CN108181428A - A kind of detection method of boracic tertiary cathode material remnants alkali contents - Google Patents
A kind of detection method of boracic tertiary cathode material remnants alkali contents Download PDFInfo
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- CN108181428A CN108181428A CN201711468354.9A CN201711468354A CN108181428A CN 108181428 A CN108181428 A CN 108181428A CN 201711468354 A CN201711468354 A CN 201711468354A CN 108181428 A CN108181428 A CN 108181428A
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- 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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Abstract
The invention discloses a kind of detection methods of boracic tertiary cathode material remnants alkali contents, this method shelters borate with mannitol, barium chloride shelters the principle of carbonate, a kind of stepwise titration method is employed, so as to the content of Accurate Determining causticity lithium and lithium carbonate, not only fully considers the influence that borate detects alkali content, and suitable for the system of a variety of salt of root containing weak acid, this method is simple and easy to do, and test result accuracy is high, suitable for enterprise practical application demand.
Description
Technical field
The present invention relates to the detection technique field of anode material for lithium-ion batteries, specially a kind of boracic tertiary cathode material
The detection method of remaining alkali content.
Background technology
Tertiary cathode material(Nickle cobalt lithium manganate)Relatively low with cost, specific capacity is higher, and raw material sources relative abundance etc. is excellent
Gesture is currently the important positive electrode of lithium ion battery.In the actual production process, the additional proportion of lithium can be slightly improved during dispensing
It is lost to make up the lithium in sintering process, leading to tertiary cathode material surface, there are a certain amount of however, residual bases(Predominantly causticity lithium
And lithium carbonate), have harmful effect to the processing performance, high-temperature behavior and security performance of electrode, remaining alkali content is had become as ternary
One of important indicator of positive electrode.
In order to improve ternary material performance, boron element is added when usually coating or adulterate(Boron oxide, boric acid), it is sintering finished
In mainly with lithium borate mLi2O·nB2O3Form exist.
At present, the detection method of tertiary cathode material remnants alkali contents is mainly acid-base titration, and this method is first by three
First material sample and water prepare solution to be measured, severe in First terminal point PH=8.2 by standard hydrochloric acid solution progress acid-base titration
Property lithium is all neutralized, and lithium carbonate is only neutralized to LiHCO3, the second terminal PH=4 ~ 5, lithium bicarbonate all neutralized, so as to
The content of causticity lithium and lithium carbonate is calculated respectively.This method is not directed to influence of the borate to titration results, leads to however, residual base
There are large errors for the measure of content.
Invention content
The purpose of the present invention is to provide a kind of detection method of boracic tertiary cathode material remnants alkali contents, in solution
State the problem of being proposed in background technology.
To achieve the above object, the present invention provides following technical solution:A kind of boracic tertiary cathode material remnants alkali contents
Detection method, include the following steps:
1)Tertiary cathode material sample m is weighed, deionized water is added to stir, whole filtrates are taken after filtering;
2)Filtrate is divided into two equal portions m1、m2, as solution to be measured, acid base titration is carried out by automatical potentiometric titrimeter;
3)Solution m to be measured1It is middle to add in excessive mannitol and barium chloride, it is titrated to the first end point of the sudden change pH about with standard hydrochloric acid solution
It is 8 ~ 9, record hydrochloric acid consumption volume V1;
4)Solution m to be measured2Middle to add in excessive mannitol, it is about 8 ~ 9 to be titrated to the first end point of the sudden change pH with standard hydrochloric acid solution, note
Record hydrochloric acid consumption volume V2;
5)Use formula(1)Calculate the content of LiOH in sample:
Formula(1)In, ω1For the contents of LiOH in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;V1For
LiOH consumes the volume of hydrochloric acid, unit mL;M is sample quality, unit g;m1For the quality of filtrate 1, unit g;m2For
The quality of filtrate 2, unit g;
6)Use formula(2)Calculate Li in sample2CO3Content:
Formula(2)In, ω2For Li2CO3Content in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;(V2-
V1)For Li2CO3It is transformed into LiHCO3The volume of consumed hydrochloric acid, unit mL;M is sample quality, unit g;m1For filtrate 1
Quality, unit g;m2For the quality of filtrate 2, unit g.
Preferably, the step 1)In, the mass ratio of tertiary cathode material sample and deionized water is(5-30):100.
