CN111366489B - Semi-quantitative detection method for lithium content in primary mixed material sample of ternary cathode material - Google Patents
Semi-quantitative detection method for lithium content in primary mixed material sample of ternary cathode material Download PDFInfo
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Abstract
The invention discloses a semi-quantitative detection method for lithium content in a primary mixed material sample of a ternary cathode material, which comprises the following steps: calculating sample weighing according to the theoretical lithium content of a given primary mixing sample in the production process, and weighing the primary mixing sample to a first container; according to the upper limit and the lower limit of the lithium content specification tolerance given in the production process, the proportion of the lithium raw material and the precursor in the upper limit sample and the lower limit sample is calculated, and the upper limit sample and the lower limit sample are respectively weighed to a second container and a third container; respectively adding water into the first container, the second container and the third container, stirring uniformly, then respectively adding acid, and stirring for reaction; and respectively testing the pH value of the solution, and judging the sample to be unqualified when the pH value of the sample is close to or exceeds the pH values of the upper limit sample and the lower limit sample. The method has the advantages of simple operation, low cost, less time consumption, high detection efficiency, small influence of external conditions such as temperature, humidity and the like, and capability of quickly judging whether the sample is qualified.
Description
Technical Field
The invention belongs to the technical field of lithium battery anode material detection, and particularly relates to a semi-quantitative detection method for lithium content in a sample in a primary mixing process in a ternary anode material production process.
Background
The lithium raw material (lithium carbonate or lithium hydroxide) is one of the important raw materials for producing the ternary cathode material, and the lithium raw material and a precursor (nickel-cobalt-manganese hydroxide or nickel-cobalt-aluminum hydroxide) need to be uniformly mixed according to a certain proportion in the production process, and the process is called as primary mixing. In order to ensure that the raw materials are uniformly mixed and the proportion is correct, the lithium content in the primary mixed material needs to be tested. The lithium content of a sample in the existing one-time material mixing process is mainly tested by adopting a potentiometric titration method, forming a working battery by an acid-base indicating electrode, a reference electrode and a tested solution, and then adding a titrant hydrochloric acid solution. In the titration process, the concentration of the detected ions is changed continuously due to the chemical reaction, so that the potential of the indicating electrode is changed along with the change. In the vicinity of the titration end point, the concentration of the ion to be measured is suddenly changed to cause a sudden change in the electrode potential, so that the titration end point can be determined from the sudden change in the electrode potential, and the measurement result can be obtained by calculation, thus being a quantitative detection method.
Although the potentiometric titration method has accurate detection result, the potentiometric titration method has the defects of long time consumption, high cost, complex pretreatment process and the like, is not beneficial to quick detection and cannot make quick response to production service.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology, and provides a semi-quantitative detection method for lithium content in a ternary cathode material primary mixed material sample, which can rapidly detect the lithium content on the premise of ensuring that the accuracy of a detection result is in a controllable range.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a semi-quantitative detection method for lithium content in a primary mixed material sample of a ternary cathode material comprises the following steps:
1) calculating sample weighing according to the theoretical lithium content of a primary mixed sample given in the production process and the following formula, and weighing the primary mixed sample to a first container;
wherein: m is sample weighing amount and g;
c-acid nominal concentration, mol/L;
v-acid addition volume, mL;
MLi-Li element molar mass, 6.941 g/mol;
w-theoretical lithium content of the sample,% (wt);
2) respectively weighing upper and lower limit samples to a second container and a third container, wherein the sample weighing amounts of lithium raw materials and precursors in the upper and lower limit samples accord with the following formula:
m2＝m-m1
wherein: m is1Weighing the sample amount of the lithium raw material, and g;
m2-weighing the precursor, g;
Δ w — upper or lower lithium content specification tolerance limit,% (wt);
wLitest lithium content in lithium feedstock,% (wt);
3) respectively adding water into the first container, the second container and the third container, stirring uniformly, then respectively adding acid with the calibration concentration of c and the volume of V, and stirring for reaction;
4) and respectively testing the pH value of the solution, and judging the sample to be a suspected unqualified sample when the pH value of the sample is close to or exceeds the pH values of the upper limit sample and the lower limit sample.
Further, the acid is a monobasic acid, and preferably, the acid is hydrochloric acid.
Further, the lithium raw material is lithium carbonate or lithium hydroxide. The precursor is nickel cobalt manganese hydroxide or nickel cobalt aluminum hydroxide.
Further, the upper and lower limit samples of step 2) need to be re-prepared when the reagent or the measuring tool is replaced.
Further, if the sample determined to be suspected to be unqualified in step 4), further determining whether the sample is qualified by a quantitative test method.
According to the method, after the acid-base ratio is calculated according to the theoretical value of the sample, the reaction is carried out according to the fixed ratio of the sample to the acid, and the pH value of the solution after the acid-base neutralization reaction is utilized to judge the excessive condition of the acid or the base, so that whether the sample is qualified or not is judged.
