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CN-118222848-B - Method for extracting and removing impurities from mixed ore leaching solution

CN118222848BCN 118222848 BCN118222848 BCN 118222848BCN-118222848-B

Abstract

The invention relates to a method for extracting and removing impurities from mixed ore leaching liquid, which comprises the steps of leaching mixed ore of nickel sulfide and laterite nickel by using perchloric acid to obtain leaching liquid, wherein the perchloric acid has strong oxidizing property, so that pressurization or addition of an oxidant is not needed during leaching, the selectivity of impurity ions is good and the extraction rate is high by adopting a synergistic extractant, the synergistic extractant can be recycled, and under the condition that new impurity ions are not introduced, an organic phase is saponified and converted into nickel soap from sodium soap, and the mixed ore leaching liquid is extracted, so that a high-purity nickel sulfate solution can be finally obtained.

Inventors

  • ZHOU ZHULIN
  • RUAN DINGSHAN
  • LI CHANGDONG
  • CHEN RUOKUI
  • RAO JINSHAN
  • LIAO YULONG

Assignees

  • 广东邦普循环科技有限公司
  • 湖南邦普循环科技有限公司

Dates

Publication Date
20260505
Application Date
20240422

Claims (20)

  1. 1. A method for extracting and removing impurities from mixed ore leaching liquid, which is characterized by comprising the following steps: (1) Leaching the mixed ore of nickel sulfide and laterite by using perchloric acid, and concentrating the obtained leaching solution to obtain a mixed ore leaching solution; (2) Mixing a first organic phase with the mixed ore leaching solution obtained in the step (1) to perform first extraction, and separating phases to obtain raffinate containing nickel and magnesium; (3) Mixing a second organic phase with the nickel-magnesium-containing raffinate obtained in the step (2) to carry out second extraction, and carrying out phase separation to obtain a nickel sulfate solution; The first organic phase is obtained by converting an organic phase formed by a first synergistic extractant and a diluent into a first organic phase obtained by converting sodium soap into nickel soap, wherein the total mass percentage of the organic phase formed by the first synergistic extractant and the diluent is 10-60wt% and the balance is the diluent, and the first synergistic extractant comprises P204 and P507, and the total mass percentage of the first synergistic extractant is 100wt% and the P204 is 10-90wt% and the balance is P507; The second organic phase is obtained by converting an organic phase formed by a second synergistic extractant and a diluent into a second organic phase obtained by converting sodium soap into nickel soap, the total mass percentage of the second organic phase formed by the second synergistic extractant and the diluent is 10-60wt%, the balance is the diluent, the second synergistic extractant comprises P507 and C272, the total mass percentage of the second synergistic extractant is 100wt%, and the P507 is 10-90wt% and the balance is C272.
  2. 2. The method of claim 1, wherein the concentration of the perchloric acid in step (1) is 1-8mol/L.
  3. 3. The method of claim 1, wherein the concentrating of step (1) is performed using an ion exchange resin.
  4. 4. The method of claim 1, wherein the flow rate of the ion exchange resin bed is controlled to be 1-8BV/h in the concentration process of step (1).
  5. 5. The method of claim 1, wherein the diluent comprises sulfonated kerosene.
  6. 6. The method of claim 1, wherein the sodium soap has a saponification degree of 10% -70%.
  7. 7. The method of claim 1, wherein the nickel soap has a saponification degree of 10% -80%.
  8. 8. The method of claim 1, wherein the mixed ore leach solution of step (1) has a nickel ion concentration of 80-120g/L, a cobalt ion concentration of 5-15g/L, and a total impurity metal ion concentration of 20-30g/L.
  9. 9. The method of claim 8, wherein the impurity metal ions comprise manganese ions, magnesium ions, copper ions, and zinc ions.
  10. 10. The method of claim 9, wherein the impurity metal ions further comprise calcium ions.
  11. 11. The process according to claim 1, wherein the first extraction of step (2) has an extraction ratio O/A of (0.2-5): 1.
  12. 12. The process according to claim 1, wherein the temperature of the first extraction of step (2) is 20-70 ℃.
  13. 13. The process according to claim 1, wherein the mixing speed of the first extraction of step (2) is 150-450rpm.
  14. 14. The method of claim 1, wherein the first extraction of step (2) is for a period of time of 0.05 to 0.5 hours.
  15. 15. The method of claim 1, wherein the first extraction of step (2) is a 2-8 stage countercurrent extraction.
  16. 16. The method of claim 1, wherein the phase separation in step (2) results in an organic phase containing impurities, and the organic phase containing impurities is subjected to a first stripping and regeneration to obtain a first synergistic extractant and recycled.
  17. 17. The process of claim 16, wherein the concentration of the acid agent used in the first stripping is from 0.1 to 6mol/L.
  18. 18. The method of claim 1, wherein the extraction of the second extraction of step (3) is the same as the extraction of the first extraction of step (2) in terms of O/a, temperature, mixing speed and time.
  19. 19. The process of claim 1, wherein the second extraction of step (3) is a 2-8 stage countercurrent extraction.
  20. 20. The method of claim 17, wherein the phase separation in step (3) results in an organic phase containing impurities, and the organic phase containing impurities is subjected to a second stripping and regeneration to obtain a second synergistic extractant and recycled.

