CN111004926A - Method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin - Google Patents
Method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin Download PDFInfo
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- CN111004926A CN111004926A CN201811165958.0A CN201811165958A CN111004926A CN 111004926 A CN111004926 A CN 111004926A CN 201811165958 A CN201811165958 A CN 201811165958A CN 111004926 A CN111004926 A CN 111004926A
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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
- 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
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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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
- C22B23/00—Obtaining nickel or cobalt
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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
- C22B3/20—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
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- 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
Abstract
The method for extracting nickel and cobalt from the low-grade laterite-nickel ore leaching solution by using resin comprises the following steps of: (1) adsorbing the low-grade laterite-nickel ore leaching solution by a copper-removing resin column to obtain a copper-removed solution; (2) adsorbing the solution after copper removal by a nickel-cobalt extraction resin column, washing the nickel-cobalt extraction resin column after saturated adsorption by water, and desorbing the nickel-cobalt extraction resin column after washing to obtain a first solution; (3) and adsorbing the first solution by a purification impurity-removal resin column to obtain a nickel sulfate and cobalt sulfate enriched solution. The method can selectively and directly separate and enrich valuable metal nickel-cobalt products from the multi-metal leaching solution with complex components, has simple process, mild reaction and cleaner production environment, can realize low-carbon, environment-friendly and clean production, has lower energy consumption and is easy to realize large-scale production.
Description
Technical Field
The invention belongs to the technical field of wet metallurgy, and particularly relates to a method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by using resin.
Background
With increasing attention on environmental control, the resin ion exchange technology is rapidly developing and playing a great role in the fields of science and technology and production in China. However, the domestic application of resin ion exchange technology has been limited to power plant water treatment, sewage treatment and pharmaceutical industry. The main reasons why the resin ion exchange technology cannot be applied to hydrometallurgy on a large scale are that: the majority of ion exchange resins currently used in the world are organic ion exchange resins with a styrene or acrylic acid polymer as a framework, and the following defects generally exist in the performance of the ion exchange resins: the method has the advantages of small exchange capacity, low exchange speed, short cycle, high water content, high transformation expansion rate and the like, and particularly has the defect of poor selectivity of ion exchange, so that the method cannot be applied to the industrialization of separating and enriching valuable metals in multi-metal acid leachate with very complex components.
In the wet acid leaching process of the laterite-nickel ore, the main product is nickel hydroxide cobalt generated by neutralization reaction, and the mass percentage of other metal impurities contained in the qualified nickel hydroxide cobalt product (nickel is 40%) in the current market is about 20%, so the market price is not high; meanwhile, with the huge change of the global energy utilization pattern at present, the demand of the high-purity nickel-cobalt product in the new energy field, especially the fields of movable equipment, new energy automobiles and the like is increasing day by day, and the high-purity nickel-cobalt product has huge market potential. Based on the current situation, how to simply and efficiently separate and extract high-purity and low-impurity nickel and cobalt from the leaching solution becomes a difficult point and a key point for processing the laterite-nickel ore by a wet method.
Disclosure of Invention
The invention provides a method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin, aiming at the problems and the defects in the existing laterite-nickel ore hydrometallurgy technology.
The invention adopts the following technical scheme:
a method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by using resin is characterized by comprising the following steps:
(1) adsorbing the low-grade laterite-nickel ore leaching solution by a copper-removing resin column to obtain a copper-removed solution;
(2) adsorbing the solution after copper removal by a nickel cobalt extraction resin column, washing the nickel cobalt extraction resin column after saturated adsorption by water, and desorbing the nickel cobalt extraction resin column after washing to obtain a first solution;
(3) and adsorbing the first solution by a purification impurity-removal resin column to obtain a nickel sulfate and cobalt sulfate enriched solution.
The method is characterized in that the copper-removing resin column after adsorption saturation is washed by water in the step (1), the copper-removing resin column is desorbed after washing to obtain a second solution, and the copper-removing resin column is washed again after desorption.
According to the method, the copper removal resin column is desorbed by adopting 35-50% by mass of sulfuric acid solution or concentrated hydrochloric acid to obtain copper sulfate enriched solution or copper chloride enriched solution.
According to the method, the copper removal resin column adopts inorganic silicon resin Si-Cu to remove copper ions in the low-grade laterite-nickel ore leaching solution.
