CN114408888B - Method for preparing battery grade ferric phosphate powder by using aluminum-containing waste acid liquid - Google Patents
Method for preparing battery grade ferric phosphate powder by using aluminum-containing waste acid liquid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for preparing battery-grade ferric phosphate powder by utilizing aluminum-containing waste acid liquid, which belongs to a resource utilization method of the aluminum-containing waste acid liquid.
Description
Technical Field
The invention belongs to a resource utilization method of aluminum-containing waste acid liquid, and particularly relates to a method for preparing battery-grade ferric phosphate powder by utilizing the aluminum-containing waste acid liquid.
Background
Aluminum is currently nonferrous metal with the largest yield and the widest application in the world, and aluminum and products thereof are widely applied to industries of building, aerospace, transportation, mechanical equipment, electronic equipment, packaging materials, electric power, daily necessities and the like. The Guangdong province in China is the great province of aluminum alloy processing, and the aluminum alloy yield in 2011 is about 500 ten thousand tons. Among them, the building aluminum alloy is an advantageous product in Guangdong province, the yield is about 50% of the whole country, the market share exceeds 45%, and the industrial scale is first in China. The key process of the aluminum alloy production and processing is aluminum surface treatment, and the aluminum alloy can be improved in corrosion resistance, prolonged in service life and enhanced in decoration through the surface treatment. Currently, the main process of surface treatment of aluminum alloy is anodic oxidation, the aluminum alloy subjected to anodic oxidation treatment accounts for about 45% of the total yield of aluminum alloy in buildings every year, in the anodic oxidation solution of an oxidation tank, the aluminum alloy with a conductive surface is placed on an anode, the process of forming an oxidation film on the surface is called anodic oxidation under the action of external current, and the generated film is an anodic oxidation film or an electrochemical oxidation film, and the electrochemical oxidation film is different from a natural oxidation film. The oxide film is in a stacked cell structure, each cell is a hexagonal cylinder, and the top end of the oxide film is an arc-shaped fine pore section with a hexagonal star shape. The oxide film has two layers, a compact thin layer is close to the base metal, and the thickness of pure AL is 0.01-0.05um 2 O 3 The film has high hardness, and the layer is a barrier layer; the outer layer is a porous oxide film layer, which is made of AL with crystal water 2 O 3 The composition and the hardness are lower. In the anodic oxidation process of aluminum alloy, chemical polishing or electrochemical polishing treatment procedures are indispensable, at present, the aluminum surface polishing mainly adopts a phosphoric acid and sulfuric acid mixed acid system, when the concentration of aluminum ions in polishing solution is increased to 20-30g/L, the polishing performance is reduced, bath solution is required to be replaced, the demand of aluminum surface treatment industry in Guangdong area only for phosphoric acid is thousands of tons according to statistics, and finally, the phosphoric acid is converted into phosphorus-containing sludge to be further treated in dangerous waste units, so that precious phosphorus resources can not be fully utilized.
Ferric phosphate is also called ferric phosphate and ferric orthophosphate, and the molecular formula is FePO 4 The powder is white and off-white monoclinic crystal powder, is a salt of ferric salt solution and sodium phosphate, wherein iron is trivalent and insoluble in water. The main application is to manufacture lithium iron phosphate battery materials, catalysts, ceramics and the like. The existing iron phosphate production process mainly comprises the steps of synthesizing iron phosphate by ferrous salt and phosphate under the oxidation of an oxidant, taking phosphoric acid, sodium dihydrogen phosphate, disodium hydrogen phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate and the like as phosphorus sources, and synthesizing the iron phosphate with the aid of additives, wherein the additives are indispensable in the process, and are beneficial to the formation of the iron phosphate.
