CN119824227B - Process for selectively extracting valuable metals of lithium battery - Google Patents
Process for selectively extracting valuable metals of lithium batteryInfo
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- CN119824227B CN119824227B CN202411931279.5A CN202411931279A CN119824227B CN 119824227 B CN119824227 B CN 119824227B CN 202411931279 A CN202411931279 A CN 202411931279A CN 119824227 B CN119824227 B CN 119824227B
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Abstract
本发明涉及一种锂电池有价金属的选择性提取的工艺，包括放电，正极材料分离，热处理，酸浸，共沉淀，沉锂等步骤，实现废旧锂电池中有价金属的高效回收和利用。The present invention relates to a process for selectively extracting valuable metals from lithium batteries, comprising the steps of discharging, separation of positive electrode materials, heat treatment, acid leaching, coprecipitation, lithium precipitation, etc., to achieve efficient recovery and utilization of valuable metals in waste lithium batteries.
Description
Technical Field
The invention belongs to the technical field of waste lithium batteries, and particularly relates to a process for selectively extracting valuable metals from a lithium battery.
Background
The lithium battery anode material LiFePO4 is applied to the fields of mobile phones, electric automobiles and the like on a large scale because of the advantages of higher discharge specific capacity, a more stable discharge platform, good cycle stability, thermal stability, low price and the like. In recent years, the yield of the lithium iron phosphate battery is gradually increased, and the scrapping amount of the lithium iron phosphate battery is gradually increased. Batteries contain toxic chemicals and high value metals that must be recycled to promote environmental protection and sustainable development. The pretreatment process of the waste lithium battery mainly comprises the procedures of classification, discharging, disassembly, crushing, separation, removal of organic binder and the like, and finally black powder rich in the positive electrode material is obtained. Therefore, the invention improves the recovery of various valuable metals by researching acid leaching treatment and the like of the waste lithium batteries.
In the traditional wet leaching, the leaching system of acid and reducing agent is widely used as the reduction criminal at present in the acid leaching process of the anode material, and the leaching system has the advantages of green environmental protection and no pollution, but has the problems of lower thermal decomposition temperature and inconvenient transportation and storage. Recently, some researchers have begun to try to use natural products as reducing agents, such as the reducing group of the shell of macadamia nut, orange peel, starch, and the like, which are also often used in acid leaching processes. These reducing agents are more environmentally friendly, and are also safe and convenient to transport or store. The natural product tea polyphenol is used as a reducing agent to construct a sulfuric acid-tea polyphenol leaching system, so that the high-selectivity recovery of each metal ion is realized. The choice of a naturally efficient reducing agent is therefore the focus of the research of the present invention.
The recovery and extraction of various valuable metals in the waste lithium batteries are treated by fractional precipitation under different process conditions, so that the recovery efficiency can be effectively improved, the environmental pollution can be reduced, and the recycling of resources can be promoted. So how to efficiently and stepwise precipitate and recycle valuable metals is the research focus of the invention.
Disclosure of Invention
The invention aims to provide a process for selectively extracting valuable metals from a lithium battery.
In order to solve the technical problems, the specific process of the invention is as follows:
The process for selectively extracting valuable metals of the lithium battery comprises discharging, separating positive electrode materials, heat treatment, acid leaching, coprecipitation and lithium precipitation, and is characterized in that sulfuric acid with the mass fraction of 10% is added into the ground positive electrode raw materials, the ratio of sulfuric acid to reducing agent is 8:2-3, the solid-liquid ratio is 30g/L, the reaction temperature is 55-60 ℃, the time is 60min, the stirring speed is controlled to 400-600rpm, and the filtrate is obtained after leaching;
Wherein the reducing agent is a gallic acid catechin solution with the mass fraction of 40-50%.
Wherein, the coprecipitation treatment is to add 30-50% of coprecipitation agent into the leaching solution, the reaction temperature is 40-50 ℃, the stirring speed is 400-500rpm, and the reaction time is 60min, so that the ternary positive electrode material precursor and the lithium-rich solution can be obtained.
