CN110629033A - Method for recovering cobalt and nickel from tungsten waste smelting slag - Google Patents
Method for recovering cobalt and nickel from tungsten waste smelting slag Download PDFInfo
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- CN110629033A CN110629033A CN201910871112.7A CN201910871112A CN110629033A CN 110629033 A CN110629033 A CN 110629033A CN 201910871112 A CN201910871112 A CN 201910871112A CN 110629033 A CN110629033 A CN 110629033A
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- cobalt
- nickel
- smelting slag
- tungsten
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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
-
- 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
-
- 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
- C22B7/04—Working-up slag
-
- 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 invention discloses a method for recovering cobalt and nickel from tungsten waste smelting slag, which comprises the following steps: (1) mixing tungsten waste smelting slag with an activating agent for activation treatment so as to obtain activated slurry; (2) mixing the activated slurry with water to obtain a diluted slurry; (3) and carrying out solid-liquid separation treatment on the diluted slurry so as to obtain a cobalt-nickel containing solution. Therefore, the method can effectively recover the cobalt and nickel elements in the tungsten waste smelting slag, compared with the traditional process, no harmful gas is emitted, the recovery rate of nickel and cobalt is up to more than 95%, the operation is simple, the investment cost is low, and the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of resource utilization of tungsten wastes, and particularly relates to a method for recovering cobalt and nickel from tungsten waste smelting slag.
Background
The tungsten waste smelting slag is a recovery slag rich in cobalt and nickel, and is cobalt-nickel slag after tungsten is extracted through oxidation smelting or saltpeter smelting. The slag mainly contains cobalt oxide, nickel oxide and the like, for a long time, the cobalt and nickel metals in the slag are recovered by adopting a strong acid reduction wet leaching technology, and the reducing agent mainly comprises sodium sulfite, sulfur dioxide, hydrogen peroxide and the like. On one hand, the addition amount of the reducing agent is large in the treatment process; on the other hand, the sodium sulfite and the sulfur dioxide can release sulfur dioxide gas in the using process, and the leaching time is long and the leaching rate is not high.
Therefore, the existing technology for processing the tungsten scrap smelting slag needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, an object of the present invention is to provide a method for recovering cobalt and nickel from tungsten scrap smelting slag, which can effectively recover cobalt and nickel elements in the tungsten scrap smelting slag, and compared with the conventional process, the method has the advantages of no emission of harmful gas, high nickel and cobalt recovery rate up to 95%, simple operation, low investment cost, and suitability for industrial production.
In one aspect of the invention, a method of recovering cobalt and nickel from tungsten scrap smelting slag is provided. According to an embodiment of the invention, the method comprises:
(1) mixing tungsten waste smelting slag with an activating agent for activation treatment so as to obtain activated slurry;
(2) mixing the activated slurry with water to obtain a diluted slurry;
(3) and carrying out solid-liquid separation treatment on the diluted slurry so as to obtain a cobalt-nickel containing solution.
According to the method for recovering cobalt and nickel from the tungsten waste smelting slag, disclosed by the embodiment of the invention, the cobalt and nickel elements in the tungsten waste smelting slag can be effectively recovered, compared with the traditional process, no harmful gas is emitted, the recovery rate of nickel and cobalt is up to more than 95%, the operation is simple, the investment cost is low, and the method is suitable for industrial production.
In addition, the method for recovering cobalt and nickel from tungsten scrap smelting slag according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the invention, in the step (1), the content of cobalt oxide in the tungsten scrap smelting slag is 5-45 wt%, and the content of nickel oxide is 2-20 wt%.
In some embodiments of the invention, in step (1), the activating agent is concentrated sulfuric acid. Therefore, the recovery rate of nickel and cobalt can be improved.
In some embodiments of the present invention, the concentrated sulfuric acid has a concentration of 60 to 98 wt%. Therefore, the recovery rate of nickel and cobalt can be improved.
