CN101349623A - Method for dissolving cobaltosic oxide and method for measuring non-cobalt metal element content - Google Patents
Method for dissolving cobaltosic oxide and method for measuring non-cobalt metal element content Download PDFInfo
- Publication number
- CN101349623A CN101349623A CNA200710130544XA CN200710130544A CN101349623A CN 101349623 A CN101349623 A CN 101349623A CN A200710130544X A CNA200710130544X A CN A200710130544XA CN 200710130544 A CN200710130544 A CN 200710130544A CN 101349623 A CN101349623 A CN 101349623A
- Authority
- CN
- China
- Prior art keywords
- cobaltosic oxide
- dissolving
- acid
- metal element
- minute
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for dissolving cobaltic-cobaltous oxide, which comprises leading cobaltic-cobaltous oxide to contact with dissolvent, and keeping the cobaltic-cobaltous oxide for 1-20 minutes under 100-1100 DEG C before the cobaltic-cobaltous oxide contacts with the dissolvent. The method can rapidly and fully dissolve cobaltic-cobaltous oxide which is difficult to dissolve, and simultaneously eliminates cobaltic-cobaltous oxide remainder in dissolved solution, and the method is beneficial for rapidly and accurately doing atomic emission spectrometry to cobaltic-cobaltous oxide, which has high testing efficiency and accuracy.
Description
Technical field
The dissolving method that the invention relates to a kind of cobaltosic oxide reaches the wherein assay method of non-cobalt metal element content, more particularly, dissolving method and the employing atomic emission spectrum that the invention relates to a kind of cobaltosic oxide carries out method for measuring to non-cobalt metal element content in the cobaltosic oxide.
Background technology
Cobaltosic oxide is a kind of preparation active substance of lithium ion battery anode LiCoO
2Raw material commonly used.The conventional high-temperature solid phase method synthesizes LiCoO
2Method in generally be with lithium carbonate (Li
2CO
3) and cobaltosic oxide (Co
3O
4) be raw material, be 1: 1 ratio preparation according to the mol ratio of Li: Co, roasting is made under 700-900 ℃ of air atmosphere then.As, described LiCoO
2The preparation method at Huang D, et al.Solid solution:New cathodes for next generation lithium-ion batteries[J] .Advanced Battery Technology, 1998 (11): describe to some extent among the 23-27.For the positive active material LiCoO that guarantees to prepare
2Meet certain requirement, as, need obtain being coated with the LiCoO of other metal
2, perhaps must limit LiCoO
2In the situation of certain metal element content, therefore, before preparation, need carry out the mensuration of non-cobalt metal element content to the raw material cobaltosic oxide.
Cobaltosic oxide is being carried out ICP-AES (atomic emission spectrum) when test, must be earlier with dissolving cobaltosic oxide in solvent, wiring solution-forming.But cobaltosic oxide is difficult to be dissolved in water, hydrochloric acid, nitric acid and the chloroazotic acid equal solvent, can only slowly be dissolved in the hot sulfuric acid, and test has brought a lot of inconvenience to ICP-AES for this.At present, when cobaltosic oxide being carried out the ICP-AES test, generally use the aqua regia dissolution cobaltosic oxide, dissolve a sample and need three hours at least, and cobaltosic oxide still can not dissolve fully, even heating can not be dissolved cobaltosic oxide fully, has some residues in the solution.As a kind of conventionally test method of cobaltosic oxide, only course of dissolution will be consuming time about three hours, and this has had a strong impact on testing efficiency, has also increased a lot of pressure to control with raw material; In addition, the residue in the lysate has influenced the accuracy of test result, has reduced the reference value of test result.
Summary of the invention
The objective of the invention is to overcome and existing non-cobalt metal element content in the cobaltosic oxide is carried out before ICP-AES measures, method condition harshness, the dissolution time of dissolving cobaltosic oxide are long, make defective that testing efficiency is low and a kind of method of dissolving cobaltosic oxide simply, fast is provided, and high efficiency non-cobalt metal element content in the cobaltosic oxide is carried out the atomic emission spectrum method for measuring.
The present inventor is surprised to find that, with cobaltosic oxide after keeping a period of time under 100-1100 ℃ the temperature, contact with acid solution again, cobaltosic oxide only needed just can be dissolved in fully in the acid solution in short 30 minutes, making the dissolving of cobaltosic oxide become is more prone to, the dissolution conditions milder, thus in measuring cobaltosic oxide, can improve testing efficiency greatly during non-cobalt metal element content.
