CN106970103B - The detection method of impurity in lithium hexafluoro phosphate - Google Patents

The detection method of impurity in lithium hexafluoro phosphate Download PDF

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CN106970103B
CN106970103B CN201710197720.5A CN201710197720A CN106970103B CN 106970103 B CN106970103 B CN 106970103B CN 201710197720 A CN201710197720 A CN 201710197720A CN 106970103 B CN106970103 B CN 106970103B
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hexafluoro phosphate
lithium hexafluoro
phosphorus
deuterated
fluorine
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CN201710197720.5A
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CN106970103A (en
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罗海英
孙伏恩
丁友婷
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广州天赐高新材料股份有限公司
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Abstract

The invention discloses a kind of detection methods of lithium hexafluoro phosphate impurity, include the following steps: that (1) is calibrated: using coaxial nuclear magnetic tube, it is separately added into the deuterated reagent solution of phenyl-hexafluoride and the deuterated reagent solution of lithium hexafluoro phosphate in inner and outer pipes, carries out fluorine spectrum detection;Using coaxial nuclear magnetic tube, it is separately added into the deuterated reagent solution of phosphoric acid and the deuterated reagent solution of lithium hexafluoro phosphate in inner and outer pipes, carries out phosphorus spectrum detection;(2) it measures: lithium hexafluoro phosphate and deuterated reagent is configured to certain density sample to be tested, fluorine spectrum and phosphorus spectrum detection are carried out using Nuclear Magnetic Resonance.The detection method can have many advantages, such as analysis time section, easy to operate, high sensitivity to the qualitative and quantitative detection containing phosphorus impurities fluorine-containing in lithium hexafluoro phosphate, opposite conventional method, can damage to avoid fluorine-containing strong corrosive material to equipment.

Description

The detection method of impurity in lithium hexafluoro phosphate

Technical field

The present invention relates to chemical analysis methods, more particularly to the detection method containing phosphorus impurities fluorine-containing in lithium hexafluoro phosphate.

Background technique

Lithium ion battery is the green high-capacity environment-protecting battery occurred the 1990s, is had been widely used at present portable The fields such as electronic product, electric tool, electric bicycle.Wherein organic electrolyte is the important component of lithium ion battery, It carries the effect that charge is transmitted between positive and negative anodes in the battery, therefore the dopant type of electrolyte and content directly influence The usability and safety of battery.

The impurity of General Influence battery performance has: water and hydrofluoric acid, foreign metal ion, the object containing oxidation or reproducibility Matter and the organic matter containing active hydrogen etc..At present in electrolyte lithium salts and organic solvent water, hydrofluoric acid, foreign metal from Son, part residual organic solvent have had more mature detection method, can preferably assess the content of these impurity.But still There are some activity relatively strong or the impurity containing redox property fail sufficiently to analyze, and just because of these active objects Matter easily causes electrolyte change colour, is unstable.The discoloration of current electrolysis liquid is also a problem urgently to be solved in battery industry, is had Relevant report shows that the trifluoro oxygen phosphorus in electrolyte, the impurity such as fluorination phosphorus form organic with color during electrolyte is stored Object or complex compound.These impurity such as trifluoro oxygen phosphorus, fluorination phosphorus are mainly introduced by electrolyte lithium salts, at present to this type in lithium salts The qualitative and quantitative report of impurity is very few.Therefore a set of quick, simple, accurately inspection is established to the qualitative, quantitative of lithium salts impurity Survey method is particularly important, by the monitoring and analysis to lithium salts impurity, to investigate the mechanism of electrolyte discoloration, to solve to change colour Problem.The service performance and security performance of lithium battery can be improved.

Summary of the invention

Based on this, the object of the present invention is to provide a kind of fluorine-containing methods containing phosphorus impurities in detection lithium hexafluoro phosphate.

Specific technical solution is as follows:

The fluorine-containing detection method containing phosphorus impurities in a kind of lithium hexafluoro phosphate, includes the following steps:

(1) it calibrates:

Using coaxial nuclear magnetic tube, be separately added into inner and outer pipes phenyl-hexafluoride deuterated reagent solution and lithium hexafluoro phosphate it is deuterated Reagent solution carries out fluorine spectrum detection;

Using coaxial nuclear magnetic tube, the deuterated examination of the deuterated reagent solution and lithium hexafluoro phosphate of phosphoric acid is separately added into inner and outer pipes Agent solution carries out phosphorus spectrum detection;

(2) it measures

Lithium hexafluoro phosphate and deuterated reagent are configured to certain density sample to be tested, fluorine spectrum is carried out using Nuclear Magnetic Resonance It composes and detects with phosphorus;

The testing conditions of the Nuclear Magnetic Resonance are as follows:

Fluorine spectral condition: NS=128;Field width is 90~-200ppm, pulse train zgfhigqn.2;

Phosphorus spectral condition: NS=512, field width are 150~-250ppm, pulse train zgpg30.

