CN103776953A - Determination method of content of cobalt in lithium battery ternary positive electrode material - Google Patents
Determination method of content of cobalt in lithium battery ternary positive electrode material Download PDFInfo
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Abstract
The invention provides a determination method of the content of cobalt in a lithium battery ternary positive electrode material, relates to a determination method of the content of cobalt in material with high manganese content, and in particular relates to a determination method of the content of cobalt in the lithium battery ternary positive electrode material. The method comprises the following steps: (1) accurately weighing moderate to-be-determined ternary positive electrode material, adding acid to dissolve and making up to volume; (2) adding perchloric acid-phosphoric acid to a certain amount of dissolved solution, heating till perchloric acid smoke emits, and adding a moderate masking agent to eliminate manganese interference; (3) performing back-titration on a potentiometric titrator by using a cobalt standard solution, drawing a differential curve and obtaining titration end point consumed volume according to a second-order differential method; and (4) computing to obtain the cobalt content in a sample according to a formula. According to the method provided by the invention, the manganese reducing operation is unnecessary, and the determination of the content of the cobalt in the sample containing manganese with the weight percent being not more than 40% cannot be influenced, the accuracy is high, the treatment process is simple and the method is easy to popularize.
Description
Technical field
The present invention relates to the assay method of cobalt content in material that a kind of manganese content is higher, be specifically related to the assay method of cobalt content in lithium battery tertiary cathode material.
Background technology
Along with in recent years the demand of energy-conservation and environmental protection being increased day by day, the application of lithium battery is also healed and is become extensively, and anode material of lithium battery is as its core critical material, and the development prospect of the sector is very good.At present, the nickel-cobalt-manganese ternary positive electrode with stratiform packed structures relies on that its height ratio capacity, cycle performance are good, Heat stability is good and the advantage such as cheap be rapidly by people institute research and utilization, is the high performance lithium ion battery anode material that a kind of tool has great prospects for development.
In the preparation process of lithium ion tertiary cathode material, nickel cobalt manganese three content proportioning has a great impact its chemical property tool, so in the time carrying out tertiary cathode material research, the content of necessary accurate analysis nickel cobalt manganese.
According to existing assay method, in nickel-cobalt-manganese ternary positive electrode, the mensuration of nickel and manganese is comparatively easy, and cobalt is often subject to the interference of various factors in the time analyzing, mensuration for trace cobalt content generally adopts atomic absorption spectrophotometry, the method is fast and convenient, has good mensuration precision, but measures and need to dilute operation for the constant of cobalt, easily produce error, precision is measured in impact.
Macro-analysis for cobalt extensively adopts potentiometric titration at present, the measurement range of cobalt content: 5%～25%, when in sample, the content of manganese is less than 0.05%, can ignore the impact of manganese amount, shortcoming is when in sample, the content of manganese is greater than 0.05%, with the excessive potassium ferricyanide cobalt oxide time, manganese (II) is also titrated, manganese (II) to measurement result for just disturbing, must adopt other method to draw total manganese amount, then from the total cobalt amount recording, deduct total manganese amount in sample, thereby obtain single cobalt content, the method not only operates comparatively loaded down with trivial details, and easily produce larger error.
Summary of the invention
For various deficiencies and the defect of current existing cobalt content determination techniques, the object of the present invention is to provide a kind of easy and simple to handle, cobalt content assay method in the high tertiary cathode material of accuracy.
For realizing above-mentioned requirements, method of the present invention is carried out according to the following steps:
point getting 10mL tertiary cathode material lysate adds in 250mL beaker, and slightly cold 10mL distilled water and the 2g complexing agent of adding immediately after adding 5mL phosphoric acid and 3mL perchloric acid to be heated to emit a large amount of perchloric acid cigarettes completely, takes off the cooling titrimetry for the treatment of;
V
1-accurately add the volume of potassium ferricyanide standard solution, unit be milliliter (mL)
V
2when-back titration, consume the volume of cobalt standard solution, unit is milliliter (mL)
The cumulative volume of V-test solution, unit is milliliter (mL)
V
3-point get the volume of test solution, unit is milliliter (mL)
The titrimetric factor of K-potassium ferricyanide standard solution to cobalt standard titration solution;
M-take the quality of sample, unit is gram (g)
ρ-cobalt normal concentration, unit is gram every milliliter (g/mL);
(2)
K-titrimetric factor, the potassium ferricyanide standard solution of unit volume consumes the volume number of cobalt standard titration solution
V
0-pipette cobalt standard solution milliliter number, mL
V
1-back titration consumes cobalt standard solution milliliter number, mL
V
2-add potassium ferricyanide standard solution milliliter number, mL.
