CN106450547B - Method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste - Google Patents
Method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste Download PDFInfo
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Abstract
The invention discloses a method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste, which specifically comprises the following steps: step one, oxidizing roasting; step two, polarizingCleaning the slices; adding phosphoric acid for ball milling activation; step four, acid washing and separating FePO4(ii) a Step five, precipitating lithium from the filtrate to obtain a target substance Li2CO3. The method has the advantages that the P, Fe and Li resources in the lithium iron phosphate waste can be fully utilized to prepare the iron phosphate and lithium carbonate products with high added values, no Fe waste residue is generated, the resource recovery rate is high, the process flow is short, the reaction system is simple, the raw material consumption is low, the cost is low, the product value is high, and the method is very suitable for industrial mass production.
Description
Technical Field
The invention belongs to the technical field of battery waste resource recycling, and relates to a method for recycling iron phosphate and lithium carbonate from lithium iron phosphate waste.
Background
In recent years, with the rapid development of the new energy automobile industry, the yield of the lithium ion power battery is increased explosively. The lithium iron phosphate lithium ion power battery has excellent safety, stability and cyclicity, is low in price and free of pollution, and is popular in industries such as electric automobiles and energy storage power stations. Along with the wide application of lithium iron phosphate power batteries, a large number of lithium iron phosphate batteries are gradually scrapped, and particularly, the price of lithium salt rises in two years, so that how to recycle the scrapped lithium ion batteries becomes a problem of general social attention.
At present, two main types of recovery methods for waste lithium iron phosphate batteries are available, one is to recover precious metals, and the other is to regenerate lithium iron phosphate positive electrode materials by a solid phase method. For example, chinese patent publication No. CN 102208707 a (application 2011-05-12) discloses a method for repairing and regenerating a waste lithium iron phosphate battery positive electrode material, which includes the steps of firstly generating lithium iron phosphate by hydrothermal reaction of a lithium source solution and recovered waste lithium iron phosphate, or performing ball milling and calcining on the recovered waste lithium iron phosphate battery material and a lithium source solid phase to perform liquid phase or solid phase direct lithium supplement repair on the waste lithium iron phosphate in a lithium-deficient state, and then performing repair and regeneration on the lithium iron phosphate positive electrode material in a targeted manner by coating a conductive agent or coating the conductive agent and doping metal ions. For example, chinese patent publication No. CN 104362408A (2014-10-28) discloses a method for recycling lithium iron phosphate waste in a lithium iron phosphate battery manufacturing process, in which a pole piece to be recycled is baked at a high temperature to decompose and disable an adhesive, lithium iron phosphate and a conductive agent are separated from a current collector aluminum foil, then the lithium iron phosphate and the conductive agent are baked at a high temperature and screened to separate lithium iron phosphate powder, and then the lithium iron phosphate powder is repaired and regenerated again to obtain a lithium iron phosphate positive electrode material. Due to the limitation of waste material sources and preparation processes, the repaired and regenerated lithium iron phosphate cathode material is easily polluted by external impurities, has low purity and poor electrical property stability, and cannot meet the quality requirements of the current market on battery materials. For example, chinese patent publication No. CN 102903985A (2012-10-22) discloses a method for recovering lithium carbonate from lithium iron phosphate waste, in which lithium iron phosphate is roasted and dissolved in sulfuric acid to obtain a mixed solution of lithium phosphate, iron phosphate and iron sulfate, then pH is adjusted and iron phosphate and iron sulfate are separated to obtain lithium carbonate, and the lithium carbonate is subjected to dissolving, impurity removal, re-synthesis and other methods. For example, chinese patent publication No. (2013-03-29) CN 103280610 a discloses a method for recovering waste pieces of positive electrodes of lithium iron phosphate batteries, which comprises dissolving the positive electrode of the lithium iron phosphate battery with alkali, filtering, dissolving filter residues with mixed acid solution, so that iron exists in the form of iron phosphate precipitate and is separated from impurities such as carbon black and the like from lithium-containing solution, and adding 95 ℃ saturated sodium carbonate solution into the lithium-containing solution to precipitate to obtain lithium carbonate. In the recovery methods, the high-efficiency and high-value-added resource recovery of the lithium iron phosphate waste is not well realized, and the recovery methods have the advantages of complex process steps, multiple flow steps, high reagent consumption, high cost and low economic cost.
