CN112374511B - Method for preparing lithium carbonate and ternary precursor by recycling waste ternary lithium battery - Google Patents
Method for preparing lithium carbonate and ternary precursor by recycling waste ternary lithium battery Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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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- 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 method for preparing lithium carbonate and a ternary precursor by recycling waste ternary lithium batteries, and belongs to the field of solid waste recycling. Graphite and a binder carried in black powder obtained after pretreatment of the waste ternary battery are used as a reducing agent, and the structure of the ternary material is destroyed through self-reduction phase conversion; converting lithium carbonate into lithium bicarbonate which is easy to be immersed in water by adopting a carbonated water immersion method, thereby realizing preferential leaching of lithium; the material after lithium extraction is directly leached by sulfuric acid without adding a reducing agent to obtain a nickel-cobalt-manganese solution. Impurities such as copper, iron, calcium and the like in the solution are deeply removed through an impurity removal process, the content of aluminum and magnesium in the solution is controlled, then nickel, cobalt and manganese in the solution are extracted into an organic phase by adopting synchronous extraction, a nickel, cobalt and manganese sulfate solution is obtained after back extraction by using sulfuric acid, and a high-quality ternary cathode material precursor can be prepared after the metal proportion is adjusted. The method has the advantages of high recovery rate of valuable metals of lithium, nickel, cobalt and manganese, short process, good product quality, economy and environmental protection.
Description
Technical Field
The invention belongs to the field of solid waste recycling, and particularly relates to a method for preparing battery-grade lithium carbonate and a ternary precursor by recycling waste ternary lithium batteries.
Background
With the development of the power automobile industry, the output and the demand of the lithium ion battery are increased year by year, and the scrappage of the power battery is increased year by year due to the effective service life of the lithium ion battery being 5-8 years, so that 35 ten thousand tons of waste lithium ion batteries are expected to be generated in 2025 years. In addition, the waste lithium ion batteries contain valuable metals such as Li, Ni, Co, Mn, Cu and the like, and the metals are expensive, so that the waste lithium ion batteries are efficiently and environmentally recycled, the environmental pressure can be solved, and considerable economic benefits can be brought.
The recovery process of the nickel-cobalt-manganese ternary lithium battery is mainly divided into a pyrogenic process and a wet process, wherein the pyrogenic process is generally used for directly smelting the waste lithium ion battery at high temperature to generate metal alloy, and then extracting valuable metals from the alloy, such as IEM of the department of beauty and germany in belgium. The wet process firstly disassembles and sorts the waste batteries, the obtained anode waste is leached by sulfuric acid, a certain amount of reducing agent is required to be added during leaching, and sulfate products of nickel, cobalt and manganese are obtained by purifying and extracting the leachate. The traditional wet process has the defects that a reducing agent is required to be added in the acid leaching process, the cost is high, the flow of the nickel-cobalt-manganese extraction separation process is long, and the operation is complex. In addition, the Li concentration in the raffinate after extracting the nickel, cobalt and manganese is lower, so that the lithium recovery rate is reduced.
In recent years, more and more attention is paid to a method for recovering valuable metals in a lithium ion battery by a combined process of a fire method and a wet method, for example, patent CN106129511A mixes a lithium ion battery anode material with a solid carbon reducing agent such as lignite and the like to perform reduction roasting, introduces carbon dioxide into a roasted product to perform water leaching to obtain a lithium bicarbonate solution, obtains a lithium carbonate product after evaporation and crystallization, and recovers nickel, cobalt and manganese after acid leaching or ammonia leaching of water leaching slag, and extracting and purifying the water leaching slag. The method takes solid carbon sources such as lignite and the like as reducing agents, the using amount of the reducing agents is large, and impurities in the reducing agents can influence the quality of nickel, cobalt and manganese products and graphite.
In the aspect of recycling nickel, cobalt and manganese, researchers propose to prepare a nickel, cobalt and manganese ternary precursor by adopting a direct coprecipitation mode, but the method needs to deeply remove impurities in a solution before precipitation, and obviously has great difficulty. The method comprises the steps of carrying out acid leaching treatment on a positive electrode material of a lithium battery in a patent CN107267759A, and carrying out multi-stage extraction on nickel, cobalt and manganese by using an alkaline saponification P507 extraction agent after impurity removal to obtain a back extraction solution of nickel, cobalt and manganese and a lithium-containing raffinate. However, when P507 is used for extraction, lithium is also extracted into the organic phase, and the lithium enters into the stripping solution during stripping, so that the quality of the nickel-cobalt-manganese precursor is affected, and the recovery rate of lithium is greatly reduced. In summary, there is a need to develop a method for efficiently and economically treating waste ternary lithium ion batteries to prepare lithium carbonate and precursors.
