CN103035977B - A kind of method of separation and recovery lithium from waste and old lithium ion battery - Google Patents
A kind of method of separation and recovery lithium from waste and old lithium ion battery Download PDFInfo
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- CN103035977B CN103035977B CN201310001972.8A CN201310001972A CN103035977B CN 103035977 B CN103035977 B CN 103035977B CN 201310001972 A CN201310001972 A CN 201310001972A CN 103035977 B CN103035977 B CN 103035977B
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- resin
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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 invention discloses a kind of method of separation and recovery lithium from waste and old lithium ion battery, split after waste and old lithium ion battery is discharged, remove battery case; Battery is pulverized; Battery inorganic acid after pulverizing and oxidant are leached, filters, obtain filtrate; The pH value of filtrate is transferred to and is more than or equal to 8, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion; With the lithium ion in resin adsorption Ethylene recov; Desorption is carried out to resin, obtains the lithium salts of separation and recovery.Recovery method of the present invention is simple, efficient, purity is high, and does not pollute.
Description
[technical field]
The present invention relates to the method for Footwall drift from old and useless battery, in waste and old lithium ion battery, particularly reclaim the method for lithium ion.
[background technology]
Lithium ion battery is the good chargeable chemical cell of a kind of combination property, there is the advantages such as operating voltage is high, specific energy is high, have extended cycle life, self discharge is little, be widely used in the fields such as mobile communication, Notebook Battery, portable dam, electric automobile.The positive electrode that lithium rechargeable battery in the market uses mainly cobalt acid lithium, LiMn2O4, LiFePO 4 and other contain the binary/ternary material of lithium, the lithium metal resource of these positive electrodes all containing preciousness.The positive electrode consumption used due to lithium ion battery is very large, consumption for non-renewable metals resources is very large, therefore while lithium ion battery use amount grows with each passing day, reclaim in waste and old lithium ion battery and be worth high, that content is larger metal, to realizing energy-saving and emission-reduction, sustainable development, tool is of great significance.
Although the commercial technologies of lithium rechargeable battery is increasingly mature in decades, but the research and development of corresponding spent lithium-ion secondary batteries recovery technology then seems more delayed, the lithium ion product recoveries particularly obtained after a chemical treatment being complexity is lower, purity is not high yet, and be mostly in the laboratory research stage, technology conveniently need optimize and perfect.
[summary of the invention]
For solving the problems of the technologies described above, the invention discloses that a kind of technique is simple, organic efficiency is high, the recovery method of purity is high from waste and old lithium ion battery lithium.
A method for separation and recovery lithium from waste and old lithium ion battery, is characterized in that comprising the steps:
(1) disassemble after waste and old lithium ion battery being discharged, get battery plus plate current-collecting body;
(2) carry out alkali leaching to battery plus plate current-collecting body, the aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder to the press filtration of alkali leaching solution;
(3) positive pole powder sulfuric acid and hydrogen peroxide are leached, adjusted to ph is 2-3, filters, obtains filtrate;
(4) by the Fe in filtrate
2+be oxidized to Fe
3+, then add calcium carbonate or solution ph is adjusted to 3.5-6.0 by magnesium oxide, iron is precipitated, after filtration, the pH value of filtrate is transferred to and is more than or equal to 8, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion;
(5) lithium ion in spent ion exchange resin absorption Ethylene recov;
(6) sour backwash, makes lithium ion be separated with resin, obtains lithium-containing solution;
(7) in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
PH value in described step (4) is 8-9.
In described step (5), resin is strong-acid ion exchange resin or chelating resin.
Described strong-acid ion exchange resin is polystyrene sulfonic acid type ion exchange resin, and described chelating resin is imido oxalic acid type chelate resin.
Described step carries out preliminary treatment to resin in (5), and described preliminary treatment comprises the steps:
(I) soaks resin with acid, then separating acid and resin;
(II) then soaks resin with alkali, then is separated alkali and resin.
Described step (I) is soak resin with the HCl solution of l-1.5mol/l, soak after 10-30 hour, separating acid and resin, remaining acid is washed away again with deionized water, described step (II) is soak resin with the Na0H solution of l-1.5mol/l, soak after 10-30 hour, be separated alkali and resin, then wash away remaining acid with deionized water.
In described step (5), described Ethylene recov pH value is transferred to 4-7, then adsorbs with resin.
The sour back-washing method of described step (6) is utilized by the resin being adsorbed with lithium ion the hydrochloric acid of 0.5-1.5mol/l or sulfuric acid to carry out backwash.
Beneficial effect of the present invention is: (1) the present invention utilizes ion exchange resin method to carry out adsorbing separation recovery to the lithium ion in waste and old lithium ion battery, and recovery method is simple, efficient, purity is high, and does not pollute; (2) after desorption, resin can also reuse, and cost is low, is applicable to industrialization promotion and uses.
