CN111082137A - Preparation method of low-turbidity lithium ion battery electrolyte - Google Patents
Preparation method of low-turbidity lithium ion battery electrolyte Download PDFInfo
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- CN111082137A CN111082137A CN201911343310.2A CN201911343310A CN111082137A CN 111082137 A CN111082137 A CN 111082137A CN 201911343310 A CN201911343310 A CN 201911343310A CN 111082137 A CN111082137 A CN 111082137A
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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
- H01M10/0566—Liquid materials
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- 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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- H01M10/0569—Liquid materials characterised by the solvents
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- 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
- Y02E60/10—Energy storage using batteries
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Abstract
The preparation method of the low-turbidity lithium ion battery electrolyte comprises the steps of S1, sequentially adding diethyl carbonate-ethylene carbonate-ethyl methyl carbonate into a mixing tank according to the corresponding weight parts, and starting a stirrer in the mixing tank to uniformly mix the raw material solutions to form a primary electrolyte; s2, adding lithium hexafluorophosphate into the primary electrolyte according to the corresponding weight parts; s3, sequentially adding propylene carbonate-vinylene carbonate into the intermediate electrolyte according to corresponding weight parts, and filtering the propylene carbonate and the vinylene carbonate in the flowing process; according to the invention, the lithium hexafluorophosphate is added before the propylene carbonate, so that the lithium hexafluorophosphate can be fully dissolved and reacted before the propylene carbonate is added, and when the propylene carbonate is added, impurities in the lithium hexafluorophosphate can not react any more, so that the turbidity problem of a final product can not be influenced, and the product quality is ensured.
Description
Technical Field
The invention belongs to the technical field of lithium ion electrolyte production, and particularly relates to a preparation method of a low-turbidity lithium ion battery electrolyte.
Background
Lithium battery electrolytes are carriers for ion transport in batteries. Generally consisting of a lithium salt and an organic solvent. The electrolyte plays a role in conducting ions between the positive electrode and the negative electrode of the lithium battery, and is a guarantee for the lithium battery to obtain the advantages of high voltage, high specific energy and the like; the electrolyte is generally prepared from raw materials such as a high-purity organic solvent, electrolyte lithium salt, necessary additives and the like according to a certain proportion under a certain condition;
the lithium battery electrolyte has the following problems in preparation, the produced electrolyte has certain turbidity, and the whole liquid is in a white and turbid state and cannot meet the product quality requirement.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a low-turbidity lithium ion battery electrolyte, and the specific technical scheme is as follows:
a preparation method of a low-turbidity lithium ion battery electrolyte comprises the following steps:
s1, sequentially adding diethyl carbonate-ethylene carbonate-ethyl methyl carbonate into the mixing tank according to the corresponding weight parts, and starting a stirrer in the mixing tank to uniformly mix the raw material liquids to form primary electrolyte;
s2, adding lithium hexafluorophosphate into the primary electrolyte according to the corresponding weight parts, and starting a stirrer in a mixing tank to uniformly mix the raw material liquids to form an intermediate electrolyte;
and S3, sequentially adding propylene carbonate-vinylene carbonate into the intermediate electrolyte according to corresponding weight parts, filtering the propylene carbonate and the vinylene carbonate in the flowing process, and starting a stirrer in a mixing tank to uniformly mix the raw material liquids to form the required liquid electrolyte.
Further, in S1, the operation time of the stirrer is 15-25 min.
Further, in S2, the operation time of the stirrer is 30-50 min.
Further, in S3, the operation time of the stirrer is 10-20 min.
Further, the weight part of the diethyl carbonate is 20-25; the weight part of the ethylene carbonate is 30-35; 18-25 parts of methyl ethyl carbonate; the weight part of the lithium hexafluorophosphate is 12-15; 5-8 parts of propylene carbonate; the vinylene carbonate accounts for 1-2 parts by weight.
Further, the propylene carbonate and the vinylene carbonate are filtered in the flowing process, and specifically the steps are as follows: the propylene carbonate and the vinylene carbonate are filtered by using a 5A molecular sieve.
