CN110068567A - The method for testing the method for cobalt content in manganese containing materials, testing the method for electrode quality and testing battery quality - Google Patents
The method for testing the method for cobalt content in manganese containing materials, testing the method for electrode quality and testing battery quality Download PDFInfo
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- CN110068567A CN110068567A CN201910266449.5A CN201910266449A CN110068567A CN 110068567 A CN110068567 A CN 110068567A CN 201910266449 A CN201910266449 A CN 201910266449A CN 110068567 A CN110068567 A CN 110068567A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
Abstract
The present invention provides the methods of cobalt content, the method tested the method for electrode quality and test battery quality in test manganese containing materials.The method of cobalt content includes: to dissolve the manganese containing materials in the test manganese containing materials, obtains the first mixture；Nitric acid-potassium chlorate saturated solution is added into first mixture, obtains the second mixture；Second mixture is filtered processing, obtains filtrate to be measured and precipitating to be measured；The first cobalt content in the filtrate to be measured is tested using potentiometric titration；The second cobalt content in the precipitating to be measured is tested using inductively coupled plasma emission spectrography；First cobalt content is added with second cobalt content, to obtain the cobalt content in the manganese containing materials.This method is simple, convenient, easy to accomplish, is easy to industrialization, and the accuracy for testing cobalt content is high, precision is high.
Description
Technical field
The present invention relates to material chemistry technical fields, and in particular, to the method for cobalt content, test in test manganese containing materials
The method of the method and test battery quality of electrode quality.
Background technique
Currently, in the ternary material for being used to prepare battery, other elements in cobalt element and the ternary material (such as
Nickel, manganese etc.) having a very big impact with comparing ternary material and be assembled into the later chemical property of battery between content, therefore
After ternary material preparation is completed, it is necessary to accurately analyze the cobalt content in the ternary material.However, due to being used to prepare battery
Ternary material in can generally also contain manganese element, and the Accurate Determining of cobalt content is always in the related technology urgently in manganese containing materials
One of technical problem to be solved, namely in the related art, still can not accurately test the cobalt content in manganese containing materials.
Thus, the relevant technologies of cobalt content still have much room for improvement in existing test manganese containing materials.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose be to propose it is a kind of it is simple, convenient, easy to accomplish, be easy to industrialization, test cobalt content accuracy it is high or
The method of cobalt content in the high test manganese containing materials of person's precision.
In one aspect of the invention, the present invention provides a kind of methods of cobalt content in test manganese containing materials.According to this
The embodiment of invention obtains the first mixture this method comprises: the manganese containing materials are dissolved；Into first mixture
Nitric acid-potassium chlorate saturated solution is added, obtains the second mixture；Second mixture is filtered processing, is obtained to be measured
Filtrate and precipitating to be measured；The first cobalt content in the filtrate to be measured is tested using potentiometric titration；Using inductive coupling etc. from
Daughter emission spectrometry tests the second cobalt content in the precipitating to be measured；By first cobalt content and second cobalt content
It is added, to obtain the cobalt content in the manganese containing materials.Inventors have found that this method is simple, convenient, it is easy to accomplish,
It is easy to industrialization, and the accuracy for testing cobalt content is high, precision is high.
According to an embodiment of the invention, be added into first mixture nitric acid-potassium chlorate saturated solution it
Before, this method further include: metal ion is added in the first mixture of Xiang Suoshu.
According to an embodiment of the invention, the metal ion includes Fe3+And Zn2+At least one of.
According to an embodiment of the invention, the metal ion is Zn2+。
According to an embodiment of the invention, second cobalt content is not higher than the 7.1% of the cobalt content.
According to an embodiment of the invention, be added into first mixture nitric acid-potassium chlorate saturated solution it
Before, this method further include: first mixture is evaporated processing.
According to an embodiment of the invention, it is 1mL~5mL that first mixture, which is evaporated processing to volume,.
According to an embodiment of the invention, it is 1mL~2mL that first mixture, which is evaporated processing to volume,.
According to an embodiment of the invention, when the manganese content in the manganese containing materials is 12mg~20mg, Xiang Suoshu first
It is 40mL~50mL that nitric acid-potassium chlorate saturated solution volume is added in mixture.
According to an embodiment of the invention, before second mixture is filtered processing, this method further include: by institute
The second mixture is stated to be heated.
According to an embodiment of the invention, the temperature of the heat treatment is 340 DEG C~400 DEG C.
According to an embodiment of the invention, the temperature of the heat treatment is 340 DEG C~380 DEG C.
According to an embodiment of the invention, the time of the heat treatment is 8min~12min.
According to an embodiment of the invention, this method meets at least one of the following conditions: recovery of standard addition be 99.7%~
101.1%；When the manganese content in the manganese containing materials is 12mg~20mg, relative standard deviation is not more than 0.64%.
According to an embodiment of the invention, when the manganese content in the manganese containing materials is 12mg~20mg, this method comprises:
Under conditions of 150 DEG C~250 DEG C, the manganese containing materials are dissolved with concentrated hydrochloric acid and hydrogen peroxide, it is mixed to obtain described first
Close object；The solution of zinc sulfate that the quality containing zinc is 100mg is added into first mixture；By first mixture into
Row evaporation process to volume is 1mL~2mL；Nitric acid-potassium chlorate saturation of 40mL~50mL is added into first mixture
Solution obtains the second mixture；Under conditions of 340 DEG C~380 DEG C, by second mixture carry out heat treatment 8min~
12min；Second mixture Jing Guo the heat treatment is filtered processing, obtain the filtrate to be measured and it is described to
Survey precipitating；The first cobalt content in the filtrate to be measured is tested using potentiometric titration；Emitted using inductively coupled plasma body
Spectroscopic methodology tests the second cobalt content in the precipitating to be measured；First cobalt content is added with second cobalt content, with
Just the cobalt content in the manganese containing materials is obtained.
