CN113917021A - Method for testing phthalate substances in anode material or coating of lithium ion battery - Google Patents

Method for testing phthalate substances in anode material or coating of lithium ion battery Download PDF

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CN113917021A
CN113917021A CN202111171179.3A CN202111171179A CN113917021A CN 113917021 A CN113917021 A CN 113917021A CN 202111171179 A CN202111171179 A CN 202111171179A CN 113917021 A CN113917021 A CN 113917021A
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lithium ion
ion battery
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丁慢慢
程丹
胡淑婉
张峥
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Gotion High Tech Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/14—Preparation by elimination of some components
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a method for testing phthalate substances in a lithium ion battery anode material or coating, which relates to the technical field of detection of phthalate substances in lithium ion battery materials, and comprises the following steps: (1) freezing and grinding the lithium ion battery anode material or the coating into powder; (2) adding a mixed solution of n-hexane and ethyl acetate into the powdery sample, and then sealing; (3) and carrying out ultrasonic treatment on the sealed sample, filtering, and carrying out GC-MS analysis on the filtrate. The invention has the beneficial effects that: the invention solves the problem of detecting phthalate substances in the lithium ion battery anode material, and skillfully solves the problem of inaccuracy caused by the conventional method by adding ethyl acetate into an extraction reagent.

Description

Method for testing phthalate substances in anode material or coating of lithium ion battery
Technical Field
The invention relates to the technical field of detection of phthalate substances in lithium ion battery materials, in particular to a method for testing phthalate substances in a lithium ion battery anode material or coating.
Background
Phthalate (PAEs) is widely used in materials such as toys, food packaging, medical supplies and the like because of its softening effect, excellent comprehensive properties, good low-temperature flexibility, good heat resistance and the like. Moreover, the phthalate ester is added into personal care products, so that the nail polish has better film forming property, aromatic perfume and fragrance and better detergent permeability. However, once they enter the body, phthalates can damage the heart, liver and kidneys, affecting the immune system, causing goiter, hypomnesis and joint stiffness. Can interfere the endocrine of men, increase the probability of suffering from breast cancer of women and harm the reproductive system of male and infant born in the future. Therefore, environmental and health problems caused by such compounds are receiving wide attention. Therefore, there are various methods for detecting phthalate esters in foods and environment in the prior art, such as the method disclosed in patent publication No. CN103267816A for measuring phthalate esters by liquid phase.
The european association and the european association council at 27/1/2003 pass the directive on the restriction of the use of certain hazardous substances in electrical and electronic devices (referred to as RoHS), which is renewed at 7/1/2011, and adds four substances and their maximum restriction concentrations to the original six restrictions: 2-ethylhexyl phthalate (DEHP, 1000ppm), butyl benzyl phthalate (BBP, 1000ppm), di-n-butyl phthalate (DBP, 1000ppm), diisobutyl phthalate (DIBP, 1000 ppm). Therefore, detection of harmful substances in the battery is indispensable. The battery material RoHS related detection is based on IEC 62321-1-8 related method standards, however, the detection of phthalate substances in the positive electrode material cannot be performed according to the IEC 62321-8 method, specifically, the recovery rate is low (45.44% -73.70%), it is preliminarily inferred that the positive electrode material is alkaline, the target analytes are all phthalates, the alkalinity possibly affects the target substances in the pretreatment process, so that the target substances are decomposed or subjected to other reactions, the target substances are consumed, and the analysis result is inaccurate. Therefore, the invention is particularly important for the method for testing the phthalate ester substances in the lithium ion battery anode material.
Disclosure of Invention
The invention aims to provide a method for testing phthalate substances in a lithium ion battery anode material, which can be used for testing the phthalate substances in various anode materials (including an anode coating) of a lithium ion battery.
The invention solves the technical problems through the following technical means:
a method for testing phthalate type substances in a positive electrode material or coating of a lithium ion battery, comprising the steps of:
(1) freezing and grinding the lithium ion battery anode material or the coating into powder;
(2) adding a mixed solution of n-hexane and ethyl acetate into the powdery sample, and then sealing;
(3) and carrying out ultrasonic treatment on the sealed sample, filtering, and carrying out GC-MS analysis on the filtrate.
Has the advantages that: the invention solves the problem of detecting phthalate substances in the lithium ion battery anode material, skillfully solves the problem of inaccuracy caused by the conventional method by adding ethyl acetate into an extraction reagent and accelerating the speed of extracting a target substance in a sample by using an ultrasonic wave, the recovery rate of the target substance is only 45.44-73.70% before the ethyl acetate is not added, the final recovery rate of the improved method is 74.66-104.26%, and the standard range of IEC 62321-8 is 70-130%, so the detection result is reliable. The method adds the reagent ethyl acetate as a low-toxicity reagent, and reduces the health hazard brought by the reagent.
