CN112129753A - Method for detecting content of chloride in electrolyte for lithium ion battery - Google Patents
Method for detecting content of chloride in electrolyte for lithium ion battery Download PDFInfo
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- CN112129753A CN112129753A CN202011127415.7A CN202011127415A CN112129753A CN 112129753 A CN112129753 A CN 112129753A CN 202011127415 A CN202011127415 A CN 202011127415A CN 112129753 A CN112129753 A CN 112129753A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 60
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003792 electrolyte Substances 0.000 title claims abstract description 22
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000000523 sample Substances 0.000 claims abstract description 28
- 239000012452 mother liquor Substances 0.000 claims abstract description 24
- 239000000654 additive Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012488 sample solution Substances 0.000 claims abstract description 15
- 150000001805 chlorine compounds Chemical class 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 32
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 17
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 10
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 6
- YTZKOQUCBOVLHL-UHFFFAOYSA-N tert-butylbenzene Chemical compound CC(C)(C)C1=CC=CC=C1 YTZKOQUCBOVLHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 4
- QHTJSSMHBLGUHV-UHFFFAOYSA-N 2-methylbutan-2-ylbenzene Chemical compound CCC(C)(C)C1=CC=CC=C1 QHTJSSMHBLGUHV-UHFFFAOYSA-N 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims description 3
- 239000004305 biphenyl Substances 0.000 claims description 3
- HHNHBFLGXIUXCM-GFCCVEGCSA-N cyclohexylbenzene Chemical compound [CH]1CCCC[C@@H]1C1=CC=CC=C1 HHNHBFLGXIUXCM-GFCCVEGCSA-N 0.000 claims description 3
- -1 fluorobiphenyl Chemical compound 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 2
- 238000007405 data analysis Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 32
- 239000012086 standard solution Substances 0.000 description 6
- 238000004879 turbidimetry Methods 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000013582 standard series solution Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/82—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a precipitate or turbidity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
-
- 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
- Y02E60/10—Energy storage using batteries
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for detecting the chloride content in electrolyte for a lithium ion battery, which belongs to the technical field of lithium ion batteries, wherein the lithium ion battery comprises benzene additives, and the detection method comprises the following steps: (1) the standard series is prepared, and the volume of the mother liquor used in the preparation of the chloride standard series is marked as A1、A2、A3......An(ii) a (2) Preparing a sample solution; (3) determination of AnThe value: the turbidity of the sample is compared with the standard chloride series one by using a turbidimetric method to find out the standard chloride series A closest to the turbidity of the samplen(ii) a (4) According to AnAnd (5) calculating the chloride content. The quantitative detection method disclosed by the invention effectively controls the influence of white suspended matters generated in the reaction of the benzene-containing additive and water on the observation result, improves the test accuracy, and can provide classification for the industrialization of lithium ion batteriesAnd data analysis and direction guidance are carried out, so that the development of the lithium ion battery industry is promoted.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a method for detecting the content of chloride in electrolyte for a lithium ion battery.
Background
The content of chloride in the electrolyte for the lithium ion battery directly corrodes the anode and cathode materials of the lithium ion battery, so that the capacity of the battery is reduced, the product quality and the performance of the battery are directly influenced, a pole piece is perforated when the battery is serious, the whole battery is damaged, and safety risk is caused. Therefore, it is very important to accurately determine the chloride content in the lithium ion battery electrolyte.
The currently commonly used chloride content quantification methods include a turbidimetry method, a potentiometric titration method, an ion chromatography method and the like, wherein the potentiometric titration method and the ion chromatography method are not suitable for detecting the content of trace chloride, and the error of a test result is large, while the turbidimetry method can be suitable for most of electrolytes, but white suspended matters appear when benzene-containing additives react with water, so that the final observation result is directly influenced by turbidimetry, and the accuracy in the chloride detection process is reduced.
