CN114054110B - Kit and method for testing HF content in electrolyte - Google Patents
Kit and method for testing HF content in electrolyte Download PDFInfo
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- CN114054110B CN114054110B CN202111363469.8A CN202111363469A CN114054110B CN 114054110 B CN114054110 B CN 114054110B CN 202111363469 A CN202111363469 A CN 202111363469A CN 114054110 B CN114054110 B CN 114054110B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- G—PHYSICS
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- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention provides a kit and a method for testing the HF content in electrolyte. The kit comprises a screw bottle body, a threaded bottle cap, a rubber plug and a gasket, wherein the threaded bottle cap is provided with a hole; the kit adopts the double combination of the silica gel sealing ring and the rubber plug, has good sealing performance and less reagent amount, can realize field test, and avoids the environmental influence in the sampling process; retarding LiPF elimination using anhydrous ethanol-containing solvent 6 The reaction rate replaces the use of ice water and low-temperature transportation and storage, and the economic benefit is good; the electrolyte and the aqueous solvent are mutually soluble and not layered through formula adjustment, so that the reaction is ensured to be carried out completely; the indicator has narrow color change range, obvious end point color mutation, accurate and effective test result and better consistency; the test process is simple to operate, has low requirements on personnel and has strong applicability.
Description
Technical Field
The invention belongs to the field of batteries, and particularly relates to a kit and a method for testing the content of HF in electrolyte.
Background
The lithium ion electrolyte is a carrier for lithium ion transmission in the battery and generally consists of 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 key guarantee for the lithium battery to obtain the advantages of high voltage, high specific energy and the like.
The trace amount of HF in the electrolyte for lithium ion batteries has great influence on the capacity, cycle life and safety of the batteries. Therefore, the HF content must be strictly monitored during the production, storage, transportation, and battery manufacturing of lithium ion battery electrolytes.
LiPF 6 Is the most important component of the electrolyte, and is easily dissolved in organic solvents such as water, low-concentration methanol, ethanol, acetone, carbonates and the like. Exposed to air or heated and rapidly decomposed by water vapor to produce PF 5 Simultaneous LiPF 6 And H 2 O is very reactive to produce HF.
H 2 O+LiPF 6 ＝POF 3 ↑+LiF↓+2HF
PF 5 +H 2 O＝2HF+POF 3 ↑
H 2 O+POF 3 ↑＝PO 2 F+2HF
In view of the above, the electrolyte in the industry is used in a dry room (relative humidity RH% is less than or equal to 2%). When the HF content of the lithium ion electrolyte is measured, sampling is carried out in a low-temperature and low-humidity environment, then the lithium ion electrolyte is stored at a low temperature and sent to a low-temperature room for testing, and an ice water system (ice water mixture is 0 ℃) is used for slowing down LiPF at the low temperature during testing 6 The rate of reaction.
The ice water system test method has the following problems: the sampling and sample feeding processes have high requirements on the sample storage environment, and the sample is very easy to be polluted; ice acquisition is not easy; the requirement on a tester is high; the organic electrolyte and ice water are mixed to have a layering phenomenon, the reaction is not thorough, the titration end point is difficult to judge, and the deviation is caused to the HF content test result.
Disclosure of Invention
The invention aims to provide a kit for testing the content of HF in electrolyte, which comprises an electrolyte diluting solvent, an indicator and a reaction reagent, is used for on-site detection, has good sealing performance, and has good mutual dissolving effect of the electrolyte and the solvent in the titration process, and no layering phenomenon. The titration end point color is distinguished, so that the judgment is easy, and the HF content test result is more accurate and effective.
The method for testing the HF content in the electrolyte provided by the invention adopts the kit for detection, and the accuracy is high.
The specific technical scheme of the invention is as follows:
a kit for testing the content of HF in electrolyte comprises a screw bottle body, a threaded bottle cap, a rubber plug and a gasket.
The screw bottle body is made of an acid and alkali corrosion resistant transparent material, preferably a PE transparent material or a PP transparent material.
The threaded bottle cap is made of PE transparent materials or PP transparent materials.
The rubber plug is made of silica gel material;
the gasket is made of a silica gel material.
The rubber plug is used for sealing the bottle mouth of the screw bottle body;
set up the trompil on the screw thread bottle lid, when screw thread bottle lid was screwed up with the cooperation of screw bottle, the trompil position of screw thread bottle lid can expose the plug, and the syringe passes the plug through the trompil position and adds electrolyte to the bottle inside of kit, and in adding electrolyte reaction process, can guarantee detecting system's leakproofness. And the threaded bottle cap and the screw bottle body are screwed up through thread adaptation, so that certain pressure can be applied to the rubber plug, and the sealing effect is ensured.