According to an embodiment of the invention, the manganese containing materials are nickel-cobalt-manganese ternary material.
In another aspect of the invention, the present invention provides a kind of methods for testing electrode quality.It is according to the present invention
Embodiment, the electrode include mentioned-above manganese containing materials, and the method includes being contained using mentioned-above method to described
The step of cobalt content in manganese material is tested.Inventors have found that this method is simple, convenient, and it is easy to accomplish, it is easy to produce
Industry, and can preferably test the chemical property of electrode.
In an additional aspect of the present invention, the present invention provides a kind of methods for testing battery quality.It is according to the present invention
Embodiment, the battery include mentioned-above electrode, the method includes using previous methods to the quality of the electrode into
The step of row test.Inventors have found that this method is simple, convenient, and it is easy to accomplish, it is easy to industrialization, and can be preferably
Test the chemical property of battery.
Detailed description of the invention
Fig. 1 shows the flow diagram of the method for cobalt content in the test manganese containing materials of one embodiment of the invention.
Fig. 2 shows the flow diagram of the method for cobalt content in the test manganese containing materials of another embodiment of the present invention.
Fig. 3 shows the flow diagram of the method for cobalt content in the test manganese containing materials of another embodiment of the invention.
Fig. 4 shows the flow diagram of the method for cobalt content in the test manganese containing materials of further embodiment of the present invention.
Fig. 5 shows the flow diagram of the method for cobalt content in the test manganese containing materials of further embodiment of the present invention.
Specific embodiment
The embodiment of the present invention is described below in detail.The embodiments described below is exemplary, and is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Particular technique or condition are not specified in embodiment, according to text in the art
It offers described technology or conditions or is carried out according to product description.Reagents or instruments used without specified manufacturer,
For can be with conventional products that are commercially available.
In one aspect of the invention, the present invention provides a kind of methods of cobalt content in test manganese containing materials.According to this
The embodiment of invention, referring to Fig.1, method includes the following steps:
S100: the manganese containing materials are dissolved, and obtain the first mixture.
According to an embodiment of the invention, in the first mixture obtained after the manganese containing materials of preset quality are dissolved,
Containing manganese ion and cobalt ions, it can be of course be appreciated by those skilled in the art that being also possible to contain other gold in the first mixture
Belong to ion, no longer excessively repeats herein.
According to an embodiment of the invention, the concrete technology condition that the manganese containing materials dissolve is not particularly limited, as long as
It meets the requirements, those skilled in the art can carry out flexible choice according to actual needs.
According to an embodiment of the invention, the temperature that the manganese containing materials dissolve can be 150 DEG C~250 DEG C, specifically,
It can be 150 DEG C, 180 DEG C, 200 DEG C, 220 DEG C or 250 DEG C etc..The temperature that the manganese containing materials dissolve more is closed as a result,
It is suitable, more easily the manganese containing materials are dissolved.
According to an embodiment of the invention, the reagent that the manganese containing materials dissolve can be concentrated hydrochloric acid and hydrogen peroxide, as a result,
Reagent source is extensive, is easy to get, and is easy to preferably dissolve the manganese containing materials, and obtained product is conducive to subsequent answer after dissolution
With.
According to an embodiment of the invention, as previously mentioned, if including concentrated hydrochloric acid by the reagent that the manganese containing materials dissolve,
The chlorine with toxic may be generated in subsequent step, thus after by manganese containing materials dissolution, it can be to institute
It states and sulfuric acid is added in the first mixture and heats, so that remaining hydrochloric acid volatilization in the first mixture, the sulfuric acid can be 1+9
Sulfuric acid (volume ratio of the concentrated sulfuric acid and water is 1:9).Chlorine will not be generated in the next steps as a result, lead to toxic and environment
Pollution.
In a specific embodiment of the invention, the manganese containing materials are dissolved to obtain the first mixture can be specially
It weighs after quantitative manganese containing materials with concentrated hydrochloric acid is added after the wetting of a small amount of water and is added dropwise after hydrogen peroxide dissolves by heating that obtain first mixed
Object is closed, 1+9 sulfuric acid is then added into first mixture, sulfuric acid cigarette is heated to and emits to the greatest extent.Thus, it is possible to preferably will be described
Manganese containing materials are dissolved, and subsequent applications are conducive to.
Nitric acid-potassium chlorate saturated solution is added in S200: Xiang Suoshu first mixture, obtains the second mixture.
According to an embodiment of the invention, after the nitric acid-potassium chlorate saturated solution is added into first mixture,
Nitric acid and potassium chlorate with strong oxidizing property can occur chemical reaction with the manganese ion in the first mixture and generate manganese dioxide,
The manganese dioxide generated exists in the form of precipitating in second mixture.
According to an embodiment of the invention, inventor is molten for nitric acid-potassium chlorate saturation is added into first mixture
The volume of liquid finds that, when the manganese content in the manganese containing materials is 12mg~20mg, Xiang Suoshu first is mixed after being optimized
Closing and nitric acid-potassium chlorate saturated solution volume is added in object is 40mL~50mL, can preferably be made in the first mixture
Manganese ion generate manganese dioxide, specifically, be added nitric acid-potassium chlorate saturated solution volume can for 40mL, 42mL, 44mL,
46mL, 48mL or 50mL etc..It will not mistake at this point, the nitric acid being added-potassium chlorate saturated solution volume is both not too high
It is low, so that the accuracy of the method for cobalt content is higher in the test manganese containing materials.
