Low-temperature electrolyte for supercapacitor and preparation method thereof

A technology for electrolyte preparation and supercapacitors, applied in capacitors, electrolytic capacitors, circuits, etc., can solve problems such as low solubility, space constraints on energy density of supercapacitors, toxicity, etc.

Inactive Publication Date: 2009-12-02
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The application of AN-based electrolytes is increasingly limited due to the toxicity and volatility of AN
TEABF 4 PC solvent in PC-based electrolyte is less toxic, but due to TEABF 4 The solubility in carbonate solvents is low (the solubility in PC at 25°C is 1mol / L), especially at low temperatures, the solubility of this ammonium salt in carbonate solvents is lower, which restricts the improvement of the energy density of supercapacitors at low temperatures Space

Method used

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  • Low-temperature electrolyte for supercapacitor and preparation method thereof
  • Low-temperature electrolyte for supercapacitor and preparation method thereof
  • Low-temperature electrolyte for supercapacitor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Using SiCl 4 , anhydrous oxalic acid, etc. to prepare TEAODFB in acetonitrile solution.

[0026] Step 1 Take 30.29g TEABF with an electronic balance in the glove box 4 , 12.55g of anhydrous oxalic acid was charged into a 500mL three-necked flask. Weigh 8mL SiCl with a 10mL graduated cylinder 4 Fill into a dropper bottle. TEABF 4 and anhydrous oxalic acid dissolved in 300mL acetonitrile, SiCl 4 Add dropwise during electromagnetic stirring. The reaction process was protected by high-purity argon at 20°C. SiCl 4 Adding is completed in about 6 hours, and then stirred for 10 hours after adding, the sign of the end of the reaction is that no gas is produced, and it is checked with pH test paper.

[0027] Step 2 Use a rotary evaporator to evaporate and concentrate the reacted solution at 35° C. until no liquid vapor is generated to obtain 27.7 g of the product.

[0028] Detection method: detect product purity with ICP, record the purity of product and be 99.28%, test ...

Embodiment 2

[0031] Using SiCl 4 , anhydrous oxalic acid, etc. to prepare TEAODFB in acetonitrile solution.

[0032] The steps are the same as in Example 1.

[0033] Step 2: Methyl formate was added according to the molar ratio of solvent and crystallizer of 12:1, the mixed solvent was recrystallized at -20°C for several times at low temperature, and 26.8 g of white crystals were obtained by filtration.

[0034] With example one, gained product is analyzed, and the result shows: the purity of product is 99.3%, moisture content (in H 2 O meter) is 8ppm.

Embodiment 3

[0036] Using SiCl 4 , anhydrous oxalic acid, etc. to prepare TEAODFB in PC+DMC solvent.

[0037] Step 1 Take 30.29g TEABF with an electronic balance in the glove box 4 , 12.55g of anhydrous oxalic acid was charged into a 500mL three-necked flask. Weigh 8mL SiCl with a 10mL graduated cylinder 4 Fill into a dropper bottle. TEABF 4 and anhydrous oxalic acid dissolved in 300mL PC+DMC (volume ratio 5:1) solution, SiCl4 Add dropwise during electromagnetic stirring. The reaction process was protected by high-purity argon at 10°C. SiCl 4 Adding is completed in about 6 hours, and then stirred for 10 hours after adding, the sign of the end of the reaction is that no gas is produced, and it is checked with pH test paper.

[0038] Step 2 Add methanol according to the molar ratio of solvent and crystallizer at 10:1, carry out multiple low-temperature recrystallizations on the mixed solvent at -30°C, and filter to obtain 26.2 g of white crystals.

[0039] With example one, gained pr...

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Abstract

The invention discloses low-temperature electrolyte for a supercapacitor and a preparation method thereof. The electrolyte comprises solute and non-aqueous organic solvent. The solute is ionic liquid tetraethylammonium-oxalate-difluoro-borate (TEAODFB) which is battery-grade TEAODFB obtained by purifying a product of reaction of a chlorine-containing compound, an oxalate-containing compound and a fluoroboric acid containing compound in acetonitrile or carbonic ester medium by adopting a method of reduced pressure evaporation or low-temperature recrystallization. The non-aqueous organic solvent is one or the combination of acetonitrile, propionitrile, methoxy propionitrile, ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, gamma-butyrolactone, N,N-dimetbylformamide, tetrahydrofuran and sulfolane. The concentration of the adopted electrolyte is 0.8 to 2mol/L. The obtained low-temperature electrolyte has high specific capacity and charge/discharge cyclic life at the temperature of 30 DEG C below zero.

Description

technical field [0001] The invention relates to the field of supercapacitors, in particular to a low-temperature electrolyte for supercapacitors and a preparation method thereof. Background technique [0002] With the rapid growth of population and the rapid development of social economy, resources and energy are becoming increasingly scarce, and the ecological environment is deteriorating. Human beings will rely more on clean and renewable new energy. Supercapacitors have excellent charge and discharge performance and large-capacity energy storage performance, and have the advantages of fast charging, long cycle life, strong environmental adaptability, no memory effect, maintenance-free, and no pollution to the environment. Global demand has grown rapidly since its launch , has become a new industrial highlight in the field of chemical power sources, and has increasingly broad application prospects in the fields of computers, communications, electric power, transportation, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G9/035
CPCY02E60/13
Inventor 张治安赖延清李劼陈绪杰高宏权郝新
Owner CENT SOUTH UNIV
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