CN111141725A - Quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte - Google Patents
Quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte Download PDFInfo
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Abstract
The invention discloses a method for quantitatively detecting lithium hexafluorophosphate in lithium ion battery electrolyte, which comprises the steps of diluting and dissolving lithium hexafluorophosphate by an organic solution, preparing standard series with different concentrations, testing the phosphorus content in a sample to be detected with the same volume by adopting a plasma emission spectrometer, measuring the peak area or peak height of each peak at the same time, and drawing a standard curve for the phosphorus concentration of the sample by using the peak area or peak height; and testing the lithium ion battery electrolyte sample to be tested by using the same test condition requirements, then directly observing the content of phosphorus ions in the electrolyte to be tested on a standard curve according to a spectrum peak or a spectrum height, and finally calculating the content of lithium hexafluorophosphate according to the content of the phosphorus ions. The technical scheme disclosed by the invention is simple and easy to implement, avoids errors introduced in the sample pretreatment process, provides analysis data and direction guidance for the development of the lithium ion battery, and promotes the industry development.
Description
Technical Field
The invention relates to the technical field of lithium ion battery electrolysis, in particular to a quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte.
Background
The concentration of lithium hexafluorophosphate in the lithium ion battery electrolyte directly influences the performances of the battery, such as conductivity, rate performance, internal resistance and the like, and then directly influences the product quality and the performance of the battery, and the lithium hexafluorophosphate is expensive, so that the accurate determination of the content of the lithium hexafluorophosphate in the lithium ion battery electrolyte is very important.
The conventional lithium hexafluorophosphate quantitative method comprises an atomic absorption method, a spectrophotometric method, an ion chromatography method and a precipitation method, and due to technical limitation, a sample needs to be subjected to pretreatment such as extraction or digestion, so that the test time is relatively long, and the test precision is difficult to meet the requirement.
The invention designs a quantitative method for lithium hexafluorophosphate in the lithium ion battery electrolyte without sample pretreatment by combining the practical experience of the analysis work of the lithium ion electrolyte for many years, thereby effectively saving time, avoiding errors introduced in the pretreatment process, simultaneously providing analysis data and direction guidance for the development of the lithium ion battery and promoting the industry development.
Disclosure of Invention
In view of the above, the invention provides a quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte, which is simple and effective, provides analysis data and direction guidance for industrialization of lithium ion batteries, and promotes development of the lithium ion battery industry.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for quantitatively detecting lithium hexafluorophosphate in lithium ion battery electrolyte is characterized in that sample pretreatment is omitted, and the content of lithium hexafluorophosphate in the lithium ion battery electrolyte is quantitatively calculated by detecting phosphorus ions in the electrolyte by using a plasma emission spectrometer.
Preferably, in the method for quantitatively detecting lithium hexafluorophosphate in the lithium ion battery electrolyte, the method specifically comprises the following steps:
(1) drawing a standard curve: diluting and dissolving lithium hexafluorophosphate by using an organic solution, preparing standard series with different concentrations, then testing the phosphorus content in a lithium hexafluorophosphate sample to be tested with the same volume by using a plasma emission spectrometer, simultaneously measuring the peak area or peak height of each peak, and drawing a standard curve for the phosphorus concentration in the lithium hexafluorophosphate sample by using the peak area or peak height;
specifically, lithium hexafluorophosphate with different masses is respectively added into an organic solution to prepare standard series with different concentrations, wherein the mass of the lithium hexafluorophosphate is weighed to be 0.15g, 0.30g, 0.45g, 0.60g and 0.75g, the lithium hexafluorophosphate with different masses is respectively diluted to 150g by the organic solution, a plasma emission spectrometer is used for testing the phosphorus content in a lithium hexafluorophosphate sample to be tested with the same volume, the peak area or peak height of each peak is simultaneously measured, and a standard curve is drawn by the peak area or peak height for the phosphorus concentration in the lithium hexafluorophosphate sample.
