CN110951969A - Method for recovering valuable metals from difficult-to-treat cobalt-nickel-containing tailings - Google Patents
Method for recovering valuable metals from difficult-to-treat cobalt-nickel-containing tailings Download PDFInfo
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- CN110951969A CN110951969A CN201911085154.4A CN201911085154A CN110951969A CN 110951969 A CN110951969 A CN 110951969A CN 201911085154 A CN201911085154 A CN 201911085154A CN 110951969 A CN110951969 A CN 110951969A
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid 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
- 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
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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
- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention is suitable for the field of recycling of valuable metals, and provides a method for recycling valuable metals from difficultly-treated cobalt-nickel-containing tailings, wherein a two-stage leaching method of normal-pressure acid leaching and pressure leaching is adopted, the leaching rate of the cobalt-nickel metals is over 99 percent, iron is removed by a goethite method, copper is removed by extraction, and lead and cadmium are precipitated by a vulcanization method and are matched with an impurity removal process, the impurity removal rate reaches over 99.5 percent, and the purity of a cobalt-nickel feed liquid is over 99 percent.
Description
Technical Field
The invention belongs to the field of valuable metal recycling, and particularly relates to a method for recycling valuable metals from difficultly-treated cobalt-nickel-containing tailings.
Background
The nickel-containing tailings are cobalt-nickel precipitates generated in the impurity removal process of nickel sulfate and cobalt sulfate solutions (copper, iron, lead, cadmium and the like), the cobalt/nickel content of the cobalt-nickel precipitates is about 3-8%, the tailings are characterized by high impurities (iron, copper, cadmium and the like) and low metal content, wherein the cobalt-nickel exists mainly in the form of sulfide, and the problems that the leaching is difficult, the impurity content of leachate is high, impurities are difficult to separate from main metals and the like exist in the treatment process of the existing treatment mode.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for recovering valuable metals from cobalt-nickel-containing tailings which are difficult to treat, and to solve the technical problems of difficult leaching, high impurity content in leachate, difficult separation of impurities from main metals, and the like in the conventional treatment method.
The method for recovering valuable metals from the difficult-to-treat cobalt-nickel-containing tailings comprises the following steps:
s1, pumping bottom water with a certain volume into a reaction kettle, then uniformly putting the cobalt-nickel-containing tailings into the reaction kettle, slowly and uniformly adding concentrated sulfuric acid into the reaction kettle at a certain flow rate, stirring while adding the concentrated sulfuric acid, controlling the pH value of the solution in the reaction kettle, stirring and slurrying for a period of time to obtain slurried slurry;
s2, performing pressure filtration on the slurried slurry obtained in the step S1, and performing solid-liquid separation to obtain filtrate and filter residue;
s3, removing impurities from the filtrate obtained in the step S2 sequentially through a goethite method iron removing line, an extraction copper removing line and a vulcanization method lead and cadmium precipitation line, and enabling the solution after the impurities are removed to enter the next process after the solution is detected to be qualified;
and S4, pulping the filter residue obtained in the step S2 according to a certain solid-liquid ratio, sending the filter residue into a presoaking tank, slowly adding a certain amount of concentrated sulfuric acid into the presoaking tank, adjusting the pH value of the solution in the presoaking tank, stirring for a period of time, sending the solution into a pressure kettle by a pump, controlling the reaction conditions in the pressure kettle to react for a period of time, cooling and depressurizing the reaction kettle after the reaction is finished, carrying out solid-liquid separation on the obtained material, merging the obtained solution into the step S3 to remove impurities, and sending the waste residue into a tailing treatment process.
Further, in step S1, the adding amount of the bottom water accounts for 1/3-1/2 of the volume of the reaction kettle, and the adding speed of the concentrated sulfuric acid is 0.2-0.3 m3The pH value of the solution in the reaction kettle is 2.0-2.5, the stirring and slurrying time is 1-3 h, and the reaction temperature is 60-70 ℃.
Further, in step S3, the flow rate of the filtrate was 10m3/h。
Further, in step S4, the adding amount of concentrated sulfuric acid is 0.1-0.2 m3The pH value of the solution in the presoaking tank is 1.5-2.0, and the stirring presoaking time is 5-8 h.
Further, in step S4, the temperature in the autoclave is 130-160 ℃, and the oxygen gas is introduced at a speed of 20-100 m3The pressure in the autoclave is 0.40-0.70 MPa, and the reaction time is 12-18 h.
The invention has the beneficial effects that: the invention provides a method for recovering valuable metals from difficultly treated cobalt-nickel-containing tailings, which adopts a two-stage leaching method of normal-pressure acid leaching and pressure leaching, wherein the leaching rate of cobalt-nickel metals is over 99 percent, and the iron is removed by a goethite method, copper is removed by extraction, and lead and cadmium are precipitated by a vulcanization method and impurity removal processes are matched, the impurity removal rate is over 99.5 percent, and the purity of cobalt-nickel feed liquid is over 99 percent.
