CN108285980A - The method of metal in inorganic Ore Leaching-bioleaching collaboration recycling lithium ion battery - Google Patents
The method of metal in inorganic Ore Leaching-bioleaching collaboration recycling lithium ion battery Download PDFInfo
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- CN108285980A CN108285980A CN201810234039.8A CN201810234039A CN108285980A CN 108285980 A CN108285980 A CN 108285980A CN 201810234039 A CN201810234039 A CN 201810234039A CN 108285980 A CN108285980 A CN 108285980A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/18—Extraction of metal compounds from ores or concentrates by wet processes with the aid of microorganisms or enzymes, e.g. bacteria or algae
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to old and useless battery metal recovery processing technology field, a kind of method that metal in lithium ion battery is recycled in inorganic Ore Leaching bioleaching collaboration includes the domestication of (1) Thiobacillus ferrooxidans；(2) battery is disassembled；(3) Ore Leaching：Inorganic acid is put into mixed electrode material powder, obtains the solution containing heavy metal and electrode powder, reaction system final pH is 1.8 2.5；(4) bioleaching：Add culture solution into above-mentioned solution, and the Thiobacillus ferrooxidans tamed is added, detach mixing liquid precipitate after reaction, isolated mixed liquor is centrifuged, and the liquid containing heavy metal centrifuged carries out heavy metal recovery.Inorganic Ore Leaching is combined by this technique with bioleaching, and sour dosage is few, and metal leaching rate is high, has played the mild advantage of bioleaching reaction condition, environmental protection, safety.
Description
Technical field
The invention belongs to old and useless battery metal recovery processing technology fields, and in particular to a kind of inorganic Ore Leaching-biology leaching
The method of metal in filter collaboration recycling lithium ion battery.
Background technology
Lithium ion battery applications are more and more extensive with the development of science and technology, and the electronic products such as mobile phone, computer use at present
Lithium ion battery is as energy storage unit, but being continuously increased for lithium ion battery learies causes serious dirt to environment
Dye.
Waste and old lithium ion battery is important non-ferrous metal secondary resource, distinguishes containing cobalt, lithium, nickel in waste lithium ion
For 5-15%, 2-7%, 0.5-2%, the also metallic elements such as Cu, Al, Fe.Especially China's cobalt resource extremely lacks, and lithium from
The mass fraction of cobalt can reach l5% in sub- battery, and cobalt content is 850 times or so of association cobalt ore content, have very high return
Receive value.
Along with the commercially use of lithium ion battery, the research recycled to it has been begun to both at home and abroad.Recycling profit
Original power is valuable metal therein, the especially non-ferrous metals such as cobalt cupro-nickel.In making profits again for waste and old lithium ion battery
It is most with hydrometallurgical technology application in technology, wherein the first step recycled is extract technology.Inorganic Ore Leaching is generally used, but
Not only inorganic acid dosage is big, and it is poor to be also easy to produce acid mist, environmental condition, and environmental protection is not up to standard, it is necessary to which acid mist collecting processing increases fortune
Row cost, moreover, after Ore Leaching, still some metal can not leach.
Invention content
Invention broadly provides the sides of metal in a kind of inorganic Ore Leaching-bioleaching collaboration recycling lithium ion battery
Method, the technique that inorganic Ore Leaching is combined with bioleaching improve metal compared to the dosage that conventional method can reduce acid
Leaching rate.Its technical solution is as follows：
A kind of method that metal in lithium ion battery is recycled in inorganic Ore Leaching-bioleaching collaboration, includes the following steps：
(1) domestication of Thiobacillus ferrooxidans：First by Thiobacillus ferrooxidans activation process, then containing mixed electrode material
It is tamed repeatedly in the culture solution at feed powder end, obtains the strong Thiobacillus ferrooxidans of tolerance；
(2) battery is disassembled：Waste and old lithium ion battery is disassembled into removal shell, electric discharge and is crushed, positive and negative anodes mixing electricity is obtained
Pole material powder；
(3) Ore Leaching：Mixed electrode material powder is put into the first reaction tank, inorganic acid is put into the first reaction tank
It is mixed with electrode material powder, hybrid reaction 2-5h, obtains the solution containing heavy metal and electrode powder that pH is 1.8-2.5,
The solution is put into the second reaction tank；
(4) bioleaching：Into the second reaction tank plus culture solution carries out pulp, and the ferrous oxide sulphur bar tamed is added
Bacterium is stirred to react 4-10 days, and mixed liquor is carried out precipitation separation, and isolated electrode powder slag carries out harmless treatment, point
It is centrifuged from obtained mixed liquor, the thalline centrifuged, which is returned in Thiobacillus ferrooxidans culture tank, to be continued to cultivate, centrifugation
The obtained liquid containing heavy metal carries out heavy metal recovery.
