Method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine

Through acid dissolution, chelation and precipitant, the nickel-cobalt ions are separated, combined with the solution crystallization and calcination steps, the problem of separation of nickel-cobalt ions in high-magnesium and low-nickel cobalt solutions is solved, and high-purity basic magnesium carbonate and high-grade nickel fine powder are prepared, achieving efficient utilization of resources and environmentally friendly treatment.

CN120483201APending Publication Date: 2025-08-15SHAANXI SCI TECH UNIV +1
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Patent Information

Application Number
CN202510794743.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-14
Publication Date
2025-08-15

AI Technical Summary

Technical Problem

The prior art is difficult to efficiently separate and enrich nickel cobalt ions in high-magnesium and low-nickel cobalt solutions, resulting in low purity of magnesium salt products and lower economic benefits, and traditional methods have risks of environmental pollution.

Method used

The serpentine is thoroughly acidic and released nickel and cobalt ions, and then the magnesium ions are separated by precipitant, combined with solution crystallization and calcination steps to prepare high-sodium magnesium carbonate and enrich nickel ions.

Benefits of technology

It realizes efficient separation of nickel-cobalt ions and magnesium salts, and prepares high-purity alkaline magnesium carbonate and high-grade nickel fine powder, with high resource utilization, no waste emissions, and simple environmental protection operation.

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Abstract

The invention relates to the technical field of hydrometallurgy, in particular to a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions. According to the method, serpentine is subjected to thorough acidolysis, and nickel and magnesium in ore are efficiently released; after ions such as nickel and cobalt in the high-magnesium low-nickel salt solution obtained through acidolysis are complexed with a chelating agent, magnesium ions in the solution are all converted into solids through a precipitator, and separation of magnesium salt solids and nickel ions is achieved; the ammonium salt in the solution is recovered by continuously using the solution crystallization method; and finally, the residual nickel-rich solution is concentrated / dried / calcined, and high-grade nickel fine powder is obtained. The method has the advantages of being simple in process, convenient to operate, high in yield, environmentally friendly, free of emission of three wastes and the like.
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Description

Technical Field

[0001] The present invention relates to the technical field of metallurgical processes, and in particular to a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions. Background Art

[0002] China has a massive accumulation of asbestos tailings, primarily concentrated in western China. For example, the Xinkang Asbestos Mine Tailings Pond and the Sichuan Asbestos Mine Tailings Pond in Shimian County, Sichuan, have a total reserve of 41.958 million cubic meters. The accumulated volume of asbestos tailings in Aksai County, Gansu, has reached over 100 million tons, primarily from nearly half a century of mining in the Hongliugou mining area. Western mining areas (such as Mangya in Qinghai and Bazhong in Xinjiang) generate over 7.5 million tons of tailings annually, bringing the cumulative volume to tens of millions of tons.

[0003] Asbestos tailings contain asbestos fibers, magnesium, silicon, iron, and other components. Long-term accumulation occupies land. Asbestos fibers are classified as a Class I carcinogen by the World Health Organization, and are known to cause diseases such as asbestosis and pleural mesothelioma. Tailings dust spreads and contaminates surrounding water sources and soil, posing a threat to local residents and the ecosystem. Tailings are rich in recoverable components like magnesium, silicon, and iron, as well as high-value elements like nickel and cobalt. However, traditional disposal methods (such as landfilling or inefficient utilization) result in a waste of resources.

[0004] There are many comprehensive development and utilization processes for serpentine ores, among which chemical processes are one of the best ways to realize their value. Taking the sulfuric acid hydrolysis of serpentine as an example, the trace elements nickel, cobalt and magnesium in the hydrolysis solution coexist in the same solution. The characteristics of this hydrolysis solution are that the price of magnesium salts is low, but the content is extremely high; while the content of high-value nickel and cobalt is extremely low (less than 1% in total). Only by taking into account the efficient recovery of magnesium salts and nickel, chromium and cobalt can the comprehensive utilization of asbestos tailings be achieved. Therefore, separating and enriching high-value nickel and cobalt (II) ions from high-magnesium and low-nickel and cobalt solutions has always been an important process link in hydrometallurgy, and it is also a key step in improving the quality of magnesium sulfate.

[0005] The existing processes for removing nickel and cobalt ions from magnesium sulfate solutions mainly include chemical precipitation, extraction, and ion exchange.

