CN111477469B - Preparation method of high-voltage electrolyte and application of high-voltage electrolyte in super capacitor - Google Patents
Preparation method of high-voltage electrolyte and application of high-voltage electrolyte in super capacitor Download PDFInfo
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- CN111477469B CN111477469B CN202010304020.3A CN202010304020A CN111477469B CN 111477469 B CN111477469 B CN 111477469B CN 202010304020 A CN202010304020 A CN 202010304020A CN 111477469 B CN111477469 B CN 111477469B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/60—Liquid electrolytes characterised by the solvent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/62—Liquid electrolytes characterised by the solute, e.g. salts, anions or cations therein
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of electrolyte, and particularly relates to a preparation method of high-voltage electrolyte and application of the high-voltage electrolyte in a super capacitor, wherein the preparation method of the high-voltage electrolyte comprises the following steps: (1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing to obtain an organic solvent mixed solution; (2) weighing ionic liquid and organic solvent mixed liquid, mixing, and performing ultrasonic oscillation and magnetic stirring to obtain the ionic liquid; the invention takes the mixed liquid of the ionic liquid and the organic solvent as the electrolyte, ensures high voltage window and high conductivity, and has relatively good fluidity, so that the super capacitor using the electrolyte has higher energy density and can reach higher power density.
Description
Technical Field
The invention belongs to the technical field of electrolyte, and particularly relates to a preparation method of a high-voltage electrolyte and application of the high-voltage electrolyte in a super capacitor.
Background
Environmental pollution, energy crisis and global warming have become great challenges for human beings, and the development of clean and efficient energy conversion/storage devices is urgent. The super capacitor is an electrochemical energy storage device which realizes energy storage by utilizing double-layer adsorption, surface pseudocapacitance reaction or the insertion and extraction reaction of electrolyte ions in an electrode material body phase. Compared with other energy storage devices, the super capacitor has the advantages of wide working temperature range, good safety, high charging and discharging efficiency, long cycle life and the like, and is widely applied to the fields of standby power systems, portable electronic equipment, electric tools, electric vehicles, smart power grids and the like. However, compared with energy storage devices such as batteries, supercapacitors have lower energy density and are limited in application. According to the energy density calculation formula: e ═ C × Δ V2)/2. Wherein C is the mass specific capacitance (F/g) of the electrochemical capacitor, Δ V is the voltage window (V), and increasing the specific capacitance of the electrode material and the potential window of the capacitor are two ways to increase the energy density of the capacitor.
At present, electrode active materials used in a supercapacitor are mainly carbon materials such as carbon nanotubes, mesoporous carbon materials, graphene, carbon aerogel and activated carbon, and the application of the activated carbon is commercialized. The key to improving the specific capacitance of the activated carbon electrode is to make a developed pore structure matched with the size of electrolyte ions, and a great deal of research is carried out on the influence of the pore structure on the specific capacitance of the super capacitor. Because the energy density is in direct proportion to the square of the potential window, the method for improving the potential window of the super capacitor is a more effective method for improving the energy density of the super capacitor. The ionic liquid has a much higher potential window than that of a water system electrolyte, and has the advantages of stable chemical property, good thermal stability, low volatility and nonflammability, so that the ionic liquid serving as the electrolyte of the super capacitor has become a main research and development direction of the super capacitor. Currently, the used ionic liquid mainly comprises 1-ethyl-3-methylimidazolium tetrafluoroborate ([ EMIM ] BF4) and 1-ethyl-3-methylimidazolium bistrifluoromethanesulfonylimide ([ EMIM ] TFSI), however, the ionic liquid has large viscosity and poor flowability, and the use of pure ionic liquid as a super capacitor electrolyte causes lower power density.
Patent No. CN201911155345.3 discloses a high-voltage resistant aqueous electrolyte and its application in a high-voltage supercapacitor, specifically disclosing inorganic or organic salt, deionized water, ionic liquid, and organic solvent, wherein the anion in the ionic liquid is tetrafluoroboric acid or bis-trifluoromethanesulfonylimide, the cation of the ionic liquid is at least one of imidazole, pyrrole, quaternary ammonium, and thiazole, wherein the imidazole ionic liquid is 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid, and the organic solvent is a low-viscosity organic solvent, including acetonitrile, propionitrile, ethylene carbonate, dimethyl carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, methylethyl carbonate, methyl acetate, ethyl acetate, ethylene sulfite, fluoroethylene carbonate, γ -butyrolactone, γ -valerolactone, and the like, At least one sulfolane.