Therefore, how to provide an accurate method for detecting the chloride content in the electrolyte for the lithium ion battery is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for detecting the chloride content in an electrolyte for a lithium ion battery, which can reduce the influence of benzene additives in the lithium ion battery on the detection precision of chloride ions.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for detecting the content of chloride in electrolyte for a lithium ion battery comprises a benzene additive, and the method comprises the following steps:
(1) preparing a standard series of: preparing standard chloride solution mother liquor with different volumes and concentrations from standard chloride solution mother liquor with different volumes and concentrations, and then respectively adding the same nitric acid solution and silver nitrate solution into the standard chloride solution series for treatment and then standing;
wherein, the standard series of chlorides is marked as A according to the volume of mother liquor used in the preparation1、A2、A3......An；
(2) Preparing a sample solution: uniformly mixing an organic solvent, distilled water and a sample to be detected, standing, taking supernatant after layering, adding the supernatant into a colorimetric tube, adding a nitric acid solution and a silver nitrate solution which have the same concentration and volume as those in the step (1) into the supernatant, and standing to obtain a sample solution;
(3) determination of AnThe value: measured by turbidimetry by mixing the sampleComparing the turbidity of the product with the standard chloride series one by one to find out the standard chloride series A closest to the turbidity of the samplen；
(4) And (4) calculating a result:
calculated as Cl according to the formula-And (3) measuring the chloride content:
in the formula:
x represents the chloride content in terms of Cl < - >, ug/g;
An-the volume value of the mother liquor in the chloride standard series, ml, closest to the turbidity of the sample;
m-the mass of the sample to be measured, g.
Has the advantages that: the organic solvent used in the invention can extract the benzene additives in the lithium ion battery, and the organic solvent is added before the sample solution is prepared, so that the benzene additives in the sample are effectively extracted and separated, the influence of white suspended matters generated when the benzene-containing additives react with water on the turbidity result of the observed sample is controlled, and the test accuracy is further improved.
Preferably, the benzene additive comprises one or more of biphenyl, cyclohexylbenzene, fluorobiphenyl, tert-butyl benzene and tert-amylbenzene.
Has the advantages that: the additives are benzene additives in the lithium ion battery, and all the additives can be dissolved in the organic solvent in the invention and then extracted and separated from the sample solution.
Preferably, the nitric acid solution in the step (1) is a 1+2 system, namely a mixed solution of 1 volume of concentrated nitric acid and 2 volumes of water, and the concentration of the silver nitrate solution is 17 g/L; the concentration of the mother liquor of the chloride standard solution is 10 mu g/ml; the volume ratio of the nitric acid solution to the silver nitrate solution to the chloride standard solution mother liquor is 5:1: 15.
Has the advantages that: under the conditions, all the chloride in the sample solution can react with the silver nitrate to generate a precipitate, so that the accuracy of a detection result is improved.
Preferably, the standing time in the step (1) is 15-20 min.
Has the advantages that: in the standing time, the reaction can be completely carried out, and the precipitate is uniformly dispersed in the solution so as to be convenient for comparison with a sample solution.
Preferably, the organic solvent is any one or more of dichloromethane or dichloroethane.
Has the advantages that: the organic solvent can effectively dissolve the benzene additives in the lithium ion battery, and meanwhile, the dichloromethane is insoluble in water, so that the benzene additives and the dichloromethane which is slightly soluble in water can be effectively separated from the water solution, and further, the influence of the benzene additives on chloride detection is reduced.
Preferably, the mass ratio of the sample, the organic solvent and the water is 1:1: 2.
Has the advantages that: under the proportion, the benzene additives in the sample can be completely transferred into the organic solvent, and the chlorides and the like in the sample can be transferred into water, so that the content of the benzene additives in the sample is greatly reduced, and the influence of the benzene additives on a chloride aqueous solution is reduced.
Preferably, the standing time in the step (2) is 15-20 min.
Has the advantages that: during the above-mentioned standing time, it is sufficient to separate the organic solvent from the aqueous sample solution, thereby facilitating the extraction.