[0006] Chemical precipitation is a common and effective method for removing metal ions. For nickel and cobalt ions in magnesium sulfate solution, the pH value of the solution or the amount of sodium sulfide or fluoride used can be adjusted to form a water-insoluble precipitate. However, in a high-magnesium, low-nickel-cobalt solution, it is difficult to achieve precise control of the complete separation of the two. The magnesium salt product is often not pure enough (90-97%) and the color is not white, which leads to low product value and decreased economic benefits. Patent CN112095013B uses fluoride to remove calcium and magnesium ions from nickel and cobalt solutions. It can deeply remove calcium and magnesium ions, but fluoride is expensive and poses an environmental threat.

[0007] Ion exchange method: The ion exchange method uses the selective adsorption capacity of ion exchange resin to adsorb nickel and cobalt ions in wastewater onto the resin, and then separates these metal ions from the resin through appropriate eluents. This method has the advantages of simple operation, good treatment effect, and easy automation. The disadvantage is that the resin is relatively expensive, and while the resin adsorbs nickel and cobalt ions, it also adsorbs a certain proportion of magnesium ions, resulting in the loss of magnesium ions. At the same time, a large amount of eluent is required, which brings certain pollution to the environment; and the adsorption and elution process is slow and time-consuming, which increases production costs. For related technologies, see patents CN108179272A, CN102994778A, etc.

[0008] Solvent extraction: Solvent extraction utilizes an organic solvent in contact with an aqueous phase containing metal ions, selectively extracting metal ions based on the differences in the partition coefficients of different substances between the two phases. For nickel and cobalt in magnesium sulfate solutions, suitable extractants and organic solvents can be selected to transfer them from the aqueous phase to the organic phase through the extraction process. The advantages of solvent extraction are high selectivity for metal ions, strong processing capacity, and ease of continuous operation. However, this method also has some limitations, such as the selection and recovery of the extractant, consumption of the organic solvent, and pollution. Furthermore, for high-magnesium, low-nickel-cobalt solutions, the cost of extracting nickel and cobalt with organic extractants is too high. Related technologies can be found in patents CN109797294A, CN112481489A, and CN108179272A. Summary of the Invention

[0009] The technical problem to be solved by the present invention is to address the deficiencies of the above-mentioned prior art and provide a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions. The method comprises the following steps: thoroughly acid-lyzing the serpentine to efficiently release nickel and magnesium in the ore; complexing nickel, cobalt and other ions in the high-magnesium, low-nickel salt solution obtained by acid hydrolysis with a chelating agent; then using a precipitant to convert all magnesium ions in the solution into solids to achieve separation of magnesium salt solids and nickel ions; and continuously recovering ammonium salts in the solution by a solution crystallization method; and finally concentrating / drying / calcining the residual nickel-rich solution to obtain high-grade nickel concentrate.

[0010] The present invention provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, comprising the following steps:

[0011] S1. pulverize nickel-containing serpentine ore, calcine the ore, and obtain a powder;

[0012] S2. Add the powder obtained in S1 to distilled water while stirring to prepare a slurry, then add an inorganic acid for acid hydrolysis, and then centrifuge to obtain a magnesium salt-rich solution and acid-hydrolyzed silica;

[0013] S3, adding a neutralizing agent to the magnesium salt solution obtained in S2, adjusting the pH value, separating after aging, washing the precipitate, and obtaining a low-nickel magnesium sulfate solution;

[0014] S4, take the low-nickel magnesium sulfate solution obtained in S3, add ammonium carbonate solution thereto, wait until the magnesium ions are completely precipitated, fully wash and then dry to obtain basic magnesium carbonate;

[0015] S5, taking the low-nickel magnesium sulfate solution obtained in S3, adding a chelating agent thereto, and stirring thoroughly to obtain a high-magnesium solution;

[0016] S6, adding a precipitant to the high-magnesium solution obtained in S5 to completely precipitate the magnesium ions, and drying to obtain a precipitated product and a residual solution containing a nickel-cobalt complex;

[0017] S7. Concentrate and crystallize the residual liquid containing the nickel-cobalt complex prepared in S6 to obtain ammonium sulfate crystals, evaporate and dry the residual liquid, and calcine to obtain nickel concentrate.