Preferably, the step (1) is implemented by adopting liquid nitrogen to grind the powder with the particle size of less than 250 μm.
Preferably, the phthalate type substance comprises DEHP, BBP, DBP, DIBP.
Preferably, the lithium ion battery positive electrode material or coating in the step (1) comprises a lithium iron phosphate material or a nickel-cobalt-manganese ternary material.
Preferably, in the step (2), the volume ratio of the n-hexane to the ethyl acetate is 1:1, and the ratio of the mass of the powdery sample to the mass of the mixed solution is 40-60mg:3 mL.
Has the advantages that: the volume ratio of n-hexane to ethyl acetate is too low or too high, which can reduce the extraction efficiency of the target substance, and if the addition amount of the mixed solution is too large, the analysis concentration is too low and is lower than the external standard analysis range, which affects the determination result.
Preferably, the step (2) further comprises a reagent blank configuration step: mixing n-hexane and ethyl acetate, and sealing.
Preferably, the step (2) further comprises a step of configuring a standard sample: after weighing the sample, adding a proper amount of standard sample mixed liquid to enable the sample mixed liquid to reach different addition amounts, and then adding n-hexane and ethyl acetate.
Preferably, an ultrasonic cleaning machine is adopted to perform ultrasonic treatment in the step (3), the power of the ultrasonic cleaning machine is 350W, and the power range is 75-85%.
Has the advantages that: too long ultrasonic time or too high power can cause volatilization of the target in the sample, and too short ultrasonic time or too low power can cause incomplete extraction of the target in the sample.
Preferably, the n-hexane and ethyl acetate are of chromatographically pure grade.
Preferably, the step (3) is carried out by filtering with a 0.22 μm or 0.45 μm filter head.
Preferably, the GC-MS analysis is quantified by an external standard method, mixed working solutions with five horizontal concentrations are prepared to obtain a working curve, the selected concentrations are 1 mu g/mL, 2 mu g/mL, 5 mu g/mL, 10 mu g/mL and 20 mu g/mL respectively, GC-MS analysis is carried out in a SIM mode, and linear fitting is carried out by taking the concentrations and peak areas obtained by quantitative analysis as values.
Preferably, the assessment of the GC-MS quantification method comprises reproducibility, detection limit, quantification limit.
The invention has the advantages that: the invention solves the problem of detecting phthalate substances in the lithium ion battery anode material, skillfully solves the problem of inaccuracy caused by the conventional method by adding ethyl acetate into an extraction reagent and accelerating the speed of extracting a target substance in a sample by using an ultrasonic wave, the recovery rate of the target substance is only 45.44-73.70% before the ethyl acetate is not added, the final recovery rate of the improved method is 74.66-104.26%, and the standard range of IEC 62321-8 is 70-130%, so the detection result is reliable. The method adds the reagent ethyl acetate as a low-toxicity reagent, and reduces the health hazard brought by the reagent.
The volume ratio of n-hexane to ethyl acetate is too low or too high, which can reduce the extraction efficiency of the target substance, and if the addition amount of the mixed solution is too large, the analysis concentration is too low and is lower than the external standard analysis range, which affects the determination result.
The purpose of the ultrasonic is to accelerate the speed of solvent extraction of the target in the sample, the target in the sample can be volatilized due to too long ultrasonic time or too high ultrasonic power, and the target in the sample can be incompletely extracted due to too short ultrasonic time or too low ultrasonic power.
Drawings
FIG. 1 is a graph of a fitted curve of four phthalate ester working curves in an example of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
In the following examples, the instrument used was a GC (traue 1300) -ms (isq qd) gas chromatography-mass spectrometer, the column type was in accordance with the specifications in IEC 62321-8 standard, the carrier gas was also in accordance with the ion source temperature, and the ion source temperature in the present invention was: at 300 ℃. The qualitative and quantitative ions of the four phthalate esters are shown in Table 1.
TABLE 1 quantitative reference mass numbers of four phthalates
Figure BDA0003293243390000051
GC-MS analysis adopts an external standard method for quantification, mixed working solutions with five horizontal concentrations are prepared to obtain a working curve, the selected concentrations are 1 mu g/mL, 2 mu g/mL, 5 mu g/mL, 10 mu g/mL and 20 mu g/mL respectively, GC-MS analysis is carried out in a SIM mode, linear fitting is carried out by taking the concentrations and peak areas obtained by quantitative analysis as values, and a fitting graph is obtained, and is shown in figure 1.
Example 1
The method for testing phthalate ester substances in the lithium ion battery anode material comprises the following steps:
(1) and (3) freezing and grinding the lithium iron phosphate anode material of the lithium ion battery into powder, and screening the powder by using a 60-mesh screen until the particle size is smaller than 250 mu m.
