CN107907625A - A kind of detection method of lithium electricity tertiary cathode material surface residual alkali content - Google Patents
A kind of detection method of lithium electricity tertiary cathode material surface residual alkali content Download PDFInfo
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Abstract
The invention discloses a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content, carries out the washing of certain time to ternary material first, takes its filtrate；Secondly according to basic acid base titration principle, corresponding indicator is added, is titrated with standard hydrochloric acid solution；Finally carry out result calculating and data processing.Beneficial effects of the present invention：By using detection method of the present invention, real result is reliable, while can greatly improve detection efficiency, and easy to operate, easy to use.
Description
Technical field
The present invention relates to lithium ion battery to produce Incoming Quality Control technical field, it particularly relates to which a kind of lithium electricity ternary is just
The detection method of pole material surface residual alkali content.
Background technology
Lithium ion battery is as a kind of energy density is high, output voltage is high, cycle performance is excellent, memory-less effect, environment
Friendly electrochmical power source system, with good economic efficiency, social benefit and strategic importance, are widely used in mobile logical
The multiple fields such as news, digital product, electric automobile.The ternary material of narrow sense refers to the violent three components layer of the nickel cobalt of stoichiometric ratio
Shape positive electrode, this kind of material are in the investigation of materials in Singapore A-Star subordinate in 1999 earliest by scholar Liu Zhaolin of Chinese origin
Reported when work with Graduate School of Engineering (IMRE), many seminars all carry out this series of material in the world afterwards
Very careful in-depth study.Ternary material (NMC) combines the advantages of tri- kinds of materials of LiCoO2, LiNiO2 and LiMnO2,
To be better than one-component layered cathode material since there are obvious cooperative effect, the performance of NMC between Ni, Co and Mn, and
It is considered as most to have one of novel anode material of application prospect.
NMC (also including NCA) surface residual alkali comparision contents height is its comparison distinct issues in practical applications.
The alkaline matter main component on NMC surfaces is Li2CO3, is existed in addition with a part in the form of Li2SO4 and LiOH.
The surface residual alkali too high levels of ternary material can bring many negative effects to chemical property.It is that it can shadow first
Coating is rung, NCA and rich nickel ternary material are readily formed g., jelly-like in homogenization process, and main is exactly the alkali because their surfaces
Caused by property oxide content too high water absorption.Influence of the surface alkalinty compound to chemical property is mainly reflected in that add can not
Inverse capacitance loss, while deteriorate cycle performance.
In addition, for NCA and rich nickel ternary material, the Li2CO3 on surface is decomposed under high voltages, is battery flatulence
One of the main reason for, so that the hidden danger in terms of bringing security.Therefore, surface residual alkali content is reduced for ternary material dynamic
Practical application in power battery has extremely important meaning.
Therefore, either in the research and development and production of positive electrode or in the follow-up application stage, it is necessary to stringent control
The residual alkali content of material surface, and the detection to residual alkali is then an element task, it is essential.The detection of residual alkali content is main
According to most basic soda acid chemistry titration, but since standard in the industry does not form unification, each details of operation is caused to have differences, material
Material producer and application side cannot approve result mutually, influence manufacturing schedule.
The content of the invention
For the above-mentioned technical problem in correlation technique, the present invention proposes that a kind of lithium electricity tertiary cathode material surface is residual
The detection method of alkali content, can overcome the above-mentioned deficiency of the prior art.
To realize above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
A kind of detection method of lithium electricity tertiary cathode material surface residual alkali content, includes the following steps：
S1：The washing of certain time is carried out to ternary material, takes its filtrate；
S2：According to basic acid base titration principle, corresponding indicator is added, is titrated with standard hydrochloric acid solution, is had
Body step includes as follows：
S2.1：Demarcate the preparation of indicator, the ethanol solution and 2g/L of the bromocresol green that the calibration indicator is 1g/L
Methyl red ethanol solution press 3：1 volume ratio is mixed to prepare；
S2.2：The preparation of standard hydrochloric acid solution；
S2.3：The calibration of standard hydrochloric acid solution；
S2.4：The calibrated concentration of calculating standard hydrochloric acid solution；
S2.5：The preparation of titrate indicator, the titrate indicator are cresol red ethanol solution, the methyl of 1g/L of 1g/L
Red ethanol solution and the aqueous solution of methylene blue of 2g/L press 4：5：1 volume ratio is uniformly mixed to prepare；
S2.6：Alkali content titrates；
S3：As a result calculating and data processing.
