AU2020102537A4 - Method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide - Google Patents

Method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide Download PDF

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AU2020102537A4
AU2020102537A4 AU2020102537A AU2020102537A AU2020102537A4 AU 2020102537 A4 AU2020102537 A4 AU 2020102537A4 AU 2020102537 A AU2020102537 A AU 2020102537A AU 2020102537 A AU2020102537 A AU 2020102537A AU 2020102537 A4 AU2020102537 A4 AU 2020102537A4
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nickel
cobalt
sulfate
liquid
calcium
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Chaoqun DENG
Qiang Li
Sanping LIU
Shuchen QIN
Lifeng Su
Haibei WANG
Yufang Wang
Keng XIE
Xuedong Zhang
Chaozhen ZHENG
Qifan ZHOU
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BGRIMM Technology Group Co Ltd
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    • 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
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/043—Sulfurated acids or salts thereof
    • 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
    • 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
    • C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
    • 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

Abstract

A method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel cobalt hydroxide is provided, and belongs to the technical field of nickel-cobalt hydrometallurgy. Sulfuric acid leaching is conducted on the mixed nickel-cobalt hydroxide; then a nickel/cobalt/manganese-based neutralizer is used to remove iron and aluminum in the solution; liquid-solid separation is conducted to obtain slag after iron removal; acid dissolution is conducted on the slag after iron removal to recycle nickel and cobalt; and a precipitant (one or more of nickel fluoride, cobalt fluoride, and manganese fluoride) is added to liquid after iron removal, to remove calcium and magnesium ions in the system. A saponified P204 extractant is used to remove Mn, Cu, Zn, and other impurities from liquid after calcium and magnesium removal; a saponified P507 extractant is used to separate nickel and cobalt from raffinate obtained after P204 extraction, to obtain battery-grade nickel sulfate and cobalt sulfate solutions; and the battery-grade nickel sulfate and cobalt sulfate solutions are subject to evaporative crystallization to obtain products. The disclosure greatly reduces a dosage of calcium oxide, the amount of calcium ions introduced into the system, and corresponding losses of nickel and cobalt, thereby avoiding the influence of calcium sulfate crystallization on the extraction, simplifying the operation of P507 extraction, and reducing purification costs. 1/1 DRAWINGS Mixed nickel-cobalt hydroxide Sulfuric acid Acid dissolution Liquid-solid separation Manganese slag (for external sales) Nickel-cobalt sulfate solution Neutralizer Neutralization for iron and aluminum removal Liquid-solid separation Liquid after iron and Nickel-cobalt-iron Precipitant aluminum removal aluminum slag Sulfuric acid Calcium and magnesium removal Acid dissolution Liquid-solidLiquid-solid separation- separation Calcium- sManganese slag magnesium slag (for external Liquid after calcium and sales) magnesium removal Nickel-cobalt Calcium sulfate solution oxide slurry P204 extraction Neutralization for for purification ironandaluminum removal P507 extraction for nickel and Liquid-solid cobalt separation separation Nickel sulfate Cobalt sulfate solution solution Liquid after iron Iron-aluminum and aluminum slag removal Evaporative Evaporative crystallization crystallization Battery-grade Battery-grade nickel sulfate cobalt sulfate FIG. 1

Description

1/1
DRAWINGS
Mixed nickel-cobalt hydroxide
Sulfuric acid
Acid dissolution
Liquid-solid separation Manganese slag (for external sales) Nickel-cobalt sulfate solution Neutralizer Neutralization for iron and aluminum removal
Liquid-solid separation
Liquid after iron and Nickel-cobalt-iron aluminum removal aluminum slag Precipitant Sulfuric acid Calcium and magnesium removal Acid dissolution
Liquid-solidLiquid-solid separation- separation Calcium- sManganese slag magnesium slag (for external Liquid after calcium and sales) magnesium removal Nickel-cobalt Calcium sulfate solution oxide slurry P204 extraction Neutralization for for purification ironandaluminum removal P507 extraction for nickel and Liquid-solid cobalt separation separation
Nickel sulfate Cobalt sulfate solution solution Liquid after iron Iron-aluminum and aluminum slag removal Evaporative Evaporative crystallization crystallization
