CN105842389B - The detection method of free lithium content is remained in a kind of lithium iron phosphate/carbon composite material - Google Patents
The detection method of free lithium content is remained in a kind of lithium iron phosphate/carbon composite material Download PDFInfo
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- CN105842389B CN105842389B CN201610156984.1A CN201610156984A CN105842389B CN 105842389 B CN105842389 B CN 105842389B CN 201610156984 A CN201610156984 A CN 201610156984A CN 105842389 B CN105842389 B CN 105842389B
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- lithium
- composite material
- iron phosphate
- carbon composite
- lithium iron
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 13
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 238000004448 titration Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 52
- 239000012086 standard solution Substances 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 14
- 229910000032 lithium hydrogen carbonate Inorganic materials 0.000 claims description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 abstract description 4
- 238000010998 test method Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 abstract 1
- 238000003556 assay Methods 0.000 abstract 1
- 229910003002 lithium salt Inorganic materials 0.000 description 6
- 159000000002 lithium salts Chemical class 0.000 description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000006183 anode active material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- 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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses the detection method that free lithium content is remained in a kind of lithium iron phosphate/carbon composite material, belong to lithium content assay method technical field.The present invention realizes the Accurate Determining to remaining free elemental lithium in LiFePO4 lithium iron phosphate/carbon composite material, and the existence form for effectively having distinguished free elemental lithium is lithium carbonate or lithium bicarbonate using the method for pH control stepwise titrations.The method of testing of the present invention is simple to operate, and test result error is small, more scientific and reasonable, accurate, and can accurately provide the existence form of free elemental lithium, has important industrial value.
Description
Technical Field
The invention relates to a method for measuring lithium content, in particular to a method for detecting the content of residual free lithium in a lithium iron phosphate/carbon composite material. The lithium iron phosphate/carbon composite material is a positive electrode material of a lithium ion battery.
Background
The lithium iron phosphate/carbon composite material is used as a lithium ion battery anode active material, and has the advantages of low price, environmental friendliness, high safety and good cycle performance, and thus, the lithium iron phosphate/carbon composite material has a large number of applications in the fields of power batteries and energy storage batteries.
The synthesis process of the lithium iron phosphate/carbon composite material generally comprises the following steps: lithium salt, ferric salt, phosphorus salt and a carbon source are mixed by a wet method, and then the mixture is dried and sintered at high temperature to prepare the lithium iron phosphate/carbon composite material. Common lithium salts for lithium iron phosphate/carbon composites are: lithium carbonate and lithium hydroxide, and a small amount of volatilization of the lithium salts can occur in the high-temperature process to cause the proportion of chemical elements of the synthesized lithium iron phosphate to be misaligned, so that the feeding amount of the lithium salts is generally increased in industrial production to compensate the loss of the lithium salts in the sintering process. However, if the amount of the lithium salt is excessively increased or the sintering is performed, a slight amount of free lithium remains in the prepared lithium iron phosphate/carbon composite material due to fluctuations in furnace temperature or sintering time. And trace amount of free lithium belongs to impurities for the lithium iron phosphate/carbon composite material, and the electrochemical performance of the lithium iron phosphate/carbon composite material is influenced by too high content of the free lithium. The performance of the lithium iron phosphate/carbon composite material can be judged by measuring the content of the residual free lithium in the lithium iron phosphate/carbon composite material, so that the problem of finding the performance of the material after the lithium iron phosphate/carbon composite material is made into a battery is solved.
At present, no published test method for residual free lithium in the lithium iron phosphate/carbon composite material exists.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for detecting the content of residual free lithium in a lithium iron phosphate/carbon composite material. The lithium iron phosphate/carbon composite material is a positive electrode material of a lithium ion battery.
The purpose of the invention is realized by the following technical scheme: a method for detecting the content of residual free lithium in a lithium iron phosphate/carbon composite material comprises the following steps:
(1) preparation of lithium iron phosphate/carbon composite material sample to-be-detected solution
Weighing 40-60g of a lithium iron phosphate/carbon composite material sample to be detected (with the mass of m) into a 500mL beaker, adding 200mL of deionized water, and carrying out ultrasonic treatment for 10min by adopting ultrasonic waves; filtering the suspension obtained after the ultrasonic treatment by using filter paper, and performing suction filtration on the filtrate by using a sand core funnel with a micropore of 0.45 mu m to obtain clear filtrate;
(2) determination of the free lithium content
Transferring 25mL of the filtrate obtained in the step (1) into a 100mL beaker, adding a magnetic stirrer, and placing the beaker on a magnetic stirrer; adjusting the rotating speed of the magnetic rotor to 100-300 rpm; when the hydrochloric acid standard solution is subjected to acceptance titration by 0.005moL/L until the pH value is 8.4, recording the volume V1 of the consumed hydrochloric acid standard solution; after the burette is zeroed, continuously titrating with 0.005moL/L hydrochloric acid standard solution until the pH value is 4.5, and recording the volume V2 of the consumed hydrochloric acid standard solution;
(3) calculation of residual free lithium content in lithium iron phosphate/carbon composite material
The percentage content of the residual free lithium element in the lithium iron phosphate/carbon composite material is calculated according to the following formula:
Li2CO3(％)＝((0.005/1000×V1)×(200/25)×73.89)/m；
LiHCO3(％)＝((0.005/1000×(V2—V1))×(200/25)×67.96)/m；
wherein,
v1 is the volume of hydrochloric acid standard solution consumed in unit ml when the hydrochloric acid standard solution is accepted and titrated to pH 8.4 by 0.005 moL/L;
v2 is the volume of hydrochloric acid standard solution consumed in unit ml when the hydrochloric acid standard solution is accepted and titrated to pH 4.5 by 0.005 moL/L;
73.89 is Li2CO3The molecular weight of (a);
67.96 is LiHCO3The molecular weight of (a);
and m is the mass of the lithium iron phosphate/carbon composite material sample to be detected and the unit g.