The invention provides a kind of dissolving method of cobaltosic oxide, this method comprises cobaltosic oxide contacted with acid solution, wherein, with cobaltosic oxide with before acid solution contacts, cobaltosic oxide was kept 1-20 minute down at 100-1100 ℃.
The present invention also provides the assay method of non-cobalt metal element content in a kind of cobaltosic oxide, and this method comprises with dissolving cobaltosic oxide and carry out the atomic emission spectrum test that wherein, the dissolving method of described cobaltosic oxide is a method provided by the invention.
Method of the present invention can be fast and is dissolved the indissoluble cobaltosic oxide fully, dissolving method is simple, dissolution conditions is gentle, eliminated the cobaltosic oxide residue in the lysate simultaneously, solved the indissoluble cobaltosic oxide when carrying out the atomic emission spectrum test, the problem of dissolving indissoluble cobaltosic oxide condition harshness, length consuming time, help fast and accurately cobaltosic oxide being carried out atomic emission spectrum and measure the accuracy height of testing efficiency and test result.
Embodiment
According to the present invention, this dissolving method comprises cobaltosic oxide contacted with acid solution, wherein, with cobaltosic oxide with before acid solution contacts, cobaltosic oxide was kept 1-20 minute down at 100-1100 ℃, be preferably and kept 1-10 minute.
The described various maintenance methods that cobaltosic oxide can be adopted this area routine the 100-1100 ℃ of method of placing down and keeping, under the preferable case, described maintenance method comprises earlier cobaltosic oxide kept 1-5 minute down at 100-180 ℃, continues to keep 1-15 minute after being warming up to 200-1100 ℃ with 10-100 ℃/minute speed then; Perhaps directly cobaltosic oxide is warming up to 100-1100 ℃ with 10-100 ℃/minute speed, and kept 1-20 minute.
The described cobaltosic oxide that makes is not particularly limited 200-1100 ℃ of atmosphere that keeps down, can be various atmosphere, as oxidizing atmosphere, reducing atmosphere or inert atmosphere, described oxidizing atmosphere can be air or oxygen, described reducing atmosphere can be one or more in hydrogen, carbon monoxide atmosphere and the methane, described inert atmosphere can be one or more in nitrogen and/or the zero group gas, as atmosphere such as helium, argon gas.
According to the present invention, the temperature of described maintenance is 100-1100 ℃, and for different atmosphere, the temperature of described maintenance also can be different, as, for reducing atmosphere, described maintenance temperature is preferably 200-600 ℃ promptly can reach goal of the invention; For inert atmosphere or oxidizing atmosphere, described maintenance temperature is preferably 800-1100 ℃.Described cobaltosic oxide is kept under 100-1100 ℃ high temperature, to the not influence of content of the metallic element in this sample.
The described cobaltosic oxide that makes is not particularly limited at 200-1100 ℃ of pressure that keeps down, gets final product under normal pressure.
Generally speaking, can contain impurity such as organic matters or powdered carbon in the cobaltosic oxide sample, in oxidizing atmosphere, keep, impurity such as organism or powdered carbon is easy to be decomposed, to reduce other the residue in the lysate, help improving test accuracy, therefore, described maintenance process is preferably carried out in oxidizing atmosphere.Described oxidizing atmosphere is that the volume content of oxygen is not less than 5% oxygen-containing gas.
According to the present invention, this method also is included in the cooling step of cobaltosic oxide after keeping under 100-1100 ℃, the method of described cooling can adopt and well known to a person skilled in the art various cooling means, as natural cooling etc., the atmosphere of described cooling is not particularly limited, can be various atmosphere, as reducing atmosphere, oxidizing atmosphere or inert atmosphere etc.Described chilling temperature is generally and is cooled to room temperature and gets final product, and also can be the temperature that is lower than room temperature, as 10 ℃-room temperature, is preferably 10-25 ℃.
Adopt method of the present invention the indissoluble cobaltosic oxide can be changed into easy molten cobaltosic oxide or cobalt protoxide, be particularly conducive to dissolving step subsequently, cobaltosic oxide is dissolved in the solvent fully.
