CN110581315A - Preparation method of high-strength alkaline polymer electrolyte - Google Patents
Preparation method of high-strength alkaline polymer electrolyte Download PDFInfo
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- CN110581315A CN110581315A CN201910892935.8A CN201910892935A CN110581315A CN 110581315 A CN110581315 A CN 110581315A CN 201910892935 A CN201910892935 A CN 201910892935A CN 110581315 A CN110581315 A CN 110581315A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method of a high-strength alkaline polymer electrolyte, which comprises the steps of weighing a certain amount of polyvinyl alcohol and tara gum, dissolving the polyvinyl alcohol and the tara gum in water, heating and stirring the polyvinyl alcohol and the tara gum at 85 ~ 100 ℃ for 0.5 ~ 4h to obtain a stable solution A, weighing a certain amount of alkali and dissolving the alkali in water to obtain a stable solution B, adding the solution B into the solution A, stirring the solution B to obtain a stable mixed solution, pouring the mixed solution into a mold, freezing the mixed solution at-20 ℃ for 10 ~ 24h, taking the mixed solution out, unfreezing the mixed solution at 4 ℃ of ~ 30 ℃ for 2 ~ 6h, and circulating the mixed solution for 1 ~ 10 times to obtain the polymer electrolyte.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a method for preparing a high-strength alkaline polymer electrolyte by using polyvinyl alcohol and tara gum.
Background
The research begins with the discovery of the conductivity of polyethylene oxide (PEO) and alkali metal ion complexes by Wright et al in 1973, and Armand et al in 1979 indicate that the ionic conductivity of PEO/alkali metal salt complexes reaches 10 at 40 ~ 60 ℃ C-5s/cm, can be used as the electrolyte of the lithium ion battery.
Since then, polymer electrolytes have rapidly developed. The polymer gel electrolyte has the characteristics of stability, plasticity, non-fluidity and the like of a solid electrolyte, and has high ionic conductivity of a liquid electrolyte. The gel electrolyte battery has many incomparable advantages such as small self-discharge rate, long service life, safety and reliability. In terms of battery applications, most of the current research is still focused on lithium ion polymer batteries or proton exchange membrane fuel cells, and the research on alkaline polymer electrolytes is less reported. The alkaline polymer electrolyte has high room-temperature conductivity (the room-temperature conductivity is generally 10)-3～10-2S/cm), easy synthesis, low cost, abundant raw materials, and the like, and has potential application value in metal-air batteries, alkaline secondary batteries, alkaline fuel cells, supercapacitors, and the like, and thus has become a research hotspot in recent years.
Basic polymer electrolytes are mainly of 3 types: PAA (polyacrylic acid) based, PEO based and PVA based. The PAA-based alkaline polymer electrolyte has the highest conductivity, but the practical application of the electrolyte is greatly limited due to poor mechanical strength. The PEO-based polymer electrolyte has low room-temperature conductivity due to high crystallinity, and cannot meet the requirements of practical battery electrolytes (up to 10)-3s/cm or more). The PVA-based polymer electrolyte has high ionic conductivity, good mechanical property and low costIs cheap, thus becoming a research hotspot.
The current electronic products develop towards the portable and wearable directions, the use conditions are complex, and the requirements on the electrolyte, such as conductivity, circulation stability and the like, and higher requirements on the strength are also provided. The gel polymer electrolyte contains a large amount of solvent, and the strength is generally poor, so that the method has practical significance for improving the strength of the gel polymer electrolyte by taking measures. The existing commonly used strengthening method mainly comprises the steps of preparing topological structure gel, nano composite gel, double-network gel and the like, wherein when the double-network gel is stretched, a first layer network becomes rigid and brittle due to a swelling effect, so that the first layer network is broken firstly, after the first layer network reaches a yield point, a large amount of first layer networks are broken and generate a thin neck phenomenon, a second layer network is used for bridging the broken first layer network to maintain the integrity of the gel, and the force applied to the gel is dissipated through the large amount of breakage of the first layer network, so that the double-network hydrogel is endowed with high mechanical properties. Based on the concept of reinforcing and toughening by the double-network structure, many other gels with high mechanical properties are also developed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a high-strength alkaline polymer electrolyte, the prepared electrolyte is a gel polymer electrolyte with high strength and high conductivity, and the electrolyte has cheap raw materials and simple preparation.
In order to solve the technical problems, the invention adopts the following technical scheme:
The method for preparing the high-strength gel polymer electrolyte by using the double-network gel structure formed by the polyvinyl alcohol and the tara gum comprises the following steps:
(1) Weighing a certain amount of polyvinyl alcohol and tara gum, dissolving in water, heating and stirring at 85 ~ 100 deg.C and 100 deg.C for 2 ~ 4h to obtain a stable solution, weighing a certain amount of alkali, dissolving in water to obtain a stable solution, adding the alkali solution into the polyvinyl alcohol solution, and stirring to obtain a stable solution.