(2) Weighing 3 parts of sieved sample powder 50.0 +/-10 mg, placing the sieved sample powder into 3 10mL screw pretreatment glass vials respectively, adding 3mL n-hexane/ethyl acetate (v/v,1/1) mixed solution into one part of the sieved sample powder, sealing the mixture, adding 30 mu L of four phthalic acid mixed standard solutions with the concentration of 500 mu g/mL into the other two parts of the sieved sample powder, and fixing the volume to 3mL by using n-hexane/ethyl acetate (v/v, 1/1). Meanwhile, another screw-top pretreatment glass vial was taken, and 3mL of a total amount of n-hexane/ethyl acetate (v/v,1/1) mixture was added thereto and sealed. Wherein 50.0 + -10 mg means that errors within 10mg have substantially no effect on the assay results.
(3) The pre-treated vial which had been sealed was placed in an ultrasonic cleaner and extracted at 280W for 40 min.
(4) The sample solution was filtered through a syringe and a 0.22 μm organic filter head, followed by quantitative analysis by GC-MS, the analysis results of which are shown in Table 2. The experimental method comprises the steps of weighing three target analysis samples in parallel, adding pure solvents or solutions with different concentrations of target analytes (o-benzene substances), and adding an analysis result with a scalar of zero to obtain a sample determination result.
(5) And judging the applicability of the method and judging whether the lithium iron phosphate material (the anode coating) meets the process standard or not according to the analysis result.
TABLE 2 determination results and spiking recovery of lithium iron phosphate materials
Figure BDA0003293243390000071
Wherein N.D. is not detected
As can be seen from table 2, the lithium iron phosphate positive electrode material in this example meets the process standard, and the minimum recovery rate of the target is 74.66%.
Example 2
(1) And (3) freezing and grinding the 523 type nickel-cobalt-manganese ternary positive electrode material of the lithium ion battery into powder, and screening the powder by using a 60-mesh screen until the particle size is smaller than 250 mu m.
(2) Weighing 3 parts of sieved sample powder 50.0 +/-10 mg, placing the powder into 3 10mL screw pretreatment glass vials respectively, adding 3mL n-hexane/ethyl acetate (v/v,1/1) into one part of the vials, sealing the vials, adding 30 mu L and 60 mu L of four phthalic acid mixed standard solutions with the concentration of 500 mu g/mL into the other two parts of the vials, and fixing the volume to 3mL by using n-hexane/ethyl acetate (v/v, 1/1). Meanwhile, another screw-top pretreated glass vial was taken, and 3mL of n-hexane/ethyl acetate (v/v,1/1) was added thereto and sealed.
(3) The pre-treated vial which had been sealed was placed in an ultrasonic cleaner and extracted at 280W for 40 min.
(4) The sample solution was filtered through a syringe and a 0.22 μm organic filter head, followed by GC-MS quantitative analysis, the analysis results of which are shown in Table 3.
(5) And judging the applicability of the method and judging whether the nickel-cobalt-manganese ternary material (the anode coating) meets the process standard or not according to the analysis result.
TABLE 3523 type Ni-Co-Mn ternary material determination result and standard recovery
Figure BDA0003293243390000081
Wherein N.D. is not detected
As can be seen from table 3, the 523-type ni-co-mn ternary cathode material in this example meets the process standard, and the target recovery rate is 77.20% at the minimum.
Example 3
(1) And (3) freezing and grinding the 622 type nickel-cobalt-manganese ternary positive electrode material of the lithium ion battery into powder, and screening the powder by using a 60-mesh screen until the particle size is smaller than 250 mu m.
(2) Weighing 3 parts of sieved sample powder 50.0 +/-10 mg, placing the powder into 3 10mL screw pretreatment glass vials respectively, adding 3mL n-hexane/ethyl acetate (v/v,1/1) into one part of the vials, sealing the vials, adding 30 mu L and 60 mu L of four phthalic acid mixed standard solutions with the concentration of 500 mu g/mL into the other two parts of the vials, and fixing the volume to 3mL by using n-hexane/ethyl acetate (v/v, 1/1). Meanwhile, another screw-top pretreated glass vial was taken, and 3mL of n-hexane/ethyl acetate (v/v,1/1) was added thereto and sealed.
(3) The pre-treated vial which had been sealed was placed in an ultrasonic cleaner and extracted at 280W for 40 min.
(4) The sample solution was filtered through a syringe and a 0.22 μm organic filter head, followed by quantitative analysis by GC-MS, the analysis results of which are shown in Table 4.
(5) And judging the applicability of the method and judging whether the nickel-cobalt-manganese ternary material (the anode coating) meets the process standard or not according to the analysis result.
TABLE 4622 type Ni-Co-Mn ternary material determination result and standard recovery
Figure BDA0003293243390000082
Figure BDA0003293243390000091
Wherein N.D. is not detected
As can be seen from table 4, the 622-type ni-co-mn ternary positive electrode material in this example meets the process standard.
