CN113035586A - Low-temperature flame-retardant organic electrolyte for electric double layer capacitor and preparation method thereof - Google Patents

Low-temperature flame-retardant organic electrolyte for electric double layer capacitor and preparation method thereof Download PDF

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CN113035586A
CN113035586A CN202110285084.8A CN202110285084A CN113035586A CN 113035586 A CN113035586 A CN 113035586A CN 202110285084 A CN202110285084 A CN 202110285084A CN 113035586 A CN113035586 A CN 113035586A
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electrolyte
low
flame
temperature
double layer
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CN113035586B (en
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彭正
吴孟强
徐自强
冯婷婷
杨俭
陈诚
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University of Electronic Science and Technology of China
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/54Electrolytes
    • H01G11/58Liquid electrolytes
    • H01G11/60Liquid electrolytes characterised by the solvent
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/54Electrolytes
    • H01G11/58Liquid electrolytes
    • H01G11/62Liquid electrolytes characterised by the solute, e.g. salts, anions or cations therein
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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Abstract

The invention provides a low-temperature flame-retardant organic electrolyte for an electric double layer capacitor and a preparation method thereof, wherein the low-temperature flame-retardant organic electrolyte comprises an electrolyte and an organic solvent, the organic solvent comprises a main solvent, a low-temperature cosolvent and a flame-retardant additive, the electrolyte is quaternary ammonium salt, the main solvent is acetonitrile, the low-temperature cosolvent is one or a combination of more of carbonic ester, gamma-butyrolactone, propionate and 1, 3-dioxolane, and the flame-retardant additive is phosphate. The invention can lead the electric double layer capacitor to have excellent low-temperature performance, and the discharge specific capacity of the electric double layer capacitor at minus 60 ℃ reaches at least 65 percent of the discharge specific capacity at 25 ℃, even can reach as high as 80 percent. Meanwhile, due to the use of the flame retardant, the electrolyte has good safety performance, no obvious combustion by-product is found in the low-temperature flame-retardant organic electrolyte for the double-electric-layer capacitor through combustion experiment tests, and the self-extinguishing time of the electrolyte is reduced by half compared with that of the electrolyte without the flame-retardant additive.