The advantage that the present invention compared with prior art had is:
compared with existing atomic absorption method, chemical titration etc., there is equipment investment few, agents useful for same is few, and the simple feature of equipment is applicable to general laboratory and uses.
Accompanying drawing explanation
Fig. 1 is according to table 1 cobalt mark addition and the made first-order derivative curve of potential change relation in the embodiment of the present invention 1
Fig. 2 is according to table 2 cobalt mark addition and the made first-order derivative curve of potential change relation in the embodiment of the present invention 2
Fig. 3 is according to table 3 cobalt mark addition and the made first-order derivative curve of potential change relation in the embodiment of the present invention 3.
Embodiment
Hydrochloric acid solution, salpeter solution, perchloric acid solution and the phosphoric acid solution etc. that in the embodiment of the present invention, adopt are commercial analytical reagent or are prepared by commercial analytical reagent.
Ammonium citrate-ammonia mixed solution: take 60g ammonium chloride, 120g lemon ammonium, measures ammoniacal liquor 500mL, adds water and is settled to 1000mL, mixes.
Cobalt standard solution [3.00mg/mL]: accurately take 3.0000g metallic cobalt, add 20mL nitric acid (l+l), after dissolution in low temperature, water cleans table ware and wall of cup, moves in 1000mL volumetric flask, with water constant volume.Every milliliter of this solution is containing cobalt 3mg.(also can adopt cobaltous sulphate preparation, EDTA demarcates).
Potassium ferricyanide standard solution: take the 17g potassium ferricyanide, add the water-soluble solution of about 250mL, move in the brown volumetric flask of 1000mL, with water constant volume after filtering.
Selecting working sample is LiNi
0.5co
0.3mn
0.2o
2tertiary cathode material, the weight content of major effect element manganese is 11.32%, the weight content of cobalt is 18.23%;
Get 1g testing sample in beaker, add 15mL hydrochloric acid and 5mL nitric acid to be heated to dissolve completely, in cooling rear immigration 250mL volumetric flask, be settled to scale and shake up with distilled water, to be measured; Get in above-mentioned lysate 10mL and beaker with transfer pipet, add 5mL phosphoric acid and 3mL perchloric acid, be placed on electric furnace, to be heated to emit after a large amount of perchloric acid cigarettes and take off about about half a minute, slightly cold 10mL distilled water and the 2g sodium fluoride of adding immediately, is cooled to normal temperature to be analyzed; Get and in a beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, the liquid to be measured of processing is added in beaker, be cooled to below 20 ℃, under agitation pour lentamente 6mL potassium ferricyanide solution into, first be titrated to and approach terminal with cobalt standard solution with fast speed, then dropwise add, record cobalt standard solution addition and potential value and obtain cobalt standard solution addition when current potential is prominent to be got over.
Accurately pipette 10.00mL cobalt standard solution in 200mL beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, accurately add 15.00mL potassium ferricyanide standard solution, on potentiometric titrimeter, use cobalt standard solution back titration, determine terminal current potential and titration end-point.Calculate the titrimetric factor of potassium ferricyanide standard solution to cobalt standard titration solution by formula 2, specific experiment data are in table 1.
Table 1
Can record titrimetric factor K=0.995 according to formula 2, make Δ E/ Δ V-V draw Fig. 1 by table 1, in curve, peak is 3.5mL as shown in Figure 1, i.e. titration is prominent more near 3.5mL, from secondary differential calculation terminal: V
eventually=3.5+0.1 × (1500)/(1500-1400)=3.55, can be calculated Co%=18.15% according to formula 1.