(2) Preparing a lithium ion battery electrolyte sample: weighing 0.50-1.50g of a sample to be detected, and dissolving the sample by using an organic solution to prepare a lithium ion battery electrolyte sample;
(3) quantitative determination of lithium hexafluorophosphate: and (3) testing the lithium ion battery electrolyte sample prepared in the step (2) by using the same test condition requirements, then directly observing the phosphorus ion content in the electrolyte to be tested on the standard curve drawn in the step (1) according to the spectrum peak or the spectrum height, and finally quantitatively calculating the content of lithium hexafluorophosphate in the electrolyte according to the phosphorus ion content.
Preferably, in the method for quantitatively detecting lithium hexafluorophosphate in the lithium ion battery electrolyte, the organic solution is a mixed solution prepared from 10g of an organic solvent, 30g of anhydrous ethanol and 50g of water.
Preferably, in the method for quantitatively detecting lithium hexafluorophosphate in the lithium ion battery electrolyte, the organic solvent is dimethyl carbonate, ethyl methyl carbonate, ethylene carbonate or ethyl methyl carbonate.
According to the technical scheme, compared with the prior art, the invention discloses a quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte, firstly, a plasma emission spectrometer is adopted to test the phosphorus content in a lithium ion battery electrolyte standard system with the same volume and different concentrations, and a standard curve is drawn at the same time;
and then, testing the electrolyte sample by using a plasma emission spectrometer, directly observing the content of phosphorus ions in the electrolyte sample on a drawn standard curve according to a spectral peak or spectral height, and finally quantitatively calculating the content of lithium hexafluorophosphate in the lithium ion battery electrolyte according to the content of the phosphorus ions.
The quantitative detection method disclosed by the invention not only effectively saves time and avoids errors introduced in a pretreatment process, but also provides analysis data and direction guidance for industrialization of the lithium ion battery, and promotes the development of the lithium ion battery industry.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a graph showing a standard curve of phosphorus concentration in a lithium hexafluorophosphate sample of 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 specification 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.
The embodiment of the invention discloses a quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte, which is simple and effective, provides analysis data and direction guidance for industrialization of lithium ion batteries, and promotes the development of the lithium ion battery industry.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
The invention discloses a quantitative detection method of lithium hexafluorophosphate in lithium ion battery electrolyte, which avoids sample pretreatment and quantitatively calculates the content of lithium hexafluorophosphate in the lithium ion battery electrolyte by adopting a plasma emission spectrometer to detect phosphorus ions in the electrolyte.
In order to further realize the technical effect of the invention, the quantitative detection method specifically comprises the following steps:
(1) drawing a standard curve: diluting and dissolving lithium hexafluorophosphate by using an organic solution, preparing standard series with different concentrations, then testing the phosphorus content in a lithium hexafluorophosphate sample to be tested with the same volume by using a plasma emission spectrometer, simultaneously measuring the peak area or peak height of each peak, and drawing a standard curve for the phosphorus concentration in the lithium hexafluorophosphate sample by using the peak area or peak height;
(2) preparing a lithium ion battery electrolyte sample: weighing 0.50-1.50g of a sample to be detected, and dissolving the sample by using an organic solution to prepare a lithium ion battery electrolyte sample;
(3) quantitative determination of lithium hexafluorophosphate: and (3) testing the lithium ion battery electrolyte sample prepared in the step (2) by using the same test condition requirements, then directly observing the phosphorus ion content in the electrolyte to be tested on the standard curve drawn in the step (1) according to the spectrum peak or the spectrum height, and finally quantitatively calculating the content of lithium hexafluorophosphate in the electrolyte according to the phosphorus ion content.
In order to further achieve the technical effect of the present invention, the organic solution in the step (1) is a mixed solution prepared from 10g of emc, 30g of anhydrous ethanol and 50g of water.
