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WO2025076819A1 - Procédé de recyclage d'aluminium et de fer à partir de scories de fer-aluminium - Google Patents

Procédé de recyclage d'aluminium et de fer à partir de scories de fer-aluminium Download PDF

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Publication number
WO2025076819A1
WO2025076819A1 PCT/CN2023/124513 CN2023124513W WO2025076819A1 WO 2025076819 A1 WO2025076819 A1 WO 2025076819A1 CN 2023124513 W CN2023124513 W CN 2023124513W WO 2025076819 A1 WO2025076819 A1 WO 2025076819A1
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WO
WIPO (PCT)
Prior art keywords
iron
aluminum
solution
slag
alkali
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/CN2023/124513
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English (en)
Chinese (zh)
Inventor
陈佳佳
阮丁山
曾志佳
陈若葵
李长东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Original Assignee
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hunan Brunp Recycling Technology Co Ltd, Guangdong Brunp Recycling Technology Co Ltd filed Critical Hunan Brunp Recycling Technology Co Ltd
Priority to PCT/CN2023/124513 priority Critical patent/WO2025076819A1/fr
Priority to CN202380011565.7A priority patent/CN117795107A/zh
Publication of WO2025076819A1 publication Critical patent/WO2025076819A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention belongs to the technical field of waste battery recycling and relates to a method for recycling aluminum and iron from iron-aluminum slag.
  • the main materials produced are graphite slag, iron-aluminum slag and sponge copper.
  • sponge copper can be sold as a product at a low price;
  • the main component of graphite slag is the negative electrode powder graphite in the battery powder;
  • the iron-aluminum slag has the largest slag volume, and its main components are iron and aluminum, and it also carries a certain amount of valuable heavy metals such as nickel, cobalt and manganese. It is very difficult to recycle or harmlessly dispose of it.
  • the industry currently treats iron-aluminum slag as solid waste or hazardous waste.
  • Iron and aluminum are metal elements with high content in nature and have high utilization value.
  • the iron-aluminum slag produced by the wet process of recycling waste batteries contains a large amount of iron and aluminum. It is very meaningful to be able to separate and recycle this part of iron and aluminum.
  • the present invention aims to provide a method for recycling aluminum and iron from iron-aluminum slag.
  • the present invention first separates sulfate from the iron-aluminum slag by alkali conversion reaction; then separates aluminum from the iron-aluminum slag after alkali conversion by alkali leaching reaction to obtain an aluminate solution, and then obtains hydroxide.
  • the aluminum product is obtained by smelting the aluminum slag, while the iron element remains in the iron slag, thereby achieving the separation of the iron and aluminum elements; then, the iron sulfate product is obtained by using the solubility principle of iron sulfate. Therefore, the method disclosed in the present invention can effectively separate and recover the iron and aluminum elements in the iron and aluminum slag.
  • the present invention adopts the following technical solutions:
  • the present disclosure provides a method for recycling aluminum and iron from iron-aluminum slag, the method comprising:
  • the present invention provides a method for recycling aluminum and iron from iron-aluminum slag.
  • sulfate radicals in the iron-aluminum slag are separated by an alkali conversion reaction to obtain a sulfate solution, and then a sulfate product is obtained;
  • aluminum elements are separated from the iron-aluminum slag after the alkali conversion by an alkali leaching reaction to obtain an aluminate solution, and then an aluminum hydroxide product is obtained, while the iron element remains in the iron slag, thereby achieving separation of the iron and aluminum elements;
  • the iron slag is first acid-dissolved and sulfuric acid is added according to the solubility principle of iron sulfate to obtain an iron sulfate product, and the acid solution can be recycled;
  • the method disclosed in the present invention can effectively separate and recover the iron and aluminum elements in the iron-aluminum slag, and can obtain sulfate products, aluminum hydroxide products and ferric sulfate products.
  • the products can be sold to generate profits, and the utilization of the iron-aluminum slag can be maximized, which is beneficial to industrial applications.
  • the iron-aluminum slag includes the iron-aluminum slag produced by wet recovery of ternary batteries.
  • the iron-aluminum slag includes aluminum ions, iron ions, nickel ions, cobalt ions, manganese ions, sulfate ions, Organic matter (COD) and impurities (such as phosphorus and/or fluorine).