According to the invention, the pH value of the solution after acid-base neutralization is used as a qualification judgment basis, the upper and lower pH limits are determined according to the upper and lower limits of the lithium content specification tolerance given in the production process, and a rapid detection judgment method can be provided for whether a sample is qualified in a primary mixing process.
The invention has the advantages that: the method has the advantages of simple operation, low cost, less time consumption, high detection efficiency, small influence of external conditions such as temperature and humidity, and the like, can quickly judge whether the sample is qualified, and can make quick response to production service.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In a specific embodiment, the method for semi-quantitatively and rapidly detecting the lithium content in the primary mixed material sample comprises the following steps:
(1) calculating sample weighing amount according to theoretical lithium content given in the production process and the following formula, and weighing the sample into a 100mL beaker;
wherein: m is sample weighing amount and g;
c-acid nominal concentration, mol/L;
v-acid addition volume, mL;
MLi-Li element molar mass, 6.941 g/mol;
w-theoretical lithium content,% (wt) of the sample.
(2) Calculating the proportion of the lithium raw material and the precursor in the upper limit sample and the lower limit sample according to the upper limit and the lower limit of the tolerance of the lithium content specification given in the production process and the following formula, and respectively weighing the upper limit sample and the lower limit sample into two 100mL beakers;
m2＝m-m1
wherein: m is1Weighing the sample amount of the lithium raw material, and g;
m2-weighing the precursor, g;
m is the sample weighing amount calculated in the step (1), g;
w-theoretical lithium content of the sample,% (wt);
Δ w — upper or lower lithium content specification tolerance limit,% (wt);
wLitest lithium content in lithium feedstock,% (wt), provided by the feedstock manufacturer or obtained by testing.
The upper and lower limit samples of step (2) need to be reconstituted only when there is a change in the reagent or the measuring volume.
(3) Respectively adding 10mL of pure water and a C30 magneton into a beaker, covering a watch glass, and stirring for 5min on a magnetic stirrer;
(4) respectively adding 10mL of 1.0mol/L hydrochloric acid into the beaker, and continuously stirring for 1 min;
(5) and (4) testing the pH value of the solution by using a pH meter, recording the test result, and judging whether the sample is qualified according to the upper limit sample result and the lower limit sample result.
When the sample result is close to or even exceeds the upper limit and the lower limit, the sample is judged to be suspected to be unqualified, and whether the sample is qualified or not is further confirmed by a quantitative test method.
Example 1:
a sample of a batch had a theoretical lithium content of 5.5% (w ═ 5.5) and a specification tolerance of ± 0.1% (Δ w ═ 0.1).
(1) A sample (1.344 g) was weighed.
(2) Sample preparation Upper Limit 1.344g (lithium raw Material 0.402g, w)Li18.72 (%), precursor 0.942g), lower limit sample 1.344g (0.388g, precursor 0.956 g).
(3) 10mL of purified water was added thereto and stirred for 5 min.
(4) 10mL of 1.0mol/L hydrochloric acid (nominal concentration of 1.06510mol/L) was added thereto, and stirring was continued for 1 min.
(5) The pH of the solution was measured with a pH meter and the sample was 4.86 with an upper limit of 5.25 and a lower limit of 2.50.
And (3) detection results: the sample is qualified.
Example 2:
for a certain primary mixed material sample, the theoretical lithium content is 5.5 percent, and the specification tolerance is +/-0.1 percent.
(1) A sample (1.344 g) was weighed.
(2) Sample preparation Upper Limit 1.344g (lithium raw Material 0.402g, w)Li18.72 (%), precursor 0.942g), lower limit sample 1.344g (0.388g, precursor 0.956 g).
(3) 10mL of purified water was added thereto and stirred for 5 min.
(4) 10mL of 1.0mol/L hydrochloric acid (nominal concentration of 1.06510mol/L) was added thereto, and stirring was continued for 1 min.
(5) The pH of the solution was measured with a pH meter and the sample was 4.50 with an upper limit of 5.28 and a lower limit of 2.60.
And (3) detection results: the sample is qualified.
Example 3:
for a certain primary mixed material sample, the theoretical lithium content is 5.5 percent, and the specification tolerance is +/-0.1 percent.
(1) Sample 1.419g was weighed.
(2) Sample preparation Upper Limit 1.419g (lithium feed 0.425g, w)Li18.70 (%), precursor 0.994g), lower limit sample 1.419g (0.410g, precursor 1.009 g).
(3) 10mL of purified water was added thereto and stirred for 5 min.
(4) 10mL of 1.0mol/L hydrochloric acid (nominal concentration of 1.12421mol/L) was added thereto, and stirring was continued for 1 min.
(5) The pH of the solution was measured with a pH meter and the sample was 4.86 with an upper limit of 5.32 and a lower limit of 2.74.
And (3) detection results: the sample is qualified.