In order to further achieve the technical effects of the present invention, the organic solvent is dimethyl carbonate, ethyl methyl carbonate, ethylene carbonate or ethyl methyl carbonate.
The technical solution of the present invention will be further described with reference to the following specific examples.
A quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte comprises the following specific steps:
(1) instrument and reagent
A. The equipment configuration: an Optima7300v type inductively coupled plasma emission spectrometer, a hydrofluoric acid corrosion resistant sample injection system;
B. organic solution: 10g of EMC, 30g of absolute ethanol and 50g of water were mixed uniformly.
(2) Drawing a standard curve:
A. weighing lithium hexafluorophosphate with different masses, dissolving the lithium hexafluorophosphate in an organic solution, and drawing a standard curve;
B. the organic solvent is a mixed solution prepared from 10g of EMC, 30g of absolute ethyl alcohol and 50g of water.
(3) Testing of samples
A. Weighing a certain amount of sample, dissolving the sample in an organic solution, and testing by using ICP-OES;
B. the weighing amount of the sample ranges from 0.50 g to 1.50 g;
C. the organic solvent is a mixed solution prepared from 10g of EMC, 30g of absolute ethyl alcohol and 50g of water.
Specifically, the detection results are as follows:
drawing a standard curve
A. Preparing a standard curve:
standard solution 1: respectively and precisely weighing 0.15g of lithium hexafluorophosphate by a one-thousandth balance to dissolve the lithium hexafluorophosphate into the organic solution, and quantifying to 150 g;
and (3) standard solution 2: respectively and precisely weighing 0.30g of lithium hexafluorophosphate by a one-thousandth balance to dissolve the lithium hexafluorophosphate into the organic solution, and quantifying to 150 g;
and (3) standard solution: respectively and precisely weighing 0.45g of lithium hexafluorophosphate by a one-thousandth balance to dissolve the lithium hexafluorophosphate into the organic solution, and quantifying to 150 g;
and (4) standard solution: respectively and precisely weighing 0.60g of lithium hexafluorophosphate by a one-thousandth balance to dissolve the lithium hexafluorophosphate into the organic solution, and quantifying to 150 g;
and (5) standard solution: 0.75g of lithium hexafluorophosphate was precisely weighed by a one-thousandth balance and dissolved in the organic solution, and the amount was determined to 150 g.
B. Drawing of standard curve
Specifically, the standard curve for lithium hexafluorophosphate is shown in figure 1. The results of the specific analysis are shown in table 1 below for the standard curve.
| Lithium hexafluorophosphate mass (g) | Phosphorus concentration C (mg/L) | Peak height intensity value A |
| 0.15 | 203.9 | 10106.1 |
| 0.30 | 409.2 | 19682.1 |
| 0.45 | 614.4 | 29929 |
| 0.60 | 819.6 | 38959.1 |
| 0.75 | 1018.1 | 47885.8 |
Wherein the standard curve is C ═ 0.0215A-16.759
In the formula: a: peak height intensity values; c: p concentration value, unit mg/L.
(II) sample testing
A. Weighing 1.0000g of electrolyte sample (m) in a clean tetrafluoro bottle, and quantifying to 30.0000g by using an organic solution; the three electrolytes are measured by adopting the preparation method, wherein two parallel test samples are prepared from the same electrolyte sample to be measured.
B. The samples formulated in step a) were tested according to ICP-OES operating requirements.
(III) calculation of results
Specific detection data and results are shown in table 2 below.
TABLE 2 results of two-time detection of three electrolyte species
The results show that the method for determining the content of the lithium hexafluorophosphate in the lithium ion battery electrolyte can completely meet the requirement of absolute error of +/-0.5 percent, has high precision, and can meet the requirement of 98-102 percent by using the recovery rate to judge the accuracy.
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 (4)
1. A quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte is characterized in that sample pretreatment is omitted, and a plasma emission spectrometer is adopted to detect phosphorus ions in the electrolyte so as to quantitatively calculate the content of lithium hexafluorophosphate in the lithium ion battery electrolyte.