S300: second mixture is filtered processing, obtains filtrate to be measured and precipitating to be measured.
Contain according to an embodiment of the invention, second mixture is filtered in the filtrate to be measured obtained after processing
Cobalt ions contains manganese dioxide precipitate in the obtained precipitating to be measured, also, the manganese dioxide precipitate also can absorbed portion
Cobalt ions.That is, containing part cobalt ions in filtrate to be measured；And in precipitating to be measured, also contain part cobalt ions,
And content that the cobalt content in the manganese containing materials should be the cobalt ions in filtrate to be measured and the cobalt ions in precipitating to be measured
The adduction of content.
According to an embodiment of the invention, the concrete mode that second mixture is filtered processing is not limited especially
System, as long as meeting the requirements, those skilled in the art can according to need carry out flexible choice.In some embodiments of the present invention
In, processing can be filtered to second mixture using slow filter paper, and then obtain the filtrate to be measured and it is described to
Survey precipitating.It is simple, convenient as a result, it is easy to accomplish, it is easy to industrialized production, and can effectively obtain the filtrate to be measured
With precipitating to be measured.
S400: the first cobalt content in the filtrate to be measured is tested using potentiometric titration.
According to an embodiment of the invention, in the first cobalt content tested using potentiometric titration in the filtrate to be measured,
Due to Co2+Co is easily formed by the dioxygen oxidation in air under alkaline environment3+, thus by directly being surveyed using potentiometric titration
Try the Co in the filtrate to be measured2+The first cobalt content to obtain in filtrate to be measured is often unable to get accurate test result,
Thus in the first cobalt content tested using potentiometric titration in the filtrate to be measured, can first it add into the filtrate to be measured
Enter excessive oxidant with by Co2+It is oxidized to Co3+, then utilize Co2+The excessive oxidant of standard solution back titration.It is sharp as a result,
The test result for testing the first cobalt content in the filtrate to be measured with potentiometric titration is more accurate.
According to an embodiment of the invention, specifically, mentioned-above oxidant can be the potassium ferricyanide.It is dripped using current potential
When the method for determining tests the first cobalt content in the filtrate to be measured, excessive potassium ferricyanide solution first is added into the filtrate to be measured
Aoxidize the Co in the filtrate to be measured2+, then utilize Co2+The excessive Fe of standard solution back titration3+, so that utilizing current potential
The test result that titration tests the first cobalt content in the filtrate to be measured is more accurate.
According to an embodiment of the invention, as previously mentioned, the calculation formula of the first cobalt content in aforementioned filtrate to be measured are as follows:
Wherein, W(Co)For first cobalt content (%)；For the concentration (mol/L) of potassium ferricyanide solution；Volume (mL) for the potassium ferricyanide solution being added into the filtrate to be measured；C(Co)For Co2+Standard solution it is dense
It spends (mol/L)；V(Co)For the excessive Fe of back titration3+When consumed Co2+The volume (mL) of standard solution；M is in step S100
The preset quality of manganese containing materials；58.93 be the relative atomic mass of cobalt.Thus, it is possible to relatively accurately obtain the filter to be measured
The first cobalt content in liquid.
According to an embodiment of the invention, further, in first tested using potentiometric titration in the filtrate to be measured
When cobalt content, can first into the filtrate to be measured be added acidity regulator with adjust the filtrate to be measured for neutrality, then plus
Enter screening agent to shelter the interference of other ions in solution to be measured, reducing agent is added so that the cobalt in solution to be measured is with Co2+
Form exist so that the test result of first cobalt content is more accurate.
In a specific embodiment of the invention, in first tested using potentiometric titration in the filtrate to be measured
When cobalt content, concrete operations may is that first is added 2 drop methyl red indicators into the filtrate to be measured, and ammonium hydroxide is then added dropwise
Red to indicator is taken off, with adjust the filtrate to be measured pH be 6.5~7.5, then again to adjust pH be 6.5~7.5
Filtrate to be measured in be added ammonium chloride, ammonium citrate-ammonium hydroxide mixed solution, stand.Finally it was added into the filtrate to be measured
The potassium ferricyanide solution of amount aoxidizes the Co in the filtrate to be measured2+, Co is then utilized on automatical potentiometric titrimeter2+Standard is molten
The excessive Fe of liquid back titration3+.It is simple, convenient as a result, it is easy to accomplish, and it is easy to industrialization.
S500: the second cobalt content in the precipitating to be measured is tested using inductively coupled plasma emission spectrography.
According to an embodiment of the invention, being tested in the precipitating to be measured using inductively coupled plasma emission spectrography
The concrete operations of second cobalt content may is that the mixed solution by the precipitating to be measured concentrated hydrochloric acid and hydrogen peroxide is dissolved simultaneously
Heating is boiled, and most hydrogen peroxide, and constant volume are caught up with.Then the second cobalt content is tested using inductively-coupled plasma spectrometer, wherein
The Detection wavelength of cobalt element is (228 ± 1) nm or (238 ± 1) nm.It is simple, convenient as a result, it is easy to accomplish, it is quickly quasi-
Really, and it is easy to industrialization.
S600: first cobalt content is added with second cobalt content, to obtain the cobalt in the manganese containing materials
Content.
According to an embodiment of the invention, as previously mentioned, second mixture is filtered processing after obtain to
It surveys in filtrate and contains cobalt ions, in the obtained precipitating to be measured, also contain part cobalt ions, and the cobalt in the manganese containing materials
Content should be the adduction of the content of the cobalt ions in filtrate to be measured and the content of the cobalt ions in precipitating to be measured, also i.e. will be described
First cobalt content is added with second cobalt content, and what is obtained is the cobalt content in the manganese containing materials.