Disclosure of Invention
The invention mainly aims to provide a method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste, which can solve the problems of complex process steps, more flow steps, high reagent consumption, high cost and low recovery rate in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows: a method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste materials is realized by the following steps:
step one, oxidizing roasting: placing the waste lithium iron phosphate positive plate into a roasting furnace, heating to 400-500 ℃, and roasting for 3-4 hours to obtain a positive plate roasting material containing a lithium iron phosphate active substance and a current collector aluminum foil;
step two, pole piece cleaning: cooling the anode plate baked in the first step to 25 ℃, then putting the anode plate into an ultrasonic cleaning tank, ultrasonically cleaning the anode plate, then taking out an aluminum foil for recycling, filtering lithium iron phosphate active substances in the cleaning solution for later use, and circularly using the filtrate as the cleaning solution of the next batch;
adding phosphoric acid for ball milling activation: adding concentrated phosphoric acid into the lithium iron phosphate active substance obtained by filtering in the step two, uniformly stirring, placing the mixture into a ball milling tank for sealing, placing the ball milling tank on a ball mill for ball milling, and then carrying out ball material separation to obtain FePO4With Li3Fe2(PO4)3A mixture of (a);
step four, acid washing and separating FePO4: FePO obtained in step three4With Li3Fe2(PO4)3Adding dilute sulfuric acid solution into the mixture, stirring and washing at normal temperature, and filtering to separate FePO4And a filtrate;
step five, precipitating lithium from the filtrate: heating the filtrate obtained in the step four to 80-95 ℃, and adding anhydrous Na2CO3Adjusting the pH value to 10-11 for reaction, filtering, washing and drying to obtain Li2CO3。
Preferably, in the second step, the time for ultrasonic cleaning is 30-60 min.
Preferably, in the third step, the solid-to-liquid ratio of the lithium iron phosphate active material to the concentrated phosphoric acid is 5: 1-6: 1, and the mass fraction of the concentrated phosphoric acid is 85-95%.
Preferably, in the third step, the rotating speed of the ball mill is 500-600 r/min, and the ball milling time is 30-60 min.
Preferably, in the third step, the separation of the ball materials is carried out by adopting a vibrating mesh screen.
Preferably, in step four, FePO4With Li3Fe2(PO4)3The solid-liquid ratio of the mixture to the dilute sulfuric acid solution is 1: 2-1: 3, and the concentration of the dilute sulfuric acid solution is 1.5-2.5 mol/L.
Preferably, in the fourth step, the stirring speed is 200-300 r/min, and the stirring time is 30-60 min.
Preferably, in the fifth step, the reaction time is 60min to 120 min.
Preferably, in the fifth step, water with the temperature of 90-100 ℃ is selected during washing.
Compared with the prior art, the invention has the beneficial effects that:
1) the method has strong adaptability to reaction materials, and the waste lithium iron phosphate pole pieces, leftover materials and waste lithium iron phosphate materials can be used as reaction raw materials of the method;
2) according to the invention, the iron phosphate and lithium carbonate products with high added values can be prepared by fully utilizing P, Fe and Li resources in the lithium iron phosphate waste, no Fe waste residue is generated, and the resource recovery rate is high;
3) the invention has the advantages of low reagent consumption, simple process, full utilization of Fe, P and Li resources, no waste slag generation and high added value FePO product4And Li2CO3。
4) The invention has short process flow, simple projection system, less raw material consumption, low cost and high product value, and is very suitable for industrial scale production.