Described solvent can be the various solvents that are used to dissolve cobaltosic oxide of this area routine, as acid solution or alkaline solution, described acid solution is preferably the mixed solution of acid and water, and described acid is preferably one or more in hydrochloric acid, nitric acid, sulfuric acid and the perchloric acid; Described basic solvent is preferably the mixed solution of alkali and water, and described alkali is preferably one or more in NaOH, potassium hydroxide and the ammoniacal liquor.The amount of the solvent that every gram cobaltosic oxide is required can be the 10-20 milliliter, is preferably the 15-20 milliliter.The concentration of described acid solution is generally the 5-20 mol, and the concentration of described alkaline solution is generally the 5-20 mol.Influence test result owing to adopting alkaline solution dissolving cobaltosic oxide may introduce metallic ion, therefore, the preferred solvent of the present invention is an acid solution.
Non-cobalt metal element content in the cobaltosic oxide is carried out atomic emission spectrum carry out method for measuring according to of the present invention, after adopting method dissolving cobaltosic oxide of the present invention, just can directly adopt atomic emission spectrum to measure the wherein content of non-cobalt metal element, described assay method is conventionally known to one of skill in the art, does not repeat them here.
Below will the present invention will be further described by specific embodiment.
Embodiment 1
Present embodiment illustrates that the dissolving method of cobaltosic oxide of the present invention reaches the wherein assay method of non-cobalt metal element content.
(be numbered ICP-01, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co with 1000 milligrams of cobaltosic oxide samples
3O
4-L-12.6) be positioned in the ceramic vessel, earlier the cobaltosic oxide sample was kept in container 2 minutes down at 150 ℃, then the cobaltosic oxide sample is positioned in the electric furnace, and in air atmosphere (volume content of oxygen is 21%), be warming up to 1000 ℃ and kept 5 minutes with 20 ℃/minute speed, take out sample then and naturally cool to room temperature.Then above-mentioned cobaltosic oxide sample is mixed with 15 milliliters of hydrochloric acid (concentration is 12 mol), and stir, sample all dissolves after 30 minutes, fixed molten with 100 milliliters volumetric flask then, get 10 ml solns and carry out ICP-AES (French JOBIN YVON JY238 type, high frequency power is 1000 watts, and gas flow is 1.04 ml/min) test, the content of non-cobalt metal element in the specimen.Test result is as shown in table 1.
Wavelength: Fe is 259.940 nanometers, and Ca is 393.366 nanometers, and Pb is 283.306 nanometers, and Mg is 279.553 nanometers, and Mn is 257.610 nanometers, and Na is 588.995 nanometers, and Ni is 221.647 nanometers.
Embodiment 2
Present embodiment illustrates that the dissolving method of cobaltosic oxide of the present invention reaches the wherein assay method of non-cobalt metal element content.
(be numbered ICP-02, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co with 1000 milligrams of cobaltosic oxide samples
3O
4-L-12.11) be positioned in the ceramic vessel, earlier the cobaltosic oxide sample was kept in container 3 minutes down at 100 ℃, then the cobaltosic oxide sample is positioned in the electric furnace, and in air atmosphere (volume content of oxygen is 21%), be warming up to 600 ℃ and kept 15 minutes with 40 ℃/minute speed, take out sample then and naturally cool to room temperature.Then above-mentioned cobaltosic oxide sample is mixed with 15 milliliters of sulfuric acid (concentration is 12 mol), and stir, sample all dissolves after 30 minutes, fixed molten with 100 milliliters volumetric flask then, get 10 ml solns and carry out ICP-AES (French JOBIN YVON JY238 type, high frequency power is 1000 watts, and gas flow is 1.04 ml/min) test, the content of non-cobalt metal element in the specimen.Test result is as shown in table 1.
Embodiment 3
Present embodiment illustrates that the dissolving method of cobaltosic oxide of the present invention reaches the wherein assay method of non-cobalt metal element content.