When the screw bottle body and the screw bottle cap are screwed up through screw thread adaptation, a rubber plug and a gasket are arranged between the screw bottle cap and the screw bottle body, the gasket is arranged above a bottle opening of the screw bottle body, the rubber plug is arranged above the gasket, and the sealing performance of the kit is ensured through double-layer sealing of the rubber plug and the gasket.
The reagent box comprises an electrolyte diluting solvent, an indicator and a reaction reagent.
And a mixed solution consisting of the electrolyte diluting solvent, the indicator and the reaction reagent is placed in the screw bottle body.
The electrolyte diluting solvent comprises pure water and an organic solvent;
the pure water accounts for 70-90% of the volume;
the organic solvent is absolute ethyl alcohol or ethyl acetate;
the volume of the absolute ethyl alcohol accounts for 10-30%.
Preferably, the electrolyte diluting solvent includes 80% by volume of pure water and 20% by volume of absolute ethanol.
The indicator is a methyl red-bromocresol green mixed indicator which is prepared by adopting the volume ratio of a methyl red solution with the concentration of 1g/L to a bromocresol green solution with the concentration of 2g/L according to 3:1;
the reaction reagent is NaOH solution or KOH solution, and the concentration is 0.01mol/L; by the principle of back titration of the alkali solution by the electrolyte, the electrolyte can be directly tested on site.
The diluting solvent containing ethanol in the kit provided by the invention not only can ensure that the mutual dissolving effect of the electrolyte and the solvent is good and the electrolyte and the solvent are not layered, but also plays a role in buffering in the whole system and slows down LiPF 6 The reaction rate can achieve the purpose of eliminating ice water.
The volume ratio of the electrolyte diluting solvent to the indicator to the reaction reagent is 20.1-0.2.
A method for testing the content of HF in electrolyte by using the kit comprises the following steps:
1) The kit containing the electrolyte dilution solvent, indicator and reaction reagent was weighed and recorded as m 0 ；
2) Absorbing electrolyte to be tested by using an injector, piercing a rubber plug of the kit by using the injector, adding the electrolyte into the solution of the kit, stopping injecting the electrolyte when the color of the solution in the kit is changed from green to light red in a sudden change manner, and marking the total weight of the kit as m 1 ；
3) And calculating the HF content in the electrolyte.
In the step 2), adding the electrolyte while shaking the kit to ensure full reaction.
The reagent kit itself contains an electrolyte diluting solvent, an indicator and a reaction reagent, and is green in color, and the weight is m 0 (ii) a Then adding electrolyte into the reagent box, and stopping changing the color from green to light red, wherein the end point is the titration end point, and the total weight is m 1 。m 1 -m 0 Is the weight of the electrolyte that participates in the reaction.
The formula for calculating the HF content in the electrolyte is as follows:
in the formula:
C 0 represents the concentration of the reaction reagent added into the kit, and the unit is mol/L;
v represents the volume of the reaction reagent added into the kit, and the unit is mL;
the molar mass of HF is 20.008g/mol;
m 0 represents the weight of the kit, in g,
m 1 represents the total weight of the kit after titration of the electrolyte in g.
The acid-base titration principle:
in the kit, pure water plays roles of diluting and dissolving in the whole system, and meanwhile, the acidity of the whole titration system is not changed; the ethanol plays a role in buffering, promotes mutual solubility between the electrolyte and the diluent, and ensures that the electrolyte and the pure water are not layered; reaction reagent NaOH solution or KOH solution provides OH - With H in HF - The reaction is carried out. The methyl red-bromocresol green indicator has narrow color change range and pH>Blue-green at 5.2; pH value<And light red at 4.6.
In the kit, the mixed solution of the newly-configured electrolyte diluting solvent, the indicator and the reaction reagent is directly sealed in the kit, and the kit is brought to the site, so that the electrolyte can be directly tested on the site (the relative humidity RH percent is less than or equal to 2%) after being sampled, ice water cooling is not needed, and the sample sending process is cancelled, thereby avoiding environmental influence; the mutual dissolving effect of the electrolyte and the solvent is better in the titration process, and the layering phenomenon cannot occur. The titration end point color is distinguished, the judgment is easy, and the HF content test result is more accurate and effective. Moreover, the kit disclosed by the invention not only adopts the gasket, but also can better seal the screw bottle body and the threaded bottle cap; the bottle mouth is sealed by the rubber plug, the mixed solution in the screw bottle body is isolated from the outside, the adopted threaded bottle cap is provided with the opening, the exposed rubber plug can be directly punctured with an injection agent when being detected to add the electrolyte to be detected, the threaded bottle cap is not required to be unscrewed to add the electrolyte, the influence of environmental factors on reaction in the detection reaction process is ensured, and the detection accuracy is kept.