Description

Low-temperature flame-retardant organic electrolyte for electric double layer capacitor and preparation method thereof
Technical Field
The invention belongs to the technical field of double electric layer capacitors, and particularly relates to a low-temperature flame-retardant organic electrolyte for a double electric layer capacitor.
Background
The double-layer capacitor is a novel energy storage device between a traditional capacitor and a battery, generally adopts an active carbon material with a large specific surface area as an electrode, stores charges by a solid/liquid interface double-layer generated by a polarizable electrode/electrolyte, and has farad-level capacitance. The double-layer capacitor has higher energy density than the traditional capacitor, has higher power density than the secondary battery, has the advantages of no maintenance, high charge-discharge efficiency, long cycle life, wide use temperature range and the like, can be used as a power auxiliary device in occasions requiring high-power discharge, can also be used as a backup power source of electronic components, can also be used as a replacement power source, and is a main power source under the condition of continuous discharge for a few milliseconds. The electrolyte solution of the electric double layer capacitor can be classified into an aqueous electrolyte solution, an organic electrolyte solution, a colloidal electrolyte solution, and a solid electrolyte. The organic electrolyte has a wider electrochemical window and higher ionic conductivity, and can be used for preparing a double electric layer capacitor with higher working voltage and higher power density, so that the organic electrolyte is widely applied.
The current double electric layer capacitor widely uses an organic electrolyte, has high conductivity and excellent electrode surface wettability, but has poor thermal stability, easy leakage and poor safety, the working temperature range is usually only within minus 40-60 ℃, the discharge performance of the device is sharply reduced at minus 50 ℃, even the device cannot work, and therefore the working requirement under certain special temperature environments cannot be met. Most of organic electrolyte adopts aprotic liquid with high dielectric constant as solvent, however, the solvent has lower flash point, and is easy to generate heat and fire when the super capacitor is used for quick charge and discharge, so that higher potential safety hazard exists, and the application of the double electric layer capacitor in the fields of military industry, aerospace and the like is limited.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a low-temperature flame-retardant organic electrolyte for an electric double layer capacitor that can stably operate at-60 ℃ and can effectively prevent ignition.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a low-temperature flame-retardant organic electrolyte for an electric double layer capacitor comprises an electrolyte and an organic solvent, wherein the concentration of the electrolyte in the electrolyte is 0.8-1.2 mol/L, the organic solvent comprises a main solvent, a low-temperature cosolvent and a flame-retardant additive, and the volume ratio of the main solvent to the low-temperature cosolvent to the flame-retardant additive is (6-8): (0.5-2): 0.5-2);
the electrolyte is quaternary ammonium salt, the main solvent is acetonitrile, the low-temperature cosolvent is one or a combination of more of carbonic ester, gamma-butyrolactone, propionate and 1, 3-dioxolane, and the flame retardant additive is phosphate.
Preferably, the quaternary ammonium salt is one or a combination of more of tetraethylammonium tetrafluoroborate, triethyl methyl tetrafluoroborate and spiro quaternary ammonium tetrafluoroborate.
Preferably, the carbonate is one or a combination of more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, dipropyl carbonate, dibutyl carbonate, ethylene carbonate and propylene carbonate.
Preferably, the propionate is one or two of methyl propionate and ethyl propionate.
Preferably, the phosphate is one or two of triethyl phosphate and triphenyl phosphate.
Preferably, the electrolyte is tetraethylammonium tetrafluoroborate with the concentration of 0.8-1.2 mol/L.
Preferably, the electrolyte is tetraethylammonium tetrafluoroborate with a concentration of 0.85 to 1.1 mol/L.
Preferably, the low-temperature electrolyte is triethyl methyl tetrafluoroborate with a concentration of 0.8 to 1.2 mol/L.
Preferably, the electrolyte is triethyl methyl tetrafluoroborate with a concentration of 0.9 to 1.15 mol/L.
Preferably, the flame retardant additive is triethyl phosphate.
The invention also provides a preparation method of the low-temperature flame-retardant organic electrolyte for the double electric layer capacitor, which comprises the following steps:
(1) mixing a main solvent and a low-temperature cosolvent according to a ratio in an environment with water and oxygen content lower than 1ppm, and then adding a flame retardant additive according to the ratio to form a final organic solvent;
(2) and adding electrolyte and completely dissolving to obtain the low-temperature flame-retardant organic electrolyte for the double-electric-layer capacitor.
The principle of the low-temperature electrolyte is as follows: firstly, the melting point of the AN-based solvent is reduced by directly adding the solvent with lower melting point, and the low-temperature performance of the electrolyte is improved. Secondly, by utilizing solvation, solvent molecules and solute ions are wrapped to form a new macromolecular structure, and the original chemical bond type is changed, so that the melting point of the system is reduced.