(be numbered ICP-03, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co with 1000 milligrams of cobaltosic oxide samples
3O
4-L-12.18) be positioned in the ceramic vessel, earlier the cobaltosic oxide sample was kept in container 2 minutes down at 120 ℃, then the cobaltosic oxide sample is positioned in the program control cabinet-type electric furnace in air atmosphere (volume content of oxygen is 21%), be warming up to 800 ℃ and kept 10 minutes with 60 ℃/minute speed, take out sample then and naturally cool to room temperature.Then the mixed solution of above-mentioned cobaltosic oxide sample with 12 milliliters of hydrochloric acid (concentration is 12 mol) and 4 milliliters of nitric acid (concentration is 14 mol) mixed, and stir, sample all dissolves after 30 minutes, fixed molten with 100 milliliters volumetric flask then, get 10 ml solns and carry out ICP-AES (French JOBIN YVONJY238 type, high frequency power is 1000 watts, and gas flow is 1.04 ml/min) test, the content of non-cobalt metal element in the specimen.Test result is as shown in table 1.
Embodiment 4
Present embodiment illustrates that the dissolving method of cobaltosic oxide of the present invention reaches the wherein assay method of non-cobalt metal element content.
(be numbered ICP-04, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co with 1000 milligrams of cobaltosic oxide samples
3O
4-L-12.19) be positioned in the electric furnace, and in air atmosphere (volume content of oxygen is 21%), be warming up to 1100 ℃ and kept 6 minutes with 40 ℃/minute speed, take out sample then and naturally cool to room temperature.Then above-mentioned cobaltosic oxide sample is mixed with 15 milliliters of nitric acid (concentration is 14 mol), and stir, sample all dissolves after 30 minutes, fixed molten with 100 milliliters volumetric flask then, get 10 ml solns and carry out ICP-AES (French JOBIN YVONJY238 type, high frequency power is 1000 watts, and gas flow is 1.04 ml/min) test, the content of non-cobalt metal element in the specimen.Test result is as shown in table 1.
Embodiment 5
Present embodiment illustrates that the dissolving method of cobaltosic oxide of the present invention reaches the wherein assay method of non-cobalt metal element content.
(be numbered ICP-01, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co with 900 milligrams of cobaltosic oxide samples
3O
4-L-12.21) (machining graphite factory buys from Pingdu City East China with 100 milligrams of graphite samples, the model of product is a P15B-RH graphite) mix, be positioned in the program control cabinet-type electric furnace in oxygen atmosphere (volume content of oxygen is 30%), be warming up to 1000 ℃ and kept 10 minutes with 50 ℃/minute speed, take out sample then and naturally cool to room temperature.Then above-mentioned biased sample is mixed with 20 milliliters of hydrochloric acid (concentration is 12 mol), and stir, sample all dissolves after 25 minutes, fixed molten with 100 milliliters volumetric flask then, get 10 ml solns and carry out ICP-AES (French JOBIN YVON JY238 type, high frequency power is 1000 watts, and gas flow is 1.04 ml/min) test, the content of non-cobalt metal element in the specimen.Test result is as shown in table 1.
Embodiment 6
Present embodiment illustrates that the dissolving method of cobaltosic oxide of the present invention reaches the wherein assay method of non-cobalt metal element content.
(be numbered ICP-01, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co to dissolve the cobaltosic oxide sample according to the method for embodiment 1
3O
4-L-12.6), and measure the wherein content of non-cobalt metal element, different is, with the cobaltosic oxide sample in nitrogen atmosphere, be warming up to 1000 ℃ and kept 5 minutes with 40 ℃/minute speed, other dissolving step and testing procedure dissolved 35 minutes consuming time with embodiment 1, and test result is as shown in table 1.
Comparative Examples 1
The dissolving method of the cobaltosic oxide of this Comparative Examples explanation prior art, and the assay method of non-cobalt metal element content wherein.
(be numbered ICP-01, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co to 1000 milligrams of cobaltosic oxide samples that will be identical with embodiment 1
3O
4-L-12.6) be positioned in the beaker, at room temperature, after mixing with the mixed solution of 15 milliliters of hydrochloric acid (concentration is 12 mol) and 5 milliliters of nitric acid (concentration is 14 mol) and stirring 3.5 hours, most of cobaltosic oxide sample dissolution, still have few sample segment residue, fixed molten with 100 milliliters volumetric flask then, and after leaving standstill 5 minutes, get 10 milliliters of supernatant liquors and carry out the ICP-AES test.Instrument parameter is with embodiment 1.Test result is as shown in table 2.
Comparative Examples 2
The dissolving method of the cobaltosic oxide of this Comparative Examples explanation prior art, and the assay method of non-cobalt metal element content wherein.