Wherein the coprecipitation agent is hydroxylamine sulfonic acid solution with the mass fraction of 20-30%.
A selective extraction process of valuable metals of a lithium battery is carried out according to the following steps:
Discharging the battery, namely discharging the waste battery for 24 hours by adopting NaCl solution with the mass fraction of 5%, and mechanically separating the battery core to obtain an anode, a cathode and a diaphragm;
cutting the positive electrode plate into small pieces with the length of 1x1cm, soaking the small pieces in 15% NMP solution, stirring the small pieces for 1h at the temperature of 100 ℃ under ultrasonic 240w, accelerating the separation of the positive electrode material, and dissolving PVDF binder;
Heat treatment, namely calcining the separated positive electrode material for 2 hours at 700 ℃ in a muffle furnace, and grinding the positive electrode material to serve as a raw material for acidolysis;
and (3) lithium precipitation, namely further precipitating the lithium-rich solution subjected to acid leaching and coprecipitation treatment, adding a NaOH solution into the lithium-rich solution to adjust the pH of the solution to 9-11, adding 30-40% of lithium precipitating agent, and reacting for 2 hours at 90-95 ℃ at the stirring rotating speed of 200-400rpm to obtain a precipitate.
Wherein the lithium precipitating agent is a disodium 5' -xanthate solution with the mass fraction of 32-46%.
The invention has the beneficial effects that:
1. According to the invention, the steps of discharging, separating the anode material, heat treatment, acid leaching, coprecipitation, lithium precipitation and the like are adopted to realize efficient recovery and utilization of valuable metals in the waste lithium battery, the extraction and leaching of the valuable metals are improved by adopting a natural reducing agent in combination with acid leaching, and the precipitation recovery of the valuable metals is increased to the greatest extent in a step-by-step precipitation mode, so that the loss of the valuable metals is reduced.
2. Wherein the phenolic hydroxyl group of the gallol catechin can reduce a metal ion or a metal oxide by providing an electron. During the pickling process, the metal ions are often present in a high valence state, while the phenolic hydroxyl groups of the gallol catechins are able to react with these metal ions, reducing them to lower valence metals, promoting their dissolution and leaching. In the acid leaching process, sulfuric acid provides an acidic environment, which is favorable for dissolving metal compounds, and gallol catechin promotes the dissolution of metals through reduction, so that the leaching efficiency is improved. The reaction process releases more heat, increasing the collision frequency between molecules, thereby accelerating the reaction.
3. Compared with tea polyphenol, the gallol catechin is used as a reducing agent in the recovery of waste batteries, has higher reducing capability, better stability and selectivity and lower environmental hazard, has certain advantages in the aspects of cost and raw material supply, can obviously improve the recovery efficiency and environmental protection of waste lithium batteries, can reduce the emission of harmful waste water and reduce the wet leaching cost.
4. The invention uses coprecipitation method to adjust PH to precipitate nickel, cobalt and manganese ions in the leaching solution and obtain the precursor product with good morphology and phase structure, and the precursor product can reduce target metal ions more effectively due to the reduction effect of hydroxylamine sulfonic acid, thereby improving the purity of the precipitate. By adjusting the concentration of hydroxylamine and the reaction conditions, the generation of byproducts can be reduced, and the selectivity of precipitation can be improved.
5. The addition of hydroxylamine sulfonic acid can be performed over a wide pH range, while other reducing agents are more sensitive to pH changes. Oxalate shows the best precipitation effect at lower pH, but is less reactive in neutral or alkaline environments. In contrast, the reducibility of hydroxylamine sulfonic acid can effectively play a role under wider acid-base conditions, and has stronger adaptability. The hydroxylamine reduction rate in hydroxylamine sulfonic acid is mild, and the particle size distribution in the precipitation process can be controlled. The more uniform reduction reaction ensures that the precipitate has a small particle size and is uniformly distributed.