2. The method according to claim 1, wherein the method specifically comprises the following steps:
(1) drawing a standard curve: diluting and dissolving lithium hexafluorophosphate by using an organic solution, preparing standard series with different concentrations, then testing the phosphorus content in a lithium hexafluorophosphate sample to be tested with the same volume by using a plasma emission spectrometer, simultaneously measuring the peak area or peak height of each peak, and drawing a standard curve for the phosphorus concentration in the lithium hexafluorophosphate sample by using the peak area or peak height;
(2) preparing a lithium ion battery electrolyte sample: weighing 0.50-1.50g of a sample to be detected, and dissolving the sample by using an organic solution to prepare a lithium ion battery electrolyte sample;
(3) quantitative determination of lithium hexafluorophosphate: and (3) testing the lithium ion battery electrolyte sample prepared in the step (2) by using the same test condition requirements, then directly observing the phosphorus ion content in the electrolyte to be tested on the standard curve drawn in the step (1) according to the spectrum peak or the spectrum height, and finally quantitatively calculating the content of lithium hexafluorophosphate in the electrolyte according to the phosphorus ion content.
3. The method according to claim 2, wherein the organic solution is a mixed solution prepared from 10g of an organic solvent, 30g of anhydrous ethanol and 50g of water.
4. The method of claim 3, wherein the organic solvent is dimethyl carbonate, ethyl methyl carbonate, ethylene carbonate or ethyl methyl carbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114184710A (en) * | 2021-12-24 | 2022-03-15 | 合肥国轩高科动力能源有限公司 | Method for detecting content of lithium hexafluorophosphate in lithium ion battery electrolyte |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005201762A (en) * | 2004-01-15 | 2005-07-28 | Toshiba Corp | Lithium leak detector and lithium leak detection method |
| CN1888893A (en) * | 2006-07-21 | 2007-01-03 | 天津力神电池股份有限公司 | Ion chromatography method for measuring lithium salt density in lithiumion cell electrolyte |
| CN105548146A (en) * | 2015-12-09 | 2016-05-04 | 九江天赐高新材料有限公司 | Determination method for concentration of lithium hexafluorophosphate in lithium-ion battery electrolyte |
| CN108614028A (en) * | 2018-04-09 | 2018-10-02 | 杉杉新材料（衢州）有限公司 | The analysis method of metal ion in a kind of lithium ion battery preparation process |
| CN109900684A (en) * | 2019-04-22 | 2019-06-18 | 杉杉新材料（衢州）有限公司 | A kind of measuring method of lithium salt in lithium ion battery electrolyte content |
-
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- 2019-12-26 CN CN201911368032.6A patent/CN111141725A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005201762A (en) * | 2004-01-15 | 2005-07-28 | Toshiba Corp | Lithium leak detector and lithium leak detection method |
| CN1888893A (en) * | 2006-07-21 | 2007-01-03 | 天津力神电池股份有限公司 | Ion chromatography method for measuring lithium salt density in lithiumion cell electrolyte |
| CN105548146A (en) * | 2015-12-09 | 2016-05-04 | 九江天赐高新材料有限公司 | Determination method for concentration of lithium hexafluorophosphate in lithium-ion battery electrolyte |
| CN108614028A (en) * | 2018-04-09 | 2018-10-02 | 杉杉新材料（衢州）有限公司 | The analysis method of metal ion in a kind of lithium ion battery preparation process |
| CN109900684A (en) * | 2019-04-22 | 2019-06-18 | 杉杉新材料（衢州）有限公司 | A kind of measuring method of lithium salt in lithium ion battery electrolyte content |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114184710A (en) * | 2021-12-24 | 2022-03-15 | 合肥国轩高科动力能源有限公司 | Method for detecting content of lithium hexafluorophosphate in lithium ion battery electrolyte |
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Application publication date: 20200512 |