CN109921126B - Method for recovering active material from waste cobalt-containing lithium ion battery positive electrode material - Google Patents
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Abstract
The invention discloses a method for recovering active materials from waste cobalt-containing lithium ion battery anode materials, which comprises the following steps: (1) weighing peroxydisulfate and oxalate, dissolving in water, and preparing into lotion; (2) immersing the waste cobalt-containing lithium battery positive electrode material into a de-washing agent, carrying out ultrasonic heating treatment, and taking out an aluminum current collector to obtain a de-washing liquid; (3) carrying out solid-liquid separation treatment on the eluent to obtain solid-state slurry, and then carrying out water washing and separation treatment to obtain water-washed solid-state slurry; (4) and carrying out thermal decomposition treatment on the water-washed solid slurry to obtain the active material. The recovery efficiency of the active material is high, the recovery period is short, and the recovery rates of lithium and cobalt are respectively as high as 98.05 percent and 99.24 percent; the method has the advantages of simple operation process and strong feasibility, the recovery process does not involve the use of any acid-alkali liquor, the dissolution loss of the aluminum current collector can be effectively reduced, the environment can not be polluted, and the method is harmless to operators.
Description
Technical Field
The invention relates to a method for recycling waste lithium ion batteries, in particular to a method for recycling active materials from a waste cobalt-containing lithium ion battery cathode material.
Background
The cobalt-containing lithium ion battery has complex composition, relatively late resource recovery and relatively low industrialization level, and the treatment aiming at the lithium battery at present mainly focuses on recovering precious metal elements in a positive electrode active material and an electrolyte of the battery. The core technology for recovering the anode material of the waste cobalt-containing lithium ion battery is mainly divided into a wet method and a fire method. The recovery process comprises several links such as pretreatment, separation, pre-recovery, impurity removal and recycling.
According to the different principle of valuable metal resource, the recovery technology of the waste cobalt-containing lithium ion battery anode material can be divided into extraction method, chemical precipitation method, electrodeposition method, acid leaching salting-out method, pyrogenic method, biological leaching method and the like. The extraction method adopts an organic solvent and valuable metals to form a specific coordination compound, and then utilizes an extracting agent to extract metal ions to synthesize a new compound, but has the problems of low recovery rate of cobalt and lithium elements, high toxicity of the extracting agent, easy generation of secondary pollution in the recovery link and the like. The chemical precipitation method is characterized in that the waste cobalt-containing lithium ion battery is subjected to simple mechanical separation, the positive electrode material is dissolved by acid and alkali to be completely dissolved to form an ionic solution, and cobalt and lithium ions are recovered and reused in a precipitation form through a chemical reaction. The electrodeposition method mainly realizes the recovery of specific elements in the waste cobalt-containing lithium ion battery through the processes of acid leaching, electromigration, electro-enrichment, cathode precipitation and the like, can obtain cobalt with higher purity and has less pollution to the surrounding ecological environment, but has the problems of coprecipitation and low lithium recovery efficiency. The acid leaching salting-out method can use two acids of inorganic acid and organic acid, an aluminum current collector is easy to dissolve in the using process, the later cobalt and lithium recovery efficiency is low, and acid liquor and alkali liquor are easy to cause potential harm to the health of operators and the surrounding environment. The pyrogenic process can be divided into direct roasting, sulfating roasting and chloridizing roasting according to different treatments of the lithium ion battery, the process is relatively simple, the treated battery has various types and is easy for large-scale production, but the combustion of other combustible components in electrolyte solution and electrodes easily causes air pollution. The bioleaching method is a method for converting valuable metals in waste cobalt-containing lithium ion batteries into metal ion solutions by using microorganisms to recover the valuable metals, but the bioleaching method has the problems of long recovery period, low recovery efficiency, high purification difficulty of cobalt and lithium and the like.