The invention has the beneficial effects that:
1. the lithium hexafluorophosphate is added before the propylene carbonate, so that the lithium hexafluorophosphate can be fully dissolved and reacted before the propylene carbonate is added, and when the propylene carbonate is added, iron ion impurities in the lithium hexafluorophosphate can not react any more, so that the turbidity problem of a final product can not be influenced, and the product quality is ensured;
2. the dissolving speed of lithium hexafluorophosphate can be improved by using a step-by-step stirring mode, so that the reaction of impurities and undissolved lithium hexafluorophosphate is avoided, and the turbidity of the product is further reduced;
3. the propylene carbonate and the vinylene carbonate are filtered in the flowing process, so that impurities can be removed to a certain degree.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A preparation method of a low-turbidity lithium ion battery electrolyte comprises the following steps:
s1, sequentially adding diethyl carbonate, ethylene carbonate and ethyl methyl carbonate into a mixing tank according to the corresponding weight parts, starting a stirrer in the mixing tank, wherein the working time of the stirrer is 15-25 min, so that the raw material liquids are uniformly mixed to form primary electrolyte; the step is used for ensuring that the diethyl carbonate, the ethylene carbonate and the methyl ethyl carbonate are fully mixed firstly so as to form primary mixed liquid more fully, further facilitating the rapid reaction of the primary mixed liquid and the lithium hexafluorophosphate and accelerating the reaction speed of the lithium hexafluorophosphate;
s2, adding lithium hexafluorophosphate into the primary electrolyte according to the corresponding weight parts, starting a stirrer in a mixing tank, wherein the working time of the stirrer is 30-50 min, so that the raw material liquids are uniformly mixed to form an intermediate electrolyte; the step is used for adding lithium hexafluorophosphate firstly, so that the lithium hexafluorophosphate is fully dissolved in advance, the lithium hexafluorophosphate is prevented from reacting with impurities in propylene carbonate, and the turbidity of the electrolyte is reduced;
s3, sequentially adding propylene carbonate-vinylene carbonate into the intermediate electrolyte according to corresponding weight parts, filtering the propylene carbonate and the vinylene carbonate in the flowing process, and starting a stirrer in a mixing tank to uniformly mix the raw material liquids to form a required liquid electrolyte; the step is used for quickly preparing the required liquid electrolyte, and the propylene carbonate and the vinylene carbonate are filtered in advance, so that the composite reaction amount can be further reduced.
In S2, the weight part of diethyl carbonate is 20-25; the weight part of the ethylene carbonate is 30-35; 18-25 parts of methyl ethyl carbonate; the weight part of the lithium hexafluorophosphate is 12-15; 5-8 parts of propylene carbonate; the vinylene carbonate accounts for 1-2 parts by weight.
As an improvement of the technical scheme, the propylene carbonate and the vinylene carbonate are filtered in the flowing process, and specifically the method comprises the following steps: the propylene carbonate and the vinylene carbonate are filtered by using a 5A molecular sieve.
The preparation method provided by the invention can effectively reduce the turbidity of the electrolyte, so that the electrolyte is clearer, excessive impurities are eliminated, and the product quality is improved.
To verify that the invention can achieve the technical effects, a first comparative test is performed according to four different methods:
the first test and the first matching are prepared by adopting the traditional sequence:
taking 2.5kg of diethyl carbonate, 3.5kg of ethylene carbonate, 1.8kg of ethyl methyl carbonate, 0.8kg of propylene carbonate, 0.2kg of vinylene carbonate and 1.2kg of lithium hexafluorophosphate; sequentially adding diethyl carbonate, ethylene carbonate, ethyl methyl carbonate, propylene carbonate, vinylene carbonate and lithium hexafluorophosphate into the mixing tank, starting a stirrer in the mixing tank, and stirring for 60min to uniformly mix the raw material liquids to form a liquid electrolyte;
and analyzing the physical and chemical properties of the obtained liquid electrolyte, and recording related parameters.
The second test and the second preparation are prepared by adopting the traditional sequence:
taking 2kg of diethyl carbonate, 3kg of ethylene carbonate, 2.5kg of ethyl methyl carbonate, 0.8kg of propylene carbonate, 0.2kg of vinylene carbonate and 1.5kg of lithium hexafluorophosphate; sequentially adding diethyl carbonate, ethylene carbonate, ethyl methyl carbonate, propylene carbonate, vinylene carbonate and lithium hexafluorophosphate into the mixing tank, starting a stirrer in the mixing tank, and stirring for 60min to uniformly mix the raw material liquids to form a liquid electrolyte;
and analyzing the physical and chemical properties of the obtained liquid electrolyte, and recording related parameters.