(be numbered ICP-02, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co to 1000 milligrams of cobaltosic oxide samples that will be identical with embodiment 2
3O
4-L-12.11) be positioned in the beaker, at room temperature, after mixing with the mixed solution of 15 milliliters of hydrochloric acid (concentration is 12 mol) and 5 milliliters of nitric acid (concentration is 14 mol) and stirring 3.5 hours, most of cobaltosic oxide sample dissolution, still have few sample segment residue, fixed molten with 100 milliliters volumetric flask then, and after leaving standstill 5 minutes, get 10 milliliters of supernatant liquors and carry out the ICP-AES test.Instrument parameter is with embodiment 1.Test result is as shown in table 2.
Comparative Examples 3
The dissolving method of the cobaltosic oxide of this Comparative Examples explanation prior art, and the assay method of non-cobalt metal element content wherein.
(be numbered ICP-03, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co to 1000 milligrams of cobaltosic oxide samples that will be identical with embodiment 3
3O
4-L-12.18) be positioned in the beaker, at room temperature, after mixing with the mixed solution of 15 milliliters of hydrochloric acid (concentration is 12 mol) and 5 milliliters of nitric acid (concentration is 14 mol) and stirring 3.5 hours, most of cobaltosic oxide sample dissolution, still have few sample segment residue, fixed molten with 100 milliliters volumetric flask then, and after leaving standstill 5 minutes, get 10 milliliters of supernatant liquors and carry out the ICP-AES test.Instrument parameter is with embodiment 1.Test result is as shown in table 2.
Comparative Examples 4
The dissolving method of the cobaltosic oxide of this Comparative Examples explanation prior art, and the assay method of non-cobalt metal element content wherein.
(be numbered ICP-04, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co to 1000 milligrams of cobaltosic oxide samples that will be identical with embodiment 4
3O
4-L-12.19) be positioned in the beaker, at room temperature, after mixing with the mixed solution of 15 milliliters of hydrochloric acid (concentration is 12 mol) and 5 milliliters of nitric acid (concentration is 14 mol) and stirring 3.5 hours, most of cobaltosic oxide sample dissolution, still have few sample segment residue, fixed molten with 100 milliliters volumetric flask then, and after leaving standstill 5 minutes, get 10 milliliters of supernatant liquors and carry out the ICP-AES test.Instrument parameter is with embodiment 1.Test result is as shown in table 2.
Comparative Examples 5
The dissolving method of the cobaltosic oxide of this Comparative Examples explanation prior art, and the assay method of non-cobalt metal element content wherein.
(be numbered ICP-01, buy from upright prosperous metal material company limited of Zhuhai section, the model of product is Co to 900 milligrams of cobaltosic oxide samples that will be identical with embodiment 5
3O
4-L-12.21) (company of machining graphite factory buys from Pingdu City East China with 100 milligrams of graphite, the model of product is a P15B-RH graphite) biased sample be positioned in the beaker, at room temperature, after mixing with 20 milliliters about 60 ℃ hot sulfuric acid (concentration is 18 mol) and stirring 3.7 hours, most of cobaltosic oxide sample dissolution, still have few part cobaltosic oxide sample and most of graphite sample residue, fixed molten with 100 milliliters volumetric flask then, filter, remove insolubles, get 10 milliliters of filtrates and carry out the ICP-AES test.Instrument parameter is with embodiment 1.Test result is as shown in table 2.
Table 1
Table 2
Table 3
Annotate: in the table 3 in the graphite sample content of each non-cobalt metal element be the mass percentage content of each non-cobalt metal element in 1000 milligrams of graphite samples.
Because embodiment 5 and Comparative Examples 5 are and adopt the model of the product in 900 milligrams of embodiment 1 or the Comparative Examples 1 is Co
3O
4The cobaltosic oxide sample of-L-12.6 and the potpourri of 100 milligrams of above-mentioned graphite samples be as specimen, and therefore, the theoretical value of the mass percentage content of each non-cobalt metal element is calculated as and obtains according to the following equation in this sample:
M theoretical value=M1 * 90 weight %+M stones * 10 weight %.