[0018] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the crushing instrument in S1 is a Raymond mill, the mesh size after crushing is 200-300 mesh, the calcination temperature is 500-700°C, and the calcination time is 0.5h.

[0019] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the inorganic acid in S2 is H2SO4 or HCl. When the inorganic acid is H2SO4, the mass volume ratio of the powder, distilled water and inorganic acid is 0.361kg:1800mL:360mL; when the inorganic acid is HCl, the mass volume ratio of the powder, distilled water and inorganic acid is 0.358kg:1500mL:700mL; the concentration of the inorganic acid is 12mol / L, the leaching temperature of the acidolysis is 90°C, the leaching time of the acidolysis is 0.5-3h, the solution for washing the solid residue is distilled water, the centrifugal speed is 5000r / min, and the centrifugal time is 10min.

[0020] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the neutralizer in S3 is any one of magnesium oxide, basic magnesium carbonate, magnesium hydroxide or basic basic magnesium carbonate, or a combination of two or more thereof, the pH value is adjusted to 5 to 7, the aging time is 1 hour, and the solution for washing the precipitate is distilled water.

[0021] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the amount of the ammonium carbonate solution in S4 is 1 to 5 times the nickel ion content in the low-nickel magnesium sulfate solution, and the concentration of the ammonium carbonate solution is 2.0 mol / L.

[0022] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the volume ratio of the low-nickel magnesium sulfate solution and the chelating agent in S5 is 200 mL: 0.10-0.20 mL, the chelating agent in S5 is any one of ethylenediamine, salicylic acid, o-phenanthroline or amino acid, and the stirring time is 0.5 h.

[0023] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the precipitant in S6 is an ammonium carbonate solution, the precipitated product is magnesium carbonate, the residual liquid is an ammonium sulfate solution, the concentration of the ammonium carbonate solution is 2.0 mol / L, and the amount of the ammonium carbonate solution is 159.4 mL.

[0024] According to the method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine provided by the present invention, the evaporation temperature in S7 is 120° C., the calcination temperature is 850° C., and the calcination time is 2 h.

[0025] Compared with the prior art, the present invention has the following advantages:

[0026] The present invention provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions. By using a complex compound and nickel-cobalt ions to form complexes, the method achieves efficient separation of nickel-cobalt ions from magnesium salts. The method has the advantages of being simple, easy to operate, high in yield, environmentally friendly, and eliminating the discharge of three wastes. The basic magnesium carbonate prepared by the present invention has high purity and a nickel ion content of less than 0.1 μg / g. The nickel ion-enriched solution can be converted into high-grade nickel concentrate, achieving high magnesium and nickel resource utilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0028] Figure 1 The present invention is a process flow chart for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions;

[0029] Figure 2 It is the phase identification diagram of acid-hydrolyzed ore;

[0030] Figure 3 This is the XRD pattern of basic magnesium carbonate. DETAILED DESCRIPTION

[0031] In the following examples, the high magnesium and low nickel salt solutions were obtained from the acid solution of serpentine. The nickel-containing serpentine was obtained from Hanzhong, Shaanxi. The phase analysis and XRF test results were as follows: Figure 1 and as shown in Table 1;

[0032] Table 1 Analysis of elemental composition of nickel-bearing serpentine rock in Hanzhong, Shaanxi

[0033]

[0034] The results of the serpentine whole rock analysis are shown in Table 2 below:

[0035] Table 2 Serpentine whole rock analysis

[0036]

[0037]

[0038] The embodiment provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, the specific steps of which are as follows:

[0039] S1. Take nickel-containing serpentine ore, grind it using a Raymond mill to a mesh size of 200-300 mesh, and calcine it at a temperature of 500-700° C. for 0.5 h to obtain a powder;

[0040] S2. Add the powder obtained in S1 to distilled water while stirring to prepare a slurry, and then add inorganic acid HCl or H2SO4 to carry out acid hydrolysis and leaching for 0.5 to 3 hours, with the concentration of the inorganic acid being 12 mol / L. After washing the solid residue, an acid hydrolysis solution is obtained, and after centrifugation at a speed of 5000 r / min for 10 minutes, a magnesium salt solution and acid-hydrolyzed white carbon black are obtained;