Experiment three, adopting the improved feeding sequence to prepare under the first proportion:
taking 2.5kg of diethyl carbonate, 3.5kg of ethylene carbonate, 1.8kg of ethyl methyl carbonate, 0.8kg of propylene carbonate, 0.2kg of vinylene carbonate and 1.2kg of lithium hexafluorophosphate; adding diethyl carbonate-ethylene carbonate-ethyl methyl carbonate-lithium hexafluorophosphate-propylene carbonate-vinylene carbonate into a mixing tank in sequence; starting a stirrer in the mixing tank, and stirring for 60min to uniformly mix the raw material liquids to form liquid electrolyte;
and analyzing the physical and chemical properties of the obtained liquid electrolyte, and recording related parameters.
The fourth test and the second test are prepared by adopting an improved feeding sequence:
taking 2kg of diethyl carbonate, 3kg of ethylene carbonate, 2.5kg of ethyl methyl carbonate, 0.8kg of propylene carbonate, 0.2kg of vinylene carbonate and 1.5kg of lithium hexafluorophosphate; adding diethyl carbonate-ethylene carbonate-ethyl methyl carbonate-lithium hexafluorophosphate-propylene carbonate-vinylene carbonate into a mixing tank in sequence; starting a stirrer in the mixing tank, and stirring for 60min to uniformly mix the raw material liquids to form liquid electrolyte;
and analyzing the physical and chemical properties of the obtained liquid electrolyte, and recording related parameters.
The relevant parameters in comparative experiment one are summarized in table 1 below:
| batches of | Moisture content | Acidity of the solution | Electrical conductivity of | Density of | Turbidity of water |
| Test 1 | 7.6 | 8.5 | 7.19 | 1.176 | 13.5 |
| Test 2 | 8.3 | 12.7 | 7.18 | 1.175 | 16.1 |
| Test 3 | 9.7 | 8.6 | 7.17 | 1.169 | 0.52 |
| Test 4 | 5.8 | 10.9 | 7.14 | 1.177 | 0.14 |
According to the product requirement, the qualified turbidity is less than 3, and the analysis table 1 shows that the turbidity of the test 1 and the test 2 does not reach the qualified requirement, and exceeds the qualified turbidity by multiple times, so that the product quality is not high; on the premise that the water content, acidity, conductivity and density of the test 3 and the test 4 can meet the requirements, the turbidity can also well meet the requirements, the turbidity is very low, and the product quality is high; the raw material ratio between the test 1 and the test 2 is different, and the raw material ratio between the test 3 and the test 4 is different, but the final results are that the traditional sequential turbidity does not reach the standard and the improved sequential turbidity reaches the standard; the problem of turbidity can be effectively solved by judging that the charging sequence of lithium hexafluorophosphate is added before propylene carbonate and vinylene carbonate;
further tests show that the reason that the turbidity is influenced by impurities generated in the traditional feeding sequence is that the propylene carbonate solution contains a certain amount of iron ion impurities, and the iron ion impurities are derived from residues in the propylene carbonate raw material, residues in a preparation tank body and residues in a molecular sieve; if the charging sequence is propylene carbonate-vinylene carbonate-lithium hexafluorophosphate, the lithium hexafluorophosphate which is just added cannot be immediately dissolved, and the lithium hexafluorophosphate can react with iron ion impurities to form iron phosphate, namely ferric phosphate and ferric orthophosphate, the molecular formula of which is FePO4Is aWhite, off-white monoclinic crystal powder; the ferric phosphate is kept until the preparation is finished, so that the turbidity of the product is influenced;
the improved charging sequence of lithium hexafluorophosphate, propylene carbonate and vinylene carbonate can realize that lithium hexafluorophosphate is fully dissolved and reacted before propylene carbonate is added, when propylene carbonate is added, iron ion impurities in the propylene carbonate can not react any more, and the iron ion impurities can be reserved until the preparation is finished, so that the turbidity problem of a final product can not be influenced, and the product quality is ensured.