In some embodiments of the invention, in step (1), the solid to liquid ratio of the activation treatment is 1: (0.5-2) for 4-24 h. Therefore, the recovery rate of nickel and cobalt can be improved.
In some embodiments of the invention, in step (1), the solid to liquid ratio of the activation treatment is 1: (1-1.5) for 8-16 h. Therefore, the recovery rate of nickel and cobalt can be improved.
In some embodiments of the invention, in the step (2), the liquid-solid ratio of the added amount of the water to the tungsten scrap smelting slag is (3-10): 1. therefore, the recovery rate of nickel and cobalt can be improved.
In some embodiments of the present invention, in the step (2), the temperature of the mixing is 60 to 100 ℃ and the time is 1 to 12 hours. Therefore, the recovery rate of nickel and cobalt can be improved.
In some embodiments of the invention, in the step (2), the temperature of the mixing is 80-90 ℃ and the time is 4-8 h. Therefore, the recovery rate of nickel and cobalt can be improved.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic flow diagram of a method for recovering cobalt and nickel from tungsten scrap melting slag according to an embodiment of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In one aspect of the invention, a method of recovering nickel and cobalt from tungsten scrap slag is provided. According to an embodiment of the invention, with reference to fig. 1, the method comprises:
s100: mixing tungsten waste smelting slag with activating agent for activation treatment
In the step, the tungsten scrap smelting slag and an activating agent are mixed for activation treatment, so that activated slurry is obtained. Preferably, the activating agent is concentrated sulfuric acid, more preferably the concentrated sulfuric acid with the concentration of 60-98 wt%, the action mechanism of the concentrated sulfuric acid activation is that the concentrated sulfuric acid reacts with cobaltous oxide in the tungsten waste smelting slag to generate cobalt sulfate and oxygen, and the reaction equation is 2Co2O3+4 concentrated H2SO4＝4CoSO4+4H2O+O2. If the concentration of the sulfuric acid is too low, the reaction condition of the sulfuric acid and cobalt oxide in the tungsten waste smelting slag is poor, the cobalt content in the slag is high, and the decomposition rate of the cobalt is low. Therefore, the cobalt decomposition rate can be obviously improved by adopting the concentrated sulfuric acid with the concentration range. Further, the solid-to-liquid ratio of the activation treatment is 1: (0.5-2) for 4-24 h, preferably the solid-to-liquid ratio is 1 (1-1.5), and the reaction time is 8-16 h. The inventor finds that if the solid-liquid ratio is too high, the activation effect is poor, the cobalt content in the slag is high, and the decomposition rate of the cobalt is low; and the solid-liquid ratio is too low, the mechanical stirring difficulty is high, the equipment requirement is high, and the operation is difficult. Specifically, the tungsten waste smelting slag is recovered slag which is rich in cobalt and nickel and is generated after tungsten is recovered by using a waste tungsten raw material in a saltpeter smelting process or an oxidation smelting process, wherein the mass content of cobalt oxide in the recovered slag is 5-45%, and the mass content of nickel oxide is 2-20%.
S200: mixing the activated slurry with water
In this step, the activated slurry obtained above is mixed with water to obtain a diluted slurry. Further, the liquid-solid ratio of the addition amount of water to the tungsten waste smelting slag is (3-10): 1. the inventor finds that if the liquid-solid ratio is too high, the energy consumption is high, the decomposition cost is high, and if the liquid-solid ratio is too low, the cobalt content in the slag is high, the decomposition rate of the cobalt is low, and the temperature in the process is 60-100 ℃, the time is 1-12 hours, preferably 80-90 ℃, and the time is 4-8 hours. The inventor finds that if the temperature is too high, the energy consumption is high, the decomposition cost is high, and if the temperature is too low, the cobalt content in the slag is high, and the decomposition rate of the cobalt is low; meanwhile, if the time is too long, the energy consumption is high, the decomposition cost is high, and the time is too short, the cobalt content in the slag is high, and the decomposition rate of the cobalt is low.