Preferably, the step 1)In, it is described to stir as magnetic agitation, time 5-30min.
Preferably, the step 1)In, described be filtered into is filtered by vacuum using neutral filter paper or miillpore filter.
Preferably, the step 3), step 4)In, a concentration of 0.1mol/L of standard hydrochloric acid solution.
Preferably, the step 3), step 4)In, mannitol 0.2 ~ 1g of addition, 0.2 ~ 1g of barium chloride addition.
Preferably, the step 3), step 4)In, the first end point of the sudden change of automatical potentiometric titrimeter pH is about 8-9.
Compared with prior art, the beneficial effects of the invention are as follows:Tertiary cathode material remnants alkali contents provided by the invention
Detection method, the content of causticity lithium and lithium carbonate can be obtained, sheltered influence of the borate to testing result in material, to be excellent
Change tertiary cathode material generation technique and data support is provided.The test method is easy to operate, and accuracy is high, meets the quick of enterprise
Detection demand, convenient for the monitoring in actual production.
Specific embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel all other embodiments obtained without making creative work belong to the model that the present invention protects
It encloses.
Embodiment one:
The present invention provides following technical solution:A kind of detection method of boracic tertiary cathode material remnants alkali contents, contains 111 types
Boron tertiary cathode material however, residual base is measured, and is included the following steps:
1)Tertiary cathode material sample 10g is weighed, 200mL deionized waters is added to stir 5min, vacuum pumping is carried out using neutral filter paper
Whole filtrates are taken after filter;
2)Filtrate is divided into two equal portions m1、m2, as solution to be measured, acid base titration is carried out by automatical potentiometric titrimeter;
3)Solution m to be measured1Middle addition 0.2g mannitol and 0.2g barium chlorides, first is titrated to 0.1mol/L standard hydrochloric acid solutions
End point of the sudden change, record hydrochloric acid consumption volume V1;
4)Solution m to be measured2Middle addition 0.2g mannitol, is titrated to the first end point of the sudden change with 0.1mol/L standard hydrochloric acid solutions, remembers
Record hydrochloric acid consumption volume V2;
5)Use formula(1)Calculate the content of LiOH in sample:
Formula(1)In, ω1For the contents of LiOH in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;V1For
LiOH consumes the volume of hydrochloric acid, unit mL;M is sample quality, unit g;m1For the quality of filtrate 1, unit g;m2For
The quality of filtrate 2, unit g;
6)Use formula(2)Calculate Li in sample2CO3Content:
Formula(2)In, ω2For Li2CO3Content in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;(V2-
V1)For Li2CO3It is transformed into LiHCO3The volume of consumed hydrochloric acid, unit mL;M is sample quality, unit g;m1For filtrate 1
Quality, unit g;m2For the quality of filtrate 2, unit g.
Pass through formula(1)And formula(2)LiOH contents are calculated respectively as 0.0378%, Li2CO3Content is 0.0280%.
Embodiment two:
A kind of detection method of boracic tertiary cathode material remnants alkali contents, to 622 type boracic tertiary cathode material however, residual bases into
Row measures, and includes the following steps:
1)Tertiary cathode material sample 10g is weighed, 200mL deionized waters is added to stir 30min, vacuum pumping is carried out using miillpore filter
Whole filtrates are taken after filter;
2)Filtrate is divided into two equal portions m1、m2, as solution to be measured, acid base titration is carried out by automatical potentiometric titrimeter;
3)Solution m to be measured1Middle addition 0.5g mannitol and 0.5g barium chlorides, first is titrated to 0.1mol/L standard hydrochloric acid solutions
End point of the sudden change, record hydrochloric acid consumption volume V1;
4)Solution m to be measured2Middle addition 0.5g mannitol, is titrated to the first end point of the sudden change with 0.1mol/L standard hydrochloric acid solutions, remembers
Record hydrochloric acid consumption volume V2;
5)Use formula(1)Calculate the content of LiOH in sample:
Formula(1)In, ω1For the contents of LiOH in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;V1For
LiOH consumes the volume of hydrochloric acid, unit mL;M is sample quality, unit g;m1For the quality of filtrate 1, unit g;m2For
The quality of filtrate 2, unit g;
6)Use formula(2)Calculate Li in sample2CO3Content:
Formula(2)In, ω2For Li2CO3Content in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;(V2-
V1)For Li2CO3It is transformed into LiHCO3The volume of consumed hydrochloric acid, unit mL;M is sample quality, unit g;m1For filtrate 1
Quality, unit g;m2For the quality of filtrate 2, unit g.