Chinese patent 200810026602.9 discloses a high-density spherical ferric phosphate and a preparation method thereof, which are mainly used for preparing lithium iron phosphate as a positive electrode material of a lithium ion battery. The method takes an iron source and an additive as raw materials, and prepares a mixed solution A by dissolving with deionized water; phosphate and neutralizer are used as raw materials, and deionized water is used for dissolving to prepare a mixed solution B. Mixing the solution A and the solution B for reaction, and washing and drying the prepared material to obtain the product with average grain diameter of 1.5-5 μm and tap density of more than or equal to 0.95g/cm 3 High-density spherical ferric phosphate with uniform particle dispersion and size. The lithium iron phosphate prepared by using the high-density spherical ferric phosphate has more perfect crystal structure, normal lithium ion intercalation/deintercalation channel and discharge capacity of 140mAh/g under the condition of 1C. The method has simple process and is easy to realize the process, and the lithium iron phosphate synthesized by the ferric phosphate has better crystallinity and better crystal structure, and can improve the electrochemical performance of the lithium iron phosphate.However, the method requires phosphate with high price to produce ferric phosphate, has high production cost, and is not beneficial to popularization of the lithium iron phosphate battery in the energy storage fields of wind power, solar power generation and the like.
Disclosure of Invention
In order to overcome the problems described above, the present invention provides a method for preparing battery grade iron phosphate powder using an aluminum-containing waste acid solution, comprising the steps of:
step one, separating aluminum ions in aluminum-containing waste acid liquid (such as chemical polishing liquid and electrolytic polishing liquid): adding the aluminum-containing waste acid liquid into a reaction kettle, starting stirring, slowly adding alkali liquor to adjust the pH value of the aluminum-containing waste acid liquid to 4-5 to obtain a solid-liquid mixture, and obtaining aluminum hydroxide and first phosphorus-containing waste liquid from the solid-liquid mixture;
step two, purifying the first phosphorus-containing waste liquid: adding 27.5wt% of hydrogen peroxide into the first phosphorus-containing waste liquid obtained in the step one, heating to 60-80 ℃ and stirring for reaction for 1-2h, adding active carbon and stirring for reaction for 0.5-2h, standing for 4-8h, and filtering to remove filter residues to obtain a second phosphorus-containing waste liquid;
step three, deeply purifying the second phosphorus-containing waste liquid: removing impurities from the second phosphorus-containing waste liquid obtained in the step two through ion exchange resin to obtain third phosphorus-containing waste liquid;
step four, synthesizing iron phosphate: adding sulfuric acid solution and a small amount of ferric phosphate powder into a reaction kettle, starting stirring, adding ferrous sulfate solution at a speed of 5-10L/min and the third phosphorus-containing waste liquid obtained in the step three, adding 27.5wt% of hydrogen peroxide at a speed of 1-2L/min, stirring for reaction, simultaneously dropwise adding sulfuric acid solution to keep the pH value of the reaction solution between 1.8 and 2.0, and performing solid-liquid separation after the reaction is finished to remove filtrate to obtain crude ferric phosphate solid;
preparing battery grade ferric phosphate powder: and (3) stirring, pulping and washing the crude ferric phosphate solid obtained in the step (IV) by adopting pure water, drying the washed crude ferric phosphate solid at 60-100 ℃ after washing until the conductivity in washing water is less than 200uS/cm, and calcining at 600-900 ℃ to obtain the battery grade ferric phosphate powder, wherein the aluminum-containing waste acid liquid contains a surfactant, so that the synthesized ferric phosphate is not easy to agglomerate.
In some embodiments of the present invention, the alkaline solution in the first step of the method for preparing battery grade iron phosphate powder by using the aluminum-containing acid pickle is at least one of sodium hydroxide solution, sodium carbonate solution and ammonia water.
In some embodiments of the present invention, the hydrogen peroxide in the second step of the method for preparing battery grade iron phosphate powder by using the aluminum-containing waste acid solution is added in an amount of 1-5L/(1000L of the first phosphorus-containing waste liquid).
In some embodiments of the present invention, the amount of activated carbon added in the method for preparing battery grade iron phosphate powder using aluminum-containing waste acid solution of the present invention is 1-3 Kg/(1000L of the first phosphorus-containing waste liquid).
In some embodiments of the invention, the impurities in the method of the invention for preparing battery grade iron phosphate powder using aluminum-containing spent acid solution include nickel and copper.
In some embodiments of the present invention, the molar ratio of the molar concentration of iron ions in the ferrous sulfate solution to the phosphate content in the third phosphorus-containing waste solution in the fourth step of the method for preparing a battery grade iron phosphate powder using an aluminum-containing waste acid solution is 1 (1.1-1.4).