Drawings
FIG. 1 is a flow chart of the recovery of valuable metals from a refractory cobalt-nickel containing tailings provided by the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In this embodiment, the method for recovering valuable metals from the refractory cobalt-nickel-containing tailings includes the following steps:
step S1, slurrying step: pumping bottom water with a certain volume into the reaction kettle, then uniformly adding the cobalt-nickel-containing tailings into the reaction kettle, slowly and uniformly adding concentrated sulfuric acid into the reaction kettle at a certain flow rate, stirring while adding the concentrated sulfuric acid, controlling the pH of the solution in the reaction kettle, and stirring and slurrying for a period of time to obtain slurried slurry.
In the step, the adding amount of the bottom water accounts for 1/3-1/2 of the volume of the reaction kettle, and the adding speed of the concentrated sulfuric acid is 0.2-0.3 m3The pH value of the solution in the reaction kettle is 2.0-2.5, the stirring and slurrying time is 1-3 h, and the reaction temperature is 60-70 ℃.
Step S2, solid-liquid separation step: and (4) carrying out pressure filtration on the slurried slurry obtained in the step (S1) and then carrying out solid-liquid separation to obtain filtrate and filter residue.
In the step, the obtained filter residue is placed into a slurrying barrel, and the next procedure is carried out.
Step S3, impurity removal of filtrate: and (4) removing impurities from the filtrate obtained in the step (S2) through a goethite method iron removing line, an extraction copper removing line and a vulcanization method lead and cadmium depositing line in sequence, and detecting qualified solution after impurity removal and then entering the next process.
In this step, the impurity removal process is performed by a conventional process in the art, and is not described herein again.
Step S4, pressure leaching of filter residue: pulping the filter residue obtained in the step S2 according to a certain solid-liquid ratio, then feeding the filter residue into a presoaking tank, slowly adding a certain amount of concentrated sulfuric acid into the presoaking tank, adjusting the pH value of the solution in the presoaking tank, stirring the solution for a period of time, then feeding the solution into a pressure kettle by a pump, controlling the reaction conditions in the pressure kettle to react for a period of time, after the reaction is finished, cooling and depressurizing the reaction kettle, then carrying out solid-liquid separation on the obtained material, merging the obtained solution into the step S3 to remove impurities, and feeding the waste residue into a tailing treatment process.
In the step, the adding amount of the concentrated sulfuric acid is 0.1-0.2 m3The pH value of the solution in the presoaking tank is 1.5-2.0, the stirring presoaking time is 5-8 hours, the temperature in the autoclave is 130-160 ℃, and the oxygen introducing speed is 20-100 m3H, in the autoclaveThe pressure is 0.40-0.70 MPa, and the reaction time is 12-18 h.
In order to explain the technical means of the present invention, the following description will be given by way of specific examples.
To a reaction kettle (25 m)3) Bottom water accounting for 1/3 vol of the reaction kettle is pumped in, then 15t of cobalt-nickel-containing tailings are evenly put into the reaction kettle, and the volume of the tailings is 0.2m3Slowly and uniformly adding concentrated sulfuric acid into the reaction kettle at a flow rate of/h, stirring while adding the concentrated sulfuric acid, controlling the pH of the solution in the reaction kettle to be 2.0-2.5, controlling the reaction temperature to be 60 ℃, stirring for slurrying for 2h to obtain slurried slurry, performing filter pressing on the slurried slurry, and performing solid-liquid separation to obtain filtrate and filter residues.
Filtrate with a volume of 10m3And (2) pumping the solution after iron removal into an iron removal device at a flow rate of/h, removing copper from the solution after iron removal in an extraction line, removing impurities from raffinate in a cadmium removal process, transferring the solution after impurity removal to the next process after the solution is qualified, and removing the impurities of iron, copper and cadmium respectively by the continuous impurity removal process to reach the removal rates of 95%, 90% and 98%.
Weighing 6t of filter residue, slurrying according to a solid-liquid ratio of 1:1.5, feeding the filter residue into a pre-soaking tank, slowly adding concentrated sulfuric acid into the pre-soaking tank, adjusting the pH of the solution in the pre-soaking tank to be 1.5-2.0, presoaking for 5h, pumping the solution into a pressure kettle, controlling the temperature in the pressure kettle to be 150-160 ℃, and controlling the oxygen introduction speed to be 80-100 m3And h, controlling the pressure in the autoclave to be 0.55-0.60 MPa, controlling the reaction time to be 12h, cooling and depressurizing after the reaction is finished, then carrying out solid-liquid separation on the obtained material, merging the filtrate into the impurity removal process, and enabling the waste residues to enter the tailing treatment process.
Through two-stage leaching reaction under normal pressure and pressurization, the leaching rate of nickel and cobalt in the tailings is over 99.5 percent.