Patent No. CN201810227792.4 discloses electrolyte of high voltage capacitor, its preparation method and capacitor device, which is obtained by dehydrating mixture of ionic liquid and ester compound with water removing agent, the ionic liquid comprises one or more of tetraethylammonium tetrafluoroborate, tetramethylammonium tetrafluoroborate, N-methylbutylpyrrolidine bistrifluoromethanesulfonimide salt, N-methylbutylpiperidine bistrifluoromethanesulfonimide salt, 3-ethyl-1-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium bistrifluoromethanesulfonimide salt, 1-ethyl-3-methylimidazolium tetrafluoroborate, trimethylpropanium bistrifluoromethanesulfonimide salt, diethylmethylaminoethylmethylether bistrifluoromethanesulfonimide salt, and 1-hexyl-3-methylimidazolium bistrifluoromethanesulfonimide salt; the ester compound comprises one or more of butyrolactone, propylene carbonate, ethyl methyl carbonate and diethyl carbonate.
Patent No. CN201910140941.8 discloses a dual-ion type hybrid capacitor and a preparation method thereof, specifically discloses that the lithium salt is one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium perchlorate and lithium bistrifluoromethanesulfonylimide, and one or more of propylene carbonate, ethylene carbonate, ethyl methyl carbonate, diethyl carbonate, dimethyl carbonate, 1-butyl-3-methylimidazolium bistrifluoromethylsulfonyl imide and 1-ethyl-3-methylimidazolium bistrifluoromethylsulfonyl imide are used as an organic solvent of an electrolyte.
However, the ionic liquid used in the prior art has high cost and high viscosity, which makes the electrolyte difficult to be applied to the super capacitor, and makes it difficult to achieve both the energy density and the power density of the super capacitor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a high-voltage electrolyte and application of the high-voltage electrolyte in a super capacitor.
The method is realized by the following technical scheme:
a preparation method of a high-voltage electrolyte comprises the following steps:
(1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing to obtain an organic solvent mixed solution;
(2) weighing the ionic liquid and the organic solvent mixed solution, mixing, and performing ultrasonic oscillation for 12-24h and magnetic stirring for 12-24h to obtain the product.
The mass ratio of ethylene carbonate to propylene carbonate in the organic solvent mixed solution is 1: (1-2).
The dosage of the ionic liquid accounts for 70-80% of the mass percent of the high-voltage electrolyte.
The ionic liquid is [ Pnim]HCO3Or [ Bmim ]]HCO3Any of the above.
The [ Pnim]HCO3The preparation method comprises the following steps: adding N-methylimidazole into a three-neck flask provided with a condenser tube and a constant-pressure dropping funnel, stirring under the protection of nitrogen, slowly dropwise adding N-propyl bromide in the stirring process, standing after reflux reaction, washing the obtained crude product with an ethyl acetate/acetonitrile mixed solvent to obtain [ Pnim [ ([ Pnim ]) ]]Br light yellow viscous liquid, vacuum drying to obtain [ Pnim]Solid Br; using acetone as solvent, [ Pnim]Br solid and NaHCO3Stirring the three to react, filtering to remove white precipitate NaBr, and adding neutral Al into the filtrate2O3Stirring, filtering, rotary evaporating to remove acetone to obtain colorless ionic liquid [ Pnim]HCO3And vacuum drying to obtain the final product.
The [ Bmim ]]HCO3The preparation method comprises the following steps: adding N-methylimidazole into a three-neck flask provided with a condenser pipe and a constant-pressure dropping funnel, stirring under the protection of nitrogen, slowly dropwise adding N-butyl bromide in the stirring process, performing reflux reaction until white turbidity appears, and standing at low temperature to obtain a white solid; recrystallizing the white solid with ethyl acetate/acetonitrile mixed solvent, and then drying in vacuum to obtain [ Bmim [ ]]Solid Br; using acetone as solvent, [ Bmim ]]Br solid and NaHCO3Filtering to remove white precipitate NaBr after complete reaction, and then removing acetone by rotary evaporationAnd then adding dichloromethane, stirring, performing suction filtration to remove sodium chloride precipitate, performing rotary evaporation to remove dichloromethane, and performing vacuum drying to obtain the product.
