CN110835116A - Preparation method of lithium-rich Prussian blue type lithium ion battery positive electrode active material, product and application thereof - Google Patents
Preparation method of lithium-rich Prussian blue type lithium ion battery positive electrode active material, product and application thereof Download PDFInfo
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- CN110835116A CN110835116A CN201911082191.XA CN201911082191A CN110835116A CN 110835116 A CN110835116 A CN 110835116A CN 201911082191 A CN201911082191 A CN 201911082191A CN 110835116 A CN110835116 A CN 110835116A
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- C01—INORGANIC CHEMISTRY
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- C01C3/08—Simple or complex cyanides of metals
- C01C3/12—Simple or complex iron cyanides
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention provides a preparation method of a lithium-rich Prussian blue type lithium ion battery anode active material, a product and an application thereof. The replacement method adopts high-concentration lithium chloride solution, non-residual oxidant and reductant to carry out immersion cleaning for a plurality of times, and uses an inductively coupled plasma emission spectrometry to detect a sample, so that lithium ions are completely replaced by sodium/potassium ions. The preparation process is relatively simple and easy to operate, and the lithium-rich Prussian blue type lithium ion battery anode active material can be obtained.
Description
Technical Field
The invention relates to a preparation method of a lithium-rich Prussian blue type lithium ion battery anode active material, a product and application thereof, in particular to Li2FeIIFeII(CN)6A preparation method of a lithium ion battery anode active material, a product and application thereof.
Technical Field
The lithium ion battery is used as a new energy source and widely applied to the civil and military fields. In order to meet various requirements, such as unmanned aerial vehicles and electric vehicle batteries, high rate performance is required, and therefore, related battery materials are required to be developed. Prussian blue materials are considered to be high-rate lithium ion battery anode materials with great potential, and the discharge rate of 50C is already available in the industry.
The existing chemical raw materials can not directly obtain the Prussian blue materials capable of inserting lithium ions, the Prussian blue materials capable of inserting the lithium ions are all obtained by synthesizing Prussian blue materials capable of inserting sodium ions or potassium ions and replacing the Prussian blue materials, and the selection of a proper replacement method has important significance for the preparation of the anode materials. Compared with a lithium-poor material, the lithium-rich material has the advantages that a proper excess of lithium ions are inserted into the positive electrode, so that the specific discharge capacity is increased, the cycling stability of the material is greatly improved, and the rate capability is higher. And detecting the last replacement reaction sample by inductively coupled plasma emission spectrometry to conclude that sodium ions in the Prussian blue are completely replaced by lithium ions.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a lithium-rich Prussian blue type lithium ion battery positive electrode active material.
Yet another object of the present invention is to: provides a lithium-rich Prussian blue type lithium ion battery anode active material product obtained by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a lithium-rich Prussian blue type lithium ion battery anode active material is characterized in that sodium ferrocyanide and aqueous solution of ferricyanide are subjected to coprecipitation reaction with corresponding transition metal soluble salt solution to obtain a Prussian blue analog correspondingly embedded with sodium ions or potassium ions, then the sodium ions or potassium ions in the Prussian blue analog are replaced by lithium ions, the replacement method adopts high-concentration lithium chloride solution matched with non-residue oxidant and reducing agent to carry out immersion washing for a plurality of times, and a sample is detected by using an inductive coupling plasma emission spectrometry to ensure that the lithium ions are completely replaced by the sodium/potassium ions, and the method comprises the specific steps of:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) will contain 0.02mol Fe3+Or other transition metal (Co/Ni/Mn/Cu) soluble salt is dissolved in 200ml deionized water, is stirred by magnetic force until being completely dissolved, is placed in a sealed separating funnel and is connected with a flask;
(3) 0.02mol of sodium ferrocyanide (Na)4Fe(CN)6Or potassium ferrocyanide (K)4Fe(CN)6Dissolved inIn 200ml deionized water, magnetically stirring until the deionized water is completely dissolved, placing the mixture into a sealed separating funnel, and connecting the separating funnel with a flask;
(4) completely sealing the reaction device, rapidly stirring by magnetic force at the rotation speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, the reaction time is 8h, standing for 24h after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution, adding a proper amount of L-ascorbic acid, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) and (5) repeating the steps (5) and (6) to obtain a final product.
Wherein, in the step (7), the steps (5) and (6) are repeated three times.
The invention provides a lithium-rich Prussian blue type lithium ion battery positive electrode active material which is prepared according to any one of the methods.
The invention provides an application of a lithium-rich lithium ion battery positive electrode active material in a non-aqueous lithium ion battery.