Compared with the prior art, the kit disclosed by the invention adopts the double combination of the silica gel sealing ring and the rubber plug, so that the sealing property is good, the reagent amount is small, the field test can be realized, and the environmental influence in the sampling process is avoided; retarding the elimination of LiPF using anhydrous alcohol-containing solvent 6 The reaction rate replaces the use of ice water and low-temperature transportation and storage, and the economic benefit is good; the electrolyte and the aqueous solvent are mutually soluble and not layered through formula adjustment, so that the reaction is ensured to be carried out completely; the indicator has narrow color change range, obvious end point color mutation, accurate and effective test result and better consistency; the test process is simple to operate, has low requirements on personnel and has strong applicability.
Drawings
FIG. 1 shows the delamination of the test results of comparative example 1;
FIG. 2 shows the titration process of the experimental results of comparative example 2, the color does not conform to the indicator color change range;
FIG. 3 is a schematic structural diagram of the kit of the present invention;
FIG. 4 is a schematic structural view of a threaded bottle cap of the kit of the present invention;
in the figure, 1 is a screw bottle body, 2 is a gasket, 3 is a rubber plug, 4 is a threaded bottle cap, and 5 is an opening.
Detailed Description
Comparative example 1 (NaOH titration electrolyte-diluting solvent ratio 100% ice water)
A method of testing the HF content of an electrolyte comprising the steps of:
1) Preparing a diluting solvent: putting ice blocks and pure water with the same volume into a beaker, and waiting for 20min to ensure that the water temperature is about 0 ℃;
2) Sample weighing: taking a conical flask, adding 20mL of ice water into the conical flask, and adding 0.1mL of methylPlacing the red-bromocresol green indicator on a balance for peeling and zeroing, adding the electrolyte, recording the weight m of the electrolyte when the solution is red 0 ；
3) NaOH titration: filling the burette with a volume V 1 0.01moL/L NaOH solution, dropping into a conical flask filled with electrolyte, stopping when the solution turns from red to dark green, and recording the volume V of the burette at the moment 2 ；
4) And (4) observation: observing the titration phenomenon to indicate the color change of the indicator;
by using a testing method of an ice water method, the solution after titration has slow color reversion and does not fade within 30 s; however, the electrolyte and ice water are layered in the whole titration process, and the color of the titration end point is difficult to judge.
Comparative example 2 (NaOH titration electrolyte-diluting solvent ratio of 100% ethanol)
A method of testing the HF content of an electrolyte comprising the steps of:
1) Preparing a diluting solvent: preparing absolute ethyl alcohol;
2) Sample weighing: adding 20mL of ethanol into a conical flask, adding 0.1mL of methyl red-bromocresol green indicator, placing on a balance, peeling, returning to zero, adding electrolyte, and recording the weight m of the electrolyte 0 ；
3) NaOH titration: filling the burette with a volume V 1 0.01moL/L NaOH solution, dropping into a conical flask filled with electrolyte, stopping when the solution turns from red to dark green, and recording the volume V of the burette at the moment 2 ；
4) And (4) observation: observing the titration phenomenon and the indicator color change;
when the proportion of the diluting solvent is 100% ethanol, the phenomenon of layering between the electrolyte and the diluting solvent is not generated in the processes of adding the electrolyte and titrating, but the color of the added electrolyte is not red but orange, which is not in accordance with the color change of the indicator, and the terminal point mutation is not obvious, so that the technical index is not realized.
Example 1
A kit for testing the content of HF in electrolyte comprises a screw bottle body 1, a threaded bottle cap 4, a rubber plug 3 and a gasket 2. The structure schematic diagram is shown in fig. 3.
The screw bottle body 1 is made of PE transparent material.
The threaded bottle cap 4 is made of PE transparent material.
The rubber plug 3 is made of silica gel material;
the gasket 2 is made of silica gel.
The rubber plug 2 is used for sealing the bottle mouth of the screw bottle body 1;
set up trompil 5 on the screw thread bottle lid 4, when screw thread bottle lid 4 was screwed up with 1 cooperation of screw bottle, the trompil position of screw thread bottle lid 4 can expose plug 3, and the syringe passes the plug through the trompil position and adds electrolyte to the bottle inside of kit, and in adding electrolyte reaction process, can guarantee detecting system's leakproofness. The threaded bottle cap 4 and the threaded bottle body 1 are screwed up through thread adaptation, so that certain pressure can be applied to the rubber plug 3, and the sealing effect is ensured.
When the screw bottle body 1 and the screw bottle cap 4 are screwed up through screw thread adaptation, a rubber plug 3 and a gasket 2 are arranged between the screw bottle cap 4 and the screw bottle body 1, the gasket 2 is arranged above the bottle mouth of the screw bottle body 1, the rubber plug 3 is arranged above the gasket 2, and the sealing performance of the kit is ensured through double-layer sealing of the rubber plug 3 and the gasket 2.