According to an embodiment of the invention, inventor carried out by the test method to cobalt content in manganese containing materials it is deep
It investigates and is found after numerous studies, in the related art, when testing the cobalt content in manganese containing materials with potentiometric titration, measurement
As a result always more higher than actual result, reason is when the cobalt content tested in manganese containing materials, if not removing manganese containing materials
In manganese, then the result that last test obtains be manganese containing materials in cobalt manganese content, therefore, test manganese containing materials in cobalt contain
It when amount, needs to remove the manganese in manganese containing materials, just can remove the interference that manganese element measures cobalt content.
According to an embodiment of the invention, further, inventor determines to use in the cobalt content tested in manganese containing materials
Nitric acid-potassium chlorate saturated solution makes manganese element with the form removal precipitated, and then removes manganese element and do for what cobalt content measured
It disturbs.However, inventor is having found after largely testing, after removing manganese element in the form precipitated, it is somebody's turn to do in test
When cobalt content in manganese containing materials, measurement result is relatively low instead.For this, inventor has carried out largely deep investigation and experiment
It is found after verifying, the relatively low reason of the test result of cobalt content is when with heavy in test manganese containing materials after removing manganese element
When the form in shallow lake removes manganese element, precipitating can also adsorb a certain amount of cobalt, and then cause test result relatively low.
Based on the above research, the method for the cobalt content in test manganese containing materials is further improved in inventor, it may be assumed that
In the form removal for being precipitated the manganese in manganese containing materials using nitric acid-potassium chlorate saturated solution, the filter tested respectively
Cobalt content in liquid and obtained precipitating, i.e., mentioned-above first cobalt content and the second cobalt content, then by first cobalt
Content and second cobalt content sum up, and obtain the cobalt content in the manganese containing materials.Thus, it is possible to test material containing manganese
The method testing result of cobalt content in material carries out effective compensation, so that the accuracy of test cobalt content is high, precision
It is high.
In other embodiments of the invention, referring to Fig. 2, the nitric acid-chlorine is being added into first mixture
Before sour potassium saturated solution, this method may also comprise the following steps::
Metal ion is added in S700: Xiang Suoshu first mixture.
According to an embodiment of the invention, inventor has found in the cobalt content tested in manganese containing materials based on the above research,
Even if will test obtained first cobalt content respectively in the cobalt content tested in manganese containing materials and second cobalt contains
It is summed up when amount, it, should although accuracy of the obtained test result compared to test result in the related technology is got higher
Test result is still not satisfactory.Based on this, inventor surprisingly sends out after having carried out largely deep investigation and experimental verification to this
It is existing, before the nitric acid-potassium chlorate saturated solution is added into first mixture, add in the first mixture of Xiang Suoshu
Enter metal ion, can further significantly improve the accuracy of the test method.
According to an embodiment of the invention, the type of the metal ion can be Mg2+、Ca2+、Zn2+And Fe3+Deng.Into
One step, inventors have found that when the metal ion is Zn2+Or Fe3+When, the method for cobalt content in the test manganese containing materials
The accuracy of test result significantly improved compared to when metal ion not being added.
According to an embodiment of the invention, inventor thinks after a large amount of experimental verification, to first mixture
After middle addition metal ion, when nitric acid-potassium chlorate saturated solution being added generating manganese dioxide precipitate, due to described first mixed
It closes in object and both containing cobalt ions or to contain the metal ion of addition noted earlier, thus, manganese dioxide precipitate generated can be right
Cobalt ions and mentioned-above metal ion generate competitive Adsorption, and the activity on manganese dioxide surface is occupied by the metal ion, from
And the amount for the cobalt ions that manganese dioxide precipitate is adsorbed is reduced, i.e., so that the content of cobalt ions is reduced in subsequent precipitating to be measured,
Further amounts of cobalt ions has stayed in filtrate to be measured.However, as previously mentioned, in theory, no matter mentioned-above first
Who is few more than who of cobalt content and the second cobalt content, as long as the first cobalt content and the second cobalt content are summed up, always it obtains
Cobalt content in manganese containing materials.However, experimental phenomena shows after metal ion is added into the first mixture, so that the
Two cobalt contents reduce, and correspondingly the first cobalt content increases, and can make the test result of the cobalt content in the test manganese containing materials more
It is accurate.It for this, is found after the analysis of inventor's further progress, in front in the method, although compensate for be measured
The cobalt adsorbed in precipitating deviation for caused by test result, but (namely the second cobalt contains the cobalt adsorbed in precipitating only to be measured
Amount) be suitable for using inductively coupled plasma emission spectrography tested when, could further such that this method accuracy
It improves.That is, into first mixture be added nitric acid-potassium chlorate saturated solution again by the second obtained mixture into
After row filtration treatment, the cobalt amount directly adsorbed in precipitating to be measured is not a known quantity, the cobalt adsorbed in the precipitating to be measured
Amount (namely the second cobalt content) is not of course applied for known analysis test method to carry out analysis test, it is then desired to
Competitive Adsorption is generated to adjust the second cobalt content by the mentioned-above addition metal ion into the first mixture, is adapted to
Analysis test is carried out using known analysis test method.Certainly, in the present invention, the analysis test of the second cobalt content is tested
Method is inductively coupled plasma emission spectrography.That is, inventor is by the way that gold is added into first mixture
Belong to ion, so that the accuracy of the second cobalt content in this method is higher, so that the accuracy of this method is higher.
