CN105810929A - Treatment method for reducing residual alkalis on surface of high nickel material - Google Patents
Treatment method for reducing residual alkalis on surface of high nickel material Download PDFInfo
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- CN105810929A CN105810929A CN201410845658.2A CN201410845658A CN105810929A CN 105810929 A CN105810929 A CN 105810929A CN 201410845658 A CN201410845658 A CN 201410845658A CN 105810929 A CN105810929 A CN 105810929A
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- nickel material
- washing
- high nickel
- residual alkali
- processing method
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000000463 material Substances 0.000 title claims abstract description 50
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims description 20
- 238000003672 processing method Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910013485 LiNixM1-xO2 Inorganic materials 0.000 claims description 3
- 229910013495 LiNixM1−xO2 Inorganic materials 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910015694 LiNi0.85Co0.1Al0.05O2 Inorganic materials 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- -1 phosphate anion Chemical class 0.000 description 2
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- 229910011328 LiNi0.6Co0.2Mn0.2O2 Inorganic materials 0.000 description 1
- 229910015872 LiNi0.8Co0.1Mn0.1O2 Inorganic materials 0.000 description 1
- 229910003005 LiNiO2 Inorganic materials 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 206010016766 flatulence Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a treatment method for reducing residual alkalis on the surface of a high nickel material. The treatment method for reducing residual alkalis on the surface of a high nickel material comprises the following steps: washing the high nickel material, wherein the solid-liquid ratio, the washing time and the stirring speed are strictly controlled in the washing process; drying the obtained solid phase; and sintering the dried solid phase at a certain temperature to make residual Li in a system return to the crystal lattice structure of the material in order to obtain a final high nickel material. The method can rapidly and effectively reduce the residual alkalis on the surface of the high nickel material, is a convenient and effective treatment way, and can effectively improve the processing performances and the electrochemical performances of the high nickel material.
Description
Technical field
The invention belongs to field of lithium ion battery anode, be specifically related to a kind of processing method reducing the residual alkali in high-nickel material surface.
Background technology
Lithium ion battery, with its high-energy, safe and reliable, life-span length, the advantage such as pollution-free, becomes high-energy secondary battery most promising at present.Lithium ion battery commercialization is over more than 20 year, and the actual capacity of positive electrode is hesitated between 100～180mAh/g all the time, and positive electrode specific capacity is low has become as the bottleneck promoting lithium ion battery specific energy.LiNiO2And doped compound is widely considered to be with its higher specific capacity and most possibly replaces LiCoO2Positive electrode.
High-nickel material LiNixM1-xO2(x >=0.6, M is one or more in Co, Mn, Al, Mg etc.) has that specific discharge capacity height, cost be low and the advantage such as environmental pollution is little.But owing to its surface residual lithium amount is more, cause that fruit jelly phenomenon occurs in slurry in electrode fabrication process, make to be difficult to be coated into pole piece.The defects such as to there is memory property poor for this material simultaneously, cycle performance difference, in actual battery is applied, flatulence problem seriously waits the commercialization that also have impact on material.In order to reduce the residual alkali of high-nickel material, in recent years, research staff have employed multiple anions and canons or polynary bulk phase-doped, stablizes the structure of high-nickel material, reaches to promote the effect of circulation and memory property.Prevent electrolyte to positive pole material corrosion additionally, cladding is also one, promote the effective ways of material circulation and storage stability.Chinese patent CN102881911A discloses a kind of employing phosphate anion and forms Li with rich nickel material surface lithium residue3PO4Precipitation removes the method for the residual alkali in surface, but owing to needing too much phosphate anion to be converted by lithium residue, therefore at the inert substance that high-nickel material Surface Creation is more.These methods unrealized harmless conversion thoroughly, and inherently it is not solved by the problem of high-nickel material alkaline impurities residual and complex process, seriously constrain high-nickel material large-scale application.
Summary of the invention
The technical problem to be solved is to provide a kind of mode of washing and reduces rapidly the residual alkali in high-nickel material surface, reduces processing cost, and improves processing characteristics and the chemical property of high-nickel material.