The parameter condition of the ultrasonic wave in the step (1) is ultrasonic wave power 100W.
In step (2), before removing 25mL of the filtrate obtained in step (1), a 25mL pipette is rinsed 3 times with the filtrate obtained in step (1) as a preferred embodiment.
As a preferred embodiment, in the step (2), the pH is detected using a precision pH meter.
The titration principle of the determination of the content of free lithium in the step (2) of the invention is as follows:
Li2CO3+HCl＝LiCl+LiHCO3(pH＝8.4)；
LiHCO3+HCl＝LiCl+H2CO3(pH＝4.5)。
compared with the prior art, the invention has the following advantages and effects:
the invention adopts a pH control step titration method to realize accurate determination of the residual free lithium element in the lithium iron phosphate/carbon composite material, and effectively distinguishes whether the existence form of the free lithium element is lithium carbonate or lithium bicarbonate. The test method provided by the invention is simple to operate, has small error of test results, is more scientific, reasonable and accurate, can accurately give the existence form of the free lithium element, and has important industrial value.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
The invention provides a method for detecting the content of residual free lithium in a lithium iron phosphate/carbon composite material, which comprises the following steps:
(1) preparation of lithium iron phosphate/carbon composite material sample to-be-detected solution
50.01g, 49.88g, 48.98g, 51.17g and 51.04g of a part of lithium iron phosphate/carbon composite material are respectively weighed and added into 5 500mL beakers, 200mL of deionized water is then respectively added, and ultrasonic treatment is carried out for 10min by adopting 100W ultrasonic wave; filtering the suspension obtained after the ultrasonic treatment by using filter paper, and performing suction filtration on the filtrate by using a sand core funnel with a micropore of 0.45 mu m to obtain 5 parts of clear filtrate;
(2) determination of the free lithium content
Rinsing a 25mL pipette with the filtrate for 3 times, transferring the 25mL filtrate into a 100mL beaker, adding a magnetic stirrer, and placing the magnetic stirrer on a magnetic stirrer; putting an electrode of a precision pH meter into a solution to be measured, and adjusting the rotating speed of a magnetic rotor to 200 rpm; when the hydrochloric acid standard solution is subjected to acceptance titration by 0.005moL/L until the pH value is 8.4, recording the volume V1 of the consumed hydrochloric acid standard solution; after the burette is zeroed, continuously titrating with 0.05moL/L hydrochloric acid standard solution until the pH value is 4.5, and recording the volume V2 of the consumed hydrochloric acid standard solution; the volumes of the 5 samples of hydrochloric acid elimination solution V1 and V2 are shown in Table 1;
(3) calculation of residual free lithium content in lithium iron phosphate/carbon composite material
The percentage content of the residual free lithium element in the lithium iron phosphate/carbon composite material is calculated according to the following formula, and the calculation result is shown in table 1:
Li2CO3(％)＝((0.005/1000×V1)×(200/25)×73.89)/m
LiHCO3(％)＝((0.005/1000×(V2—V1))×(200/25)×67.96)/m；
wherein,
v1 is the volume of hydrochloric acid standard solution consumed in unit ml when the hydrochloric acid standard solution is accepted and titrated to pH 8.4 by 0.005 moL/L;
v2 is the volume of hydrochloric acid standard solution consumed in unit ml when the hydrochloric acid standard solution is accepted and titrated to pH 4.5 by 0.005 moL/L;
73.89 is Li2CO3The molecular weight of (a);
67.96 is LiHCO3The molecular weight of (a);
and m is the mass of a weighed lithium iron phosphate/carbon composite material sample and the unit g.