The qualitative impurity of peak shift is composed according to fluorine spectrum and phosphorus, further according to the peak area quantification impurity content of fluorine spectrum, is calculated public Formula is as follows:

In formula: W is content, and unit is μ g/g;

A1For impurity peak area;

A2For the peak area of lithium hexafluoro phosphate

n1For the proton number of impurity group;

n2For the proton number of lithium hexafluoro phosphate;

M1For the molal weight of impurity, g/mol

M2For the molal weight of lithium hexafluoro phosphate, g/mol

C2For the content (m/m) of lithium hexafluoro phosphate;%.

In wherein some embodiments, the fluorine spectral condition: NS=128;Field width is 90~-200ppm, pulse train is Zgfhigqn.2, data point 64k, single acquisition time are 6s.

In wherein some embodiments, phosphorus spectral condition: NS=512, field width are 150~-250ppm, and pulse train is Zgpg30, single acquisition time are 0.5s, data point 976k.

In wherein some embodiments, the concentration of phenyl-hexafluoride is 150-250 μ g/ in the deuterated reagent solution of the phenyl-hexafluoride G, the concentration of lithium hexafluoro phosphate is 10~40wt% in the deuterated reagent solution of the lithium hexafluoro phosphate;The deuterated examination of the phosphoric acid The concentration of phosphoric acid is 800-1200 μ g/g in agent solution, the time that the lithium hexafluorophosphate solution that is configured is stood be 0min~ 60min。

In wherein some embodiments, the deuterated reagent is deuterated acetone, deuterated acetonitrile or deuterated dimethyl sulfoxide.

In wherein some embodiments, the deuterated reagent also need carry out pre-treatment, by moisture content be down to 10 μ g/g with It is interior.

In wherein some embodiments, the method for the pre-treatment are as follows: deuterated reagent is subjected to molecular sieve dehydration or use Calcium hydride reflux distillation water removal.

In wherein some embodiments, the impurity in the lithium hexafluoro phosphate is fluorine-containing phosphorus-containing compound.

In wherein some embodiments, the fluorine-containing phosphorus-containing compound is phosphorus pentafluoride, phosphorus trifluoride, trifluoro oxygen phosphorus, two Fluorophosphoric acid, difluorophosphate, monofluorophosphoric acid lithium or monofluorophosphoric acid.

The advantages of above-mentioned detection method: firstly, commercially available deuterated reagent all contains a certain amount of moisture, (600 μ g/g are left It is right), and part deuterated reagent water imbibition is very big, such as deuterated acetonitrile, deuterated dimethyl sulfoxide.Moisture pair in deuterated reagent Lithium salts test has a great impact, and the accuracy of testing result can be improved by removing water;Second, trifluoro oxygen phosphorus, phosphorus pentafluoride Equal impurity belong to harmful influence and unstable, it is more difficult to obtain standard sample, be not necessarily to standard reagent using relative measurement method.Third is right In this kind of fluorine-containing strong corrosive material, relatively traditional chromatographic process will not damage equipment;4th, the sample that this method needs The advantages that product amount is few, the testing time is short, high sensitivity.Impurity can be carried out simultaneously qualitative;5th, this method is suitable for electrolysis The fluorine-containing quantitative analysis containing phosphorus impurities in liquid.

The detection method quantitative to lithium hexafluoro phosphate impurity quantification using Nuclear Magnetic Resonance of the invention, using relative measurement Method detects the fluorine-containing phosphorus impurities that contain in lithium hexafluoro phosphate.Its data studies electrolyte Discoloration mechanism, electrolyte stores Stable investigation provides theoretical foundation.It can be used for improving the safety of electrolyte, battery.

The detection method can have analysis time to the qualitative and quantitative detection containing phosphorus impurities fluorine-containing in lithium hexafluoro phosphate The advantages that short, easy to operate, high sensitivity, opposite conventional method can damage to avoid fluorine-containing strong corrosive material to equipment. This method is widely used, and can be widely applied to the measurement of electrolyte lithium salt impurity.