According to an embodiment of the invention, based on the above analysis, inventor is for the gold that is added into first mixture
The competitive Adsorption for belonging to ion and cobalt ions is tested, and can be obtained by experimental result, when the metal ion is Zn2+Or Fe3+
When, compared to other kinds of metal ion, the cobalt amount (i.e. the second cobalt content) adsorbed in mentioned-above precipitating to be measured is added
It is significant relatively low.As a result, it has been recognised by the inventors that mentioned-above second cobalt content should be made as few as possible, the test material containing manganese may make
The accuracy of the method for cobalt content is higher in material.
According to an embodiment of the invention, further, inventor has found after lot of experiment validation, when second cobalt
When content is not higher than 7.1% of the cobalt content in the manganese containing materials, the survey of cobalt content in mentioned-above test manganese containing materials
The accuracy of test result further increases and precision also further increases.
According to an embodiment of the invention, as previously mentioned, when the metal ion is Zn2+Or Fe3+When, which contains manganese
The accuracy of the method testing result of cobalt content is significantly improved compared to when metal ion not being added in material, further,
When testing cobalt content, due to Fe3+Coexist and need to use excessive ammonium citrate to be sheltered as screening agent, if masking is not
Test result can then be had an impact completely, thus, it is Zn in the metal ion being added into first mixture2+When, it should
The accuracy of the method for cobalt content in test manganese containing materials reaches more preferably.
In other embodiment of the invention, further, referring to Fig. 3, institute is being added into first mixture
Before stating nitric acid-potassium chlorate saturated solution, this method may also comprise the following steps::
S800: first mixture is evaporated processing.
According to an embodiment of the invention, inventor has carried out the method for cobalt content in the test manganese containing materials further again
Optimization, inventors have found that before the nitric acid-potassium chlorate saturated solution is added into first mixture, by described the
One mixture is evaporated processing, it is also possible that the accuracy of the method for cobalt content further mentions in the test manganese containing materials
It is high.
According to an embodiment of the invention, inventor is for being evaporated that treated for first mixture, volume is carried out
It is found after further investigation, when by first mixture, to be evaporated processing to volume be 1mL~5mL, the standard of this method
Exactness is higher, specifically, first mixture can be evaporated processing to volume be 1mL, 2mL, 3mL, 4mL or
5mL etc..Further, when by first mixture be evaporated processing to volume be 1mL~2mL when, the standard of this method
Exactness further increases.
In still other embodiments of the invention, further, referring to Fig. 4, second mixture is filtered place
Before reason, this method may also comprise the following steps::
S900: second mixture is heated.
According to an embodiment of the invention, inventors have found that before second mixture is filtered processing, it will be described
Second mixture carries out heat treatment can be further such that mentioned-above precipitating to be measured precipitating completely, and can be accelerated instead
Rate is answered, testing efficiency is improved.
According to an embodiment of the invention, further, the temperature and time of heat treatment is optimized in inventor
After obtain, when the heat treatment temperature be 340 DEG C~400 DEG C, specifically, can be 340 DEG C, 360 DEG C or 380 DEG C etc.
When；The time of the heat treatment is 8min~12min, specifically, when can be 8min, 10min or 12min, this method
Accuracy it is higher.
According to an embodiment of the invention, this method meets at least one of the following conditions: recovery of standard addition be 99.7%~
101.1%；When the manganese content in the manganese containing materials is 12mg~20mg, relative standard deviation is not more than 0.64%.Specifically
Ground, the recovery of standard addition of the method can be 99.7%, 99.9% or 101.1% etc..As a result, in the test manganese containing materials
The method accuracy of cobalt content is high and precision is high.
In addition, in a specific embodiment of the invention, referring to Fig. 5, when the manganese content in the manganese containing materials is
When 12mg~20mg, this method comprises: S100 ': under conditions of 150 DEG C~250 DEG C, by the manganese containing materials concentrated hydrochloric acid and
Hydrogen peroxide is dissolved, and first mixture is obtained；The quality containing zinc is added in S700 ': Xiang Suoshu first mixture is
The solution of zinc sulfate of 100mg；S800 ': it is 1mL~2mL that first mixture, which is evaporated processing to volume,；S200 ': to
Nitric acid-potassium chlorate saturated solution of 40mL~50mL is added in first mixture, obtains the second mixture；S900 ':
Under conditions of 340 DEG C~380 DEG C, second mixture is subjected to heat treatment 8min~12min；S300 ': will be by described
Second mixture of heat treatment is filtered processing, obtains the filtrate to be measured and the precipitating to be measured；S400: it utilizes
Potentiometric titration tests the first cobalt content in the filtrate to be measured；S500: inductively coupled plasma emission spectrography is utilized
Test the second cobalt content in the precipitating to be measured；S600: first cobalt content is added with second cobalt content, so as to
Obtain the cobalt content in the manganese containing materials.As a result, in the test manganese containing materials in the method for cobalt content, a parameter reaches
Preferably, so that the accuracy of this method is significantly improved compared to the method for test cobalt content in the related technology, precision
It significantly improves, and this method is simple, convenient, easy to accomplish, cost is relatively low, is easy to industrialization.
In some embodiments of the invention, the manganese containing materials can be nickel-cobalt-manganese ternary material.This method is suitable as a result,
It is tested together in nickel-cobalt-manganese ternary material cobalt content, so that in cell production process, especially lithium ion battery
Production process in, test obtain the cobalt content in positive electrode active materials, in order to the positive electrode in lithium ion battery
Chemical property optimizes.
In another aspect of the invention, the present invention provides a kind of methods for testing electrode quality.It is according to the present invention
Embodiment, the electrode include mentioned-above manganese containing materials, and the method includes being contained using mentioned-above method to described
The step of cobalt content in manganese material is tested.Inventors have found that this method is simple, convenient, and it is easy to accomplish, it is easy to produce
Industry, and can preferably test the chemical property of electrode.
