CN106673018B - A kind of recoverying and utilizing method of waste and old lithium titanate - Google Patents
A kind of recoverying and utilizing method of waste and old lithium titanate Download PDFInfo
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- CN106673018B CN106673018B CN201611245696.XA CN201611245696A CN106673018B CN 106673018 B CN106673018 B CN 106673018B CN 201611245696 A CN201611245696 A CN 201611245696A CN 106673018 B CN106673018 B CN 106673018B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/02—Preparation by double decomposition
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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
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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
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The present invention provides a kind of recoverying and utilizing methods of waste and old lithium titanate, including：A, waste and old lithium titanate is provided, and the waste and old lithium titanate is subjected to amorphous processing, obtains amorphous waste and old lithium titanate；B, the amorphous lithium titanate mixed with water, peroxide, alkali compounds, adjust acid-base value to alkalinity, leached, lithium titanate leachate is obtained by filtration；C, by the lithium titanate leachate and precipitant mix, the first filter residue and titaniferous filtrate are obtained after ageing, filtering, the filter residue is to be precipitated containing lithium；D, the titaniferous filtrate is heated to boiling and fluidized state is kept to be precipitated completely up to solid, the second filter residue is obtained by filtration, second filter residue is obtained into metatitanic acid after pickling, washing, drying successively.Lithium carbonate is prepared using the valuable element lithium in waste and old lithium titanate, titanium dioxide is prepared using valuable element titanium, to achieve the purpose that comprehensive utilization of resources.
Description
Technical field
The present invention relates to a kind of metal material recycling field more particularly to a kind of recoverying and utilizing methods of waste and old lithium titanate.
Background technology
In recent years, with the sharp increase of battery volume of production and marketing, the recycling and processing of old and useless battery cause the extensive pass of people
Note.Lithium ion battery is widely used to the fields, wherein titanium such as electric vehicle, space flight, energy storage and small-sized movable electronic equipment
Acid lithium battery is mainly used for power battery and large-scale energy-storage battery field, fast-developing in electric vehicle and large-scale energy storage field
Today, it is necessary to pay attention to the recycling problem of lithium titanate battery.
There are mainly three types of the sources of waste and old lithium titanate：1) the lithium titanate refuse battery to fail；2) underproof metatitanic acid pole piece：
As made pole piece defective work, Yi Jibian caused by the reasons such as misoperation, crawling, de- material, dimensional discrepancy in the process
Corner material etc.；3) underproof lithium titanate powder.These waste and old lithium titanates all cannot be used directly, if however, abandoning can both waste
A large amount of valuable elements (Li and Ti), can also cause environment seriously to stain, it is therefore necessary to recycle it.However, mesh
The preceding report recycled to waste and old lithium titanate is seldom, and waste and old lithium titanate is burnt by patent 201610665778.3 again, makes titanium
Sour lithium regeneration, however firing is difficult to obtain the lithium titanate of function admirable again.To in waste and old lithium titanate lithium and titanium be subject to respectively
Using being another effective way, related report is had not yet to see, the present invention prepares lithium carbonate, titanium dioxide respectively using lithium and titanium
The high value added products such as titanium and metatitanic acid, product can be used for multiple fields.
Invention content
In view of this, the present invention provides a kind of waste and old lithium titanate that can titanium and lithium recycled and be made full use of respectively
Recoverying and utilizing method.
In order to solve the above technical problems, the technical scheme is that using a kind of recycling side of waste and old lithium titanate
Method, including：
A, waste and old lithium titanate is provided, and the waste and old lithium titanate is subjected to amorphous processing, obtains amorphous waste and old metatitanic acid
Lithium；
B, the amorphous lithium titanate mixed with water, peroxide, alkali compounds, adjust acid-base value to alkalinity, leaching
Go out, lithium titanate leachate is obtained by filtration；
C, by the lithium titanate leachate and precipitant mix, the first filter residue and titaniferous filtrate, institute are obtained after ageing, filtering
It is to be precipitated containing lithium to state filter residue；
D, the titaniferous filtrate is heated to boiling and keeps fluidized state until solid precipitation completely, is obtained by filtration second
Second filter residue is obtained metatitanic acid by filter residue after pickling, washing, drying successively.
Preferably, further include：
E, the metatitanic acid is calcined, obtains titanium dioxide.
Preferably, described to calcine the metatitanic acid, obtaining titanium dioxide is specially：
E1, it metatitanic acid is calcined into 1~6h at 500~1000 DEG C obtains titanium dioxide.
Preferably, the waste and old lithium titanate of offer is specially：The calcining of waste and old metatitanic acid pole piece is removed into no-bonder and conduction
Agent, and waste and old lithium titanate is removed from the pole piece.
Preferably, described to calcine waste and old metatitanic acid pole piece except no-bonder and conductive agent are specially：
By waste and old metatitanic acid pole piece at 300~500 DEG C in air calcine 0.5~2h remove pole piece in binder and
Conductive agent.
Preferably, amorphous handle is specially：In ratio of grinding media to material (5~40):1,150~400 revs/min of rotating speed, by institute
State 1~5h of waste and old lithium titanate ball milling.
Preferably, step b is specially：
B1, by the amorphous lithium titanate and water by weight being 1:(1~5) it mixes and according to titanium elements in lithium titanate
With the molar ratio 1 of peroxide root：(2~5) peroxide is added；
B2, with alkali compounds by the pH value of the obtained systems of b1 to 8~12, then leach 10min at 20~70 DEG C
~2h, filtering, obtains lithium titanate leachate.
Preferably, the precipitating reagent is that sodium carbonate, potassium carbonate, ammonium carbonate, one or more of carbon dioxide can be with
Li reactions generate the compound of precipitation.
Preferably, the additive amount of the precipitating reagent is by carbonate：The molar ratio of Li is (1~1.3)：2.
Preferably, the pickling is specially and washes second filter residue with the dust technology of 0.5wt%~2wt% or dilute hydrochloric acid
It washs.
The underproof lithium titanate powder of performance or underproof lithium titanate are given up pole piece (because of misoperation, coating by the present invention
The reasons such as unevenness, de- material, off-dimension cause) and valuable element lithium in waste and old lithium titanate battery and titanium carry out it is effective
It utilizes, lithium carbonate, metatitanic acid and titanium dioxide three classes product can be prepared.First metatitanic acid pole piece is calcined, is removed viscous in pole piece
Agent and conductive agent are tied, binder is made to lose cementation, so that the active material lithium titanate on pole piece and aluminium foil or copper foil
Separation, aluminium foil or copper foil separately make metal recovery processing.
The recoverying and utilizing method of waste and old lithium titanate provided by the invention, first by waste and old lithium titanate mechanical activation to amorphous
Structure, then using peroxide root as complexing agent, generate peroxide titanium complex stable at room temperature；The pH value of regulation system is alkali simultaneously
Property so that the lithium in lithium titanate is also dissolved in system, is made titanium and lithium while being leached.Add precipitating reagent so that lithium ion with
Carbonate reaction generates lithium carbonate precipitation, and peroxide titanium complex is very stable at room temperature at this time, and titanium is still deposited in the form of a solution
, therefore solid-liquor separation can detach lithium-titanium, and precipitation is calcined up to lithium carbonate.Filtrate is peroxide titanium complex, heating
Peroxotitanium complexes titanium to after boiling starts to hydrolyze, and it is anti-that ion exchange occurs after the second precipitation weak acid scrubbing of formation
It answers, metatitanic acid is generated, up to titanium dioxide after metatitanic acid calcining.
In summary the present invention compare the prior art the advantages of be：
(1) present invention provides new for the recycling of waste and old lithium titanate, waste and old metatitanic acid pole piece and lithium titanate battery
Approach, added value of product are high, at the same to economizing on resources, environmental protection there is positive effect.
(2) waste and old lithium titanate is leached at normal temperatures under alkaline condition using peroxide root complexometry, is not necessarily to high temperature
High pressure, leaching velocity is fast, and leaching rate is high (titanium, lithium leaching almost all leach), and titanium, the rate of recovery of lithium are high, and alkaline condition pair is set
Standby corrosion is small (relative to acidity), therefore equipment requirement is relatively low, can reduce production cost, be easy to industrialized production.
(3) three kinds of lithium carbonate, metatitanic acid, titanium dioxide products can be obtained simultaneously, and product purity is high.
Description of the drawings
Fig. 1, the embodiment of the present invention 1 prepare the XRD spectrum of lithium carbonate；
Fig. 2, the embodiment of the present invention 1 prepare the XRD spectrum of titanium dioxide.
Specific implementation mode
In order to make those skilled in the art more fully understand technical scheme of the present invention, With reference to embodiment
The present invention is described in further detail.
Embodiment 1
A. by waste and old metatitanic acid pole piece, calcining 1h removes binder and conductive agent in pole piece in air at 350 DEG C,
Then lithium titanate and aluminium foil are removed, waste and old lithium titanate is obtained, by waste and old lithium titanate mechanical activation 3h (ratios of grinding media to material 20:1, rotating speed
200 revs/min), obtain the amorphous lithium titanate of powdery；
B. it leaches：By lithium titanate:Deionized water quality is than 1:3 deionized water is added into amorphous lithium titanate, and stirring is equal
It is even, by peroxide root:The molar ratio 3 of Ti:1 is added the hydrogenperoxide steam generator that mass concentration is 20%, and hydrogen is then added while stirring
Sodium oxide molybdena, the pH value of regulation system then continue leaching 1h to 10 or so at 30 DEG C, and filtering obtains lithium titanate leachate；
C. lithium carbonate is prepared：By carbonate:Li molar ratios 1.1:2 sodium carbonate is added into leachate, stops after reacting 1h
Stirring is aged 8h, filters to obtain filter residue A and titaniferous filtrate, filter residue A is washed with deionized 3 times, is forged at 500 DEG C after dry
It burns 1h and obtains lithium carbonate (content 99.6%)；
D. titanium dioxide is prepared：Gained titaniferous filtrate in step c is heated to boiling, keeps boiling 0.5h that titanium is made to hydrolyze,
Filter residue B is filtered to obtain, filter residue B is washed 1 time with 1% dust technology, then is washed with deionized 1 time, by filter residue B at 100 DEG C
Dry metatitanic acid, calcines 5h at 600 DEG C by metatitanic acid and obtains titanium dioxide (Detitanium-ore-type, content 99.4%).
Embodiment 2
A. by waste and old metatitanic acid pole piece, calcining 2h removes binder and conductive agent in pole piece in air at 300 DEG C,
Then lithium titanate and aluminium foil are removed, waste and old lithium titanate is obtained, by waste and old lithium titanate mechanical activation 2h (ratios of grinding media to material 30:1, rotating speed
150 revs/min), obtain the amorphous lithium titanate of powdery；
B. it leaches：By lithium titanate:Deionized water quality is than 1:5 deionized water is added into amorphous lithium titanate, and stirring is equal
It is even, by peroxide root:The molar ratio 2 of Ti:1 is added the hydrogenperoxide steam generator that mass concentration is 30%, and ammonia is then added while stirring
Water, the pH value of regulation system then continue leaching 2h to 8 or so at 70 DEG C, and filtering obtains lithium titanate leachate；
C. lithium carbonate is prepared：By carbonate:Li molar ratios 1.3:2 are passed through carbon dioxide gas into leachate, reaction
Stop stirring after 0.5h, be aged 12h, filter to obtain filter residue A and titaniferous filtrate, filter residue A is washed with deionized 3 times, after dry
2h is calcined at 350 DEG C obtains lithium carbonate (content 99.8%)；
D. titanium dioxide is prepared：Gained titaniferous filtrate in step c is heated to boiling, keeps boiling 1h that titanium is made to hydrolyze, mistake
Filter residue B is filtered to obtain, filter residue B is washed 1 time with 0.5% dust technology, then is washed with deionized 1 time, by filter residue B at 200 DEG C
Dry metatitanic acid, calcines 2h at 900 DEG C by metatitanic acid and obtains titanium dioxide (rutile-type, content 99.7%).