Further, in step sl, the time of the washing is 5min.
Further, in step S2.1, the calibration specific preparation steps of indicator are：
S2.1.1：Take 0.1g bromocresol greens to be dissolved in 95% ethanol, and be diluted to 100mL with 95% ethanol and obtain solution I；
S2.1.2：Take 0.2g methyl reds to be dissolved in 95% ethanol, and be diluted to 100mL with 95% ethanol and obtain solution II；
S2.1.3：30mL solution Is are taken, 10mL solution IIs, are uniformly mixed.
Further, in step S2.2, the preparation steps of the standard hydrochloric acid solution are：9mL top grade pure hydrochloric acids are measured,
It is settled in 1000mL water, shakes up.
Further, in step S2.3, the specific steps of the standard hydrochloric acid solution calibration include：
S2.3.1：0.2g is weighed in the anhydrous Na of 270-300 DEG C of calcination to constant weight2CO3, it is dissolved in 50mL pure water；
S2.3.2：Add the calibration indicator described in 10 drops, titrated with the normal hydrochloric acid liquid prepared, Na2CO3Solution by
Green is changed into kermesinus, boils 2min, and it is in kermesinus again to continue to be titrated to solution after cooling, it is parallel three times.
Further, in step S2.4, the formula of the calibrated concentration of calculating standard hydrochloric acid solution is：C (HCl)=
m/V/0.05299；Wherein, C is the calibrated concentration of standard hydrochloric acid solution, and m is anhydrous Na2CO3Quality g, V are hydrochloric acid solution dosage
ML, 0.05299 is the anhydrous Na represented with g suitable with 1.00mL hydrochloric acid standard solutions2CO3Quality.
Further, in step S2.5, the titrate indicator concrete configuration step includes as follows：
S2.5.1：The methylene blue 4mL of the methyl red 20mL, 2g/L of the cresol red 16mL, 1g/L of 1g/L are pipetted, by more than
Three kinds of solution uniformly mix, wherein, cresol red and methyl red are ethanol solution, and methylene blue is aqueous solution.
Further, in step S2.6, the step of alkali content titration, includes：
S2.6.1：20.000g samples are weighed, 100mL tertiary effluents, stirring 5min is moved into and filters, while pipette 60mL extremely
In 250mL conical flasks；
S2.6.2：Add 10 drop titrate indicators and shake up, in purple, titrated with the hydrochloric acid standard solution demarcated, drop
Determine to record V to bright green1, continue to be titrated to a piece red record V2。
Further, in step s3, the result is calculated is with the formula of data processing：
Total alkali content %=C × V2/2/1000×m2/m3/m1×73.89×100；
Li2CO3Content %=C × (V2-V1)/1000×m2/m3/m1×73.89×100；
LiOH contents %=C × (2V1-V2)/1000×m2/m3/m1×23.95×100；
Wherein：C is the calibrated concentration of normal hydrochloric acid liquid；V1For the titer volume of first color transition point consumption；V2For drop
Determine the titer volume of terminal consumption；m1To weigh sample weight；m2To pipette the quality of water；m3For the filtrate of gained after filtering
Quality.
Beneficial effects of the present invention：By using detection method of the present invention, real result is reliable, while can be big
It is big to improve detection efficiency and easy to operate, it is easy to use.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, drawings in the following description are only some implementations of the present invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is a kind of detection method of the lithium electricity tertiary cathode material surface residual alkali content described according to embodiments of the present invention
Flow chart；
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art's all other embodiments obtained, belong to what the present invention protected
Scope.
A kind of as shown in Figure 1, inspection of lithium electricity tertiary cathode material surface residual alkali content according to embodiments of the present invention
Survey method, includes the following steps：
S1：The washing of certain time is carried out to ternary material, takes its filtrate；
S2：According to basic acid base titration principle, corresponding indicator is added, is titrated with standard hydrochloric acid solution, is had
Body step includes as follows：
S2.1：Demarcate the preparation of indicator, the ethanol solution and 2g/L of the bromocresol green that the calibration indicator is 1g/L
Methyl red ethanol solution press 3：1 volume ratio is mixed to prepare；
S2.2：The preparation of standard hydrochloric acid solution；
S2.3：The calibration of standard hydrochloric acid solution；
S2.4：The calibrated concentration of calculating standard hydrochloric acid solution；
S2.5：The preparation of titrate indicator, the titrate indicator are cresol red ethanol solution, the methyl of 1g/L of 1g/L
Red ethanol solution and the aqueous solution of methylene blue of 2g/L press 4：5：1 volume ratio is uniformly mixed to prepare；
S2.6：Alkali content titrates；
S3：As a result calculating and data processing.