Battery-grade Battery-grade nickel sulfate cobalt sulfate
FIG. 1
I
METHOD FOR PREPARING BATTERY-GRADE NICKEL SULFATE AND COBALT SULFATE FROM MIXED NICKEL-COBALT HYDROXIDE TECHNICAL FIELD The disclosure belongs to the technical field of nickel-cobalt hydrometallurgy, and relates to a method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide. BACKGROUND Any discussion of the background art throughout the specification should in no way be considered as an admission that such background art is prior art, nor that such background art is widely known or forms part of the common general knowledge in the field. With the exploitation and depletion of nickel sulfide ores and the increasing demand for nickel, the extraction of nickel and cobalt from abundant laterite nickel ores has received increasing attention. At present, a hydrometallurgical treatment process for laterite nickel ores is mainly a high-pressure acid leaching method. To facilitate transportation and reduce costs, the laterite nickel ore is usually processed into a mixed nickel-cobalt hydroxide precipitate (MHP) intermediate product that is prepared by high-pressure acid leaching, purification, and neutralization and precipitation. The mixed nickel-cobalt hydroxide is an important raw material for producing products such as battery-grade nickel sulfate and cobalt sulfate. A hydrometallurgical process is mostly adopted to produce battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide. The process generally includes sulfuric acid leaching, iron and aluminum removal by neutralization, extraction and purification, nickel and cobalt separation, etc. For example, Jiangxi Tungsten Industry Group Co., Ltd, Jinchuan Group Co., Ltd, Zhejiang Huayou Cobalt Co., Ltd, etc. all adopt this method. Due to complex components of mixed nickel-cobalt hydroxide and extremely strict requirements on impurities in battery-grade nickel sulfate and cobalt sulfate, purification and separation processes for leachate of the mixed nickel-cobalt hydroxide are not perfect. The sulfuric acid leachate of the mixed nickel-cobalt hydroxide further contains Fe, Al, Ca, Mg, Cr, Cu, Mn, Zn, etc. in addition to Ni and Co. A large number of common impurity ions can be removed by an oxidation-neutralization method, a replacement method, a sulfide method, a fluoride method, an extraction method, etc. At present, the removal of iron and aluminum from an acidic nickel-cobalt solution prepared from mixed nickel-cobalt hydroxide is mainly conducted by using a neutralization method based on calcium oxide slurry. This process is widely used, but there exist problems as follows: A large amount of iron-aluminum slag with nickel content of 6-12% is obtained after iron and aluminum removal through neutralization by using calcium oxide. A large loss of nickel is caused because nickel cannot be recovered, and a nickel loss rate is approximately 1.5%. In addition, Ca ions are introduced into the system due to the addition of calcium oxide. Because the Ca ions in the nickel-cobalt solution are saturated, a large number of calcium sulfate crystals are precipitated during P204 extraction and stripping of the Ca ions, blocking a pipeline, and seriously hindering the extraction process. This has become a technical problem that needs to be solved urgently. A fluoride precipitation method, a solvent extraction method, etc. are main methods for the removal of calcium and magnesium in the nickel-cobalt solution. In the fluoride precipitation method, based on a characteristic that MgF2 and CaF 2 have extremely low solubility, a NaF reagent is added to remove calcium and magnesium ions in the solution. A disadvantage of this method is that a large number of sodium ions are introduced into the solution. In the solvent extraction method, P204 extraction is adopted to remove Ca, Mn, Cu, Zn, and other impurities, and P507 extraction is adopted to separate nickel, cobalt, and magnesium from raffinate obtained after the P204 extraction, to produce battery-grade nickel sulfate and cobalt sulfate products. This method is also currently applied widely. Problems existing in the extraction method for the removal of calcium and magnesium are as follows: During the P204 extraction for calcium removal, a large number of calcium sulfate crystals block an extraction tank and a pipeline, which requires regular removal of calcium sulfate crystals. During the P507 extraction for magnesium separation, a large number of extraction stages are required, and it is also quite difficult to conduct separation. Therefore, a new