CN109411742A - The method for preparing lithium battery material - Google Patents
The method for preparing lithium battery material Download PDFInfo
- Publication number
- CN109411742A CN109411742A CN201811240405.7A CN201811240405A CN109411742A CN 109411742 A CN109411742 A CN 109411742A CN 201811240405 A CN201811240405 A CN 201811240405A CN 109411742 A CN109411742 A CN 109411742A
- Authority
- CN
- China
- Prior art keywords
- composition
- aquo
- lithium
- metal ion
- partly
- 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.)
- Withdrawn
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of methods for preparing lithium battery material, comprising: the lithium-containing materials roasted with flooding acid, to obtain the Aquo-composition for including Li+ and at least one metal ion;React the Aquo-composition comprising Li+ at least one Aquo-composition reacting metal ion with alkali, until the ph value of reactant is met reactant and precipitated at least one metal ion in the form of at least one hydroxide at least partly to obtain sediment and Aquo-composition comprising at least one hydroxide, and the Aquo-composition is separated with the sediment;Then make the Aquo-composition and contacts ionic exchange resin containing Li+, to at least partly remove at least one metal ion from the composition, to obtain the Aquo-composition of lithium-containing compound, electrolysis or electrodialysis then are carried out to obtain the lithium battery material containing at least partly lithium hydroxide to the Aquo-composition of the lithium compound.
Description
Technical field
The present invention relates to field of new energy technologies, in particular to a kind of method for preparing lithium battery material.
Background technique
It is employed so far for electrolysis (such as United States Patent (USP) that the method that production prepares lithium battery material usually utilizes lithium chloride
Described by 3597340), or lithium carbonate is converted (such as the institute of United States Patent (USP) 8691169 and 8669260 for lithium chloride by soda ash
Description), then with white lime by the lithium carbonate causticization being thusly-formed (as described in United States Patent (USP) 4207297).
The above method of known prior art is relatively expensive and inefficient.For example, single water is generated from the electrolysis of lithium chloride
Conjunction lithium hydroxide utilizes the electricity of the very high amount of about > 5,000KWh/MT LiOH.H2O and the current efficiency lower than 65%, referring to
U.S. Patent Publication case 2012/0107210.It is expensive for generating LiOH.H2O from lithium carbonate using white lime causticization, because its
Lithium carbonate is generated firstly the need of from lithium chloride, expensive purifying white lime is then used to carry out causticization as raw material.This transfers to produce
Raw relatively impure monohydrate lithium hydroxide product.Calcium impurities are introduced in the lattice of LiOH.H2O by white lime, must be led to
Expensive known method purifying is crossed, and then increases production cost.This is attempting to generate high-purity LITHIUM BATTERY monohydrate lithium hydroxide,
It is especially problematic when as having greater than the monohydrate lithium hydroxide of 99.9 weight % purity.
Method of the invention is substantially to overcome one or more in the above problem relevant to prior art approach, or extremely
Its applicable alternative solution is provided less as a target.
The aforementioned discussion of background technique is intended merely to be easy to understand the present invention.The material referred to is not approved or is recognized in this discussion
Any one of be in the priority date of the application or be once public common sense a part.
Summary of the invention
The invention proposes a kind of methods for preparing lithium battery material, which comprises is contained with what flooding acid roasted
Lithium material, to obtain the Aquo-composition for including Li+and at least one metal ion;Make comprising Li+the aqueous combination
Object is reacted at least one Aquo-composition reacting metal ion with alkali, until the ph value of reactant meets reactant at least
At least one metal ion is precipitated in the form of at least one hydroxide partly to obtain includes at least one
The sediment and Aquo-composition of hydroxide, and the Aquo-composition is separated with the sediment;
Then make it is described containing Li+Aquo-composition and contacts ionic exchange resin, thus at least partly from the composition
At least one metal ion of middle removing, so that the Aquo-composition of lithium-containing compound is obtained, then to the institute of the lithium compound
It states Aquo-composition and carries out electrolysis or electrodialysis to obtain the lithium battery material containing at least partly lithium hydroxide.
It preferably, include the lithiumation wherein being electrolysed the Aquo-composition, and in the electrolytic process
The Aquo-composition for closing object is at least substantially maintained at the pH of the value with about 9.6 to about 12.8.
Preferably, wherein being electrolysed the Aquo-composition, the Aquo-composition includes the lithium compound
PH is 7.2-14.