Example 4
(1) And (3) freezing and grinding the 811 type nickel-cobalt-manganese ternary positive electrode material of the lithium ion battery into powder, and screening the powder by using a 60-mesh screen until the particle size is smaller than 250 mu m.
(2) Weighing 3 parts of sieved sample powder 50.0 +/-10 mg, placing the powder into 3 10mL screw pretreatment glass vials respectively, adding 3mL n-hexane/ethyl acetate (v/v,1/1) into one part of the vials, sealing the vials, adding 30 mu L and 60 mu L of four phthalic acid mixed standard solutions with the concentration of 500 mu g/mL into the other two parts of the vials, and fixing the volume to 3mL by using n-hexane/ethyl acetate (v/v, 1/1). Meanwhile, another screw-top pretreated glass vial was taken, and 3mL of n-hexane/ethyl acetate (v/v,1/1) was added thereto and sealed.
(3) The pre-treated vial which had been sealed was placed in an ultrasonic cleaner and extracted at 280W for 40 min.
(4) The sample solution was filtered through a syringe and a 0.22 μm organic filter head, followed by GC-MS quantitative analysis, the analysis results of which are shown in Table 5.
(5) And judging the applicability of the method and judging whether the nickel-cobalt-manganese ternary material (the anode coating) meets the process standard or not according to the analysis result.
TABLE 5811 measurement results of Ni-Co-Mn ternary material and standard recovery
Figure BDA0003293243390000092
Figure BDA0003293243390000101
Wherein N.D. is not detected
As can be seen from table 5, the 811-type ni-co-mn ternary cathode material in this example meets the process standard, and the target recovery rate is 92.18% at the minimum.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for testing phthalate ester substances in a positive electrode material or a coating of a lithium ion battery is characterized by comprising the following steps: the method comprises the following steps:
(1) freezing and grinding the lithium ion battery anode material or the coating into powder;
(2) adding a mixed solution of n-hexane and ethyl acetate into the powdery sample, and then sealing;
(3) and carrying out ultrasonic treatment on the sealed sample, filtering, and carrying out GC-MS analysis on the filtrate.
2. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: and (2) in the step (1), liquid nitrogen is adopted for grinding until the particle size of the powder is less than 250 mu m.
3. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: the phthalate ester substances comprise DEHP, BBP, DBP and DIBP.
4. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: the lithium ion battery anode material or the coating in the step (1) comprises a lithium iron phosphate material or a nickel-cobalt-manganese ternary material.
5. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: in the step (2), the volume ratio of n-hexane to ethyl acetate is 1:1, and the mass ratio of the powdery sample to the mixed solution is 40-60mg:3 mL.
6. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: the step (2) further comprises a reagent blank configuration step: mixing n-hexane and ethyl acetate, and sealing.
7. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: the step (2) further comprises a step of standard sample adding configuration: after weighing the sample, adding a proper amount of standard sample mixed liquid to enable the sample mixed liquid to reach different addition amounts, and then adding n-hexane and ethyl acetate.
8. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: and (4) performing ultrasonic treatment by using an ultrasonic cleaning machine in the step (3), wherein the power of the ultrasonic cleaning machine is 350W, and the power range is 75-85%.
9. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: the normal hexane and the ethyl acetate are in chromatographic purity grade.
10. The method for testing phthalate type substances in a lithium ion battery positive electrode material or coating according to claim 1, wherein: and (3) filtering by using a 0.22 mu m or 0.45 mu m filter head.
CN202111171179.3A 2021-10-08 2021-10-08 Method for testing phthalate substances in anode material or coating of lithium ion battery Pending CN113917021A (en)

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Publication number Priority date Publication date Assignee Title
JP2008009701A (en) * 2006-06-29 2008-01-17 Shin Nippon Air Technol Co Ltd Analysis method of molecular contaminant
CN108008029A (en) * 2017-11-13 2018-05-08 浙江省海洋水产研究所 The dispersive solid-phase extraction of Phthalates of Environment Hormone-gas chromatography-mass spectrum detection method in a kind of marine sediment
CN112730662A (en) * 2020-12-22 2021-04-30 中华人民共和国乌鲁木齐海关 Method for simultaneously determining phthalate and adipate plasticizers in textile solid waste
CN113075338A (en) * 2021-04-20 2021-07-06 品测(上海)检测科技有限公司 Method for detecting phthalate esters in animal food

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Title
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GOVINDAN MALARVANNAN 等: "Phthalate and alternative plasticizers in indwelling medical devices in pediatric intensive care units" *
卢俊文 等: "同位素稀释-气相色谱-串联质谱法快速测定糕点类食品中邻苯二甲酸酯" *
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