CN118126354A - Double-network hydrogel electrolyte with high water retention and preparation method and application thereof - Google Patents
Double-network hydrogel electrolyte with high water retention and preparation method and application thereof Download PDFInfo
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- CN118126354A CN118126354A CN202410300114.1A CN202410300114A CN118126354A CN 118126354 A CN118126354 A CN 118126354A CN 202410300114 A CN202410300114 A CN 202410300114A CN 118126354 A CN118126354 A CN 118126354A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 120
- 239000003792 electrolyte Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 81
- 206010016807 Fluid retention Diseases 0.000 claims abstract description 71
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 64
- 239000011780 sodium chloride Substances 0.000 claims abstract description 32
- 239000000499 gel Substances 0.000 claims abstract description 31
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 28
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 28
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 238000004132 cross linking Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 81
- 238000003756 stirring Methods 0.000 claims description 58
- 239000000243 solution Substances 0.000 claims description 30
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 13
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 230000009977 dual effect Effects 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 22
- 239000002001 electrolyte material Substances 0.000 abstract description 14
- 229920000642 polymer Polymers 0.000 abstract description 11
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 61
- 238000012360 testing method Methods 0.000 description 28
- 239000011149 active material Substances 0.000 description 18
- 230000000694 effects Effects 0.000 description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 16
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- 210000004027 cell Anatomy 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000001035 drying Methods 0.000 description 12
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 12
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 11
- 238000005520 cutting process Methods 0.000 description 10
- -1 polytetrafluoroethylene Polymers 0.000 description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 9
- 239000002033 PVDF binder Substances 0.000 description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 9
- 239000006260 foam Substances 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 8
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- 150000002500 ions Chemical class 0.000 description 6
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
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- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
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Abstract
The invention belongs to the technical field of polymer chemistry and functional energy storage devices, and discloses a high-water-retention double-network hydrogel electrolyte, a preparation method and application thereof. The preparation method comprises the following steps: dropwise adding acrylic acid into a sodium hydroxide solution, uniformly mixing, sequentially adding acrylamide, sodium chloride and a crosslinking agent, uniformly mixing, adding an initiator, uniformly mixing, and performing heat treatment to thermally initiate crosslinking to form gel, thereby obtaining a composite hydrogel matrix; immersing the composite hydrogel matrix in potassium hydroxide solution for immersing, and taking out after immersing, thus obtaining the double-network hydrogel electrolyte with high water retention. According to the preparation method, the hydrogel material with the double-network structure is constructed, so that the mechanical toughness and the comprehensive stability of the hydrogel material are improved, and the water retention of the hydrogel is enhanced by doping high-concentration inorganic salt in the preparation process of the hydrogel material, so that the obtained hydrogel electrolyte material with the high-water retention double-network structure can be used as an electrolyte of a zinc-air battery.
Description
Technical Field
The invention relates to the technical field of polymer chemistry and functional energy storage devices, in particular to a double-network hydrogel electrolyte with high water retention and a preparation method and application thereof.
Background
The zinc-air battery has higher energy density compared with a lithium ion battery, and positive and negative electrode materials of the zinc-air battery are zinc foil, foam nickel and the like, so that the zinc-air battery has good flexibility, and is suitable for flexible devices.
Currently, the electrolytes in existing zinc-air batteries are mainly potassium hydroxide liquid electrolytes and solid electrolytes. Wherein, the liquid electrolyte is easy to volatilize and leak, and has safety problem; while solid state electrolytes have low conductivity and are not flexible. Therefore, both of the above electrolyte materials are not suitable for flexible batteries, and there is a need to develop a novel material that is free from leakage and has excellent electrical conductivity.
In order to solve the above technical problems, those skilled in the art propose to use hydrogel as an electrolyte, wherein the hydrogel is a hydrophilic three-dimensional network structure, swells in water but does not dissolve, can effectively solve the problem of electrolyte leakage, exerts excellent electrochemical performance, is easy to bend and bend, and is an ideal electrolyte of a flexible battery. However, the existing hydrogel is mainly polyvinyl alcohol (PVA) and Polyacrylamide (PAM), and the semi-open structure of the zinc-air battery is that the water in the polyvinyl alcohol (PVA) and Polyacrylamide (PAM) hydrogel is easy to run off to the external environment, so that the ionic conductivity of the electrolyte is reduced, and the battery performance is reduced.
Therefore, the invention provides a double-network hydrogel electrolyte with high water retention, and a preparation method and application thereof.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a double-network hydrogel electrolyte with high water retention, and a preparation method and application thereof. According to the preparation method, the hydrogel material with the double-network structure is constructed, so that the mechanical toughness and the comprehensive stability of the hydrogel material are improved, meanwhile, the water retention of the hydrogel is enhanced by doping high-concentration inorganic salt in the preparation process of the hydrogel material, and the obtained hydrogel electrolyte material with the high-water retention double-network structure can be used as an electrolyte of a zinc-air battery.
The invention relates to a double-network hydrogel electrolyte with high water retention, and a preparation method and application thereof, which are realized by the following technical scheme:
The first object of the invention is to provide a preparation method of a high-water-retention double-network hydrogel electrolyte, which comprises the following steps:
And step 1, acrylic acid is added into a sodium hydroxide solution in a dropwise manner, and the mixture is stirred and mixed uniformly to obtain a mixed solution A.
