CN108946799A - The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate - Google Patents
The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate Download PDFInfo
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- CN108946799A CN108946799A CN201811126060.2A CN201811126060A CN108946799A CN 108946799 A CN108946799 A CN 108946799A CN 201811126060 A CN201811126060 A CN 201811126060A CN 108946799 A CN108946799 A CN 108946799A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2006/40—Electric properties
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention is a kind of method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate.The technical solution of use: the following steps are included: mixing: the titanium dioxide of out-phase containing rutile and lithium carbonate being taken to compare ingredient according to 1:0.37-0.40 mass, it is added in distilled water, polyethylene glycol is added, said mixture material is sanded through zirconium ball again, it is 2-4 hours that the time, which is sanded, obtains lithium titanate precursor slurry；It is dry: above-mentioned lithium titanate precursor slurry is transferred to 80-90 DEG C of drying with water bath of progress, drying time 4-6 hour in drying with water bath device；High-temperature process: material needs to carry out two sections of high temperature sintering processing after drying and grinding, and leading portion sintering is by presoma material after drying and grinding, in 550 DEG C of -650 DEG C of processing；Back segment sintering are as follows: material after cooling tentatively be crushed into 150 mesh screens, 600 DEG C of lasting 3h sintering are then carried out, finally in 730 DEG C~750 DEG C continuous sintering 12h.
Description
Technical field
The invention belongs to lithium ion battery production technology field, specifically a kind of titanium dioxide of out-phase containing rutile synthesizes titanium
The method of sour lithium.
Background technique
Currently, lithium electricity New Energy Industry is rapid, and in the case where country widelys popularize, high energy density cells are fast with high current
Fast charge and discharge battery is vigorously advocated by country, and lithium titanate material is due to its volume " zero strain ", cycle performance is superior and environment
Close friend etc., and more applied in terms of rate battery research and development, while in terms of newest sodium-ion battery research, lithium titanate
Material is also proven to have sodium ion storage effect.
The main synthesis material of lithium titanate material is titanium dioxide and lithium salts, and common model mainly wants anatase structured and golden
Red stone structure, it is anatase structured when using titanium dioxide as lithium titanate battery material reaction raw materials, it is proved to be more suitable for titanium
The preparation of sour lithium material.Early stage as materials such as lithium titanate and titanium dioxide prepares enterprise, and the special rich new material science and technology in Jiangsu has
The solid sharp preferential company of power science and technology of limit company and alliance of CITIC Guoan has done numerous studies to the preparation of lithium titanate material and has known
Know property right protection,
Meng Guli company of CITIC Guoan: patent " industrial synthesis method for lithium titanate 201010236451.7 " is by lithium salts and titanium dioxide
Organic solvent pretreatment is used respectively；It is obtained with a scattered manner for the ratio ingredient of 0.7-0.9 and after mixing dispersion in lithium titanium molar ratio
Presoma；Presoma is put into Muffle furnace to heat, 500-700 DEG C of heating temperature, heating time 1-12 hour;Natural cooling
Lithium titanate material is obtained to room temperature." the lithium titanate material preparation method 201210334372.9 of high-tap density " by lithium source,
Titanium source, fluxing agent and dispersing agent ball mill mixing by a certain percentage, it is dry after low temperature presintering, it is cooling after high-temperature calcination generate metatitanic acid
Lithium." a kind of preparation method 201210359963.1 for synthesizing lithium titanate nanosphere " mixes titanium dioxide and water or organic solvent
It closes, using TiO2 nanosphere is obtained after mist projection granulating, is mixed after gained TiO2 nanosphere is heat-treated with lithium salts, passed through
High-temperature process obtains Li4Ti5O12 nanosphere.
A kind of patent of Jiangsu Te Feng new material Science and Technology Ltd.: " synthesis preparation method of lithium titanate
201710477521.X " pre-process lithium carbonate and titanium dioxide with dehydrated alcohol respectively；Again by processed lithium carbonate and two
Titanium oxide for the ratio ingredient of 0.5-1.2 and obtains presoma after mixing dispersion with a scattered manner in lithium titanium molar ratio；Then will before
It drives body and is put into batch-type furnace heat treatment, generate lithium titanate after 600 DEG C of coolings of heating temperature.A kind of " high capacity lithium titanate material system
Preparation Method 201710526344.X ": by lithium source, titanium source, fluxing agent and dispersing agent ball mill mixing by a certain percentage, it is dry after low temperature
Pre-burning, high-temperature calcination generates lithium titanate after cooling.
Even in the major customer enterprise of lithium titanate, such as Yin Long new energy limited liability company, also to lithium titanate patent
Carried out related layouts, patent " preparation method 201610592460.7 of lithium titanate " by the lithium salts of titanium-oxide-coated, incendiary agent,
Oxidant is according to molar ratio Ti: incendiary agent: oxidant is 1:(1.34~4.5): (1.34~4.5) are pressed into base after mixing
The green body is placed in air and is preheated to certain temperature with certain heating rate by body, causes green body burning, ultimately produces titanium
Sour lithium material.Patent " a kind of lithium titanate composite material and preparation method thereof, negative electrode tab and lithium ion battery
201711145359.8 " material preparation has been carried out by following steps: 1) preparing ruthenic oxide/titanium dioxide compound；2) with
Ruthenic oxide/titanium dioxide compound, lithium source are raw material, prepare lithium titanate composite material.
