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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- 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
- 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 41
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 35
- 238000001514 detection method Methods 0.000 title claims abstract description 11
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 51
- 239000012086 standard solution Substances 0.000 claims description 23
- 239000000706 filtrate Substances 0.000 claims description 14
- 229910000032 lithium hydrogen carbonate Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 abstract description 4
- 238000004448 titration Methods 0.000 abstract description 4
- 229910052493 LiFePO4 Inorganic materials 0.000 abstract description 3
- 238000010998 test method Methods 0.000 abstract description 3
- 238000003556 assay Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 235000011167 hydrochloric acid Nutrition 0.000 description 17
- 229910003002 lithium salt Inorganic materials 0.000 description 6
- 159000000002 lithium salts Chemical class 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 description 1
- 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
- PNEFIWYZWIQKEK-UHFFFAOYSA-N carbonic acid;lithium Chemical compound [Li].OC(O)=O PNEFIWYZWIQKEK-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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 present invention relates to lithium content assay method, is related specifically to remain in a kind of lithium iron phosphate/carbon composite material and dissociates
The detection method of lithium content.Described lithium iron phosphate/carbon composite material is the positive electrode of lithium ion battery.
Background technology
Lithium iron phosphate/carbon composite material is as a kind of anode active material of lithium ion battery, because it has cheap, ring
Border is friendly, safe, good cycle, has substantial amounts of application in electrokinetic cell and energy-storage battery field.
Lithium iron phosphate/carbon composite material is generally in building-up process：Wet method is carried out using lithium salts, molysite, microcosmic salt and carbon source
Mixing, after then drying, carry out high temperature sintering and lithium iron phosphate/carbon composite material is made.For lithium iron phosphate/carbon composite material
Conventional lithium salts is：Lithium carbonate, lithium hydroxide, and these lithium salts occur that a small amount of volatilization causes the phosphorus of synthesis in pyroprocess
Sour iron lithiumation element ratio misalignment, to solve this problem, it can typically increase the inventory of lithium salts in the industrial production to intend
Lithium salts in sintering process is mended to lose.But if increased lithium salts amount is excessive or during sintering due to the fluctuation of furnace temperature or sintering time
It can cause micro free lithium residual in obtained lithium iron phosphate/carbon composite material be present.And micro free lithium is for phosphorus
Sour iron lithium/carbon composite material belongs to impurity, and too high levels can influence the chemical property of lithium iron phosphate/carbon composite material.Pass through
To the measure of the free lithium content remained in lithium iron phosphate/carbon composite material, it can be determined that the property of lithium iron phosphate/carbon composite material
Can, the problem of preventing from lithium iron phosphate/carbon composite material being fabricated in the performance for just finding material after battery.
Dissociate lithium there is not yet disclosed method of testing for the residual in lithium iron phosphate/carbon composite material at present.
The content of the invention
It is an object of the invention to overcome shortcoming and deficiency present in above-mentioned prior art, there is provided and a kind of LiFePO4/
The detection method of free lithium content is remained in carbon composite.Described lithium iron phosphate/carbon composite material is lithium ion battery
Positive electrode.
Purpose of the present invention provides following technical proposals and realized：Trip is remained in a kind of lithium iron phosphate/carbon composite material
From the detection method of lithium content, comprise the following steps：
(1) lithium iron phosphate/carbon composite material sample prepare liquid is prepared
The lithium iron phosphate/carbon composite material sample to be measured for weighing 40-60g (quality m) into 500mL beakers, adds
200mL deionized waters, ultrasonic 10min is carried out using ultrasonic wave；Then the obtained suspension after ultrasound is carried out using filter paper
After filtering, then filtrate is filtered to the filtrate clarified using the sand core funnel disengaging of 0.45 μm of micropore；
(2) measure of free lithium content
The filtrate of 25mL steps (1) acquisition is pipetted into 100mL beakers, magnetic stir bar is added and is put into magnetic stirring apparatus
On；The rotating speed of magnetic rotor is adjusted to 100rpm~300rpm；Using 0.005moL/L hydrochloric acid standard solutions check and accept be titrated to pH as
When 8.4, the volume V1 of record consumption hydrochloric acid standard solution；After buret is returned to zero, continue molten with 0.005moL/L normal hydrochloric acids
Liquid be titrated to pH for 4.5 when, record consumption hydrochloric acid standard solution volume V2；
(3) free elemental lithium cubage is remained in lithium iron phosphate/carbon composite material
The percentage composition that free elemental lithium is remained in lithium iron phosphate/carbon composite material calculates acquisition 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 body that hydrochloric acid standard solution is consumed when checking and accepting to be titrated to pH as 8.4 using 0.005moL/L hydrochloric acid standard solutions
Product, units/ml；
V2 is the body that hydrochloric acid standard solution is consumed when checking and accepting to be titrated to pH as 4.5 using 0.005moL/L hydrochloric acid standard solutions
Product, units/ml；
73.89 it is Li2CO3Molecular weight；
67.96 it is LiHCO3Molecular weight；
M be lithium iron phosphate/carbon composite material sample to be measured quality, unit g.
The Parameter Conditions of ultrasonic wave described in step (1) are ultrasonic power 100W.
In step (2), before the filtrate for pipetting 25mL steps (1) acquisition, as preferred embodiment, step is first used
(1) the filtrate rinse 25mL pipettes obtained 3 times.
As preferred embodiment, in step (2), the pH is detected using accurate pH meter.
The titration principle of the measure of free lithium content is in the step (2) of the present invention：
Li2CO3+ HCl=LiCl+LiHCO3(pH=8.4)；
LiHCO3+ HCl=LiCl+H2CO3(pH=4.5).
