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
  • 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
• • 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
  • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
  • C02F1/62—Heavy metal compounds
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F9/00—Multistage treatment of water, waste water or sewage
• • 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
• • 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
  • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
  • C22B26/20—Obtaining alkaline earth metals or magnesium
  • C22B26/22—Obtaining magnesium
• • 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
  • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/02—Treatment of water, waste water, or sewage by heating
  • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
  • C02F1/048—Purification of waste water by evaporation
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/28—Treatment of water, waste water, or sewage by sorption
  • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
  • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
  • C02F1/5272—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using specific organic precipitants
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F2101/00—Nature of the contaminant
  • C02F2101/10—Inorganic compounds
  • C02F2101/20—Heavy metals or heavy metal compounds
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
  • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
• • 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 process for producing nickel by the HPAL route consists essentially of the following steps: (i) preparation of nickel lateritic ore, (ii) nickel leaching under sulfuric acid pressure, (iii) nickel precipitation, (iv) re-leaching, (v) solvent extraction of nickel and (vi) electro-refining to produce nickel cathode (99.95% pure nickel metal) . Due to the significant presence of cobalt in the ore, it will be obtained as a co-product, also in metallic form.
• the extraction levels of this process reach values from 92 to 96% for nickel and 90 to 92% for cobalt. Normally, to obtain this degree of extraction, the reaction suspension after chemical attack should have a residual free acid concentration of 30 to 50 g / L.
• step (b) solid / liquid separation of the metal sulfides obtained in step (b) and formation of a metal free liquid phase;
• the process object of the present invention further includes the following steps: d) addition of amine - in solution and in the proportion of 50 to 250 g / l - to the liquid phase, with precipitation of magnesium in the form of hydroxide - Mg (OH) 2; and e) amine recovery by depletion and rectification.
• Figure 2 is a flow chart of the process for treating liquid effluents and recovering metals object of the present invention.
• the process object of this invention also makes it possible to remove remaining metals in the liquid effluent such as manganese (Mn), zinc (Zn), cobalt (Co), copper (Cu), among others, thus creating conditions for their complete recycling in the wastewater. process, as well as providing additional micronutrient production for agricultural applications, among others.
• Mn manganese
• Zn zinc
• Co cobalt
• Cu copper
• liquid effluent 1 is received in agitated tanks for equalization.
• the homogenized (equalized) effluent 2 receives sulfide additions 3, in the form of Na 2 S and / or H 2 S, for precipitation of the remaining metals such as Ni, Co, Mn, Zn, Cu, among others. 4.
• sulfides are subjected to a solid-liquid separation operation, resulting in a rich stream of metal sulfides. 5.
• the sulfides are oxidized in stirred reactors with oxygen injection. 6 and The resulting solution 7 is crystallized to obtain the respective fractionated or mixed salts 8 which are stored and sent for dispatch 9.
• the substantially metal-free liquid phase or effluent thus treated is transferred to the stirred reaction system, where it is contacted with low boiling amines via recovered amine 12 and replacement amine streams. 11, resulting from this reaction a suspension of precipitated magnesium hydroxide 13.
• the amine is added at a rate of 50 to 250 g / l at a temperature of 25 to 70 ° C, solids content of 1 to 10% w / p, residence time 0.5 to 2 hours and suspension recycle ratio 5 to 40: 1.
• this cake is subjected to drying and calcination, resulting in the obtaining of magnesia 17, which is stored, being part recycled to the nickel extraction process and the remainder traded 18.
• the amine / effluent ratio It must be kept in the range of 100 to 200 g / L and is optimized according to the magnesium content in solution.
• Part of the suspension of precipitated magnesium hydroxide is recirculated from the thickener underflow to the contact reactors in order to promote the growth of Mg (OH) 2 crystals through seeds.
• the gaseous streams exiting the precipitation reactors and drying of magnesium hydroxide are transferred to an amine absorption system and returned to reprocessing the precipitation reactors.
• the supernatant liquid phase of thickener 19 proceeds to the amine recovery step via distillation in two steps by depletion and then by rectification.
• the depletion of the amine is effected by heating the amine-containing weak acid solution 19 to temperatures in the range 90 to 120 ° C with low pressure steam 27 - 1.5 to 3.0 kgf / cm 2 (man.) - fed continuously. This results in a tower bottom mass stream 21 consisting of weak acid and traces of amine, which is transferred to activated carbon columns to remove residual amounts of amine contained. The resulting weak acid 22 is transferred to the storage area, thereafter 23 for reuse in the hydrometallurgical process. Saturated activated carbon 24 proceeds to the regeneration step, after which 25 is recomposed with the addition of new carbon 26.
• the amine recovery tests were performed in a laboratory distiller, coupled to a reactor-crystallizer, with the purpose of recycling the amine by fractional distillation and recovery of Mg (OH) 2.
• the reactor was heated by a thermostated bath at 70 ° C.
• a coil capacitor was connected to the reactor.
• the condenser jacket was fed with water at 60 ° C and circulated by means of a peristaltic pump to keep the temperature constant.
• the amine gas proceeded to bubbling in H 2 SO 4 solution (10% w / w).
• the acid solution, receptor of all recovered amine was later analyzed to calculate the recovery of the organic reagent.
• an inflated air stream was used into the reactor.
• the pH of the solution was monitored throughout the experiment using a fingerprint meter.
• Table 3 shows the evolution of liquid effluent quality during the treatment process object of this invention.
• Mg is recovered as precipitated magnesium hydroxide, which can be easily recycled to earlier process steps as a low-cost alternative to state-of-the-art techniques. art.
• sulfur is recovered in acidic water from the polishing operation on the coal columns.
• the amine evaporates at lower temperatures, allowing the magnesium and sulfur recovered in this process step to be recirculated for the leaching operation.