  • COD Organic matter
  • impurities such as phosphorus and/or fluorine
  • nickel ions, cobalt ions and manganese ions are precipitated into the iron-aluminum slag after alkali conversion through alkali conversion reaction, and then enter the iron slag through alkali leaching reaction, and then dissolved in acid through acid dissolution, and finally remain in the acid solution.
  • the acid solution can be reused in the acid dissolution step or returned to the battery recycling production line to recover nickel, cobalt and manganese.
  • the alkaline substance in the first alkali solution in step (1) includes at least one of sodium hydroxide, calcium hydroxide and sodium carbonate.
  • the alkaline substance of the first alkali solution when at least one of sodium hydroxide, calcium hydroxide and sodium carbonate is used as the alkaline substance of the first alkali solution, it can undergo an alkali conversion reaction with iron-aluminum slag, and the obtained sulfate solution is a sodium sulfate solution.
  • the main chemical components of the iron aluminum slag are iron alum (NaFe 3 (SO 4 ) 2 (OH) 6 ) and aluminum alum (NaAl 3 (SO 4 ) 2 (OH) 6 ).
  • iron alum NaFe 3 (SO 4 ) 2 (OH) 6
  • aluminum alum NaAl 3 (SO 4 ) 2 (OH) 6
  • reaction equation of the iron aluminum slag and sodium hydroxide is as follows:
  • step (2) the liquid-to-solid mass ratio of the second alkali solution to the alkali-converted iron-aluminum slag is 5:1.
  • the temperature of the alkali leaching reaction in step (2) is 60-80°C, for example, 60°C, 65°C, 70°C, 75°C or 80°C
  • the time of the alkali leaching reaction is 2-4h, for example, 2h, 2.5h, 3h, 3.5h or 4h, etc.
  • the alkali leaching reaction is carried out at a temperature of 60 to 80° C. for 2 to 4 hours to effectively leach aluminum.
  • the Bayer process is a chemical process for producing aluminum oxide from bauxite.
  • the Bayer process is used to prepare aluminum hydroxide, which has low energy consumption, low cost, high product purity, and the separated solution can be recycled without wasting alkali, which greatly reduces costs.
  • the Bayer process includes the following steps:
  • the aluminate solution in step (2) is mixed with seed crystals, and aluminum hydroxide and aluminate mother liquor are obtained after seed separation.
  • the obtained aluminum hydroxide product complies with the product standard GB/T4294-2010 and can be sold externally.
  • the seed crystals include aluminum hydroxide.
  • the amount of the seed crystal added is 0.5 to 1.5 times the theoretical amount required for all aluminum elements in the aluminate solution to be converted into aluminum hydroxide, for example, it can be 0.5 times, 0.7 times, 1 times, 1.2 times, 1.3 times, 1.4 times or 1.5 times, etc. However, it is not limited to the listed values, and other values not listed within the numerical range are also applicable.
  • the decomposition rate of aluminum hydroxide is low; if the amount of seed crystals added is too much, the decomposition rate increases only slightly, resulting in waste.
  • the seeding temperature is 50-60°C, for example, 50°C, 52°C, 54°C, 56°C, 58°C or 60°C
  • the seeding time is 1-10h, for example, 1h, 2h, 4h, 6h, 8h or 10h.
  • it is not limited to the listed values, and other values not listed within the numerical range may be used. The same applies to values.
  • the aluminum hydroxide can be effectively seeded by performing seeding at a temperature of 50 to 60° C. for 1 to 10 hours.
  • the seeding process is accompanied by stirring, and the stirring speed is 150-300 r/min, for example, 150 r/min, 200 r/min, 250 r/min or 300 r/min, etc. However, it is not limited to the listed values, and other values not listed in the numerical range are also applicable.
  • the stirring is continued at a rate of 150 to 300 r/min, so that the seed crystals can be fully dispersed in the solution and fully contact the solution.
  • the mass concentration of aluminum in the aluminate mother solution is 9 to 12 g/L, for example, 9 g/L, 10 g/L, 11 g/L or 12 g/L.
  • the aluminate mother liquor is mixed with the ferroaluminum slag after alkali conversion to carry out alkali leaching reaction, and an aluminate solution and iron slag are obtained after solid-liquid separation.