And 2, dispersing acrylamide and sodium chloride in the mixed solution A in sequence to obtain a mixed solution B.
And step 3, dispersing the cross-linking agent and the initiator in the mixed solution B in sequence to obtain a mixed solution C.
And 4, carrying out heat treatment on the mixed solution C at 50-70 ℃ to thermally initiate and crosslink the mixed solution C to form gel through heat treatment, thereby obtaining the composite hydrogel matrix.
And 5, immersing the composite hydrogel matrix in potassium hydroxide solution, carrying out immersing treatment, and taking out after the immersing is finished, thus obtaining the high-water-retention double-network hydrogel electrolyte.
Preferably, the mass ratio of the sodium hydroxide in the sodium hydroxide solution to the acrylic acid is 10-20:5-10.
Preferably, the dosage ratio of the sodium chloride to the mixed solution A is 0.5-1 mol:1L.
Preferably, the mass ratio of the acrylamide to the acrylic acid in the mixed solution A is 1-3:5-10.
Preferably, the cross-linking agent is N' N-methylenebisacrylamide; and the dosage of the cross-linking agent is 0.1 to 0.15 weight percent of the mass of the mixed solution B.
Preferably, the initiator is ammonium persulfate; and the dosage of the initiator is 0.1 to 0.2 weight percent of the mass of the mixed solution B.
Preferably, the heat treatment is performed for a treatment time of 2 to 4 hours.
Preferably, the soaking treatment is carried out at room temperature for 24-72 h.
Preferably, the concentration of the potassium hydroxide solution is 6-7.5 mol/L.
Preferably, the concentration of sodium hydroxide in the sodium hydroxide solution is 6-8 mol/L.
Preferably, in preparing the mixed solution A, the stirring speed is 50-100 r/min, and the stirring time is 1-3 min.
Preferably, after the acrylamide is added, the stirring speed is 100-120 r/min, and the stirring time is 10-15 min.
Preferably, after adding sodium chloride, the stirring speed is 150-200 r/min, and the stirring time is 1-2h.
Preferably, after the crosslinking agent is added, the stirring speed is 150-200 r/min, and the stirring time is 1-3 h.
Preferably, after the initiator is added, the stirring speed is 50-80 r/min, and the stirring time is 5-10 s.
The second object of the invention is to provide a high-water-retention double-network hydrogel electrolyte prepared by the preparation method.
A third object of the present invention is to provide an application of the above-mentioned high water-retention dual-network hydrogel electrolyte in the preparation of zinc-air batteries, wherein the high water-retention dual-network hydrogel electrolyte is used as an electrolyte of the zinc-air batteries.
Preferably, the zinc-air cell is produced by the steps of:
And sequentially superposing the anode, the high-water-retention double-network hydrogel electrolyte and the cathode to form a sandwich structure, and then fixing by using a breathable adhesive tape to obtain the zinc-air battery.
Preferably, the area ratio of the positive electrode, the high water retention dual network hydrogel electrolyte and the negative electrode is 2cm 2:1.5cm2:2cm2.
Preferably, the positive electrode is composed of a current collector, and an active material supported on the current collector, and the positive electrode is prepared by:
1) Uniformly mixing an active substance, conductive carbon black and polyvinylidene fluoride, then dropwise adding N-methyl pyrrolidone, and uniformly grinding to obtain an active slurry; wherein the dosage ratio of the active substance, the conductive carbon black, the polyvinylidene fluoride and the N-methyl pyrrolidone is 9-9.5 mmol, 0.1g and 5ml.
2) And coating the active slurry on a current collector, and drying to form an active material layer on the current collector, thereby obtaining the positive electrode.
Preferably, the active substance is an oxide or peroxide.
Preferably, the current collector is made of foam nickel or carbon cloth; and the thickness of the current collector is 1.5mm.
Preferably, the drying temperature is 55-65 ℃ and the drying time is 8-16 h.
Preferably, the negative electrode is prepared by the steps of:
and (3) polishing the zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, thus obtaining the negative electrode.
Compared with the prior art, the invention has the following beneficial effects:
According to the preparation method, the hydrogel material with the double-network structure is constructed, so that the mechanical toughness and the comprehensive stability of the hydrogel material are improved, meanwhile, the water retention of the hydrogel is enhanced by doping high-concentration inorganic salt in the preparation process of the hydrogel material, and the obtained hydrogel electrolyte material with the high-water retention double-network structure can be used as an electrolyte of a zinc-air battery.
The invention uses the acrylic acid and the acrylamide together as the skeleton of the polymer, so that the hydrogel material finally formed by the invention has a double-network structure, thereby improving the mechanical property, toughness and water retention property of the hydrogel material.
According to the invention, sodium chloride is introduced in the process of preparing the hydrogel, so that sodium chloride is used as a water retaining agent of the hydrogel, and the introduction of Na + and Cl - enables free water to be combined into combined water, so that the quantity and fluidity of the free water are reduced, and the polymer network structure is smaller and denser. In addition, after ion doping, the network structure of the polymer is influenced by the salinization effect in the hydrogel polymerization process, and ions form hydrogen bonds among polymer chains, so that the polymer chains spontaneously collapse to form small pores, and the good mechanical property can be maintained in the process of soaking the potassium hydroxide solution. The combined water combined with Na + and Cl - is less prone to escape than free water, the water retention of the zinc-air battery is greatly improved, two ions can move freely, and the conductivity of the hydrogel is effectively improved.