Preferably, the acclimation method of Thiobacillus ferrooxidans is in step (1), will contain ferrous oxide sulphur bar after activation
Bacterium bacterium solution adds in culture solution, adjusts initial pH to 1.8-3, and mixed electrode material powder, which is added, makes its a concentration of 0.8-1.2g/
L, shaking table culture, periodic measurement culture solution pH terminate to cultivate when culture solution pH maintains 1.8-3.5, and above-mentioned is a cycle, under
One cycle repeats aforesaid operations, and each cycle ensures to draw in the bacterium solution to new culture solution in upper Cyclic culture liquid
The relatively upper cycle of the addition of mixed electrode material increases 5-15%, until mixed electrode material powder concentration increases to 1.5-
Cycle terminates when 2.0g/L, and domestication is completed.
Preferably, culture solution described in step (1) is 9K fluid nutrient mediums, the addition containing ferrous oxide influenza bacterium bacterium solution
Amount accounts for the 1/4-1/6 of nutrient solution volume.
Preferably, acid described in step (3) is inorganic acid, and the inorganic acid is sulfuric acid and hydrogen peroxide according to 1:0.5-1's
Mass ratio configures, and the sulfuric acid concentration is 0.75mol/L.
Preferably, the solid-liquid mass volume ratio of electrode material powder and inorganic acid dosage is (1 in step (3):10-15)
g/L。
Preferably, culture solution described in step (4) is 9K fluid nutrient mediums.
Using the above scheme, the present invention has the following advantages：
The present invention obtains one plant of Thiobacillus ferrooxidans through long-term separation, screening, domestication
(Thiobacillusferrooxidans, T.f), the bacterial strain have the characteristics that adaptable, tolerance various heavy, especially
The heavy metals such as copper, nickel, zinc, the cobalt of enduring high-concentration.(referred to as using this plant of Thiobacillus ferrooxidans：CHFe) to inorganic Ore Leaching
Used Li ion cell material powder afterwards carries out biology leaching drip and leaches, is useless to obtain the high leaching rate of the metals such as cobalt, copper, nickel
The subsequent metal recovery of lithium ion battery provides preparation.
Inorganic Ore Leaching is combined by this technique with bioleaching, it is possible to reduce sour dosage improves environmental condition, improves
The leaching rate of metal, while having played the mild advantage of bioleaching reaction condition, whole process less acid-consuming, environmental protection, safety.
Specific implementation mode
Experimental method in following embodiment is conventional method unless otherwise required, involved experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
Embodiment 1
1. the domestication of Thiobacillus ferrooxidans
First three times by the activation of CHFe bacterium, then domestication 6 months is carried out.Steps are as follows for domestication：The CHFe bacterium solutions of activation are taken
In the conical flask of 20ml to 105ml 9K culture solutions, initial pH to 1.8-3 (best is 2) is adjusted, 0.1-0.15g is added (most
Good is 0.125g) mixed electrode material powder, be uniformly mixed be placed on shaking table, 30 DEG C, 120rmin-1Lower mixing training
It supports 14 days, a pH value was surveyed every 24 hours, until pH is maintained within the scope of 1.8-3.5 and no longer risen.Repeat above-mentioned steps,
But the dosage of mixed electrode material increases by 10% in each repetitive process, continues domestication culture, points to mixed electrode material
Powder concn increases to 1.5-2.0g/L, after the last one is recycled to the 14th day, mixed electrode of the CHFe bacterium to 1.5-2.0g/L
PH maintains 2-3 ranges in material mixed liquor, stops domestication.
Through detaching, screen for a long time, tame, obtain one plant of Thiobacillus ferrooxidans (Thiobacillusferrooxidans,
T.f), which has the characteristics that adaptable, tolerance various heavy, the especially copper of enduring high-concentration, nickel, zinc, cobalt etc.
Heavy metal.(referred to as using this plant of Thiobacillus ferrooxidans：CHFe) to the used Li ion cell material powder after inorganic Ore Leaching,
It carries out biology leaching drip to leach, is the subsequent metal recovery of used Li ion cell to obtain the high leaching rate of the metals such as cobalt, copper, nickel
It provides and prepares.
2. battery dismantling, decladding, crushing
Waste and old lithium ion battery is disassembled into decapsidate, electric discharge, crushing, respectively obtains the powder of anode and cathode mixed materials.
3. inorganic Ore Leaching
The powder of mixed electrode material is put into the first reaction tank, by H2SO4(concentration 0.75mol/L) and H2O2According to
1:0.5-1 mass ratios configure, by 1:10-15 (g/L) (optimal proportion 1:13) solid-liquid mass volume ratio ratio is added to
In one reaction tank, mixed with mixed electrode powder.Hybrid reaction 3 hours, it is 2.0 containing heavy metal and electrode powder to obtain pH
The solution is put into the second reaction tank by solution.
