CN112630334B - Organic phase ratio detection method of electrolyte containing TMSP - Google Patents
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Abstract
The invention discloses a method for detecting an organic phase ratio of electrolyte containing TMSP, which comprises the steps of utilizing TMSP to react with water very easily to generate silanol with a small molecular weight, and then using a gas phase method to detect and determine the content easily, so that lithium salt in the electrolyte is dissolved in water by adding water into the electrolyte, adding dichloromethane serving as a strong dissolving solvent according to a certain proportion to serve as an extracting agent, fully mixing, carrying out centrifugal separation on a high-speed centrifuge, removing a water layer, obtaining a sample after pretreatment of the electrolyte, and carrying out detection through a gas phase chromatography. The detection method can effectively avoid interference, ensure stability, effectively improve detection effect and ensure real and effective detection; and various organic components in the electrolyte can be accurately detected at the same time.
Description
Technical Field
The invention belongs to the technical field of lithium battery electrolyte, and particularly relates to a method for detecting an organic phase ratio of electrolyte containing TMSP.
Background
Lithium ion batteries are gradually replacing lead acid batteries as the mainstream of new energy batteries due to the advantages of high energy density, long service life, safety and cleanness. The important components of the lithium ion battery, called as the electrolyte of the "blood" of the lithium ion battery, affect the high and low temperature, rate charge and discharge, cycle performance and service life of the lithium ion battery. The electrolyte consists of a solvent, lithium salt and an additive; the solvent is generally chain carbonates or carboxylic acid esters, the lithium salt is lithium hexafluorophosphate, and the additive has different types according to different requirements.
The detection of the components of the electrolyte has important significance for controlling the quality of the electrolyte, and the proportion control of the component content plays an extremely important role in verifying the functionality and the safety of the electrolyte; the existing detection method is a gas chromatography direct sample injection method for detection, technically, the method is relatively stable in the industry, although the melting point of a solvent is generally low, the detection is convenient for a gas phase method, the additive has larger difference due to different battery requirements, and the requirement of the test cannot be met by the single direct sample injection gas phase method.
Although the electrolyte direct injection method gas phase detection is mature, lithium salt and various additives in the electrolyte are directly injected to cause great damage to a chromatographic column of the gas chromatography, meanwhile, the phenomena of miscellaneous peaks, ghost peaks and unstable baseline are easy to appear on a detection result map, and for the detection of low-content organic phase additives, the detection is easily influenced by interference peaks, so that the content of the additives cannot be accurately quantified. TMSP, chinese name: tris (trimethylsilane) phosphate. TMSP has become more and more widely used in lithium battery electrolyte formulations in recent years as a novel additive. Some specially applied electrolytes contain TMSP, which has large molecular weight, wide temperature range of gas phase temperature rise program and long test time; meanwhile, TMSP is extremely unstable and is easily decomposed into other various byproducts, so that the quantitative analysis of TMSP has a great problem.
The existing literature carries out related research and report on a detection method of an additive TMSP in lithium ion battery electrolyte, for example, in patent literature CN109142612A, a determination method of TMSP in lithium battery electrolyte is reported, wherein sulfuric acid is adopted to prepare a regeneration liquid, then an eluent is adopted to prepare an eluent, a TMSP sample is treated by the regeneration liquid and the eluent to carry out detection, finally a standard sample and a test sample are detected, and the accurate content of TMSP in the sample is calculated through a formula. In the detection method, a regeneration solution and a leacheate need to be prepared, a standard solution needs to be prepared, the concentration range of TMSP in the standard solution is small and can only be between 50ppm and 75ppm, and the sample solution needs to be strictly controlled within 20min from sampling to diluting. Further, as disclosed in patent document CN 110389182 a, a method for quantitatively detecting TMSP in an electrolyte of a lithium ion battery, in which TMSP is reacted with lithium hexafluorophosphate to produce a TMSF intermediate, and then the amount of TMSP added is determined by measuring the absorption peak area of TMSF, requires the use of a fluorine-containing lithium salt, and cannot detect other organic components in the electrolyte, is disclosed.