In above-mentioned many patents, applicant has been concentrated on to lithium source and titanium source ratio, oxidant, cosolvent and spraying
It is granulated the research of material form etc., it is the problem of without practical concern titanium dioxide actual production process and right
The performance of lithium titanate influences；Conventional titanium dioxide (titanium dioxide) manufacturer, actual production process are commonly present a small amount of golden red
Stone is mutually mixed into or is grown in anatase titania, and in view of the difference of Rutile Type and anatase structures, it is such
Situation often makes the big heavy discount of lithium titanate anode material chemical property obtained, and this patent passes through to current domestic industry type of production
Anatase titania sets out, and solves the problems, such as the anatase titanium dioxide containing a small amount of rutile structure in lithium titanate synthesis,
Good result is obtained, lithium titanate anode material is prepared for industrial production and provides the necessary technical support.
Summary of the invention
A kind of method for being designed to provide the titanium dioxide of out-phase containing rutile synthesis lithium titanate of the content of present invention, passes through
Mixing and leading portion preheating using lithium salts solve the problems, such as that industrial rutile titania mineral facies are unpurified, finally go out materials serve
Best electrochemical performance.
The purpose of the present invention can be achieved through the following technical solutions:
The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate, comprising the following steps:
(1) mixing: take the titanium dioxide of out-phase containing rutile and lithium carbonate as fundamental reaction object, by the two according to 1:0.37-
0.40 mass ratio carries out ingredient, while being added in distilled water, and solid content exists control titanium dioxide in the mixture with lithium carbonate
Then the polyethylene glycol for accounting for said mixture gross mass 0.2-0.4% ratio is added in 45%-50%, then by said mixture material through zirconium
Ball is sanded, and it is 2-4 hours that the time, which is sanded, obtains lithium titanate precursor slurry；
(2) dry: above-mentioned lithium titanate precursor slurry is transferred to 80-90 DEG C of drying with water bath of progress in drying with water bath device, it is dry
Time 4-6 hour finally grinds the material after drying；
(3) high-temperature process: material needs to carry out two sections of high temperature sintering processing after drying and grinding,
Leading portion sintering is by presoma material after drying and grinding, and in 550 DEG C of -650 DEG C of processing, the processing time is 3-6 hours, then
Natural cooling；
Back segment sintering are as follows: material after cooling tentatively be crushed into 150 mesh screens, 600 DEG C of lasting 3h sintering are then carried out, finally exist
730 DEG C~750 DEG C continuous sintering 12h.
Preferably, titanium dioxide is anatase structured titanium dioxide in the step (1)；
Preferably, polyethylene glycol is one of PEG400, PEG800, PEG1000 in the step (1) or theirs is mixed
Close object.
Preferably, sand mill zirconium ball size is 0.3-0.4 μm or 0.5-0.6 μm in the step (1)；
Preferably, drying with water bath device is water-bath magnetic stirring apparatus or electric stirring water-bath in the step (2).
Beneficial effects of the present invention: the method for the present invention can be pre-processed by mixing with carbonic acid lithium source and leading portion high temperature,
Solving the mutually impure bring of anatase titania object present in current industrial processes influences, and avoids final metatitanic acid
The problem that lithium material performance is not in full use and titanium dioxide production purification difficulty is big；Change relative to industrialized purification
Into this method has more economical Practical significance.
Detailed description of the invention
Fig. 1 is the SEM figure that the specific embodiment of the invention one obtains pole piece.
Fig. 2 is the SEM figure that specific comparative example one of the invention obtains pole piece.
Fig. 3 is the button electricity 1C gram volume comparison of the specific embodiment of the invention one and comparative example one.
Fig. 4 is the XRD material phase analysis comparison of the specific embodiment of the invention one and comparative example one.
Specific embodiment
Present invention is further described in detail in the following with reference to the drawings and specific embodiments.
Test object of the invention is lithium ion battery metatitanic acid pole piece.
Specific embodiment one
The anatase titania (Shanghai, anatase) for choosing domestic titanium dioxide producer production, using it with lithium carbonate as basic
The two is carried out ingredient according to 5.2816: 1.9936 mass ratio by reactant, and above-mentioned material is added in distilled water, after mixing
Material solid content be 50%, add the polyethylene glycol (PEG-400) for accounting for 0.4% ratio of gross mass;
By said mixture material after zirconium ball is sanded 2 hours, lithium titanate precursor slurry is obtained；
90 DEG C of drying with water baths of progress in rotary evaporator are transferred to, finally the material after drying is ground, is then put
In being sintered in Muffle furnace；
Sintering processes are sintered first, in accordance with 600 DEG C of time 3h of sintering process of pure phase anatase structure, and high temperature sintering terminates
Afterwards, natural cooling is most crushed through airslide disintegrating mill afterwards, and sieving, then row are sintered 3 hours according to above-mentioned 600 DEG C, then at 730 DEG C
Sintering 12 hours, finally obtains lithium titanate finished product.
