CN111244542A - Low-temperature-resistant lithium battery electrolyte and preparation process thereof - Google Patents
Low-temperature-resistant lithium battery electrolyte and preparation process thereof Download PDFInfo
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- 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
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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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
- H01M10/052—Li-accumulators
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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Abstract
The invention discloses a low-temperature-resistant lithium battery electrolyte and a preparation process thereof, and relates to the technical field of lithium batteries. The invention comprises the following raw materials in parts by weight: 10-12 parts of ethylene carbonate, 10-15 parts of dimethyl carbonate, 5-8 parts of methyl ethyl carbonate, 16-18 parts of phosphorus pentafluoride, 5-9 parts of benzotriazole, 4-7 parts of hydrofluoric acid, 5-8 parts of trihydroxy triethylamine, 3-5 parts of diethylene glycol, 20-25 parts of an additive and 22-27 parts of a buffering agent.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a low-temperature-resistant lithium battery electrolyte and a preparation process thereof.
Background
The electrolyte of the lithium battery is a carrier for ion transmission in the battery, generally consists of lithium salt and an organic solvent, and plays a role in conducting ions between the positive electrode and the negative electrode of the lithium battery; because the electrochemical reaction of the electrolyte is related to the ambient temperature, the temperature in the environment has the greatest influence on the charge and discharge performance of the battery; at low temperature, the viscosity of the electrolyte is reduced, the conductivity is reduced, the activity of the active substance is also reduced, the concentration difference of the electrolyte is increased, the polarization is enhanced, and the charging is terminated early; more importantly, the diffusion rate of lithium ions in the carbon negative electrode will be slower. Lithium is easily precipitated, the temperature is lowered, and the reaction rate of the electrode is also lowered. Assuming that the battery voltage remains constant, the discharge current decreases and the power output of the battery also decreases.
At present, the lithium iron phosphate battery is the most applied to electric vehicles, the battery has high safety and long service life of a monomer, but the lithium iron phosphate has a fatal defect, and the low-temperature performance of the lithium iron phosphate battery is slightly poorer than that of batteries of other technical systems; the low temperature has influence on the anode and cathode of the lithium iron phosphate, the electrolyte, the adhesive and the like; the viscosity of the electrolyte increases at low temperature, the lithium ion migration impedance also increases, and the output power of the power battery is further influenced, so that the development of the electrolyte for the lithium battery at low temperature and the preparation process thereof are technical problems to be solved by technical personnel in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a low-temperature-resistant lithium battery electrolyte and a preparation process thereof, and solves the problems in the background art.
In order to achieve the purpose, the invention is realized by the following technical scheme: the low-temperature-resistant lithium battery electrolyte is prepared from the following raw materials in parts by weight:
10-12 parts of ethylene carbonate, 10-15 parts of dimethyl carbonate, 5-8 parts of methyl ethyl carbonate, 16-18 parts of phosphorus pentafluoride, 5-9 parts of benzotriazole, 4-7 parts of hydrofluoric acid, 5-8 parts of trihydroxy triethylamine, 3-5 parts of diethylene glycol, 20-25 parts of an additive and 22-27 parts of a buffering agent.
Further, the feed is prepared from the following raw materials in parts by weight:
11-12 parts of ethylene carbonate, 12-14 parts of dimethyl carbonate, 6-8 parts of methyl ethyl carbonate, 16-17 parts of phosphorus pentafluoride, 6-7 parts of benzotriazole, 5-7 parts of hydrofluoric acid, 5-6 parts of trihydroxy triethylamine, 4-5 parts of diethylene glycol, 21-24 parts of an additive and 23-25 parts of a buffering agent;
the ethylene carbonate is an organic solvent with excellent performance and can dissolve various polymers; in addition, the compound can be used as an organic intermediate, can replace ethylene oxide to be used for a dioxygenation reaction, and can be applied to lithium battery electrolyte;
dimethyl carbonate is a chemical raw material with low toxicity, excellent environmental protection performance and wide application, is an important organic synthesis intermediate, contains functional groups such as carbonyl, methyl, methoxyl and the like in a molecular structure, and has various reaction performances;
methyl ethyl carbonate is also called ethyl methyl carbonate, is colorless transparent liquid, is insoluble in water, can be used for organic synthesis, and is an excellent solvent of the lithium ion battery electrolyte.
Further, the additive is prepared from the following raw materials in parts by weight:
13-15 parts of diethyl carbonate, 15-20 parts of lithium hexafluorophosphate, 2-5 parts of sodium benzoate, 6-9 parts of propylene glycol and 2-5 parts of polysorbate;
propylene glycol can be used as raw material of unsaturated polyester resin, and can be used as humectant in cosmetics, toothpaste and soap in combination with glycerol or sorbitol; it is used in hair dye as a conditioning agent, a hair conditioner, an antifreeze, a cellophane, a plasticizer and a pharmaceutical industry.