The present invention is had the following advantages relative to prior art and effect：
The present invention is realized to residual in LiFePO4 lithium iron phosphate/carbon composite material using the method for pH control stepwise titrations
The Accurate Determining of free elemental lithium is stayed, and the existence form for effectively having distinguished free elemental lithium is lithium carbonate or bicarbonate
Lithium.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 be gone on a tour
From the existence form of elemental lithium, there is important industrial value.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
The invention provides the detection method that free lithium content is remained in a kind of lithium iron phosphate/carbon composite material, the side
Method comprises the following steps：
(1) lithium iron phosphate/carbon composite material sample prepare liquid is prepared
For a lithium iron phosphate/carbon composite material, weigh respectively 50.01g, 49.88g, 48.98g, 51.17g,
51.04g is added in 5 500mL beakers, is then respectively adding 200mL deionized waters, is surpassed using power 100W ultrasonic waves
Sound 10min；Then after the obtained suspension after ultrasound is filtered using filter paper, then by filtrate using 0.45 μm of micropore
Sand core funnel disengaging, which filters, obtains the filtrate of 5 parts of clarifications；
(2) measure of free lithium content
First use filtrate rinse 25mL pipettes 3 times, pipette 25mL filtrates in 100mL beakers, add magnetic stir bar and put
Onto magnetic stirring apparatus；The electrode of accurate pH meter is put into solution to be measured, adjusts the rotating speed of magnetic rotor to 200rpm；With
0.005moL/L hydrochloric acid standard solutions check and accept be titrated to pH for 8.4 when, record consumption hydrochloric acid standard solution volume V1；Will titration
Pipe zeroing after, continue with 0.05moL/L hydrochloric acid standard solutions be titrated to pH for 4.5 when, record consumption hydrochloric acid standard solution body
Product V2；The disappear volume V1 and V2 of hydrochloric acid solution of 5 samples is shown in Table 1；
(3) free elemental lithium cubage is remained in lithium iron phosphate/carbon composite material
The percentage composition that free elemental lithium is remained in lithium iron phosphate/carbon composite material calculates according to the following formula, calculates knot
Fruit 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 body that hydrochloric acid standard solution is consumed when checking and accepting to be titrated to pH as 8.4 using 0.005moL/L hydrochloric acid standard solutions
Product, units/ml；
V2 is the body that hydrochloric acid standard solution is consumed when checking and accepting to be titrated to pH as 4.5 using 0.005moL/L hydrochloric acid standard solutions
Product, units/ml；
73.89 it is Li2CO3Molecular weight；
67.96 it is LiHCO3Molecular weight；
M be weigh lithium iron phosphate/carbon composite material sample quality, unit g.
The measurement result of the sample of 1 embodiment of table 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 and free lithium content is remained in lithium iron phosphate/carbon composite material, the average value of carbonic acid lithium content is 0.0901%,
Standard deviation is 0.0011；The content average value of lithium bicarbonate is 0.0378%, standard deviation 0.0014.Can using the method
Free lithium content is remained in lithium iron phosphate/carbon composite material to measure, and can accurately provide the content of lithium carbonate and lithium bicarbonate,
The error of measurement is small.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (4)
1. the detection method of free lithium content is remained in a kind of lithium iron phosphate/carbon composite material, it is characterised in that：Including following step
Suddenly：
(1) lithium iron phosphate/carbon composite material sample prepare liquid is prepared
The lithium iron phosphate/carbon composite material sample to be measured for weighing 40-60g (quality m) into 500mL beakers, adds 200mL and gone
Ionized water, ultrasonic 10min is carried out using ultrasonic wave；Then after the obtained suspension after ultrasound is filtered using filter paper,
Filtrate is filtered to the filtrate clarified using the sand core funnel disengaging of 0.45 μm of micropore again；
(2) measure of free lithium content
The filtrate of 25mL steps (1) acquisition is pipetted into 100mL beakers, magnetic stir bar is added and is put on magnetic stirring apparatus；Adjust
The rotating speed of magnetic rotor is saved to 100rpm~300rpm；When being titrated to pH as 8.4 using the examination of 0.005moL/L hydrochloric acid standard solutions,
The volume V1 of record consumption hydrochloric acid standard solution；After buret is returned to zero, continue to be titrated with 0.005moL/L hydrochloric acid standard solutions
To pH be 4.5 when, record consumption hydrochloric acid standard solution volume V2；
(3) free elemental lithium cubage is remained in lithium iron phosphate/carbon composite material
The percentage composition that free elemental lithium is remained in lithium iron phosphate/carbon composite material calculates acquisition 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 when checking and accepting to be titrated to pH as 8.4 using 0.005moL/L hydrochloric acid standard solutions, to consume the volume of hydrochloric acid standard solution, single
Position ml；
V2 is when checking and accepting to be titrated to pH as 4.5 using 0.005moL/L hydrochloric acid standard solutions, to consume the volume of hydrochloric acid standard solution, single
Position ml；
73.89 it is Li2CO3Molecular weight；
67.96 it is LiHCO3Molecular weight；
M be lithium iron phosphate/carbon composite material sample to be measured quality, unit g.
2. the detection method of free lithium content, its feature are remained in lithium iron phosphate/carbon composite material according to claim 1
It is：The Parameter Conditions of ultrasonic wave described in step (1) are that Parameter Conditions are ultrasonic power 100W.
3. the detection method of free lithium content, its feature are remained in lithium iron phosphate/carbon composite material according to claim 1
It is：In step (2), before the filtrate for pipetting 25mL steps (1) acquisition, the filtrate rinse 25mL first obtained with step (1) is moved
Liquid pipe 3 times.
4. the detection method of free lithium content, its feature are remained in lithium iron phosphate/carbon composite material according to claim 1
It is：In step (2), the pH is detected using accurate 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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