According to the method, the nickel cobalt extraction resin column adopts inorganic silicon resin Si-2 to adsorb the nickel cobalt in the copper-removed solution.
According to the method, the nickel-cobalt extraction resin column is desorbed by adopting 35-50% by mass of sulfuric acid solution or concentrated hydrochloric acid to obtain nickel sulfate enriched solution and cobalt sulfate enriched solution or nickel chloride enriched solution and cobalt chloride enriched solution.
The method as described above, characterized in that the nickel cobalt extraction resin column is subjected to desorption and then to water washing again.
The method is characterized in that the water washing process of the nickel cobalt extraction resin column adopts six stages of countercurrent washing.
The invention has the beneficial technical effects that: the Si series inorganic ion exchange resin product with silica gel as a framework adopted by the invention can form a very stable chelate for various heavy metals, can selectively enrich metal ions such as copper, cobalt, nickel and the like from water containing a large amount of harmless alkali metals such as calcium, magnesium, potassium, sodium and the like, and alkaline earth metals, has a long service life, and can be expected to fundamentally solve the problems of organic resin in hydrometallurgy application; the invention mainly adopts three-stage process: carrying out resin decoppering on the low-grade laterite-nickel ore leaching solution, carrying out resin enrichment on the leaching solution subjected to decoppering to extract nickel and cobalt, and further purifying the obtained nickel and cobalt enriched solution to remove impurities, wherein the obtained product can be directly used as a production raw material of a ternary precursor of a battery material; the method has the advantages of simple process, mild reaction, cleaner production environment, low carbon, environmental protection and cleaner production, low energy consumption and easy realization of large-scale production.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Referring to fig. 1, the method for extracting nickel and cobalt from the low-grade laterite-nickel ore leaching solution by using resin comprises the following steps: (1) pumping the low-grade laterite-nickel ore leaching solution into a copper removal resin column for adsorption at a flow rate of 4BV/h-6BV/h (V represents the effective volume of the resin column) by a liquid inlet pump to obtain a copper removal solution, preferably, removing copper ions in the low-grade laterite-nickel ore leaching solution by the copper removal resin column by adopting inorganic silicon resin Si-Cu; after the copper-removing resin column is adsorbed and saturated, carrying out first washing on the copper-removing resin column by adopting 3BV deionized water, wherein the washing flow rate is 4BV/h-6 BV/h; desorbing the copper-removing resin column after washing to obtain a second solution, preferably, desorbing the copper-removing resin column by using 35-50% by mass of sulfuric acid solution or concentrated hydrochloric acid to obtain copper sulfate enriched solution or copper chloride enriched solution; and after desorption, washing the copper-removing resin column for the second time by adopting 6BV deionized water, wherein the washing flow rate is 6BV/h-8 BV/h. (2) Adsorbing the solution after copper removal by a nickel-cobalt extraction resin column, preferably, adsorbing the nickel and cobalt in the solution after copper removal by the nickel-cobalt extraction resin column by adopting inorganic silicon resin Si-2, wherein the adsorption flow rate is 4BV/h-6 BV/h; after the nickel cobalt extraction resin column is adsorbed and saturated, carrying out first six-stage countercurrent washing on the nickel cobalt extraction resin column by adopting 3BV deionized water, wherein the washing flow rate is 4BV/h-6 BV/h; the method comprises the following steps of (1) desorbing a nickel-cobalt extraction resin column after washing to obtain a first solution, preferably, desorbing the nickel-cobalt extraction resin column by using 35-50% by mass of sulfuric acid solution or concentrated hydrochloric acid to obtain nickel sulfate enriched solution and cobalt sulfate enriched solution or nickel chloride enriched solution and cobalt chloride enriched solution, wherein when the sulfuric acid solution is used as a desorption agent, the obtained nickel sulfate enriched solution and cobalt sulfate enriched solution can be directly used as production raw materials of a ternary precursor of a battery material, when the concentrated hydrochloric acid is used as the desorption agent, the nickel sulfate enriched solution and cobalt chloride enriched solution can be converted into nickel chloride enriched solution and cobalt chloride enriched solution with higher purity, and nickel oxide and cobalt oxide products with higher purity are obtained after high-temperature calcination; and after desorption, 6BV of deionized water is adopted to carry out secondary six-stage countercurrent washing on the nickel-cobalt extraction resin column, and the washing flow rate is 6BV/h-8 BV/h. (3) And adsorbing the first solution by a deep purification impurity removal resin column to obtain a nickel-cobalt enriched solution, wherein the adsorption flow rate is 4BV/h-6 BV/h.
