CN107871912B - Method for removing iron and aluminum from leachate generated during recovery of valuable metals in waste lithium ion batteries - Google Patents
Method for removing iron and aluminum from leachate generated during recovery of valuable metals in waste lithium ion batteries Download PDFInfo
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Abstract
The invention belongs to the field of solution purification in hydrometallurgy, and discloses a method for removing iron and aluminum from leachate (nickel-cobalt-manganese sulfate solution) generated when valuable metals in waste lithium ion batteries are recovered. The method comprises the following steps: (1) adjusting the pH value of the leachate to 1.5-2.0, and adding an oxidant to oxidize ferrous iron into ferric iron; (2) adjusting the pH value of the system to 2.5-3.5, aging, and filtering to obtain a filtrate and iron-aluminum slag; (3) and adjusting the pH value of the system to 4.5-5.0, aging and filtering to obtain a purified liquid and aluminum slag. And (4) using the aluminum slag obtained in the step (3) as a regulator for regulating the pH value of the system in the step (2). The method can reduce the contents of iron and aluminum in the solution to the required values for production, the produced slag has good filtering performance, the valuable metals carried in the slag are few, the obtained aluminum slag can be repeatedly used for removing iron in the system, the aim of reducing the slag is fulfilled, and the method has good economic benefit and environmental benefit.
Description
Technical Field
The invention belongs to the field of solution purification in hydrometallurgy, and particularly relates to a method for removing iron and aluminum from leachate (nickel-cobalt-manganese sulfate solution) generated when valuable metals in waste lithium ion batteries are recovered.
Background
Since the commercialization of lithium ion batteries, lithium ion batteries have unique advantages of high specific energy, small volume, light weight, wide application temperature range, long cycle life, good safety performance and the like, and are widely used in the civil and military fields, such as video cameras, mobile phones, notebook computers, portable measuring instruments and the like, and meanwhile, lithium ion batteries have become one of the preferred light-weight high-energy power batteries for new energy electric vehicles. After 500-1500 charge-discharge cycles, the active substances of the lithium ion battery lose activity, so that the capacity of the battery is reduced and the battery is scrapped. The wide use of lithium ion batteries tends to bring a large amount of waste batteries, and if the waste batteries are discarded at will, the environment is seriously polluted, and resources are wasted. The lithium ion battery contains more metal resources such as nickel (Ni), cobalt (Co), copper (Cu), lithium (Li), aluminum (Al), manganese (Mn) and the like, wherein the contents of the cobalt, the nickel, the manganese and the lithium can respectively reach 30%, 20% and 35%, and even higher. Therefore, the method has great significance in recycling the metal with high economic value in the waste lithium ion battery, both from the aspect of environmental protection and the aspect of recycling resources.
At present, valuable metals are recycled and then prepared into battery materials in the industries for recycling waste lithium ion batteries, but the battery materials have high requirements on impurity content. The waste lithium ion battery contains elements such as iron, aluminum, zinc, copper, carbon and the like, so that the leaching solution needs to be purified in the process of recovering valuable metals in the battery, and the problems that the iron and the aluminum in the leaching solution can be completely removed, the amount of metals carried in slag is small, the generation amount of the slag is small, the impurity removal cost is low and the like are always puzzling the battery recovery industry are solved. By referring to a large number of references, no technical personnel at home have been engaged in the research of removing iron and aluminum by using a two-step method.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the first object of the present invention is to provide a simple and efficient method for removing iron and aluminum from the leachate (nickel-cobalt-manganese sulfate solution) generated during the recovery of valuable metals from waste lithium ion batteries, so as to solve various problems encountered in removing iron and aluminum during the recovery of valuable metals from waste lithium ion batteries.
The purpose of the invention is realized by the following scheme:
a simple and efficient method for removing iron and aluminum from leachate (nickel-cobalt-manganese sulfate solution) generated in the process of recovering valuable metals in waste lithium ion batteries comprises the following steps:
(1) adjusting the pH value of the leachate to 1.5-2.0, and adding an oxidant to oxidize ferrous iron into ferric iron;
(2) adjusting the pH value of the system to 2.5-3.5, aging, and filtering to obtain a filtrate and iron-aluminum slag;
(3) and adjusting the pH value of the system to 4.5-5.0, aging and filtering to obtain a purified liquid and aluminum slag.