6. In lithium-rich solutions, there is typically some salt effect that enhances the solvation effect and weakens the interactions between ions, resulting in the ions in the solution not being able to effectively contact and react during the reaction. The affinity of the phosphate group in the disodium xanthate and lithium ions is strong, so that the collision probability between the phosphate ions and the lithium ions in the solution can be effectively increased, and the generation of lithium phosphate is further promoted. The phosphate group of the disodium 5' -xanthate can effectively form a complex with lithium ions, and the influence of the ionic strength in the solution is reduced, so that the inhibition effect of a salt effect is overcome, and the precipitation of lithium phosphate is promoted. The disodium xanthate not only improves the reaction efficiency of lithium ions and phosphate ions through phosphate radical in the structure, but also has a certain structural stabilization effect on purine ring parts, so that the phosphate ions are more stable in the solution and are not easy to be interfered by other salt ions, thereby improving the precipitation efficiency of lithium.
Detailed Description
The present invention will be described in further detail with reference to examples. The waste lithium battery is a nickel cobalt lithium manganate battery (NCM 523 type), the waste battery is discharged for 24 hours by adopting NaCl solution with the mass fraction of 5%, the battery core is mechanically separated to obtain an anode, a cathode and a diaphragm, the anode plate is cut into small pieces with the size of 1x1cm, the small pieces are soaked in NMP solution with the mass fraction of 15% and are stirred for 1 hour at the temperature of 100 ℃ by ultrasonic 240w, the separation of the anode material is accelerated, PVDF binder is dissolved, the separated anode material is calcined for 2 hours in a muffle furnace with the temperature of 700 ℃, and then ground to serve as raw materials for acidolysis, and the following test is carried out.
Example 1
Acid leaching treatment, namely adding 10% sulfuric acid into the ground anode raw material, wherein the reducing agent is 45% gallol catechin solution, the ratio of the sulfuric acid to the reducing agent is 8:2.5, the solid-liquid ratio is 30g/L, the reaction temperature is 58 ℃ and the time is 60min, the stirring speed is controlled to be 500rpm, and filtering is carried out after leaching to obtain filtrate;
Example 2
Acid leaching treatment, namely adding 10% of sulfuric acid into the ground anode raw material, wherein the reducing agent is 40% of gallic acid catechin solution, the ratio of the sulfuric acid to the reducing agent is 8:2, the solid-liquid ratio is 30g/L, the reaction temperature is 60 ℃, the time is 60min, the stirring speed is controlled to be 400rpm, and filtering is carried out after leaching to obtain filtrate;
Example 3
Acid leaching treatment, namely adding 10% of sulfuric acid into the ground anode raw material, wherein the reducing agent is 50% of gallic acid catechin solution, the ratio of the sulfuric acid to the reducing agent is 8:3, the solid-liquid ratio is 30g/L, the reaction temperature is 55 ℃, the time is 60min, the stirring speed is controlled to be 600rpm, and filtering is carried out after leaching to obtain filtrate;
Comparative example 1
The present comparative example is different from example 1 in that the gallol catechin solution in the present comparative example is a tea polyphenol solution, and the rest is the same as example 1.
Comparative example 2
The comparative example is different from example 1 in the addition amount of the gallol catechin solution, specifically, the acid leaching treatment is performed by adding 10% by mass of sulfuric acid, 45% by mass of the gallol catechin solution as a reducing agent, the ratio of the sulfuric acid to the reducing agent is 8:4, the solid-liquid ratio is 30g/L, the reaction temperature is 58 ℃ and the time is 60min, the stirring speed is controlled to 500rpm, leaching and filtering are performed to obtain a filtrate, and the rest is the same as in example 1.
Comparative example 3
The comparative example is different from example 1 in the addition amount of the gallol catechin solution, specifically, the acid leaching treatment is performed by adding 10% by mass of sulfuric acid, 45% by mass of the gallol catechin solution as a reducing agent, the ratio of the sulfuric acid to the reducing agent is 8:1, the solid-liquid ratio is 30g/L, the reaction temperature is 58 ℃ and the time is 60min, the stirring speed is controlled to 500rpm, leaching and filtering are performed to obtain a filtrate, and the rest is the same as in example 1.
Test 1 leaching Rate
And (5) leaching the filtrate after the acid leaching treatment, detecting the concentration of metal ions, and measuring the leaching rate (zeta).