The low-temperature flame retardant principle of the invention is as follows: triethyl phosphate (TEP) and triphenyl phosphate (TPP) are non-combustible phosphorus-containing compounds, gaseous products formed by pyrolysis easily contain PO, the PO can capture main components H of a solvent combustion chain branching reaction such as carbonic ester and acetonitrile, and due to insufficient H, the solvent combustion chain branching reaction can be inhibited, so that the flammability of the electrolyte is reduced.
The invention has the beneficial effects that: compared with the prior art, the low-temperature flame-retardant organic electrolyte for the electric double layer capacitor can enable the electric double layer capacitor to have excellent low-temperature performance, and the discharge specific capacity of the electric double layer capacitor at the temperature of-60 ℃ reaches at least 65% of the discharge specific capacity at the temperature of 25 ℃, even can reach 80%. Meanwhile, due to the use of the flame retardant, the electrolyte has good safety performance, no obvious combustion by-product is found in the low-temperature flame-retardant organic electrolyte for the double-electric-layer capacitor through combustion experiment tests, and the self-extinguishing time of the electrolyte is reduced by half compared with that of the electrolyte without the flame-retardant additive.
Drawings
Fig. 1 (a) to (e) are graphs showing charge and discharge of the button type electric double layer capacitors prepared in examples 1 to 5 at-60 c and different current densities, respectively.
Fig. 1(f) is a graph showing the specific capacity at-60 c for button type electric double layer capacitors prepared in examples 1 to 5 at different current densities.
In fig. 2, (a) and (b) are a magnification graph and a cyclic voltammogram of the button type electric double layer capacitor prepared in example 6 at different temperatures, respectively;
in fig. 2, (c) and (d) are a magnification graph and a cyclic voltammogram of the button type electric double layer capacitor prepared in example 7 at different temperatures, respectively;
in fig. 2, (e) and (f) are a magnification graph and a cyclic voltammogram of the button type electric double layer capacitor prepared in example 8 at different temperatures, respectively;
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Examples
The embodiment provides a low-temperature flame-retardant organic electrolyte for an electric double layer capacitor, which comprises an electrolyte and an organic solvent, wherein the concentration of the electrolyte in the electrolyte is 0.8-1.2 mol/L, the organic solvent comprises a main solvent, a low-temperature cosolvent and a flame-retardant additive, and the volume ratio of the main solvent, the low-temperature cosolvent and the flame-retardant additive is (6-8): (0.5-2): 0.5-2;
the electrolyte is quaternary ammonium salt, and the quaternary ammonium salt is one or a combination of more of tetraethylammonium tetrafluoroborate, triethyl methyl tetrafluoroborate and spiro quaternary ammonium tetrafluoroborate.
The main solvent is acetonitrile;
the low-temperature cosolvent is one or a combination of more of carbonic ester, gamma-butyrolactone, propionate and 1, 3-dioxolane, and the carbonic ester is one or a combination of more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, dipropyl carbonate, dibutyl carbonate, ethylene carbonate and propylene carbonate. The propionate is one or two of methyl propionate and ethyl propionate.
The flame retardant additive is phosphate. The phosphate is one or two of triethyl phosphate and triphenyl phosphate.
Preferably, the electrolyte is tetraethylammonium tetrafluoroborate with the concentration of 0.8-1.2 mol/L.
Preferably, the electrolyte is tetraethylammonium tetrafluoroborate with the concentration of 0.85-1.1 mol/L.
Preferably, the low-temperature electrolyte is triethyl methyl tetrafluoroborate with the concentration of 0.8-1.2 mol/L.
Preferably, the electrolyte is triethyl methyl tetrafluoroborate with the concentration of 0.9-1.15 mol/L.
Preferably, the flame retardant additive is triethyl phosphate.
The embodiment also provides a preparation method of the low-temperature flame-retardant organic electrolyte for the electric double layer capacitor, which comprises the following steps:
(1) mixing a main solvent and a low-temperature cosolvent according to a ratio in an environment with water and oxygen content lower than 1ppm, and then adding a flame retardant additive according to the ratio to form a final organic solvent;
(2) and adding electrolyte and completely dissolving to obtain the low-temperature flame-retardant organic electrolyte for the double-electric-layer capacitor.
The formulations in the examples are shown in Table 1:
table 1 formulations of the examples
Figure BDA0002980117620000041
Second, Performance test experiment
1. Combustion experiment
The procedure for the combustion experiment was as follows:
glass wool is used as a raw material to prepare glass wool balls with the diameter of 5mm, the glass wool balls are weighed and arranged on a thin iron wire folded into an O shape, electrolyte solutions with different proportions are respectively taken out by a register and injected on the glass wool to be rapidly ignited, and the time from the moment when an ignition device is removed to the moment when flame is automatically extinguished is recorded.
Table 2 combustion experimental data and analysis:
self-extinguishing time Combustion by-products
Control group 1 45s Multiple purpose
Control group
2 44s Multiple purpose
Example 1 33s Small amount of
Example 2 20s Is free of
Example 3 34s Small amount of
Example 4 20s Is free of
Example 5 22s Is free of
Example 6 32s Small amount of
Example 7 32s Small amount of
Example 8 33s Small amount of
Example 9 38s Much more
Example 10 33s Small amount of
Example 11 37s Much more
Example 12 25s Small amount of
Third, Charge and discharge experiment