Another object of the present invention is to provide the use of a high voltage electrolyte in a supercapacitor having an electrical cut-off voltage of not less than 4.8V.
Has the advantages that:
the invention takes the ionic liquid and organic solvent mixed liquid as the electrolyte, ensures high voltage window and high conductivity, and has relatively good fluidity, so that the super capacitor using the electrolyte has higher energy density and higher power density, the working voltage of the super capacitor can be improved, the stability of the electrolyte can be improved, the conductivity of the electrolyte and the high and low temperature performance of the electrolyte can be improved
By using the electrolyte disclosed by the invention as a dielectric, the electrochemical window of the super capacitor can be improved to 6V at most, and the energy density and the cycling stability are also improved. Compared with the traditional organic electrolyte, the electrolyte for the high-voltage super capacitor can provide a wider voltage window and has better stability. Compared with the traditional electrolyte of a water system and an organic system, the electrolyte has the characteristics of wide electrochemical window, stable chemical property, good thermal stability, low volatility, nonflammability and the like; therefore, the method can be used for constructing a high-performance super capacitor and can also solve the problem of low energy density of an electric double layer capacitor.
Compared with other ionic liquid super capacitors, the super capacitor assembled by the ionic liquid prepared by the invention not only provides larger power density, but also provides wider working temperature range (-45-250 ℃), so that the requirements of weaponry in various environments can be met, and the super capacitor has great national defense application prospect.
Drawings
FIG. 1 is a graph of the AC impedance of the high voltage electrolyte of examples 1-4;
FIG. 2 is a graph showing the energy density and power density of the high voltage electrolyte in examples 1 to 4.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A preparation method of a high-voltage electrolyte comprises the following steps:
(1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing according to the mass ratio of 1:2 to obtain an organic solvent mixed solution;
(2) will [ Pnim]HCO3Mixing the organic solvent mixed solution according to the mass ratio of 7:3, then carrying out ultrasonic oscillation for 12-24h, and then carrying out magnetic stirring for 12-24h until the liquid is uniformly mixed, thus obtaining the high-voltage electrolyte;
the ionic liquid [ Pnim [ ]]HCO3The preparation method comprises the following steps: adding 0.5mol of N-methylimidazole into a 250mL three-neck flask provided with a condenser tube and a constant-pressure dropping funnel, stirring under the protection of nitrogen, slowly dropping N-propyl bromide with the amount of the substances in the stirring process, refluxing for 2 hours, standing, washing the obtained crude product for 3 times by using a mixed solvent of ethyl acetate/acetonitrile (the volume ratio is 2:1) to obtain [ Pnim []Br light yellow viscous liquid, vacuum drying at 80 ℃ for 12h to obtain [ Pnim]Solid Br; then accurately weighing [ Pnim ] with the molar ratio of 1:1]Br solid and NaHCO3Adding into a ground conical flask with a drying tube, adding 100mL acetone, stirring for reaction for 48 hr, filtering to remove white precipitate NaBr, adding neutral Al into the filtrate2O3Stirring for 5h, filtering to remove Al2O3And removing acetone by rotary evaporation to obtain colorless ionic liquid [ Pnim]HCO3Vacuum drying at 80 deg.C for 12 hr to obtain 90% yield;
assembling the button cell with the prepared high-voltage electrolyte, and carrying out electrochemical performance test; as a result: the specific capacity is 164.77F/g; it provided an energy density of 16.76Wh/kg at a power density of 288.97W/kg, showing better performance. The capacity retention rate of the carbon aerogel material reaches 95.38 percent after the carbon aerogel material is circulated for 2000 circles under the current density of 0.1A/g, and the carbon aerogel material shows higher stability. The relevant electrochemical performance tests are shown in fig. 1 and 2 below.