According to an embodiment of the invention, it will be understood by those skilled in the art that except mentioned-above to the manganese containing materials
In cobalt content the step of being tested other than, the method for the test electrode quality further includes other testing procedures, herein no longer
Excessively repeat.
In an additional aspect of the present invention, the present invention provides a kind of methods for testing battery quality.It is according to the present invention
Embodiment, the battery include mentioned-above electrode, the method includes using previous methods to the quality of the electrode into
The step of row test.Inventors have found that this method is simple, convenient, and it is easy to accomplish, it is easy to industrialization, and can be preferably
Test the chemical property of battery.
According to an embodiment of the invention, it will be understood by those skilled in the art that removing the mentioned-above matter to the electrode
Other than the step of amount is tested, the method for the test battery quality further includes other testing procedures, is no longer excessively repeated herein.
The embodiment of the present invention is described below in detail.Instrument used in embodiment and reagent are as follows:
916 type potentiometric titrimeters (Switzerland ten thousand is logical)；ICAP7400 inductively-coupled plasma spectrometer (U.S. Thermo
Scientific company)；Smart Plus-N ultrapure water machine (Shanghai power health)；Electronic balance: sensitivity 0.0001g；ICP-OES
Cobalt standard solution: 1000ug/mL, using 5%HCl as matrix, it is bent that dilution is configured to 0,2.5ug/mL, 5ug/mL, 10ug/mL standard
Linear system column；Analyze pure hydrochloric acid: HCl content is about 36%-38%；Analyze pure nitric acid: HNO3Content is about 70%；Hydrogen peroxide: matter
Measure concentration 30%；(1+9) sulfuric acid: 1 volume sulfuric acid and 9 volume of water；Solution of zinc sulfate: 8.8g Zinc vitriol is weighed, water is added
Dissolution, is settled to 200mL, every milliliter of 10mg containing zinc of this solution；Nitric acid-potassium chlorate saturated solution: 500mL concentrated nitric acid is measured to palm fibre
In color reagent bottle, potassium chlorate is added and stirs to not being redissolved, and is excessive, placement uses afterwards for 24 hours；Methyl red indicator: it weighs
0.2g methyl red is dissolved in dehydrated alcohol, is settled to 100mL, is shaken up；Ammonium hydroxide: mass concentration >=28%；Ammonium chloride: analysis is pure；
Ammonium citrate-ammonium hydroxide mixed solution: weigh 50g ammonium citrate be placed in 1000mL beaker plus 500mL water and 500mL ammonium hydroxide it is mixed
It is even；Cobalt standard solution: it accurately weighs 1g metallic cobalt (Co >=99.98%) and is placed in addition 50mL dust technology (nitric acid in 250mL beaker
The electric hot plate that temperature setting is 100 DEG C is placed on water volume ratio 1:4) to dissolve by heating, is cooled to room temperature, and 1000mL appearance is transferred to
Constant volume in measuring bottle shakes up；Potassium ferricyanide standard solution: it weighs the 11.2g potassium ferricyanide and is placed in 250mL beaker about 150mL is added
Water is placed on the electric hot plate that temperature setting is 70 DEG C~80 DEG C and dissolves by heating, is filled into 1000mL volumetric flask, adds water constant volume
It to graduation mark, shakes up, is stored in brown reagent bottle, it is fixed using advance rower.
Embodiment 1
0.1g nickel-cobalt-manganese ternary material is weighed into 250mL beaker, a small amount of water soaks sample, and rinses wall of cup, and 5mL is added
Hydrochloric acid is added solution of zinc sulfate 10mL (zinc content 100mg), is added 1mL (1+9) after few drops of hydrogen peroxide heating for dissolving are added dropwise
Sulfuric acid is heated to sulfuric acid cigarette on low-temperature furnace and emits to the greatest extent, slightly cold, and a small amount of deionized water is added and rinses wall of cup, dissolves by heating sample, steams
Being sent to volume is 1~2mL or so, and nitric acid-potassium chlorate saturated solution 50mL is added, is placed on 340 DEG C~380 DEG C electric hot plates and carries out
Heat treatment covers surface plate, boils 4~6 minutes, add 0.5g potassium chlorate solid, continue to boil after yellow green smog is emerged
Boiling removes cooling in 4~6 minutes, washes with water watch glass and beaker to liquid volume and reaches 80mL or so, is filtered using slow filter paper
Beaker and precipitating are washed for several times into another 250mL beaker, and with hot water, and then obtain filtrate to be measured and precipitating to be measured.
2 drop methyl red indicators are added into filtrate to be measured, the red that ammonium hydroxide to indicator is added dropwise is decorporated, at this time solution PH
Iron hydrogenation potassium solution and excessive 5mL or so is added, certainly in ≈ 7, addition 5g ammonium chloride, 50mL ammonium citrate-ammonium hydroxide mixed solution
By the program of instrument setting on electrokinetic potential titrator, with Co2+Standard solution is titrated, and instrument automatic identification terminal simultaneously calculates knot
Fruit obtains the first cobalt content.
By the resulting precipitating to be measured of above-mentioned filtering, washed with hydrochloric acid-hydrogen peroxide mixed solution into former beaker, heating is boiled
Boiling, catches up with most hydrogen peroxide, is settled in 100mL volumetric flask, test precipitating to be measured using inductively coupled plasma emission spectrography
In the second cobalt content.
First cobalt content is added with second cobalt content, to obtain the cobalt content in the manganese containing materials.