In addition, the sodium chloride is used as an additive of the hydrogel, so that dendrite formation and side reaction of the zinc electrode can be effectively inhibited, the problem of possible short circuit of the zinc-air battery in the use process is solved, and the durability of the zinc-air battery is improved.
Drawings
Fig. 1 is a schematic structural view of a zinc-air cell of the present invention.
Fig. 2 is a graph showing the results of the water retention test at normal temperature for the hydrogel electrolyte materials prepared in example 1, and comparative examples 1 and 2.
Fig. 3 is a graph showing the results of the water retention test at 75 c for the hydrogel electrolyte materials prepared in example 1, and comparative examples 1 and 2.
Fig. 4 is an ac impedance test result of the hydrogel electrolyte materials prepared in example 1, comparative example 1 and comparative example 2.
Fig. 5 shows gel conductivities σ of example 1, comparative example 1, and comparative example 2.
Fig. 6 is a graph showing charge and discharge performance of the zinc-air cells prepared in example 4, comparative example 3 and comparative example 4.
Fig. 7 is a charge and discharge long cycle test result at a current density of 2mA cm -2 of the zinc-air cells prepared in example 4, comparative example 3, and comparative example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below.
The invention provides a preparation method of a high-water-retention double-network hydrogel electrolyte, which comprises the following steps:
And step 1, acrylic acid is added into a sodium hydroxide solution in a dropwise manner, and the mixture is stirred and mixed uniformly to obtain a mixed solution A.
The invention takes the acrylic acid as one of the skeletons of the hydrogel material, has the advantages of excellent mechanical property and alkali resistance, but because the pH value of the acrylic acid is 4.5, and the acidic environment is unfavorable for crosslinking to form gel, the invention takes sodium hydroxide as a neutralizer, and the sodium hydroxide is prepared into solution, and then the acrylic acid is fully contacted with the sodium hydroxide in the solution, so that the pH value of the acrylic acid is adjusted to 6.5-7 by neutralizing the acidity of the acrylic acid by the sodium hydroxide solution, thereby forming the sodium acrylate solution.
In the invention, the acrylic acid is added into the sodium hydroxide solution in a dropwise adding mode in consideration of the factor of violent heat release of the neutralization reaction of the acrylic acid and the sodium hydroxide, so as to achieve the purpose of neutralizing the solution. After the completion of the acrylic acid dropwise addition, the two were brought into contact with each other sufficiently by stirring to form a sodium acrylate solution. In order to ensure that the acrylic acid is sufficiently contacted with the sodium hydroxide in solution by stirring, in a preferred embodiment of the present invention, the stirring is carried out at a rate of 50 to 100r/min for a period of 1 to 3min.
In order to ensure that acrylic acid and sodium hydroxide are brought into sufficient contact in solution to form a sodium acrylate solution, in a preferred embodiment of the invention the mass ratio of sodium hydroxide in the sodium hydroxide solution to acrylic acid is 10-20:5-10.
And step 2, adding acrylamide into the mixed solution A, stirring and mixing uniformly, and then adding sodium chloride and stirring and mixing uniformly to obtain a mixed solution B.
The invention uses the acrylamide as one of the skeletons of the hydrogel material, namely uses the acrylic acid and the acrylamide as the skeletons of the hydrogel material together, so that the hydrogel material finally formed by the invention has a double-network structure, thereby improving the mechanical property, toughness and water retention property of the hydrogel material.
In order to make the finally obtained hydrogel material have a double-network structure, in a preferred embodiment of the invention, the dosage ratio of the acrylamide to the acrylic acid in the mixed solution A is 1-3:5-10, so as to achieve the purpose of enhancing the double-network crosslinking density and enabling the hydrogel to have better mechanical properties. And in order to fully and uniformly mix the acrylamide with the mixed solution A, in another preferred embodiment of the present invention, the stirring speed is 100-120 r/min and the stirring time is 10-15 min after the acrylamide is added.
In order to increase the water retention property of the hydrogel and improve the factor of ionic conductivity of the hydrogel, sodium chloride is added after acrylamide is uniformly mixed with the mixed solution A, sodium chloride is used as a water retention agent of the hydrogel, and the introduction of Na + and Cl - enables free water to be combined into combined water, so that the quantity and fluidity of the free water are reduced, and the polymer network structure is smaller and denser. In addition, after ion doping, the network structure of the polymer is influenced by the salinization effect in the hydrogel polymerization process, and ions form hydrogen bonds among polymer chains, so that the polymer chains spontaneously collapse to form small pores, and the good mechanical property can be maintained in the process of soaking the potassium hydroxide solution. The combined water combined with Na + and Cl - is less prone to escape than free water, the water retention of the zinc-air battery is greatly improved, two ions can move freely, and the conductivity of the hydrogel is effectively improved. In addition, the sodium chloride is used as an additive of the hydrogel, so that dendrite formation and side reaction of the zinc electrode can be effectively inhibited, the problem of possible short circuit of the zinc-air battery in the use process is solved, and the durability of the zinc-air battery is improved.
In order to enable the above-mentioned effects to be achieved by adding sodium chloride, in a preferred embodiment of the present invention, the ratio of the sodium chloride to the mixed solution A is 0.5 to 1mol:1L. And in another preferred embodiment of the present invention, after adding sodium chloride, stirring is performed at a stirring rate of 100 to 120r/min for 1 to 2 hours so that sodium chloride is completely dissolved.