method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide is urgently needed, to solve the technical problem in the prior art that calcium sulfate crystals block a pipeline and seriously hinder extraction, and improve the yields of nickel and cobalt and the production efficiency. SUMMARY In the disclosure, a new neutralizer is adopted to remove iron and aluminum, slag obtained after iron removal is subject to acid dissolution to recover nickel and cobalt, and liquid after iron removal is subject to purification and separation. In addition, a process for removing calcium and magnesium by using a new precipitant and conducting P204 extraction for purification and P507 extraction for nickel and cobalt separation on liquid after calcium and magnesium is proposed. In a solution purification method adopted in this new process, no new impurity ions are introduced, greatly reducing a dosage of calcium oxide and losses of nickel and cobalt in the iron and aluminum removal process, greatly reducing the influence of calcium sulfate crystallization on the P204 extraction, and simplifying the operation of the P507 extraction for magnesium separation. This process is an efficient and green method for removing calcium and magnesium from a nickel-cobalt solution. The disclosure provides a method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide. Sulfuric acid leaching is conducted on the mixed nickel-cobalt hydroxide; then a new neutralizer is used for neutralization to remove iron and aluminum in a nickel-cobalt sulfate solution; and a new precipitant is added to liquid after iron removal to remove calcium and magnesium ions in the system. A saponified P204 extractant is used to remove Mn, Cu, Zn, and other impurities from liquid after calcium and magnesium removal; a saponified P507 extractant is used to separate nickel and cobalt from raffinate obtained after P204 extraction, to obtain battery-grade nickel sulfate and cobalt sulfate solutions; and the battery-grade nickel sulfate and cobalt sulfate solutions are subject to evaporative crystallization to obtain battery-grade nickel sulfate and cobalt sulfate products. In this purification method, the mixed nickel-cobalt hydroxide is used as a neutralizer for iron and aluminum removal, which can reduce a dosage of calcium oxide, the amount of calcium ions introduced into the system, and losses of nickel and cobalt in the iron and aluminum removal process; and the new precipitant is used to remove calcium and magnesium, avoiding the influence of calcium sulfate crystallization on the extraction, simplifying the operation of P507 extraction, reducing purification costs, and effectively removing impurity ions in the nickel-cobalt solution to obtain the nickel sulfate and cobalt sulfate products. The technical solution adopted in the disclosure is as follows. A method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide is provided, including the following steps: (1) acid dissolution: slurrying the mixed nickel cobalt hydroxide with water, adding sulfuric acid for dissolution, and conducting liquid-solid separation to obtain manganese slag and a nickel-cobalt sulfate solution; (2) neutralization for iron and aluminum removal: adding a nickel/cobalt/manganese-based neutralizer to the nickel-cobalt sulfate solution obtained in step (1) for reaction, and conducting liquid-solid separation to obtain nickel-cobalt-iron-aluminum slag and liquid after iron and aluminum removal; (3) secondary acid dissolution: slurrying the nickel-cobalt-iron-aluminum slag obtained in step (2) with water, adding sulfuric acid for dissolution, and conducting liquid-solid separation to obtain manganese slag and a nickel-cobalt sulfate solution; (4) secondary neutralization for iron and aluminum removal: adding calcium oxide slurry to the nickel-cobalt sulfate solution obtained in step (3) for reaction, and conducting liquid-solid separation to obtain iron-aluminum slag and liquid after iron and aluminum removal; (5) calcium and magnesium removal: combining the liquid after iron and aluminum removal obtained in step (2) and step (4), adding a precipitant for reaction, and conducting liquid-solid separation to obtain calcium-magnesium slag and liquid after calcium and magnesium removal;