4. bioleaching
Into the second reaction tank plus culture solution carries out pulp, while the cultured ferrous oxide sulphur bar in culture tank is added
Bacterium is (referred to as：CHFe), 30 DEG C of controlling reaction temperature open stirring, after reacting 4-10 days, stop stirring, and it is heavy that mixed liquor is entered
The precipitation separation of shallow lake pond, electrode powder slag enter harmlessness disposing, and mixed liquor enters the thalline that centrifuge obtains and flows back into oxygen
Change and continue to cultivate in ferrous Thiobacillus culture tank, in the technique of subsequent recovery containing heavy metal solution centrifuged.
Embodiment 2
Battery is disassembled：Used Li ion cell is disassembled into decapsidate, electric discharge, crushing, obtains positive and negative anodes mixed electrode material
Powder 1.5kg.
Ore Leaching：The positive and negative anodes mixed electrode material powder 1.5kg put into the first reaction tank, by 1：13 solid-liquids
H is added in mass volume ratio2SO4(concentration 0.75mol/L)-H2O2(1：1)19.5m3, reaction mixing 3 hours, it is 2 to contain to obtain pH
Solution is put into the second reaction tank by the solution for having heavy metal and electrode powder.
Bioleaching：1m is added in the second reaction tank3The CHFe bacterium solutions tamed through 1 acclimation method of embodiment and 9K
Culture solution (1:5.5), 30 DEG C of controlling reaction temperature open stirring, after reacting 7 days, stop stirring, mixing liquid is precipitated
Separation, isolated electrode powder slag carry out harmless treatment, and isolated liquid is centrifuged, and centrifugation is contained
Heavy metal liquid, the thalline centrifuged, which is back in Thiobacillus ferrooxidans culture tank, to be continued to cultivate.It will obtain containing a huge sum of money
Belong to liquid to recycle by follow-up conventional recycling processes, obtain cobalt in inorganic acid-bioleaching technique, nickel, copper the rate of recovery divide
It Wei 94.3%, 94.0% and 96.8%.
Comparative example 1
Bioleaching step in embodiment 2 is omitted, and improves the concentration of sulfuric acid in Ore Leaching step to 5mol/L, by 1：
H is added in 13 solid-liquid mass volume ratios2SO4(concentration 5mol/L)-H2O2(1：1)19.5m3, other steps are the same as embodiment 2, directly general
The liquid phase that Ore Leaching obtains using recovery process recycle, obtain the cobalt in inorganic acid extract technology, nickel, copper the rate of recovery be respectively
91.7%, 93.6%, 96.4%.
Compared to Ore Leaching-bioleaching technique, individual acidleach is although simple for process, but to obtain higher satisfaction
The metal recovery rate of industrial requirements, it is necessary to the concentration and dosage of acid are improved, and the acid of high concentration can etching apparatus, generation acid
Mist causes environmental condition poor, and acid mist absorption treating device can also increase cost.
Comparative example 2
Ore Leaching step in embodiment 2 is omitted, directly the powder of mixed electrode material is added in the second reaction tank, and
The reaction time is improved to 14 days, other steps are with embodiment 2, the recovered work of liquid containing heavy metal that directly obtains bioleaching
Skill recycle, obtain the cobalt in bioleaching technique, nickel, copper the rate of recovery be respectively 64.3%, 6.3%, 54.5%.
Bioleaching technique, which leaches the heavy metal in used Li ion cell, has acid consumption few, at low cost, easy to operate
Advantage, but relative to Ore Leaching-bioleaching technique, the individual bioleaching technological reaction duration is longer, and return
Yield is very low.
Comparative example 3
By in embodiment 2 Ore Leaching and bioleaching step exchange, i.e., first carry out bioleaching step carry out acidleach again
Go out step, it is specific as follows：
Battery is disassembled：Used Li ion cell is disassembled into decapsidate, electric discharge, crushing, obtains positive and negative anodes mixed electrode material
Powder 1.5kg.
Bioleaching：The anode and cathode mixed materials powder 1.5kg that battery is disassembled is added in the first reaction tank, and adds
Enter 1m3The CHFe bacterium solutions tamed through 1 acclimation method of embodiment and 9K culture solutions (1:5.5), 30 DEG C of controlling reaction temperature, are opened
Stirring is opened, after reacting 7 days, stops stirring, mixed liquor is subjected to precipitation separation, isolated electrode powder slag enters Ore Leaching
Step, isolated mixed liquor is centrifuged, then mixed liquor is centrifuged, and obtains liquid containing heavy metal and thalline, thalline
It returns in Thiobacillus ferrooxidans culture tank and continues to cultivate, liquid containing heavy metal retains spare.