Detailed description of the invention

Fig. 1 is 1 lithium hexafluoro phosphate fluorine of embodiment spectrum;

Fig. 2 is 1 lithium hexafluoro phosphate phosphorus of embodiment spectrum;

Fig. 3 is the lithium hexafluoro phosphate fluorine spectrum of 1 nuclear-magnetism testing conditions of embodiment screening;

Fig. 4 is the lithium hexafluoro phosphate fluorine spectrum of 1 nuclear-magnetism testing conditions of embodiment screening;

Fig. 5 is the lithium hexafluoro phosphate fluorine spectrum of 1 nuclear-magnetism testing conditions of embodiment screening;

Fig. 6 is the enlarged drawing of Fig. 5;

Fig. 7 is the lithium hexafluoro phosphate fluorine spectrum of 1 nuclear-magnetism testing conditions of embodiment screening;

Fig. 8 is the enlarged drawing of Fig. 7.

Specific embodiment

It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes It is more thorough and comprehensive to the understanding of the disclosure.

Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases Any and all combinations of the listed item of pass.

Reagent and instrument:

Reagent: lithium hexafluoro phosphate (99.99% or more content), deuterated acetonitrile, deuterated acetone, deuterated dimethyl sulfoxide (deuterium It is sigma reagent for reagent);Calcium hydride, phenyl-hexafluoride, phosphoric acid

Instrument: PABBO BB probe, the molecular sieve, distilling apparatus, moisture of glove box, 400M NMR (Brooker), 5mm The nuclear magnetic tube of instrument, 5mm.

Embodiment 1

The present embodiment detects lithium hexafluoro phosphate impurity quantification and quantitative approach, comprising the following steps:

(1) deuterated solvent pre-treatment;

In nitrogen charging glove box, deuterated acetonitrile is removed water within 10 μ g/g using molecular sieve (using karl Fischer moisture Instrument tests moisture content).

(2) it calibrates

Using coaxial nuclear magnetic tube, be separately added into inner and outer pipes concentration be 200 μ g/g phenyl-hexafluoride deuterated acetonitrile solution and The deuterated acetonitrile solution of lithium hexafluoro phosphate carries out fluorine spectrum detection;As shown in Figure 1.

Be separately added into inner and outer pipes concentration be 1000 μ g/g phosphoric acid deuterated acetonitrile solution and lithium hexafluoro phosphate it is deuterated Acetonitrile solution carries out phosphorus spectrum detection;As shown in Figure 2.

(3) lithium hexafluoro phosphate preparation of samples;

In glove box, the deuterated acetonitrile of the water removal of step (1) is taken, a certain amount of lithium hexafluoro phosphate is added and is configured to The solution of 40wt% pipettes lithium hexafluorophosphate solution 0.5ml to nuclear magnetic tube, and lid is to be measured after covering to be detected at once.

(4) nuclear magnetic tube sample is taken out to the detection for carrying out fluorine spectrum and phosphorus spectrum immediately, nuclear-magnetism testing conditions from glove box are as follows: Fluorine composes NS=128;Field width is 90~-200ppm, pulse train zgfhigqn.2, data point 64k, and the single acquisition time is 6s;Phosphorus composes NS=512, and field width is 150~-250ppm, and pulse train zgpg30, the single acquisition time is 0.5s, data point For 976k.

According to nuclear magnetic resonance coupling, a point principle is split, spin/spin coupling effect of adjacent atom core and resonant nucleus makes to resonate The principle that frequency is split point, in analysis of spectra each peak split point and coupling condition, the composition of qualitative impurity, as shown in table 1, Impurity content is quantified further according to fluorine spectral peak area, shown in calculation formula such as formula (1): testing result is as shown in table 2.

In formula: W is content, and unit is μ g/g;

A1For impurity peak area;

A2For the peak area of lithium hexafluoro phosphate

n1For the proton number of impurity group;

n2For the proton number of lithium hexafluoro phosphate;

M1For the molal weight of impurity, g/mol

M2For the molal weight of lithium hexafluoro phosphate, g/mol

C2For the content (m/m) of lithium hexafluoro phosphate;%.

The screening of nuclear-magnetism testing conditions:

(1) parameter be field width be 90~-200ppm, pulse train zgfhigqn.2;AQ=0.5s;TD=32k, NS= 256

For spectrogram as shown in figure 3, collection point is inadequate, the single acquisition time is short, and spectrogram is observed that baseline is poor when amplifying, And it is difficult adjustment phase place, it can not accurately obtain integral area.But from the point of view of NS, impurity appearance is apparent.

(2) parameter be field width be 90~-200ppm, pulse train zgfhigqn.2;AQ=0.5s;TD=64k, NS= 128

Spectrogram is as shown in figure 4, spectrogram is observed that baseline is still poor when amplifying, and is difficult adjustment phase place, but phase There is part improvement for Fig. 3.But still it can not accurately obtain integral area.But from the point of view of NS, reduction remains to meet demand, together When with respect to Fig. 3 can shorten detection time.