C is the value of the concentration of ions in the leaching solution, g/L, V is the value of the volume of the leaching solution, L, m is the value of the mass of the raw material, g and w are the values of the content of each valuable metal in the raw material, and% are units.
The results are shown in Table 1.
TABLE 1
| Sample of | Li extraction Rate (%) | Ni leaching yield (%) | Co leaching Rate (%) | Mn leaching yield (%) |
| Example 1 | 99.84 | 99.46 | 99.58 | 99.21 |
| Example 2 | 99.69 | 99.23 | 99.47 | 99.05 |
| Example 3 | 99.78 | 99.31 | 99.52 | 99.14 |
| Comparative example 1 | 92.65 | 93.14 | 91.65 | 91.36 |
| Comparative example 2 | 97.48 | 98.02 | 96.48 | 97.08 |
| Comparative example 3 | 95.27 | 96.52 | 94.61 | 95.69 |
The following embodiments are all performed on the basis of example 1.
Example 4
And coprecipitation, namely adding 40% of hydroxylamine sulfonic acid solution with the mass fraction of 25% into the leaching solution, wherein the reaction temperature is 45 ℃, the stirring speed is 450rpm, and the reaction time is 60 minutes, so that a ternary positive electrode material precursor and a lithium-rich solution can be obtained.
And (3) precipitating lithium, namely further precipitating the lithium-rich solution, adding a NaOH solution into the lithium-rich solution to adjust the pH of the solution to 10, adding 35% of 39% of 5' -disodium xanthate solution, and reacting for 2 hours at 92 ℃ at the stirring rotating speed of 300rpm to obtain a precipitate.
Example 5
And coprecipitation, namely adding 30% of hydroxylamine sulfonic acid solution with the mass fraction of 20% into the leaching solution, wherein the reaction temperature is 50 ℃, the stirring speed is 400rpm, and the reaction time is 60 minutes, so that a ternary positive electrode material precursor and a lithium-rich solution can be obtained.
And (3) precipitating lithium, namely further precipitating the lithium-rich solution, adding a NaOH solution into the lithium-rich solution to adjust the pH of the solution to 11, adding 30% of 46% of 5' -disodium xanthate solution, and reacting for 2 hours at 90 ℃ at the stirring speed of 400rpm to obtain a precipitate.
Example 6
And coprecipitation, namely adding 50% of hydroxylamine sulfonic acid solution with the mass fraction of 30% into the leaching solution, wherein the reaction temperature is 50 ℃, the stirring speed is 500rpm, and the reaction time is 60 minutes, so that a ternary positive electrode material precursor and a lithium-rich solution can be obtained.
And (3) precipitating lithium, namely further precipitating the lithium-rich solution, adding a NaOH solution into the lithium-rich solution to adjust the pH of the solution to 11, adding 40% of 32% of disodium 5' -xanthate solution, and reacting for 2 hours at 95 ℃ at the stirring rotating speed of 200rpm to obtain a precipitate.
Comparative example 4
The present comparative example is different from example 4 in that hydroxylamine sulfonic acid in the present comparative example is ammonium oxalate, and the rest is the same as example 4.
Comparative example 5
The comparative example differs from example 4 in that the amount of hydroxylamine sulfonic acid added in the comparative example was different, specifically coprecipitation in that a hydroxylamine sulfonic acid solution having a mass fraction of 25% was added to the leachate, the reaction temperature was 45 ℃, the stirring rotation speed was 450rpm, and the reaction time was 60 minutes, whereby a ternary positive electrode material precursor and a lithium-rich solution were obtained, and the rest was the same as in example 4.
Comparative example 6
The comparative example differs from example 4 in that the amount of hydroxylamine sulfonic acid added in the comparative example was different, specifically coprecipitation in that a hydroxylamine sulfonic acid solution having a mass fraction of 25% was added to the leachate, the reaction temperature was 45 ℃, the stirring rotation speed was 450rpm, and the reaction time was 60 minutes, at which time a ternary positive electrode material precursor and a lithium-rich solution were obtained, and the rest was the same as in example 4.