In conclusion, although there are many methods for rapidly activating the anode material of the waste cobalt-containing lithium ion battery at present, the methods have the problems of complex operation process, large consumption of acid and alkali liquor, low cobalt-lithium recovery efficiency, long recovery period, environmental pollution and the like to different degrees.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems, the invention provides a method for recovering an active material from a waste cobalt-containing lithium ion battery positive electrode material, which has the advantages of simple operation process, no use of acid and alkali liquor, high cobalt-lithium recovery efficiency, short recovery period and low loss rate of an aluminum current collector.
The technical scheme is as follows: the method for recovering the active material from the anode material of the waste cobalt-containing lithium ion battery comprises the following steps:
(1) weighing peroxydisulfate and oxalate, dissolving in water, and preparing into lotion;
(2) immersing the waste cobalt-containing lithium battery positive electrode material into a detergent, carrying out ultrasonic heating treatment, dissolving and desorbing the positive electrode material from an aluminum current collector, and taking out the aluminum current collector to obtain a detergent;
(3) carrying out solid-liquid separation treatment on the eluent to obtain solid slurry, and then carrying out water washing and separation treatment to obtain water-washed solid slurry;
(4) and carrying out thermal decomposition treatment on the water-washed solid slurry to obtain the active material.
And (3) washing the taken aluminum current collector with water, recovering the washing liquid, mixing the washing liquid with a desolventizing liquid, and performing subsequent steps (3) and (4) on the mixed liquid, wherein the recovery rate of cobalt and lithium can be improved by recovering the washing liquid.
And (4) primarily evaporating the solid slurry washed in the step (4) to obtain a cobalt-lithium recovered raw material, and then carrying out thermal decomposition treatment. The initial evaporation of the solid slurry after water washing can improve the thermal decomposition efficiency of the cobalt-lithium recovery raw material.
The molar ratio of the peroxydisulfate to the oxalate in the step (1) is 1: 1.2-2.8, and preferably 1: 1.5-2.5.
The concentration of the peroxydisulfate in the detergent in the step (1) is 0.02-0.20 mol/L, preferably 0.05-0.15 mol/L.
The solid-liquid ratio of the waste cobalt-containing lithium battery anode material to the detergent in the step (2) is 1: 25-70, and preferably 1: 30-60.
The ultrasonic treatment time in the step (2) is 4-6 hours, and the heating temperature is 50-70 ℃.
The thermal decomposition temperature in the step (4) is 750-950 ℃, and the thermal decomposition time is 1-3 h.
The working principle is as follows: in the process that the waste cobalt-containing lithium ion battery anode material is immersed in the eluent to be eluted, the potassium persulfate is decomposed by heating to generate sulfate radicals, and meanwhile, the cavity effect and the foaming implosion effect generated by ultrasonic waves can strengthen the thermal decomposition process of the potassium persulfate, so that the generation rate of the sulfate radicals is improved, and the sulfate radicals can oxidize organic glue between the active material and the aluminum current collector to promote the active material to fall off from the aluminum current collector. Simultaneously sulfate radical reacts with sodium oxalate to generate carbon dioxide radical
Carbon dioxide free radical reacts with trivalent cobalt in the anode material of the waste cobalt-containing lithium ion battery to generate carbonate and divalent cobalt
Thereby promoting the release of cobalt ions and lithium ions and the dissolution and desorption of the anode material on the aluminum current collector. The water ripple generated by the ultrasonic wave can improve the mass transfer process of the carbon dioxide free radical, press the contact distance between the carbon dioxide free radical and the anode material of the waste cobalt-containing lithium ion battery, and strengthen the reduction effect of the carbon dioxide free radical on the trivalent cobalt. Divalent cobalt ions released by the reduction reaction react with redundant oxalate radicals to generate flocculent cobalt oxalate precipitates
Released lithium ion and carbonAcid radical reaction to generate lithium carbonate precipitate