(3) parameter be field width be 90~-200ppm, pulse train zgfhigqn.2;AQ=3s;TD=64k, NS=16

Spectrogram is as shown in Figure 5 and Figure 6, and Fig. 6 is the enlarged drawing of Fig. 5.Fig. 5 baseline has had a greater degree of improvement, but Find out that still some are slight uneven in enlarged drawing.But from the point of view of NS, 16 scanning circle numbers, some are less than normal, though it is still able to accumulate Point, but impurity smaller for content goes out the more difficult embodiment of summit, while being also not easy to integrate.

(4) parameter be field width be 90~-200ppm, pulse train zgfhigqn.2;AQ=6s;TD=64k, NS= 128

Spectrogram is as shown in FIG. 7 and 8, and Fig. 8 is the enlarged drawing of Fig. 7.It is seen as optimal effectiveness from amplification spectrogram, due to test It is the impurity of g/g grades of tens μ, need to ensures that baseline is smooth, integral is accurate, it is ensured that the accurate premise of test result.

Embodiment 2

The present embodiment detects lithium hexafluoro phosphate impurity quantification and quantitative approach, comprising the following steps:

(1) deuterated solvent pre-treatment;

In nitrogen charging glove box, deuterated acetone is removed water within 10 μ g/g using calcium hydride reflux distillation (using karr Take not Moisture Meter test moisture content).

(2) it calibrates

Using coaxial nuclear magnetic tube, be separately added into inner and outer pipes concentration be 200 μ g/g phenyl-hexafluoride deuterated acetone solution and The deuterated acetone solution of lithium hexafluoro phosphate carries out fluorine spectrum detection;

Be separately added into inner and outer pipes concentration be 1000 μ g/g phosphoric acid deuterated acetone solution and lithium hexafluoro phosphate it is deuterated Acetone soln carries out phosphorus spectrum detection;

(3) lithium hexafluoro phosphate preparation of samples;

In glove box, the deuterated acetone of the water removal of step (1) is taken, a certain amount of lithium hexafluoro phosphate is added and is configured to The solution of 20wt% pipettes lithium hexafluorophosphate solution 0.5ml to nuclear magnetic tube, and it is to be measured that lid stands 30min after covering.

(4) nuclear magnetic tube sample is taken out to the detection that fluorine spectrum and phosphorus spectrum are carried out after standing 20min, nuclear-magnetism testing conditions are as follows: fluorine Compose NS=128;Field width is 90~-200ppm, pulse train zgfhigqn.2, data point 64k, and the single acquisition time is 6s;Phosphorus composes NS=512, and field width is 150~-250ppm, and pulse train zgpg30, the single acquisition time is 0.5s, data point For 976k.According to the qualitative impurity of peak shift out, impurity content, calculation formula such as formula (1) institute are quantified further according to fluorine spectral peak area Show: testing result is as shown in table 2.

Embodiment 3

The present embodiment detects lithium hexafluoro phosphate impurity quantification and quantitative approach, comprising the following steps:

(1) deuterated solvent pre-treatment;

In nitrogen charging glove box, deuterated dimethyl sulfoxide is removed water within 10 μ g/g using molecular sieve (using karr expense Not Moisture Meter tests moisture content).

(2) it calibrates

Using coaxial nuclear magnetic tube, the deuterated dimethyl sulfoxide for the phenyl-hexafluoride that concentration is 200 μ g/g is separately added into inner and outer pipes The deuterated dimethyl sulfoxide solution of solution and lithium hexafluoro phosphate carries out fluorine spectrum detection;

Using coaxial nuclear magnetic tube, the deuterated dimethyl sulfoxide that the phosphoric acid that concentration is 1000 μ g/g is separately added into inner and outer pipes is molten The deuterated dimethyl sulfoxide solution of liquid and lithium hexafluoro phosphate carries out phosphorus spectrum detection;

(3) lithium hexafluoro phosphate preparation of samples;

In glove box, the deuterated dimethyl sulfoxide of the water removal of step (1) is taken, a certain amount of lithium hexafluoro phosphate is added and prepares At the solution of 5wt%, lithium hexafluorophosphate solution 0.5ml is pipetted to nuclear magnetic tube, lid is to be measured after covering.

(4) nuclear magnetic tube sample is taken out to the detection that fluorine spectrum and phosphorus spectrum are carried out after standing 60min, nuclear-magnetism testing conditions are as follows: fluorine Compose NS=128;Field width is 90~-200ppm, pulse train zgfhigqn.2, data point 64k, and the single acquisition time is 6s;Phosphorus composes NS=512, and field width is 150~-250ppm, and pulse train zgpg30, the single acquisition time is 0.5s, data point For 976k.According to the qualitative impurity of peak shift out, impurity content, calculation formula such as formula (1) institute are quantified further according to fluorine spectral peak area Show: testing result is as shown in table 2.