The invention is further illustrated by the following specific examples. The elements and their concentrations in the low-grade lateritic nickel ore leachate used in the following examples are referred to table 1.
Table 1 elements and their concentrations in low grade laterite-nickel ore leaching liquor
Example 1
Measuring 200mL of low-grade laterite-nickel ore leaching solution 1, pumping the low-grade laterite-nickel ore leaching solution into an inorganic silicon resin Si-Cu column with the diameter phi of 30mm multiplied by 290mm at the flow rate of 4BV/h through a peristaltic pump for solution adsorption, stopping adsorption when the color of the solution in a liquid outlet pipe above the inorganic silicon resin Si-Cu column is basically consistent with that of the stock solution, and obtaining the solution with less than 0.001g/L of copper after adsorption after copper removal. Pumping the solution after copper removal into a phi 30mm multiplied by 240mm inorganic silicon resin Si-2 column for solution adsorption through a peristaltic pump at the flow rate of 4BV/h, performing first six-stage countercurrent washing on the inorganic silicon resin Si-2 column by using 480mL deionized water at the flow rate of 4BV/h after adsorption, and desorbing the inorganic silicon resin Si-2 column by using 35 mass percent of sulfuric acid solution after washing to obtain a first solution, wherein the desorption flow rate is 3 BV/h; after all the desorption agent enters the inorganic silicon resin Si-2 column, 960mL deionized water is used for carrying out secondary six-stage countercurrent washing on the inorganic silicon resin Si-2 column, and the washing flow rate is 4 BV/h. The first solution contains 17.5g/L of nickel, 0.35g/L of cobalt, 0.018g/L of iron, 0.013g/L of zinc and less than 0.001g/L of other impurity elements, the first solution is pumped into a purification and impurity removal resin column with the diameter of phi 30mm multiplied by 240mm for adsorption, 17.2g/L of nickel, 0.34g/L of cobalt and less than 0.001g/L of other impurities such as Fe, Zn, Ca, Mg, Cu, Pb and Na are contained in the adsorbed solution.
Example 2
Measuring 15L of low-grade laterite-nickel ore lixivium 1, pumping into an inorganic silicon resin Si-Cu column with phi 138mm multiplied by 1000mm at a flow rate of 5BV/h through a peristaltic pump for solution adsorption, stopping adsorption when the color of the solution in a liquid outlet pipe above the inorganic silicon resin Si-Cu column is basically consistent with that of the stock solution, and obtaining a solution with less than 0.001g/L of copper after adsorption after copper removal. Pumping the solution after copper removal into an inorganic silicon resin Si-2 column with the diameter of 89mm multiplied by 1000mm at the flow rate of 5BV/h through a peristaltic pump for solution adsorption, performing first six-stage countercurrent washing on the inorganic silicon resin Si-2 column by using 15L of deionized water at the flow rate of 5BV/h after adsorption, and desorbing the inorganic silicon resin Si-2 column by using a sulfuric acid solution with the mass percentage of 35% after washing to obtain a first solution, wherein the desorption flow rate is 3 BV/h; and after all the desorption agent enters the inorganic silicon resin Si-2 column, performing secondary six-stage countercurrent washing on the inorganic silicon resin Si-2 column by using 30L of deionized water, wherein the washing flow rate is 5 BV/h. The first solution contains 21.56g/L of nickel, 0.43g/L of cobalt, 0.053g/L of iron, 0.026g/L of zinc and less than 0.001g/L of other impurity elements, the first solution is pumped into a purification and impurity removal resin column with the diameter of 89mm multiplied by 1000mm for adsorption, 21.37g/L of nickel, 0.45g/L of cobalt and less than 0.001g/L of other impurities of Fe, Zn, Ca, Mg, Cu, Pb and Na are contained in the adsorbed solution.