Therefore, it is desired to provide a method for detecting TMSP, which is simple and efficient, and can simultaneously and accurately detect an organic phase in an electrolyte containing TMSP.
Disclosure of Invention
In order to solve the problems, the invention provides a method for detecting an organic phase ratio of TMSP-containing electrolyte, which can effectively avoid interference, ensure stability, effectively improve detection effect and ensure real and effective detection.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for detecting an organic phase ratio of TMSP-containing electrolyte comprises the following steps:
s10, absorbing the electrolyte sample and injecting the electrolyte sample into a centrifuge tube;
s20, adding deionized water into the centrifuge tube, wherein the volume ratio of the deionized water to the electrolyte is 1: 3-2: 1, shaking and shaking uniformly to enable the additive TMSP in the electrolyte to fully react with water to generate silanol, and simultaneously fully dissolving inorganic lithium salt in the electrolyte in the water;
s30, adding an analytically pure dichloromethane solvent into the centrifuge tube, wherein the volume ratio of the dichloromethane solvent to the electrolyte is 3: 1-5: shaking and shaking uniformly to enable an organic phase in the electrolyte to be extracted into dichloromethane gradually to obtain a mixed sample;
s40, placing the centrifuge tube filled with the mixed sample on a centrifuge for centrifugation, and fully separating the water phase and the organic phase;
s50, extracting the supernatant of the centrifuge tube, and removing the upper aqueous phase to obtain a detection sample;
s60, sucking the lower organic phase liquid in the detection sample into a gas chromatography sample feeding bottle, and performing gas chromatography on the lower organic phase liquid in a sample feeding amount of 1 mu l and a split ratio of 50: 1. under the condition that the chromatographic column is DB-1701, the organic phase component proportion of the electrolyte is obtained by detecting the peak area of data processing through an area normalization method.
The detection method provided by the invention not only can detect TMSP in the electrolyte, but also can detect organic components in the conventional electrolyte. For example, for other organic solvent components in the electrolyte: solvents DMC (dimethyl carbonate), EMC (ethyl methyl carbonate), DEC (diethyl carbonate), EC (ethylene carbonate), PC (propylene carbonate), etc., and other conventional additive components: VC (vinylene carbonate), FEC (fluoroethylene carbonate), PS (1, 3-propane sultone) and the like have good detection results, and the proportions of various organic phase components in the electrolyte can be detected and obtained simultaneously.
The detection principle adopted by the detection method is as follows: when the gas chromatography is adopted to detect each organic component in the lithium ion battery electrolyte, a peak shape at a specific position is generated on a chromatogram map under the same detection method, the content of each substance is in a direct proportion relation with the peak area, each substance has a response value in an instrument, the sample proportion is converted according to the response value proportion value, the response value is the peak area/the sample mass, and the response value is a fixed value after the detection method is determined and is related to the detection precision of the instrument.
The method can easily obtain the proportion of each organic phase component, and because the additive TMSP in the electrolyte generates silanol, the inorganic lithium salt is fully dissolved in water, and then each organic phase is extracted into dichloromethane through the extracting agent for detection, the detection method can not cause damage to a chromatographic column of the gas chromatography, and meanwhile, the phenomena of miscellaneous peaks, ghost peaks and unstable base lines do not appear on a detection result map, and the detection result has high accuracy.
In the detection method, the extraction of the organic phase is necessary by adopting the extraction agent dichloromethane, and compared with the detection method without the extraction of the organic phase, the detection result of the organic phase has higher accuracy.
Preferably, the volume ratio of the deionized water to the electrolyte in step S20 is 1: 1.
preferably, the volume ratio of the dichloromethane solvent to the electrolyte in step S30 is 3: 1.
further, the organic phase comprises other organic solvents and/or additives besides TMSP, the organic solvents comprise any combination of dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethylene carbonate and propylene carbonate, and the additives comprise any combination of vinylene carbonate, fluoroethylene carbonate and 1, 3-propane sultone.