  • the aluminate solution is further subjected to seed separation using the Bayer process to obtain aluminum hydroxide and new aluminate mother liquor.
  • the aluminate mother liquor is mixed with the alkali-converted iron-aluminum slag, and no alkali is added, so that the alkali in the solution is recycled and the alkali cost is reduced.
  • the aluminate mother liquor can be recycled for many times.
  • the sulfate (such as sodium sulfate) and impurities (such as COD and a small amount of phosphorus and fluorine) in the aluminate mother liquor are highly enriched, the impurities are removed and then evaporated and crystallized to obtain sulfate.
  • the acid used in the acid dissolution process of step (3) includes sulfuric acid, and the concentration of the acid is 2 to 4 mol/L, for example, 2 mol/L, 2.5 mol/L, 3 mol/L, 3.5 mol/L or 4 mol/L.
  • the concentration of the acid is 2 to 4 mol/L, for example, 2 mol/L, 2.5 mol/L, 3 mol/L, 3.5 mol/L or 4 mol/L.
  • the solute in the solution obtained by acid dissolution is mainly ferrous sulfate.
  • high mass concentration sulfuric acid is added to obtain a saturated solution, and then cooled and crystallized to precipitate ferrous sulfate crystals to achieve resource utilization of iron.
  • the recovery rate of ferrous sulfate is 90-99.5% (for example, it can be 90%, 92%, 95% or 98%, etc.). If the mass concentration of sulfuric acid is too low, the ferrous sulfate reaches the solubility and the ferrous sulfate does not precipitate.
  • the acid solution after solid-liquid separation in step (3) mainly contains nickel sulfate/cobalt/manganese and acid, which can be returned to the acid dissolution or to the leaching and impurity removal process of the battery recovery production line to achieve comprehensive recovery and utilization of valuable metals.
  • the present invention has the following beneficial effects:
  • the present invention provides a method for recycling aluminum and iron from iron-aluminum slag.
  • sulfate radicals in the iron-aluminum slag are separated by an alkali conversion reaction to obtain a sulfate solution, and then a sulfate product is obtained;
  • aluminum elements are separated from the iron-aluminum slag after the alkali conversion by an alkali leaching reaction to obtain an aluminate solution, and then an aluminum hydroxide product is obtained, while the iron element remains in the iron slag, thereby achieving separation of the iron and aluminum elements;
  • the iron slag is first acid-dissolved and sulfuric acid is added according to the solubility principle of iron sulfate to obtain an iron sulfate product, and the acid solution can be recycled;
  • the method disclosed in the present invention can effectively separate and recover the iron and aluminum elements in the iron and aluminum slag, and obtain sulfate products, aluminum hydroxide products and iron sulfate products, which can be sold to obtain income, and can maximize the utilization of the iron and aluminum slag, which is beneficial to industrial application.
  • the method is simple, low in cost, no waste is generated, and the wastewater output is extremely small.
  • FIG1 is a schematic diagram of a process for recycling aluminum and iron from iron-aluminum slag provided in one embodiment of the present disclosure.
  • the present disclosure provides a method for recycling aluminum and iron from iron-aluminum slag, the process of which is shown in FIG1 , and the method comprises the following steps:
  • step (3) treating the sodium aluminate solution in step (2) by the Bayer process to obtain Al(OH) 3 and sodium aluminate mother liquor; adding alkali-converted iron-aluminum slag to the sodium aluminate mother liquor for alkali leaching reaction to obtain a sodium aluminate solution, and continuing to treat the sodium aluminate solution by the Bayer process, and repeating the cycle in this manner; when the sodium aluminate mother liquor becomes a solution containing a large amount of impurity sodium sulfate, the solution is decontaminated, and then evaporated and crystallized to obtain sodium sulfate;
  • step (2) Acid dissolving the nickel-iron slag in step (2) and adding sulfuric acid to obtain ferric sulfate crystals. After solid-liquid separation, ferric sulfate and mother liquor are obtained. The mother liquor can be recycled to prepare ferric sulfate crystals and can also be used to recover nickel, cobalt and manganese in battery lines.
  • This embodiment provides a method for recycling aluminum and iron from iron-aluminum slag, wherein the mass contents of the components in the iron-aluminum slag are: 0.5% nickel, 56% sulfate, 10.5% aluminum and 14.5% iron, and the rest are trace impurities (F and P) and COD.