Under the background of continuous action of carbon dioxide free radicals, the precipitation of cobalt and lithium ions accelerates the dissolution and desorption of the anode material on the aluminum current collector. And (3) washing and separating the solid slurry to quickly remove sodium sulfate and sodium oxalate attached to the solid slurry. The solid slurry is subjected to primary evaporation to dryness, so that the thermal decomposition efficiency of the cobalt-lithium recovery raw material can be improved. At high temperature, the cobalt-lithium recovery raw material is thermally decomposed, and the cobalt oxalate and the lithium carbonate are decomposed and fused to generate lithium cobaltate, cobaltous oxide and carbon dioxide (CoC)2O4+Li2C2O4→LiCoO2+Co2O3+CO2) And the recovery of active materials in the anode materials of the waste cobalt-containing lithium ion batteries is realized.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: (1) the recovery efficiency of the active material is high, the recovery period is short, and the recovery rates of lithium and cobalt are respectively as high as 98.05 percent and 99.24 percent; (2) the method has the advantages of simple operation process and strong feasibility, the recovery process does not involve the use of any acid-alkali liquor, the dissolution loss of the aluminum current collector can be effectively reduced, the environment can not be polluted, and the method is harmless to operators.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
Example 1
Influence of molar ratio of potassium peroxodisulfate to sodium oxalate on recovery efficiency of cobalt and lithium and loss rate of aluminum current collector
The method comprises the steps of respectively weighing potassium peroxodisulfate and sodium oxalate according to a molar ratio of 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:2, 1:2.5, 1:2.6, 1:2.7 and 1:2.8 at room temperature, dissolving the potassium peroxodisulfate and the sodium oxalate in water to prepare a eluent, immersing the positive electrode material of the waste cobalt-containing lithium ion battery in the eluent with the concentration of 0.05 mol/L, taking out the positive electrode sheet, drying, cutting the positive electrode sheet into pieces appropriately to facilitate later recovery of an aluminum current collector, immersing the positive electrode material of the waste cobalt-containing lithium ion battery in the eluent according to a solid-liquid ratio of 1:30(g: m L), carrying out ultrasonic treatment at 50 ℃ for 6 hours, dissolving the positive electrode material from the aluminum, desorbing, taking out aluminum out the aluminum current collector out the ultrasonic treatment, obtaining a slurry, separating the solid-state lithium current collector by water, carrying out the separation of the solid-liquid slurry, carrying out the slurry separation on the solid-liquid slurry obtained by the dissolution and the slurry obtained by the slurry separation of the slurry, the slurry obtained by the slurry, and the slurry obtained by the slurry recovery of the slurry, the slurry obtained by the slurry, and the slurry obtained by the slurry separation, and the slurry obtained.
It should be noted that the present invention is not limited to the peroxodisulfate and formate, and may be other salts such as sodium peroxodisulfate, potassium oxalate, etc. besides the potassium peroxodisulfate and sodium oxalate mentioned in the examples of the present invention, as long as the purpose of the present invention is not limited.
In order to determine the recovery rates of cobalt and lithium and the loss rate of the aluminum current collector, the inventors performed the following experiments:
and (3) analyzing the recovery efficiency of cobalt and lithium: dissolving the anode material of the waste cobalt-containing lithium ion battery by using strong acid, fixing the volume by using the strong acid, and determining the concentration of cobalt and lithium in a strong acid solution by using an inductively coupled plasma spectral generator; and (3) dissolving the recovered active material by using strong acid, titrating to the volume which is the same as that of the strong acid solution of the anode material of the waste cobalt-containing lithium ion battery by using the strong acid, and determining the concentration of cobalt and lithium in the strong acid solution by using an inductively coupled plasma spectral generator. Wherein, the recovery rate of cobalt is equal to the percentage of the concentration of cobalt in the strong acid solution of the recovered active material and the concentration of cobalt in the strong acid solution of the anode material of the waste cobalt-containing lithium ion battery; the recovery rate of lithium is equal to the percentage of the concentration of lithium in the strong acid solution of the recovered active material and the concentration of lithium in the strong acid solution of the anode material of the waste cobalt-containing lithium ion battery.