Reliability of the present invention represents with relative standard deviation: relative standard deviation=(standard deviation/arithmetic mean) × 100%
Accuracy of the present invention represents by the recovery: the recovery=(Specimen Determination value/standard value) × 100%
For the cobalt content in the working sample of accurate quick more, following adopted DZ-2 type automatical potentiometric titrimeter carries out the mensuration of multiple Duplicate Samples, and specific experiment data are in table 2
Table 2
Above data are known, adopt automatical potentiometric titrimeter higher to the degree of accuracy of measuring and the accuracy of cobalt content in tertiary cathode material, meet analyze requirement completely.
Selecting working sample is LiNi
0.4co
0.2mn
0.4o
2tertiary cathode material, the weight content of major effect element manganese is 22.84%, the weight content of cobalt is 12.25%;
Get 1g testing sample in beaker, add 15mL hydrochloric acid and 5mL nitric acid to be heated to dissolve completely, in cooling rear immigration 250mL volumetric flask, be settled to scale and shake up with distilled water, to be measured; Get in above-mentioned lysate 10mL and beaker with transfer pipet, add 5mL phosphoric acid and 3mL perchloric acid, be placed on electric furnace, to be heated to emit after a large amount of perchloric acid cigarettes and take off about about half a minute, slightly cold 10mL distilled water and the 2g sodium fluoride of adding immediately, is cooled to normal temperature to be analyzed; Get and in a beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, the liquid to be measured of processing is added in beaker, be cooled to below 20 ℃, under agitation pour lentamente 6mL potassium ferricyanide solution into, first be titrated to and approach terminal with cobalt standard solution with fast speed, then dropwise add, record cobalt standard solution addition and potential value and obtain cobalt standard solution addition when current potential is prominent to be got over.
Accurately pipette 10.00mL cobalt standard solution in 200mL beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, accurately add 15.00mL potassium ferricyanide standard solution, on potentiometric titrimeter, use cobalt standard solution back titration, determine terminal current potential and titration end-point, calculate the titrimetric factor of potassium ferricyanide standard solution to cobalt standard titration solution by formula 2.Specific experiment data are in table 3.
Table 3
Can record titrimetric factor K=0.995 according to formula 2, make Δ E/ Δ V-V draw Fig. 2 by table 3, in curve, peak is 4.3mL as shown in Figure 2, i.e. titration is prominent more near 4.3mL, from secondary differential calculation terminal: V
eventually=4.3+0.1 × (1400)/(1400-1400)=4.35, can be calculated Co%=12.15% according to formula 1.
Reliability of the present invention represents with relative standard deviation: relative standard deviation=(standard deviation/arithmetic mean) × 100%
Accuracy of the present invention represents by the recovery: the recovery=(Specimen Determination value/standard value) × 100%.
For the cobalt content in the working sample of accurate quick more, following adopted DZ-2 type automatical potentiometric titrimeter carries out the mensuration of multiple Duplicate Samples, and specific experiment data are in table 4.
Table 4
Above data are known, adopt automatical potentiometric titrimeter higher to the degree of accuracy of measuring and the accuracy of cobalt content in tertiary cathode material, meet analyze requirement completely.
Selecting working sample is Li
1.2ni
0.16co
0.08mn
0.56o
2tertiary cathode material, the weight content of major effect element manganese is 36.1%, the weight content of cobalt is 5.53%;
Get 1g testing sample in beaker, add 15mL hydrochloric acid and 5mL nitric acid to be heated to dissolve completely, in cooling rear immigration 250mL volumetric flask, be settled to scale and shake up with distilled water, to be measured; Get in above-mentioned lysate 10mL and beaker with transfer pipet, add 5mL phosphoric acid and 3mL perchloric acid, be placed on electric furnace, to be heated to emit after a large amount of perchloric acid cigarettes and take off about about half a minute, slightly cold 10mL distilled water and the 2g sodium fluoride of adding immediately, is cooled to normal temperature to be analyzed; Get and in a beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, the liquid to be measured of processing is added in beaker, be cooled to below 20 ℃, under agitation pour lentamente 4mL potassium ferricyanide solution into, first be titrated to and approach terminal with cobalt standard solution with fast speed, then dropwise add, record cobalt standard solution addition and potential value and obtain cobalt standard solution addition when current potential is prominent to be got over.