(2) And pouring the mixed solution into a mold, freezing at-20 ℃ for 10 ~ 24h, taking out, and unfreezing at 4 ℃ and ~ 30 ℃ for 2 ~ 6h to obtain the polymer electrolyte membrane after 1 ~ 10 times of freezing-unfreezing cycle.
The molecular weight range of the polyvinyl alcohol in the step (1) is 6 ten thousand ~ 15 ten thousand, the alcoholysis degree is 95 ~ 99% and the mass concentration of the polyvinyl alcohol in the hydrogel is 5% ~ 20%.
The mass ratio of the tara gum to the polyvinyl alcohol in the step (1) is 5:100 ~ 30:100
the alkali in the step (1) is one or more of potassium hydroxide, sodium hydroxide and lithium hydroxide, and the molar concentration of the alkali in the mixed solution is 1 ~ 9 mol/L.
The water used in the step (1) is distilled water or deionized water.
The invention has the beneficial effects that: the polyvinyl alcohol and the tara gum prepared by the method form a double-network gel structure, the first network is formed by the polyvinyl alcohol through freezing and thawing circulation, the second network is formed by ion crosslinking, and the mechanical strength of the gel polymer electrolyte is improved through the double networks.
The polymer electrolyte has high strength, and can meet the requirements of wearable energy storage equipment; two networks of the double network are physically crosslinked, no crosslinking agent and initiator are needed, and the system is pure.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The preparation method of the high-strength alkaline polymer electrolyte of the embodiment is as follows:
Weighing 5g of polyvinyl alcohol (with the molecular weight of 6 ten thousand and the alcoholysis degree of 98%) and 1.5g of tara gum, dissolving in 70g of deionized water, and heating and stirring at 95 ℃ for 4 hours to obtain a stable solution; weighing 5.6g of potassium hydroxide and dissolving in 30g of deionized water to obtain a stable solution; adding the potassium hydroxide solution into the polyvinyl alcohol solution and stirring to obtain a stable solution. Pouring the mixed solution into a mold, freezing at-20 ℃ for 18h, taking out, thawing at 4 ℃ for 3h, and performing a freezing-thawing cycle for 10 times to obtain the polymer electrolyte membrane.
The obtained alkaline polymer electrolyte membrane has the conductivity of 0.025S/cm, the tensile strength of 0.06MPa and the elongation at break of 4.2 mm/mm.
Example 2
The preparation method of the high-strength alkaline polymer electrolyte of the embodiment is as follows:
Weighing 20g of polyvinyl alcohol (with the molecular weight of 15 ten thousand and the alcoholysis degree of 95%) and 2g of tara gum, dissolving in 70g of deionized water, and heating and stirring at 98 ℃ for 3h to obtain a stable solution; weighing 8g of sodium hydroxide and 16.8g of lithium hydroxide, and dissolving in 30g of deionized water to obtain a stable solution; adding the alkali solution into the polyvinyl alcohol solution and stirring to obtain a stable solution. Pouring the mixed solution into a mold, freezing at-20 ℃ for 10h, taking out, thawing at 30 ℃ for 2h, and performing 5 times of freezing-thawing cycle to obtain the polymer electrolyte membrane.
the obtained alkaline polymer electrolyte membrane has the conductivity of 0.082S/cm, the tensile strength of 1.33MPa and the elongation at break of 8.5 mm/mm.
Example 3
the preparation method of the high-strength alkaline polymer electrolyte of the embodiment is as follows:
Weighing 15g of polyvinyl alcohol (with the molecular weight of 7.5 ten thousand and the alcoholysis degree of 98%) and 1.5g of tara gum, dissolving in 70g of deionized water, and heating and stirring at 90 ℃ for 2 hours to obtain a stable solution; weighing 39.2g of potassium hydroxide, and dissolving in 30g of deionized water to obtain a stable solution; adding the potassium hydroxide solution into the polyvinyl alcohol solution and stirring to obtain a stable solution. Pouring the mixed solution into a mold, freezing for 24h at-20 ℃, taking out, thawing for 4h at 4 ℃, and performing freeze-thaw cycle for 3 times to obtain the polymer electrolyte membrane.
The obtained alkaline polymer electrolyte membrane had an electrical conductivity of 0.19S/cm, a tensile strength of 2.08 MPa, and an elongation at break of 11.58 mm/mm.
Example 4
The preparation method of the high-strength alkaline polymer electrolyte of the embodiment is as follows:
Weighing 12g of polyvinyl alcohol (with the molecular weight of 15 ten thousand and the alcoholysis degree of 99%) and 0.6g of tara gum, dissolving in 70g of deionized water, and heating and stirring at 100 ℃ for 0.5h to obtain a stable solution; 28.05g of potassium hydroxide is weighed and dissolved in 30g of deionized water to obtain a stable solution; adding the potassium hydroxide solution into the polyvinyl alcohol solution and stirring to obtain a stable solution. Pouring the mixed solution into a mold, freezing at-20 ℃ for 12h, taking out, thawing at 25 ℃ for 3h, and performing a freezing-thawing cycle for 6 times to obtain the polymer electrolyte membrane.