Disclosure of Invention
Aiming at the defects in the prior art, the method aims to provide a method for recycling and preparing battery-grade lithium carbonate and a ternary precursor from waste ternary lithium batteries.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a method for recycling and preparing lithium carbonate and a ternary precursor from a waste ternary lithium battery is characterized in that graphite and a binder carried in black powder obtained after pretreatment of the waste ternary battery are used as reducing agents, and the structure of the ternary material is destroyed through self-reduction phase conversion; converting lithium carbonate into lithium bicarbonate which is easy to be immersed in water by adopting a carbonated water immersion method, thereby realizing preferential leaching of lithium; the material after lithium extraction is directly leached by sulfuric acid without adding a reducing agent to obtain a nickel-cobalt-manganese solution. Removing impurities such as copper, iron, calcium and the like in the solution through the impurity removal working depth, controlling the content of aluminum and magnesium in the solution, then extracting nickel, cobalt and manganese in the solution into an organic phase by adopting synchronous extraction, and performing back extraction by using sulfuric acid to obtain a nickel, cobalt and manganese sulfate solution, wherein the lithium concentration in the back extraction solution is extremely low due to preferential recovery of the lithium (the water leaching rate is more than 90 percent), and the high-quality ternary anode material precursor can be prepared after the metal ratio is adjusted.
The method for preparing the lithium carbonate and the ternary precursor by recycling the waste ternary lithium battery comprises the following specific preparation steps:
(1) discharging, disassembling and crushing the waste ternary batteries, and screening the crushed materials, wherein oversize products comprise copper foils and aluminum foils, and undersize products comprise anode and cathode powder, a binder, a conductive agent and the like; roasting the undersize product under the condition of air isolation, wherein the roasting temperature is 500-700 ℃, and the roasting time is 1-3 hours;
(2) introducing CO into the roasted product2The lithium-containing solution and the water leaching slag are obtained by water leaching under the condition of (1), the solid-to-liquid ratio of the water leaching is 200-1000 g/L, and CO is added into each liter of solution2The feeding speed is 400-1000 mL/min, the water immersion temperature is 10-50 ℃, and the leaching rate of lithium is higher than 90%; heating the water leaching solution, and evaporating and crystallizing to obtain a lithium carbonate product;
(3) leaching the water leaching residue with sulfuric acid to obtain an acidic leaching solution of nickel, cobalt and manganese; adjusting the pH value of the pickle liquor, adding iron powder to remove copper impurities, removing impurities of iron and aluminum in the pickle liquor by a neutralization method, and removing calcium and magnesium by a fluoridation precipitation method;
(4) synchronously extracting nickel, cobalt and manganese in the solution after impurity removal by adopting an organic phosphoric acid extracting agent subjected to alkali saponification, and performing back extraction by adopting a sulfuric acid solution after washing to obtain a high-purity solution of nickel-cobalt-manganese sulfate;
(5) and (3) adjusting the proportion of nickel, cobalt and manganese in the nickel-cobalt-manganese salt solution by adding a pure reagent to reach the proportion of elements in the target ternary battery, adding an alkali solution, and preparing a ternary positive electrode material precursor in a reactor.
Further, the dosage of sulfuric acid in the sulfuric acid leaching in the step (3) is 1.1-2.0 times of the sum of the molar weight of nickel, cobalt and manganese, the solid-to-liquid ratio is 100-300 g/L, the leaching temperature is 20-50 ℃, and the leaching time is 1-3 hours.
Further, the pH value of the acid leaching solution is adjusted to be 1.5-2.0 in the step (3), and a precipitator for fluoride precipitation is one of sodium fluoride and potassium fluoride.
In the step (4), the extracting agent is an organic phosphoric acid extracting agent, the extracting agent is saponified in one of sodium hydroxide, potassium hydroxide and ammonia water, the saponification degree is 35% -70%, the synchronous extraction phase ratio is 1: 1-8: 1, and the pH value of the water phase is 3.5-6.0.
Compared with the prior art, the invention has the beneficial effects that:
(1) by adopting the method of preferentially extracting lithium, the problem that lithium cannot be effectively recovered due to low-lithium-concentration raffinate generated during the synchronous leaching of lithium is avoided, and the recovery rate of lithium is more than 90%.