Further, the buffering agent is prepared from the following raw materials in parts by weight:
15-18 parts of propylene carbonate, 12-15 parts of ethylene sulfate, 3-5 parts of n-sebacic acid and 4-7 parts of methyl benzotriazole;
the sebacic acid has wide application, is mainly used for preparing esters of the sebacic acid, has wide application, such as dibutyl sebacate, dioctyl sebacate and diisooctyl sebacate, and can be used as a plasticizer of plastics and cold-resistant rubber;
the vinyl sulfate is white crystal or crystalline powder, is light brown or brown when not pure, is easy to absorb water and hydrolyze in humid air, shows strong acidity and is unstable to heat, and can be used as an additive of lithium ion battery electrolyte;
the invention also provides a preparation process of the low-temperature-resistant lithium battery electrolyte, which comprises the following steps:
the method comprises the following steps: mixing the ethylene carbonate, the dimethyl carbonate, the phosphorus pentafluoride and the benzotriazole in sequence at 15 ℃ to prepare a mixed solution A;
step two: heating the mixed solution A to 23 ℃, adding an additive in the heating process, mixing with methyl ethyl carbonate and hydrofluoric acid respectively to prepare a mixed solution B,
step three: mixing the mixed solution B with a buffering agent, and adding trihydroxy triethylamine in the mixing process to prepare a mixed solution C;
step four: and reducing the temperature of the mixture C to 5 ℃, and fully mixing the mixture C with diethylene glycol to prepare electrolyte.
Furthermore, the mixing process of the electrolyte preparation technology is a closed environment, the mixing air pressure in the first step is 0.015-0.018MPa, the mixing air pressure in the second step is 0.012-0.013MPa, the mixing air pressure in the third step is 0.025-0.029MPa, and the mixing air pressure in the fourth step is 0.019-0.021 MPa.
Further, the stirring time in the first step is 30 minutes, the stirring time in the second step is 60 minutes, the stirring time in the third step is 10 minutes, and the stirring time in the fourth step is 70 minutes.
The invention has the following beneficial effects:
according to the low-temperature-resistant lithium battery electrolyte and the preparation process thereof, the components of the electrolyte are optimized through the additive and the buffering agent, so that the electrolyte has excellent low-temperature resistance, the electrical cycle activity of the electrolyte is improved, and the lithium battery still has stable charge and discharge performance in a low-temperature environment.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a process flow for preparing a low temperature resistant lithium battery electrolyte according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, the present invention provides a technical solution: the low-temperature-resistant lithium battery electrolyte is prepared from the following raw materials in parts by weight:
10 parts of ethylene carbonate, 10 parts of dimethyl carbonate, 5 parts of methyl ethyl carbonate, 16 parts of phosphorus pentafluoride, 5 parts of benzotriazole, 4 parts of hydrofluoric acid, 5 parts of trihydroxy triethylamine, 3 parts of diethylene glycol, 20 parts of additives and 22 parts of buffering agents.
The additive is prepared from the following raw materials in parts by weight:
diethyl carbonate 13, lithium hexafluorophosphate 15, sodium benzoate 2, propylene glycol 6 and polysorbate 2.
The buffering agent is prepared from the following raw materials in parts by weight:
15 parts of propylene carbonate, 12 parts of ethylene sulfate, 3 parts of n-sebacic acid and 4 parts of methyl benzotriazole.
A preparation process of low-temperature-resistant lithium battery electrolyte comprises the following steps:
the method comprises the following steps: mixing ethylene carbonate, dimethyl carbonate, phosphorus pentafluoride and benzotriazole in sequence at 15 ℃ to prepare a mixed solution A;
step two: heating the mixed solution A to 23 ℃, adding an additive in the heating process, mixing with methyl ethyl carbonate and hydrofluoric acid respectively to prepare a mixed solution B,
step three: mixing the mixed solution B with a buffering agent, and adding trihydroxy triethylamine in the mixing process to prepare a mixed solution C;
step four: and reducing the temperature of the mixture C to 5 ℃, and fully mixing the mixture C with diethylene glycol to prepare the electrolyte.
Wherein, the mixing process of the electrolyte preparation process is a closed environment, the mixing air pressure in the first step is 0.015-0.018MPa, the mixing air pressure in the second step is 0.012-0.013MPa, the mixing air pressure in the third step is 0.025-0.029MPa, and the mixing air pressure in the fourth step is 0.019-0.021 MPa.
Wherein the stirring time in the first step is 30 minutes, the stirring time in the second step is 60 minutes, the stirring time in the third step is 10 minutes, and the stirring time in the fourth step is 70 minutes.