Drawings
Fig. 1 is a flow chart of a method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the following description is only used for explaining the present invention with reference to the accompanying drawings and the embodiments, and is not intended to limit the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Example 1:
step one, oxidizing roasting: putting the tray filled with 1kg of waste lithium iron phosphate positive plates into a roasting furnace, heating to 450 ℃, roasting for 3.5 hours to disable the binder PTFE, volatilizing the conductive agent carbon black, and taking out the tray to obtain the positive plate roasting material containing the lithium iron phosphate active substance and the current collecting aluminum foil, wherein the reaction principle is as follows: 6LiFePO4+3/2O2＝2Li3Fe2(PO4)3+Fe2O3；
Step two, pole piece cleaning: cooling the anode plate roasted in the first step to 25 ℃, putting the anode plate into an ultrasonic cleaning tank, ultrasonically cleaning the anode plate for 30min, taking out the aluminum foil for recycling (at the moment, the anode material on the aluminum foil completely falls off), filtering the lithium iron phosphate active substance in the cleaning solution for later use, and circularly using the filtrate as the cleaning solution of the next batch;
adding phosphoric acid into the positive electrode material, and carrying out ball milling activation: adding 85ml of concentrated phosphoric acid with the mass fraction of 85% into 500g of the lithium iron phosphate active material obtained by filtering in the step two, uniformly stirring, placing the mixture into a ball milling tank for sealing, placing the ball milling tank on a ball mill for ball milling, placing the ball milling tank on the ball mill for ball milling for 30min at the rotating speed of 500r/min, stopping ball milling, and then separating balls by using a vibrating mesh screen to obtain FePO4With Li3Fe2(PO4)3Wherein the reaction principle is as follows: fe2O3+2H3PO4＝2FePO4+3H2O；
Step four, acid washing and separating FePO4: FePO obtained in step three4With Li3Fe2(PO4)3Adding 1L of 2mol/L dilute sulfuric acid solution into the mixture, stirring and washing at normal temperature at the stirring speed of 200r/min for 60min, and filtering to separate FePO4And a filtrate; the reaction principle is as follows: 2Li3Fe2(PO4)3+3H2SO4＝3Li2SO4+2H3PO4+4FePO4；
Step five, precipitating lithium from the filtrate: heating the filtrate obtained in the fourth step to 85 ℃, and adding 170g of anhydrous Na2CO3Adjusting pH to 10, reacting for 120min, filtering to obtain white precipitate, washing with 95 deg.C hot water for three times, and drying to obtain Li2CO372.1g of solid, the reaction principle being: li2SO4+Na2CO3＝Na2SO4+Li2CO3。
Example 2:
step one, oxidizing roasting: placing the tray filled with 1kg of waste lithium iron phosphate positive plates into a roasting furnace, heating to 400 ℃, roasting for 3.5 hours to disable the binder PTFE, volatilizing the conductive agent carbon black, and taking out the tray to obtain a positive plate roasting material containing lithium iron phosphate active substances and a current collector aluminum foil;
step two, pole piece cleaning: cooling the anode plate roasted in the first step to 25 ℃, putting the anode plate into an ultrasonic cleaning tank, ultrasonically cleaning the anode plate for 30min, taking out the aluminum foil for recycling (at the moment, the anode material on the aluminum foil completely falls off), filtering the lithium iron phosphate active substance in the cleaning solution for later use, and circularly using the filtrate as the cleaning solution of the next batch;
adding phosphoric acid into the positive electrode material, and carrying out ball milling activation: adding 55ml of concentrated phosphoric acid with the mass fraction of 85% into 300g of the lithium iron phosphate active material obtained by filtering in the step two, uniformly stirring, sealing a ball milling tank, putting the ball milling tank on a ball mill for ball milling, putting the ball milling tank on the ball mill for ball milling for 50min at the rotating speed of 600r/min, stopping ball milling, and then separating balls by using a vibrating mesh screen to obtain FePO4With Li3Fe2(PO4)3A mixture of (a);
step four, acid washing and separating FePO4: FePO obtained in step three4With Li3Fe2(PO4)3Adding 600ml of 2mol/L dilute sulfuric acid solution into the mixture, stirring and washing at normal temperature at the stirring speed of 200r/min for 60min, and filtering to separate FePO4And a filtrate;
step five, precipitating lithium from the filtrate: heating the filtrate obtained in the fourth step to 95 ℃, and adding 100g of anhydrous Na2CO3Adjusting pH to 10, reacting for 80min, filtering to obtain white precipitate, washing with 95 deg.C hot water for three times, and drying to obtain Li2CO344.7g of solid.