Test result:
(1) manganese content in the nickel-cobalt-manganese ternary material in embodiment 1 (weighs 0.1g sample, that is, contains manganese for 12%
12mg), it is tested according to the test method in embodiment 1,6 groups of parallel testing, test result is as shown in table 1；
1 test result of table and Precision test result
Same nickel-cobalt-manganese ternary material parallel is tested 6 times it can be seen from 1 data of table, result error is smaller, it is seen that this
Method precision is high, as a result stable.
(2) it is tested according to the test method in embodiment 1 with 1-Nitroso-2-naphthol gravimetry in the related technology
The same nickel-cobalt-manganese ternary material, and recovery testu is carried out, test result is as shown in table 2；
The accuracy experimental result of 2 measuring method of table
| Analysis method | Cobalt content (%) | Cobalt content (%) after mark-on 10% | Recovery of standard addition (%) |
| Embodiment 1 | 10.09 | 20.20 | 101.1 |
| 1-Nitroso-2-naphthol gravimetry | 10.18 | 20.35 | 101.7 |
1 method therefor of embodiment and 1-Nitroso-2-naphthol gravimetry survey the survey of cobalt it can be seen from 2 data of table
Test result is compared, and two methods result is close, and recovery of standard addition can illustrate that this method accuracy is higher close to 100%, but
Operating procedure, test period are substantially better than 1-Nitroso-2-naphthol gravimetry.
(3) standard sample of nickel-cobalt-manganese ternary material is prepared, nickeliferous 50mg in the sample, cobalt 10mg are separately added into difference
Content Mn2+(four water manganese acetates) verifies the method in embodiment 1 for Mn2+Interference eradicating efficacy, the results are shown in Table 3；
The experiment of 3 manganese mutual interference eradicating efficacy of table
| Mn2+Additional amount/mg | 5 | 10 | 15 | 20 |
| Cobalt content measured value/mg | 10.04 | 9.97 | 9.98 | 10.03 |
It can be seen that the Mn that 20mg is added by 3 data of table2+Also the cobalt measurement for not influencing method in embodiment 1, illustrates to use
Nitric acid-potassium chlorate saturated solution processing sample can be by the As in nickel-cobalt-manganese ternary material3+、Fe2+、Cr3+It is oxidizing to high price, and
Mn2+It is oxidized to MnO2Precipitation form removes, As in practical nickel-cobalt-manganese ternary material3+、Fe2+、Cr3+Content it is lower, itself not
The test result of cobalt content is impacted, and Mn2+Content generally 20% hereinafter, therefore, method of the invention contains in manganese
When amount is 20% or less, interference is completely eliminated.
(4) test is carried out to the test method in embodiment 1 and carries out control experiment, one group of experiment is according in embodiment 1
Method carries out；Another group of experiment, which removes, is added without solution of zinc sulfate (Zn2+) other than, test result identical as the method in embodiment 1
As shown in table 4；
Whether table 4 is added Zn2+The influence of the measured value of second cobalt content
| Test condition | The measured value (%) of second cobalt content |
| Not plus Zn2+ | 0.98 |
| Zn is added2+ | 0.67 |
It can be seen from 4 data of table in a heated condition, due to being hydrated MnO2To Co2+There is stronger adsorption capacity, is added
The competing ions Zn of high concentration2+, make to be hydrated MnO2Active site largely occupied, make it to Co2+Adsorption capacity limited
System reduces Co2+Co-precipitation, thus guarantee inductively coupled plasma emission spectrography (ICP-OES) test the second cobalt contain
Amount is in reasonable range, and excessive Zn2+To in subsequent step constant-current titration and ICP-OES test it is noiseless, not shadow
Ring the accuracy of result.
The selection of 2 metal ion of embodiment
Prepare the standard sample of nickel-cobalt-manganese ternary material, nickeliferous 50mg, cobalt 10mg, manganese 20mg, according to implementation in the sample
Test method in example 1 is added without solution of zinc sulfate, and solution of zinc sulfate is replaced with to the Na containing 100mg respectively+、Mg2+、Ca2 +、Fe3+Solution, with the standard sample of the nickel-cobalt-manganese ternary material that metal ion is not added, the Zn of 100mg is added2+Nickel cobalt manganese
The standard sample of ternary material synchronizes experiment, the result of adsorbed cobalt content such as table 5 in the precipitating to be measured tested:
After same amount of metal ion is added in table 5, the cobalt content that is adsorbed in precipitating to be measured
| Sample | Metal ion is not added | Na+ | Mg2+ | Ca2+ | Zn2+ | Fe3+ |
| The cobalt content (mg) adsorbed in precipitating | 0.98 | 1.01 | 0.96 | 0.88 | 0.67 | 0.50 |
The result shows that Na is added compared with metal ion is not added+、Mg2+、Ca2+Afterwards, to the cobalt content adsorbed in precipitating
Influence it is smaller, be added Zn2+、Fe3+There is a degree of reduction to adsorbance afterwards.
Influence of the volume of first mixture to test result before the addition nitric acid-potassium chlorate saturated solution of embodiment 3
According to the test method in embodiment 1, after catching up with most sulfuric acid cigarette, different amounts of deionized water is added and extracts sample, adds
Enter 50mL nitric acid-potassium chlorate saturated solution and carry out oxidation separation, tests the same nickel-cobalt-manganese ternary material, manganese content in the sample
It is 12%, cobalt content is 10% (weighing 0.1g sample, i.e. 12mg containing manganese or so).Test result is as follows:
Influence of the volume of first mixture to test result before the addition nitric acid-potassium chlorate saturated solution of table 6
Being stepped up with liquor capacity it can be seen from data in table 6, test result is gradually increased, and can be speculated
For Mn in the first mixture2+Separation not exclusively, causes measurement result bigger than normal by the interference of manganese.When liquor capacity is 1~2mL
When, test result and true value are close.