Compared with the prior art, the invention has the beneficial effects that:
according to the method for preparing the battery-grade ferric phosphate powder by utilizing the aluminum-containing waste acid liquid, the aluminum-containing waste acid liquid is subjected to multistage purification and impurity removal, and then is synthesized with ferrous sulfate and hydrogen peroxide, so that the quality of the ferric phosphate meets the requirement of battery-grade ferric phosphate, the recycling of phosphorus resources is realized, the production cost of the ferric phosphate is reduced, and the method has a promoting effect on the energy storage and application of the lithium battery in the fields of wind power, solar power generation and the like, and has good economic and environmental benefits.
Detailed Description
The following are several specific examples of the method for preparing battery grade iron phosphate using phosphorus resources in aluminum-containing waste acid solution according to the present invention, which are only specific descriptions of the method for preparing battery grade iron phosphate powder using aluminum-containing waste acid solution according to the present invention, and are not intended to limit the scope of the present invention.
In the following examples, the aluminum-containing waste acid liquid was obtained from chemical polishing waste acid of an aluminum anodizing enterprise, 25g/L of aluminum ions, 480g/L of phosphoric acid, 200g/L of sulfuric acid and 98wt% of concentrated sulfuric acid.
Example 1
The method for preparing the battery grade ferric phosphate powder by utilizing the aluminum-containing waste acid liquid comprises the following steps:
step one, separating aluminum ions in aluminum-containing waste acid liquid: adding the aluminum-containing waste acid liquid into a reaction kettle, starting stirring, slowly adding a sodium hydroxide solution to adjust the pH value of the aluminum-containing waste acid liquid to 4 to obtain a solid-liquid mixture, and obtaining aluminum hydroxide and first phosphorus-containing waste liquid from the solid-liquid mixture;
step two, purifying the first phosphorus-containing waste liquid: adding 27.5wt% of hydrogen peroxide into the first phosphorus-containing waste liquid obtained in the step one, heating to 80 ℃ and stirring for reaction for 1h, then adding active carbon, stirring for reaction for 1h, standing for 8h, filtering and removing filter residues to obtain a second phosphorus-containing waste liquid, wherein the adding amount of the hydrogen peroxide is 5L/(1000L of the first phosphorus-containing waste liquid), and the adding amount of the active carbon is 3 Kg/(1000L of the first phosphorus-containing waste liquid).
Step three, deeply purifying the second phosphorus-containing waste liquid: removing impurities (copper) from the second phosphorus-containing waste liquid obtained in the step two through ion exchange resin to obtain third phosphorus-containing waste liquid;
step four, synthesizing iron phosphate: adding sulfuric acid solution and a small amount of ferric phosphate powder into a reaction kettle, starting stirring, adding ferrous sulfate solution at a speed of 5L/min and the third phosphorus-containing waste liquid obtained in the third step (through detection analysis, the copper ion content is less than 2mg/L, the phosphate radical content is 3.63 mol/L), adding 27.5wt% of hydrogen peroxide at a speed of 1L/min, stirring for reaction, simultaneously dropwise adding sulfuric acid solution to keep the pH of the reaction liquid between 1.8, and performing solid-liquid separation after the reaction is finished, discarding filtrate to obtain crude ferric phosphate solid, wherein the molar ratio of the iron ion concentration in the ferrous sulfate solution to the phosphate radical content in the third phosphorus-containing waste liquid is 1:1.1.
Preparing battery grade ferric phosphate powder: and (3) stirring, pulping and washing the crude ferric phosphate solid obtained in the step (IV) by adopting pure water, drying the washed crude ferric phosphate solid at 90 ℃ after washing until the conductivity of the washing water is 180uS/cm, and calcining at 700 ℃ to obtain the battery grade ferric phosphate powder, wherein the aluminum-containing waste acid liquid contains a surfactant, so that the synthesized ferric phosphate is not easy to agglomerate.