In one embodiment, in step sl, the time of the washing is 5min.
In one embodiment, in step S2.1, the calibration specific preparation steps of indicator are：
S2.1.1：Take 0.1g bromocresol greens to be dissolved in 95% ethanol, and be diluted to 100mL with 95% ethanol and obtain solution I；
S2.1.2：Take 0.2g methyl reds to be dissolved in 95% ethanol, and be diluted to 100mL with 95% ethanol and obtain solution II；
S2.1.3：30mL solution Is are taken, 10mL solution IIs, are uniformly mixed.
In one embodiment, in step S2.2, the preparation steps of the standard hydrochloric acid solution are：It is excellent to measure 9mL
Level pure hydrochloric acid, is settled in 1000mL water, shakes up.
In one embodiment, in step S2.3, the specific steps of the standard hydrochloric acid solution calibration include：
S2.3.1：0.2g is weighed in the anhydrous Na of 270-300 DEG C of calcination to constant weight2CO3, it is dissolved in 50mL pure water；
S2.3.2：Add the calibration indicator described in 10 drops, titrated with the normal hydrochloric acid liquid prepared, Na2CO3Solution by
Green is changed into kermesinus, boils 2min, and it is in kermesinus again to continue to be titrated to solution after cooling, it is parallel three times.
In one embodiment, in step S2.4, the formula of the calibrated concentration of calculating standard hydrochloric acid solution is：
C (HCl)=m/V/0.05299；Wherein, C is the calibrated concentration of standard hydrochloric acid solution, and m is anhydrous Na2CO3Quality g, V are hydrochloric acid
Solution usage mL, 0.05299 is the anhydrous Na represented with g suitable with 1.00mL hydrochloric acid standard solutions2CO3Quality.
In one embodiment, in step S2.5, the titrate indicator concrete configuration step includes as follows：
S2.5.1：The methylene blue 4mL of the methyl red 20mL, 2g/L of the cresol red 16mL, 1g/L of 1g/L are pipetted, by more than
Three kinds of solution uniformly mix, wherein, cresol red and methyl red are ethanol solution, and methylene blue is aqueous solution.
In one embodiment, in step S2.6, the step of alkali content titration, includes：
S2.6.1：20.000g samples are weighed, 100mL tertiary effluents, stirring 5min is moved into and filters, while pipette 60mL extremely
In 250mL conical flasks；
S2.6.2：Add 10 drop titrate indicators and shake up, in purple, titrated with the hydrochloric acid standard solution demarcated, drop
Determine to record V to bright green1, continue to be titrated to a piece red record V2。
In one embodiment, in step s3, the result is calculated is with the formula of data processing：
Total alkali content %=C × V2/2/1000×m2/m3/m1×73.89×100；
Li2CO3Content %=C × (V2-V1)/1000×m2/m3/m1×73.89×100；
LiOH contents %=C × (2V1-V2)/1000×m2/m3/m1×23.95×100；
Wherein：C is the calibrated concentration of normal hydrochloric acid liquid；V1For the titer volume of first color transition point consumption；V2For drop
Determine the titer volume of terminal consumption；m1To weigh sample weight；m2To pipette the quality of water；m3For the filtrate of gained after filtering
Quality.
In order to facilitate understand the present invention above-mentioned technical proposal, below by way of in specifically used mode to the present invention it is above-mentioned
Technical solution is described in detail.
When specifically used, the present invention carries out ternary material in the water of certain time according to basic acid base titration principle
Wash, take its filtrate, using corresponding indicator, titrated with standard hydrochloric acid solution.Wherein, washing time is set to 5min；Mark
The ethanol for calibrating the ethanol solution for the bromocresol green that the indicator applied during quasi- hydrochloric acid solution is 1g/L and the methyl red of 2g/L is molten
Liquid presses 3：1 ratio mixing；The indicator that alkali content is applied when titrating is cresol red ethanol solution, the methyl red of 1g/L of 1g/L
Ethanol solution and 2g/L aqueous solution of methylene blue press 4：5：1 ratio mixing.