Example 4:
for a certain primary mixed material sample, the theoretical lithium content is 5.5 percent, and the specification tolerance is +/-0.1 percent.
(1) Sample 1.419g was weighed.
(2) Sample preparation Upper Limit 1.419g (lithium feed 0.425g, w)Li18.70 (%), precursor 0.994g), lower limit sample 1.419g (0.410g, precursor 1.009 g).
(3) 10mL of purified water was added thereto and stirred for 5 min.
(4) 10mL of 1.0mol/L hydrochloric acid (nominal concentration of 1.12421mol/L) was added thereto, and stirring was continued for 1 min.
(5) The pH of the solution was measured with a pH meter and the sample was 4.69 with an upper limit of 5.31 and a lower limit of 2.53.
And (3) detection results: the sample is qualified.
Example 5:
for a certain primary mixed material sample, the theoretical lithium content is 5.6 percent, and the specification tolerance is +/-0.1 percent.
(1) Sample 1.392g was weighed.
(2) Sample preparation Upper limit of 1.392g (lithium raw material 0.424g, w)Li18.71 (%), precursor 0.968g), lower limit sample 1.392g (0.409g, precursor 0.983 g).
(3) 10mL of purified water was added thereto and stirred for 5 min.
(4) 10mL of 1.0mol/L hydrochloric acid (nominal concentration of 1.12283mol/L) was added thereto, and stirring was continued for 1 min.
(5) The pH of the solution was measured with a pH meter and the sample was 5.34 with an upper limit of 6.02 and a lower limit of 3.96.
And (3) detection results: the sample is qualified.
And (3) experimental verification:
when the theoretical lithium content is 5.6%, the detection values of the original potentiometric titration method and the detection method are compared by measuring the content of lithium carbonate in the same sample. The results of the experiment are shown in the following table:
from the above data, the more the actual value is lower than the theoretical value, the smaller the pH value is; when the actual lithium content is very close to the theoretical lithium content of 5.6%, the pH value is about 5.4; when the actual lithium content is below about 0.1% of theoretical, the pH is around 4.0. The difference between the samples is obvious, so when the theoretical value is 5.6%, the experiment can judge whether the actual lithium content of the sample exceeds the upper limit and the lower limit of the theoretical value, better reflects the difference between a qualified sample and an unqualified sample, and can be used for semi-quantitative test of a lithium carbonate sample in a primary material mixing process.
The foregoing is considered as illustrative of the preferred embodiments of the invention and is not to be construed as limiting the invention in any way. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (7)
1. A semi-quantitative detection method for lithium content in a primary mixed material sample of a ternary cathode material is characterized by comprising the following steps:
1) calculating sample weighing according to the theoretical lithium content of a primary mixed sample given in the production process and the following formula, and weighing the primary mixed sample to a first container;
wherein: m is sample weighing amount and g;
c-acid nominal concentration, mol/L;
v-acid addition volume, mL;
MLi-Li element molar mass, 6.941 g/mol;
w-theoretical lithium content of the sample,% (wt);
2) respectively weighing upper and lower limit samples to a second container and a third container, wherein the sample weighing amounts of lithium raw materials and precursors in the upper and lower limit samples accord with the following formula:
m 2 =m−m 1
wherein: m is1Weighing the sample amount of the lithium raw material, and g;
m2-weighing the precursor, g;
∆w-upper or lower lithium content specification tolerance limits,% (wt);
wLi-test lithium content,% (wt) in lithium feedstock;
3) respectively adding water into the first container, the second container and the third container, stirring uniformly, then respectively adding acid with the calibration concentration of c and the volume of V, and stirring for reaction;
4) and respectively testing the pH value of the solution, and judging the sample to be a suspected unqualified sample when the pH value of the sample exceeds the pH values of the upper limit sample and the lower limit sample.
2. The semi-quantitative detection method for lithium content in the primary mixed material sample of the ternary cathode material according to claim 1, characterized in that the acid is monoacid.
3. The semi-quantitative detection method for lithium content in the primary mixed material sample of the ternary cathode material according to claim 2, characterized in that the acid is hydrochloric acid.
4. The semi-quantitative detection method for the lithium content in the primary mixed material sample of the ternary cathode material according to claim 1, characterized in that the lithium raw material is lithium carbonate or lithium hydroxide.
5. The semi-quantitative detection method for lithium content in a primary mixed material sample of a ternary cathode material according to claim 1, characterized in that the precursor is nickel cobalt manganese hydroxide or nickel cobalt aluminum hydroxide.
6. The semi-quantitative detection method for the lithium content in the primary mixed material sample of the ternary cathode material according to claim 1, characterized in that the upper and lower limit samples in step 2) need to be re-prepared when a reagent or a measuring tool is replaced.
7. The semi-quantitative detection method for the lithium content in the ternary cathode material primary mixed material sample according to claim 1, characterized in that if the sample is judged to be suspected to be unqualified in step 4), whether the sample is qualified or not is further confirmed by a quantitative test method.
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