Ore Leaching：Mixed electrode material of the input by bioleaching processing in the second reaction tank, by 1：13 solid-liquid matter
It measures volume ratio and H is added2SO4(concentration 0.75mol/L)-H2O2(1：1)19.5m3, reaction mixing 3 hours, then solid is separated out, and
Retain liquid phase.The liquid containing heavy metal handled through bioleaching is mixed with the liquid phase obtained through Ore Leaching.By follow-up
Conventional recycling processes recycle, obtain the cobalt in inorganic acid-bioleaching technique, nickel, copper the rate of recovery be respectively 78.9%,
30.2%, 73.5%.
Technique before bioleaching to be placed on to Ore Leaching as known from the above is relatively low for the rate of recovery of metal.And by acidleach
Good reaction environment can be provided for bioleaching technique before going out to be placed on bioleaching, be conducive to Thiobacillus ferrooxidans life
The long and leaching to metal, will be higher by much the rate of recovery of metal.
It will be apparent to those skilled in the art that technical solution that can be as described above and design, make various other
Corresponding change and deformation, and all these changes and deformation should all belong to the protection domain of the claims in the present invention
Within.
Claims (6)
1. the method for metal in a kind of inorganic Ore Leaching-bioleaching collaboration recycling lithium ion battery, it is characterised in that：Including with
Lower step：
(1) domestication of Thiobacillus ferrooxidans：First by Thiobacillus ferrooxidans activation process, then containing mixed electrode material powder
It is tamed repeatedly in the culture solution at end, obtains the strong Thiobacillus ferrooxidans of tolerance；
(2) battery is disassembled：Waste and old lithium ion battery is disassembled into removal shell, electric discharge and is crushed, positive and negative anodes mixed electrode material is obtained
Feed powder end；
(3) Ore Leaching：Mixed electrode material powder is put into the first reaction tank, inorganic acid and electricity are put into the first reaction tank
Pole material powder mixing, hybrid reaction 2-5h obtain the solution containing heavy metal and electrode powder that pH is 1.8-2.5, will be molten
Liquid is put into the second reaction tank；
(4) bioleaching：Into the second reaction tank plus culture solution carries out pulp, and the Thiobacillus ferrooxidans tamed is added,
It is stirred to react 4-10 days, mixed liquor is subjected to precipitation separation, isolated electrode powder slag carries out harmless treatment, detaches
To mixed liquor centrifuged, the thalline centrifuged, which is returned in Thiobacillus ferrooxidans culture tank, to be continued to cultivate, and centrifugation obtains
Liquid containing heavy metal carry out heavy metal recovery.
2. the method for metal in inorganic Ore Leaching according to claim 1-bioleaching collaboration recycling lithium ion battery,
It is characterized in that：The acclimation method of Thiobacillus ferrooxidans is in step (1), will contain Thiobacillus ferrooxidans bacterium solution after activation
It adds in culture solution, adjusts initial pH to 1.8-3, mixed electrode material powder, which is added, makes its a concentration of 0.8-1.2g/L, shaking table
Culture, periodic measurement culture solution pH terminate to cultivate when culture solution pH maintains 1.8-3.5, and above-mentioned is a cycle, subsequent cycle
To draw in the bacterium solution to new culture solution in upper Cyclic culture liquid, aforesaid operations are repeated, and each cycle ensures mixing electricity
The relatively upper cycle of the addition of pole material increases 5-15%, when mixed electrode material powder concentration increases to 1.5-2.0g/L
Cycle terminates, and domestication is completed.
3. the method for metal in inorganic Ore Leaching according to claim 2-bioleaching collaboration recycling lithium ion battery,
It is characterized in that：Culture solution described in step (1) is 9K fluid nutrient mediums, and the addition containing ferrous oxide influenza bacterium bacterium solution accounts for training
The 1/4-1/6 of nutrient solution volume.
4. the method for metal in inorganic Ore Leaching according to claim 1-bioleaching collaboration recycling lithium ion battery,
It is characterized in that：Acid described in step (3) is inorganic acid, and the inorganic acid is sulfuric acid and hydrogen peroxide according to 1:The mass ratio of 0.5-1
Example configures, and the sulfuric acid concentration is 0.75mol/L.
5. the method for metal in inorganic Ore Leaching according to claim 1-bioleaching collaboration recycling lithium ion battery,
It is characterized in that：The solid-liquid mass volume ratio of electrode material powder and inorganic acid dosage is (1 in step (3):10-15)g/L.
6. the method for metal in inorganic Ore Leaching according to claim 1-bioleaching collaboration recycling lithium ion battery,
It is characterized in that：Culture solution described in step (4) is 9K fluid nutrient mediums.
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| CN114959304A (en) * | 2022-03-25 | 2022-08-30 | 上海第二工业大学 | Method for selectively leaching and recycling lithium in black powder of waste lithium iron phosphate power battery by using acidithiobacillus ferrooxidans |
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