And step 3, adding the cross-linking agent into the mixed solution B, stirring and mixing uniformly, and then adding the initiator and stirring and mixing uniformly to obtain a mixed solution C.
In order to fully dissolve the cross-linking agent, the cross-linking agent is firstly added into the mixed solution B and stirred, so that the cross-linking agent and the mixed solution B are uniformly mixed, and the cross-linking can be uniformly generated in the subsequent heat treatment, so that the hydrogel material with uniform components is formed. And in order to ensure that the crosslinking agent is sufficiently mixed with the mixed solution B, in another preferred embodiment of the present invention, the stirring rate is 100 to 120r/min and the stirring time is 1 to 3 hours after the crosslinking agent is added.
The invention is taken as an example of factors of fully dissolving and uniformly mixing the cross-linking agent, adding the initiator after uniformly mixing the cross-linking agent, and stirring to ensure that the initiator is uniformly mixed with the mixed solution B mixed with the cross-linking agent so as to facilitate the rapid cross-linking polymerization of sodium acrylate and acrylamide. And in order to ensure adequate mixing of the initiator, in a preferred embodiment of the invention, the stirring rate is 50-80 r/min and the stirring time is 5-10 s after the initiator is added.
In order to ensure that the cross-linking agent can sufficiently cross-link each component, in a preferred embodiment of the invention, N' N-methylene bisacrylamide is used as the cross-linking agent, and the content of the added cross-linking agent is 0.1-0.15 wt% of the mass of the mixed solution B.
In order to ensure that the initiator can sufficiently crosslink to form gel through thermal initiation in the subsequent heat treatment process, in a preferred embodiment of the invention, ammonium persulfate is used as the initiator, and the content of the ammonium persulfate added is 0.1-0.2 wt% of the mass of the mixed solution B. In order to facilitate uniform mixing of ammonium persulfate with the mixed solution B, in another preferred embodiment of the present invention, ammonium persulfate is added in the form of an aqueous ammonium persulfate solution having a mass concentration of 25 to 35mg/mL.
And 4, carrying out heat treatment on the mixed solution C to thermally initiate crosslinking of the mixed solution C to form gel through heat treatment, thereby obtaining the composite hydrogel matrix.
It should be noted that the present invention adopts a thermal initiation method, so that the mixed solution C is thermally initiated to crosslink to form a gel. And in order to ensure that the mixed solution C can be thermally induced crosslinked to form a gel by a heat treatment, in a preferred embodiment of the present invention, the temperature of the heat treatment is 50 to 70 ℃ and the treatment time is 2 to 4 hours.
And 5, immersing the composite hydrogel matrix in potassium hydroxide solution, carrying out immersing treatment, and taking out after the immersing is finished, thus obtaining the high-water-retention double-network hydrogel electrolyte.
In order to improve the electrochemical performance of the gel-based zinc-air battery, the invention uses potassium hydroxide solution as electrolyte, and the composite hydrogel matrix prepared in the step 4 is immersed in the potassium hydroxide solution, so that the solvent exchange effect of the potassium hydroxide solution on the composite hydrogel matrix is carried out, and the double-network hydrogel electrolyte with high water retention property is further obtained.
In order to ensure that the above effect can be achieved on the composite hydrogel matrix by a soaking treatment, in a preferred embodiment of the present invention, the soaking treatment is performed at room temperature for 24 to 72 hours; and the concentration of the potassium hydroxide solution is 6-7.5 mol/L.
Referring to fig. 1, the present invention further provides a zinc-air battery, and the zinc-air battery is prepared by the following steps:
and sequentially superposing the anode, the prepared high-water-retention double-network hydrogel electrolyte and the cathode to form a sandwich structure, and then fixing by using a breathable adhesive tape to obtain the zinc-air battery.
In order to ensure the electrochemical performance of the zinc-air battery, the area ratio of the positive electrode, the high-water-retention double-network hydrogel electrolyte and the negative electrode is 2cm 2:1.5cm2:2cm2.
The positive electrode adopted by the invention consists of a current collector and an active material loaded on the current collector, and is prepared by the following steps:
1) Uniformly mixing an active substance, conductive carbon black and polyvinylidene fluoride, then dropwise adding N-methyl pyrrolidone, and uniformly grinding to obtain an active slurry; wherein the dosage ratio of the active substance, the conductive carbon black, the polyvinylidene fluoride and the N-methyl pyrrolidone is 9-9.5 mmol, 0.1g and 5ml.
2) And coating the active slurry on a current collector, and drying to form an active material layer on the current collector, thereby obtaining the positive electrode.
The active material used in the present invention is oxide or peroxide. And in order to ensure a catalytically active reaction rate of the active material employed, in a preferred embodiment of the present invention, the active material employed is manganese dioxide.
The current collector is foam nickel or carbon cloth; and the thickness of the current collector is 1.5mm.
In order to ensure that the drying process is enabled, the active slurry is allowed to cure on the current collector to form the active material, in a preferred embodiment of the invention, the drying is at a temperature of 55 to 65 ℃ for a drying time of 8 to 16 hours.
The negative electrode of the invention is prepared by the following steps: and (3) polishing the zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, thus obtaining the negative electrode.