Accurately pipette 10.00mL cobalt standard solution in 200mL beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, accurately add 15.00mL potassium ferricyanide standard solution, on potentiometric titrimeter, use cobalt standard solution back titration, determine terminal current potential and titration end-point, calculate the titrimetric factor of potassium ferricyanide standard solution to cobalt standard titration solution by formula 2.
Table 5
Can record titrimetric factor K=0.995 according to formula 2, make Δ E/ Δ V-V draw Fig. 3 by table 5, in curve, peak is 3.2mL as shown in Figure 3, i.e. titration is prominent more near 3.2mL, from secondary differential calculation terminal: V
eventually=3.2+0.1 × (1100)/(1100-1200)=3.248, can be calculated Co%=5.49% according to formula 1
Reliability of the present invention represents with relative standard deviation: relative standard deviation=(standard deviation/arithmetic mean) × 100%
Accuracy of the present invention represents by the recovery: the recovery=(Specimen Determination value/standard value) × 100%
For the cobalt content in the working sample of accurate quick more, following adopted DZ-2 type automatical potentiometric titrimeter carries out the mensuration of multiple Duplicate Samples, and specific experiment data are in table 4
Table 6
Above data are known, adopt automatical potentiometric titrimeter higher to the degree of accuracy of measuring and the accuracy of cobalt content in tertiary cathode material, meet analyze requirement completely.
Claims (8)
1. an assay method for cobalt content in lithium battery tertiary cathode material, is characterized in that, comprises the following steps:
(1) accurately take a certain amount of tertiary cathode material in beaker, add appropriate sour heating for dissolving complete, evaporating liquid takes off during to small size cooling, transfers to constant volume in volumetric flask;
(2) divide and get a certain amount of tertiary cathode material lysate and add in beaker, slightly cold a small amount of distilled water and the appropriate complexing agent of adding immediately after adding appropriate phosphoric acid and perchloric acid to be heated to emit a large amount of perchloric acid cigarettes completely, takes off the cooling titrimetry for the treatment of;
(3) toward before add the ammonium citrate ammonia mixed solution of appropriate ammonium sulfate and certain volume in the sample beaker processed of oxidation complexation, be cooled to below 20 ℃, under agitation pour lentamente a certain amount of potassium ferricyanide solution into, first be titrated to and approach terminal with cobalt standard solution with fast speed, then dropwise add, record cobalt standard solution addition and potential value and obtain cobalt standard solution addition when current potential is prominent to be got over, calculate (1) as follows:
V
1-accurately add the volume of potassium ferricyanide standard solution, unit be milliliter (mL)
V
2when-back titration, consume the volume of cobalt standard solution, unit is milliliter (mL)
The cumulative volume of V-test solution, unit is milliliter (mL)
V
3-point get the volume of test solution, unit is milliliter (mL)
The titrimetric factor of K-potassium ferricyanide standard solution to cobalt standard titration solution;
M-take the quality of sample, unit is gram (g)
ρ-cobalt normal concentration, unit is gram every milliliter (g/mL).
2. cobalt content assay method in tertiary cathode material according to claim 1, is characterized in that: the acid of described dissolving tertiary cathode material is hydrochloric acid and nitric acid.
3. cobalt content assay method in tertiary cathode material according to claim 1, is characterized in that: described complexing agent is sodium fluoride.
4. cobalt content assay method in tertiary cathode material according to claim 1, is characterized in that: the volume that consumes cobalt standard solution when back titration adopts second-order differential method to show that titration end-point consumes volume.
5. cobalt content assay method in tertiary cathode material according to claim 1, is characterized in that: described a certain amount of potassium ferricyanide solution is depending on Co amount, excessive 2～5mL.
6. cobalt content assay method in tertiary cathode material according to claim 1, is characterized in that: described titrimetric factor adopts the back titration of cobalt titer to measure.