According to the technical scheme, compared with the prior art, the method for detecting the chloride content in the electrolyte for the lithium ion battery is disclosed, wherein the quantitative detection method disclosed by the invention not only effectively controls the influence of white suspended matters generated when the benzene-containing additive reacts with water on an observation result, improves the test accuracy, but also saves time, provides analysis data and direction guidance for the industrialization of the lithium ion battery, and promotes the development of the lithium ion battery industry.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The embodiment of the invention discloses a method for detecting the content of chloride in electrolyte for a lithium ion battery, wherein the lithium ion battery comprises benzene additives, and the detection method comprises the following steps:
(1) preparing a standard series of: preparing standard chloride solution mother liquor with different volumes and concentrations from standard chloride solution mother liquor with different volumes and concentrations, and then respectively adding the same nitric acid solution and silver nitrate solution into the standard chloride solution series for treatment and then standing;
wherein, the standard series of chlorides is marked as A according to the volume of mother liquor used in the preparation1、A2、A3......An；
(2) Preparing a sample solution: uniformly mixing an organic solvent, distilled water and a sample to be detected, standing, taking supernatant after layering, adding the supernatant into a colorimetric tube, adding a nitric acid solution and a silver nitrate solution which have the same concentration and volume as those in the step (1) into the supernatant, and standing to obtain a sample solution;
(3) determination of AnThe value: the turbidity of the sample is compared with the standard chloride series one by using a turbidimetric method to find out the standard chloride series A closest to the turbidity of the samplen；
(4) And (4) calculating a result:
calculated as Cl according to the formula-And (3) measuring the chloride content:
in the formula:
x- - -with Cl-Calculating the chloride content, ug/g;
Anvolume value of mother liquor in standard series of chlorides closest to turbidity of the sample，ml；
m-the mass of the sample to be measured, g.
Further, the benzene additives comprise any one or more of biphenyl, cyclohexylbenzene, fluorobiphenyl, tert-butyl benzene and tert-amylbenzene.
In order to further optimize the technical scheme, the nitric acid solution in the step (1) is a 1+2 system, and the concentration of the silver nitrate solution is 17 g/L; the concentration of the mother liquor of the chloride standard solution is 10 mu g/ml; the volume ratio of the nitric acid solution, the silver nitrate solution and the chloride standard solution mother liquor is 5:1: 15.
Further, the standing time in the step (1) is 15-20 min.
Further, the organic solvent is any one or more of dichloromethane or dichloroethane.
Further, the mass ratio of the sample, the organic solvent and the water is 1:1: 2.
Further, the standing time in the step (2) is 15-20 min.
Example 1
A method for detecting the chloride content in electrolyte for a lithium ion battery comprises the following steps of:
(1) glassware and reagent
A. Glass instrument: a 50ml colorimetric cylinder;
B. reagent: nitric acid solution (1+ 2); silver nitrate solution (17 g/L); chloride standard solution mother liquor (1ml solution containing 10ug of chloride); dichloromethane (analytical pure).
(2) Preparing a standard series of:
transferring 0.20ml, 0.40ml, 0.60ml, 0.80ml and 1.00ml of chloride standard solution mother liquor (1ml is 10ug chloride) into a series of 50ml colorimetric tubes, diluting the mixture with water to about 15ml, adding 5ml of nitric acid solution and 1ml of silver nitrate solution, diluting the mixture with water to 25ml, shaking the mixture evenly, and standing the mixture for 15min to obtain a chloride standard series. Wherein the chloride standard series are respectively marked as A according to the volume of the added mother liquor1、A2、A3、A4、A5。
(3) Testing of samples
Weighing 10g of sample to be detected, adding 10g of dichloromethane and 20ml of distilled water, uniformly mixing, standing for 30min, layering, taking 15ml of supernatant, adding into a 50ml colorimetric tube, simultaneously treating with the standard series solution from the addition of 5ml of nitric acid solution, comparing with the standard series one by one, and finding out A close to the A in the standard seriesnValue (ml).