Furthermore, 1-2ml of electrolyte sample is sucked up through a 3ml plastic pipette and injected into a 10ml plastic centrifuge tube with a cover.
Further, deionized water with the same volume is added into the plastic centrifugal tube, a cover is covered, shaking and shaking are carried out for 1-3min, so that the additive TMSP in the electrolyte fully reacts with water to generate silanol, and most inorganic lithium salt in the electrolyte can be dissolved in water.
Furthermore, analytically pure dichloromethane solvent with three times volume of electrolyte solution is added into the centrifuge tube, and the centrifuge tube is covered with a cover and shaken for 1-3min, so that the organic phase in the electrolyte solution is gradually extracted into dichloromethane.
Further, placing the centrifuge tube containing the mixed sample on a centrifuge machine for centrifuging for 5-10min, and fully separating the water phase and the organic phase.
Further, extracting supernatant liquid of the centrifuge tube by using an injector, and removing an upper aqueous phase; and sucking about 2ml of lower organic phase liquid into a gas chromatography sampling bottle by using a 3ml plastic suction pipe, and performing gas detection by using gas chromatography.
The beneficial effects of the technical scheme are as follows:
according to the invention, TMSP is very easy to react with water to generate silanol with a small molecular weight, the content is easy to detect and determine through a gas phase method, lithium salt in electrolyte is dissolved in water by adding water into the electrolyte, strong dissolving solvent dichloromethane is added according to a certain proportion to serve as an extracting agent, each organic phase component in the electrolyte is extracted, a water layer is removed through centrifugal separation on a high-speed centrifuge, a sample after pretreatment of the electrolyte is obtained, and detection is carried out through the gas phase chromatography, so that interference can be effectively avoided, the stability is ensured, the detection effect is effectively improved, and the truth and the effectiveness of detection are ensured. The detection method provided by the invention can be used for simultaneously and accurately detecting various organic components in the electrolyte.
According to the invention, the lithium salt in the electrolyte is dissolved by water, and then dichloromethane is used for extraction, so that the electrolyte solvent and the additive extracted into dichloromethane are relatively clean, the sample detection result has few peaks, the chromatographic column loss is low, and the reproducibility of the component test result is strong.
In the present invention, when TMSP reacts with water to form silanol having a small molecular weight, TMSP can be detected more easily in a gas phase, and TMSP is prevented from decomposing into various byproducts, which makes it difficult to quantify TMSP.
According to the invention, the temperature range of the temperature-rising program of the gas chromatograph of the test sample is smaller by processing the obtained test sample, so that the test period is shortened, and the loss of the chromatographic column, the influence on the test result and the service life of the chromatographic column caused by overhigh temperature-rising program setting are reduced;
the method provided by the invention has a diluting effect on the conventional and simple electrolyte component detection that the additive does not react with water, so that the peak shape of the detection result is more stable, and the method is superior to a direct sample introduction mode, and the service life of gas chromatography equipment is longer.
Drawings
FIG. 1 is a schematic flow chart of the method for detecting the organic phase ratio of the TMSP-containing electrolyte according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described with reference to the accompanying drawings.
Example 1
In this embodiment, referring to fig. 1, the present invention provides a method for detecting an organic phase ratio of an electrolyte containing TMSP, comprising the steps of:
s10, absorbing the electrolyte sample and injecting the electrolyte sample into a centrifuge tube;
s20, adding deionized water with the same volume of electrolyte into the centrifugal tube, shaking and shaking uniformly to enable the additive TMSP in the electrolyte to fully react with water to generate silanol, and simultaneously fully dissolving inorganic lithium salt in the electrolyte into water;
s30, adding an analytically pure dichloromethane solvent with the volume being three times that of the electrolyte into the centrifugal tube, shaking and shaking uniformly to enable the organic phase in the electrolyte to be extracted into dichloromethane gradually, and obtaining a mixed sample;
s40, placing the centrifuge tube filled with the mixed sample on a centrifuge for centrifugation, and fully separating the water phase and the organic phase;
s50, extracting the supernatant of the centrifugal tube, and removing the upper aqueous phase to obtain a detection sample;
s60, sucking the lower organic phase liquid in the detection sample into a gas chromatography sample feeding bottle, and performing gas chromatography on the lower organic phase liquid in a sample feeding amount of 1 mu l and a split ratio of 50: 1. under the condition that the chromatographic column is DB-1701, the organic phase component proportion of the electrolyte is obtained by detecting the peak area of data processing through an area normalization method.