[accompanying drawing explanation]
Fig. 1 is present invention process flow chart.
[embodiment]
Process chart of the present invention as shown in Figure 1, comprises the steps: that (1) disassembles after being discharged by waste and old lithium ion battery, gets battery plus plate current-collecting body; (2) carry out alkali leaching to battery plus plate current-collecting body, the aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder to the press filtration of alkali leaching solution; (3) positive pole powder sulfuric acid and hydrogen peroxide are leached, adjusted to ph is 2-3, filters, obtains filtrate; (4) by the Fe in filtrate
2+be oxidized to Fe
3+, then add calcium carbonate or solution ph is adjusted to 3.5-6.0 by magnesium oxide, iron is precipitated, after filtration, the pH value of filtrate is transferred to and is more than or equal to 8, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion; (5) lithium ion in spent ion exchange resin absorption Ethylene recov; (6) sour backwash, makes lithium ion be separated with resin, obtains lithium-containing solution; (7) in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
Describe the present invention below in conjunction with the drawings and specific embodiments.
Embodiment 1:
Disassemble after waste and old lithium ion battery is discharged, get battery plus plate current-collecting body, excessive NaOH is added to battery plus plate current-collecting body and carries out alkali leaching, aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder, positive pole powder sulfuric acid and hydrogen peroxide are leached the press filtration of alkali leaching solution, adjusted to ph is 2-3, filter, obtain filtrate, by Fe in filtrate
2+by oxidizing be Fe
3+, then add calcium carbonate solution ph is adjusted to 3.5-6.0, iron is precipitated, after filtration, the pH value of filtrate is transferred to 8, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion; Ethylene recov containing lithium ion being adjusted to PH is 4, highly acid spent ion exchange resin G-26 adsorbs the lithium ion in Ethylene recov, the hydrochloric acid of 1mol/l is utilized to carry out sour backwash, lithium ion is separated with resin, obtain lithium-containing solution, in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
Embodiment 2:
Disassemble after waste and old lithium ion battery is discharged, get battery plus plate current-collecting body, excessive potassium hydroxide is added to battery plus plate current-collecting body and carries out alkali leaching, aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder, positive pole powder sulfuric acid and hydrogen peroxide are leached the press filtration of alkali leaching solution, adjusted to ph is 2-3, filter, obtain filtrate, by Fe in filtrate
2+by oxidizing be Fe
3+, then add calcium carbonate or solution ph is adjusted to 5.0 by magnesium oxide, iron is precipitated, after filtration, the pH value of filtrate is transferred to 9, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion; Ethylene recov containing lithium ion being adjusted to PH is 6, the lithium ion in Ethylene recov is adsorbed with strong-acid ion exchange resin AMb.35, the hydrochloric acid of 0.5mol/l is utilized to carry out sour backwash, lithium ion is separated with resin, obtain lithium-containing solution, in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
Embodiment 3:
Disassemble after waste and old lithium ion battery is discharged, get battery plus plate current-collecting body, excessive potassium hydroxide is added to battery plus plate current-collecting body and carries out alkali leaching, aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder, positive pole powder sulfuric acid and hydrogen peroxide are leached the press filtration of alkali leaching solution, adjusted to ph is 2-3, filter, obtain filtrate, by Fe in filtrate
2+by oxidizing be Fe
3+, then add calcium carbonate or solution ph is adjusted to 3.5-6.0 by magnesium oxide, iron is precipitated, after filtration, the pH value of filtrate is transferred to and is more than or equal to 8, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion; Ethylene recov containing lithium ion being adjusted to PH is 5.5, spent ion exchange resin Amb.IRC748 adsorbs the lithium ion in Ethylene recov, the hydrochloric acid of 1mol/l is utilized to carry out sour backwash, lithium ion is separated with resin, obtain lithium-containing solution, in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
Embodiment 4:
Disassemble after waste and old lithium ion battery is discharged, get battery plus plate current-collecting body, excessive potassium hydroxide is added to battery plus plate current-collecting body and carries out alkali leaching, aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder, positive pole powder sulfuric acid and hydrogen peroxide are leached the press filtration of alkali leaching solution, adjusted to ph is 2.5, filter, obtain filtrate, by Fe in filtrate
2+by oxidizing be Fe
3+, then add calcium carbonate or solution ph is adjusted to 6.0 by magnesium oxide, iron is precipitated, after filtration, the pH value of filtrate is transferred to 8.5, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion; Ethylene recov containing lithium ion being adjusted to PH is 5, lithium ion in spent ion exchange resin D751 resin adsorption Ethylene recov, the sulfuric acid of 1mol/l is utilized to carry out sour backwash, lithium ion is separated with resin, obtain lithium-containing solution, in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
Resin in above-described embodiment is handled as follows before adsorbing: soak resin with the HCl solution of l-1.5mol/l, soak after 10-30 hour, separating acid and resin, then wash away remaining acid with deionized water; Soak resin with the Na0H solution of l-1.5mol/l again, soak after 10-30 hour, be separated alkali and resin, then wash away remaining acid with deionized water.Above-mentioned steps can also be utilized respectively to process to the resin after desorption, the resin after process can be reused.