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Organic Chemistry (AREA)
• Environmental & Geological Engineering (AREA)
• Life Sciences & Earth Sciences (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Manufacturing & Machinery (AREA)
• Materials Engineering (AREA)
• Geology (AREA)
• General Life Sciences & Earth Sciences (AREA)
• Geochemistry & Mineralogy (AREA)
• Hydrology & Water Resources (AREA)
• Water Supply & Treatment (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Manufacture And Refinement Of Metals (AREA)
• Removal Of Specific Substances (AREA)
• Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

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• 2010
  • 2010-08-09 BR BRPI1003193-6A patent/BRPI1003193B1/pt not_active IP Right Cessation
• 2011
  • 2011-08-09 CN CN201180043673.XA patent/CN103097558B/zh not_active Expired - Fee Related
  • 2011-08-09 PE PE2013000249A patent/PE20131206A1/es not_active Application Discontinuation
  • 2011-08-09 US US13/816,205 patent/US9410223B2/en not_active Expired - Fee Related
  • 2011-08-09 EA EA201390226A patent/EA023878B1/ru not_active IP Right Cessation
  • 2011-08-09 WO PCT/BR2011/000274 patent/WO2012019265A1/pt not_active Ceased
  • 2011-08-09 KR KR1020137005206A patent/KR101843598B1/ko not_active Expired - Fee Related
  • 2011-08-09 AU AU2011288945A patent/AU2011288945B2/en not_active Ceased
  • 2011-08-09 EP EP11815938.3A patent/EP2604712B1/en not_active Not-in-force
  • 2011-08-09 JP JP2013523444A patent/JP5752794B2/ja not_active Expired - Fee Related
  • 2011-08-09 MX MX2013001599A patent/MX2013001599A/es not_active Application Discontinuation
  • 2011-08-09 PH PH1/2013/500273A patent/PH12013500273A1/en unknown
  • 2011-08-09 CA CA2811452A patent/CA2811452C/en active Active
• 2013
  • 2013-02-08 CL CL2013000410A patent/CL2013000410A1/es unknown
  • 2013-02-18 ZA ZA2013/01249A patent/ZA201301249B/en unknown

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