Table 1 measurement results of the sample of example 1
| Numbering | 1 | 2 | 3 | 4 | 5 |
| Weight m (g) | 50.01 | 49.88 | 48.98 | 51.17 | 51.04 |
| V1(mL) | 15.2 | 15.0 | 14.9 | 15.9 | 15.6 |
| V2(mL) | 22.4 | 21.6 | 21.8 | 22.8 | 22.9 |
| Li2CO3(％) | 0.0898 | 0.0889 | 0.0899 | 0.0918 | 0.0903 |
| LiHCO3(％) | 0.0391 | 0.0360 | 0.0383 | 0.0367 | 0.0389 |
Detecting the content of residual free lithium in the lithium iron phosphate/carbon composite material, wherein the average value of the content of lithium carbonate is 0.0901%, and the standard deviation is 0.0011; the content of lithium hydrogencarbonate had an average value of 0.0378% and a standard deviation of 0.0014. By using the method, the content of residual free lithium in the lithium iron phosphate/carbon composite material can be measured, the contents of lithium carbonate and lithium bicarbonate can be accurately given, and the measurement error is small.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. A method for detecting the content of residual free lithium in a lithium iron phosphate/carbon composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of lithium iron phosphate/carbon composite material sample to-be-detected solution
Weighing 40-60g of a lithium iron phosphate/carbon composite material sample to be detected (with the mass of m) into a 500mL beaker, adding 200mL of deionized water, and carrying out ultrasonic treatment for 10min by adopting ultrasonic waves; filtering the suspension obtained after the ultrasonic treatment by using filter paper, and performing suction filtration on the filtrate by using a sand core funnel with a micropore of 0.45 mu m to obtain clear filtrate;
(2) determination of the free lithium content
Transferring 25mL of the filtrate obtained in the step (1) into a 100mL beaker, adding a magnetic stirrer, and placing the beaker on a magnetic stirrer; adjusting the rotating speed of the magnetic rotor to 100-300 rpm; when the hydrochloric acid standard solution is subjected to acceptance titration by 0.005moL/L until the pH value is 8.4, recording the volume V1 of the consumed hydrochloric acid standard solution; after the burette is zeroed, continuously titrating with 0.005moL/L hydrochloric acid standard solution until the pH value is 4.5, and recording the volume V2 of the consumed hydrochloric acid standard solution;
(3) calculation of residual free lithium content in lithium iron phosphate/carbon composite material
The percentage content of the residual free lithium element in the lithium iron phosphate/carbon composite material is calculated according to the following formula:
Li2CO3(％)＝((0.005/1000×V1)×(200/25)×73.89)/m；
LiHCO3(％)＝((0.005/1000×(V2—V1))×(200/25)×67.96)/m；
wherein,
v1 is the volume of hydrochloric acid standard solution consumed in unit ml when the hydrochloric acid standard solution is accepted and titrated to pH 8.4 by 0.005 moL/L;
v2 is the volume of hydrochloric acid standard solution consumed in unit ml when the hydrochloric acid standard solution is accepted and titrated to pH 4.5 by 0.005 moL/L;
73.89 is Li2CO3The molecular weight of (a);
67.96 is LiHCO3The molecular weight of (a);
and m is the mass of the lithium iron phosphate/carbon composite material sample to be detected and the unit g.
2. The method for detecting the content of residual free lithium in the lithium iron phosphate/carbon composite material according to claim 1, wherein the method comprises the following steps: the parameter condition of the ultrasonic wave in the step (1) is that the parameter condition is that the ultrasonic wave power is 100W.
3. The method for detecting the content of residual free lithium in the lithium iron phosphate/carbon composite material according to claim 1, wherein the method comprises the following steps: in step (2), a 25mL pipette was rinsed 3 times with the filtrate obtained in step (1) before removing 25mL of the filtrate obtained in step (1).
4. The method for detecting the content of residual free lithium in the lithium iron phosphate/carbon composite material according to claim 1, wherein the method comprises the following steps: in the step (2), the pH is detected by using a precision pH meter.
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| CN106248670A (en) * | 2016-08-16 | 2016-12-21 | 格林美（无锡）能源材料有限公司 | The method of residual alkali in multiple positive electrode is measured based on automatic titering process |
| CN106770244A (en) * | 2016-12-21 | 2017-05-31 | 浙江超威创元实业有限公司 | LiOH and Li in a kind of nickelic ternary material2CO3The assay method of content |
| CN109917070A (en) * | 2019-03-26 | 2019-06-21 | 东莞东阳光科研发有限公司 | The detection method of free lithium content is remained in tertiary cathode material |
| CN111366489B (en) * | 2020-03-26 | 2022-05-20 | 湖南长远锂科股份有限公司 | Semi-quantitative detection method for lithium content in primary mixed material sample of ternary cathode material |
| CN111948335B (en) * | 2020-06-29 | 2021-08-24 | 北京当升材料科技股份有限公司 | Method for testing residual alkali content in coated modified cathode material and application thereof |
| CN112903904A (en) * | 2021-01-14 | 2021-06-04 | 陕西彩虹新材料有限公司 | Detection method for free lithium on surface of positive electrode material |
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