Example 2
The method for preparing the battery grade ferric phosphate powder by utilizing the aluminum-containing waste acid liquid comprises the following steps:
step one, separating aluminum ions in aluminum-containing waste acid liquid: adding the aluminum-containing waste acid liquid into a reaction kettle, starting stirring, slowly adding ammonia water to adjust the pH value of the aluminum-containing waste acid liquid to 5 to obtain a solid-liquid mixture, and obtaining aluminum hydroxide and first phosphorus-containing waste liquid from the solid-liquid mixture;
step two, purifying the first phosphorus-containing waste liquid: adding 27.5wt% of hydrogen peroxide into the first phosphorus-containing waste liquid obtained in the step one, heating to 70 ℃, stirring and reacting for 2 hours, adding active carbon, stirring and reacting for 2 hours, standing for 4 hours, filtering and removing filter residues to obtain a second phosphorus-containing waste liquid, wherein the adding amount of the hydrogen peroxide is 2L/(1000L of the first phosphorus-containing waste liquid), and the adding amount of the active carbon is 1 Kg/(1000L of the first phosphorus-containing waste liquid).
Step three, deeply purifying the second phosphorus-containing waste liquid: removing impurities (copper) from the second phosphorus-containing waste liquid obtained in the step two through ion exchange resin to obtain third phosphorus-containing waste liquid;
step four, synthesizing iron phosphate: adding sulfuric acid solution and a small amount of ferric phosphate powder into a reaction kettle, starting stirring, adding ferrous sulfate solution at a speed of 10L/min and the third phosphorus-containing waste liquid obtained in the third step (through detection analysis, the copper ion content is less than 2mg/L, the phosphate radical content is 2.8 mol/L), adding 27.5wt% of hydrogen peroxide at a speed of 2L/min, stirring for reaction, simultaneously dropwise adding sulfuric acid solution to keep the pH of the reaction liquid between 1.8, performing solid-liquid separation after the reaction is finished, and discarding filtrate to obtain crude ferric phosphate solid, wherein the molar ratio of the iron ion concentration in the ferrous sulfate solution to the phosphate radical content in the third phosphorus-containing waste liquid is 1:1.4.
Preparing battery grade ferric phosphate powder: and (3) stirring, pulping and washing the crude ferric phosphate solid obtained in the step (IV) by adopting pure water, drying the washed crude ferric phosphate solid at 100 ℃ after washing until the conductivity of the washing water is 190uS/cm, and calcining at 900 ℃ to obtain the battery grade ferric phosphate powder, wherein the aluminum-containing waste acid liquid contains a surfactant, so that the synthesized ferric phosphate is not easy to agglomerate.
Example 3
The method for preparing the battery grade ferric phosphate powder by utilizing the aluminum-containing waste acid liquid comprises the following steps:
step one, separating aluminum ions in aluminum-containing waste acid liquid: adding the aluminum-containing waste acid liquid into a reaction kettle, starting stirring, slowly adding sodium carbonate solution, adjusting the pH value of the aluminum-containing waste acid liquid to 4.5 to obtain a solid-liquid mixture, and obtaining aluminum hydroxide and first phosphorus-containing waste liquid from the solid-liquid mixture;
step two, purifying the first phosphorus-containing waste liquid: adding 27.5wt% of hydrogen peroxide into the first phosphorus-containing waste liquid obtained in the step one, heating to 60 ℃, stirring and reacting for 1h, adding active carbon, stirring and reacting for 0.5h, standing for 6h, filtering and removing filter residues to obtain a second phosphorus-containing waste liquid, wherein the adding amount of the hydrogen peroxide is 3L/(1000L of the first phosphorus-containing waste liquid), and the adding amount of the active carbon is 2 Kg/(1000L of the first phosphorus-containing waste liquid).
Step three, deeply purifying the second phosphorus-containing waste liquid: removing impurities (nickel) from the second phosphorus-containing waste liquid obtained in the step two through ion exchange resin to obtain third phosphorus-containing waste liquid;
step four, synthesizing iron phosphate: adding sulfuric acid solution and a small amount of ferric phosphate powder into a reaction kettle, starting stirring, adding ferrous sulfate solution at a speed of 7L/min and the third phosphorus-containing waste liquid obtained in the third step (through detection analysis, the copper ion content is less than 2mg/L, the phosphate radical content is 3.63 mol/L), adding 27.5wt% of hydrogen peroxide at a speed of 1.5L/min, stirring for reaction, simultaneously dropwise adding sulfuric acid solution to keep the pH value of the reaction liquid between 2.0, performing solid-liquid separation after the reaction is finished, and discarding filtrate to obtain crude ferric phosphate solid, wherein the molar concentration of ferric ions in the ferrous sulfate solution and the molar ratio of the phosphate radical content in the third phosphorus-containing waste liquid are 1:1.2.