In the formula, the M theoretical value is respectively the theoretical value of the mass percentage content of each non-cobalt metal element in the above-mentioned biased sample;
M1 is the mass percentage content of each non-cobalt metal element in the cobaltosic oxide sample of 1000 milligrams of embodiment 1 or Comparative Examples 1;
M stone is the mass percentage content of each non-cobalt metal element in 1000 milligrams of graphite samples.
For the cobaltosic oxide sample among the embodiment 1-6, wherein the content of non-cobalt metal element (impurity) can think that promptly this sample is standard compliant as long as within following ranges.
Fe＜0.010 weight %; Ca＜0.018 weight %; Pb＜0.030 weight %; Mg＜0.010 weight %; Mn＜0.010 weight %; Na＜0.050 weight %; Ni＜0.050 weight %.
Data from table 1 and table 2 adopt the reference method of method of the present invention and Comparative Examples to test the content of non-cobalt metal element in the cobaltosic oxide sample that obtains all within above-mentioned scope as can be seen.But existing reference method of testing is consuming time very long in the dissolving cobaltosic oxide, needs three hours at least, and the dissolution conditions harshness, has had a strong impact on testing efficiency.In addition, in course of dissolution, still there is sample segment to dissolve, the existence of residue has rung the accuracy of test result, therefore, adopting the reference method to test the content of the some of them non-cobalt metal element that obtains might be on the low side, this has also increased a lot of pressure to control with raw material, has reduced the reference value of test result.And adopting the time of method dissolving cobaltosic oxide of the present invention short, the dissolution conditions gentleness has improved testing efficiency greatly.In addition, method of the present invention can be dissolved cobaltosic oxide fully, does not have residue, and test result is more accurate.
Data from table 3 as can be seen, under the situation of potpourri as specimen with cobaltosic oxide and graphite, the mass percentage content that adopts method of the present invention to test each non-cobalt metal element in the sample that obtains more approaches theoretical value, therefore explanation, the result precision height that adopts method of the present invention to test.
Claims (8)
1, a kind of dissolving method of cobaltosic oxide, this method comprise cobaltosic oxide are contacted with solvent, it is characterized in that, with cobaltosic oxide with before solvent contacts, cobaltosic oxide was kept 1-20 minute down at 100-1100 ℃.
2, method according to claim 1, wherein, the described retention time is 1-10 minute.
3, method according to claim 1, wherein, the method of described maintenance comprises earlier cobaltosic oxide kept 1-5 minute down at 100-180 ℃, is warming up to 10-100 ℃/minute speed then and continues after 200-1100 ℃ to keep 1-15 minute or cobaltosic oxide directly is warming up to 100-1100 ℃ and kept 1-20 minute with 10-100 ℃/minute speed.
4, method according to claim 1, wherein, the described process that cobaltosic oxide is kept under 100-1100 ℃ is carried out in oxidizing atmosphere.
5, method according to claim 4, wherein, described oxidizing atmosphere is that the volume content of oxygen is not less than 5% oxygen-containing gas.
6, method according to claim 1, wherein, described solvent is an acid solution; Described acid solution is the mixed solution of acid and water, and described acid is selected from one or more in sulfuric acid, hydrochloric acid, nitric acid and the perchloric acid; The amount of the solvent that every gram cobaltosic oxide is required is the 10-20 milliliter.
7, method according to claim 1, wherein, this method comprises that also the temperature of described cooling is 10 a ℃-room temperature with the cooling step of cobaltosic oxide after keeping under 100-1100 ℃.