(2) After reduction roasting is adopted, nickel, cobalt and manganese are converted into metal or low-valent oxide forms, the acid leaching difficulty is reduced, and the leaching rate of nickel, cobalt and manganese is more than 98% under the conditions that a reducing agent is not needed and the leaching condition is milder;
(3) because of preferential extraction of lithium, accurate control of impurity content and synchronous extraction processes, the high-quality anode material precursor is directly obtained, the process is greatly shortened, the recovery rate of valuable metals is high, and the method has obvious advantages in the aspect of economy compared with the traditional process.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which however falls within the scope of protection of the present invention.
Example 1
And (3) discharging the waste ternary lithium ion battery in saline water, and then disassembling, crushing and screening. 50g of undersize powder is taken and calcined for 2 hours at 550 ℃ under the condition of air isolation. The roasted product is leached by mechanical agitation with 200mL of water at 45 ℃ and continuously introducing CO at a flow rate of 200mL/min2. After the reaction is finished, lithium-containing water extract and water extract slag are obtained through solid-liquid separation, the leaching rate of lithium is 90.2% through detection and calculation, the leaching rates of nickel, cobalt and manganese are respectively 0.65%, 0.08% and 0.12%, and the lithium-containing water extract is evaporated and crystallized at the temperature of 100 ℃ to obtain a lithium carbonate product with the purity of more than 99%. And (3) carrying out acid leaching on the water leaching slag by using sulfuric acid with the molar weight of nickel, cobalt and manganese being 1.4 times of that of the water leaching slag, carrying out acid leaching for 2 hours at the temperature of 30 ℃ and at the acid leaching solid-liquid ratio of 150g/L, and filtering to obtain a mixed solution containing nickel, cobalt and manganese sulfate, wherein the leaching rates of nickel, cobalt and manganese are respectively 98.7%, 98.8% and 99.1%. Adjusting the pH value of the pickle liquor to 1.5, adding a certain amount of iron powder to remove copper impurities, removing impurities of iron and aluminum in the pickle liquor by a neutralization method, and removing calcium and magnesium in the pickle liquor by sodium fluoride to obtain a purified liquor containing nickel sulfate, cobalt sulfate and manganese sulfate. Synchronously extracting the solution after impurity removal by using P507 with the saponification rate of 35%, wherein the volume ratio of an organic phase to a water phase is 2: 1, controlling the pH value of the water phase to be 4.0, performing extraction and separation on the organic phase by adopting 2mol/L sulfuric acid to obtain a back extraction solution containing nickel, cobalt and manganese, adjusting the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese salt solution to be 1:1:1 by adding nickel sulfate, cobalt sulfate and manganese sulfate pure reagents, adding an alkali solution, and preparing the precursor of the NCM111 anode material in a reactor.
Example 2
And (3) discharging the waste ternary lithium ion battery in saline water, and then disassembling, crushing and screening. 50g of undersize powder is taken and calcined for 3 hours at 600 ℃ in the absence of air.The roasted product was mechanically stirred and leached with 250mL of water at 40 ℃ and CO was continuously introduced at a flow rate of 100mL/min2. After the reaction is finished, lithium-containing water extract and water extract slag are obtained through solid-liquid separation, the leaching rate of lithium is 91.3% through detection and calculation, the leaching rates of nickel, cobalt and manganese are respectively 0.64%, 0.05% and 0.16%, and the lithium-containing water extract is evaporated and crystallized at the temperature of 100 ℃ to obtain a lithium carbonate product with the purity of more than 99%. And (2) carrying out acid leaching on the water leaching slag by using sulfuric acid with the molar weight of nickel, cobalt and manganese being 1.2 times of that of the water leaching slag, carrying out acid leaching for 1h under the conditions of an acid leaching solid-liquid ratio of 250g/L and a temperature of 25 ℃, and filtering to obtain a mixed solution containing nickel, cobalt and manganese sulfate, wherein the leaching rates of nickel, cobalt and manganese are respectively 98.9%, 99.1% and 99.5%. Adjusting the pH value of the pickle liquor to 1.6, adding a certain amount of iron powder to remove copper impurities, removing impurities of iron and aluminum in the pickle liquor by a neutralization method, and removing calcium and magnesium in the pickle liquor by sodium fluoride to obtain a purified liquor containing nickel sulfate, cobalt sulfate and manganese sulfate. Synchronously extracting the solution after impurity removal by using P204 with saponification rate of 40%, wherein the volume ratio of the organic phase to the aqueous phase is 3: 1, controlling the pH value of the water phase to be 4.5, performing extraction and separation on the organic phase by adopting 2mol/L sulfuric acid to obtain a back extraction solution containing nickel, cobalt and manganese, adjusting the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese salt solution to be 8:1:1 by adding nickel sulfate, cobalt sulfate and manganese sulfate pure reagents, adding an alkali solution, and preparing the precursor of the NCM811 positive electrode material in a reactor.