The present invention utilizes ion exchange resin method to carry out adsorbing separation recovery to the lithium ion in waste and old lithium ion battery, and recovery method is simple, efficient, purity is high, and does not pollute; Resin after desorption can also reuse, and cost is low, is applicable to industrialization promotion and uses.
In sum; although the present invention by embodiment to invention has been detailed description; but persons skilled in the art should be understood that; above-described embodiment is only the description to the preferred embodiments of the present invention; but not limiting the scope of the invention; persons skilled in the art are in the technical scope disclosed by the present invention, and the change that can expect easily, all within protection scope of the present invention.
Claims (8)
1. the method for separation and recovery lithium from waste and old lithium ion battery, is characterized in that comprising the steps:
(1) disassemble after waste and old lithium ion battery being discharged, get battery plus plate current-collecting body;
(2) carry out alkali leaching to after battery plus plate current-collecting body fragmentation, the aluminum metal in plus plate current-collecting body is dissolved, and obtains positive pole powder to the press filtration of alkali leaching solution;
(3) positive pole powder sulfuric acid and hydrogen peroxide are leached, adjusted to ph is 2-3, filters, obtains filtrate;
(4) by the Fe in filtrate
2+be oxidized to Fe
3+, then add calcium carbonate or solution ph is adjusted to 3.5-6.0 by magnesium oxide, iron is precipitated, after filtration, the pH value of filtrate is transferred to and is more than or equal to 8, cross and filter impurity and precipitation, obtain the Ethylene recov containing lithium ion;
(5) lithium ion in spent ion exchange resin absorption Ethylene recov, carry out preliminary treatment to resin, described preliminary treatment comprises the steps:
(I) soaks resin with acid, then separating acid and resin;
(II) then soaks resin with alkali, then is separated alkali and resin;
(6) sour backwash, makes lithium ion be separated with resin, obtains lithium-containing solution;
(7) in lithium-containing solution, add carbonate, heating be concentrated, isolated by filtration, drying, obtain lithium carbonate product.
2. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 1, is characterized in that: the dissolved aluminum salt in described step (2) can be used as battery binding agent.
3. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 1, is characterized in that: in described step (4), the pH value of filtrate is 8-9.
4. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 1, is characterized in that: in described step (5), resin is strong-acid ion exchange resin or chelating resin.
5. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 4, it is characterized in that: described strong-acid ion exchange resin is polystyrene sulfonic acid type ion exchange resin, described chelating resin is imido oxalic acid type chelate resin.
6. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 1, it is characterized in that: described step (I) is soak resin with the HCl solution of l-1.5mol/L, soak after 10-30 hour, separating acid and resin, wash away remaining acid with deionized water again, described step (II) is soak resin by the NaOH solution of l-1.5mol/L, soaks after 10-30 hour, be separated alkali and resin, then wash away remaining alkali with deionized water.
7. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 1, is characterized in that: in described step (5), described Ethylene recov pH value is transferred to 4-7, then adsorbs with resin.
8. the method for separation and recovery lithium from waste and old lithium ion battery as claimed in claim 1, is characterized in that: the sour back-washing method of described step (6) is utilized by the resin being adsorbed with lithium ion the hydrochloric acid of 0.5-1.5mol/L or sulfuric acid to carry out backwash.
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| CN201310001972.8A CN103035977B (en) | 2013-01-05 | 2013-01-05 | A kind of method of separation and recovery lithium from waste and old lithium ion battery |
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| CN201310001972.8A CN103035977B (en) | 2013-01-05 | 2013-01-05 | A kind of method of separation and recovery lithium from waste and old lithium ion battery |
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| CN103035977B true CN103035977B (en) | 2015-09-09 |
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| CN111977704A (en) * | 2020-07-27 | 2020-11-24 | 昆明理工大学 | Rapid regeneration method of waste ternary lithium ion battery anode material |
| CN112886085B (en) * | 2021-03-09 | 2022-03-04 | 昆明理工大学 | Method for regenerating ternary lithium ion battery anode material by ion exchange method |
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| CN115747521A (en) * | 2022-12-29 | 2023-03-07 | 江苏电科环保有限公司 | Method for recovering and preparing lithium carbonate from waste lithium ion battery positive electrode material |
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