Example two
Referring to fig. 1, the present invention further provides a technical solution: the low-temperature-resistant lithium battery electrolyte is prepared from the following raw materials in parts by weight:
ethylene carbonate 12, dimethyl carbonate 15, methyl ethyl carbonate 8, phosphorus pentafluoride 18, benzotriazole 9, hydrofluoric acid 7, trihydroxy triethylamine 8, diethylene glycol 5, additive 25 and buffer 27.
The additive is prepared from the following raw materials in parts by weight:
15 parts of diethyl carbonate, 20 parts of lithium hexafluorophosphate, 5 parts of sodium benzoate, 9 parts of propylene glycol and 5 parts of polysorbate.
The buffering agent is prepared from the following raw materials in parts by weight:
18 parts of propylene carbonate, 15 parts of ethylene sulfate, 5 parts of n-sebacic acid and 7 parts of methyl benzotriazole.
A preparation process of low-temperature-resistant lithium battery electrolyte comprises the following steps:
the method comprises the following steps: mixing ethylene carbonate, dimethyl carbonate, phosphorus pentafluoride and benzotriazole in sequence at 15 ℃ to prepare a mixed solution A;
step two: heating the mixed solution A to 23 ℃, adding an additive in the heating process, mixing with methyl ethyl carbonate and hydrofluoric acid respectively to prepare a mixed solution B,
step three: mixing the mixed solution B with a buffering agent, and adding trihydroxy triethylamine in the mixing process to prepare a mixed solution C;
step four: and reducing the temperature of the mixture C to 5 ℃, and fully mixing the mixture C with diethylene glycol to prepare the electrolyte.
Wherein, the mixing process of the electrolyte preparation process is a closed environment, the mixing air pressure in the first step is 0.015-0.018MPa, the mixing air pressure in the second step is 0.012-0.013MPa, the mixing air pressure in the third step is 0.025-0.029MPa, and the mixing air pressure in the fourth step is 0.019-0.021 MPa.
Wherein the stirring time in the first step is 30 minutes, the stirring time in the second step is 60 minutes, the stirring time in the third step is 10 minutes, and the stirring time in the fourth step is 70 minutes.
EXAMPLE III
Referring to fig. 1, the present invention further provides a technical solution: the low-temperature-resistant lithium battery electrolyte is prepared from the following raw materials in parts by weight:
ethylene carbonate 11, dimethyl carbonate 13, methyl ethyl carbonate 6, phosphorus pentafluoride 17, benzotriazole 7, hydrofluoric acid 6, trihydroxy triethylamine 6, diethylene glycol 4, additive 23 and buffer 26.
The additive is prepared from the following raw materials in parts by weight:
diethyl carbonate 14, lithium hexafluorophosphate 18, sodium benzoate 4, propylene glycol 8 and polysorbate 4.
The buffering agent is prepared from the following raw materials in parts by weight:
17 parts of propylene carbonate, 14 parts of ethylene sulfate, 4 parts of n-sebacic acid and 6 parts of methyl benzotriazole.
A preparation process of low-temperature-resistant lithium battery electrolyte comprises the following steps:
the method comprises the following steps: mixing ethylene carbonate, dimethyl carbonate, phosphorus pentafluoride and benzotriazole in sequence at 15 ℃ to prepare a mixed solution A;
step two: heating the mixed solution A to 23 ℃, adding an additive in the heating process, mixing with methyl ethyl carbonate and hydrofluoric acid respectively to prepare a mixed solution B,
step three: mixing the mixed solution B with a buffering agent, and adding trihydroxy triethylamine in the mixing process to prepare a mixed solution C;
step four: and reducing the temperature of the mixture C to 5 ℃, and fully mixing the mixture C with diethylene glycol to prepare the electrolyte.
Wherein, the mixing process of the electrolyte preparation process is a closed environment, the mixing air pressure in the first step is 0.015-0.018MPa, the mixing air pressure in the second step is 0.012-0.013MPa, the mixing air pressure in the third step is 0.025-0.029MPa, and the mixing air pressure in the fourth step is 0.019-0.021 MPa.
Wherein the stirring time in the first step is 30 minutes, the stirring time in the second step is 60 minutes, the stirring time in the third step is 10 minutes, and the stirring time in the fourth step is 70 minutes.
Example four
The invention also provides a comparison technical scheme: the lithium battery electrolyte is prepared from the following raw materials in parts by weight:
10 parts of ethylene carbonate, 10 parts of dimethyl carbonate, 5 parts of methyl ethyl carbonate, 16 parts of phosphorus pentafluoride and 4 parts of hydrofluoric acid.