It is an object of the invention to be achieved through the following technical solutions:
A kind of processing method reducing the residual alkali in high-nickel material surface, uses solvent that high-nickel material is washed, then carries out solid-liquid separation and dry, finally calcine to obtain the high-nickel material of final low residual alkali in oxygen atmosphere at 500 ~ 700 DEG C.
Concrete, the technical program is: a kind of processing method reducing the residual alkali in high-nickel material surface, mainly comprises the steps that high-nickel material is dissolved in solvent by solid-to-liquid ratio 1:1 ~ 1:15 by (1) and washs, and wash time is 1 ~ 120min, then carries out solid-liquid separation；(2) filter cake after separating is dried at 40 DEG C ~ 120 DEG C and obtains dry powder；(3) dry powder obtained is heated in oxygen-containing atmosphere to 500 ~ 700 DEG C of calcinings, be incubated 1 ~ 15 hour, be then cooled to room temperature, finally give the high-nickel material of low residual alkali.
In above-mentioned preparation method, the high-nickel material described in step (1) has the average composition that following chemical formula is expressed:
(chemical formula 1) LiNixM1-xO2
Wherein, 0.6≤x≤1.0, M in Co, Mn, Al, Mg one or more.
In above-mentioned preparation method, the solvent described in step (1) is at least one in deionized water, ethanol.
In above-mentioned preparation method, the washing described in step (1) is one or more in drip washing, pulping and washing, filter pressing washing, immersion；Wherein, when described washing is drip washing, wash time is 1 ~ 60min；When described washing is pulping and washing, wash time is 10 ~ 120min；When described washing is washing by soaking, wash time is 5 ~ 120min.
The technical problem to be solved is to provide a kind of mode of washing and reduces rapidly high-nickel material surface lithium residual, and sintering makes the Li of residual in system back within material lattice structure when by uniform temperature, it is a kind of convenient effective process means, can effectively improve nickelic drawing abillity and chemical property.
Accompanying drawing explanation
Accompanying drawing 1 is cycle performance comparison diagram under 1C multiplying power before and after the residual alkali in carrying out washing treatment high-nickel material surface in embodiment 1.
Embodiment
Embodiment 1:
By high-nickel material LiNi0.85Co0.1Al0.05O2Being placed in pumping and filtering device, when sucking filtration, solid-to-liquid ratio is that it is carried out quick drip washing by the deionized water of 1:15, and the drip washing time is 2min, is dried by the filter cake after separating in vacuum drying oven, and oven temperature is 120 DEG C.The dry powder obtained is heated in oxygen-containing atmosphere to 600 DEG C, be incubated 5 hours, then naturally cool to room temperature, finally give the high-nickel material of low residual alkali.
By raw material high-nickel material LiNi0.85Co0.1Al0.05O2And the product after washing is assembled into button cell respectively, within the scope of 3.0 ~ 4.3V, carry out discharge and recharge.Fig. 1 is cycle performance comparison diagram under 1C multiplying power, it can be seen that removes the material circulation performance after the residual lithium in surface and is greatly improved.
Embodiment 2:
By LiNi0.85Co0.1Al0.05O2Joining in deionized water by solid-to-liquid ratio 1:5, stirring 30min forms slurry, and sucking filtration in above-mentioned slurry is made solid-liquid sharp separation.Filter cake after separating is dried at 100 DEG C.The dry powder obtained is heated in oxygen-containing atmosphere to 700 DEG C, be incubated 4 hours, then naturally cool to room temperature, finally give the high-nickel material of low residual alkali.
Embodiment 3:
By LiNi0.6Co0.2Mn0.2O2Join in deionized water by solid-to-liquid ratio 1:10, after infiltration 60min, carry out sucking filtration and make solid-liquid sharp separation.Filter cake after separating is dried at 100 DEG C.The dry powder obtained is heated in oxygen-containing atmosphere to 630 DEG C, be incubated 6 hours, then naturally cool to room temperature, finally give the high-nickel material of low residual alkali.