The fluorine spectrum and phosphorus spectral displacement of 1. lithium hexafluoro phosphate of table fluorine-containing phosphorus containg substances in deuterated acetonitrile

Note;Ownership is the group for having underscore meaning

The content of 2. lithium hexafluoro phosphate impurity of table

Note: N=8

Lithium hexafluoro phosphate is heated easily to be decomposed, and hydrofluoric acid, difluorophosphate, monofluorophosphoric acid lithium, simultaneously synthesizing technique are also easy to produce Also these impurity, especially trifluoro oxygen phosphorus are readily incorporated.By analyzing the content of these impurity, it is pure can preferably to assess product Degree, as can be seen from Table 2, these impurity can preferably assess its content by Nuclear Magnetic Resonance, and reproducible.Simultaneously This method is also applied for the analysis of fluorine-containing impurity in electrolyte.

Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.

The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (8)

1. the detection method of impurity in a kind of lithium hexafluoro phosphate, which comprises the steps of:
(1) deuterated reagent pre-treatment;
Pre-treatment is carried out to the deuterated reagent, moisture content is down within 10 μ g/g;
(2) it calibrates:
Using coaxial nuclear magnetic tube, the deuterated reagent solution of phenyl-hexafluoride and the deuterated reagent of lithium hexafluoro phosphate are separately added into inner and outer pipes Solution carries out fluorine spectrum detection;
Using coaxial nuclear magnetic tube, the deuterated reagent of deuterated reagent solution and lithium hexafluoro phosphate that phosphoric acid is separately added into inner and outer pipes is molten Liquid carries out phosphorus spectrum detection;
(3) it measures
Lithium hexafluoro phosphate and deuterated reagent are configured to certain density sample to be tested, fluorine spectrum and phosphorus are carried out using Nuclear Magnetic Resonance Spectrum detection;
The testing conditions of the Nuclear Magnetic Resonance are as follows:
Fluorine spectral condition: NS=128;Field width is 90~-200ppm, pulse train zgfhigqn.2;
Phosphorus spectral condition: NS=512, field width are 150~-250ppm, pulse train zgpg30;
The qualitative impurity of peak shift is composed according to fluorine spectrum and phosphorus, further according to the peak area of fluorine spectrum and phosphorus spectrum and uses relative measurement method, Impurity is quantified as follows;
In formula: W is content, and unit is μ g/g;
A1For impurity peak area;
A2For the peak area of lithium hexafluoro phosphate
n1For the proton number of impurity group;
n2For the proton number of lithium hexafluoro phosphate;
M1For the molal weight of impurity, g/mol
M2For the molal weight of lithium hexafluoro phosphate, g/mol
C2For the content (m/m) of lithium hexafluoro phosphate;%.
2. detection method according to claim 1, which is characterized in that the fluorine spectral condition: NS=128;Field width be 90~- 200ppm, pulse train zgfhigqn.2, data point 64k, single acquisition time are 6s.
3. detection method according to claim 1, which is characterized in that the phosphorus spectral condition: NS=512, field width 150 ~-250ppm, pulse train zgpg30, single acquisition time are 0.5s, data point 976k.
4. detection method according to claim 1, which is characterized in that the deuterated reagent is deuterated acetone, deuterated acetonitrile Or deuterated dimethyl sulfoxide.
5. detection method according to claim 1, which is characterized in that phenyl-hexafluoride in the deuterated reagent solution of the phenyl-hexafluoride Concentration be 150-250 μ g/g, in the deuterated reagent solution of the lithium hexafluoro phosphate concentration of lithium hexafluoro phosphate be 10~ 40wt%;The concentration of phosphoric acid is 800-1200 μ g/g in the deuterated reagent solution of the phosphoric acid.
6. detection method according to claim 1, which is characterized in that the method for the pre-treatment are as follows: by deuterated reagent into Row molecular sieve dehydration is removed water using calcium hydride reflux distillation.
7. detection method according to claim 1-5, which is characterized in that the impurity in the lithium hexafluoro phosphate is Fluorine-containing phosphorus-containing compound.
8. detection method according to claim 7, which is characterized in that the fluorine-containing phosphorus-containing compound is phosphorus pentafluoride, three It is fluorinated phosphorus, trifluoro oxygen phosphorus, difluorophosphoric acid, difluorophosphate, monofluorophosphoric acid lithium or monofluorophosphoric acid.
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