Example 1
The embodiment provides a double-network hydrogel electrolyte with high water retention, and the double-network hydrogel electrolyte is prepared through the following steps:
Step 1, 5g of Acrylic Acid (AA) was added dropwise to 10mL of a sodium hydroxide solution having a concentration of 6mol/L, and stirred at a stirring rate of 50r/min for 1min to obtain a mixed solution A.
Step 2, adding 3g of acrylamide (AAm) into the mixed solution A obtained in the step 1, and stirring for 10min at a stirring rate of 100 r/min; then, 0.44g of sodium chloride (NaCl) was further added thereto and stirred at a stirring rate of 150r/min for 60 minutes to obtain a mixed solution B.
Step 3, adding 30mgN 'N' methylene bisacrylamide into the mixed solution B prepared in the step 2, and stirring for 120min at a stirring rate of 150 r/min; then, 1mL of an aqueous ammonium persulfate solution having a mass concentration of 30mg/mL was stirred at a stirring rate of 50r/min for 10s to obtain a mixed solution C.
And 4, transferring the mixed solution C prepared in the step 3 into a polytetrafluoroethylene mould, and then placing the polytetrafluoroethylene mould containing the mixed solution C in a vacuum drying oven at 60 ℃ for 3 hours, so that the mixed solution C is thermally initiated and crosslinked to form gel through heat treatment, and a composite hydrogel matrix is obtained.
And 5, completely immersing the composite hydrogel matrix prepared in the step 4 in a 6mol/L potassium hydroxide solution, immersing at room temperature for 48 hours, and taking out to obtain the double-network hydrogel electrolyte with high water retention, which is abbreviated as PANa +PAM+NaCl.
Example 2
The embodiment provides a double-network hydrogel electrolyte with high water retention, and the double-network hydrogel electrolyte is prepared through the following steps:
Step 1, 5g of acrylic acid was added dropwise to 10mL of a sodium hydroxide solution having a concentration of 6mol/L, and stirred at a stirring rate of 50r/min for 1min to obtain a mixed solution A.
Step2, adding 3g of acrylamide into the mixed solution A obtained in the step 1, and stirring for 10min at a stirring rate of 100 r/min; then, 0.87g of sodium chloride was further added thereto and stirred at a stirring rate of 150r/min for 120 minutes to obtain a mixed solution B.
Step 3, adding 30mg of N 'N' methylene bisacrylamide into the mixed solution B prepared in the step 2, and then stirring for 120min at a stirring rate of 150 r/min; then, 1mL of an aqueous ammonium persulfate solution having a mass concentration of 30mg/mL was stirred at a stirring rate of 50r/min for 10s to obtain a mixed solution C.
And 4, transferring the mixed solution C prepared in the step 3 into a polytetrafluoroethylene mould, and then placing the polytetrafluoroethylene mould containing the mixed solution C in a vacuum drying oven at 60 ℃ for 3 hours, so that the mixed solution C is thermally initiated and crosslinked to form gel through heat treatment, and a composite hydrogel matrix is obtained.
And 5, completely immersing the composite hydrogel matrix prepared in the step 4 in a 6mol/L potassium hydroxide solution, immersing at room temperature for 48 hours, and taking out to obtain the double-network hydrogel electrolyte with high water retention.
Example 3
The embodiment provides a double-network hydrogel electrolyte with high water retention, and the double-network hydrogel electrolyte is prepared through the following steps:
Step 1, 5g of acrylic acid was added dropwise to 10mL of a sodium hydroxide solution having a concentration of 6mol/L, and stirred at a stirring rate of 50r/min for 1min to obtain a mixed solution A.
Step 2, adding 5g of acrylamide into the mixed solution A obtained in the step 1, and stirring for 15min at a stirring rate of 120 r/min; then, 0.44g of sodium chloride was further added thereto and stirred at a stirring rate of 150r/min for 60 minutes to obtain a mixed solution B.
Step 3, adding 30mgN 'N' methylene bisacrylamide into the mixed solution B prepared in the step 2, and stirring for 120min at a stirring rate of 150 r/min; then, 1mL of an aqueous ammonium persulfate solution having a mass concentration of 30mg/mL was stirred at a stirring rate of 50r/min for 10smin to obtain a mixed solution C.
And 4, transferring the mixed solution C prepared in the step 3 into a polytetrafluoroethylene mould, and then placing the polytetrafluoroethylene mould containing the mixed solution C in a vacuum drying oven at 60 ℃ for 3 hours, so that the mixed solution C is thermally initiated and crosslinked to form gel through heat treatment, and a composite hydrogel matrix is obtained.
And 5, completely immersing the composite hydrogel matrix prepared in the step 4 in a 6mol/L potassium hydroxide solution, immersing at room temperature for 48 hours, and taking out to obtain the double-network hydrogel electrolyte with high water retention.
Example 4
The embodiment provides a zinc-air battery, which is prepared by the following steps:
step 1, preparing a positive electrode:
1) Respectively adding 0.8g of manganese dioxide, 0.1g of conductive carbon black and 0.1g of polyvinylidene fluoride into a mortar, dropwise adding 5mL of N-methylpyrrolidone, grinding and uniformly mixing to obtain active slurry.