Preferably, wherein the Aquo-composition containing Li+and at least one metal ion is reacted with the alkali, with
Obtain the pH of about 5.2 to about 6.0.
Preferably, wherein the method includes make comprising Li+the Aquo-composition and at least one metal from
The reduction content of son is reacted with another alkali, to obtain the pH of about 9.6 to about 11.8.
Preferably, wherein the lithium-containing materials of the acid roasting are preparatory and H2 SO 4β-spodumene of reaction.
The method can reduce the energy consumption in production process.
Specific embodiment
In order to enable the objectives, technical solutions, and advantages of the present invention are more clearly understood, below in conjunction with embodiment, to this
Invention is further elaborated；It should be appreciated that described herein, the specific embodiments are only for explaining the present invention, not
For limiting the present invention.To those skilled in the art, after access is described in detail below, other systems of the present embodiment
System, method and/or feature will become obvious.All such additional systems, method, feature and advantage are intended to be included in
It in this specification, is included within the scope of the invention, and by the protection of the appended claims.In description described in detail below
The other feature of the disclosed embodiments, and these characteristic roots will be apparent according to described in detail below.
Embodiment one:
The invention proposes a kind of methods for preparing lithium battery material, which comprises the material containing lithium roasted with flooding acid
Material, to obtain the Aquo-composition for including Li+and at least one metal ion;Make comprising Li+the Aquo-composition with
At least one Aquo-composition reacting metal ion is reacted with alkali, until the ph value of reactant meets reactant at least partly
It includes at least one hydrogen-oxygen that ground, which precipitates at least one metal ion in the form of at least one hydroxide to obtain,
The sediment and Aquo-composition of compound, and the Aquo-composition is separated with the sediment;
Then make it is described containing Li+Aquo-composition and contacts ionic exchange resin, thus at least partly from the composition
At least one metal ion of middle removing, so that the Aquo-composition of lithium-containing compound is obtained, then to the institute of the lithium compound
It states Aquo-composition and carries out electrolysis or electrodialysis to obtain the lithium battery material containing at least partly lithium hydroxide.
It preferably, include the lithiumation wherein being electrolysed the Aquo-composition, and in the electrolytic process
The Aquo-composition for closing object is at least substantially maintained at the pH of the value with about 9.6 to about 12.8.
Preferably, wherein being electrolysed the Aquo-composition, the Aquo-composition includes the lithium compound
PH is 7.2-14.
Preferably, wherein the Aquo-composition containing Li+and at least one metal ion is reacted with the alkali, with
Obtain the pH of about 5.2 to about 6.0.
Preferably, wherein the method includes make comprising Li+the Aquo-composition and at least one metal from
The reduction content of son is reacted with another alkali, to obtain the pH of about 9.6 to about 11.8.
Preferably, wherein the lithium-containing materials of the acid roasting are preparatory and H2 SO 4β-spodumene of reaction.
Embodiment two:
This example is continuing with the method for preparing lithium battery material, which comprises contains lithium with what flooding acid roasted
Material, to obtain the Aquo-composition for including Li+and at least one metal ion;Make comprising Li+the Aquo-composition
It is reacted at least one Aquo-composition reacting metal ion with alkali, to obtain the pH of about 4.5 to about 6.5, thus at least
At least one metal ion is precipitated in the form of at least one hydroxide partly to obtain includes at least one
The sediment and Aquo-composition of hydroxide it includes Li+and have containing for at least one metal ion reduced
Amount, and the Aquo-composition is separated with the sediment;Optionally make it is described containing Li+Aquo-composition with it is described
The reduction content of at least one metal ion is reacted with another alkali.In order to obtain the pH of about 9.5 to about 11.5, and appoint
Selection of land at least one metal carbonate, at least partly precipitate at least one metal ion optionally at least one carbonic acid
The form of salt exists, to obtain the optionally sediment comprising at least one carbonate and comprising Li+and with reduction
The Aquo-composition of at least one metal ion content, and the Aquo-composition and Aquo-composition precipitating are divided
From;Make it is described containing Li+Aquo-composition and the ion exchange resin of content reduction of at least one metal ion connect
Touching, so that at least one metal ion is at least partly removed from the composition, to obtain the aqueous of lithium-containing compound
Composition;Under conditions of being suitable for converting lithium hydroxide at least part lithium compound, provide comprising the lithiumation
The Aquo-composition for closing object carries out electrolysis or electrodialysis.Wherein the lithium-containing materials of the acid roasting are preparatory and H2 SO 4
β-spodumene of reaction.
Embodiment three.