The aluminum slag obtained in the step (3) can be used as a regulator for regulating the pH value of the system in the step (2). Thereby removing iron and obtaining the iron-aluminum slag.
When the aluminum slag is used in the step (2), preferably, the aluminum slag is added into the system in the step (2) to react for 0.5h or more, and then the pH value of the system is continuously adjusted; more preferably for 0.5 to 1 hour.
The leaching solution in the step (1) is preferably a nickel-cobalt-manganese sulfate solution generated in the process of recovering valuable metals in waste lithium ion batteries, and is more preferably a nickel-cobalt-manganese sulfate solution after copper removal.
The oxidant in the step (1) is an oxidant which is conventionally used in the field, such as hydrogen peroxide, sodium chlorate, potassium permanganate and the like.
The amount of oxidant used is such that all of the ferrous iron in the system is oxidized to tertiary iron.
The pH adjustment in the steps (1) to (3) can be performed by using alkali or acid, and the alkali can be at least one of sodium carbonate, sodium hydroxide, calcium carbonate, calcium hydroxide, calcium oxide and the like.
The aging time in the step (2) and the step (3) is preferably 0.5h or more, preferably 0.5-1 h.
And (3) washing the iron-aluminum slag obtained in the step (2) by adopting water or dilute acid.
And (3) the iron-aluminum slag obtained in the step (2) can be sold for the outside.
And (3) the purifying solution is the target solution after removing iron and aluminum, and can be used for subsequent valuable metal recovery treatment.
The process of the invention preferably comprises the following steps:
(1) adjusting the pH value of the leachate to 1.5-2.0, and adding an oxidant to oxidize ferrous iron into ferric iron;
(2) adjusting the pH value of the system to 2.5-3.5, aging, and filtering to obtain a filtrate and iron-aluminum slag;
(3) adjusting the pH value of the system to 4.5-5.0, aging and filtering to obtain a purified liquid and aluminum slag;
(4) adding the aluminum slag obtained in the step (3) as a pH regulator into the system pH regulated in the step (2) to remove iron, thereby obtaining iron-aluminum slag;
(5) and circulating the steps to realize the continuous iron and aluminum removal of the leachate.
The method adopts a two-step method to remove iron and aluminum from the nickel-cobalt-manganese sulfate solution generated when valuable metals in the waste lithium ion batteries are recovered, so that the content of iron and aluminum in the solution can be reduced to a production required value, the generated slag has good filtering performance, the valuable metals carried in the slag are less, more importantly, the amount of the slag is obviously reduced compared with a one-step method for removing the iron and the aluminum, and the reduction target of the slag is realized, so that the method for removing the iron and the aluminum by using the two-step method has better economic benefit and environmental benefit.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the method takes nickel-cobalt-manganese sulfate solution generated in the process of recovering valuable metals in waste lithium ion batteries as a raw material, and completely removes iron and aluminum in the nickel-cobalt-manganese sulfate solution after copper removal by a two-step iron and aluminum removal method. The method has the advantages of simple process and simple and convenient operation, the generated iron-aluminum slag has less amount, the slag is mixed with less amount of valuable metals such as nickel, cobalt, manganese and the like, and the obtained aluminum slag can be repeatedly used for removing iron in a system, thereby not only realizing the purification of iron and aluminum in the solution, but also realizing the reduction of the slag and having better environmental benefit and economic benefit.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The materials referred to in the following examples are commercially available.
Example 1
The process flow is shown in figure 1. Taking 500mL of the nickel, cobalt and manganese sulfate solution without copper, adjusting the pH value to 1.5 by using sodium carbonate, adding hydrogen peroxide with the mass fraction of 20% into the solution to oxidize all ferrous iron in the system into ferric iron, and sampling and detecting whether the ferrous iron in the system is completely oxidized by using potassium ferricyanide. Adding aluminum slag into the oxidized solution, reacting for 0.5h, adding calcium carbonate solution to adjust pH to 2.5 (when no aluminum slag exists in the primary treatment, directly adding calcium carbonate solution to adjust pH to 2.5), aging for 30min, filtering, allowing the filtrate to flow into a reaction kettle except aluminum, washing iron and aluminum slag, and selling. Adjusting the pH of the filtrate to 4.5 with sodium carbonate solution, aging for 1h, filtering to obtain purified liquid and aluminum slag, allowing the purified liquid to flow into the next step, and removing iron from the aluminum slag in the previous step to obtain iron-aluminum slag. Through detection, the purified solution has the iron concentration of 5mg/L and the aluminum concentration of 75mg/L, and meets the production requirement; the content of nickel in the iron-aluminum slag (dry basis) is 0.5 wt%, the content of cobalt is 0.2 wt%, and the content of manganese is 0.8 wt%, which meets the production control standard.