  • the method comprises the following specific steps:
  • the sodium sulfate solution is frozen and crystallized in a freezing reactor at 5°C. After the crystallization is completed, it is quickly centrifuged and dried to obtain alkali solution and sodium sulfate crystals.
  • the sodium sulfate recovery rate is 53.57%.
  • Alkali leaching process the alkali-converted iron-aluminum slag of the above step (1) is subjected to alkali leaching, and a sodium hydroxide solution is prepared, wherein the amount of sodium hydroxide used is 1.5 times the theoretical amount required for all aluminum elements to be converted into sodium aluminate, the liquid-to-solid (mass) ratio is 5:1, and the leaching temperature is 60° C.
  • nickel-iron slag and sodium aluminate solution wherein the nickel content of the nickel-iron slag is 1.0%, the iron content is 29%, and the aluminum content is 6.3%; the aluminum content of the sodium aluminate solution is 14.7 g/L, the ⁇ k is 1.55, and the aluminum leaching rate is 70%;
  • step (2) adding 2 mol/L sulfuric acid to the nickel-iron slag obtained in step (2), at a temperature of 60° C., a reaction time of 4 h, and a liquid-to-solid (mass) ratio of 5:1; filtering after the reaction, the iron acid solubility is 80%, and 8 g of waste residue and an acid-dissolved solution are obtained; the acid-dissolved solution contains 46.4 g/L iron and 1.4 g/L nickel; continuing to add an equal volume of 60% sulfuric acid to the acid-dissolved solution, cooling to precipitate iron sulfate crystals, centrifuging to separate the solid and the liquid, the iron recovery rate is 90%, and the solid is the product iron sulfate, which meets the product standard of HG/T4816-2015, and the data are shown in Table 2; wherein the sulfuric acid solution is recycled to the front end acid dissolve or precipitate iron sulfate crystals.
  • the sodium sulfate solution is frozen and crystallized in a frozen reactor at 5° C. After the crystallization is completed, it is quickly centrifuged and dried to obtain an alkali solution and sodium sulfate crystals, and the sodium sulfate recovery rate is 71.43%;
  • Seeding process adding seed aluminum hydroxide to the sodium aluminate solution obtained in the alkali leaching process in an amount equal to 1 times the theoretical amount of aluminum, stirring at a speed of 200 r/min, and reacting at a temperature of 55° C. for 7 h. After the reaction is completed, filtering is performed to obtain a sodium aluminate mother liquor with an aluminum content of 11.53 g/L and aluminum hydroxide; the aluminum decomposition rate is 41%, and the aluminum hydroxide meets the product standard of GB/T4294-2010.
  • Table 1 The specific data are shown in Table 1;
  • step (3) (4) adding the ferroaluminum slag after alkali conversion from the alkali conversion process to the sodium aluminate mother liquor obtained in step (3) to reduce ⁇ k to 1.55-1.65 without adding sodium hydroxide, and repeating the alkali leaching and seed separation process;
  • This embodiment provides a method for recycling aluminum and iron from iron-aluminum slag, wherein the mass contents of the components in the iron-aluminum slag are: 0.5% nickel, 56% sulfate, 10.5% aluminum and 14.5% iron, and the rest are trace impurities (F and P) and COD.
  • the method comprises the following specific steps:
  • the sodium sulfate solution is frozen and crystallized in a frozen reactor at 5° C. After the crystallization is completed, it is quickly centrifuged and dried to obtain an alkali solution and sodium sulfate crystals, and the sodium sulfate recovery rate is 89.29%;
  • Alkali leaching process the alkali-converted ferroaluminum slag of the above step (1) is subjected to alkali leaching, and a sodium hydroxide solution is prepared, wherein the amount of sodium hydroxide used is 2.5 times the theoretical amount required for all aluminum elements to be converted into sodium aluminate, the liquid-to-solid ratio is 5:1, and the leaching temperature is 80°C, and the stirring reaction is carried out for 2 hours; after the reaction is completed, it is filtered while hot to obtain 35g of nickel-iron slag and sodium aluminate solution, wherein the nickel content of the nickel-iron slag is 1.43%, the iron content is 41.43%, and the aluminum content is 0.7%; the aluminum content of the sodium aluminate solution is 20.52g/L, the ⁇ k is 1.65, and the aluminum leaching rate is 97.7%;
  • Seeding process adding seed aluminum hydroxide to the sodium aluminate solution obtained in the alkali leaching process in an amount of 1.5 times the theoretical amount of aluminum, stirring at a speed of 250 r/min, and reacting at a temperature of 50° C. for 8 h. After the reaction is completed, filtering is performed to obtain a sodium aluminate mother liquor with an aluminum content of 11.13 g/L and aluminum hydroxide; the aluminum decomposition rate is 47%, and the aluminum hydroxide meets the product standard GB/T4294-2010.