Example 2
A preparation method of a high-voltage electrolyte comprises the following steps:
(1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing according to the mass ratio of 1:2 to obtain an organic solvent mixed solution;
(2) will [ Bmim ]]HCO3Mixing the electrolyte with an organic solvent mixed solution according to a mass ratio of 7:3, then carrying out ultrasonic oscillation for 12-24h, and then carrying out magnetic stirring for 12-24h until the liquid is uniformly mixed, thus obtaining a high-voltage liquid electrolyte;
the ionic liquid [ Bmim [ ]]HCO3The preparation method comprises the following steps: adding 0.5mol of N-methylimidazole into a 250mL three-neck flask provided with a condenser tube and a constant-pressure dropping funnel, introducing nitrogen for stirring under protection, slowly dropping N-butyl bromide with the amount of other substances in the stirring process, performing reflux reaction for 2 hours, stopping the reaction until white turbidity appears in a reaction bottle, and cooling overnight to obtain a white solid; recrystallizing the obtained crude product with ethyl acetate/acetonitrile (volume ratio of 2:1) mixed solvent for 3 times, and vacuum drying at 80 deg.C for 12h to obtain [ Bmim ]]Solid Br; using acetone as solvent, and reacting [ Bmim [ ]]Br and NaHCO3Reacting according to the mass ratio of 1:1, after the reaction is completed, filtering to remove white precipitate NaBr, performing rotary evaporation to remove acetone, adding dichloromethane, stirring for 1h, performing suction filtration to remove precipitated sodium chloride, performing rotary evaporation to remove dichloromethane, and performing vacuum drying at 80 ℃ for 12h to obtain the compound;
assembling the button cell by using the prepared high-voltage liquid electrolyte, and carrying out electrochemical performance test; as a result: the specific capacity is 178.77F/g; it provided an energy density of 21.32Wh/kg at a power density of 546.97W/kg, showing better performance; the capacity retention rate of the carbon aerogel material reaches 96.10% after the carbon aerogel material is circulated for 2000 circles under the current density of 0.1A/g, and the carbon aerogel material shows higher stability. The relevant electrochemical performance tests are shown in fig. 1 and 2 below.
Example 3
A preparation method of a high-voltage electrolyte comprises the following steps:
(1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing the ethylene carbonate and the propylene carbonate according to the mass ratio of 1:1 to obtain an organic solvent mixed solution;
(2) will [ Pnim]HCO3Mixing the organic solvent mixed solution according to the mass ratio of 8:2, then carrying out ultrasonic oscillation for 12-24h, and then carrying out magnetic stirring for 12-24h until the liquid is uniformly mixed, thus obtaining the high-voltage electrolyte;
the ionic liquid [ Pnim [ ]]HCO3The preparation method comprises the following steps: adding 0.5mol of N-methylimidazole into a 250mL three-neck flask provided with a condenser pipe and a constant-pressure dropping funnel, stirring under the protection of nitrogen, slowly dropwise adding N-propyl bromide in an amount equal to that of the substances in the stirring process, refluxing for 2 hours, standing, washing the obtained crude product for 3 times by using a mixed solvent of ethyl acetate and acetonitrile (the volume ratio is 2:1) to obtain [ Pmim [ ([ Pmim ])]Br light yellow viscous liquid, vacuum drying at 80 ℃ for 12h to obtain [ Pnim]Solid Br; then accurately weighing [ Pnim ] with the molar ratio of 1:1]Br solid and NaHCO3Adding into a ground conical flask with a drying tube, adding 100mL acetone, stirring for reaction for 48 hr, filtering to remove white precipitate NaBr, adding neutral Al into the filtrate2O3Stirring for 5h, filtering to remove Al2O3And removing acetone by rotary evaporation to obtain colorless ionic liquid [ Pnim]HCO3Vacuum drying at 80 deg.C for 12 hr to obtain 90% yield;
and assembling the button cell by using the prepared high-voltage electrolyte, and carrying out electrochemical performance test. As a result: the specific capacity is 186.34F/g; it provided an energy density of 22.65Wh/kg at a power density of 603.54W/kg, showing better performance; the capacity retention rate of the carbon aerogel material reaches 94.27 percent after the carbon aerogel material is circulated for 2000 circles under the current density of 0.1A/g, and the carbon aerogel material shows higher stability. The relevant electrochemical performance tests are shown in fig. 1 and 2 below.