2) And (3) coating the active slurry prepared in the step (1) on foam nickel with the thickness of 1.5mm, drying to form an active material layer on a current collector, and cutting the active material layer to the size of 2cm multiplied by 1cm to obtain the positive electrode.
Step 2, preparing a negative electrode:
polishing a zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, and cutting the polished zinc foil to the size of 2cm multiplied by 1cm to obtain the negative electrode.
Step 3, preparing electrolyte:
the high water retention dual-network hydrogel electrolyte prepared in example 1 was cut to a size of 1.5cm×1cm to obtain an electrolyte.
Step 4, composing a zinc-air battery:
And sequentially superposing the positive electrode, the electrolyte and the negative electrode which are obtained through the preparation to form a sandwich structure, and then fixing the sandwich structure by using a breathable adhesive tape to obtain the zinc-air battery.
Example 5
The embodiment provides a zinc-air battery, which is prepared by the following steps:
step 1, preparing a positive electrode:
1) Respectively adding 0.8g of manganese dioxide, 0.1g of conductive carbon black and 0.1g of polyvinylidene fluoride into a mortar, dropwise adding 5mL of N-methylpyrrolidone, grinding and uniformly mixing to obtain active slurry.
2) And (3) coating the active slurry prepared in the step (1) on foam nickel with the thickness of 1.5mm, drying to form an active material layer on a current collector, and cutting the active material layer to the size of 2cm multiplied by 1cm to obtain the positive electrode.
Step 2, preparing a negative electrode:
polishing a zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, and cutting the polished zinc foil to the size of 2cm multiplied by 1cm to obtain the negative electrode.
Step 3, preparing electrolyte:
The high water retention dual-network hydrogel electrolyte prepared in example 2 was cut to a size of 1.5cm×1cm to obtain an electrolyte.
Step 4, composing a zinc-air battery:
And sequentially superposing the positive electrode, the electrolyte and the negative electrode which are obtained through the preparation to form a sandwich structure, and then fixing the sandwich structure by using a breathable adhesive tape to obtain the zinc-air battery.
Example 6
The embodiment provides a zinc-air battery, which is prepared by the following steps:
step 1, preparing a positive electrode:
1) Respectively adding 0.8g of manganese dioxide, 0.1g of conductive carbon black and 0.1g of polyvinylidene fluoride into a mortar, dropwise adding 5mL of N-methylpyrrolidone, grinding and uniformly mixing to obtain active slurry.
2) And (3) coating the active slurry prepared in the step (1) on foam nickel with the thickness of 1.5mm, drying to form an active material layer on a current collector, and cutting the active material layer to the size of 2cm multiplied by 1cm to obtain the positive electrode.
Step 2, preparing a negative electrode:
polishing a zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, and cutting the polished zinc foil to the size of 2cm multiplied by 1cm to obtain the negative electrode.
Step 3, preparing electrolyte:
the high water retention dual-network hydrogel electrolyte prepared in example 3 was cut to a size of 1.5cm×1cm to obtain an electrolyte.
Step 4, composing a zinc-air battery:
And sequentially superposing the positive electrode, the electrolyte and the negative electrode which are obtained through the preparation to form a sandwich structure, and then fixing the sandwich structure by using a breathable adhesive tape to obtain the zinc-air battery.
Comparative example 1
This comparative example provides a hydrogel electrolyte, and it is prepared by the steps of:
Step 1, 5g of acrylic acid was added dropwise to 10mL of a sodium hydroxide solution having a concentration of 6mol/L, and stirred at a stirring rate of 50r/min for 1min to obtain a mixed solution A.
Step 2, adding 3g of acrylamide to the mixed solution A obtained in the step 1, and stirring for 10min at a stirring rate of 100r/min to obtain a mixed solution B.
Step 3, adding 30mgN 'N' methylene bisacrylamide into the mixed solution B prepared in the step 2, and stirring for 120min at a stirring rate of 150 r/min; then, 1mL of an aqueous ammonium persulfate solution having a mass concentration of 30mg/mL was stirred at a stirring rate of 50r/min for 10smin to obtain a mixed solution C.
And 4, transferring the mixed solution C prepared in the step 3 into a polytetrafluoroethylene mould, and then placing the polytetrafluoroethylene mould containing the mixed solution C in a vacuum drying oven at 60 ℃ for 3 hours, so that the mixed solution C is thermally initiated and crosslinked to form gel through heat treatment, and a composite hydrogel matrix is obtained.
And 5, completely immersing the composite hydrogel matrix prepared in the step 4 in a 6mol/L potassium hydroxide solution, immersing at room temperature for 48 hours, and taking out to obtain the double-network hydrogel electrolyte with high water retention.
Namely, this comparative example is different from example 1 only in that:
In this comparative example, sodium chloride was not added.
The high water retention dual network hydrogel electrolyte of this comparative example is abbreviated PANa +pam.
Comparative example 2
This comparative example provides a hydrogel electrolyte, and it is prepared by the steps of:
Step 1, 5g of acrylic acid was added dropwise to 10mL of a sodium hydroxide solution having a concentration of 6mol/L, and stirred at a stirring rate of 50r/min for 1min to obtain a mixed solution A.
Step 2, adding 30mgN 'N' methylene bisacrylamide into the mixed solution A prepared in the step 1, and stirring for 120min at a stirring rate of 150 r/min; then, 1mL of an aqueous ammonium persulfate solution having a mass concentration of 30mg/mL was stirred at a stirring rate of 50r/min for 10smin to obtain a mixed solution B.
