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Preparation method of ion liquid crystal/polyimidazole semi-interpenetrating network polymer electrolyte

A semi-interpenetrating network, ionic liquid crystal technology, which is applied in the field of preparation of all-solid polymer electrolytes, can solve the problems of high investment cost and low energy consumption, and achieves the effects of simple and convenient operation, fast polymerization speed, and suitability for industrial applications.

Active Publication Date: 2018-04-20
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Radiation initiation can directly initiate the polymerization reaction, avoiding the introduction of impurities due to the addition of initiators. Compared with thermal polymerization initiation, the reaction is more thorough, and the energy consumption is low, but the investment cost is high

Method used

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  • Preparation method of ion liquid crystal/polyimidazole semi-interpenetrating network polymer electrolyte
  • Preparation method of ion liquid crystal/polyimidazole semi-interpenetrating network polymer electrolyte
  • Preparation method of ion liquid crystal/polyimidazole semi-interpenetrating network polymer electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Preparation of n-hexyl methacrylate-3-butylimidazolium bromide (MOBIm-Br):

[0040] Under the condition of ice bath, in a 250mL three-necked flask with a stirring bar, under N 2 Under the atmosphere, add 9g of 6-bromo-n-hexanol mixed solution dissolved in 30mL of dichloromethane, after stirring for 0.5h, slowly add 5.25g of triethylamine mixed solution dissolved in 30mL of dichloromethane (about 1 drop / second), add After stirring for 0.5h, add dropwise 4.9g of methacryloyl chloride dissolved in 30mL of dichloromethane and stir for 0.5h, then remove the ice area. Stir at room temperature for 18h. After the reaction was completed, suction filtered, and then 30 mL of deionized water was added to wash the filtrate for 4 times. Remove the water layer, add 3g of anhydrous magnesium sulfate to the organic layer for drying, after suction filtration, pour the liquid into a 250mL single-necked round-bottom flask and spin dry under vacuum, and spin dry with solvent to prepare 1-...

Embodiment 2

[0042] Imidazole liquid (MOBIm-BF 4 ) preparation:

[0043] (1) Put 29.7g of 1-n-hexyl methacrylate-3-butylimidazolium bromide in a round bottom flask, add 100mL of deionized water and stir. 7.45g LiBF 4 Dissolve in 30mL of water, add a stir bar and place on a magnetic stirrer to stir for 1h. Drop LiBF 4 The solution was slowly added dropwise to the MOBIm-Br solution. The reaction was stirred at room temperature for 5h.

[0044] (2) After the reaction is complete, extract the organic phase containing the ionic liquid with dichloromethane, and wash the resulting organic phase with deionized water until there is no Br - So far (with 0.1g mol －1 Silver nitrate Ag 2 NO 3 solution testing). Afterwards, add anhydrous magnesium sulfate to remove water, filter with suction, and remove dichloromethane by rotary vacuum evaporation to obtain a brownish-yellow viscous liquid which is the product MOBIm-BF 4 .

Embodiment 3

[0047] To 0.25g MOBIm-BF 4 , 0.0417g[Cmim]BF 4 and 0.0323g LiBF 4 Add 2-hydroxyl-2-methylpropiophenone (1 drop, as an initiator), add 0.5mL acetonitrile and stir for 30min to photopolymerize, then add 0.0833g PEGDA and 2-hydroxyl-2-methylpropiophenone (1 drop, (as an initiator) was added into 0.5 mL of acetonitrile solution for blending, stirred for 30 min, and cured to form a film under ultraviolet light irradiation. Then put it in a vacuum oven for vacuum drying for 24 hours.

[0048] And the product prepared in Example 3 is designated as Sample 1.

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Abstract

The invention relates to the technical field of a battery material, and provides a preparation method of an ion liquid crystal / polyimidazole semi-interpenetrating network polymer electrolyte. The method comprises the steps of taking an imidazole liquid (MOBIm-BF4), polyethylene glycol diacrylate (PEGDA), ion liquid crystal ([Cmin]BF4) and lithium tetrafluoroborate (LiBF4) as raw materials, performing ultraviolet irradiation curing to form a film in an organic solvent under a condition that a photoinitiator participates, and obtaining the cross-linked polymerization semi-interpenetrating network solid-state polymer electrolyte after drying, wherein the MOBIm-BF4 can be photo-initiated and polymerized to obtain polyimidazole, and then photo-initiation polymerization is performed after the polyimidazole, the PEGDA, the [Cmin]BF4 and the LiBF4 are mixed, or photo-initiation polymerization is performed on the MOBIm-BF4, the [Cmin]BF4 and the LiBF4 and then photo-initiation polymerization isperformed after the PEGDA is added for mixing. The method is simple and efficient and is suitable for industrial application. The maximum electrical conductivity of the ion liquid crystal / polyimidazole semi-interpenetrating network polymer electrolyte prepared by the method can reach 10<-5>S cm<-1>.

Description

technical field [0001] The invention relates to the technical field of battery materials, in particular to a preparation process of an all-solid polymer electrolyte. Background technique [0002] Lithium-ion battery is a green high-energy battery that appeared in the 1990s, and has attracted much attention in the fields of energy chemistry and material chemistry. Electrolytes are key materials for lithium-ion batteries. All-solid polymers are used as electrolytes in lithium-ion batteries. Because of its high electrical conductivity, easy processing, safety, and no pollution, it has attracted the attention and attention of researchers in the research community. Coupled with the continuous enhancement of people's awareness of environmental protection, the research on polymer electrolytes is imperative. [0003] According to the existing popular classification methods, polymer electrolytes can be divided into three categories: dry polymer electrolytes, gel polymer electrolyt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0565H01M10/0525
CPCH01M10/0525H01M10/0565H01M2300/0082H01M2300/0091Y02E60/10
Inventor 谢宇陈玺茜童永芬许裕忠徐波
Owner NANCHANG HANGKONG UNIVERSITY
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