(6) P204 extraction for purification: conducting P204 extraction for purification on the liquid after calcium and magnesium removal obtained in step (5) to remove copper, manganese, zinc, and calcium impurities to obtain raffinate after the P204 extraction, and recycling a loaded organic phase according to steps of stripping, Fe stripping, and chlorine scrubbing; (7) P507 extraction for nickel and cobalt separation: conducting P507 extraction for nickel and cobalt separation on the raffinate after the P204 extraction obtained in step (6) to obtain pure nickel sulfate and cobalt sulfate solutions; and (8) evaporative crystallization: conducting evaporative crystallization on the pure nickel sulfate and cobalt sulfate solutions to obtain battery-grade nickel sulfate and cobalt sulfate products. Liquid-solid ratios in the disclosure are mass ratios of liquid to solid. Further, the nickel/cobalt/manganese-based neutralizer in step (2) is one or more of mixed nickel-cobalt hydroxide, nickel hydroxide, cobalt hydroxide, nickel carbonate, cobalt carbonate, basic nickel carbonate, basic cobalt carbonate, cobalt oxide, nickel oxide, manganese hydroxide, manganese carbonate, basic manganese carbonate, and manganese oxide. Further, the precipitant in step (5) is one or more of nickel fluoride, cobalt fluoride, and manganese fluoride. Further, a dosage of the precipitant in step (5) is: a ratio of the amount of substance of fluorine in the added precipitant to the amount of substance of calcium and magnesium ions in the liquid after iron and aluminum removal is 2:1. Further, a liquid-solid ratio is controlled to be 2:1-4:1 during the slurrying with water in step (1); and specific conditions for adding the sulfuric acid for dissolution are: the sulfuric acid is added to control the pH value of the slurry to be 1.0-2.0, the dissolution temperature is 25-90°C, and the dissolution time is 1-3 h. Further, specific conditions for adding the neutralizer for reaction in step (2) are: the final pH value of the slurry is controlled to be 3.5-5.0, the reaction temperature is 25-90°C, and the reaction time is 2-5 h. Further, a liquid-solid ratio is controlled to be 3:1-4:1 during the slurrying with water in step (3); and specific conditions for adding the sulfuric acid for dissolution are: the sulfuric acid is added to control the pH value of the slurry to be 1.0-2.0, the dissolution temperature is 25-90°C, and the dissolution time is 1-3 h. Further, specific conditions for adding the calcium oxide slurry for reaction in step (4) are: the final pH value of the slurry is controlled to be 3.5-5.0, the reaction temperature is 25-90°C, and the reaction time is 2-5 h. Further, the organic phase in step (6) is composed of 10-25% P204 and sulfonated kerosene; sodium saponification is conducted by using liquid alkali, and a sodium saponification rate is %-60%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 10-30 g/L Ni2+, a scrubbing solution is 0.1-0.5 mol/L H 2 SO 4 , a stripping solution is 1.0-2.0 mol/L HCl, a Fe stripping solution is 4.5-6.0 mol/L HCl, and a chlorine scrubbing solution is 2-10 g/L H 2 SO 4
. Further, an organic phase in step (7) is composed of 10-25% P507 and sulfonated kerosene; sodium saponification is conducted by using liquid alkali, and a sodium saponification rate is %-60%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 10-30 g/L Ni2+, a scrubbing solution is 0.1-0.5 mol/L H 2 SO 4 , a stripping solution is 0.1-0.5 mol/L H 2 SO 4 , and an acid scrubbing solution is 2-10 g/L H 2 SO4
. The method provided in the disclosure involves the following reaction principles: During neutralization for iron and aluminum removal, OH- or CO 3 2 - can be decomposed from the added new precipitant in the solution system; after free H+ in the residual acid in leachate of the mixed nickel-cobalt hydroxide, namely the nickel-cobalt solution, reacts with OH or CO3 2 - in the precipitant, the amount of free H+is decreased, but the amount of OH-is increased. Fe 3+ and A13+ will form precipitate with OH-, and the following reactions occur: Fe 3 *+30H-=Fe(OH)3 1 A13++30H-=A(OH) 3 1 In this way, iron and aluminum are removed from the nickel-cobalt solution. During calcium and magnesium removal conducted by a precipitation method, fluoride ions can be decomposed from the added precipitant in the solution system. Calcium fluoride and magnesium fluoride are insoluble in water, and the fluoride ions in the precipitant are bonded with calcium and magnesium ions in a nickel-cobalt-manganese solution to form precipitate for removal. The following reactions occur in this process: 2F-+Ca 2+=CaF21 2F-+Mg 2+=MgF21 In this way, calcium and magnesium are removed from the nickel-cobalt-manganese solution. In the extraction process, an extractant is used to form an extraction complex with metal ions (Me"+) in the solution, and the extraction complex is allowed to enter an organic solvent (loaded organic). The loaded organic is mixed with a stripping solution to allow the metal ions to return back to the stripping solution. Impurity ion removal and nickel and cobalt separation are realized by using different capabilities of P204 and P507 for extracting different metal ions. The following reaction occurs during the extraction: Me"*+nHX=MeXn+nH+ Innovation points and advantages of the disclosure are as follows:
(1) During iron and aluminum removal conducted by using a new neutralizer, preferably, a raw material mixed nickel-cobalt hydroxide can be used as a neutralization reagent. This can greatly reduce (greater than 90%) a dosage of a conventional neutralizer calcium oxide , greatly reduce (greater than 90%) calcium ions introduced into the nickel-cobalt solution system , and greatly reduce (greater than 90%) losses of nickel and cobalt in the process of neutralization for iron and aluminum removal. (2) During calcium and magnesium removal conducted by using a new precipitant, no new impurity ions are introduced, which can greatly reduce the influence of calcium sulfate crystallization on P204 extraction, and simplify the operation of P507 extraction for magnesium separation. (3) The disclosure has a simple process and strong operability, and easy to implement in industry. According to another aspect of the invention there is provided a method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide, comprising the following steps: (1) acid dissolution: slurrying the mixed nickel-cobalt hydroxide with water, adding sulfuric acid for dissolution, and conducting liquid-solid separation to obtain manganese slag and a nickel-cobalt sulfate solution; (2) neutralization for iron and aluminum removal: adding a nickel/cobalt/manganese-based neutralizer to the nickel-cobalt sulfate solution obtained in step (1) for reaction, and conducting liquid-solid separation to obtain nickel-cobalt-iron-aluminum slag and liquid after iron and aluminum removal; (3) secondary acid dissolution: slurrying the nickel-cobalt-iron-aluminum slag obtained in step (2) with water, adding sulfuric acid for dissolution, and conducting liquid-solid separation to obtain manganese slag and a nickel-cobalt sulfate solution; (4) secondary neutralization for iron and aluminum removal: adding calcium oxide slurry to the nickel-cobalt sulfate solution obtained in step (3) for reaction, and conducting liquid-solid separation to obtain iron-aluminum slag and liquid after iron and aluminum removal; (5) calcium and magnesium removal: combining the liquid after iron and aluminum removal obtained in step (2) and step (4), adding a precipitant for reaction, and conducting liquid-solid separation to obtain calcium-magnesium slag and liquid after calcium and magnesium removal; (6) P204 extraction for purification: conducting P204 extraction for purification on the liquid after calcium and magnesium removal obtained in step (5) to remove copper, manganese, zinc, and calcium impurities to obtain raffinate after the P204 extraction, and recycling a loaded organic phase according to steps of stripping, Fe stripping, and chlorine scrubbing;
(7) P507 extraction for nickel and cobalt separation: conducting P507 extraction for nickel and cobalt separation on the raffinate after the P204 extraction obtained in step (6) to obtain pure nickel sulfate and cobalt sulfate solutions; and (8) evaporative crystallization: conducting evaporative crystallization on the pure nickel sulfate and cobalt sulfate solutions to obtain battery-grade nickel sulfate and cobalt sulfate products. Throughout this specification, unless the context requires otherwise, the words "comprise", "comprises" and "comprising" will be understood to imply the inclusion of a stated step or element or group of steps or elements but not the exclusion of any other step or element or group of steps or elements. BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a schematic flowchart of a process according to the disclosure. DETAILED DESCRIPTION Example 1 Main components of a mixed nickel-cobalt hydroxide intermediate product obtained by high-pressure acid leaching, neutralization for purification, and precipitation on laterite nickel ore in a foreign factory are shown in the table below. Element Ca Co Ni Cu Fe Mg Mn Si Al Zn Content/% 0.15 3.92 40.85 0.10 0.076 1.46 5.25 0.14 0.24 0.73