Example 2
Taking 500mL of the nickel, cobalt and manganese sulfate solution without copper, adjusting the pH value of the nickel, cobalt and manganese sulfate solution to 2.0 by using sodium carbonate, adding hydrogen peroxide with the mass fraction of 20% into the solution to oxidize all ferrous iron into ferric iron, and detecting whether the ferrous iron is completely oxidized in a system by sampling potassium ferricyanide. Adding aluminum slag into the oxidized solution, reacting for 1h, adding a calcium carbonate solution to adjust the pH to 3.5, aging for 30min, filtering, allowing the filtrate to flow into an aluminum-removing reaction kettle, and washing iron and aluminum slag for sale. Adjusting the pH of the filtrate to 5.0 with sodium carbonate solution, aging for 0.5h, filtering to obtain purified liquid and aluminum slag, allowing the purified liquid to flow into the next process, and removing iron from the aluminum slag in the previous step to obtain iron-aluminum slag. Through detection, the purified solution has the iron concentration of 8mg/L and the aluminum concentration of 51mg/L, and meets the production requirement; the content of nickel in the iron-aluminum slag (dry basis) is 0.36 wt%, the content of cobalt is 0.15 wt%, and the content of manganese is 0.57 wt%, which meets the production control standard.
Example 3
Taking 500mL of the nickel, cobalt and manganese sulfate solution without copper, adjusting the pH value of the nickel, cobalt and manganese sulfate solution to 1.5 by using sodium carbonate, adding hydrogen peroxide with the mass fraction of 20% into the solution to oxidize all ferrous iron into ferric iron, and detecting whether the ferrous iron is completely oxidized by using potassium ferricyanide. Adding aluminum slag into the oxidized solution, reacting for 40min, adding calcium carbonate solution to adjust pH to 3.5, aging for 30min, filtering, allowing the filtrate to flow into a reaction kettle for removing aluminum, and washing iron and aluminum slag with water for sale. Adjusting the pH of the filtrate to 4.8 with sodium carbonate solution, aging for 50min, filtering to obtain purified liquid and aluminum slag, allowing the purified liquid to flow into the next step, and removing iron from the aluminum slag in the previous step to obtain iron-aluminum slag. Through detection, the purified solution has the iron concentration of 4mg/L and the aluminum concentration of 63mg/L, and meets the production requirement; the content of nickel in the iron-aluminum slag (dry basis) is 0.40 wt%, the content of cobalt is 0.11 wt%, and the content of manganese is 0.52 wt%, which meets the production control standard.
Example 4
Taking 500mL of the nickel, cobalt and manganese sulfate solution without copper, adjusting the pH value of the nickel, cobalt and manganese sulfate solution to 1.8 by using sodium carbonate, adding hydrogen peroxide with the mass fraction of 20% into the solution to oxidize all ferrous iron into ferric iron, and detecting whether the ferrous iron is completely oxidized by using potassium ferricyanide. Adding aluminum slag into the oxidized solution, reacting for 0.5h, adding a calcium carbonate solution to adjust the pH to 3.0, aging for 30min, filtering, allowing the filtrate to flow into an aluminum removal reaction kettle, and washing iron and aluminum slag for sale. Adjusting the pH of the filtrate to 4.5 with sodium carbonate solution, aging for 0.5h, filtering to obtain purified liquid and aluminum slag, allowing the purified liquid to flow into the next process, and removing iron from the aluminum slag in the previous step to obtain iron-aluminum slag. Through detection, the purified solution has the iron concentration of 4mg/L and the aluminum concentration of 72mg/L, and meets the production requirement; the content of nickel in the iron-aluminum slag (dry basis) is 0.32 wt%, the content of cobalt is 0.11 wt%, and the content of manganese is 0.48 wt%, which meets the production control standard.