[0041] S3, adding a neutralizer to the magnesium salt solution obtained in S2, wherein the neutralizer is any one of magnesium oxide, basic magnesium carbonate, magnesium hydroxide or basic basic magnesium carbonate or a combination of two or more thereof, adding an appropriate amount of hydrogen peroxide or bubbling air at a later stage, adjusting the pH value to 5-7, separating after aging for 1 hour, washing the precipitate with distilled water, and obtaining a low-nickel magnesium sulfate solution;

[0042] S4, take 200mL of the low-nickel magnesium sulfate solution obtained in S3, add thereto a 2.0mol / L ammonium carbonate solution, the amount of the ammonium carbonate solution being 1 to 5 times the nickel ion content in the low-nickel magnesium sulfate solution, wait until the magnesium ions are completely precipitated, fully wash and then dry to obtain basic magnesium carbonate;

[0043] S5. Take 200 mL of the low-nickel magnesium sulfate solution obtained in S3, add 0.10 to 0.20 mL of a chelating agent thereto, wherein the chelating agent is any one of ethylenediamine, salicylic acid, o-phenanthroline or amino acid, and stir thoroughly for 0.5 h to obtain a high-magnesium solution;

[0044] S6, to the high magnesium solution obtained in S5, 159.4 mL of a 2.0 mol / L precipitant ammonium carbonate solution was added to completely precipitate the magnesium ions, and after drying, a precipitated product of high-purity basic magnesium carbonate and an ammonium sulfate solution residue containing a nickel-cobalt complex was obtained;

[0045] S7. Concentrate and crystallize the residual liquid containing the nickel-cobalt complex prepared in S6 to obtain ammonium sulfate crystals, evaporate and dry the residual liquid, and calcine to obtain nickel concentrate.

[0046] Example 1

[0047] This embodiment provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, the specific steps of which are as follows:

[0048] S1. After preliminary crushing of nickel-containing serpentine, grind it to 200-300 mesh using a Raymond mill, take 0.400 kg and calcine it at 650 ° C for 0.5 h to obtain 0.361 kg of powder;

[0049] S2. While stirring, add 0.361 kg of the powder obtained in S1 to 1800 mL of distilled water to make a pulp, then add 360 mL of 12 mol / L H2SO4 solution, leaching at 90°C for 1 hour and then separating, washing the solid residue twice with a small amount of distilled water and collecting the two washing liquids, combining the two washing liquids to obtain an acid hydrolysis solution, and after preliminary centrifugation, obtaining a crude magnesium sulfate solution and acid-hydrolyzed white carbon black; the centrifugal speed is 5000 r / min, and the centrifugal time is 10 min.

[0050] S3. Add an appropriate amount of basic magnesium carbonate powder to the crude magnesium sulfate solution obtained in S2, adjust the pH to 6.9, age for 1 hour, separate, wash the orange-red precipitate twice with a small amount of distilled water, and combine the liquids to obtain 2565 mL of low-nickel magnesium sulfate solution, wherein the contents of nickel, manganese and cobalt are 376 mg / L, 104 mg / L and 31 mg / L, respectively;

[0051] S4, take 200mL of the low-nickel magnesium sulfate solution obtained in S3, add 167.0mL of 2.0mol / L ammonium carbonate solution thereto, wait for the magnesium ions to be completely precipitated, wash 3 times and then dry to obtain 30.364g of basic magnesium carbonate, the physical analysis of which is as follows: Figure 3 As shown;

[0052] S5. Take 200 mL of the low-nickel magnesium sulfate solution obtained in S3, add 0.10 mL of ethylenediamine thereto, and stir for 0.5 h to obtain a high-magnesium solution;

[0053] S6. Add 159.4 mL of 2.0 mol / L ammonium carbonate solution to the high-magnesium solution obtained in S5 to completely precipitate the magnesium ions. After drying, 29.395 g of basic magnesium carbonate and an ammonium sulfate solution containing a nickel-cobalt complex are obtained.

[0054] Example 2

[0055] This embodiment provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, the specific steps of which are as follows:

[0056] In this example, 2565 mL of low-nickel magnesium sulfate solution prepared in S3 of Example 1 was used as raw material;

[0057] S5. Take 200 mL of the low-nickel magnesium sulfate solution obtained in S3, add 0.15 mL of ethylenediamine thereto, and stir for 0.5 h to obtain a high-magnesium solution;

[0058] S6. Add 160.2 mL of 2.0 mol / L ammonium carbonate solution to the high-magnesium solution obtained in S5 to completely precipitate the magnesium ions. After drying, 29.760 g of basic magnesium carbonate and an ammonium sulfate solution containing a nickel-cobalt complex are obtained.