In the embodiment of the invention, the leaching rate of cobalt and nickel metal is more than 99 percent by adopting a normal-pressure acid leaching and pressure leaching two-stage leaching method, and the iron removal, the copper removal by extraction and the lead and cadmium precipitation by a vulcanization method are matched with an impurity removal process, the impurity removal rate reaches more than 99.5 percent, the purity of the cobalt and nickel material liquid is more than 99 percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A method for recovering valuable metals from a difficult-to-process cobalt-nickel-containing tailing, which is characterized by comprising the following steps:
s1, pumping bottom water with a certain volume into a reaction kettle, then uniformly putting the cobalt-nickel-containing tailings into the reaction kettle, slowly and uniformly adding concentrated sulfuric acid into the reaction kettle at a certain flow rate, stirring while adding the concentrated sulfuric acid, controlling the pH value of the solution in the reaction kettle, stirring and slurrying for a period of time to obtain slurried slurry;
s2, performing pressure filtration on the slurried slurry obtained in the step S1, and performing solid-liquid separation to obtain filtrate and filter residue;
s3, removing impurities from the filtrate obtained in the step S2 sequentially through a goethite method iron removing line, an extraction copper removing line and a vulcanization method lead and cadmium precipitation line, and enabling the solution after the impurities are removed to enter the next process after the solution is detected to be qualified;
and S4, pulping the filter residue obtained in the step S2 according to a certain solid-liquid ratio, sending the filter residue into a presoaking tank, slowly adding a certain amount of concentrated sulfuric acid into the presoaking tank, adjusting the pH value of the solution in the presoaking tank, stirring for a period of time, sending the solution into a pressure kettle by a pump, controlling the reaction conditions in the pressure kettle to react for a period of time, cooling and depressurizing the reaction kettle after the reaction is finished, carrying out solid-liquid separation on the obtained material, merging the obtained solution into the step S3 to remove impurities, and sending the waste residue into a tailing treatment process.
2. The method of claim 1, wherein in step S1, the bottom water is added in an amount of 1/3-1/2 volume of the reaction kettle, and the concentrated sulfuric acid is added at a speed of 0.2-0.3 m3The pH of the solution in the reaction kettle is 2.0 to c2.5, stirring and slurrying for 1-3 h, wherein the reaction temperature is 60-70 ℃.
3. The method for recovering valuable metals from refractory cobalt-nickel containing tailings as claimed in claim 1, wherein the flow rate of the filtrate in step S3 is 10m3/h。
4. The method for recovering valuable metals from refractory cobalt-nickel containing tailings as claimed in claim 1, wherein in step S4, the amount of concentrated sulfuric acid added is 0.1-0.2 m3The pH value of the solution in the presoaking tank is 1.5-2.0, and the stirring presoaking time is 5-8 h.
5. The method of claim 1, wherein the temperature in the autoclave is 130-160 ℃ and the oxygen is introduced at a rate of 20-100 m in step S43The pressure in the autoclave is 0.40-0.70 MPa, and the reaction time is 12-18 h.
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| CN201911085154.4A CN110951969B (en) | 2019-11-08 | 2019-11-08 | Method for recovering valuable metals from difficult-to-treat cobalt-nickel-containing tailings |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146919A (en) * | 2013-04-01 | 2013-06-12 | 广西冶金研究院 | Method for strongly leaching laterite-nickel ore at normal pressure by using sulphuric acid |
| CN103314124A (en) * | 2010-12-17 | 2013-09-18 | 奥图泰有限公司 | Method for separating nickel from material with low nickel content |
| CN104805306A (en) * | 2014-12-31 | 2015-07-29 | 金川集团股份有限公司 | New method for recovering nickel, cobalt and iron from low-grade laterite-nickel ore |
| CN110205493A (en) * | 2019-05-09 | 2019-09-06 | 厦门钨业股份有限公司 | Cobalt slag mixes the method for leaching and extracting cobalt, nickel with nickel-molybdenum ore |
| CN110257633A (en) * | 2019-06-25 | 2019-09-20 | 西部矿业股份有限公司 | It is a kind of to handle wet process zinc abstraction copper-cadmium slag, method of the nickel cobalt slag to prepare copper sponge, Spongy Cadmium simultaneously |
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2019
- 2019-11-08 CN CN201911085154.4A patent/CN110951969B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103314124A (en) * | 2010-12-17 | 2013-09-18 | 奥图泰有限公司 | Method for separating nickel from material with low nickel content |
| CN103146919A (en) * | 2013-04-01 | 2013-06-12 | 广西冶金研究院 | Method for strongly leaching laterite-nickel ore at normal pressure by using sulphuric acid |
| CN104805306A (en) * | 2014-12-31 | 2015-07-29 | 金川集团股份有限公司 | New method for recovering nickel, cobalt and iron from low-grade laterite-nickel ore |
| CN110205493A (en) * | 2019-05-09 | 2019-09-06 | 厦门钨业股份有限公司 | Cobalt slag mixes the method for leaching and extracting cobalt, nickel with nickel-molybdenum ore |
| CN110257633A (en) * | 2019-06-25 | 2019-09-20 | 西部矿业股份有限公司 | It is a kind of to handle wet process zinc abstraction copper-cadmium slag, method of the nickel cobalt slag to prepare copper sponge, Spongy Cadmium simultaneously |
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