Example 5
Taking 500mL of the nickel, cobalt and manganese sulfate solution without copper, adjusting the pH value of the nickel, cobalt and manganese sulfate solution to 2.0 by using sodium carbonate, adding hydrogen peroxide with the mass fraction of 20% into the solution to oxidize all ferrous iron into ferric iron, and detecting whether the ferrous iron is completely oxidized by using potassium ferricyanide. Adding aluminum slag into the oxidized solution, reacting for 0.5h, adding a calcium carbonate solution to adjust the pH to 3.5, aging for 30min, filtering, allowing the filtrate to flow into an aluminum removal reaction kettle, and washing iron and aluminum slag for sale. Adjusting the pH of the filtrate to 4.8 with sodium carbonate solution, aging for 45min, filtering to obtain purified liquid and aluminum slag, allowing the purified liquid to flow into the next step, and removing iron from the aluminum slag in the previous step to obtain iron-aluminum slag. Through detection, the purified solution has the iron concentration of 9mg/L and the aluminum concentration of 59mg/L, and meets the production requirements; the content of nickel in the iron-aluminum slag (dry basis) is 0.45 wt%, the content of cobalt is 0.21 wt%, and the content of manganese is 0.65 wt%, which meets the production control standard.
Example 6
Taking 500mL of the nickel, cobalt and manganese sulfate solution without copper, adjusting the pH value of the nickel, cobalt and manganese sulfate solution to 2.0 by using sodium carbonate, adding hydrogen peroxide with the mass fraction of 20% into the solution to oxidize all ferrous iron into ferric iron, and detecting whether the ferrous iron is completely oxidized by using potassium ferricyanide. Adding aluminum slag into the oxidized solution, reacting for 45min, adding a calcium carbonate solution to adjust the pH to 3.0, aging for 30min, filtering, allowing the filtrate to flow into an aluminum-removing reaction kettle, and washing iron and aluminum slag for sale. Adjusting the pH of the filtrate to 4.6 with sodium carbonate solution, aging for 1h, filtering to obtain purified liquid and aluminum slag, allowing the purified liquid to flow into the next step, and removing iron from the aluminum slag in the previous step to obtain iron-aluminum slag. Through detection, the purified solution has the iron concentration of 6mg/L and the aluminum concentration of 76mg/L, and meets the production requirement; the content of nickel in the iron-aluminum slag (dry basis) is 0.43 wt%, the content of cobalt is 0.16 wt%, and the content of manganese is 0.71 wt%, which meets the production control standard.
The method takes nickel-cobalt-manganese sulfate solution generated in the process of recovering valuable metals in waste lithium ion batteries as a raw material, and completely removes iron and aluminum in the nickel-cobalt-manganese sulfate solution after copper removal by a two-step iron and aluminum removal method. The method has simple process and simple and convenient operation, generates less iron-aluminum slag, and has less content of valuable metals such as nickel, cobalt, manganese and the like mixed in the slag, thereby not only realizing the removal of iron and aluminum in the solution, but also realizing the reduction of the slag and having better environmental benefit and economic benefit.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A method for removing iron and aluminum from leachate generated during the recovery of valuable metals in waste lithium ion batteries is characterized by comprising the following steps of:
(1) adjusting the pH value of the leachate to 1.5-2.0, and adding an oxidant to oxidize ferrous iron into ferric iron;
(2) adjusting the pH value of the system to 2.5-3.5, aging, and filtering to obtain a filtrate and iron-aluminum slag;
(3) adjusting the pH value of the system to 4.5-5.0, aging and filtering to obtain a purified liquid and aluminum slag;
the aluminum slag obtained in the step (3) is used as a regulator for regulating the pH value of the system in the step (2);
adjusting the pH value in the steps (1) to (3) by adopting alkali or acid;
the alkali is at least one of sodium carbonate, sodium hydroxide, calcium carbonate, calcium hydroxide and calcium oxide.