Comparative example 7
The comparative example was different from example 4 in that the disodium 5' -xanthylate of the comparative example was sodium carbonate, and the rest was the same as example 4.
Comparative example 8
The comparative example is different from example 4 in the addition amount of the disodium 5 '-xanthate solution in the comparative example, and specifically, lithium is precipitated by further precipitating a lithium-rich solution, adding NaOH solution into the lithium-rich solution to adjust the pH of the solution to 10, adding 50% of 39% of the disodium 5' -xanthate solution, and reacting at 92 ℃ at a stirring speed of 300rpm for 2 hours to obtain a precipitate, and the rest is the same as example 4.
Comparative example 9
The comparative example is different from example 4 in the addition amount of the disodium 5 '-xanthate solution in the comparative example, and specifically, lithium is precipitated by further precipitating a lithium-rich solution, adding NaOH solution into the lithium-rich solution to adjust the pH of the solution to 10, adding 20% of 39% of the disodium 5' -xanthate solution, and reacting at 92 ℃ at a stirring speed of 300rpm for 2 hours to obtain a precipitate, and the rest is the same as example 4.
Comparative example 10
The difference between this comparative example and example 4 is that the one-step precipitation method was used, specifically, 40% of an ammonium oxalate solution with a mass fraction of 25% was added to the leachate, the reaction temperature was 45℃and the stirring speed was 450rpm, and the reaction time was 60 minutes, at which time precipitation was obtained.
Test 2 Total recovery
The valuable metal content in the waste lithium battery before the treatment and the valuable metal content obtained after the treatment were measured to obtain the total recovery rate as shown in the following table 2.
TABLE 2
Claims (3)
1. The process for selectively extracting valuable metals of the lithium battery comprises the steps of discharging, separating positive electrode materials, heat treatment, acid leaching, coprecipitation and lithium precipitation, and is characterized in that the process comprises the following steps:
Discharging the battery, namely discharging the waste battery for 24 hours by adopting NaCl solution with the mass fraction of 5%, and mechanically separating the battery core to obtain an anode, a cathode and a diaphragm;
cutting the positive electrode plate into small pieces with the length of 1x1cm, soaking the small pieces in 15% NMP solution, stirring the small pieces for 1h at the temperature of 100 ℃ under ultrasonic 240w, accelerating the separation of the positive electrode material, and dissolving PVDF binder;
Heat treatment, namely calcining the separated positive electrode material for 2 hours at 700 ℃ in a muffle furnace, and grinding the positive electrode material to serve as a raw material for acidolysis;
the acid leaching treatment comprises the steps of adding sulfuric acid with the mass fraction of 10% into the ground anode raw material, wherein the ratio of sulfuric acid to reducing agent is 8:2-3, the solid-liquid ratio is 30g/L, the reaction temperature is 55-60 ℃, the time is 60min, the stirring speed is controlled to 400-600rpm, and filtering is carried out after leaching to obtain filtrate;
The reducing agent is a gallic acid catechin solution with the mass fraction of 40-50%;
The coprecipitation treatment is to add 30-50% of coprecipitation agent into the leaching solution, the reaction temperature is 40-50 ℃, the stirring rotation speed is 400-500rpm, and the reaction time is 60min, so that a ternary positive electrode material precursor and a lithium-rich solution can be obtained;
the coprecipitate is hydroxylamine sulfonic acid solution with the mass fraction of 20-30%.
2. The process for selectively extracting valuable metals from lithium batteries according to claim 1, wherein the lithium precipitation process is characterized in that acid leaching and further precipitating a lithium-rich solution after coprecipitation treatment, adding NaOH solution into the lithium-rich solution to adjust the pH of the solution to 9-11, adding 30-40% of lithium precipitating agent, and reacting for 2 hours at 90-95 ℃ at a stirring speed of 200-400rpm to obtain precipitate.
3. The process for selectively extracting valuable metals from a lithium battery according to claim 2, wherein the lithium precipitating agent is a solution of disodium 5' -xanthate with a mass fraction of 32-46%.
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