Pass through formula(1)And formula(2)LiOH contents are calculated respectively as 0.1583%, Li2CO3Content is 0.1895%.
Comparative example 1
Comparative example uses conventional acid-base titration method, and the however, residual base of 111 type boracic tertiary cathode materials is measured, operation step
Suddenly it is:Sample 5.00g is weighed in 250mL beakers, adds in 100mL deionized waters, stirs 5min, suction filtration takes whole filtrates, makes
Acid-base titration is carried out on automatical potentiometric titrimeter with the standard hydrochloric acid solution of 0.1mol/L, records first, second end point of the sudden change
Consumed hydrochloric acid volume, so as to calculate the content of causticity lithium and lithium carbonate respectively.
Comparative example 2
This comparative example is measured the however, residual base of 622 type boracic tertiary cathode materials, and operating procedure is:Weigh sample 5.00g
In 250mL beakers, 100mL deionized waters are added in, stir 30min, suction filtration takes whole filtrates, uses the standard salt of 0.1mol/L
Acid solution carries out acid-base titration on automatical potentiometric titrimeter, and first, second end point of the sudden change of record consumes hydrochloric acid volume, so as to
The content of causticity lithium and lithium carbonate is calculated respectively.
Embodiment and comparative example is to 111 types and 622 type boracic tertiary cathode material however, residual base content detection result such as following tables
It is shown.
The present inventor passes through the study found that lithium borate mLi2O·nB2O3Belong to weak acid root salt, H is hydrolyzed to when being dissolved in water3BO3
And OH-, because of H3BO3With HCO3 -Dissociation constant it is close, during using conventional direct titration method, lithium borate also can be in First terminal point
It is neutralized;The polyhydroxy-alcohols such as mannitol or glycerine are added, are complexed with borate, complexing acid strength is more than HCO3 -, but with
H2CO3Dissociation constant approach, the second terminal of conventional titration method forms complex acid.Therefore, the present invention devises a kind of substep
Titration method, a solution addition mannitol and barium chloride, shelter borate and carbonate, First terminal point only neutralize OH-, it is another
Part solution only adds mannitol, shelters borate, in First terminal point and OH-With CO3 2-, so as to accurately obtain causticity lithium and
The content of lithium carbonate.
Meanwhile alkali content substep detection method of the invention, because titration end-point is pH8-9, avoid weak in acid condition
The neutralization of acid group, detection when being also applied in this way in material containing other weak acid root salt, such as fluoride salt, oxalates, Asia
Phosphate etc..
The detection method of tertiary cathode material remnants alkali contents provided by the invention can obtain containing for causticity lithium and lithium carbonate
Amount, has sheltered influence of the borate to testing result in material, and providing data for optimization tertiary cathode material generation technique supports.
The test method is easy to operate, and accuracy is high, meets the quick detection demand of enterprise, convenient for the monitoring in actual production.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of detection method of boracic tertiary cathode material remnants alkali contents, it is characterised in that:Include the following steps:
1)Tertiary cathode material sample m is weighed, deionized water is added to stir, whole filtrates are taken after filtering;
2)Filtrate is divided into two equal portions m1、m2, as solution to be measured, acid base titration is carried out by automatical potentiometric titrimeter;
3)Solution m to be measured1It is middle to add in excessive mannitol and barium chloride, it is titrated to the first end point of the sudden change pH about with standard hydrochloric acid solution
It is 8 ~ 9, record hydrochloric acid consumption volume V1;
4)Solution m to be measured2Middle to add in excessive mannitol, it is about 8 ~ 9 to be titrated to the first end point of the sudden change pH with standard hydrochloric acid solution, note
Record hydrochloric acid consumption volume V2;
5)Use formula(1)Calculate the content of LiOH in sample:
Formula(1)In, ω1For the contents of LiOH in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;V1For
LiOH consumes the volume of hydrochloric acid, unit mL;M is sample quality, unit g;m1For the quality of filtrate 1, unit g;m2For
The quality of filtrate 2, unit g;
6)Use formula(2)Calculate Li in sample2CO3Content:
Formula(2)In, ω2For Li2CO3Content in the sample;Concentration of the C for standard hydrochloric acid solution, unit mol/L;(V2-
V1)For Li2CO3It is transformed into LiHCO3The volume of consumed hydrochloric acid, unit mL;M is sample quality, unit g;m1For filtrate 1
Quality, unit g;m2For the quality of filtrate 2, unit g.
