WO2021217682A1 - 一种纯无机胶状体的制备方法及其应用 - Google Patents

一种纯无机胶状体的制备方法及其应用 Download PDF

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WO2021217682A1
WO2021217682A1 PCT/CN2020/088548 CN2020088548W WO2021217682A1 WO 2021217682 A1 WO2021217682 A1 WO 2021217682A1 CN 2020088548 W CN2020088548 W CN 2020088548W WO 2021217682 A1 WO2021217682 A1 WO 2021217682A1
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zinc
colloid
mol
bromide
acetate
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PCT/CN2020/088548
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French (fr)
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高超
褚星远
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杭州高烯科技有限公司
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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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to a preparation method of a pure inorganic colloid.
  • the pure inorganic colloid can work stably at high temperature, and is especially suitable for the field of batteries.
  • Hydrogel is a kind of dispersion system formed by the absorption of water by the spatial network framework.
  • the hydrogel has flexibility and excellent mechanical properties so that it can be used in many fields.
  • the hydrogel can possess ionic conductivity.
  • Hydrogels with ion conductivity can be used as electrolytes and are used in the field of energy storage, especially flexible energy storage devices.
  • the existing hydrogel is composed of polymers, which cannot withstand high temperatures, and the operation of the battery usually causes the temperature of the battery to rise. Therefore, the existing polymer-based hydrogels cannot guarantee the high temperature environment. The normal operation of electrical equipment.
  • An object of the present invention is to provide a method for preparing pure inorganic colloids, which is based on the principle that acetate inhibits the crystallization process and allows inorganic ions in the system to form three-dimensional inorganic polymers, and water is used as a dispersion medium to form colloids.
  • Zinc chloride, zinc bromide and zinc acetate are sequentially put into the dispersion medium, heated to dissolve and then naturally cooled to obtain a zinc chloride-zinc bromide-zinc acetate gel with a total salt concentration of 60-100 mol kg -1 body.
  • the concentration range of zinc chloride is 20-30 mol kg -1
  • the concentration range of zinc bromide is 20-30 mol kg -1
  • the concentration range of zinc acetate is 20-40 mol kg -1 .
  • the colloid prepared by the method has properties similar to hydrogel, and the mixed system in the strain bottle is reversed, and the mixed system will not flow.
  • acetate has a "end-capping" effect, preventing the continuous growth of zinc chloride and zinc bromide crystals, making the system an inorganic three-dimensional polymer.
  • the skeleton uses water as a dispersion medium to form a colloid.
  • the pure inorganic colloid After testing, the pure inorganic colloid has an electrical conductivity of 10 -4 to 10 -3 S m -1 at room temperature. At high temperatures (80 to 100 degrees Celsius), it has a conductivity of 2 ⁇ 10 -4 to 2 ⁇ 10 -3 S m -1.
  • the temperature during the dissolution process is 120 to 130°C.
  • Another object of the present invention is to provide the application of the above-mentioned pure inorganic colloid as a battery colloidal electrolyte.
  • this pure inorganic colloid has advantages similar to hydrogels, and is beneficial to inhibit the growth of zinc dendrites.