Description

Method for extracting and removing impurities from mixed ore leaching solution Technical Field The invention relates to the technical field of hydrometallurgy, in particular to a method for extracting and removing impurities from mixed ore leaching liquid. Background At present, the explosive development of new energy industry is increasing the demand of high-purity battery grade nickel sulfate solution, so that reasonable development and utilization of nickel resources are needed. In recent years, the domestic high-quality nickel sulfide ore resources are gradually exhausted, and development of low-quality laterite nickel ores or mixed ores of nickel sulfide and laterite nickel, which are large in reserves and difficult to use, is forced to be turned to. The method for treating limonite type laterite nickel ore and sulphide ore by acid leaching is a mature process in the industry, but impurity metal ions such as iron, aluminum, manganese, copper, zinc, calcium, magnesium and the like can be synchronously dissolved into the leaching solution while valuable metals such as nickel, cobalt and the like are dissolved out, so that the leaching solution is subjected to impurity removal, and the obtained high-purity nickel sulfate solution has wide market and prospect. CN 116043032a discloses a nickel cobalt sulphide treatment method. The method comprises the steps of taking nickel cobalt sulfide as a hydrometallurgical intermediate product of laterite nickel ore as a raw material, adding an oxidant, a catalyst and a neutralizer, controlling reaction conditions, carrying out selective oxidation leaching and preliminary impurity removal, separating nickel from impurities to obtain a nickel-containing solution, carrying out deep extraction impurity removal on the nickel-containing solution to obtain a nickel sulfate solution, carrying out evaporation crystallization to obtain a nickel sulfate crystal, carrying out organic reverse extraction, returning an organic phase to the extraction impurity removal step, and returning an impurity sulfate solution to the selective oxidation leaching step. The invention can realize deep extraction and impurity removal, but an oxidant is required to be additionally added during acid leaching, so that the raw material cost is increased. CN 115180653A discloses a method for efficiently utilizing limonite-type and magnesia-type laterite-nickel ore in a combined mode, which comprises the steps of S1, leaching residues obtained by acid leaching of limonite-type low-nickel laterite-nickel ore under normal pressure, filtering to obtain a first leaching solution, S2, carrying out pyrometallurgy on laterite-nickel ore to obtain a ferronickel alloy, S3, leaching the ferronickel alloy after acid matching and water of the first leaching solution to obtain a second leaching solution, and S4, adding a impurity remover into the second leaching solution to purify and remove impurities, and filtering to obtain a high-purity ferrous solution and a nickel cobalt sulfide product; S5, adding the high-purity ferrous solution into an oxidant and a phosphorus source to synthesize ferric phosphate dihydrate. However, this method still involves the risk of impurity metal ions remaining in the nickel sulfate solution produced. Therefore, in order to overcome the defects of the prior art, a method for extracting and removing impurities from leaching liquid, which is simple to operate, does not need to add an oxidant, has good impurity removing effect and does not introduce new impurities, is needed. Disclosure of Invention The invention aims to provide a method for extracting and removing impurities from mixed ore leaching liquid, which adopts perchloric acid to leach metal ions from mixed ore of nickel sulfide and laterite nickel, and extracts and removes impurity ions from the leaching liquid, and does not introduce new impurities, and has the advantages of good impurity removing effect and simple operation. In order to achieve the aim of the invention, the invention adopts the following technical scheme: the invention provides a method for extracting and removing impurities from mixed ore leaching liquid, which comprises the following steps: (1) Leaching the mixed ore of nickel sulfide and laterite by using perchloric acid, and concentrating the obtained leaching solution to obtain a mixed ore leaching solution; (2) Mixing a first organic phase with the mixed ore leaching solution obtained in the step (1) to perform first extraction, and separating phases to obtain raffinate containing nickel and magnesium; (3) Mixing a second organic phase with the nickel-magnesium-containing raffinate obtained in the step (2) to carry out second extraction, and carrying out phase separation to obtain a nickel sulfate solution; The first organic phase in the step (2) is a first organic phase obtained after the organic phase formed by the first synergistic extractant and the diluent is converted into nickel soap through sod