7. cobalt content assay method in tertiary cathode material according to claim 6, is characterized in that: described titrimetric factor is measured and comprised the following steps:
Accurately pipette 10.00mL cobalt standard solution in beaker;
The ammonium citrate ammonia mixed solution that adds appropriate ammonium sulfate ammonium sulfate and certain volume, accurately adds 15.00mL potassium ferricyanide standard solution;
On potentiometric titrimeter, use cobalt standard solution back titration, determine terminal current potential and titration end-point, (2) calculate the titrimetric factor of potassium ferricyanide standard solution to cobalt standard titration solution as follows
（2）
K-titrimetric factor, the potassium ferricyanide standard solution of unit volume consumes the volume number of cobalt standard titration solution
V
0-pipette cobalt standard solution milliliter number, mL
V
1-back titration consumes cobalt standard solution milliliter number, mL
V
2-add potassium ferricyanide standard solution milliliter number, mL.
8. according to cobalt content assay method in the described tertiary cathode material of one of claim 1-7, it is characterized in that: technical scheme is for comprising the following steps:
accurately pipette 10.00mL cobalt standard solution in 200mL beaker, add 3～5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, accurately add 15.00mL potassium ferricyanide standard solution, on potentiometric titrimeter, use cobalt standard solution back titration, determine terminal current potential and titration end-point, calculate the titrimetric factor of potassium ferricyanide standard solution to cobalt standard titration solution by formula (2).
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Cited By (6)
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| CN104316643A (en) * | 2014-10-10 | 2015-01-28 | 荆门市格林美新材料有限公司 | Three-element determination method of nickel-cobalt-manganese ternary material |
| CN106290334A (en) * | 2016-08-05 | 2017-01-04 | 江苏理工学院 | Cobalt and the chemistry in detecting of Fe content in cobalt manganese raw material |
| CN109324094A (en) * | 2018-11-05 | 2019-02-12 | 西安热工研究院有限公司 | A kind of method of conductimetric titration detection sulfate radical content |
| CN111129486A (en) * | 2019-12-27 | 2020-05-08 | 中天新兴材料有限公司 | Method for preparing ternary cathode material of lithium battery |
| CN113740485A (en) * | 2021-09-06 | 2021-12-03 | 穆索诺伊矿业简易股份有限公司 | Method for measuring cobalt content in high-manganese crude cobalt hydroxide by potentiometric titration |
| CN113884617A (en) * | 2020-07-03 | 2022-01-04 | 荆门市格林美新材料有限公司 | Method for measuring cobalt and aluminum contents in aluminum-doped cobalt battery material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104316643A (en) * | 2014-10-10 | 2015-01-28 | 荆门市格林美新材料有限公司 | Three-element determination method of nickel-cobalt-manganese ternary material |
| CN106290334A (en) * | 2016-08-05 | 2017-01-04 | 江苏理工学院 | Cobalt and the chemistry in detecting of Fe content in cobalt manganese raw material |
| CN106290334B (en) * | 2016-08-05 | 2019-01-08 | 江苏理工学院 | The chemistry in detecting of cobalt and manganese content in cobalt manganese raw material |
| CN109324094A (en) * | 2018-11-05 | 2019-02-12 | 西安热工研究院有限公司 | A kind of method of conductimetric titration detection sulfate radical content |
| CN109324094B (en) * | 2018-11-05 | 2020-12-01 | 西安热工研究院有限公司 | Method for detecting sulfate radical content by conductivity titration |
| CN111129486A (en) * | 2019-12-27 | 2020-05-08 | 中天新兴材料有限公司 | Method for preparing ternary cathode material of lithium battery |
| CN113884617A (en) * | 2020-07-03 | 2022-01-04 | 荆门市格林美新材料有限公司 | Method for measuring cobalt and aluminum contents in aluminum-doped cobalt battery material |
| CN113740485A (en) * | 2021-09-06 | 2021-12-03 | 穆索诺伊矿业简易股份有限公司 | Method for measuring cobalt content in high-manganese crude cobalt hydroxide by potentiometric titration |
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Application publication date: 20140507 |