Example 3
And (3) discharging the waste ternary lithium ion battery in saline water, and then disassembling, crushing and screening. 50g of undersize powder was calcined at 650 ℃ in the absence of air for 1 hour. The roasted product is leached by mechanical agitation with 300mL of water at 25 ℃ and continuously introducing CO at a flow rate of 150mL/min2. After the reaction is finished, lithium-containing water extract and water extract slag are obtained through solid-liquid separation, the leaching rate of lithium is 90.4% through detection and calculation, the leaching rates of nickel, cobalt and manganese are respectively 0.69%, 0.09% and 0.18%, and the lithium-containing water extract is evaporated and crystallized at the temperature of 100 ℃ to obtain a lithium carbonate product with the purity of more than 99%. Acid leaching is carried out on the water leaching slag by using sulfuric acid with the molar weight of nickel, cobalt and manganese being 1.6 times of that of the water leaching slag, and the solid-to-liquid ratio of the acid leaching is 200g/L and 35 g/LAcid leaching is carried out for 3h under the condition of DEG C, and a mixed solution containing nickel, cobalt and manganese sulfate is obtained after filtering, wherein the leaching rates of nickel, cobalt and manganese are respectively 98.7%, 98.5% and 99.4%. Adjusting the pH value of the pickle liquor to 1.8, adding a certain amount of iron powder to remove copper impurities, removing impurities of iron and aluminum in the pickle liquor by a neutralization method, and removing calcium and magnesium in the pickle liquor by sodium fluoride to obtain a purified liquor containing nickel sulfate, cobalt sulfate and manganese sulfate. Synchronously extracting the solution after impurity removal by using P507 with the saponification rate of 45%, wherein the volume ratio of an organic phase to a water phase is 4: controlling the pH value of the water phase to be 5.0, performing back extraction on the organic phase by adopting 2mol/L sulfuric acid after extraction and separation to obtain a back extraction solution containing nickel, cobalt and manganese, adjusting the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese salt solution to be 5:2:3 by adding nickel sulfate, cobalt sulfate and manganese sulfate pure reagents, adding an alkali solution, and preparing the precursor of the NCM523 positive electrode material in a reactor.
Example 4
And (3) discharging the waste ternary lithium ion battery in saline water, and then disassembling, crushing and screening. 50g of undersize powder is taken and calcined for 2.5 hours at the temperature of 500 ℃ under the condition of air isolation. The roasted product was mechanically stirred and leached with 200mL of water at 50 ℃ and CO was continuously introduced at a flow rate of 100mL/min2. After the reaction is finished, lithium-containing water extract and water extract slag are obtained through solid-liquid separation, the leaching rate of lithium is up to 91.7% through detection and calculation, the leaching rates of nickel, cobalt and manganese are respectively 0.56%, 0.11% and 0.16%, and the lithium-containing water extract is evaporated and crystallized at the temperature of 100 ℃ to obtain a lithium carbonate product with the purity of more than 99%. And (3) carrying out acid leaching on the water leaching slag by using sulfuric acid with the molar weight of nickel, cobalt and manganese being 1.9 times of that of the water leaching slag, carrying out acid leaching for 2.5 hours at the temperature of 50 ℃ under the condition that the acid leaching solid-to-liquid ratio is 300g/L, and filtering to obtain a mixed solution containing nickel, cobalt and manganese sulfate, wherein the leaching rates of nickel, cobalt and manganese are respectively 98.9%, 99.2% and 98.4%. Adjusting the pH value of the pickle liquor to 1.7, adding a certain amount of iron powder to remove copper impurities, removing impurities of iron and aluminum in the pickle liquor by a neutralization method, and removing calcium and magnesium in the pickle liquor by sodium fluoride to obtain a purified liquor containing nickel sulfate, cobalt sulfate and manganese sulfate. The solution after impurity removal is synchronously extracted by using Cyanex272 with the saponification rate of 50 percent, wherein the volume ratio of an organic phase to a water phase is 6: controlling the pH value of the water phase to be 6.0, performing back extraction on the organic phase by adopting 2mol/L sulfuric acid after extraction and separation to obtain a back extraction solution containing nickel, cobalt and manganese, adjusting the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese salt solution to be 6:2:2 by adding nickel sulfate, cobalt sulfate and manganese sulfate pure reagents, adding an alkali solution, and preparing the precursor of the NCM622 positive electrode material in a reactor.