(4) Calculation of results
In the formula: x represents the chloride content in terms of Cl < - >, ug/g;
An-volume value of mother liquor in chloride standard series, ml, closest to turbidity of the sample;
m-mass (g) of the sample to be measured.
And (4) carrying out three times of full-item detection on the same batch of samples in the step (3), wherein the results are as follows:
example 2
A method for detecting the chloride content in electrolyte for a lithium ion battery is different from that in embodiment 1:
in the step (3), dichloroethane is used as an organic solvent for extraction.
The results show that the method for measuring the chloride content has RSD percent less than 3, can completely meet the error requirement and has higher precision.
Comparative example 1
A method for detecting the chloride content in electrolyte for a lithium ion battery is different from that in embodiment 1:
no organic solvent was used for extraction during sample solution preparation.
After three full-item detections are performed on the same batch of samples in the step (3), the results are as follows:
in the detection process, after a sample meets a nitric acid aqueous solution, the sample becomes turbid without adding a silver nitrate solution, and the subsequent turbidity result is influenced, and compared with the example 1-2, the relative deviation in the example 1-2 is obviously lower than that in the comparative example 1, namely, the test result in the example 1-2 of the invention is close to the true value, the turbidity result in the method in the comparative example is higher, and the test data is inaccurate.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A method for detecting the chloride content in electrolyte for a lithium ion battery is characterized in that the lithium ion battery comprises benzene additives, and the detection method comprises the following steps:
(1) preparing a standard series of: preparing standard chloride solution mother liquor with different volumes and concentrations from standard chloride solution mother liquor with different volumes and concentrations, adding the same nitric acid solution and silver nitrate solution into the standard chloride solution mother liquor, and standing;
wherein, the standard series of chlorides is marked as A according to the volume of mother liquor used in the preparation1、A2、A3......An；
(2) Preparing a sample solution: uniformly mixing an organic solvent, distilled water and a sample to be detected, standing, taking supernatant after layering, adding the supernatant into a colorimetric tube, adding a nitric acid solution and a silver nitrate solution which have the same concentration and volume as those in the step (1) into the supernatant, and standing to obtain a sample solution;
(3) determination of AnThe value: the turbidity of the sample solution is compared with the standard chloride series one by using a turbidimetric method to obtain the standard chloride series A closest to the turbidity of the samplen；
(4) And (4) calculating a result:
according to the volume value A of the mother liquor in the chloride standard series closest to the turbidity of the sample solutionnAnd calculating the mass of the sample to be measured by using Cl in the sample solution-And (6) calculating the chloride content.
2. The method for detecting the chloride content in the electrolyte for the lithium ion battery according to claim 1, wherein the benzene additive comprises any one or a mixture of biphenyl, cyclohexylbenzene, fluorobiphenyl, tert-butyl benzene and tert-amylbenzene.
3. The method for detecting the chloride content in the electrolyte for the lithium ion battery according to claim 2, wherein the nitric acid solution in the step (1) is a 1+2 system, and the concentration of the silver nitrate solution is 17 g/L; the concentration of the mother liquor chloride is 10 mu g/ml; the volume ratio of the nitric acid solution to the silver nitrate solution to the mother liquor is 5:1: 15.
4. The method for detecting the chloride content in the electrolyte for the lithium ion battery according to claim 2, wherein the standing time in the step (1) is 15-20 min.
5. The method for detecting the chloride content in the electrolyte for the lithium ion battery according to any one of claims 1 to 4, wherein the organic solvent in the step (2) is any one or more of dichloromethane or dichloroethane.
6. The method for detecting the chloride content in the electrolyte for the lithium ion battery according to claim 5, wherein the mass ratio of the sample, the organic solvent and the distilled water in the step (2) is 1:1: 2.
7. The method for detecting the chloride content in the electrolyte for the lithium ion battery according to claim 5, wherein the standing time in the step (2) is 15-20 min.
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