Specifically, first, the preparation and calibration of carry out standard hydrochloric acid solution of the present invention：Calibration indicator is prepared first, is taken
0.1g bromocresol greens are dissolved in 95% ethanol, and are diluted to 100mL with 95% ethanol and obtain solution I, take 0.2g methyl reds to be dissolved in 95%
Ethanol, and 100mL solution IIs are diluted to 95% ethanol, 30mL solution Is are taken, 10mL solution IIs, are uniformly mixed；Then mark is prepared
Quasi- hydrochloric acid solution, specially measures 9mL top grade pure hydrochloric acids, is settled in 1000mL water, shakes up；Secondly, to standard hydrochloric acid solution
Demarcated, specific method is：0.2g (being accurate to 0.0001g) is weighed in the anhydrous of 270-300 DEG C of calcination to constant weight (3h)
Na2CO3, be dissolved in 50mL pure water, add 10 drops demarcate (bromocresol green-methyl red) indicator, with the standard hydrochloric acid solution prepared into
Row titration, Na2CO3Solution is changed into kermesinus from green, boils 2min, and it is in kermesinus (0.5 again to continue to be titrated to solution after cooling
Drop -1 drop), it is parallel three times；The calibrated concentration of standard hydrochloric acid solution is finally calculated, formula is：C (HCl)=m/V/0.05299, its
In：M is anhydrous Na2CO3Quality g, V are hydrochloric acid solution dosage mL, and 0.05299 is and 1.00mL hydrochloric acid standard solution (concentration
1.000mol/L) the suitable anhydrous Na represented with g2CO3Quality.
Secondly, the test of total alkali content, configures titrate indicator (cresol red-methyl red-methylene blue indicator), tool first
Body is the methylene blue 4mL of the methyl red 20mL, 2g/L of the cresol red 16mL, 1g/L that pipette 1g/L, and three of the above solution is equal
Even mixing, wherein, cresol red and methyl red are ethanol solution, and methylene blue is aqueous solution；Then alkali content titration is carried out：Specifically
To weigh 20.000g samples, moving into 100mL tertiary effluents, stirring 5min and filter, pipette 60mL into 250mL conical flasks, add
Enter 10 drop titrate indicators and shake up, in purple, titrated with the hydrochloric acid standard solution demarcated, be titrated to bright green record V1,
Continue to be titrated to a piece red record V2。
Find that total alkali is in rising trend, and following table is certain as the time for adding water to stir lengthens in conventional practice
The total alkali measured under 622 ternary product difference mixings time.As can be seen from the data：After 20 minutes, as the time increases
Long, total alkali will not be further added by substantially, be because the remaining alkali of material surface is all soluble in water；And stir five minutes
With stirring halfhour gap very little, so selection stirring can greatly improve detection efficiency in five minutes.
Finally carry out result calculating and data processing：Specific formula is as follows：
Total alkali content %=C × V2/2/1000×m2/m3/m1×73.89×100；
Li2CO3Content %=C × (V2-V1)/1000×m2/m3/m1×73.89×100；
LiOH contents %=C × (2V1-V2)/1000×m2/m3/m1×23.95×100；
Wherein：C is the calibrated concentration of normal hydrochloric acid liquid；V1For the titer volume of first color transition point consumption；V2For drop
Determine the titer volume of terminal consumption；m1To weigh sample weight；m2To pipette the quality of water；m3For the filtrate of gained after filtering
Quality.
In conclusion by using detection method of the present invention, real result is reliable, while can greatly improve inspection
Efficiency is surveyed, and it is easy to operate, it is easy to use.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention god.
Claims (9)
1. the detection method of a kind of lithium electricity tertiary cathode material surface residual alkali content, it is characterised in that include the following steps：
S1：The washing of certain time is carried out to ternary material, takes its filtrate；
S2：According to basic acid base titration principle, corresponding indicator is added, is titrated with standard hydrochloric acid solution, specific step
Suddenly include as follows：
S2.1：Demarcate the preparation of indicator, the ethanol solution of bromocresol green and the first of 2g/L that the calibration indicator is 1g/L
The red ethanol solution of base presses 3：1 volume ratio is mixed to prepare；
S2.2：The preparation of standard hydrochloric acid solution；
S2.3：The calibration of standard hydrochloric acid solution；
S2.4：The calibrated concentration of calculating standard hydrochloric acid solution；
S2.5：The preparation of titrate indicator, the titrate indicator are the methyl red of the cresol red ethanol solution of 1g/L, 1g/L
The aqueous solution of methylene blue of ethanol solution and 2g/L press 4：5：1 volume ratio is uniformly mixed to prepare；
S2.6：Alkali content titrates；
S3：As a result calculating and data processing.
2. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step sl, the time of the washing is 5min.
3. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step S2.1, the calibration specific preparation steps of indicator are：
S2.1.1：Take 0.1g bromocresol greens to be dissolved in 95% ethanol, and be diluted to 100mL with 95% ethanol and obtain solution I；
S2.1.2：Take 0.2g methyl reds to be dissolved in 95% ethanol, and be diluted to 100mL with 95% ethanol and obtain solution II；
S2.1.3：30mL solution Is are taken, 10mL solution IIs, are uniformly mixed.
4. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step S2.2, the preparation steps of the standard hydrochloric acid solution are：9mL top grade pure hydrochloric acids are measured, are settled to 1000mL water
In, shake up.
5. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step S2.3, the specific steps of the standard hydrochloric acid solution calibration include：
S2.3.1：0.2g is weighed in the anhydrous Na of 270-300 DEG C of calcination to constant weight2CO3, it is dissolved in 50mL pure water；
S2.3.2：Add the calibration indicator described in 10 drops, titrated with the normal hydrochloric acid liquid prepared, Na2CO3Solution is by green
Be changed into kermesinus, boil 2min, it is in kermesinus again to continue to be titrated to solution after cooling, it is parallel three times.
6. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step S2.4, the formula of the calibrated concentration of calculating standard hydrochloric acid solution is：C(HCl)=m/V/0.05299；Its
In, C is the calibrated concentration of standard hydrochloric acid solution, and m is anhydrous Na2CO3Quality g, V are hydrochloric acid solution dosage mL, 0.05299 be with
The suitable anhydrous Na represented with g of 1.00mL hydrochloric acid standard solutions2CO3Quality.
7. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step S2.5, the titrate indicator concrete configuration step includes as follows：
S2.5.1：The methylene blue 4mL of the methyl red 20mL, 2g/L of the cresol red 16mL, 1g/L of 1g/L are pipetted, by three of the above
Solution uniformly mixes, wherein, cresol red and methyl red are ethanol solution, and methylene blue is aqueous solution.
8. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 1, its feature exist
In in step S2.6, the step of alkali content titration includes：
S2.6.1：20.000g samples are weighed, 100mL tertiary effluents, stirring 5min is moved into and filters, while pipette 60mL to 250mL
In conical flask；
S2.6.2：Add 10 drop titrate indicators and shake up, in purple, titrated, be titrated to the hydrochloric acid standard solution demarcated
Bright green records V1, continue to be titrated to a piece red record V2。
9. a kind of detection method of lithium electricity tertiary cathode material surface residual alkali content according to claim 8, its feature exist
In in step s3, the result is calculated is with the formula of data processing：
Total alkali content %=C × V2/2/1000×m2/m3/m1×73.89×100；
Li2CO3Content %=C × (V2-V1)/1000×m2/m3/m1×73.89×100；
LiOH contents %=C × (2V1- V2)/1000×m2/m3/m1×23.95×100；
Wherein：C is the calibrated concentration of normal hydrochloric acid liquid；V1For the titer volume of first color transition point consumption；V2For titration eventually
Select the titer volume of consumption；m1To weigh sample weight；m2To pipette the quality of water；m3For the filtrate quality of gained after filtering.
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| 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 |
| CN111289686A (en) * | 2020-03-06 | 2020-06-16 | 凤阳泰和九思科技有限公司 | Method for measuring content of residual alkali in solution and application thereof |
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| CN109856315A (en) * | 2018-12-17 | 2019-06-07 | 刘洪河 | The detection method of free amine content in a kind of NMP |
| 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 |
| CN111289686A (en) * | 2020-03-06 | 2020-06-16 | 凤阳泰和九思科技有限公司 | Method for measuring content of residual alkali in solution and application thereof |
| CN111948335A (en) * | 2020-06-29 | 2020-11-17 | 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 |
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| CN113702473A (en) * | 2021-08-26 | 2021-11-26 | 中国科学院青岛生物能源与过程研究所 | Method for measuring alkalinity of surfactant based on potentiometric titration method |
| CN117074398A (en) * | 2023-10-12 | 2023-11-17 | 天津力神电池股份有限公司 | Pre-lithiated material effectiveness detection method and pole piece pre-lithiated material detection method |
| CN117074398B (en) * | 2023-10-12 | 2024-01-12 | 天津力神电池股份有限公司 | Pre-lithiated material effectiveness detection method and pole piece pre-lithiated material detection method |
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