Example 4
A preparation method of a high-voltage electrolyte comprises the following steps:
(1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing the ethylene carbonate and the propylene carbonate according to the mass ratio of 1:1 to obtain an organic solvent mixed solution;
(2) will [ Bmim ]]HCO3Mixing the electrolyte with an organic solvent mixed solution according to a mass ratio of 4:1, then carrying out ultrasonic oscillation for 12-24h, and then carrying out magnetic stirring for 12-24h until the liquid is uniformly mixed, thus obtaining a high-voltage electrolyte;
the ionic liquid [ Bmim [ ]]HCO3The preparation method comprises the following steps: adding 0.5mol of N-methylimidazole into a 250mL three-neck flask provided with a condenser tube and a constant-pressure dropping funnel, introducing nitrogen for stirring under protection, slowly dropping N-butyl bromide with the amount of other substances in the stirring process, performing reflux reaction for 2 hours, stopping the reaction until white turbidity appears in a reaction bottle, and cooling overnight to obtain a white solid; recrystallizing the obtained crude product with ethyl acetate/acetonitrile (volume ratio of 2:1) mixed solvent for 3 times, and vacuum drying at 80 deg.C for 12h to obtain [ Bmim ]]Solid Br; using acetone as solvent, and reacting [ Bmim [ ]]Br and NaHCO3Reacting according to the mass ratio of 1:1, after the reaction is completed, filtering to remove white precipitate NaBr, performing rotary evaporation to remove acetone, adding dichloromethane, stirring for 1h, performing suction filtration to remove precipitated sodium chloride, performing rotary evaporation to remove dichloromethane, and performing vacuum drying at 80 ℃ for 12h to obtain the compound;
assembling the button cell by using the prepared high-voltage electrolyte, and carrying out electrochemical performance test; as a result: the specific capacity is 175.77F/g; it provided an energy density of 19.32Wh/kg at a power density of 521.86W/kg, showing better performance; the capacity retention rate of the carbon aerogel material reaches 92.33 percent after the carbon aerogel material is circulated for 2000 circles under the current density of 0.1A/g, and the carbon aerogel material shows higher stability. The relevant electrochemical performance tests are shown in fig. 1 and 2 below.
Claims (3)
1. The preparation method of the high-voltage electrolyte is characterized by comprising the following steps of:
(1) weighing ethylene carbonate and propylene carbonate, and uniformly mixing to obtain an organic solvent mixed solution;
(2) weighing ionic liquid and organic solvent mixed liquid, mixing, and performing ultrasonic oscillation for 12-24h and magnetic stirring for 12-24h to obtain the product;
the mass ratio of ethylene carbonate to propylene carbonate in the organic solvent mixed solution is 1: (1-2);
the dosage of the ionic liquid accounts for 70-80% of the mass percent of the high-voltage electrolyte;
the ionic liquid is [ Pnim]HCO3、[Bmim]HCO3Any one of the above;
the application of the high-voltage electrolyte in the super capacitor ensures that the cut-off voltage of the super capacitor is not lower than 4.8V.
2. The method of claim 1, wherein [ Pmim ] is]HCO3The preparation method comprises the following steps: adding N-methylimidazole into a three-neck flask provided with a condenser tube and a constant-pressure dropping funnel, stirring under the protection of nitrogen, slowly dropwise adding N-propyl bromide in the stirring process, standing after reflux reaction, washing the obtained crude product with an ethyl acetate/acetonitrile mixed solvent to obtain [ Pnim [ ([ Pnim ]) ]]Br light yellow viscous liquid, vacuum drying to obtain [ Pnim]Solid Br; using acetone as solvent, [ Pnim]Br solid and NaHCO3Stirring the three to react, filtering to remove white precipitate NaBr, and adding neutral Al into the filtrate2O3Stirring, filtering, rotary evaporating to remove acetone to obtain colorless ionic liquid [ Pnim]HCO3And vacuum drying to obtain the final product.
3. The method for preparing the high voltage electrolyte of claim 1, wherein [ Bmim ] is]HCO3The preparation method comprises the following steps: adding N-methylimidazole into a three-neck flask provided with a condenser pipe and a constant-pressure dropping funnel, stirring under the protection of nitrogen, slowly dropwise adding N-butyl bromide in the stirring process, performing reflux reaction until white turbidity appears, and standing at low temperature to obtain a white solid; recrystallizing the white solid with ethyl acetate/acetonitrile mixed solvent, and then drying in vacuum to obtain [ Bmim [ ]]Solid Br; using acetone as solvent, [ Bmim ]]Br solid and NaHCO3And (3) taking a reactant, performing suction filtration to remove white precipitate NaBr after complete reaction, performing rotary evaporation to remove acetone, adding dichloromethane, stirring, performing suction filtration to remove sodium chloride precipitate, performing rotary evaporation to remove dichloromethane, and performing vacuum drying to obtain the catalyst.
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