And 3, transferring the mixed solution B prepared in the step2 into a polytetrafluoroethylene mould, and then placing the polytetrafluoroethylene mould containing the mixed solution C in a vacuum drying oven at 60 ℃ for 3 hours, so that the mixed solution C is thermally initiated and crosslinked to form gel through heat treatment, and a composite hydrogel matrix is obtained.
And 4, completely immersing the composite hydrogel matrix prepared in the step 3 in a 6mol/L potassium hydroxide solution, immersing at room temperature for 48 hours, and taking out to obtain the double-network hydrogel electrolyte with high water retention.
Namely, this comparative example is different from example 1 only in that:
In this comparative example, neither sodium chloride nor acrylamide was added.
The high water retention dual network hydrogel electrolyte of this comparative example is abbreviated PANa.
Comparative example 3
This comparative example provides a zinc air cell and is made by the steps of:
step 1, preparing a positive electrode:
1) Respectively adding 0.8g of manganese dioxide, 0.1g of conductive carbon black and 0.1g of polyvinylidene fluoride into a mortar, dropwise adding 5mL of N-methylpyrrolidone, grinding and uniformly mixing to obtain active slurry.
2) And (3) coating the active slurry prepared in the step (1) on foam nickel with the thickness of 1.5mm, drying to form an active material layer on a current collector, and cutting the active material layer to the size of 2cm multiplied by 1cm to obtain the positive electrode.
Step 2, preparing a negative electrode:
polishing a zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, and cutting the polished zinc foil to the size of 2cm multiplied by 1cm to obtain the negative electrode.
Step 3, preparing electrolyte:
The high-water-retention dual-network hydrogel electrolyte prepared in comparative example 1 was cut to a size of 1.5cm×1cm to obtain an electrolyte.
Step 4, composing a zinc-air battery:
And sequentially superposing the positive electrode, the electrolyte and the negative electrode which are obtained through the preparation to form a sandwich structure, and then fixing the sandwich structure by using a breathable adhesive tape to obtain the zinc-air battery.
Namely, this comparative example differs from example 4 only in that:
In this comparative example, the electrolyte material used was the high water retention dual network hydrogel electrolyte prepared in comparative example 1.
Comparative example 4
This comparative example provides a zinc air cell and is made by the steps of:
step 1, preparing a positive electrode:
1) Respectively adding 0.8g of manganese dioxide, 0.1g of conductive carbon black and 0.1g of polyvinylidene fluoride into a mortar, dropwise adding 5mL of N-methylpyrrolidone, grinding and uniformly mixing to obtain active slurry.
2) And (3) coating the active slurry prepared in the step (1) on foam nickel with the thickness of 1.5mm, drying to form an active material layer on a current collector, and cutting the active material layer to the size of 2cm multiplied by 1cm to obtain the positive electrode.
Step 2, preparing a negative electrode:
polishing a zinc foil with the thickness of 0.1mm by using sand paper to remove impurities and oxides on the surface of the zinc foil, and cutting the polished zinc foil to the size of 2cm multiplied by 1cm to obtain the negative electrode.
Step 3, preparing electrolyte:
The high-water-retention dual-network hydrogel electrolyte prepared in comparative example 2 was cut to a size of 1.5cm×1cm to obtain an electrolyte.
Step 4, composing a zinc-air battery:
And sequentially superposing the positive electrode, the electrolyte and the negative electrode which are obtained through the preparation to form a sandwich structure, and then fixing the sandwich structure by using a breathable adhesive tape to obtain the zinc-air battery.
Namely, this comparative example differs from example 4 only in that:
In this comparative example, the electrolyte material used was the high water retention dual network hydrogel electrolyte prepared in comparative example 2.
Experimental part
(One) Water Retention test
The present invention was subjected to water retention tests at room temperature and 75 ℃ respectively using the hydrogel electrolyte materials prepared in example 1 and comparative examples 1 and 2 as an example, and the test results are shown in fig. 2 and 3.
The water-retaining property testing method of the invention comprises the following steps:
The hydrogel electrolyte materials prepared in example 1 and comparative examples 1 and 2 were placed in a vacuum drying oven at 75 ℃ in a dry and sealed environment, respectively, the mass of the gel test gel was taken out every 30 minutes, the initial mass was m, the measured mass was taken out every 30 minutes, the mass was m 1, and the water retention rate R of the gel taken out every 30 minutes was calculated according to formula I.
Fig. 2 is a water retention test result of the hydrogel electrolyte materials prepared in example 1 and comparative examples 1 and 2 at normal temperature, and the test result of fig. 2 shows that the water retention effect of example 1 is optimal, the water retention effect of comparative example 1 is inferior, and the water retention effect of comparative example 2 is worst after testing for 140 hours at normal temperature. And it is known from the water retention effects of comparative examples 1 and 2 that the gel of the double network structure is more excellent than that of the single network. As is evident from the water retention effects of comparative examples 1 and 1, the addition of NaCl effectively improved the water retention effect of the gel. The invention can improve the water retention effect of the hydrogel material, and is realized by the combination of the built gel double-network structure and NaCl through organic cooperation.