Taking 2.5kg of diethyl carbonate, 3.5kg of ethylene carbonate, 1.8kg of ethyl methyl carbonate, 0.8kg of propylene carbonate, 0.2kg of vinylene carbonate and 1.2kg of lithium hexafluorophosphate; according to the implementation steps provided by the invention:
and (5) testing:
s1, sequentially adding diethyl carbonate, ethylene carbonate and ethyl methyl carbonate into a mixing tank according to the corresponding weight parts, starting a stirrer in the mixing tank, and stirring for 20min to uniformly mix the raw material liquids to form primary electrolyte;
s2, adding lithium hexafluorophosphate into the primary electrolyte according to the corresponding weight parts, starting a stirrer in a mixing tank, and stirring for 30min to uniformly mix the raw material solutions to form an intermediate electrolyte;
and S3, sequentially adding propylene carbonate-vinylene carbonate into the intermediate electrolyte according to the corresponding weight parts, starting a stirrer in a mixing tank, and stirring for 10min to uniformly mix the raw material liquids to form the required liquid electrolyte.
And (3) carrying out physical and chemical property analysis on the prepared electrolyte, recording relevant parameters, and drawing:
TABLE 2
| Batches of | Moisture content | Acidity of the solution | Electrical conductivity of | Density of | Turbidity of water |
| Test 3 | 9.7 | 8.6 | 7.17 | 1.169 | 0.52 |
| Test 5 | 9.5 | 8.1 | 7.16 | 1.173 | 0.06 |
Through the contrast discovery, even under experimental 3, experimental 5 all can reach under the prerequisite of turbidity requirement, experimental 5's turbidity is obviously less than experimental 3, consequently utilizes the segmentation stirring to add prefiltering's mode, can improve lithium hexafluorophosphate and dissolve reaction effect to further avoid impurity 1 and undissolved lithium hexafluorophosphate reaction, thereby further reduction product turbidity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The preparation method of the low-turbidity lithium ion battery electrolyte is characterized by comprising the following steps of: the method comprises the following steps:
s1, sequentially adding diethyl carbonate-ethylene carbonate-ethyl methyl carbonate into the mixing tank according to the corresponding weight parts, and starting a stirrer in the mixing tank to uniformly mix the raw material liquids to form primary electrolyte;
s2, adding lithium hexafluorophosphate into the primary electrolyte according to the corresponding weight parts, and starting a stirrer in a mixing tank to uniformly mix the raw material liquids to form an intermediate electrolyte;
and S3, sequentially adding propylene carbonate-vinylene carbonate into the intermediate electrolyte according to corresponding weight parts, filtering the propylene carbonate and the vinylene carbonate in the flowing process, and starting a stirrer in a mixing tank to uniformly mix the raw material liquids to form the required liquid electrolyte.
2. The method for preparing the low turbidity lithium ion battery electrolyte according to claim 1, wherein the method comprises the following steps: in S1, the working time of the stirrer is 15-25 min.
3. The method for preparing the low turbidity lithium ion battery electrolyte according to claim 1, wherein the method comprises the following steps: in S2, the operation time of the stirrer is 30-50 min.
4. The method for preparing the low turbidity lithium ion battery electrolyte according to claim 1, wherein the method comprises the following steps: in S3, the operation time of the stirrer is 10-20 min.
5. The method for preparing the low turbidity lithium ion battery electrolyte according to claim 1, wherein the method comprises the following steps: 20-25 parts of diethyl carbonate; the weight part of the ethylene carbonate is 30-35; 18-25 parts of methyl ethyl carbonate; the weight part of the lithium hexafluorophosphate is 12-15; 5-8 parts of propylene carbonate; the vinylene carbonate accounts for 1-2 parts by weight.
6. The method for preparing the low turbidity lithium ion battery electrolyte according to claim 1, wherein the method comprises the following steps: the propylene carbonate and the vinylene carbonate are filtered in the flowing process, and specifically the steps are as follows: the propylene carbonate and the vinylene carbonate are filtered by using a 5A molecular sieve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112803073A (en) * | 2021-04-06 | 2021-05-14 | 浙江金羽新能源科技有限公司 | Additive, electrolyte and battery |
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Non-Patent Citations (2)
| Title |
|---|
| 曹炳炎: "《石油化工毒物手册》", 31 May 1992 * |
| 王巧娟;冯兵;任园: "水分和杂质离子对电解液的影响和脱除", 《电池工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112803073A (en) * | 2021-04-06 | 2021-05-14 | 浙江金羽新能源科技有限公司 | Additive, electrolyte and battery |
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Application publication date: 20200428 |