The mixed nickel-cobalt hydroxide was slurried with water to control its liquid-solid ratio to be 4:1. At 70°C, the pH value of the slurry was controlled to be 1.5 by adding sulfuric acid, and the slurry was dissolved for 2 h. Liquid-solid separation was conducted to obtain manganese slag and a nickel-cobalt sulfate solution. Components of the nickel-cobalt sulfate solution are shown in the table below. Element Al As Ba Be Bi Ca Cd Co Content/(g/L) 0.25 <0.001 <0.05 <0.05 <0.05 0.15 <0.001 9.09 Element Cr Cu Fe Li Mg Mn Ni Pb Content/(g/L) 0.025 0.24 0.045 <0.05 1.56 3.54 95.7 0.01 Element Sb Sn Sr Ti V Zn Content/(g/L) <0.05 <0.05 <0.05 0.033 <0.05 1.73
500 mL of the above solution was heated to 70°C, the mixed nickel-cobalt hydroxide was added to adjust the pH of the solution to 3.50, iron and aluminum removal was conducted for 3 h, and liquid-solid separation was conducted to obtain slag after iron and aluminum removal and liquid after iron removal. Main components of the liquid after iron removal are as follows:
Element Al Ca Cr Co Cu Fe Content/(g/L) 0.064 0.67 0.0152 10.45 0.28 0.0045 Element Mn Mg Ni Zn Si Na Content/(g/L) 4.69 1.80 110.22 2.63 0.041 0.03
500 mL of the above solution was heated to 70°C, 4.44 g of nickel fluoride was added according to the theoretical amount of calcium and magnesium, calcium and magnesium removal was conducted for 6 h, and liquid-solid separation was conducted to obtain calcium-magnesium slag and liquid after calcium and magnesium removal. The liquid after calcium and magnesium removal contains 0.01 g/L of calcium and 0.02 g/L of magnesium. The liquid after calcium and magnesium removal was subject to P204 extraction for purification, an organic phase was composed of 20% P204 and 80% sulfonated kerosene; sodium saponification was conducted by using 32% NaOH, and a sodium saponification rate was 60%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 20 g/L Ni 2 +, a scrubbing solution was 0.5 mol/L H 2 SO 4 , a stripping solution was 2.0 mol/L HCl, a Fe stripping solution was 6.0 mol/L HCl, and a chlorine scrubbing solution was 5 g/L H 2 SO 4 .
Raffinate obtained after the P204 extraction was subject to P507 extraction for nickel and cobalt separation, an organic phase in the P507 extraction was composed of 20% P507 and 80% kerosene; sodium saponification was conducted by using 32% NaOH, and a sodium saponification rate was 30%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 20 g/L Ni 2+, a scrubbing solution was 0.1 mol/L H 2 SO 4 , a stripping solution was 0.5 mol/L H 2 SO 4 , and an acid scrubbing solution was 5 g/L H 2 SO4 . Nickel sulfate and cobalt sulfate solutions were obtained, subject to evaporative crystallization, washed, and dried to obtain battery-grade nickel sulfate and cobalt sulfate products. Example 2 A mixed nickel-cobalt hydroxide intermediate product obtained by high-pressure acid leaching, neutralization for purification, and precipitation on laterite nickel ore in a foreign factory contains water 65%, and contains Ni 35.0%, Co 4.0% and Mn 5.13% on a dry basis. The mixed nickel-cobalt hydroxide was slurried with water to control its liquid-solid ratio to be 3.8:1. At 25°C, the pH value of the slurry was controlled to be 2.0 by adding sulfuric acid, and the slurry was dissolved for 3 h. Liquid-solid separation was conducted to obtain manganese slag and a nickel-cobalt sulfate solution. Components of the nickel-cobalt sulfate solution are shown in the table below.
Element Al Ca Mn Ni Co Mg Content/(g/L) 0.29 0.22 3.36 97.6 8.29 2.0
500 mL of the above solution was heated to 90°C, cobalt hydroxide was added to adjust the pH of the solution to 3.50, iron and aluminum removal was conducted for 3 h, and liquid-solid separation was conducted to obtain slag after iron and aluminum removal and liquid after iron removal. Main components of the liquid after iron removal are as follows: Element Al Ca Fe Mn Ni Co Mg Content/(g/L) 0.034 0.23 <0.001 3.36 98.2 8.35 2.0
500 mL of the above solution was heated to 70°C, 1.50 g of nickel fluoride was added according to the theoretical amount of calcium and magnesium, calcium and magnesium removal was conducted for 3 h, and liquid-solid separation was conducted to obtain calcium-magnesium slag and liquid after calcium and magnesium removal. The liquid after calcium and magnesium removal contains 0.08 g/L of calcium and 0.01 g/L of magnesium. The liquid after calcium and magnesium removal was subject to P204 extraction for purification, an organic phase was composed of 15% P204 and 85% sulfonated kerosene; sodium saponification was conducted by using 32% NaOH, and a sodium saponification rate was 50%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 10 g/L Ni 2 +, a scrubbing solution was 0.35 mol/L H 2 SO 4 , a stripping solution was 1.5 mol/L HCl, a Fe stripping solution was 5.0 mol/L HCl, and a chlorine scrubbing solution was 8 g/L H 2 SO 4 .