Embodiment 4:
By LiNi0.8Co0.1Mn0.1O2Joining in alcoholic solution by solid-to-liquid ratio 1:1, stirring 80min forms slurry, then by above-mentioned slurry sucking filtration, makes solid-liquid sharp separation.Solid phase after separating is dried at 40 DEG C.The dry powder obtained is heated in oxygen-containing atmosphere to 500 DEG C, be incubated 10 hours, then naturally cool to room temperature, finally give the high-nickel material of low residual alkali.
Claims (5)
1. reduce a processing method for the residual alkali in high-nickel material surface, use solvent that high-nickel material is washed, then carry out solid-liquid separation and dry, in oxygen atmosphere, finally at 500 ~ 700 DEG C, calcine to obtain the high-nickel material of final low residual alkali.
2. the processing method of the residual alkali in reduction high-nickel material surface according to claim 1, it is characterised in that described high-nickel material has the average composition that following chemical formula is expressed:
(chemical formula 1) LiNixM1-xO2
Wherein, 0.6≤x≤1.0, M in Co, Mn, Al, Mg one or more.
3. the processing method of the residual alkali in reduction high-nickel material surface according to claim 1, it is characterized in that high-nickel material is carried out washing and washs in solvent for being joined by solid-to-liquid ratio 1:1 ~ 1:15 by high-nickel material by described use solvent, wash time is 1 ~ 120min.
4. the processing method reducing the residual alkali in high-nickel material surface according to claim 1 or 3, it is characterised in that the solvent described in step is at least one in deionized water, ethanol.
5. the processing method reducing the residual alkali in high-nickel material surface according to claim 1 or 3, it is characterised in that described washing is one or more in drip washing, pulping and washing, filter pressing washing, immersion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410845658.2A CN105810929A (en) | 2014-12-31 | 2014-12-31 | Treatment method for reducing residual alkalis on surface of high nickel material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410845658.2A CN105810929A (en) | 2014-12-31 | 2014-12-31 | Treatment method for reducing residual alkalis on surface of high nickel material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105810929A true CN105810929A (en) | 2016-07-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410845658.2A Pending CN105810929A (en) | 2014-12-31 | 2014-12-31 | Treatment method for reducing residual alkalis on surface of high nickel material |
Country Status (1)
| Country | Link |
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| CN (1) | CN105810929A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107968193A (en) * | 2017-11-22 | 2018-04-27 | 江门市科恒实业股份有限公司 | A kind of preparation method and battery of high power capacity tertiary cathode material |
| CN108063245A (en) * | 2017-10-30 | 2018-05-22 | 广东邦普循环科技有限公司 | A kind of method for reducing rich nickel ternary material surface lithium impurity |
| CN108878863A (en) * | 2018-06-01 | 2018-11-23 | 合肥国轩高科动力能源有限公司 | Method for improving surface residual alkalinity of ternary positive electrode material of lithium ion battery |
| CN109546088A (en) * | 2018-11-19 | 2019-03-29 | 常州大学 | A kind of nickelic tertiary cathode material method for washing |
| CN109713228A (en) * | 2019-01-04 | 2019-05-03 | 南通瑞翔新材料有限公司 | A kind of washing drop alkali method that lithium ion battery ternary material is recyclable |
| CN110040791A (en) * | 2019-04-30 | 2019-07-23 | 合肥国轩高科动力能源有限公司 | Ternary cathode material and preparation method thereof |
| CN111422922A (en) * | 2020-02-25 | 2020-07-17 | 蜂巢能源科技有限公司 | Positive electrode material and preparation method and application thereof |