This example prepares lithium battery material method continuing with described, comprising: the lithium-containing materials roasted with flooding acid, to obtain
It must include the Aquo-composition of Li+and at least one metal ion;Make comprising Li+the Aquo-composition and it is described at least
A kind of water-soluble composition reacting metal ion is reacted with alkali, to obtain the pH of about 4.5 to about 6.5, thus at least partly with
The form precipitating of at least one hydroxide at least one metal ion, to obtain comprising at least one hydroxide
The sediment and Aquo-composition of object, it includes Li+and have reduce at least one metal ion content, and will
The Aquo-composition is separated with the sediment;Optionally make it is described containing Li+Aquo-composition and at least one
The reduction content of metal ion is reacted with another alkali.In order to obtain the pH of about 9.5 to about 11.5, and optionally at least
A kind of metal carbonate, at least partly precipitate at least one metal ion optionally in the form of at least one carbonate
In the presence of, so as to obtain optionally comprising at least one carbonate sediment and comprising Li+and have reduce described at least
A kind of Aquo-composition of metal ion content, and the Aquo-composition is separated with the Aquo-composition.Precipitating;Make institute
State containing Li+Aquo-composition and at least one metal ion the contacts ionic exchange resin that reduces of content, thus extremely
At least one metal ion is partially removed from the composition, to obtain the Aquo-composition of lithium-containing compound;Such as
It will include institute under conditions of being suitable for converting lithium hydroxide at least part lithium compound described in claim 246
The Aquo-composition for stating lithium compound carries out electrolysis or electrodialysis.
Example IV:
In this example, the method for preparing lithium battery material includes: to be suitable for converting hydrogen-oxygen at least part lithium sulfate
Under conditions of changing lithium, the Aquo-composition comprising lithium sulfate is set to carry out electrodialysis or electrolysis, wherein in the electrodialysis or electrolysis
In the process, the Aquo-composition comprising lithium sulfate is at least substantially maintained under the pH that pH value is about 9.5 to about 12.5.Wherein exist
During the electrodialysis, the pH is at least substantially maintained at the value of about 11 to about 12.The aqueous combination comprising lithium sulfate
Object is at least substantially maintained at about 10 to about 20g/L sulfuric acid lithium concentration.Wherein during the process, electric current is at least basic
On be maintained at steady state value.Wherein voltage is at least substantially maintained at steady state value.
Embodiment five:
The method of a kind of material preparing lithium battery of this example, which comprises be suitable at least part sulfuric acid
Lithium is converted under conditions of lithium hydroxide, and the Aquo-composition comprising lithium sulfate is committed to electrolysis, wherein being electrolysed described
Cheng Zhong, the Aquo-composition include lithium.The pH value of sulfate is greater than 7.Wherein the method in the electrolytic cell comprising film into
Row, and the pH of the lithium sulfate is greater than 8.0.Wherein the pH of the lithium sulfate is greater than 8.5.
The temperature of the Aquo-composition of the sulfur acid lithium is at least substantially maintained at about 20 to about 80 DEG C of value.Wherein exist
During the method, the temperature of the Aquo-composition comprising lithium sulfate is at least substantially maintained at about 40 to about 60 DEG C
Value.Wherein during the process, electric current is at least substantially maintained at about 400 to about 600A/m 2 density.
Wherein during the process, voltage is at least substantially maintained at about 3 to about 10V steady state value.Wherein described
In electrolytic process, the pH of the Aquo-composition comprising lithium sulfate is 7-14.
Although describing the present invention by reference to various embodiments above, but it is to be understood that of the invention not departing from
In the case where range, many changes and modifications can be carried out.That is methods discussed above, system or equipment etc. show
Example.Various configurations can be omitted suitably, replace or add various processes or component.For example, in alternative configuration, can with
Described order in a different order executes method, and/or can add, and omits and/or combine the various stages.Moreover, about
The feature of certain configuration descriptions can be combined with various other configurations.Can combine in a similar way configuration different aspect and
Element.In addition, many elements are only range of the example without limiting the disclosure or claims with the development of technology.
Give detail in the description to provide to the thorough understanding for including the exemplary configuration realized.However,
Configuration can be practiced without these specific details for example, having been illustrated with well-known circuit, process, calculation
Method, structure and technology are without unnecessary details, to avoid fuzzy configuration.The description only provides example arrangement, and unlimited
The scope of the claims processed, applicability or configuration.It is used on the contrary, front will provide the description of configuration for those skilled in the art
Realize the enabled description of described technology.It, can be to the function of element without departing from the spirit or the scope of the present disclosure
It can and arrange and carry out various changes.
