Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G51/00—Compounds of cobalt
  • C01G51/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G53/00—Compounds of nickel
• • 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
  • C22B23/00—Obtaining nickel or cobalt
  • C22B23/04—Obtaining nickel or cobalt by wet processes
  • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
  • C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
• • 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
  • C22B23/00—Obtaining nickel or cobalt
  • C22B23/04—Obtaining nickel or cobalt by wet processes
  • C22B23/0476—Separation of nickel from cobalt
  • C22B23/0484—Separation of nickel from cobalt in acidic type 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
  • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
  • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
  • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
  • C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
  • C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
• • 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 invention relates to a process for the selective separation of nickel and lead from acidic aqueous co-solutions, in particular co-carbonate, sulfate or chloride solutions, by reactive extraction with acidification using a carbonate solution.
• the object of the invention is to process cobalt and lead-containing solutions, in particular carbonate, sulfate or chloride solutions, using reactive extraction.
• the task may also be to separate nickel from cobalt.
• the process is said to be able to be carried out in conventional mixer-separator apparatuses or also in extraction columns and, in addition to improving the quality, is also intended to increase the cobalt yield.
• the pH adjustment in the aqueous system for the precipitation of iron ions is carried out with the aid of carbonate solutions, in particular cobalt or potassium carbonate solutions.
• the pH adjustment can be carried out with sodium hydroxide solution and 'a part.
• the invention relates to a process for cleaning cobalt- and / or nickel-containing mixtures, in particular ores, ore mines, alloys or Co / Ni-containing scrap other metals or metal ions using cobalt and / or nickel-containing aqueous solutions with the following steps:
• step F cleaning and working up the cobalt-containing organic phase from step F) and / or cleaning and working up the nickel-containing aqueous phase from step F).
• the carbonate-containing solution preferably contains sodium, calcium, potassium, or cobalt carbonate or a mixture of these carbonates.
• the phosphoric acid ester for carrying out steps E) and / or F) is preferably selected from di- (2-ethylhexyl) phosphoric acid or bis- (2,4,4-trimethylpentyl) phosphinic acid or any mixture of these two compounds.
• a ion exchanger is particularly preferably a mixture of di- (2-ethylhexyl) phosphoric acid and bis- (2,4,4-trimethylpentyl) phosphinic acid in a weight ratio of 10:90 to 90:10, preferably 20:80 to 80:20 used.
• An organic solvent of the organic extractant for carrying out steps E) and / or F) is particularly preferably an aliphatic or aromatic hydrocarbon or a mixture of such hydrocarbons, in particular an aliphatic or aromatic hydrocarbon with 4 to 18, particularly preferably 10 to 14, carbon atoms ,
• the solution extraction according to step E) and / or F) is particularly preferably carried out at a ratio between solution and extracting agent of 1: 5 to 5: 1, preferably 1: 2 to 2: 1.
• An embodiment of the method is particularly preferred in which the pH of the solution rises to up to 3.5 in the course of the extraction in step E).
• a variant of the process is particularly preferred, which is characterized in that in the event that cobalt carbonate is obtained from the purification in step G), part of this cobalt carbonate is used in step B) as a carbonate source for the carbonate solution.
• the acidic, aqueous co-solution should be adjusted to a basic pH with a carbonate solution. This should preferably be in the range of 1 to 2. However, higher pH values from 1 to 4 can also be set here.
• the process can be used in the known extraction devices (stirred tanks, mixer-separator devices, extraction columns or also centrifugal extractors.
• the devices can be connected in cascades or used as intermediate stages. Setting the required pH values for extraction can be done with the usual acids and bases. It was surprisingly found that cobalt and lead have a much larger separation factor in carbonate-containing systems than in pure sulfate or chloride systems.
• a stock solution with cobalt, nickel and lead was prepared.
• the metals were used in the solution as cobalt chloride, nickel chloride and lead chloride.
• To dissolve the metal salts the aqueous phase was acidified with hydrochloric acid.
• the solutions prepared were then centrifuged and thus undissolved salts were separated off. After centrifugation, the solution was divided into 5 batches. The 5 batches were mixed with sodium hydroxide solution, ammonia, sodium carbonate, calcium carbonate and potash according to Table 1. The concentration of the metal ions was then determined analytically.
• the organic phase is made from Cyanex 272 and Escaid 120.
• a mixture of 20 Vöi% Cyanex 272 in Escaid 120 was used for this. This mixture was pre-stripped with HC1 (9 vol%).
• the mixture was mixed at 60 ° C. in a volume ratio of 1: 3 (hydrochloric acid to organic phase) for 20 min.
• the organic phase was activated.
• a 12.5 vol% sodium hydroxide solution and the organic phase in a volume ratio of 1:15 (sodium hydroxide solution to organic phase) were used.
• Activation was carried out at 60 ° C.
• the organic phase was used to carry out the equilibrium experiments.
• the shaking tests were carried out at 60 ° C.
• the contact time was 20 minutes.
• the existing aqueous solution is mixed with 40 mL NH 3 (25%)
• the aqueous solution present was treated with 23.1 g of Na 2 CO 3
• the aqueous solution present was treated with 30.12 g of K 2 CO 3
• the ratio of the components was determined with 10% by volume bis- (2,4,4-trimethyl-penryl) -phosphinic acid, 10% by volume from di- (2-ethylhexyl) -phosphoric acid and 80% by volume Escaid 120.
• Table 8 Extraction yields for the extraction of a cobalt chloride solution, which was blunted with cobalt carbonate and then with a mixture of Escaid 120, bis- (2,4,4-trimethylpentyl) -phosphinic acid and from di- (2-ethylhexyl) -phosphoric acid was extracted.
• Example 2 To carry out the tests, the solution analogous to that in Example 2.A) was used.
• the pH adjustment for the various test points was carried out analogously to Table 9.
• the organic phase was composed of 20% by volume of di- (2-ethylhexyl) phosphoric acid and 80% by volume Escaid 120.
• the experiments were carried out in a phase ratio of 100 ml aqueous cobalt chloride solution and 300 ml organic phase. The two phases were mixed intensively at 30 ° C. for 15 min and then separated. Table 10 shows the results obtained
• FIG. 2 shows the extraction yields and the corresponding shift in the lead isotherm by using a mixture of di- (2-ethylhexyl) phosphoric acid and bis- (2,4,4-trimethylpentyl) phosphinic acid.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Metallurgy (AREA)
• Manufacturing & Machinery (AREA)
• Mechanical Engineering (AREA)
• Materials Engineering (AREA)
• Inorganic Chemistry (AREA)
• Geology (AREA)
• Life Sciences & Earth Sciences (AREA)
• Environmental & Geological Engineering (AREA)
• Geochemistry & Mineralogy (AREA)
• General Life Sciences & Earth Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Manufacture And Refinement Of Metals (AREA)
• Extraction Or Liquid Replacement (AREA)

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• 2003
  • 2003-12-05 DE DE10356822A patent/DE10356822A1/de not_active Withdrawn
• 2004
  • 2004-11-26 JP JP2006541852A patent/JP2007515552A/ja active Pending
  • 2004-11-26 AU AU2004295078A patent/AU2004295078A1/en not_active Abandoned
  • 2004-11-26 EP EP04798091A patent/EP1692079A1/de not_active Withdrawn
  • 2004-11-26 WO PCT/EP2004/013432 patent/WO2005054137A1/de not_active Application Discontinuation

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