The electrolyte preparation process comprises the following steps:
the method comprises the following steps: mixing ethylene carbonate, phosphorus pentafluoride and hydrofluoric acid in sequence to prepare a mixed solution a;
step two: and mixing the mixed solution a with dimethyl carbonate and ethyl methyl carbonate respectively to prepare the electrolyte.
Wherein, the mixing process of the electrolyte preparation technology is a closed environment, the mixing air pressure of the step one is 0.015-0.018MPa, and the mixing air pressure of the step two is 0.019-0.021 MPa.
Wherein the stirring time in the first step is 30 minutes, and the stirring time in the second step is 70 minutes.
And (3) performance detection:
the electrolytes prepared in examples 1 to 4 were fabricated into lithium batteries, and tested in an outdoor environment at-10 ℃ using an outdoor environment at 25 ℃ as a reference standard, and the test data are as follows:
| example one | Example two | EXAMPLE III | Example four | |
| Capacity of battery | 85％ | 91％ | 87％ | 72％ |
| Discharge current | 2.1A | 2.5A | 2.3A | 1.8A |
From the experimental parameters, the second embodiment is the best embodiment, and compared with the fourth embodiment of the control group, the battery capacity and the discharge current are both in higher levels at the outdoor environment of-10 ℃, so that the second embodiment has the outstanding advantage of cold resistance, and the influence of low temperature on the battery performance is reduced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The low-temperature-resistant lithium battery electrolyte is characterized by comprising the following raw materials in parts by weight:
10-12 parts of ethylene carbonate, 10-15 parts of dimethyl carbonate, 5-8 parts of methyl ethyl carbonate, 16-18 parts of phosphorus pentafluoride, 5-9 parts of benzotriazole, 4-7 parts of hydrofluoric acid, 5-8 parts of trihydroxy triethylamine, 3-5 parts of diethylene glycol, 20-25 parts of an additive and 22-27 parts of a buffering agent.
2. The electrolyte for the low-temperature-resistant lithium battery as claimed in claim 1, which is prepared from the following raw materials in parts by weight:
11-12 parts of ethylene carbonate, 12-14 parts of dimethyl carbonate, 6-8 parts of methyl ethyl carbonate, 16-17 parts of phosphorus pentafluoride, 6-7 parts of benzotriazole, 5-7 parts of hydrofluoric acid, 5-6 parts of trihydroxy triethylamine, 4-5 parts of diethylene glycol, 21-24 parts of an additive and 23-25 parts of a buffering agent.
3. The electrolyte for the low-temperature-resistant lithium battery as claimed in claim 1, wherein the additive is prepared from the following raw materials in parts by weight:
13-15 parts of diethyl carbonate, 15-20 parts of lithium hexafluorophosphate, 2-5 parts of sodium benzoate, 6-9 parts of propylene glycol and 2-5 parts of polysorbate.
4. The electrolyte for the low-temperature-resistant lithium battery as claimed in claim 1, wherein the buffer is prepared from the following raw materials in parts by weight:
15-18 parts of propylene carbonate, 12-15 parts of ethylene sulfate, 3-5 parts of n-sebacic acid and 4-7 parts of methyl benzotriazole.
5. A process for preparing a low temperature resistant lithium battery electrolyte as claimed in any one of claims 1 to 4, comprising the steps of:
the method comprises the following steps: mixing the ethylene carbonate, the dimethyl carbonate, the phosphorus pentafluoride and the benzotriazole in sequence at 15 ℃ to prepare a mixed solution A;
step two: heating the mixed solution A to 23 ℃, adding an additive in the heating process, mixing with methyl ethyl carbonate and hydrofluoric acid respectively to prepare a mixed solution B,
step three: mixing the mixed solution B with a buffering agent, and adding trihydroxy triethylamine in the mixing process to prepare a mixed solution C;
step four: and reducing the temperature of the mixture C to 5 ℃, and fully mixing the mixture C with diethylene glycol to prepare electrolyte.
6. The preparation process of the low temperature resistant lithium battery electrolyte as claimed in claim 5, wherein the mixing process of the preparation process of the electrolyte is a closed environment, the mixing air pressure in the first step is 0.015-0.018MPa, the mixing air pressure in the second step is 0.012-0.013MPa, the mixing air pressure in the third step is 0.025-0.029MPa, and the mixing air pressure in the fourth step is 0.019-0.021 MPa.
7. The process according to claim 5, wherein the stirring time in the first step is 30 minutes, the stirring time in the second step is 60 minutes, the stirring time in the third step is 10 minutes, and the stirring time in the fourth step is 70 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112290095A (en) * | 2020-10-26 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Lithium ion battery electrolyte suitable for high-nickel material system and preparation method thereof |
| CN114678156A (en) * | 2022-01-24 | 2022-06-28 | 中国科学院兰州化学物理研究所 | Oil-soluble conductive additive and preparation method thereof |
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