2. a kind of detection method of boracic tertiary cathode material remnants alkali contents according to claim 1, it is characterised in that:
The step 1)In, the mass ratio of tertiary cathode material sample and deionized water is(5-30):100.
3. a kind of detection method of boracic tertiary cathode material remnants alkali contents according to claim 1, it is characterised in that:
The step 1)In, it is described to stir as magnetic agitation, time 5-30min.
4. a kind of detection method of boracic tertiary cathode material remnants alkali contents according to claim 1, it is characterised in that:
The step 1)In, described be filtered into is filtered by vacuum using neutral filter paper or miillpore filter.
5. a kind of detection method of boracic tertiary cathode material remnants alkali contents according to claim 1, it is characterised in that:
The step 3), step 4)In, a concentration of 0.1mol/L of standard hydrochloric acid solution.
6. a kind of detection method of boracic tertiary cathode material remnants alkali contents according to claim 1, it is characterised in that:
The step 3), step 4)In, mannitol 0.2 ~ 1g of addition, 0.2 ~ 1g of barium chloride addition.
7. a kind of detection method of boracic tertiary cathode material remnants alkali contents according to claim 1, it is characterised in that:
The step 3), step 4)In, the first end point of the sudden change of automatical potentiometric titrimeter pH is about 8-9.
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Cited By (8)
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CN108362824A (en) * | 2018-01-16 | 2018-08-03 | 中蓝长化工程科技有限公司 | The assay method of carbonate and bicarbonate radical in a kind of containing borate brine |
CN108896618A (en) * | 2018-06-28 | 2018-11-27 | 桑顿新能源科技有限公司 | A kind of method and application of the variation of detection anode slice of lithium ion battery residual alkali |
CN109781929A (en) * | 2019-02-12 | 2019-05-21 | 合肥国轩高科动力能源有限公司 | Measure LiOH and CO in lithium hydroxide32-The potentiometric titration 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 |
CN110320315A (en) * | 2019-07-29 | 2019-10-11 | 株洲升华科技有限公司 | The residual alkali detection method of content of tertiary cathode material and its application |
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 |
CN112881589A (en) * | 2021-03-12 | 2021-06-01 | 江西云威新材料有限公司 | Method for detecting carbonate ion content in lithium hydroxide monohydrate |
CN113376316A (en) * | 2021-04-09 | 2021-09-10 | 万向一二三股份公司 | Method for detecting content of residual lithium carbonate in high-nickel ternary positive electrode material |
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CN108362824A (en) * | 2018-01-16 | 2018-08-03 | 中蓝长化工程科技有限公司 | The assay method of carbonate and bicarbonate radical in a kind of containing borate brine |
CN108362824B (en) * | 2018-01-16 | 2020-07-14 | 中蓝长化工程科技有限公司 | Method for determining carbonate radical and bicarbonate radical in borate-containing brine |
CN108896618A (en) * | 2018-06-28 | 2018-11-27 | 桑顿新能源科技有限公司 | A kind of method and application of the variation of detection anode slice of lithium ion battery residual alkali |
CN109781929A (en) * | 2019-02-12 | 2019-05-21 | 合肥国轩高科动力能源有限公司 | Measure LiOH and CO in lithium hydroxide32-The potentiometric titration 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 |
CN110320315A (en) * | 2019-07-29 | 2019-10-11 | 株洲升华科技有限公司 | The residual alkali detection method of content of tertiary cathode material and its application |
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 |
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 |
CN112881589A (en) * | 2021-03-12 | 2021-06-01 | 江西云威新材料有限公司 | Method for detecting carbonate ion content in lithium hydroxide monohydrate |
CN113376316A (en) * | 2021-04-09 | 2021-09-10 | 万向一二三股份公司 | Method for detecting content of residual lithium carbonate in high-nickel ternary positive electrode material |
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