Raffinate obtained after the P204 extraction was subject to P507 extraction for nickel and cobalt separation, an organic phase in the P507 extraction was composed of 15% P507 and 85% kerosene; sodium saponification was conducted by using 32% NaOH, and a sodium saponification rate was 35%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 10 g/L Ni 2+, a scrubbing solution was 0.2 mol/L H 2 SO 4 , a stripping solution was 0.35 mol/L H 2 SO 4 , and an acid scrubbing solution was 8 g/L H 2 SO 4 .
Nickel sulfate and cobalt sulfate solutions were obtained, subject to evaporative crystallization, washed, and dried to obtain battery-grade nickel sulfate and cobalt sulfate products. Example 3 A mixed nickel-cobalt hydroxide intermediate product obtained by high-pressure acid leaching, neutralization for purification, and precipitation on laterite nickel ore in a foreign factory contains water 63.5%, and contains Ni 32.0%, Co 3.8% and Mn 4.62% on a dry basis. The mixed nickel-cobalt hydroxide was slurried with water to control its liquid-solid ratio to be
3.5:1. At 90°C, the pH value of the slurry was controlled to be 1.0 by adding sulfuric acid, and the slurry was dissolved for 1 h. Liquid-solid separation was conducted to obtain manganese slag and a nickel-cobalt sulfate solution. Components of the nickel-cobalt sulfate solution are shown in the table below. Element Al Ca Mn Ni Co Mg Content/(g/L) 0.64 0.36 6.23 90.6 10.83 1.86
500 mL of the above solution was heated to 60°C, nickel carbonate was added to adjust the pH of the solution to 3.50, iron and aluminum removal was conducted for 4.0 h, and liquid-solid separation was conducted to obtain slag after iron and aluminum removal and liquid after iron removal. Main components of the liquid after iron removal are as follows: Element Al Ca Fe Mn Ni Co Mg Content/(g/L) 0.04 0.42 <0.001 6.36 93.9 10.83 1.80
500 mL of the above solution was heated to 60°C, 2.80 g of nickel fluoride was added according to the theoretical amount of calcium and magnesium, calcium and magnesium removal was conducted for 4 h, and liquid-solid separation was conducted to obtain calcium-magnesium slag and liquid after calcium and magnesium removal. The liquid after calcium and magnesium removal contains 0.05 g/L of calcium and 0.06 g/L of magnesium. The liquid after calcium and magnesium removal was subject to P204 extraction for purification, an organic phase was composed of 25% P204 and 75% sulfonated kerosene; sodium saponification was conducted by using 32% NaOH, and a sodium saponification rate was 40%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 15 g/L Ni 2 +, a scrubbing solution was 0.5 mol/L H 2 SO 4 , a stripping solution was 2.0 mol/L HCl, a Fe stripping solution was 4.5 mol/L HCl, and a chlorine scrubbing solution was 10 g/L H 2 SO 4 .
Raffinate obtained after the P204 extraction was subject to P507 extraction for nickel and cobalt separation, an organic phase in the P507 extraction was composed of 25% P507 and 75% kerosene; sodium saponification was conducted by using 32% NaOH, and a sodium saponification rate was 40%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 15 g/L Ni 2+, a scrubbing solution was 0.5 mol/L H 2 SO 4 , a stripping solution was 0.5 mol/L H 2 SO 4 , and an acid scrubbing solution was 10 g/L H 2 SO 4 .
Nickel sulfate and cobalt sulfate solutions were obtained, subject to evaporative
crystallization, washed, and dried to obtain battery-grade nickel sulfate and cobalt sulfate products.