2. The method according to claim 1, wherein the iron and aluminum are removed from the leachate generated during the recovery of valuable metals from the spent lithium ion batteries, the method comprising the steps of: and (3) adding the aluminum slag into the system in the step (2) to react for more than 0.5h, and then continuously adjusting the pH value of the system.
3. The method according to claim 1, wherein the iron and aluminum are removed from the leachate generated during the recovery of valuable metals from the spent lithium ion batteries, the method comprising the steps of: the leaching solution in the step (1) is a nickel-cobalt-manganese sulfate solution generated when valuable metals in the waste lithium ion batteries are recycled.
4. The method according to claim 1, wherein the iron and aluminum are removed from the leachate generated during the recovery of valuable metals from the spent lithium ion batteries, the method comprising the steps of: the oxidant in the step (1) is at least one of hydrogen peroxide, sodium chlorate and potassium permanganate.
5. The method according to claim 1, wherein the iron and aluminum are removed from the leachate generated during the recovery of valuable metals from the spent lithium ion batteries, the method comprising the steps of: the aging time in the step (2) and the step (3) is respectively more than 0.5 h.
6. The method according to claim 1, wherein the iron and aluminum are removed from the leachate generated during the recovery of valuable metals from the spent lithium ion batteries, the method comprising the steps of: the aging time in the step (2) and the step (3) is 0.5-1 h respectively.
7. The method according to claim 1, wherein the step of removing iron and aluminum from the leachate generated during the recovery of valuable metals from the spent lithium ion batteries comprises the steps of:
(1) adjusting the pH value of the leachate to 1.5-2.0, and adding an oxidant to oxidize ferrous iron into ferric iron;
(2) adjusting the pH value of the system to 2.5-3.5, aging, and filtering to obtain a filtrate and iron-aluminum slag;
(3) adjusting the pH value of the system to 4.5-5.0, aging and filtering to obtain a purified liquid and aluminum slag;
(4) adding the aluminum slag obtained in the step (3) as a pH regulator into the system pH regulated in the step (2) to remove iron, thereby obtaining iron-aluminum slag;
(5) and circulating the steps to realize the continuous iron and aluminum removal of the leachate.
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| CN109439907A (en) * | 2018-11-22 | 2019-03-08 | 湖南邦普循环科技有限公司 | A method of iron aluminium is removed from the pickle liquor during recycling used Li ion cell |
| CN109574091A (en) * | 2018-11-23 | 2019-04-05 | 湖南中伟新能源科技有限公司 | The method of ternary precursor sulfate liquor purification iron |
| CN111020194B (en) * | 2019-11-16 | 2023-10-13 | 银隆新能源股份有限公司 | Method for synthesizing titanium-aluminum alloy from waste lithium titanate anode and cathode powder |
| CN111471864B (en) * | 2020-04-24 | 2022-02-18 | 广东邦普循环科技有限公司 | Method for recovering copper, aluminum and iron from waste lithium ion battery leachate |
| WO2022045973A1 (en) * | 2020-08-24 | 2022-03-03 | Green Li-Ion Pte. Ltd. | Process for removing impurities in the recycling of lithium-ion batteries |
| CN112126783B (en) * | 2020-08-25 | 2022-06-14 | 湖南邦普循环科技有限公司 | Recycling method of iron and aluminum in nickel-cobalt-manganese solution |
| KR20240017988A (en) | 2022-04-18 | 2024-02-08 | 그린 라이온 피티이. 리미티드 | Method and system for recovering lithium from lithium ion batteries |
| CN114853078B (en) * | 2022-05-12 | 2023-09-29 | 中国科学院过程工程研究所 | Method for removing iron and aluminum from iron-aluminum-containing solution and recycling aluminum |
| CN115180661B (en) * | 2022-07-22 | 2024-02-13 | 余姚市鑫和电池材料有限公司 | Method for recovering nickel-cobalt-copper mixed sulfate from iron-aluminum waste residues |
| CN117098860A (en) * | 2023-06-30 | 2023-11-21 | 青美邦新能源材料有限公司 | Method for removing iron and aluminum in laterite nickel ore leaching solution by goethite method |
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| CN102057064B (en) * | 2008-06-06 | 2013-08-07 | 悉尼大学 | Multi-stage leaching process |
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