The use of hydrogen peroxide to oxidize transition metal elements facilitates the oxidation of Na in Prussian blue materials+/K+And (4) removing.
The L-ascorbic acid is used for reducing the transition metal elements, so that the prussian blue material can be conveniently inserted into Li in a large amount of high-concentration lithium chloride solution+。
The oxidizing agent and the reducing agent are alternately used for a plurality of times, so that the effect of replacing lithium ions is achieved.
And finally, using a reducing agent for the last time, so that the final product can be inserted with more lithium ions and is a lithium-rich cathode material.
The invention has the advantages that: according to the method, the Prussian blue material containing sodium ions (or potassium ions) is immersed into the solution containing high-concentration lithium ions, the active replacement mode is improved into the mode of alternately performing oxidation-reduction reactions for a plurality of times, the ion replacement is driven passively, the ion replacement efficiency and the ion replacement speed are greatly improved, and therefore the lithium-rich lithium ion battery positive electrode active material is obtained. The preparation process is relatively simple and easy to operate, and the lithium-rich Prussian blue type lithium ion battery anode active material can be obtained.
Drawings
FIG. 1 shows Li in example 12FeIIFeII(CN)6SEM image of material.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A lithium-rich Prussian blue type lithium ion battery positive electrode active material is prepared by carrying out coprecipitation reaction on aqueous solutions of sodium ferrocyanide and corresponding transition metal soluble salt solutions to obtain Prussian blue analogs correspondingly embedded with sodium ions or potassium ions, then replacing the sodium ions or the potassium ions in the Prussian blue analogs with lithium ions, carrying out immersion washing for a plurality of times by adopting a high-concentration lithium chloride solution in cooperation with a non-residue oxidant and a reducing agent to enable the lithium ions to be completely replaced with the sodium/potassium ions, and carrying out preparation according to the following steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) 0.02mol FeCl3Completely dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(3) 0.02mol of sodium ferrocyanide (Na)4Fe(CN)6Or potassium ferrocyanide (K)4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(4) completely sealing the reaction device, stirring by using a magnetic force at a high speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, dripping the mixture into a flask, fully reacting for 8 hours, standing for 24 hours after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide oxidation product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution by using L-ascorbic acid again to reduce the product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) repeating the steps (5) and (6) for 3 times, and drying in an oven at 80 ℃ to obtain a final product, wherein the product is shown in figure 1.
Example 2
A lithium-rich Prussian blue type lithium ion battery positive electrode active material is prepared by the following steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) 0.02mol of CoSO4Completely dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(3) 0.02mol of Na4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(4) completely sealing the reaction device, rapidly stirring by magnetic force at the rotation speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, dripping the mixture into a flask, fully reacting for 8 hours, standing and precipitating for 24 hours after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide oxidation product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution, adding a proper amount of L-ascorbic acid reduction product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) repeating the steps (5) and (6) for three times, and drying in an oven at the temperature of 80 ℃ to obtain a final product.
Example 3
A lithium-rich Prussian blue type lithium ion battery positive electrode active material is prepared by the following steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) 0.02mol of FeSO4Completely dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(3) 0.02mol of K4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(4) completely sealing the reaction device, rapidly stirring by magnetic force at the rotation speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, dripping the mixture into a flask, fully reacting for 8 hours, standing and precipitating for 24 hours after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide oxidation product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution, adding a proper amount of L-ascorbic acid reduction product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) and (4) repeating the steps (5) and (6) for 3 times, and drying in an oven at the temperature of 80 ℃ to obtain a final product.
Claims (7)
1. A preparation method of a lithium-rich Prussian blue type lithium ion battery anode active material is characterized in that sodium ferrocyanide and aqueous solution of ferrocyanide are subjected to coprecipitation reaction with corresponding transition metal soluble salt solution to obtain a Prussian blue analog correspondingly embedded with sodium ions or potassium ions, then the sodium ions or potassium ions in the Prussian blue analog are replaced by lithium ions, and the replacement method adopts high-concentration lithium chloride solution matched with a non-residual oxidant and a reducing agent to carry out immersion washing for a plurality of times so that the lithium ions are completely replaced by the sodium/potassium ions, and comprises the following steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) will contain 0.02mol Fe3+Or other transition metal (Co/Ni/Mn/Cu) soluble salt is dissolved in 200ml deionized water, is stirred by magnetic force until being completely dissolved, is placed in a sealed separating funnel and is connected with a flask;
(3) 0.02mol of sodium ferrocyanide (Na)4Fe(CN)6Or potassium ferrocyanide (K)4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring to dissolve completely, placing in sealed separating funnel, and connecting with flaskConnecting;
(4) completely sealing the reaction device, rapidly stirring by magnetic force at the rotation speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, the reaction time is 8h, standing for 24h after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution, adding a proper amount of L-ascorbic acid, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) and (5) repeating the steps (5) and (6) to obtain a final product.