[0059] Example 3

[0060] This embodiment provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, the specific steps of which are as follows:

[0061] In this example, 2565 mL of low-nickel magnesium sulfate solution prepared in S3 of Example 1 was used as raw material;

[0062] S5. Take 200 mL of the low-nickel magnesium sulfate solution obtained in S3, add 0.20 mL of ethylenediamine thereto, and stir for 0.5 h to obtain a high-magnesium solution;

[0063] S6. Add 159.0 mL of 2.0 mol / L ammonium carbonate solution to the high-magnesium solution obtained in S5 to completely precipitate the magnesium ions. After drying, 29.248 g of basic magnesium carbonate and an ammonium sulfate solution containing a nickel-cobalt complex are obtained.

[0064] 1.000 g of the basic magnesium carbonate samples from the above three examples were dissolved in an excess of sulfuric acid solution and placed in a 100 mL volumetric flask. The results of the nickel, manganese and cobalt content tests in the basic magnesium carbonate are shown in Table 3 below:

[0065] Table 3 Nickel, manganese and cobalt content detection in basic magnesium carbonate in three embodiments

[0066]

[0067]

[0068] Example 4

[0069] The ammonium sulfate solutions containing the nickel-cobalt complex in S6 of Examples 1, 2, 3 and other more examples were mixed, concentrated and crystallized to obtain ammonium sulfate crystals. The residual liquid was evaporated and dried at a temperature of 120° C., and calcined at a temperature of 850° C. for 2 h to obtain 2.282 g of nickel powder, of which NiO accounted for 51.75%, MnO accounted for 14.59%, and CoO accounted for 4.29%. The calcined tail gas was collected and further converted into a by-product, ammonium (sulfite).

[0070] Based on Examples 1 to 4, using the method provided by the present invention for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, the magnesium element recovery rate was 96.8%, the nickel element recovery rate was 96.21%, and the manganese and cobalt recovery rates were 96.68% and 96.93%, respectively.

[0071] Example 5

[0072] This embodiment provides a method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, the specific steps of which are as follows:

[0073] S1. After preliminary crushing of nickel-containing serpentine, grind it to 200-300 mesh using a Raymond mill, take 0.400 kg and calcine it at 650 ° C for 0.5 h to obtain 0.361 kg of powder;

[0074] S2. While stirring, add 0.358 kg of the powder obtained in S1 to 1500 mL of distilled water to make a pulp, then add 700 mL of 12 mol / L HCl solution, leaching at 90°C for 1 hour and then separating, washing the solid residue twice with a small amount of distilled water and collecting the two washings, combining the two washings to obtain an acid hydrolysis solution, and obtaining a crude magnesium sulfate solution and acid-hydrolyzed white carbon black after preliminary centrifugation; the centrifugal speed is 5000 r / min, and the centrifugation time is 10 min.

[0075] S3. Add an appropriate amount of basic magnesium carbonate powder to the crude magnesium sulfate solution obtained in S2, adjust the pH to 6.9, age for 1 hour, separate, wash the orange-red precipitate twice with a small amount of distilled water, and combine the liquids to obtain 2565 mL of low-nickel magnesium sulfate solution, wherein the contents of nickel, manganese and cobalt are 376 mg / L, 104 mg / L and 31 mg / L, respectively;

[0076] S4, take 200mL of the low-nickel magnesium sulfate solution obtained in S3, add 167.0mL of 2.0mol / L ammonium carbonate solution thereto, wait for the magnesium ions to be completely precipitated, wash 3 times and then dry to obtain 30.364g of basic magnesium carbonate, the physical analysis of which is as follows: Figure 3 As shown;

[0077] S5. Take 200 mL of the low-nickel magnesium sulfate solution obtained in S3, add 0.10 mL of ethylenediamine thereto, and stir for 0.5 h to obtain a high-magnesium solution;

[0078] S6. Add 159.4 mL of 2.0 mol / L ammonium carbonate solution to the high-magnesium solution obtained in S5 to completely precipitate the magnesium ions. After drying, 29.395 g of basic magnesium carbonate and an ammonium sulfate solution containing a nickel-cobalt complex are obtained.