  • it does not decompose at high temperature, can maintain ion transmission capacity, and can solve the high temperature stability problem of existing gel batteries.
  • the positive electrode of the battery is made of carbon material
  • the negative electrode is made of metallic zinc, zinc-containing alloy or other inert metals.
  • the carbon materials include carbon nanotubes, natural graphite, expanded graphite, graphene, graphene assemblies, and other carbon materials with a graphite lattice structure.
  • the beneficial effect of the present invention is that the present invention prevents the continuous growth of zinc chloride and zinc bromide crystals through the "end-capping" effect of acetate, so that the system becomes an inorganic three-dimensional polymer.
  • the skeleton uses water as a dispersion medium to form a gel.
  • the shape body on the one hand, maintains the advantages of the polymer colloid, and on the other hand, it can not decompose at high temperature, can maintain the ion transmission capacity, and can solve the high temperature stability problem of the existing gel battery.
  • Figure 1 Aqueous colloid of zinc chloride-zinc bromide-zinc acetate with a total concentration of 60mol kg -1.
  • the concentration is expressed by the ratio of solute to solvent.
  • 60-100 mol kg -1 means that the amount of solute dissolved per kilogram of water is 60-100 mol.
  • the conductivity measured at room temperature is 10 -3 S m -1 .
  • the electrical conductivity measured at 100°C is 2 ⁇ 10 -3 S m -1 .
  • the test method is: stacking the titanium foil, the colloidal sheet and the titanium foil in sequence in the Swaglok battery mold, pressure and heat sealing.
  • the resistance is measured by the AC impedance method, and the conductivity can be obtained by calculation.
  • the battery cell has a mass specific capacity of 80 mAh g -1 (calculated based on the positive electrode active material) at a current density of 0.1 A g -1 at room temperature. At a current density of 0.1A g -1 at 100° C., its mass specific capacity is 102 mAh g -1 (calculated based on the positive electrode active material).
  • the battery cell has a mass specific capacity of 60 mAh g -1 (calculated based on the positive electrode active material) at a current density of 0.1A g -1 at room temperature. At a current density of 0.1A g -1 at 100° C., its mass specific capacity is 75 mAh g -1 (calculated based on the positive electrode active material).
  • the titanium foil current collector no negative electrode, the negative electrode active material is derived from the metal zinc deposited on the titanium foil by the first charge of zinc ions
  • the colloidal sheet and the graphene film positive electrode are sequentially superimposed into the battery mold. Pressure heat sealing.
  • the battery cell has a mass specific capacity of 79 mAh g -1 (calculated based on the positive active material) at a current density of 0.1A g -1 at room temperature. At a current density of 0.1A g -1 at 100° C., its mass specific capacity is 98 mAh g -1 (calculated based on the positive electrode active material).
  • the zinc negative electrode, the colloidal flake and the neutral microsphere graphite positive electrode are sequentially stacked in the battery mold for pressure and heat sealing.
  • the battery cell has a mass specific capacity of 55 mAh g -1 (calculated based on the positive electrode active material) at a current density of 0.1A g -1 at room temperature.
  • its mass specific capacity is 72 mAh g -1 (calculated based on the positive electrode active material).