Claims (4)
1. A method for recycling and preparing lithium carbonate and a ternary precursor from a waste ternary lithium battery is characterized in that graphite and a binder carried in black powder obtained after pretreatment of the waste ternary battery are used as reducing agents, and the structure of the ternary material is destroyed through self-reduction phase conversion; converting lithium carbonate into lithium bicarbonate which is easy to be immersed in water by adopting a carbonated water immersion method, thereby realizing preferential leaching of lithium; the material after lithium extraction is directly leached by sulfuric acid without adding a reducing agent to obtain a nickel-cobalt-manganese solution; removing impurities such as copper, iron and calcium in the solution through impurity removal working depth, controlling the content of aluminum and magnesium in the solution, extracting nickel, cobalt and manganese in the solution into an organic phase by synchronous extraction, performing back extraction by using sulfuric acid to obtain a nickel, cobalt and manganese sulfate solution, and preparing a high-quality ternary anode material precursor after adjusting metal proportion due to preferential recovery of lithium on the premise that the water leaching rate needs to be higher than 90%;
the preparation method comprises the following specific steps:
(1) discharging, disassembling and crushing the waste ternary batteries, and screening the crushed materials, wherein oversize products comprise copper foils and aluminum foils, and undersize products comprise anode and cathode powder, a binder and a conductive agent; roasting the undersize product under the condition of air isolation, wherein the roasting temperature is 500-700 ℃, and the roasting time is 1-3 hours;
(2) introducing CO into the roasted product2Carrying out water leaching under the condition to obtain a lithium-containing solution and water leaching slag, wherein the solid-to-liquid ratio of water leaching is 200-1000 g/L, and CO is contained in each liter of solution2The feeding speed is 400-1000 mL/min, the water immersion temperature is 10-50 ℃, and the leaching rate of lithium is higher than 90%; heating the water leaching solution, and evaporating and crystallizing to obtain a lithium carbonate product;
(3) leaching the water leaching residue with sulfuric acid to obtain an acidic leaching solution of nickel, cobalt and manganese; adjusting the pH value of the pickle liquor, adding iron powder to remove copper impurities, removing impurities of iron and aluminum in the pickle liquor by a neutralization method, and removing calcium and magnesium by a fluoridation precipitation method;
(4) synchronously extracting nickel, cobalt and manganese in the solution after impurity removal by adopting an organic phosphoric acid extracting agent subjected to alkali saponification, and performing back extraction by adopting a sulfuric acid solution after washing to obtain a high-purity solution of nickel-cobalt-manganese sulfate;
(5) and (3) adjusting the proportion of nickel, cobalt and manganese in the nickel-cobalt-manganese salt solution by adding a pure reagent to reach the proportion of elements in the target ternary battery, adding an alkali solution, and preparing a ternary positive electrode material precursor in a reactor.
2. The method for preparing lithium carbonate and a ternary precursor by recycling the waste ternary lithium battery as claimed in claim 1, is characterized in that: the dosage of sulfuric acid in the sulfuric acid leaching in the step (3) is 1.1-2.0 times of the sum of the molar weight of nickel, cobalt and manganese, the solid-to-liquid ratio is 100-300 g/L, the leaching temperature is 20-50 ℃, and the leaching time is 1-3 hours.
3. The method for preparing lithium carbonate and a ternary precursor by recycling the waste ternary lithium battery as claimed in claim 1, is characterized in that: and (4) adjusting the pH range of the pickle liquor in the step (3) to be 1.5-2.0, wherein the precipitator of the fluoridation is one of sodium fluoride and potassium fluoride.
4. The method for preparing lithium carbonate and a ternary precursor by recycling the waste ternary lithium battery as claimed in claim 1, is characterized in that: the extracting agent used in the step (4) is an organic phosphoric acid extracting agent, the extracting agent is saponified in one of sodium hydroxide, potassium hydroxide and ammonia water, the saponification degree is 35% -70%, the O/A ratio of synchronous extraction is 1: 1-8: 1, and the pH value of a water phase is 3.5-6.0.
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| CN111206148A (en) * | 2020-03-16 | 2020-05-29 | 宁波容百新能源科技股份有限公司 | Method for recycling and preparing ternary cathode material by using waste ternary lithium battery |
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