Fig. 3 is a water retention test result at 75 ℃ for the hydrogel electrolyte materials prepared in example 1 and comparative examples 1 and 2, and the test result of fig. 3 shows that the water retention effect of example 1 is optimal, the water retention effect of comparative example 1 is inferior, and the water retention effect of comparative example 2 is worst after testing at 75 ℃ for 1.5 hours. The invention can improve the water retention effect of the hydrogel material, and is realized by the combination of the built gel double-network structure and NaCl through organic cooperation.
(II) gel conductivity test
The alternating current impedance of the hydrogel electrolyte materials prepared in example 1, comparative example 1 and comparative example 2 was tested by using Shanghai Chenhua CHI600E electrochemical workstation, and the test results are shown in FIG. 4.
The alternating current impedance test conditions of the invention are: the frequency ranges from 100kHz to 0Hz, and the voltage amplitude is 5mV.
And it can be seen from the test results of fig. 4 that the results of the volume resistance R b of the intersection points of the three electrolytes of example 1, and comparative examples 1 and 2 with the X-axis vary. And the result of the R b value is: PANa > PANa +PAM > PANa +PAM+NaCl. The addition of PAM forms double-network hydrogel and the addition of NaCl can even effectively reduce the impedance value of gel electrolyte.
According to the test results of fig. 4, gel conductivities σ corresponding to example 1, comparative example 1 and comparative example 2 are calculated according to formula II, respectively.
And the calculation results are summarized as shown in fig. 5.
Wherein d is the thickness of the electrolyte;
A is the surface area of the electrolyte.
And the test results of fig. 5 show that: the gel conductivity of example 1 is superior to those of comparative examples 1 and 2, and it is understood from the gel conductivities of comparative examples 1 and 2 that the gel of the double network structure is more excellent than that of the single network. As can be seen from the gel conductivities of comparative example 1 and comparative example 1, the addition of NaCl effectively increases the conductivity of the gel. The invention can improve the conductivity of the hydrogel material, and is realized by the combination of the built gel double-network structure and the addition of NaCl through organic cooperation.
(III) charge and discharge testing of Zinc-air Battery
The zinc-air batteries prepared in example 4, comparative example 3 and comparative example 4 were subjected to charge and discharge tests by using a Shenzhen Xinwei CT-400 charge and discharge tester, and the test results are shown in FIG. 6.
And the test results of fig. 6 show that: the zinc-air cells prepared in example 4, comparative example 3 and comparative example 4 were each capable of stable discharge in the current density range of 0.1 to 10mA cm -2, indicating that the zinc-air cells prepared in example 4, comparative example 3 and comparative example 4 were each capable of stable discharge in the large current density range and had good reversibility.
(IV) Long cycle performance test of charging and discharging
The present invention was carried out using the zinc-air cells prepared in example 4, comparative example 3 and comparative example 4 as an example, and a charge-discharge long cycle test was carried out at a current density of 2mA cm -2 for 20min as one cycle, and the test results are shown in FIG. 7.
And the test results of fig. 7 show that: the cycle time of the zinc-air cell of comparative example 4 was 65h, the cycle time of the zinc-air cell of comparative example 3 was 80h, and the cycle time of the zinc-air cell of example 4 was 110h, indicating that the addition of the constructed gel double-network structure and NaCl not only can improve the water retention effect of the hydrogel, but also can improve the cycle life of the cell.
It should be apparent that the embodiments described above are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the double-network hydrogel electrolyte with high water retention is characterized by comprising the following steps of:
Dropwise adding acrylic acid into a sodium hydroxide solution, and stirring and uniformly mixing to obtain a mixed solution A;
Dispersing acrylamide and sodium chloride in the mixed solution A in sequence to obtain a mixed solution B;
Dispersing a cross-linking agent and an initiator in the mixed solution B in sequence to obtain a mixed solution C;
Carrying out heat treatment on the mixed solution C at 50-70 ℃ to thermally initiate crosslinking of the mixed solution C to form gel through heat treatment, so as to obtain a composite hydrogel matrix;
Immersing the composite hydrogel matrix in potassium hydroxide solution, carrying out immersing treatment, and taking out after the immersing is finished, thus obtaining the high-water-retention double-network hydrogel electrolyte.
2. The method according to claim 1, wherein the mass ratio of sodium hydroxide in the sodium hydroxide solution to the acrylic acid is 10 to 20:5 to 10.
3. The method according to claim 1, wherein the ratio of the sodium chloride to the mixed solution A is 0.5 to 1 mol/1L.
4. The preparation method according to claim 1, wherein the mass ratio of the acrylamide to the acrylic acid in the mixed solution A is 1-3:5-10.
5. The method of claim 1, wherein the cross-linking agent is N' N-methylenebisacrylamide;
and the dosage of the cross-linking agent is 0.1 to 0.15 weight percent of the mass of the mixed solution B.
6. The method of manufacture of claim 1 wherein the initiator is ammonium persulfate;
and the dosage of the initiator is 0.1 to 0.2 weight percent of the mass of the mixed solution B.
7. The method according to claim 1, wherein the concentration of the potassium hydroxide solution is 6 to 7.5mol/L.
8. The process according to claim 1, wherein the concentration of sodium hydroxide in the sodium hydroxide solution is 6 to 8mol/L.
9. A high water retention dual network hydrogel electrolyte prepared by the method of any one of claims 1-8.
10. Use of the high water retention dual network hydrogel electrolyte of claim 9 in the preparation of a zinc air cell.
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