Abstract

一种纯无机胶状体的制备方法，由氯化锌、溴化锌、醋酸锌在水中溶解获得，所述体系具有任意单一组分不具备的性质，三种组分在水中的总溶解度极高，高于单一的氯化锌、溴化锌或醋酸锌，总浓度可调，可达100mol kg-1。该体系呈类似水凝胶状态，具有离子电导率(10-3S m-1)，高温下保持高电导率，可用作凝胶电池的电解质。以石墨类碳材料为正极，以金属锌、含锌合金或其它惰性金属为负极，以该胶状体为电解质组装成电池，正极比容量可达100mAh g-1。该体系制备简单，成本低廉，性质独特，在储能等领域具有广阔的应用前景。

Description

一种纯无机胶状体的制备方法及其应用 技术领域
本发明涉及一种纯无机胶状体的制备方法，该纯无机胶状体可在高温下稳定工作，尤其适用于电池领域。
背景技术
水凝胶是由空间网状骨架吸水形成的一种分散体系。水凝胶具有柔性，优异的力学性能使其可在许多领域获得应用。一般地，通过引入盐的方法，水凝胶可具备离子导电性。具有离子导电性的水凝胶可做为电解质，在能源储存领域，尤其是柔性储能器件方面获得应用。
然而，现有的水凝胶由聚合物构成其骨架，聚合物无法耐受高温，而电池的运行通常会导致电池温度升高，因此，现有的聚合物基水凝胶无法保证高温环境下电力设备的正常运行。
发明内容
本发明的一个目的在于提供一种纯无机胶状体的制备方法，该方法基于醋酸根抑制结晶过程并使体系内的无机离子形成三维无机高分子，以水为分散介质形成胶状体原理，具体的：将氯化锌、溴化锌和醋酸锌依次到分散介质中，加热溶解后自然冷却，得到盐总浓度为60～100mol kg -1的氯化锌-溴化锌-醋酸锌胶状体。其中，氯化锌的浓度范围为20～30mol kg -1，溴化锌的浓度范围为20～30mol kg -1，醋酸锌的浓度范围为20～40mol kg -1。该方法制备得到的胶状体具有类似水凝胶的性质，将菌种瓶中的该混合体系倒扣，混合体系不会流动。其中，醋酸根具有“封端”作用，阻止氯化锌和溴化锌晶体的不断生长，使体系成为的无机三维高分子，该骨架以水为分散介质形成胶状体。
经测试，该纯无机胶状体室温下具有10 -4～10 -3S m -1的电导率。在高温(80～～100摄氏度)下，具有2×10 -4～2×10 -3S m -1的电导率。
通常的，溶解过程中的温度为120～～130℃。
本发明的另一个目的在于提供上述纯无机胶状体作为电池胶状体电解质的应用，这种纯无机胶状体一方面具有类似于水凝胶的优势，有利于抑制锌枝晶生长，另一方面在高温下不分解，可保持离子传输能力，可以解决现有凝胶电池的高温稳定性问题。
在某些实施例中，所述电池正极为碳材料，负极为金属锌、含锌合金或其它惰性金属。
在某些实施例中，所述碳材料包括碳纳米管、天然石墨、膨胀石墨、石墨烯、石墨烯组装体及其它具有石墨晶格结构的碳材料。
本发明的有益效果在于：本发明通过醋酸根的“封端”作用，阻止氯化锌和溴化锌晶体的不断生长，使体系成为的无机三维高分子，该骨架以水为分散介质形成胶状体，一方面保持高分子胶状体的优势，另一方面可在高温下不分解，可保持离子传输能力，可以解决现有凝胶电池的高温稳定性问题。
附图说明
图1：总浓度为60mol kg -1的氯化锌-溴化锌-醋酸锌水系胶状体。
具体实施方式
下面通过实施例对本发明进行具体描述，本实施例只用于对本发明做进一步的说明，不能理解为对本发明保护范围的限制，本领域的技术人员根据上述发明的内容做出一些非本质的改变和调整，均属于本发明的保护范围。
本发明中，除特别说明，浓度均采用溶质溶剂比表示，60～100mol kg -1指的是每千克水所溶解的溶质的物质的量为60～100mol。
实施例1：
(1)将0.2mol氯化锌、0.2mol溴化锌和0.2mol醋酸锌依次加入到10g去离子水中，加热至120℃溶解，自然冷却至室温后得到总浓度为60mol kg -1的氯化锌-溴化锌-醋酸锌水系胶状体。
(2)将所得胶状体置于一玻璃瓶中，倒置后可见无流动性，见图1，由此可知其具有类似水凝胶的性质。
(3)将0.2mol氯化锌、0.2mol溴化锌和0.2mol醋酸锌依次加入到10g去离子水中，加热至120℃溶解，将可流动的混合体系浇在聚四氟乙烯膜上，其上覆盖第二层聚四氟乙烯膜，压铁块，冷却以获得厚度为0.1mm的胶状薄片。
室温下测得其电导率为10 -3S m -1。100℃下测得其电导率为2×10 -3S m -1。
测试方法为：将钛箔、胶状体薄片和钛箔依次叠加到Swaglok电池模具中加压热封。使用交流阻抗方法测得其电阻，通过计算可得其电导率。