8, the assay method of non-cobalt metal element content in a kind of cobaltosic oxide, this method comprise dissolving cobaltosic oxide and carry out the atomic emission spectrum test, it is characterized in that the dissolving method of described cobaltosic oxide is the dissolving method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710130544XA CN101349623B (en) | 2007-07-16 | 2007-07-16 | Method for dissolving cobaltosic oxide and method for measuring non-cobalt metal element content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710130544XA CN101349623B (en) | 2007-07-16 | 2007-07-16 | Method for dissolving cobaltosic oxide and method for measuring non-cobalt metal element content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101349623A true CN101349623A (en) | 2009-01-21 |
| CN101349623B CN101349623B (en) | 2010-10-06 |
Family
ID=40268492
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200710130544XA Expired - Fee Related CN101349623B (en) | 2007-07-16 | 2007-07-16 | Method for dissolving cobaltosic oxide and method for measuring non-cobalt metal element content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101349623B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758844A (en) * | 2016-02-26 | 2016-07-13 | 兰州金川新材料科技股份有限公司 | Determining method for trace silicon in cobaltosic oxide |
| CN107389781A (en) * | 2017-08-25 | 2017-11-24 | 金川集团股份有限公司 | Silver-colored rapid assay methods in a kind of cobaltosic oxide, cobalt acid lithium |
| CN113189088A (en) * | 2021-05-28 | 2021-07-30 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
| CN115165861A (en) * | 2022-07-06 | 2022-10-11 | 科立鑫(珠海)新能源有限公司 | Method for measuring content of non-cobalt metal elements in cobaltosic oxide |
-
2007
- 2007-07-16 CN CN200710130544XA patent/CN101349623B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758844A (en) * | 2016-02-26 | 2016-07-13 | 兰州金川新材料科技股份有限公司 | Determining method for trace silicon in cobaltosic oxide |
| CN107389781A (en) * | 2017-08-25 | 2017-11-24 | 金川集团股份有限公司 | Silver-colored rapid assay methods in a kind of cobaltosic oxide, cobalt acid lithium |
| CN113189088A (en) * | 2021-05-28 | 2021-07-30 | 金川集团股份有限公司 | Method for measuring contents of elemental copper and zinc in cobaltosic oxide |
| CN115165861A (en) * | 2022-07-06 | 2022-10-11 | 科立鑫(珠海)新能源有限公司 | Method for measuring content of non-cobalt metal elements in cobaltosic oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101349623B (en) | 2010-10-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kumar et al. | Selective recovery of Li and FePO4 from spent LiFePO4 cathode scraps by organic acids and the properties of the regenerated LiFePO4 | |
| CN107565121B (en) | Preparation method of modified positive electrode material of lithium battery | |
| US8153032B2 (en) | Transition metal hydroxide and oxide, method of producing the same, and cathode material containting the same | |
| CN101349623B (en) | Method for dissolving cobaltosic oxide and method for measuring non-cobalt metal element content | |
| CN108428871A (en) | A kind of nickel cobalt aluminium ternary method for preparing anode material of lithium-ion battery | |
| CN107634220B (en) | Preparation method of prussian blue energy storage material | |
| CN106684374A (en) | Preparation method for porous spherical lithium nickel cobalt manganate used as ternary positive electrode material of lithium ion battery | |
| CN109148878A (en) | A kind of method, positive electrode and lithium ion battery handling the residual lithium in surface containing lithium anode material | |
| CN112582600A (en) | Preparation method of high-entropy single crystal battery positive electrode material and obtained product | |
| Rostami et al. | Recovery of lithium, cobalt, nickel, and manganese from spent lithium-ion batteries through a wet-thermal process | |
| CN113620353B (en) | Strontium titanate modified nickel cobalt lithium manganate positive electrode material and lithium ion battery containing same | |
| CN107055613B (en) | A kind of no substrate niobium pentoxide nano chip arrays negative material and its preparation method and application | |
| CN115806318A (en) | Production method of manganese sulfate | |
| CN115092970B (en) | Aluminum-doped needle-shaped cobaltosic oxide and preparation method thereof | |
| CN108285133A (en) | Phosphoric acid vanadium lithium and preparation method thereof | |
| CN114350957A (en) | Method for comprehensively recovering valuable elements from waste lithium batteries | |
| CN109037672A (en) | A kind of preparation method of power battery nickel-cobalt lithium manganate material | |
| CN115149095A (en) | High-purity silver germanite phase sulfide solid electrolyte and preparation method thereof | |
| CN114899392A (en) | Preparation method of lithium iron phosphate or lithium ferromanganese anode material of lithium ion battery | |
| CN113979420A (en) | Preparation method of aluminum-doped high-compaction long-cycle lithium iron phosphate positive electrode material | |
| CN113880100A (en) | Preparation method of lithium nickel cobalt oxide battery regenerated ternary cathode material | |
| CN113860321A (en) | Preparation method of regenerated precursor material of waste lithium cobaltate battery | |
| CN110797528A (en) | Preparation method of high-rate composite ternary cathode material | |
| CN116706026B (en) | Negative electrode material of sodium ion battery and preparation method thereof | |
| CN113353991B (en) | Lithium removal material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101006 Termination date: 20170716 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |