CN107359381B - A kind of method of accurate efficient process automobile lithium battery lithium iron phosphate positive material - Google Patents
A kind of method of accurate efficient process automobile lithium battery lithium iron phosphate positive material Download PDFInfo
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- CN107359381B CN107359381B CN201710462246.4A CN201710462246A CN107359381B CN 107359381 B CN107359381 B CN 107359381B CN 201710462246 A CN201710462246 A CN 201710462246A CN 107359381 B CN107359381 B CN 107359381B
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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
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Abstract
The present invention is suitable for anode material of lithium battery process field, provides a kind of method of accurate efficient process automobile lithium battery lithium iron phosphate positive material.Several data points are arranged in acidleach pH value, alkali leaching pH value, the experience value range of readjustment pH value in the present invention, then it is directed to the lithium iron phosphate positive material of different vendor, excessively taken turns acidleach pH value when a rate of recovery highest is found in test, alkali leaching pH value, readjustment pH value and soluble lithium salt standard solution dosage D, and these parameters are uploaded to database together with manufacturer's classification number and are shared, the processing plant of different location can share these data；When processing, the trade name and weight of input processing material directly in system terminal, download corresponding most suitably used parameter, it can also be converted to obtain the actual capacity of soluble lithium salt standard solution according to weight, lithium iron phosphate positive material recovery processing is carried out according to these data, specific aim is higher, and the processing parameter of the lithium iron phosphate positive material of different vendor is different, can reach the maximum lithium rate of recovery.
Description
Technical field
The invention belongs to anode material of lithium battery processing technology field more particularly to a kind of accurate efficient process automobile lithium electricity
The method of pond lithium iron phosphate positive material.
Background technique
New-energy automobile comes into high-speed development period at present, and the core of new-energy automobile is lithium battery.In view of lithium electricity
The restricted lifetime in pond, these new-energy automobile lithium batteries will progress into the superseded date of retirement after the several years, contain in positive electrode
There is lithium, if the great wasting of resources will be caused by random discarding.
Main force of the ferric phosphate lithium cell because becoming dynamic lithium battery with good thermal stability and cycle performance.Phosphoric acid
Iron lithium anode material complicated composition contain the impurity such as a large amount of copper and aluminium simple substance and a small amount of iron simple substance.Current processing method
Process is as follows: first roasting the positive electrode of recycling, then passes through step of acid dipping and adjust pH value, go after being separated by filtration
Acidleach filter residue, then alkali soaks step and adjusts pH value, and alkali lixivium is taken after being separated by filtration, finally adjusts back pH in alkali lixivium
Value, and soluble lithium salt solution is added and is stirred to react, it is finally separated by solid-liquid separation, the filter residue being collected into is lithium phosphate product.
There are several parameter values more crucial in this technique, directly influences the rate of recovery of final LiFePO4, specifically have
Acidleach pH value, alkali leaching pH value, the dosage for adjusting back pH value and last soluble lithium salt solution.At present in technique, these parameters
Empirical value is generally taken, for example the range of acidleach pH value is 0.5-2.0, the range that alkali soaks pH value is 12-14, adjusts back the range of pH value
It is 6-8, and the soluble lithium salt solution being added is according to different selections, the not determining value of dosage.And for the lithium of different company electricity
Pond product, there may be differences for the component and amount containing lithium of positive electrode, if do not distinguished, the positive electrode of recycling into
It goes after being uniformly processed, the LiFePO4 rate of recovery will necessarily be made different, more or less occur recycling incomplete or acid-base solution
Or soluble lithium salt solution usage it is excessive the problems such as.
Summary of the invention
In view of the above problems, the purpose of the present invention is to provide a kind of accurate efficient process automobile lithium battery LiFePO4s just
The method of pole material, it is intended to solve existing lithium iron phosphate positive material handle it is insufficient, none unified parameter and standard
Technical problem.
The present invention adopts the following technical scheme:
Lithium iron phosphate positive material processing database is established, includes manufacturer's classification number and corresponding place in the database
Manage parameter detail；
For each lithium battery manufacturer, the lithium iron phosphate positive material for taking the manufacturer to produce, then by LiFePO4
Positive electrode is developed into powder；
A wheel test is carried out, prepares acid solution of the pH value equal to A and pH value is equal to the lye of B, select the phosphorus of certain mass
Sour iron lithium anode material, which is placed in crucible, to be roasted, and then product of roasting is placed in progress acidleach processing in the acid solution of preparation, then
Separation of solid and liquid takes filter residue, then will collect obtained filter residue and be added to progress alkali leaching processing in the lye of preparation, after leaching point
The pH value of alkali lixivium is pulled back to C by the alkali lixivium from after, and the alkali lixivium etc. after readjustment is distributed into multiple test tubes,
The dosage of soluble lithium salt standard solution in each test tube is stepped up, and then stirring is until reaction completely, finally calibration is each
Lithium concentration in a test tube selects lithium ion content close to 0 and the least test tube of standard solution dosage, and is filtered point
From filter residue containing lithium is collected, the dry filter residue containing lithium is simultaneously weighed, and soluble lithium salt standard solution dosage is finally converted into unit
The soluble lithium salt standard solution dosage D of quality lithium iron phosphate positive material records this wheel test lithium iron phosphate positive material
Manufacturer's classification number and the pH value A of acid solution, the pH value B of lye, readjustment pH value C, soluble lithium salt standard solution dosage D, contain lithium
Filter residue dry weight E；
Next round test is carried out, one in tri- parameters of A, B, C is altered in steps in each round test, and records this wheel examination
Five parameter A to E under testing, A, B, C parameter traversals finish after excessively being taken turns test, and it is dry that filter residue containing lithium is found from all tests
The weight maximum record of E, and corresponding parameter A to D and manufacturer's classification number are uploaded to database, wherein at parameter A-D composition
Manage parameter detail；
When being recycled to a collection of lithium battery LiFePO 4 anode material, this batch is inputted in controlling terminal system
Then the trade name and weight of lithium iron phosphate positive material are downloaded corresponding processing parameter detail A-D and are shown from database
Show, wherein soluble lithium salt standard solution dosage D needs are further converted into actual amount according to weight；
Then according to the soluble lithium salt standard solution actual amount after the parameter A-C of downloading display and conversion, to this
Criticize lithium battery LiFePO 4 anode material recovery processing.
Further, in test, the data point of the pH value of acid solution has 0.8,1.1,1.4,1.7,2.0, and the pH value of lye takes
Value point has 12,12.5,13,13.5, and the data point for adjusting back pH value has 6.5,7,7.5,8.
Further, the method also includes following step:
When database receives data more new command, more new data and more new database are received.
The beneficial effects of the present invention are: in existing lithium iron phosphate positive material treatment process, generally by empirical value
The dosage of acidleach pH value, alkali leaching pH value, readjustment pH value and last soluble lithium salt solution is set, this necessarily makes ferric phosphate
The lithium rate of recovery is different；Several values are arranged in acidleach pH value, alkali leaching pH value, the experience value range of readjustment pH value in the present invention
Then point is directed to the lithium iron phosphate positive material of different vendor, is excessively taken turns acidleach pH when a rate of recovery highest is found in test
Value, alkali leaching pH value, readjustment pH value and soluble lithium salt standard solution dosage D, and by these parameters together on manufacturer's classification number
It reaches database to be shared, the processing plant of different location can share these data；When progress lithium iron phosphate positive material
When processing, the trade name and weight of input processing material directly in system terminal can be downloaded corresponding from database
Most suitably used parameter, including acidleach pH value, alkali leaching pH value, readjustment pH value, and can also be converted to obtain according to weight can
The actual capacity of dissolubility lithium salts standard solution carries out lithium iron phosphate positive material recovery processing according to these data, and specific aim is more
The processing parameter of height, the lithium iron phosphate positive material of different vendor is different, can reach the maximum lithium rate of recovery.
Detailed description of the invention
Fig. 1 is the method for accurate efficient process automobile lithium battery lithium iron phosphate positive material provided in an embodiment of the present invention
Flow chart.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The method of accurate efficient process automobile lithium battery lithium iron phosphate positive material provided in this embodiment is specific as follows:
Step S1, establish lithium iron phosphate positive material processing database, include in the database manufacturer's classification number and
Corresponding processing parameter detail.
Idea of the invention is that by establishing a shared data bank, the ferric phosphate of different vendor's production is preserved in the inside
The different disposal parameter detail of lithium anode material, without being handled by empirical value, and the company of different location can be total to
This database is enjoyed, can accomplish that data timely update and share, so that the lithium iron phosphate positive material for different vendor has
It is targetedly handled, processing difference is embodied, to guarantee the rate of recovery of lithium iron phosphate positive material.Therefore this step is first
Establish database.
Step S2, it is directed to each lithium battery manufacturer, the lithium iron phosphate positive material for taking the manufacturer to produce, then by ferric phosphate
Lithium anode material is developed into powder.
The present invention needs to establish the lithium iron phosphate positive material processing parameter of different vendor, therefore firstly the need of to different factories
The lithium iron phosphate positive material of quotient is tested.Lithium iron phosphate positive material is taken, powder is then developed into.Establishing database number
According to when, need to choose the lithium iron phosphate positive material of each manufacturer, then sampling carries out more wheel tests.The present invention is by LiFePO4
Positive electrode is developed into powder, convenient for chemical treatment reaction, shortens test period, saves time cost.
Step S3, a wheel test is carried out, prepares acid solution of the pH value equal to A and pH value is equal to the lye of B, select certain matter
The lithium iron phosphate positive material of amount, which is placed in crucible, to be roasted, and is then placed in product of roasting in the acid solution of preparation and is carried out at acidleach
Then reason is separated by solid-liquid separation and takes filter residue, then will collect obtained filter residue and be added to progress alkali leaching processing in the lye of preparation, after
Alkali lixivium after leaching separation, pulls back to C for the pH value of alkali lixivium, the alkali lixivium etc. after readjustment is distributed into multiple examinations
The dosage of Guan Zhong, the soluble lithium salt standard solution in each test tube are stepped up, and then stirring is until reaction completely, is finally marked
Lithium concentration in fixed each test tube selects lithium ion content close to 0 and the least test tube of standard solution dosage, and carried out
Filter separates and collects filter residue containing lithium, and the dry filter residue containing lithium simultaneously weighs, is finally converted into soluble lithium salt standard solution dosage
The soluble lithium salt standard solution dosage D of unit mass lithium iron phosphate positive material records this wheel test iron phosphate lithium positive pole material
Manufacturer's classification number of material and the pH value A of acid solution, the pH value B of lye, readjustment pH value C, soluble lithium salt standard solution dosage D,
The dry weight of filter residue containing lithium E.
For the lithium iron phosphate positive material of current selection manufacturer, idea of the invention is that: for pH value A, the alkali of acid solution
The pH value B of liquid, readjustment these three parameters of pH value C, first keep two of them parameter constant, then another parameter is in empirical value range
It inside takes a little, carries out test of many times, then proceed to change parameter.For example first keeping A, B value is starting point, and is remained unchanged, so
The data point for gradually changing C in experience range afterwards is excessively taken turns test.Hereafter A continues constant, and B takes next data point, so
The data point for gradually changing C in experience range afterwards is excessively taken turns test.And so on, it can traverse parameter ABC's in this way
All data points.For example, the data point of the pH value of acid solution has 0.8,1.1,1.4,1.7,2.0, the pH value data point of lye has 12,
12.5,13,13.5, the data point for adjusting back pH value has 6.5,7,7.5,8.Such a manufacturer's lithium iron phosphate positive material need through
80 wheel tests are crossed, but in practice, test can be taken turns more while being carried out, for example directly can directly take five groups of difference pH value first
Acid solution, then tested, only need 16 tests in this way, therefore entire test is time-consuming controllable.Even can more people it is same
Shi Jinhang test, can be further reduced test period.As long as after obtained optimized parameter, subsequent each branch company all may be used
To share this data, the economic benefit of institute's band is lost considerably beyond test period.
In this step, after pH value pulls back to C, the alkali lixivium etc. after readjustment is distributed into multiple test tubes, for example is filled
Enter in 5 test tubes, the dosage of the soluble lithium salt standard solution in each test tube is stepped up in experience range, soluble lithium
The content of the effective component of salt standard solution is fixed, therefore the dosage (volume) of standard solution directly determines alkali lixivium
The number of middle lithium content.After soluble lithium salt standard solution is added, stirring is finally demarcated in each test tube until reaction completely
Lithium concentration selects lithium ion content close to 0 and the least test tube of standard solution dosage, and be separated by filtration collection containing lithium
Filter residue, the dry filter residue containing lithium are simultaneously weighed, and soluble lithium salt standard solution dosage is finally converted into unit mass ferric phosphate
The soluble lithium salt standard solution dosage D of lithium anode material.Specifically, assuming the lithium iron phosphate positive material quality of crucible roasting
For x, the soluble lithium salt standard solution dosage of the smallest test tube of lithium concentration is d, then D=5d/x.It is different by experiment
The dosage of soluble lithium salt standard solution is gradually incremented by test tube, select lithium ion content close to 0 and standard solution dosage it is minimum
Test tube, the dosage of soluble lithium salt standard solution is most suitable at this time, neither too much nor too little.Record this wheel test parameter A, B,
The soluble lithium salt standard solution dosage D of C and unit mass lithium iron phosphate positive material.
Step S4, next round test is carried out, one in tri- parameters of A, B, C is altered in steps in each round test, and remember
Five parameter A to E under this wheel test are recorded, A, B, C parameter traversals finish after excessively being taken turns test, find and contain from all tests
The maximum record of lithium filter residue dry weight E, and corresponding parameter A to D and manufacturer's classification number are uploaded to database, wherein parameter A-
D forms processing parameter detail.
Test is excessively taken turns, the maximum record of the dry weight E of filter residue containing lithium is found from all tests, it is corresponding to illustrate that this is recorded
Lithium rate of recovery highest under the conditions of parameter A, B, C, therefore it is current manufacturer's iron phosphate lithium positive pole material that this, which records corresponding parameter A-D,
Expect most adaptable recovery processing parameter.
Step S5, when being recycled to a collection of lithium battery LiFePO 4 anode material, in controlling terminal system
Then the trade name and weight for inputting this batch of lithium iron phosphate positive material download corresponding processing parameter detail from database
A-D simultaneously shows that wherein soluble lithium salt standard solution dosage D needs are further converted into actual amount according to weight.
When various regions branch company carries out lithium battery LiFePO 4 anode material processing, battery is divided by company, manufacturer first
Then class inputs and inputs trade name and weight on system terminal, automatic download process parameter detail A-D, while according to weight
Amount and unit mass soluble lithium salt standard solution dosage D directly convert and obtain actual amount.
Step S6, it is then used according to the soluble lithium salt standard solution after the parameter A-C of downloading display and conversion is practical
Amount is recycled this batch of lithium battery LiFePO 4 anode material.
Finally according to the parameter A-C of display and soluble lithium salt standard solution actual amount, staff is according to this
Parameter carries out follow-up process processing, can significantly improve the lithium rate of recovery of lithium battery LiFePO 4 anode material.
In embodiments of the present invention, in addition, if discovery parameter error is larger in actual production, practical lithium recycling is influenced
Rate, company can also be according to actual modification parameters, and then to when database sending and receiving go out data more new command, database is received more
New data simultaneously updates.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (2)
1. a kind of method of accurate efficient process automobile lithium battery lithium iron phosphate positive material, which is characterized in that the method packet
Include following step:
Lithium iron phosphate positive material processing database is established, includes that manufacturer's classification number and corresponding processing are joined in the database
Number detail；
For each lithium battery manufacturer, the lithium iron phosphate positive material for taking the manufacturer to produce, then by lithium iron phosphate positive material
It is developed into powder；
A wheel test is carried out, prepares acid solution of the pH value equal to A and pH value is equal to the lye of B, select the ferric phosphate of certain mass
Lithium anode material is placed in crucible and roasts, and then product of roasting is placed in progress acidleach processing in the acid solution of preparation, then solid-liquid
Separation takes filter residue, then will collect obtained filter residue and be added to progress alkali leaching processing in the lye of preparation, after leaching separation
Alkali lixivium, the pH value of alkali lixivium is pulled back into C, the alkali lixivium etc. after readjustment is distributed into multiple test tubes, each
The dosage of soluble lithium salt standard solution in test tube is stepped up, and then stirring is until reaction completely, finally demarcates each examination
Lithium concentration in pipe selects lithium ion content close to 0 and the least test tube of standard solution dosage, and carries out being separated by filtration receipts
Collect filter residue containing lithium, the dry filter residue containing lithium is simultaneously weighed, and soluble lithium salt standard solution dosage is finally converted into unit mass
The soluble lithium salt standard solution dosage D of lithium iron phosphate positive material records the manufacturer of this wheel test lithium iron phosphate positive material
Classification number and the pH value A of acid solution, the pH value B of lye, readjustment pH value C, soluble lithium salt standard solution dosage D, filter residue containing lithium
Dry weight E；
Next round test is carried out, one in tri- parameters of A, B, C is altered in steps in each round test, and is recorded under this wheel test
Five parameter A to E, excessively taken turns test after A, B, C parameter traversals finish, the dry weight of filter residue containing lithium E is found from all tests
Maximum record, and corresponding parameter A to D and manufacturer's classification number are uploaded to database, wherein the processing of parameter A-D composition is joined
Number detail；
When being recycled to a collection of lithium battery LiFePO 4 anode material, this batch of phosphoric acid is inputted in controlling terminal system
Then the trade name and weight of iron lithium anode material are downloaded corresponding processing parameter detail A-D and are shown from database,
Middle soluble lithium salt standard solution dosage D needs are further converted into actual amount according to weight；
Then according to the soluble lithium salt standard solution actual amount after the parameter A-C of downloading display and conversion, to this batch of lithium
The recovery processing of battery lithium iron phosphate positive material；
In test, the data point of the pH value of acid solution has 0.8,1.1,1.4,1.7,2.0, the pH value data point of lye has 12,12.5,
13,13.5, the data point for adjusting back pH value has 6.5,7,7.5,8.
2. the method for accurate efficient process automobile lithium battery lithium iron phosphate positive material as described in claim 1, which is characterized in that
The method also includes following step:
When database receives data more new command, more new data and more new database are received.
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| TWI231063B (en) * | 2003-11-14 | 2005-04-11 | Ind Tech Res Inst | Process of recovering valuable metals from waste secondary batteries |
| CN101599563B (en) * | 2009-07-08 | 2011-03-23 | 中南大学 | Method for efficiently recovering active materials of positive poles in waste lithium batteries |
| CN102956936B (en) * | 2011-08-25 | 2015-04-15 | 深圳市格林美高新技术股份有限公司 | Method for treating lithium iron phosphate cathode material of waste and old power lithium battery of automobile |
| JP5898021B2 (en) * | 2012-09-11 | 2016-04-06 | 株式会社日立製作所 | Method and apparatus for recycling lithium ion battery |
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