(4)将锌负极、胶状体薄片和石墨烯膜正极依次叠加到Swaglok电池模具中加压热封。经测试，该电池单体，室温时在0.1A g -1的电流密度下，其质量比容量为80mAh g -1(基于正极活性物质计算)。100℃时在0.1A g -1的电流密度下，其质量比容量为102mAh g -1(基于正极活性物质计算)。
实施例2：
(1)将0.3mol氯化锌、0.3mol溴化锌和0.4mol醋酸锌依次加入到10g去离子水中，加热至130℃溶解，自然冷却至室温得到总浓度为100mol kg -1的氯化锌-溴化锌-醋酸锌水系胶状体。
(2)将所得胶状体置于一玻璃瓶中，倒置后可见无流动性。
(3)将0.3mol氯化锌、0.3mol溴化锌和0.4mol醋酸锌依次加入到10g去离子水中，加热至130℃溶解，将可流动的混合体系浇在聚四氟乙烯膜上，其上覆盖第二层聚四氟乙烯膜，压铁块，冷却以获得厚度为0.1mm的胶状薄片。室温下测得其电导率为10 -4S m -1。100℃下测得其电导率为2*10 -4S m -1。测试方法同实施例1。
(4)将锌负极、胶状体薄片和石墨烯膜正极依次叠加到电池模具中加压热封。经测试，该电池单体，室温时在0.1A g -1的电流密度下，其质量比容量为60mAh g -1(基于正极活性物质计算)。100℃时在0.1A g -1的电流密度下，其质量比容量为75mAh g -1(基于正极活性物质计算)。
实施例3：
(1)将0.2mol氯化锌、0.2mol溴化锌和0.2mol醋酸锌依次加入到10g去离子水中，加热至120℃溶解，自然冷却至室温得到总浓度为60mol kg -1的氯化锌-溴化锌-醋酸锌水系胶状体。
(2)将所得胶状体置于一玻璃瓶中，倒置后可见无流动性.。
(3)将0.2mol氯化锌、0.2mol溴化锌和0.2mol醋酸锌依次加入到10g去离子水中，加热至120℃溶解，将可流动的混合体系浇在聚四氟乙烯膜上，其上覆盖第二层聚四氟乙烯膜，压铁块，冷却以获得厚度为0.1mm的胶状薄片。室温下测得其电导率为10 -3S m -1。100℃下测得其电导率为2*10 -3S m -1。测试方法同实施例1。
(4)将钛箔集流体(无负极，负极活性物质来源于第一次充电锌离子在钛箔上沉积得到的金属锌)、胶状体薄片和石墨烯膜正极依次叠加到电池模具中加压热封。经测试，该电池单体，室温时在0.1A g -1的电流密度下，其质量比容量为79mAh g -1(基于正极活性物质计算)。100℃时在0.1A g -1的电流密度下，其质量比容量为98mAh g -1(基于正极活性物质计算)。
实施例4：
(1)将0.3mol氯化锌、0.3mol溴化锌和0.4mol醋酸锌依次加入到10g去离子水中， 加热至120℃溶解，自然冷却至室温得到总浓度为100mol kg -1的氯化锌-溴化锌-醋酸锌水系胶状体。
(2)将所得胶状体置于一玻璃瓶中，倒置后可见无流动性。
(3)将0.3mol氯化锌、0.3mol溴化锌和0.4mol醋酸锌依次加入到10g去离子水中，加热至120℃溶解，将可流动的混合体系浇在聚四氟乙烯膜上，其上覆盖第二层聚四氟乙烯膜，压铁块，冷却以获得厚度为0.1mm的胶状薄片。室温下测得其电导率为10 -4S m -1。100℃下测得其电导率为2×10 -4S m -1。测试方法同实施例1。
(4)将锌负极、胶状体薄片和中向微球石墨正极依次叠加到电池模具中加压热封。经测试，该电池单体，室温时在0.1A g -1的电流密度下，其质量比容量为55mAh g -1(基于正极活性物质计算)。100℃时在0.1A g -1的电流密度下，其质量比容量为72mAh g -1(基于正极活性物质计算)。

Claims (5)

  1. 一种纯无机胶状体的制备方法，其特征在于，该方法为：将氯化锌、溴化锌和醋酸锌到分散水中，加热溶解后冷却，得到盐总浓度为60～100mol kg -1的氯化锌-溴化锌-醋酸锌胶状体。其中，氯化锌的浓度范围为20～30mol kg -1，溴化锌的浓度范围为20～30mol kg -1，醋酸锌的浓度范围为20～40mol kg -1。
  2. 根据权利要求1所述方法制备得到的胶状体，其特征在于，具有10 -4～10 -3S m -1的电导率。
  3. 如权利要求1所述方法制备得到的胶状体作为凝胶电池电解质的应用。
  4. 根据权利要求3所述的应用，其特征在于，所述凝胶电池正极为碳材料，负极为金属锌、含锌合金或其它惰性金属。
  5. 根据权利要求4所述的应用，其特征在于，所述碳材料包括碳纳米管、天然石墨、膨胀石墨、石墨烯、石墨烯组装体及其它具有石墨晶格结构的碳材料。
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