Preparing battery grade ferric phosphate powder: and (3) stirring, pulping and washing the crude ferric phosphate solid obtained in the step (IV) by adopting pure water, drying the washed crude ferric phosphate solid at 60 ℃ after washing until the conductivity of the washing water is 170uS/cm, and calcining at 900 ℃ to obtain the battery grade ferric phosphate powder, wherein the aluminum-containing waste acid liquid contains a surfactant, so that the synthesized ferric phosphate is not easy to agglomerate.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (6)
1. A method for preparing battery grade ferric phosphate powder by using aluminum-containing waste acid liquid is characterized by comprising the following steps of
Step one, separating aluminum ions in aluminum-containing waste acid liquid: adding the aluminum-containing waste acid liquid into a reaction kettle, starting stirring, slowly adding alkali liquor to adjust the pH value of the aluminum-containing waste acid liquid to 4-5 to obtain a solid-liquid mixture, and obtaining aluminum hydroxide and first phosphorus-containing waste liquid from the solid-liquid mixture;
step two, purifying the first phosphorus-containing waste liquid: adding 27.5wt% of hydrogen peroxide into the first phosphorus-containing waste liquid obtained in the step one, heating to 60-80 ℃ and stirring for reaction for 1-2h, adding active carbon and stirring for reaction for 0.5-2h, standing for 4-8h, and filtering to remove filter residues to obtain a second phosphorus-containing waste liquid;
step three, deeply purifying the second phosphorus-containing waste liquid: removing impurities from the second phosphorus-containing waste liquid obtained in the step two through ion exchange resin to obtain third phosphorus-containing waste liquid;
step four, synthesizing iron phosphate: adding sulfuric acid solution and a small amount of ferric phosphate powder into a reaction kettle, starting stirring, adding ferrous sulfate solution at a speed of 5-10L/min and the third phosphorus-containing waste liquid obtained in the step three, adding 27.5wt% of hydrogen peroxide at a speed of 1-2L/min, stirring for reaction, simultaneously dropwise adding sulfuric acid solution to keep the pH value of the reaction solution between 1.8 and 2.0, and performing solid-liquid separation after the reaction is finished to remove filtrate to obtain crude ferric phosphate solid;
preparing battery grade ferric phosphate powder: stirring, pulping and washing the crude ferric phosphate solid obtained in the step four by adopting pure water, washing until the conductivity in washing water is less than 200uS/cm, drying the washed crude ferric phosphate solid at 60-100 ℃, and calcining at 600-900 ℃ to obtain the battery grade ferric phosphate powder;
the aluminum-containing waste acid liquid is chemical polishing liquid or electrolytic polishing liquid.
2. The method for preparing battery grade iron phosphate powder by using aluminum-containing waste acid solution according to claim 1, wherein the alkali solution in the first step is at least one of sodium hydroxide solution, sodium carbonate solution and ammonia water.
3. The method for preparing battery grade iron phosphate powder by utilizing aluminum-containing waste acid liquid as claimed in claim 1, wherein the adding amount of hydrogen peroxide in the second step is 1-5L/(1000L of the first phosphorus-containing waste liquid).
4. The method for preparing battery grade iron phosphate powder by using aluminum-containing waste acid solution as claimed in claim 1, wherein the addition amount of the activated carbon in the second step is 1-3 Kg/(1000L of the first phosphorus-containing waste liquid).
5. The method for preparing battery grade iron phosphate powder using aluminum-containing waste acid solution according to claim 1, wherein the impurities in the third step include nickel and copper.
6. The method for preparing battery grade iron phosphate powder by using aluminum-containing waste acid solution according to claim 1, wherein the molar ratio of the iron ion concentration in the ferrous sulfate solution to the phosphate content in the third phosphorus-containing waste solution in the fourth step is 1 (1.1-1.4).
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| CN116161633A (en) * | 2022-12-05 | 2023-05-26 | 广东工业大学 | Method for preparing ferric phosphate by utilizing aluminum product sewage and application of ferric phosphate |
| CN117466502A (en) * | 2023-12-28 | 2024-01-30 | 深圳星河环境股份有限公司 | Recovery method of phosphorus-containing waste liquid |
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