  • Table 1 The specific data are shown in Table 1;
  • step (3) (4) adding the ferroaluminum slag after alkali conversion from the alkali conversion process to the sodium aluminate mother liquor obtained in step (3) to reduce ⁇ k to 1.55-1.65 without adding sodium hydroxide, and repeating the alkali leaching and seed separation process;
  • step (2) Add 4 mol/L sulfuric acid to the nickel-iron slag obtained in step (2), the temperature is 60° C., and the reaction time is 4h, liquid-solid ratio 5:1; after the reaction was completed, it was filtered, the iron acid solubility was 98.6%, and 1g of waste residue and acid solution were obtained; the acid solution contained 81.65g/L iron and 2.82g/L nickel; an equal volume of 98% sulfuric acid was continued to be added to the acid solution, and iron sulfate crystals were precipitated after cooling. The solid and liquid were separated by centrifugation, and the iron recovery rate was 99.5%. The solid was the product iron sulfate, which met the product standard of HG/T4816-2015, and the data are shown in Table 2; the sulfuric acid solution was recycled to dissolve in the front end acid or precipitate iron sulfate crystals.
  • Alkali leaching process Add sodium hydroxide solution with a theoretical amount of aluminum element to the washed aluminum slag. At this time, aluminum alum and iron alum react with sodium hydroxide to obtain sodium aluminate solution and nickel-iron slag. The leaching rate of aluminum is only 25%;
  • Example 1 compared with the aluminum leaching rate and iron recovery rate of Example 1, the method of Comparative Example 1 cannot effectively separate and recover aluminum and iron, the recovery rates of the two are low, and no sodium sulfate product is recovered.

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Abstract

L'invention concerne un procédé de recyclage d'aluminium et de fer à partir de scories de fer-aluminium. Le procédé consiste à : (1) mélanger des scories de fer-aluminium avec une première liqueur alcaline afin de réaliser une réaction de conversion alcaline, et effectuer une séparation solide-liquide, de façon à obtenir une solution de sulfate et des scories de fer-aluminium converties en milieu alcalin ; (2) mélanger les scories de fer-aluminium converties en milieu alcalin avec une seconde liqueur alcaline afin de réaliser une réaction de lixiviation alcaline, et effectuer une séparation solide-liquide, de façon à obtenir une solution d'aluminate et des scories de fer ; et (3) soumettre les scories de fer à une dissolution d'acide, puis ajouter de l'acide sulfurique afin de précipiter du sulfate ferrique, et effectuer une séparation solide-liquide, de façon à obtenir des cristaux de sulfate ferrique et une solution acide. Au moyen du procédé, le fer et l'aluminium dans les scories de fer-aluminium peuvent être efficacement séparés et recyclés.
PCT/CN2023/124513 2023-10-13 2023-10-13 Procédé de recyclage d'aluminium et de fer à partir de scories de fer-aluminium Pending WO2025076819A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/CN2023/124513 WO2025076819A1 (fr) 2023-10-13 2023-10-13 Procédé de recyclage d'aluminium et de fer à partir de scories de fer-aluminium
CN202380011565.7A CN117795107A (zh) 2023-10-13 2023-10-13 一种铁铝渣资源化回收铝和铁的方法

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Application Number Priority Date Filing Date Title
PCT/CN2023/124513 WO2025076819A1 (fr) 2023-10-13 2023-10-13 Procédé de recyclage d'aluminium et de fer à partir de scories de fer-aluminium

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CN119120904A (zh) * 2024-09-05 2024-12-13 广东邦普循环科技有限公司 一种全链条一体化回收铁铝渣的方法和应用

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