the active dispersant is one or more of polyacrylamide, polyacrylic acid and sodium salt thereof, hydroxymethyl cellulose and polyvinyl alcohol;
the polyamine curing agent mixture consists of diethylenetriamine, tetramethylenediamine and methylene dicyclohexylamine, wherein the diethylenetriamine accounts for 20-50 wt% of the total mass of the polyamine curing agent mixture, the tetramethylenediamine accounts for 20-50 wt% of the total mass of the polyamine curing agent mixture, and the methylene dicyclohexylamine accounts for 5-15 wt% of the total mass of the polyamine curing agent mixture.
2. The method for preparing the non-reaction area of the insulating high-strength ion exchange membrane according to claim 1, wherein the non-reaction area of the ion exchange membrane is coated by adding an insulating resin mixture into a full-automatic coating machine under the following coating conditions: the air source is nitrogen, the air pressure is 0.05-0.5MPa, the distance between the spray head and the surface of the ion exchange membrane is 0.1-10cm, the running speed of the spray head is 0.1-50cm/s, and the coated ion exchange membrane is dried at normal temperature to obtain the ion exchange membrane with the insulating high-strength non-reaction zone.
3. The method for preparing the non-reaction area of the insulated high-strength ion exchange membrane according to claim 2, which is characterized by comprising the following steps:
s1, weighing the epoxy resin according to the proportion, and uniformly stirring and mixing to obtain an epoxy resin mixture;
s2, weighing the nano-scale ceramic powder according to the proportion, adding the nano-scale ceramic powder into the epoxy resin mixture and uniformly stirring the mixture;
s3, weighing the active dispersant according to the proportion, adding the active dispersant into the components obtained in the step S2, and stirring and adding the active dispersant until the components are uniformly stirred;
s4, weighing the polyamine curing agent according to the proportion, adding the polyamine curing agent into the component S3, and stirring while adding until the mixture is uniformly stirred to obtain an insulating resin mixture.
4. An all vanadium flow battery ion exchange membrane having the insulating high strength ion exchange membrane non-reaction zone of claim 1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101533915A (en) * | 2008-03-11 | 2009-09-16 | 上海清能燃料电池技术有限公司 | Membrane electrode and current collecting board element of electrochemical cell and electrochemical cell module |
| CN102838921A (en) * | 2012-09-28 | 2012-12-26 | 北京天山新材料技术股份有限公司 | Brushed high-strength abrasion-resistant anticorrosive coating and preparation method |
| CN103074022A (en) * | 2012-12-29 | 2013-05-01 | 东莞市松山湖微电子材料研发中心 | Heat-conducting electronic pouring sealant containing modified filler |
| CN106558662A (en) * | 2015-09-28 | 2017-04-05 | 大连融科储能技术发展有限公司 | Ion-conductive membranes, using the flow battery and preparation method of the ion-conductive membranes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6537703B2 (en) * | 1998-11-12 | 2003-03-25 | Valence Technology, Inc. | Polymeric mesoporous separator elements for laminated lithium-ion rechargeable batteries |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101533915A (en) * | 2008-03-11 | 2009-09-16 | 上海清能燃料电池技术有限公司 | Membrane electrode and current collecting board element of electrochemical cell and electrochemical cell module |
| CN102838921A (en) * | 2012-09-28 | 2012-12-26 | 北京天山新材料技术股份有限公司 | Brushed high-strength abrasion-resistant anticorrosive coating and preparation method |
| CN103074022A (en) * | 2012-12-29 | 2013-05-01 | 东莞市松山湖微电子材料研发中心 | Heat-conducting electronic pouring sealant containing modified filler |
| CN106558662A (en) * | 2015-09-28 | 2017-04-05 | 大连融科储能技术发展有限公司 | Ion-conductive membranes, using the flow battery and preparation method of the ion-conductive membranes |
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