2. The method for preparing the lithium-rich prussian blue-based lithium ion battery positive active material according to claim 1, wherein steps (5) and (6) are repeated three times in step (7).
3. The preparation method of the lithium-rich prussian blue type lithium ion battery positive electrode active material according to claim 1 or 2, which is characterized by comprising the following specific steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) 0.02mol FeCl3Completely dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(3) 0.02mol of sodium ferrocyanide (Na)4Fe(CN)6Or potassium ferrocyanide (K)4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(4) completely sealing the reaction device, stirring by using a magnetic force at a high speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, dripping the mixture into a flask, fully reacting for 8 hours, standing for 24 hours after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide oxidation product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution by using L-ascorbic acid again to reduce the product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) repeating the steps (5) and (6) for 3 times, and drying in an oven at 80 ℃ to obtain the final product.
4. The preparation method of the lithium-rich prussian blue type lithium ion battery positive electrode active material according to claim 1 or 2, characterized by comprising the following steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) 0.02mol of CoSO4Completely dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(3) 0.02mol of Na4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(4) completely sealing the reaction device, rapidly stirring by magnetic force at the rotation speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, dripping the mixture into a flask, fully reacting for 8 hours, standing and precipitating for 24 hours after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide oxidation product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution, adding a proper amount of L-ascorbic acid reduction product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) repeating the steps (5) and (6) for three times, and drying in an oven at the temperature of 80 ℃ to obtain a final product.
5. The preparation method of the lithium-rich prussian blue type lithium ion battery positive electrode active material according to claim 1 or 2, characterized by comprising the following steps:
(1) 500ml of hydrochloric acid with pH =1 is taken and filled into a flask;
(2) 0.02mol of FeSO4Completely dissolved in 200ml deionized water, and magnetically stirred until the solution is completely dissolvedDissolving, placing in a sealed separating funnel, and connecting with a flask;
(3) 0.02mol of K4Fe(CN)6Dissolving in 200ml deionized water, magnetically stirring until completely dissolving, placing in a sealed separating funnel, and connecting with a flask;
(4) completely sealing the reaction device, rapidly stirring by magnetic force at the rotation speed of 800r/min, controlling the flow rates of the two separating funnels to be consistent, wherein the flow rates are both 1ml/min, dripping the mixture into a flask, fully reacting for 8 hours, standing and precipitating for 24 hours after the reaction is finished, and centrifugally cleaning for 3-4 times;
(5) putting the product obtained in the step (4) into deionized water, adding a proper amount of hydrogen peroxide oxidation product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(6) putting the product obtained in the step (5) into a large amount of 1mol/L lithium chloride solution, adding a proper amount of L-ascorbic acid reduction product, quickly stirring for 0.5h, precipitating, and centrifugally cleaning;
(7) and (4) repeating the steps (5) and (6) for 3 times, and drying in an oven at the temperature of 80 ℃ to obtain a final product.
6. A lithium-rich prussian blue-based positive electrode active material for lithium ion batteries, which is prepared by the method according to any one of claims 1 to 5.
7. Use of the positive electrode active material for a lithium-rich lithium ion battery according to claim 6 in a non-aqueous lithium ion battery.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551550A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cobalt hexacyanoferrate lithium ion battery positive electrode active material, product and application thereof |
| CN112645354A (en) * | 2020-12-21 | 2021-04-13 | 电子科技大学 | Surface-modified sodium-manganese-iron-based Prussian blue material and preparation method and application thereof |
| CN114447290A (en) * | 2021-12-21 | 2022-05-06 | 西安理工大学 | Modification method and application of lithium-rich manganese-based positive electrode material of lithium ion battery |
-
2019
- 2019-11-07 CN CN201911082191.XA patent/CN110835116A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 陈寿椿主编: "《重要无机化学反应》", 31 December 1982, 上海科学技术出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551550A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cobalt hexacyanoferrate lithium ion battery positive electrode active material, product and application thereof |
| CN112645354A (en) * | 2020-12-21 | 2021-04-13 | 电子科技大学 | Surface-modified sodium-manganese-iron-based Prussian blue material and preparation method and application thereof |
| CN114447290A (en) * | 2021-12-21 | 2022-05-06 | 西安理工大学 | Modification method and application of lithium-rich manganese-based positive electrode material of lithium ion battery |
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