The obtained alkaline polymer electrolyte membrane had an electrical conductivity of 0.105S/cm, a tensile strength of 1.83 MPa, and an elongation at break of 15.6 mm/mm.
Example 5
The preparation method of the high-strength alkaline polymer electrolyte of the embodiment is as follows:
Weighing 10g of polyvinyl alcohol (with the molecular weight of 8 ten thousand and the alcoholysis degree of 98%) and 2g of tara gum, dissolving the mixture in 70g of distilled water, and heating and stirring the mixture at 95 ℃ for 2 hours to obtain a stable solution; weighing 33.66g of potassium hydroxide and dissolving in 30g of distilled water to obtain a stable solution; adding the potassium hydroxide solution into the polyvinyl alcohol solution and stirring to obtain a stable solution. Pouring the mixed solution into a mold, freezing at-20 ℃ for 24h, taking out, thawing at 4 ℃ for 4h, and performing freeze-thaw cycle for 1 time to obtain the polymer electrolyte membrane.
the obtained alkaline polymer electrolyte membrane had an electrical conductivity of 0.122S/cm, a tensile strength of 0.13MPa, and an elongation at break of 3.7 mm/mm.
The reagents and starting materials used in the examples are conventional materials commercially available.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for preparing a high-strength alkaline polymer electrolyte, characterized by comprising the steps of:
(1) Weighing a certain amount of polyvinyl alcohol and tara gum, dissolving the polyvinyl alcohol and the tara gum in water, heating and stirring the solution at 85 ~ 100 ℃ for 0.5 ~ 4h to obtain a stable solution A, weighing a certain amount of alkali, dissolving the alkali in the water to obtain a stable solution B, adding the solution B into the solution A, and stirring the solution B to obtain a stable mixed solution;
(2) And pouring the mixed solution into a mold, freezing for 10 ~ 24h at-20 ℃, taking out, and unfreezing for 2 ~ 6h at ~ 30 ℃ at 4 ℃ for 1 ~ 10 times as a freezing-unfreezing cycle to obtain the polymer electrolyte.
2. The method according to claim 1, wherein the polyvinyl alcohol has a molecular weight of 6 ten thousand ~ 15 ten thousand, an alcoholysis degree of 95 ~ 99%, and a mass concentration of 5% to ~ 20% in the mixed solution.
3. The preparation method according to claim 1, wherein the mass ratio of the tara gum to the polyvinyl alcohol is 5:100 ~ 30: 100.
4. the preparation method according to claim 1, wherein the alkali is one or more of potassium hydroxide, sodium hydroxide and lithium hydroxide, and the molar concentration of the alkali in the mixed solution is 1 ~ 9 mol/L.
5. the method of claim 1, wherein: the water is distilled water or deionized water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112259832A (en) * | 2020-09-24 | 2021-01-22 | 江苏理工学院 | Preparation method and application of graphene-modified all-solid-state electrolysis |
| CN112713293A (en) * | 2021-01-25 | 2021-04-27 | 郑州大学 | High-conductivity gel polymer electrolyte applied to aluminum-air battery and preparation method and application thereof |
| JP2023512375A (en) * | 2020-02-14 | 2023-03-27 | カウンシル・オブ・サイエンティフィック・アンド・インダストリアル・リサーチ・アン・インディアン・レジスタード・ボディ・インコーポレイテッド・アンダー・ザ・レジストレーション・オブ・ソサエティーズ・アクト・(アクト・21・オブ・1860) | Functional transparent gel electrolyte system and its fast switching electrochromic/electrochemical device |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2023512375A (en) * | 2020-02-14 | 2023-03-27 | カウンシル・オブ・サイエンティフィック・アンド・インダストリアル・リサーチ・アン・インディアン・レジスタード・ボディ・インコーポレイテッド・アンダー・ザ・レジストレーション・オブ・ソサエティーズ・アクト・(アクト・21・オブ・1860) | Functional transparent gel electrolyte system and its fast switching electrochromic/electrochemical device |
| JP7402311B2 (en) | 2020-02-14 | 2023-12-20 | カウンシル・オブ・サイエンティフィック・アンド・インダストリアル・リサーチ・アン・インディアン・レジスタード・ボディ・インコーポレイテッド・アンダー・ザ・レジストレーション・オブ・ソサエティーズ・アクト・(アクト・21・オブ・1860) | Functional transparent gel electrolyte system and its high-speed switching electrochromic/electrochemical device |
| CN112259832A (en) * | 2020-09-24 | 2021-01-22 | 江苏理工学院 | Preparation method and application of graphene-modified all-solid-state electrolysis |
| CN112259832B (en) * | 2020-09-24 | 2021-09-28 | 江苏理工学院 | Preparation method and application of graphene-modified all-solid-state electrolysis |
| CN112713293A (en) * | 2021-01-25 | 2021-04-27 | 郑州大学 | High-conductivity gel polymer electrolyte applied to aluminum-air battery and preparation method and application thereof |
| CN112713293B (en) * | 2021-01-25 | 2022-05-10 | 郑州大学 | High-conductivity gel polymer electrolyte applied to aluminum-air battery and preparation method and application thereof |
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