Example 2
As another embodiment of the above example 1, a method for detecting an organic phase ratio of an electrolyte solution containing TMSP, comprising the steps of:
s10, sucking 1-2ml of electrolyte sample through a 3ml plastic suction pipe, and injecting the electrolyte sample into a 10ml plastic centrifuge tube with a cover;
s20, adding deionized water which accounts for 1/3 of the volume ratio of the electrolyte into the plastic centrifuge tube, covering a cover, shaking and shaking uniformly for 1-3min to ensure that an additive TMSP in the electrolyte fully reacts with water to generate silanol and inorganic lithium salt in the electrolyte is fully dissolved in the water;
s30, adding analytically pure dichloromethane solvent with five times of volume of electrolyte into the centrifugal tube, covering a cover, and vibrating for 1-3min to gradually extract the organic phase in the electrolyte into dichloromethane to obtain a mixed sample;
s40, placing the centrifuge tube filled with the mixed sample on a centrifuge for centrifuging for 5-10min, and fully separating the water phase and the organic phase;
s50, extracting supernatant of the centrifuge tube by using a syringe, and removing an upper aqueous phase;
s60, sucking about 2ml of lower organic phase liquid into a gas chromatography sampling bottle by using a 3ml plastic pipette, and performing gas chromatography on the organic phase liquid in a sampling amount of 1 mu l and a split ratio of 50: 1. under the condition that the chromatographic column is DB-1701, the organic phase component proportion of the electrolyte is obtained by detecting through a data processing peak area normalization method.
Examples of the experiments
The selected electrolyte sample is subjected to component detection as follows: organic solvent system DMC/EMC/EC ═ 1: 1:1 (V: V: V), the content of the additive TMSP is divided into four groups according to the weight percentage: four groups of TMSP samples with different ratios were tested in parallel three times with 0%/0.5%/1%/1.5%, 1% of each additive VC and FEC, and 1mol/l of lithium salt. The above-mentioned symbols represent: DMC (dimethyl carbonate), EMC (ethyl methyl carbonate), EC (ethylene carbonate), VC (vinylene carbonate), FEC (fluoroethylene carbonate), TMSP (tris (trimethylsilane) phosphate).
The GC detection method is as follows: adopting an Agilent 7890B gas chromatograph, and carrying out chromatographic column separation: DB-1701, Detector: FID hydrogen flame ion detector. Sample introduction amount: 1 microliter, split ratio: 50:1, temperature rising program: 40 ℃ -90 ℃ -160 ℃, speed: 10-20 ℃/min, each standing time is 2 min.
The composition ratios of the four sets of electrolyte samples disposed are, for example, table 1:
TABLE 1 preparation of electrolyte sample component ratios
The instrumental response values of the components of the organic phases in the electrolyte are shown in table 2:
TABLE 2 Instrument response values for the ingredients
The results of the organic phase component detection of the four groups of samples by the detection method of the present invention in example 1 are shown in tables 3 to 6.
TABLE 30% TMSP electrolyte sample test results
TABLE 40.5% TMSP electrolyte sample test results
TABLE 51% TMSP electrolyte sample test results
TABLE 61.5% TMSP electrolyte sample assay results
As can be seen from tables 3-6, the detection method provided by the invention can be used for simultaneously detecting various organic phase components in the electrolyte, and has the advantages of high detection result accuracy, small organic phase detection proportion deviation in each group of parallel samples, and small detection proportion error between the parallel samples and real samples, wherein the detection proportion error is lower than 0.1%.