Analysis of loss rate of aluminum current collector: dissolving the anode material of the waste cobalt-containing lithium ion battery by using strong acid, fixing the volume by using the strong acid, and determining the aluminum concentration in a strong acid solution by using an inductively coupled plasma spectrum generator; and (3) dissolving the recovered active material by using strong acid, titrating to the volume which is the same as that of the strong acid solution of the anode material of the waste cobalt-containing lithium ion battery by using the strong acid, and determining the aluminum concentration in the strong acid solution by using an inductively coupled plasma spectrum generator. The loss rate of the aluminum current collector is equal to the percentage of the concentration of aluminum in the recovered strong acid solution of the active material and the concentration of aluminum in the strong acid solution of the anode material of the waste cobalt-containing lithium ion battery.
The anode material of the waste cobalt-containing lithium ion battery dissolved by strong acid and the anode material treated by the method are both taken from the anode plate in the same waste cobalt-containing lithium ion battery, and the using amount of the anode material is the same.
The results of the tests on the cobalt and lithium recovery efficiency and the loss rate of the aluminum current collector with respect to the change in the molar ratio of potassium peroxodisulfate to sodium oxalate are shown in Table 1.
TABLE 1 influence of molar ratio of potassium peroxodisulfate and sodium oxalate on cobalt, lithium recovery efficiency and aluminum current collector loss
As can be seen from table 1, when the molar ratio of potassium peroxodisulfate to sodium oxalate is higher than 1:1.5 (as shown in table 1, the molar ratio of potassium peroxodisulfate to sodium oxalate is 1:1.4, 1:1.3, 1:1.2, and higher ratios not shown in table 1), the recovery efficiency of cobalt and lithium is less than 85% because the content of sodium oxalate is relatively small and the amount of cobalt oxalate and lithium carbonate generated after the reaction of sulfate radicals with sodium oxalate is reduced. Meanwhile, due to the lack of the neutralization effect of excessive sodium oxalate, the content of sulfuric acid in the desorption solution is high, the dissolution amount of the aluminum current collector is increased, and the loss rate of the aluminum current collector is more than 5%; when the molar ratio of potassium peroxodisulfate to sodium oxalate is equal to 1: 1.5-2.5, continuously generating cobalt oxalate and lithium carbonate, and simultaneously enabling the pH of a desorption solution to be alkaline, wherein the recovery efficiency of cobalt and lithium is more than 90%, and the loss rate of an aluminum current collector is lower than 3%; when the molar ratio of potassium peroxodisulfate to sodium oxalate is less than 1:2.5 (as in table 1, the molar ratio of potassium peroxodisulfate to sodium oxalate is 1:2.6, 1:2.7, 1:2.8, and lower ratios not listed in table 1), the amount of sulfate radicals generated decreases due to the decrease in the potassium peroxodisulfate content, so that the amount of active material released from the aluminum current collector decreases, and the trivalent cobalt reduction efficiency becomes slow, resulting in a decrease in the cobalt and lithium recovery efficiency. Therefore, in summary, the recycling of active materials in the anode materials of the waste cobalt-containing lithium ion batteries is most facilitated when the molar ratio of potassium peroxodisulfate to sodium oxalate is 1: 1.5-2.5 in combination with the benefit and cost.
Example 2
Effect of the concentration of Potassium persulfate in the Desubstituent on the cobalt and lithium recovery efficiency and the aluminum Current collector loss Rate
The method comprises the steps of weighing potassium peroxodisulfate and sodium oxalate according to a molar ratio of 1:2 of potassium peroxodisulfate to sodium oxalate at room temperature, dissolving the potassium peroxodisulfate and the sodium oxalate in water to prepare a eluent, wherein the concentrations of the potassium peroxodisulfate in the eluent are respectively 0.02 mol/L, 0.03 mol/L, 0.04 mol/L, 0.05 mol/L, 0.10 mol/L, 0.15 mol/L, 0.16 mol/L, 0.18 mol/L and 0.20 mol/L, immersing the cobalt-containing lithium ion battery anode material into the eluent according to a solid-liquid ratio of 1:45(g: m L), carrying out ultrasonic treatment at 60 ℃ for 5 hours to obtain the eluent, taking out the aluminum current collector, washing the aluminum current collector with water, recovering the eluent, mixing the washing liquid and the eluent, separating solid from the eluent to obtain solid slurry, carrying out water washing and solid-liquid separation, carrying out water separation again, carrying out primary water separation, carrying out primary water recovery on the waste cobalt-lithium-containing lithium ion slurry to obtain a raw material, and carrying out water recovery.