In addition, many operations can be in parallel or concurrently although each operation can describe the operations as sequential process
It executes.Furthermore it is possible to rearrange the sequence of operation.One process may have other steps.Furthermore, it is possible to pass through hardware, soft
Part, firmware, middleware, code, hardware description language or any combination thereof carry out the example of implementation method.When software, firmware, in
Between when realizing in part or code, program code or code segment for executing necessary task can store in such as storage medium
In non-transitory computer-readable medium, and described task is executed by processor.
To sum up, be intended to foregoing detailed description be considered as it is illustrative and not restrictive, and it is to be understood that described
Claim (including all equivalents) is intended to limit the spirit and scope of the present invention.The above embodiment is interpreted as only using
In illustrating the present invention rather than limit the scope of the invention.After the content for having read record of the invention, technology
Personnel can make various changes or modifications the present invention, these equivalence changes and modification equally fall into the claims in the present invention and limited
Fixed range.
Claims (6)
1. the method for preparing lithium battery material, which comprises the lithium-containing materials roasted with flooding acid, to be included
The Aquo-composition of Li+and at least one metal ion;Make comprising Li+the Aquo-composition contain at least one
Water composition reacting metal ion is reacted with alkali, until the ph value of reactant meets reactant at least partly at least one hydrogen
The form of oxide precipitate at least one metal ion with obtain include at least one hydroxide sediment and
Aquo-composition, and the Aquo-composition is separated with the sediment;
Then make it is described containing Li+Aquo-composition and contacts ionic exchange resin, thus at least partly from the composition
At least one metal ion of middle removing, so that the Aquo-composition of lithium-containing compound is obtained, then to the institute of the lithium compound
It states Aquo-composition and carries out electrolysis or electrodialysis to obtain the lithium battery material containing at least partly lithium hydroxide.
2. the method as described in claim 1, wherein being electrolysed the Aquo-composition, and in the electrolytic process
In, the Aquo-composition comprising the lithium compound is at least substantially maintained at the pH of the value with about 9.6 to about 12.8.
3. the method as described in claim 1, wherein being electrolysed the Aquo-composition, the Aquo-composition includes institute
The pH for stating lithium compound is 7.2-14.
4. the method as described in claim 1, wherein the Aquo-composition containing Li+and at least one metal ion and
The alkali reaction, to obtain the pH of about 5.2 to about 6.0.
5. the method as described in claim 1, wherein the method includes make comprising Li+the Aquo-composition with it is described
The reduction content of at least one metal ion is reacted with another alkali, to obtain the pH of about 9.6 to about 11.8.
6. method as claimed in claim 5, wherein the lithium-containing materials of the acid roasting are preparatory and H2 SO 4β-lithium of reaction
Pyroxene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811240405.7A CN109411742A (en) | 2018-10-24 | 2018-10-24 | The method for preparing lithium battery material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811240405.7A CN109411742A (en) | 2018-10-24 | 2018-10-24 | The method for preparing lithium battery material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109411742A true CN109411742A (en) | 2019-03-01 |
Family
ID=65469452
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811240405.7A Withdrawn CN109411742A (en) | 2018-10-24 | 2018-10-24 | The method for preparing lithium battery material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109411742A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105849047A (en) * | 2013-10-23 | 2016-08-10 | 内玛斯卡锂公司 | Processes for preparing lithium carbonate |
| CN108101077A (en) * | 2017-12-28 | 2018-06-01 | 中国地质科学院矿产综合利用研究所 | Integrated process for extracting lithium by utilizing spodumene and synthesizing mineral fertilizer |
| CN108474061A (en) * | 2016-01-12 | 2018-08-31 | 尤米科尔公司 | Metallurgical slag rich in lithium |
-
2018
- 2018-10-24 CN CN201811240405.7A patent/CN109411742A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105849047A (en) * | 2013-10-23 | 2016-08-10 | 内玛斯卡锂公司 | Processes for preparing lithium carbonate |
| CN108474061A (en) * | 2016-01-12 | 2018-08-31 | 尤米科尔公司 | Metallurgical slag rich in lithium |
| CN108101077A (en) * | 2017-12-28 | 2018-06-01 | 中国地质科学院矿产综合利用研究所 | Integrated process for extracting lithium by utilizing spodumene and synthesizing mineral fertilizer |
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Legal Events
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|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190301 |