Comparative example 1
The method of example 1 is used to detect the samples in the experimental examples, except that in the comparative example scheme, the organic phase is not extracted by using an extracting agent, but the detection is directly performed by an external standard method for preparing a standard curve by preparing a standard solution, and the calculation method refers to patent document CN109142612a, and the result shows that: the detection proportion deviation of the organic phase in each group of parallel samples is more than 0.5 percent, and the detection proportion error between the organic phase and the real sample is more than 1 percent.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The method for detecting the organic phase ratio of the electrolyte containing TMSP is characterized by comprising the following steps of:
s10, sucking an electrolyte sample, and injecting the electrolyte sample into a centrifuge tube;
s20, adding deionized water into the centrifugal tube, wherein the volume ratio of the deionized water to the electrolyte is 1:1, shaking and shaking uniformly to enable the additive TMSP in the electrolyte to fully react with water to generate silanol, and meanwhile, fully dissolving inorganic lithium salt in the electrolyte into water;
s30, adding an analytically pure dichloromethane solvent into the centrifugal tube, wherein the volume ratio of the dichloromethane solvent to the electrolyte is 3: 1-5: 1, shaking and shaking uniformly, so that an organic phase in the electrolyte is gradually extracted into dichloromethane to obtain a mixed sample;
s40, placing the centrifuge tube filled with the mixed sample on a centrifuge for centrifugation, and fully separating the water phase and the organic phase;
s50, extracting the supernatant of the centrifugal tube, and removing the upper aqueous phase to obtain a detection sample;
s60, sucking the lower organic phase liquid in the detection sample into a gas chromatography sample feeding bottle, and detecting by using a gas chromatography through a data processing peak area normalization method, wherein the gas chromatography detection conditions are as follows: a chromatographic column: DB-1701, Detector: FID hydrogen flame ion detector, sample introduction amount: 1 mul, the split ratio is 50:1, the temperature rising program: 40 ℃ -90 ℃ -160 ℃, speed: 10-20 ℃/min, each standing time is 2 min; obtaining the organic phase component proportion of the electrolyte;
the organic phase comprises TMSP and other organic solvents and/or additives except TMSP, the organic solvents comprise any combination of dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate, and the additives comprise any combination of vinylene carbonate and fluoroethylene carbonate; the TMSP is tris (trimethylsilane) phosphate.
2. The method for detecting the organic phase ratio of the TMSP-containing electrolyte solution as claimed in claim 1, wherein the volume ratio of the dichloromethane solvent to the electrolyte solution in step S30 is 3: 1.
3. The method for detecting the organic phase ratio of the electrolyte containing TMSP as claimed in claim 1, wherein an equal volume of deionized water is added into the plastic centrifuge tube, the plastic centrifuge tube is covered with a cover, and the plastic centrifuge tube is shaken and shaken uniformly for 1-3min to ensure that the additive TMSP in the electrolyte fully reacts with water to generate silanol and simultaneously the inorganic lithium salt in the electrolyte is fully dissolved in water.
4. The method for detecting the organic phase ratio of the electrolyte containing TMSP as claimed in claim 3, wherein the analytical pure dichloromethane solvent is added into the centrifuge tube in three times volume of the electrolyte, and the cover is closed and shaken for 1-3min to gradually extract the organic phase in the electrolyte into dichloromethane.
5. The method for detecting the organic phase ratio of the electrolyte containing TMSP as claimed in claim 4, wherein the centrifuge tube containing the mixed sample is placed on a centrifuge for 5-10min to separate the aqueous phase and the organic phase sufficiently.
6. The method for detecting the organic phase ratio of the electrolyte containing TMSP as claimed in claim 5, wherein a syringe is used to extract the supernatant of the centrifuge tube and remove the supernatant of the aqueous phase; using a 3ml plastic pipette, 2ml of the lower organic phase liquid was aspirated into a gas chromatography sample bottle, and gas detection was performed using gas chromatography.
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