Influence of 4 nitric acid of embodiment-potassium chlorate saturated solution additional amount to measurement result
Prepare the standard sample of nickel-cobalt-manganese ternary material, nickeliferous 50mg, cobalt 10mg, manganese 20mg, according to implementation in the sample
Test method in example 1 is separately added into different amounts of nitric acid-potassium chlorate saturated solution, tests the mark of the nickel-cobalt-manganese ternary material
The test result of cobalt content such as table 7 in quasi- sample:
Influence of 7 nitric acid of table-potassium chlorate saturated solution additional amount to measurement result
| Nitric acid-potassium chlorate saturated solution additional amount/mL | 10 | 20 | 30 | 40 | 50 |
| Cobalt content/mg | 17.58 | 12.66 | 11.64 | 10.11 | 9.97 |
| The rate of recovery | 175.8% | 126.6% | 116.4% | 101.1% | 99.7% |
It can be seen from data in table 7 when nitric acid-potassium chlorate saturated solution additional amount is 40mL~50mL, surveyed
As a result it tends towards stability, and close to theoretical value.
Influence of the temperature and time that embodiment 5 heats to measurement result
According to the test method in embodiment 1, the temperature and time of different heat treatment is selected, tests the same nickel cobalt
Manganese ternary material, manganese content is 12% in the nickel-cobalt-manganese ternary material, and cobalt content is 10% (to weigh 0.1g sample, that is, contain manganese
12mg or so).Test result such as table 8:
Influence of the temperature and time that table 8 heats to measurement result
From 8 data of table: when the temperature of heat treatment is 340 DEG C~400 DEG C, when time 8min~12min, cobalt content
Test result stablize 10% or so, but at 380 DEG C~400 DEG C of temperature, adsorption of cobalt amount is more in precipitating to be measured, is unfavorable for
ICP-OES method measures the second cobalt content, therefore the temperature of heat treatment is selected as 340 DEG C~380 DEG C, selection of time be 8min~
12min；In addition, adding a postassium hypochlorite solid in the test process of embodiment 1, to supplement the reaction consumption of potassium chlorate, make
Reaction carries out more thorough.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of method of cobalt content in test manganese containing materials characterized by comprising
The manganese containing materials are dissolved, the first mixture is obtained；
Nitric acid-potassium chlorate saturated solution is added into first mixture, obtains the second mixture；
Second mixture is filtered processing, obtains filtrate to be measured and precipitating to be measured；
The first cobalt content in the filtrate to be measured is tested using potentiometric titration；
The second cobalt content in the precipitating to be measured is tested using inductively coupled plasma emission spectrography；
First cobalt content is added with second cobalt content, to obtain the cobalt content in the manganese containing materials.
2. the method according to claim 1, wherein the nitric acid-chlorine is added into first mixture
Before sour potassium saturated solution, further includes:
Metal ion is added into first mixture,
Optionally, the metal ion includes Fe3+And Zn2+At least one of, preferably Zn2+。
3. according to the method described in claim 2, it is characterized in that, second cobalt content is not higher than the cobalt content
7.1%.
4. the method according to claim 1, wherein the nitric acid-chlorine is added into first mixture
Before sour potassium saturated solution, further includes:
First mixture is evaporated processing,
Optionally, first mixture is evaporated processing to volume is 1mL~5mL, preferably 1mL~2mL.
5. the method according to claim 1, wherein when the manganese content in the manganese containing materials is 12mg~20mg
When, it is 40mL~50mL that nitric acid-potassium chlorate saturated solution volume is added in the first mixture of Xiang Suoshu.
6. the method according to claim 1, wherein being gone back before second mixture is filtered processing
Include:
Second mixture is heated,
Optionally, the temperature of the heat treatment be 340 DEG C~400 DEG C, preferably 340 DEG C~380 DEG C,
Optionally, the time of the heat treatment is 8min~12min.
7. the method according to claim 1, wherein meeting at least one of the following conditions:
Recovery of standard addition is 99.7%~101.1%；
When the manganese content in the manganese containing materials is 12mg~20mg, relative standard deviation is not more than 0.64%.
8. the method according to claim 1, wherein when the manganese content in the manganese containing materials is 12mg~20mg
When, comprising:
Under conditions of 150 DEG C~250 DEG C, the manganese containing materials are dissolved with concentrated hydrochloric acid and hydrogen peroxide, obtains described
One mixture；
The solution of zinc sulfate that the quality containing zinc is 100mg is added into first mixture；
It is 1mL~2mL that first mixture, which is evaporated processing to volume,；
Nitric acid-potassium chlorate saturated solution of 40mL~50mL is added into first mixture, obtains the second mixture；
Under conditions of 340 DEG C~380 DEG C, second mixture is subjected to heat treatment 8min~12min；
Second mixture Jing Guo the heat treatment is filtered processing, obtains the filtrate to be measured and described to be measured
Precipitating；
The first cobalt content in the filtrate to be measured is tested using potentiometric titration；
The second cobalt content in the precipitating to be measured is tested using inductively coupled plasma emission spectrography；
First cobalt content is added with second cobalt content, to obtain the cobalt content in the manganese containing materials,
Optionally, the manganese containing materials are nickel-cobalt-manganese ternary material.
9. a kind of method for testing electrode quality, the electrode includes manganese containing materials according to any one of claims 1 to 8,
It is characterized in that, the method includes utilizing method described in any one of claim 1~8 to the cobalt in the manganese containing materials
The step of content is tested.
10. a kind of method for testing battery quality, the battery includes electrode described in claim 9, which is characterized in that institute
State the step of method is tested including the use of quality of the method as claimed in claim 9 to the electrode.
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