The cobalt and lithium recovery efficiency analysis and the aluminum current collector loss rate analysis were the same as in example 1, and the test results are shown in table 2.
TABLE 2 Effect of potassium peroxodisulfate concentration in the desludging agent on cobalt and lithium recovery efficiency and aluminum current collector loss
As can be seen from table 2, when the concentration of potassium peroxodisulfate in the eluent is less than 0.05 mol/L (as in table 2, the concentration of potassium peroxodisulfate in the eluent is 0.02 mol/L, 0.03 mol/L, 0.04 mol/L and lower ratios not listed in table 2), the reduction of the elution amount of active material and the yield of carbon dioxide directly results in a decrease of trivalent cobalt ion reduction and lithium ion precipitation rate, resulting in cobalt and lithium recovery efficiency of less than 80%, due to a decrease of sulfate radical yield, cobalt oxalate and lithium carbonate continue to be generated when the concentration of potassium peroxodisulfate in the eluent is 0.05 to 0.15 mol/L, the eluent is alkaline, cobalt and lithium recovery efficiency is greater than 93%, the aluminum current collector loss rate is less than 3%, when the concentration of potassium peroxodisulfate in the eluent is greater than 0.15 mol/L (as in table 2, the concentration of potassium peroxodisulfate in the eluent is 0.16/L, the concentration of potassium peroxodisulfate in the eluent is 0.19 mol/732, the lithium ion recovery efficiency is slightly greater than 20%, and the lithium ion recovery efficiency is equal to 20.15 mol/462, and the lithium ion recovery efficiency is higher than 20%, when the total potassium peroxodisulfate recovery efficiency of cobalt and the lithium ion recovery efficiency is 0.05 to 0.15 mol/35% in the lithium ion recovery efficiency is equal to 0.15 mol/L, respectively listed in the lithium ion recovery efficiency of the anode.
Example 3
Influence of the ratio of the positive electrode material to the solid-liquid ratio of the eluent on the recovery efficiency of cobalt and lithium and the loss rate of the aluminum current collector
The method comprises the steps of weighing potassium peroxodisulfate and sodium oxalate according to a molar ratio of 1:2 of potassium peroxodisulfate to sodium oxalate at room temperature, dissolving the potassium peroxodisulfate and the sodium oxalate in water to prepare a detergent, wherein the concentration of potassium peroxodisulfate in the detergent is 0.10 mol/L, immersing the waste cobalt-containing lithium ion battery positive electrode material into the detergent according to a solid-liquid ratio of 1:25, 1:27, 1:29, 1:30, 1:40, 1:50, 1:60, 1:65 and 1:70(g: m L), carrying out ultrasonic treatment at 70 ℃ for 4 hours to obtain a detergent, taking out an aluminum current collector, washing the aluminum current collector with water and recovering the washing liquid, mixing the washing liquid and the detergent, carrying out solid-liquid separation on the mixed liquid to obtain solid slurry, carrying out water washing on the separated solid slurry, carrying out re-separation again, carrying out water washing-separation for three times to obtain water-washed solid slurry, evaporating the water-washed solid lithium-solid slurry to obtain a primary raw material, carrying out thermal decomposition at 950 ℃ to obtain a raw material, and recovering the active material.
The cobalt and lithium recovery efficiency analysis and the aluminum current collector loss rate analysis were the same as in example 1, and the test results are shown in table 3.