And preparing the prepared electrolyte into a formed button type double-layer capacitor according to the manufacturing standard of the double-layer capacitor, wherein the electrode material adopts active carbon. Testing specific capacity at 20 +/-5 ℃ at current densities of 0.1A/g, 0.2A/g, 0.5A/g, 1A/g and 2A/g, and testing cyclic voltammetry curve at 5 mV/s; after standing at a low temperature (0 ℃ C., -20 ℃ C., -40 ℃ C., -60 ℃ C.) for 16 hours, the specific capacity was measured at a current density of 0.1A/g, and the cyclic voltammogram was measured at 5 mV/s.
Fig. 1 (a) to (e) are graphs showing charge and discharge of the button type electric double layer capacitors prepared in examples 1 to 5 at-60 c and different current densities, respectively.
Fig. 1(f) is a graph showing the specific capacity at-60 c for button type electric double layer capacitors prepared in examples 1 to 5 at different current densities.
In fig. 2, (a) and (b) are a magnification graph and a cyclic voltammogram of the button type electric double layer capacitor prepared in example 6 at different temperatures, respectively;
in fig. 2, (c) and (d) are a magnification graph and a cyclic voltammogram of the button type electric double layer capacitor prepared in example 7 at different temperatures, respectively;
in fig. 2, (e) and (f) are a magnification graph and a cyclic voltammogram of the button type electric double layer capacitor prepared in example 8 at different temperatures, respectively;
the foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. A low-temperature flame-retardant organic electrolyte for an electric double layer capacitor is characterized in that: the electrolyte is prepared from an electrolyte and an organic solvent, wherein the concentration of the electrolyte in an electrolyte is 0.8-1.2 mol/L, the organic solvent comprises a main solvent, a low-temperature cosolvent and a flame retardant additive, and the volume ratio of the main solvent to the low-temperature cosolvent to the flame retardant additive is (6-8): (0.5-2): 0.5-2);
the electrolyte is quaternary ammonium salt, the main solvent is acetonitrile, the low-temperature cosolvent is one or a combination of more of carbonic ester, gamma-butyrolactone, propionate and 1, 3-dioxolane, and the flame retardant additive is phosphate.
2. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, wherein: the quaternary ammonium salt is one or a combination of more of tetraethyl ammonium tetrafluoroborate, triethyl methyl tetrafluoroborate and spiro quaternary ammonium tetrafluoroborate.
3. The low-temperature-resistant flame-retardant organic electrolyte for electric double layer capacitors according to claim 1 or 2, characterized in that: the carbonate is one or a combination of more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, dipropyl carbonate, dibutyl carbonate, ethylene carbonate and propylene carbonate.
4. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, wherein: the propionate is one or two of methyl propionate and ethyl propionate.
5. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, wherein: the phosphate is one or two of triethyl phosphate and triphenyl phosphate.
6. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, wherein: the electrolyte is tetraethylammonium tetrafluoroborate with the concentration of 0.8-1.2 mol/L.
7. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, wherein: the electrolyte is tetraethylammonium tetrafluoroborate with the concentration of 0.85-1.1 mol/L.
8. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, characterized in that: the low-temperature electrolyte is triethyl methyl tetrafluoroborate with the concentration of 0.8-1.2 mol/L.
9. The low-temperature flame-retardant organic electrolyte for electric double layer capacitors according to claim 1, characterized in that: the electrolyte is triethyl methyl tetrafluoroborate with the concentration of 0.9-1.15 mol/L.
10. The method for preparing a low-temperature flame-retardant organic electrolyte for electric double layer capacitors as recited in any one of claims 1 to 9, comprising the steps of:
(1) mixing a main solvent and a low-temperature cosolvent according to a ratio in an environment with water and oxygen content lower than 1ppm, and then adding a flame retardant additive according to the ratio to form a final organic solvent;
(2) and adding electrolyte and completely dissolving to obtain the low-temperature flame-retardant organic electrolyte for the double-electric-layer capacitor.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150029640A1 (en) * 2012-02-27 2015-01-29 Panasonic Corporation Electrolyte solution for electric double layer capacitors, and electric double layer capacitor
CN104584164A (en) * 2012-09-04 2015-04-29 大金工业株式会社 Electrolyte solution and electrochemical device
CN105336506A (en) * 2015-11-11 2016-02-17 湖北诺邦科技股份有限公司 Fire-retardant super capacitor electrolyte
CN109616325A (en) * 2019-01-28 2019-04-12 江苏法拉电子有限公司 A kind of take gamma-butyrolacton as the organic electrolyte of basic solvent
CN109727788A (en) * 2017-10-30 2019-05-07 江苏国泰超威新材料有限公司 A kind of double layer capacitor low-temperature electrolyte

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150029640A1 (en) * 2012-02-27 2015-01-29 Panasonic Corporation Electrolyte solution for electric double layer capacitors, and electric double layer capacitor
CN104584164A (en) * 2012-09-04 2015-04-29 大金工业株式会社 Electrolyte solution and electrochemical device
CN105336506A (en) * 2015-11-11 2016-02-17 湖北诺邦科技股份有限公司 Fire-retardant super capacitor electrolyte
CN109727788A (en) * 2017-10-30 2019-05-07 江苏国泰超威新材料有限公司 A kind of double layer capacitor low-temperature electrolyte
CN109616325A (en) * 2019-01-28 2019-04-12 江苏法拉电子有限公司 A kind of take gamma-butyrolacton as the organic electrolyte of basic solvent

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