Specific embodiment two
The anatase titania (Shanghai, anatase) for choosing domestic titanium dioxide producer production, using it with lithium carbonate as basic
It is carried out ingredient according to 5.2816: 1.9936 mass ratio, said mixture material is added in distilled water, is obtained by reactant
The mixture of solid content 50% adds the polyethylene glycol (PEG-1000) for the 0.2% gross mass ratio that accounts for；
Mixed material obtains lithium titanate precursor slurry after zirconium ball is sanded 2 hours；
90 DEG C of drying with water baths of progress in rotary evaporator are transferred to, in Muffle after finally grinding the material after drying
Sintering in furnace；
It is sintered first, in accordance with 600 DEG C of -6h of sintering process of pure phase anatase structure, after high temperature sintering, natural cooling,
Finally after being smashed by air jet mill, after sieving, then row, according to 600 DEG C of sintering 3h, then 730 DEG C of sintering 12h, which are sintered, obtains
Obtain lithium titanate finished product.
Comparative example one
Choose and be the same as example 1 the raw material of specification and carry out, titanium dioxide and lithium carbonate as fundamental reaction object, by its according to
5.2816: 1.9936 mass ratio carries out ingredient, while the polyethylene glycol (PEG-400) of 0.4% gross mass ratio is added, mixing
Material is added in distilled water, in the mixture for being 50% by above-mentioned solid content after zirconium ball is sanded 2 hours, obtains lithium titanate forerunner
Somaplasm material is transferred in rotary evaporator 90 DEG C of drying with water baths of progress, after finally the material after drying is ground in
In Muffle furnace, sintering process is according to above-mentioned 600 DEG C of sintering 3h, and then 730 DEG C of sintering 12h, final to obtain lithium titanate finished product.
The mixing of carbonic acid lithium source and the pretreatment of leading portion high temperature, by the rutile out-phase titanium dioxide in anatase titania
Ingredient handles calcination processing, and avoiding single sintering process from leading to rutile out-phase titanium dioxide, there are brings in finished-product material
The problem of reducing material property.
The technique that the early period of addition, sintering process was changed in production can carry out directly, effective solution titanium dioxide
The purification problem in production process is produced, this method has more economical Practical significance, is suitble to promote the use of.
Claims (4)
1. a kind of method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate, which comprises the following steps:
(1) mixing: take the titanium dioxide of out-phase containing rutile and lithium carbonate as fundamental reaction object, by the two according to 1:0.37-
0.40 mass ratio carries out ingredient, while being added in distilled water, and solid content exists control titanium dioxide in the mixture with lithium carbonate
Then the polyethylene glycol for accounting for said mixture gross mass 0.2-0.4% ratio is added in 45%-50%, then by said mixture material through zirconium
Ball is sanded, and it is 2-4 hours that the time, which is sanded, obtains lithium titanate precursor slurry；
(2) dry: above-mentioned lithium titanate precursor slurry is transferred to 80-90 DEG C of drying with water bath of progress in drying with water bath device, it is dry
Time 4-6 hour finally grinds the material after drying；
(3) high-temperature process: material needs to carry out two sections of high temperature sintering processing after drying and grinding,
Leading portion sintering is by presoma material after drying and grinding, and in 550 DEG C of -650 DEG C of processing, the processing time is 3-6 hours, then
Natural cooling；
Back segment sintering are as follows: material after cooling tentatively be crushed into 150 mesh screens, 600 DEG C of lasting 3h sintering are then carried out, finally exist
730 DEG C~750 DEG C continuous sintering 12h.
2. the method for the titanium dioxide of out-phase containing rutile synthesis lithium titanate according to claim 1, which is characterized in that described
Titanium dioxide is anatase structured titanium dioxide in step (1)；
The method of the titanium dioxide of out-phase containing rutile synthesis lithium titanate according to claim 1, which is characterized in that the step
Suddenly polyethylene glycol is one of PEG400, PEG800, PEG1000 or their mixture in (1).
3. the method for the titanium dioxide of out-phase containing rutile synthesis lithium titanate according to claim 1, which is characterized in that described
Sand mill zirconium ball size is 0.3-0.4 μm or 0.5-0.6 μm in step (1).
4. the method for the titanium dioxide of out-phase containing rutile synthesis lithium titanate according to claim 1, which is characterized in that described
Drying with water bath device is water-bath magnetic stirring apparatus or electric stirring water-bath in step (2).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174197A (en) * | 2020-09-29 | 2021-01-05 | 攀钢集团研究院有限公司 | Method for preparing lithium battery negative electrode material lithium titanate by taking titanium tetrachloride as raw material |
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| CN112174197A (en) * | 2020-09-29 | 2021-01-05 | 攀钢集团研究院有限公司 | Method for preparing lithium battery negative electrode material lithium titanate by taking titanium tetrachloride as raw material |
| CN112174197B (en) * | 2020-09-29 | 2022-05-24 | 攀钢集团研究院有限公司 | Method for preparing lithium battery cathode material lithium titanate by taking titanium tetrachloride as raw material |
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Application publication date: 20181207 |