Table 3 influence of the positive electrode material and the solid-liquid ratio of the eluent on the recovery efficiency of cobalt and lithium and the loss rate of the aluminum current collector
As can be seen from table 3, when the solid-to-liquid ratio of the positive electrode material to the eluent is higher than 1:30 (as in table 3, the solid-to-liquid ratio of the positive electrode material to the eluent is 1:29, 1:27, 1:25(g: m L), and higher ratios not listed in table 3), the eluent is relatively small, the supply of potassium peroxodisulfate and sodium oxalate is insufficient, so that the elution amount of the active material and the yield of carbon dioxide are reduced, resulting in cobalt and lithium recovery efficiencies of less than 85%, when the solid-to-liquid ratio of the positive electrode material to the eluent is equal to 1:30 to 60(g: m 2), cobalt oxalate and lithium carbonate are continuously generated, the eluent is alkaline, the cobalt and lithium recovery efficiencies are both greater than 94%, and the aluminum current collector loss rate is less than 2%, when the solid-to-liquid ratio of the positive electrode material to the eluent is lower than 1:60(g: m L) (as in table 3, the solid-to-liquid ratio of the positive electrode material to the eluent is 1:65, 1:70(g: m L), and when the solid-to-liquid ratio of the positive electrode material to the lithium ion recovery efficiency is slightly higher than 1:60 (as in table 3), and when the cobalt recovery efficiency of the cobalt-to lithium ion recovery efficiency is equal to the lithium ion recovery efficiency is equal to 1.82), respectively, and the highest efficiency is equal to the lithium recovery efficiency is equal to the highest as in table 3, and the recovery efficiency is equal to the overall efficiency is equal to the lithium.
Claims (6)
1. A method for recovering active materials from waste cobalt-containing lithium ion battery positive electrode materials is characterized by comprising the following steps:
(1) weighing peroxydisulfate and oxalate, dissolving in water, and preparing into lotion;
(2) immersing the waste cobalt-containing lithium battery positive electrode material into a de-washing agent, carrying out ultrasonic heating treatment, and taking out an aluminum current collector to obtain a de-washing liquid;
(3) carrying out solid-liquid separation treatment on the eluent to obtain solid slurry, and then carrying out water washing and separation treatment to obtain water-washed solid slurry;
(4) carrying out thermal decomposition treatment on the water-washed solid slurry to obtain an active material;
the molar ratio of the peroxydisulfate to the oxalate in the step (1) is 1: 1.2-2.8, and the concentration of the peroxydisulfate in the eluent is 0.02-0.20 mol/L;
the solid-liquid ratio of the waste cobalt-containing lithium battery anode material to the detergent in the step (2) is 1: 25-70, the ultrasonic treatment time is 4-6 hours, and the heating temperature is 50-70 ℃;
the thermal decomposition temperature in the step (4) is 750-950 ℃, and the thermal decomposition time is 1-3 h.
2. The method for recovering the active material from the cathode material of the waste cobalt-containing lithium ion battery as claimed in claim 1, wherein the step (2) further comprises washing the taken out aluminum current collector with water, recovering the washing liquid, and mixing with the washing liquid.
3. The method for recovering the active material from the cathode material of the waste cobalt-containing lithium ion battery as claimed in claim 1, wherein the water-washed solid slurry in the step (4) is subjected to preliminary evaporation and then thermal decomposition treatment.
4. The method for recovering the active material from the waste cobalt-containing lithium ion battery cathode material according to claim 1, wherein the molar ratio of the peroxodisulfate to the oxalate in the step (1) is 1: 1.5-2.5.
5. The method for recovering the active material from the cathode material of the waste cobalt-containing lithium ion battery as claimed in claim 1, wherein the concentration of the peroxydisulfate in the step (1) of the detergent is 0.05-0.15 mol/L.
6. The method for recovering the active material from the cathode material of the waste cobalt-containing lithium ion battery as claimed in claim 1, wherein the solid-to-liquid ratio of the cathode material of the waste cobalt-containing lithium ion battery to the detergent in the step (2) is 1: 30-60.
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