Claims (5)

  1. What is claimed is: 1. A method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide, comprising the following steps: (1) acid dissolution: slurrying the mixed nickel-cobalt hydroxide with water, adding sulfuric acid for dissolution, and conducting liquid-solid separation to obtain manganese slag and a nickel-cobalt sulfate solution; (2) neutralization for iron and aluminum removal: adding a nickel/cobalt/manganese-based neutralizer to the nickel-cobalt sulfate solution obtained in step (1) for reaction, and conducting liquid-solid separation to obtain nickel-cobalt-iron-aluminum slag and liquid after iron and aluminum removal; (3) secondary acid dissolution: slurrying the nickel-cobalt-iron-aluminum slag obtained in step (2) with water, adding sulfuric acid for dissolution, and conducting liquid-solid separation to obtain manganese slag and a nickel-cobalt sulfate solution; (4) secondary neutralization for iron and aluminum removal: adding calcium oxide slurry to the nickel-cobalt sulfate solution obtained in step (3) for reaction, and conducting liquid-solid separation to obtain iron-aluminum slag and liquid after iron and aluminum removal; (5) calcium and magnesium removal: combining the liquid after iron and aluminum removal obtained in step (2) and step (4), adding a precipitant for reaction, and conducting liquid-solid separation to obtain calcium-magnesium slag and liquid after calcium and magnesium removal; (6) P204 extraction for purification: conducting P204 extraction for purification on the liquid after calcium and magnesium removal obtained in step (5) to remove copper, manganese, zinc, and calcium impurities to obtain raffinate after the P204 extraction, and recycling a loaded organic phase according to steps of stripping, Fe stripping, and chlorine scrubbing; (7) P507 extraction for nickel and cobalt separation: conducting P507 extraction for nickel and cobalt separation on the raffinate after the P204 extraction obtained in step (6) to obtain pure nickel sulfate and cobalt sulfate solutions; and (8) evaporative crystallization: conducting evaporative crystallization on the pure nickel sulfate and cobalt sulfate solutions to obtain battery-grade nickel sulfate and cobalt sulfate products.
  2. 2. The method according to claim 1, wherein the nickel/cobalt/manganese-based neutralizer in step (2) is one or more of mixed nickel-cobalt hydroxide, nickel hydroxide, cobalt hydroxide, nickel carbonate, cobalt carbonate, basic nickel carbonate, basic cobalt carbonate, cobalt oxide, nickel oxide, manganese hydroxide, manganese carbonate, basic manganese carbonate, and manganese oxide.
  3. 3. The method according to claim 1 or 2, wherein the precipitant in step (5) is one or more of nickel fluoride, cobalt fluoride, and manganese fluoride; wherein a dosage of the precipitant in step (5) is: a ratio of the amount of substance of fluorine in the added precipitant to the amount of substance of calcium and magnesium ions in the liquid after iron and aluminum removal is 2:1; wherein a liquid-solid ratio is controlled to be 2:1-4:1 during the slurrying with water in step (1); and specific conditions for adding the sulfuric acid for dissolution are: the sulfuric acid is added to control the pH value of the slurry to be 1.0-2.0, the dissolution temperature is 25-90°C, and the dissolution time is 1-3 h; wherein specific conditions for adding the neutralizer for reaction in step (2) are: the final pH value of the slurry is controlled to be 3.5-5.0, the reaction temperature is 25-90°C, and the reaction time is 2-5 h; wherein a liquid-solid ratio is controlled to be 3:1-4:1 during the slurrying with water in step (3); and specific conditions for adding the sulfuric acid for dissolution are: the sulfuric acid is added to control the pH value of the slurry to be 1.0-2.0, the dissolution temperature is 25-90°C, and the dissolution time is 1-3 h; and wherein specific conditions for adding the calcium oxide slurry for reaction in step (4) are: the final pH value of the slurry is controlled to be 3.5-5.0, the reaction temperature is 25-90°C, and the reaction time is 2-5 h.
  4. 4. The method according to claim 1, wherein the organic phase in step (6) is composed of -25% P204 and sulfonated kerosene; sodium saponification is conducted by using liquid alkali, and a sodium saponification rate is 30%-60%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 10-30 g/L Ni 2 +, a scrubbing solution is 0.1-0.5 mol/L H 2 SO 4 , a stripping solution is 1.0-2.0 mol/L HCl, a Fe stripping solution is 4.5-6.0 mol/L HCl, and a chlorine scrubbing solution is 2-10 g/L H 2 SO 4 .
  5. 5. The method according to claim 1, wherein an organic phase in step (7) is composed of -25% P507 and sulfonated kerosene; sodium saponification is conducted by using liquid alkali, and a sodium saponification rate is 30%-60%; and a sodium saponified organic is subject to nickel saponification by using a nickel sulfate solution with 10-30 g/L Ni 2 +, a scrubbing solution is 0.1-0.5 mol/L H 2 SO 4 , a stripping solution is 0.1-0.5 mol/L H 2 SO 4 , and an acid scrubbing solution is 2-10 g/L H 2 SO 4 .
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