| CN112340783A (en) * | 2020-09-30 | 2021-02-09 | 宜宾锂宝新材料有限公司 | Modification method for reducing residual alkali on surface of high-nickel ternary cathode material, high-nickel ternary cathode material prepared by modification method and lithium ion battery |
| CN113394390A (en) * | 2020-03-11 | 2021-09-14 | 中国石油化工股份有限公司 | Method for reducing alkali residue of high-nickel ternary material of lithium ion battery |
| CN114682575A (en) * | 2022-05-31 | 2022-07-01 | 宜宾锂宝新材料有限公司 | Method for reducing residual alkali on surface of high-nickel anode material, obtained material and application |
| CN115557542A (en) * | 2022-09-27 | 2023-01-03 | 万华化学(四川)电池材料科技有限公司 | Preparation method of high-nickel ternary cathode material with low residual alkali |
| WO2023231448A1 (en) * | 2022-05-31 | 2023-12-07 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method for positive and negative electrode materials, and lithium-ion battery |
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| CN102683672A (en) * | 2012-01-06 | 2012-09-19 | 吉安市优特利科技有限公司 | Method for decreasing pH value of ternary material |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108063245A (en) * | 2017-10-30 | 2018-05-22 | 广东邦普循环科技有限公司 | A kind of method for reducing rich nickel ternary material surface lithium impurity |
| CN108063245B (en) * | 2017-10-30 | 2020-06-30 | 广东邦普循环科技有限公司 | Method for reducing lithium impurities on surface of nickel-rich ternary material |
| CN107968193A (en) * | 2017-11-22 | 2018-04-27 | 江门市科恒实业股份有限公司 | A kind of preparation method and battery of high power capacity tertiary cathode material |
| CN108878863A (en) * | 2018-06-01 | 2018-11-23 | 合肥国轩高科动力能源有限公司 | Method for improving surface residual alkalinity of ternary positive electrode material of lithium ion battery |
| CN109546088A (en) * | 2018-11-19 | 2019-03-29 | 常州大学 | A kind of nickelic tertiary cathode material method for washing |
| CN109713228A (en) * | 2019-01-04 | 2019-05-03 | 南通瑞翔新材料有限公司 | A kind of washing drop alkali method that lithium ion battery ternary material is recyclable |
| CN109713228B (en) * | 2019-01-04 | 2021-07-23 | 南通瑞翔新材料有限公司 | Recyclable washing alkali reduction method for ternary material of lithium ion battery |
| CN110040791A (en) * | 2019-04-30 | 2019-07-23 | 合肥国轩高科动力能源有限公司 | Ternary cathode material and preparation method thereof |
| CN110040791B (en) * | 2019-04-30 | 2021-10-08 | 合肥国轩高科动力能源有限公司 | Ternary cathode material and preparation method thereof |
| CN111422922A (en) * | 2020-02-25 | 2020-07-17 | 蜂巢能源科技有限公司 | Positive electrode material and preparation method and application thereof |
| CN113394390B (en) * | 2020-03-11 | 2024-05-17 | 中国石油化工股份有限公司 | Method for reducing residual alkali of high-nickel ternary material of lithium ion battery |
| CN113394390A (en) * | 2020-03-11 | 2021-09-14 | 中国石油化工股份有限公司 | Method for reducing alkali residue of high-nickel ternary material of lithium ion battery |
| CN112340783A (en) * | 2020-09-30 | 2021-02-09 | 宜宾锂宝新材料有限公司 | Modification method for reducing residual alkali on surface of high-nickel ternary cathode material, high-nickel ternary cathode material prepared by modification method and lithium ion battery |
| WO2023231448A1 (en) * | 2022-05-31 | 2023-12-07 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method for positive and negative electrode materials, and lithium-ion battery |
| CN114682575A (en) * | 2022-05-31 | 2022-07-01 | 宜宾锂宝新材料有限公司 | Method for reducing residual alkali on surface of high-nickel anode material, obtained material and application |
| CN115557542A (en) * | 2022-09-27 | 2023-01-03 | 万华化学(四川)电池材料科技有限公司 | Preparation method of high-nickel ternary cathode material with low residual alkali |
| CN115557542B (en) * | 2022-09-27 | 2023-12-29 | 万华化学(四川)电池材料科技有限公司 | Preparation method of low-residual-alkali high-nickel ternary cathode material |
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Application publication date: 20160727 |