Example 3
Measuring 100L of low-grade laterite-nickel ore lixivium 2, pumping into an inorganic silicon resin Si-Cu column with the diameter of 300mm multiplied by 2000mm at the flow rate of 6BV/h by a liquid inlet pump for solution adsorption, stopping adsorption when the color of the solution in a liquid outlet pipe above the inorganic silicon resin Si-Cu column is basically consistent with that of the stock solution, and obtaining the solution with less than 0.001g/L of copper after copper is removed after adsorption. Pumping the solution after copper removal into a phi 300mm multiplied by 2000mm inorganic silicon resin Si-2 column for solution adsorption at the flow rate of 6BV/h through a peristaltic pump, performing first six-stage countercurrent washing on the inorganic silicon resin Si-2 column by using 300L of deionized water at the flow rate of 6BV/h after adsorption, and desorbing the inorganic silicon resin Si-2 column by using 35 mass percent of sulfuric acid solution after washing to obtain a first solution, wherein the desorption flow rate is 3 BV/h; and after all the desorption agent enters the inorganic silicon resin Si-2 column, performing second six-stage countercurrent washing on the inorganic silicon resin Si-2 column by using 600L of deionized water, wherein the washing flow rate is 6 BV/h. The first solution contains 27.28g/L of nickel, 0.54g/L of cobalt, 0.062g/L of iron, 0.092g/L of zinc and less than 0.001g/L of other impurity elements, the first solution is pumped into a purification and impurity removal resin column with the diameter of 300mm multiplied by 1000mm for adsorption, 27.26g/L of nickel, 0.53g/L of cobalt and less than 0.001g/L of other impurities such as Fe, Zn, Ca, Mg, Cu, Pb and Na are contained in the adsorbed solution.
Claims (8)
1. A method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by using resin is characterized by comprising the following steps:
(1) adsorbing the low-grade laterite-nickel ore leaching solution by a copper-removing resin column to obtain a copper-removed solution;
(2) adsorbing the solution after copper removal by a nickel cobalt extraction resin column, washing the nickel cobalt extraction resin column after saturated adsorption by water, and desorbing the nickel cobalt extraction resin column after washing to obtain a first solution;
(3) and adsorbing the first solution by a purification impurity-removal resin column to obtain a nickel sulfate and cobalt sulfate enriched solution.
2. The method according to claim 1, wherein the copper removal resin column after adsorption saturation is washed with water in step (1), the copper removal resin column is desorbed after washing to obtain a second solution, and the copper removal resin column is washed with water again after desorption.
3. The method according to claim 2, wherein the copper removal resin column is desorbed by 35-50% by mass of a sulfuric acid solution or concentrated hydrochloric acid to obtain a copper sulfate-rich solution or a copper chloride-rich solution.
4. The method according to the claim 1, characterized in that the decoppering resin column removes copper ions from the low-grade lateritic nickel ore leachate using inorganic silicon resin Si-Cu.
5. The method of claim 1, wherein the nickel cobalt extraction resin column adsorbs nickel cobalt in the copper-removed solution with inorganic silicone Si-2.
6. The method according to claim 1, wherein the nickel cobalt extraction resin column is desorbed by 35-50% by mass of a sulfuric acid solution or concentrated hydrochloric acid to obtain a nickel sulfate-rich solution and a cobalt sulfate-rich solution or a nickel chloride-rich solution and a cobalt chloride-rich solution.
7. The method of claim 1 wherein the nickel cobalt extraction resin column is stripped and then washed again with water.
8. The method of claim 1 wherein the water wash of the nickel cobalt extraction resin column employs six counter current washes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811165958.0A CN111004926A (en) | 2018-10-08 | 2018-10-08 | Method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin |
| PCT/CN2018/114822 WO2020073410A1 (en) | 2018-10-08 | 2018-11-09 | Method for resin extraction of nickel and cobalt from low-grade laterite nickel ore leaching liquid |
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| CN201811165958.0A CN111004926A (en) | 2018-10-08 | 2018-10-08 | Method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin |
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| CN112403029A (en) * | 2020-11-18 | 2021-02-26 | 鸣洋(武汉)化工工程有限公司 | Novel resin decoppering process flow |
| CN113061748A (en) * | 2021-03-12 | 2021-07-02 | 中国恩菲工程技术有限公司 | Laterite nickel ore leaching liquid treatment system and method |
| CN113293293A (en) * | 2021-05-26 | 2021-08-24 | 中国恩菲工程技术有限公司 | Method for recovering nickel and cobalt from laterite-nickel ore by resin adsorption method |
| CN113512650A (en) * | 2021-05-27 | 2021-10-19 | 金川集团股份有限公司 | Method for efficiently recovering metal cobalt from wet-process smelting tailings of copper oxide cobalt ores |
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