Embodiment 3
A. by waste and old metatitanic acid pole piece, calcining 0.5h removes binder and conduction in pole piece in air at 500 DEG C
Then agent removes lithium titanate and copper foil, obtain waste and old lithium titanate, then by waste and old lithium titanate mechanical activation 5h (ratios of grinding media to material 5:1,
300 revs/min of rotating speed), obtain the amorphous lithium titanate of powdery；
B. it leaches：By lithium titanate:Deionized water quality is than 1:1 deionized water is added into amorphous lithium titanate, and stirring is equal
It is even, by peroxide root:The molar ratio 5 of Ti:1 is added the sodium peroxide solution that mass concentration is 10%, and hydrogen is then added while stirring
Sodium oxide molybdena, the pH value of regulation system then continue leaching 10min to 12 at 40 DEG C, and filtering obtains lithium titanate leachate；
C. lithium carbonate is prepared：By carbonate:Li molar ratios 1:2 ammonium carbonate is added into leachate, stops stirring after reacting 2h
It mixes, is aged 0.5h, filters to obtain filter residue A and titaniferous filtrate, filter residue A is washed with deionized 3 times, forged at 750 DEG C after dry
0.5h is burnt up to lithium carbonate (content 99.9%)；
D. titanium dioxide is prepared：Gained titaniferous filtrate in step c is heated to boiling, keeps boiling 10min that titanium is made to hydrolyze,
Filter residue B is filtered to obtain, filter residue B is washed 1 time with 2% dilute hydrochloric acid, then is washed with deionized 1 time, filter residue B is done at 80 DEG C
It is dry to obtain metatitanic acid, metatitanic acid is calcined into 1h at 1000 DEG C and obtains titanium dioxide (rutile-type, content 99.8%).
Embodiment 4
A. by waste and old metatitanic acid pole piece, calcining 1h removes binder and conductive agent in pole piece in air at 400 DEG C,
Then lithium titanate and aluminium foil are removed, obtains waste and old lithium titanate, then by waste and old lithium titanate mechanical activation 1h (ratios of grinding media to material 40:1, turn
400 revs/min of speed), obtain the amorphous lithium titanate of powdery；
B. it leaches：By lithium titanate:Deionized water quality is than 1:3 deionized water is added into amorphous lithium titanate, and stirring is equal
It is even, by peroxide root:The molar ratio 3 of Ti:1 is added the potassium peroxide that mass concentration is 15%, and ammonium hydroxide is then added while stirring, adjusts
The pH value of section system then continues leaching 0.5h to 10 or so at 20 DEG C, and filtering obtains lithium titanate leachate；
C. lithium carbonate is prepared：It is added into leachate and contains potassium carbonate, carbonate:Li molar ratios are 1:2~1.15:2, reaction
Stop stirring after 0.5h, be aged 6h, filter to obtain filter residue A and titaniferous filtrate, filter residue A is washed with deionized 3 times, it is dry after
1h is calcined at 450 DEG C obtains lithium carbonate (content 99.2%)；
D. titanium dioxide is prepared：Gained titaniferous filtrate in step c is heated to boiling, keeps boiling 0.5h that titanium is made to hydrolyze,
Filter residue B is filtered to obtain, filter residue B is washed 1 time with 1% dust technology, then is washed with deionized 1 time, by filter residue B at 150 DEG C
Dry metatitanic acid, calcines 6h at 700 DEG C by metatitanic acid and obtains titanium dioxide (Detitanium-ore-type, content 99.7%).
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be subject to claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change
Protection scope of the present invention is also should be regarded as into retouching.
Claims (7)
1. a kind of recoverying and utilizing method of waste and old lithium titanate, which is characterized in that
A, waste and old lithium titanate is provided, and the waste and old lithium titanate is subjected to amorphous processing, obtains amorphous waste and old lithium titanate；
B, the amorphous waste and old lithium titanate mixed with water, peroxide, alkali compounds, adjust acid-base value to alkalinity, leaching
Go out, lithium titanate leachate is obtained by filtration；When peroxide is added, according to the molar ratio 1 of titanium elements in lithium titanate and peroxide root:
(2~5) peroxide is added；
C, by the lithium titanate leachate and precipitant mix, the first filter residue and titaniferous filtrate, the filter are obtained after ageing, filtering
Slag is to be precipitated containing lithium；The precipitating reagent is that sodium carbonate, potassium carbonate, ammonium carbonate, one or more of carbon dioxide can be with
Li reactions generate the compound of precipitation；
D, the titaniferous filtrate is heated to boiling and keeps fluidized state until completely, the second filter is obtained by filtration in solid precipitation
Second filter residue is obtained metatitanic acid by slag after pickling, washing, drying successively；
E, metatitanic acid at 500~1000 DEG C is calcined into 1~6h and obtains titanium dioxide.
2. recoverying and utilizing method according to claim 1, which is characterized in that described to provide waste and old lithium titanate and be specially：It will
Waste and old metatitanic acid pole piece calcining removes no-bonder and conductive agent, and waste and old lithium titanate is removed from the pole piece.
3. recoverying and utilizing method according to claim 2, which is characterized in that described calcine waste and old metatitanic acid pole piece removes
Binder and conductive agent are specially：
By waste and old metatitanic acid pole piece, 0.5~2h of calcining removes binder and conduction in pole piece in air at 300~500 DEG C
Agent.
4. recoverying and utilizing method according to claim 1, which is characterized in that it is described it is amorphous processing be specially：In ball material
Than (5~40): 1,150~400 revs/min of rotating speed, by 1~5h of the waste and old lithium titanate ball milling.
5. recoverying and utilizing method according to claim 1, which is characterized in that step b is specially：
B1, by the amorphous lithium titanate and water by weight being 1: (1~5) mixes and according to titanium elements in lithium titanate and mistake
The molar ratio 1 of oxygen root: peroxide is added in (2~5)；
B2, with alkali compounds by the pH value of the obtained systems of b1 to 8~12, then at 20~70 DEG C leach 10min~2h,
Filtering, obtains lithium titanate leachate.
6. recoverying and utilizing method according to claim 1, which is characterized in that the additive amount of the precipitating reagent is by carbonate
: the molar ratio of Li is (1~1.3): 2.
7. recoverying and utilizing method according to claim 1, which is characterized in that the pickling is specially by second filter residue
It is washed with the dust technology of 0.5wt%~2wt% or dilute hydrochloric acid.
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| CN109546252A (en) * | 2017-09-22 | 2019-03-29 | 银隆新能源股份有限公司 | The recycling method of valuable metal in the cathode pole piece of waste and old lithium titanate battery |
| CN108134150A (en) * | 2017-12-20 | 2018-06-08 | 山东高佳新能源有限公司 | The method of valuable element in hydro-thermal synthetical recovery waste lithium iron phosphate positive electrode |
| CN110735038B (en) * | 2018-07-21 | 2021-04-13 | 浙江遨优动力系统有限公司 | Method for recycling electrode metal material from waste lithium titanate battery |
| CN109037722A (en) * | 2018-08-17 | 2018-12-18 | 湖南金凯循环科技有限公司 | A method of recycling lithium in waste and old lithium titanate series lithium ion battery negative electrode tab |
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| CN101967010A (en) * | 2010-11-04 | 2011-02-09 | 中南大学 | Method for preparing nano-TiO2 serving as cathode material of lithium ion battery |
| CN102390863A (en) * | 2011-08-15 | 2012-03-28 | 佛山市邦普循环科技有限公司 | Method for regenerating lithium titanate serving as anode material of waste lithium ion battery |
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| CN103346365A (en) * | 2013-07-22 | 2013-10-09 | 田东 | Method for recycling negative material from waste lithium ion battery |
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| CN101967010A (en) * | 2010-11-04 | 2011-02-09 | 中南大学 | Method for preparing nano-TiO2 serving as cathode material of lithium ion battery |
| CN102390863A (en) * | 2011-08-15 | 2012-03-28 | 佛山市邦普循环科技有限公司 | Method for regenerating lithium titanate serving as anode material of waste lithium ion battery |
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