Example 3:
step one, oxidizing roasting: placing the tray filled with 1kg of waste lithium iron phosphate positive plate into a roasting furnace, heating to 500 ℃, roasting for 4 hours to ensure that the binder PTFE is ineffective, the conductive agent carbon black is volatilized, and taking out the tray to obtain a positive plate roasting material containing lithium iron phosphate active substances and a current collector aluminum foil;
step two, pole piece cleaning: cooling the anode plate roasted in the first step to 25 ℃, then putting the anode plate into an ultrasonic cleaning tank, ultrasonically cleaning for 60min, then taking out the aluminum foil for recycling (at the moment, the anode material on the aluminum foil completely falls off), filtering the lithium iron phosphate active substance in the cleaning solution for later use, and circularly taking the filtrate as the cleaning solution of the next batch;
adding phosphoric acid into the positive electrode material, and carrying out ball milling activation: adding 85ml of concentrated phosphoric acid with the mass fraction of 85% into 500g of the lithium iron phosphate active material obtained by filtering in the step two, uniformly stirring in a container, sealing a ball milling tank, then placing the ball milling tank on a ball mill for ball milling, placing the ball milling tank on the ball mill for ball milling at the rotating speed of 500r/min for 60min, stopping ball milling, and then separating the ball material by using a vibrating mesh screen to obtain FePO4With Li3Fe2(PO4)3A mixture of (a);
step four, acid washing and separating FePO4: FePO obtained in step three4With Li3Fe2(PO4)3Adding 600ml of 2mol/L dilute sulfuric acid solution into the mixture, stirring and washing at normal temperature at the stirring speed of 300r/min for 30min, and filtering to separate FePO4And a filtrate;
step five, precipitating lithium from the filtrate: heating the filtrate obtained in the fourth step to 95 ℃, and adding 160g of anhydrous Na2CO3Adjusting pH to 11, reacting for 60min, filtering to obtain white precipitate, washing with 95 deg.C hot water for three times, and oven drying to obtain Li2CO368.7g of solid.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste is characterized by comprising the following steps:
step one, oxidizing roasting: placing the waste lithium iron phosphate positive plate into a roasting furnace, heating to 400-500 ℃, and roasting for 3-4 hours to obtain a positive plate roasting material containing a lithium iron phosphate active substance and a current collector aluminum foil;
step two, pole piece cleaning: cooling the anode plate baked in the first step to 25 ℃, then putting the anode plate into an ultrasonic cleaning tank, ultrasonically cleaning the anode plate, then taking out an aluminum foil for recycling, filtering lithium iron phosphate active substances in the cleaning solution for later use, and circularly using the filtrate as the cleaning solution of the next batch;
adding phosphoric acid for ball milling activation: adding 85-95% by mass of concentrated phosphoric acid into the lithium iron phosphate active substance obtained by filtering in the second step, uniformly stirring, placing the mixture into a ball milling tank for sealing, placing the ball milling tank on a ball mill, carrying out ball milling for 30-60 min at the rotating speed of the ball mill of 500-600 r/min, and then carrying out ball material separation to obtain FePO4With Li3Fe2(PO4)3A mixture of (a); wherein the solid-to-liquid ratio of the lithium iron phosphate active material to the concentrated phosphoric acid is 5: 1-6: 1;
step four, acid washing and separating FePO4: FePO obtained in step three4With Li3Fe2(PO4)3Adding dilute sulfuric acid solution into the mixture, stirring and washing at normal temperature, and filtering to separate FePO4And a filtrate; wherein, FePO4With Li3Fe2(PO4)3The solid-liquid ratio of the mixture to the dilute sulfuric acid solution is 1: 2-1: 3;
step five, precipitating lithium from the filtrate: heating the filtrate obtained in the step four to 80-95 ℃, and adding anhydrous Na2CO3Adjusting the pH value to 10-11 for reaction, filtering, washing and drying to obtain Li2CO3。
2. The method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste according to claim 1, wherein in the second step, the ultrasonic cleaning time is 30-60 min.
3. The method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste material according to claim 1, wherein in the third step, the separation of the pellets is performed by using a vibrating mesh screen.
4. The method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste according to claim 1, wherein in the fourth step, the concentration of the dilute sulfuric acid solution is 1.5-2.5 mol/L.
5. The method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste according to claim 1, wherein in the fourth step, the stirring speed is 200-300 r/min, and the stirring time is 30-60 min.
6. The method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste material according to claim 1, wherein in the fifth step, the reaction time is 60-120 min.
7. The method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste according to claim 1, wherein in the fifth step, water with a temperature of 90-100 ℃ is selected for washing.
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| CN111370800B (en) * | 2020-03-03 | 2021-10-22 | 湖南雅城新材料有限公司 | Method for recovering waste lithium iron phosphate anode material |
| CN111653846B (en) * | 2020-07-27 | 2021-10-29 | 中南大学 | Treatment method of waste lithium iron phosphate battery |
| CN112142077B (en) * | 2020-09-08 | 2021-10-29 | 北京科技大学 | Method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste |
| CN112340717A (en) * | 2020-10-26 | 2021-02-09 | 荆门市格林美新材料有限公司 | Comprehensive recovery method of lithium iron phosphate |
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