[0079] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent variation made to the above embodiment based on the essence of the invention technology shall still fall within the scope of protection of the technical solution of the present invention.

Claims

1. A method for preparing high-purity basic magnesium carbonate from nickel-containing serpentine and enriching nickel (II) ions, characterized in that: The following steps are involved: S1. pulverize nickel-containing serpentine ore, calcine the ore, and obtain a powder; S2. Add the powder obtained in S1 to distilled water while stirring to prepare a slurry, then add an inorganic acid for acid hydrolysis, and then centrifuge to obtain a magnesium salt solution and acid-hydrolyzed silica; S3, adding a neutralizing agent to the magnesium salt solution obtained in S2, adjusting the pH value, separating after aging, washing the precipitate, and obtaining a low-nickel magnesium sulfate solution; S4, take the low-nickel magnesium sulfate solution obtained in S3, add ammonium carbonate solution thereto, wait until the magnesium ions are completely precipitated, fully wash and then dry to obtain basic magnesium carbonate; S5, take the low-nickel magnesium sulfate solution obtained in S3, add a chelating agent thereto, and stir thoroughly to obtain a high-magnesium solution; S6, adding a precipitant to the high-magnesium solution obtained in S5 to completely precipitate the magnesium ions, and drying to obtain a precipitated product and a residual solution containing a nickel-cobalt complex; S7. Concentrate and crystallize the residual liquid containing the nickel-cobalt complex prepared in S6 to obtain ammonium sulfate crystals, evaporate and dry the residual liquid, and calcine to obtain nickel concentrate.

2. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: The pulverization instrument in S1 is a Raymond mill, the mesh size after pulverization is 200-300 mesh, the calcination temperature is 500-700° C., and the calcination time is 0.5 h.

3. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: The inorganic acid in S2 is H2SO4 or HCl. When the inorganic acid is H2SO4, the mass volume ratio of the powder, distilled water and inorganic acid is 0.361kg:1800mL:360mL; when the inorganic acid is HCl, the mass volume ratio of the powder, distilled water and inorganic acid is 0.358kg:1500mL:700mL; the concentration of the inorganic acid is 12mol / L, the leaching temperature of the acid hydrolysis is 90°C, the leaching time of the acid hydrolysis is 0.5~3h, the solution for washing the solid residue is distilled water, the centrifugal speed is 5000r / min, and the centrifugal time is 10min.

4. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: The neutralizing agent in S3 is any one of magnesium oxide, basic magnesium carbonate, magnesium hydroxide or basic basic magnesium carbonate, or a combination of two or more thereof. The pH value after adjustment is 5 to 7, the aging time is 1 hour, and the solution for washing the precipitate is distilled water.

5. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: The amount of the ammonium carbonate solution in S4 is 1 to 5 times the nickel ion content in the low-nickel magnesium sulfate solution, and the concentration of the ammonium carbonate solution is 2.0 mol / L.

6. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: The volume ratio of the low-nickel magnesium sulfate solution and the chelating agent in S5 is 200 mL: 0.10-0.20 mL, the chelating agent in S5 is any one of ethylenediamine, salicylic acid, o-phenanthroline or amino acid, and the stirring time is 0.5 h.

7. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: In S6, the precipitant is ammonium carbonate solution, the precipitated product is magnesium carbonate, the residual liquid is ammonium sulfate solution, the concentration of the ammonium carbonate solution is 2.0 mol / L, and the amount of the ammonium carbonate solution used is 159.4 mL.

8. The method for preparing high-purity basic magnesium carbonate and enriching nickel (II) ions from nickel-containing serpentine according to claim 1, characterized in that: The evaporation temperature in S7 is 120° C., the calcination temperature is 850° C., and the calcination time is 2 h.

Citation Information

Patent Citations

  • Method for separating and enriching cobalt from leach liquor used for pickling and vulcanizing tailing

    CN102994778A

  • Cobalt and magnesium separation method in cobalt nickel wet metallurgy process

    CN108179272A

  • Method for recycling nickel and cobalt from magnesium water

    CN109797294A

  • Methods for removing calcium and magnesium ions from nickel-cobalt-manganese solutions and methods for recycling nickel-cobalt-manganese ternary waste.

    CN112095013B

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    CN112481489A