Preparing an electrolyte diluting solvent by adopting pure water with the volume ratio of 80% and ethanol with the volume ratio of 20%, filling 10mL of the freshly prepared electrolyte diluting solvent, 0.1mL of a mixed solution of a methyl red-bromocresol green indicator with the volume ratio of a methyl red solution with the concentration of 1g/L and a bromocresol green solution with the concentration of 2g/L, which is prepared according to 3:1 and a NaOH solution with the concentration of 0.5mL0.01mol/L into a screw bottle body 1, quickly placing a gasket 2 above the bottle opening of the screw bottle body 1, sealing the bottle opening of the screw bottle body by using a rubber plug 3, and finally screwing a screw bottle cap 4 with an opening 5 to obtain the reagent kit which is accurately weighed, wherein the mass is m at the moment 0 。
The method for testing the HF content in the electrolyte by using the kit comprises the following steps of (electrolyte titration NaOH solution-kit method for testing the HF content in the electrolyte)
And (3) electrolyte titration: in the dry stateIn the dry room, relative humidity RH% is less than or equal to 2%, after the to-be-measured electrolyte is absorbed by an injector, the injector penetrates through the position of a hole 5 on a threaded bottle cap 4, the injector needle pierces a rubber plug to inject the to-be-measured electrolyte into a reagent kit, the electrolyte is injected into the reagent kit while shaking, the injection is stopped when the color in the reagent kit is changed from green to light red in a sudden change manner, the total weight m of the reagent kit and the electrolyte participating in the titration reaction is accurately weighed 1 ；
The HF content in the electrolyte was calculated by the following formula:
wherein 0.5 represents the volume of NaOH solution added into the kit in unit mL;0.01 represents the concentration of NaOH solution added into the kit, and the unit is mol/L; the molar mass of HF is 20.008g/mol, m 0 Represents the weight of the kit, unit g, m 1 Represents the total weight of the kit and the electrolyte participating in the reaction, in g.
The reagent kit is used for testing the electrolyte to perform back titration, repeatability and reproducibility verification, and the result is as follows;
pure water with the volume ratio of 80% and 20% ethanol are used as diluting solvents, the solution after titration has slow color reversion, and the color is not deepened within 30 s; and the indicator is in color change at a preset pH value, and meanwhile, the electrolyte and the diluent are not layered, so that the technical index of testing HF by the electrolyte can be realized.
And (3) carrying out back titration verification: the relative deviation between the data of the content of HF in the electrolyte measured by using the kit and the result of the titration of the electrolyte by using the NaOH solution is less than 2 percent, the test method has high feasibility and ensures the effectiveness. The results are shown in Table 1.
Table 1 example 1 back titration experiment
And (3) repeatability verification: the sample 1 is tested 6 times by using the kit under the same condition, the relative standard deviation of the test result is 1.82%, the test result is less than 5%, the test method is high in feasibility, and the effectiveness is guaranteed. The results are shown in Table 2.
Table 2 example 1 repeatability verification
And (3) verifying the reproducibility: different personnel use the kit to test the sample 1 for 6 times, the relative standard deviation of the test result is 1.88 percent, the test result is less than 5 percent, the test method has high feasibility and the effectiveness is ensured.
Claims (9)
1. A kit for testing the content of HF in electrolyte is characterized by comprising a screw bottle body, a threaded bottle cap, a rubber plug and a gasket;
the screw bottle body is made of an acid-base corrosion resistant transparent material;
the reagent box comprises an electrolyte diluting solvent, an indicator and a reaction reagent; the electrolyte diluting solvent comprises pure water and an organic solvent;
the pure water accounts for 70-90% of the volume.
2. The kit according to claim 1, wherein the organic solvent is absolute ethanol or ethyl acetate.
3. The kit of claim 1, wherein the indicator is a methyl red-bromocresol green mixed indicator.
4. The kit of claim 1, wherein the reaction reagent is NaOH solution or KOH solution.
5. The kit of claim 1, wherein the screw bottle is a PE transparent material or a PP transparent material.
6. The kit according to claim 1, wherein the rubber plug is a silica gel material; the gasket is made of a silica gel material.
7. The kit of claim 1, wherein the threaded cap is provided with an opening.
8. A method for testing the HF content of an electrolyte, characterized in that the detection is carried out using a kit according to any one of claims 1 to 7.
9. The method according to claim 8, characterized in that the method is in particular:
1) The kit containing the electrolyte dilution solvent, indicator and reaction reagent was weighed and recorded as m 0 ；
2) Absorbing electrolyte to be tested by using an injector, piercing a rubber plug of the kit by using the injector, adding the electrolyte into the solution of the kit, stopping injecting the electrolyte when the color of the solution in the kit is changed from green to light red in a sudden change manner, and marking the total weight of the kit as m 1 ；
3) And calculating the HF content in the electrolyte.
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