S300: subjecting the diluted slurry to solid-liquid separation treatment
In the step, the obtained diluted slurry is subjected to solid-liquid separation treatment to obtain a cobalt-nickel containing solution. The diluted slurry is preferably supplied from the dilution step to the solid-liquid separation step by a pump. Specifically, the obtained diluted slurry is subjected to solid-liquid separation treatment, the obtained filter residue is washed by hot water, a washing solution is added into the filtrate to obtain a cobalt-nickel-containing solution, the cobalt and nickel in the filter residue can be washed cleanly by washing, and the recovery rate is improved. It should be noted that the solid-liquid separation mode is any technology capable of realizing solid-liquid separation in the prior art, such as plate-and-frame filter pressing, filtration, and the like, and details are not described here.
According to the method for recovering cobalt and nickel from the tungsten waste smelting slag, the tungsten waste smelting slag and the activating agent are mixed for activation treatment, so that cobalt oxide in the tungsten waste smelting slag is reacted to generate cobalt sulfate, the obtained activation slurry is diluted and then subjected to solid-liquid separation, cobalt and nickel elements in the tungsten waste smelting slag can be effectively recovered, compared with the traditional process, harmful gas is not discharged, the recovery rate of nickel and cobalt is up to more than 95%, the operation is simple, the investment cost is low, and the method is suitable for industrial production.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
S1, adding 2000kg of tungsten waste smelting slag (the mass content of cobalt oxide is 45 percent, the mass content of nickel oxide is 2 percent) into 98 percent concentrated sulfuric acid 4m3And activating for 24 hours.
S2, adding 20m of water into the slurry obtained in the step S13Heating to 100 ℃ and reacting for 12 h. After the reaction, the diluted slurry is filtered to remove waste residues by a solid-liquid separation device, so that a cobalt-nickel-containing solution is obtained, the cobalt recovery rate is 96.8%, and the nickel recovery rate is 95.9%.
Example 2
S1, adding 1500kg of tungsten scrap smelting slag (the mass content of cobalt oxide is 40 percent, the mass content of nickel oxide is 5 percent) into 90 percent concentrated sulfuric acid 2.25m3And activating for 16 h.
S2, adding 12m of water to the slurry obtained in the step S13Heating to 85 deg.C, and reacting for 8 h. After the reaction, the diluted slurry is filtered to remove waste residues by a solid-liquid separation device, so that a cobalt-nickel-containing solution is obtained, the cobalt recovery rate is 95.5%, and the nickel recovery rate is 96.1%.
Example 3
S1, adding 1200kg of tungsten scrap smelting slag (the mass content of cobalt oxide is 35 percent, the mass content of nickel oxide is 10 percent) into 80 percent concentrated sulfuric acid with the mass fraction of 1.5m3And activating for 12 h.
S2, adding 7.2m of water to the slurry obtained in the step S13Heating to 60 ℃ and reacting for 4 h. After the reaction, the diluted slurry is filtered to remove waste residues by a solid-liquid separation device, so that a solution containing cobalt and nickel is obtained, wherein the recovery rate of cobalt is 95.1 percent, and the recovery rate of nickel is 95.7 percent.
Example 4
S1, adding 1500kg of tungsten scrap smelting slag (the mass content of cobalt oxide is 25 percent, the mass content of nickel oxide is 15 percent) into 70 percent concentrated sulfuric acid with the mass fraction of 1.5m3And activating for 8 hours.
S2, adding 4.5m of water into the slurry obtained in the step S13Heating to 80 ℃ and reacting for 8 h. After the reaction, the diluted slurry liquid is filtered to remove waste residues through solid-liquid separation equipment, so that a cobalt-nickel-containing solution is obtained, the cobalt recovery rate is 96.3%, and the nickel recovery rate is 96.1%.
Example 5
S1, adding 2000kg of tungsten scrap smelting slag (the mass content of cobalt oxide is 5 percent, the mass content of nickel oxide is 20 percent) into 60 percent concentrated sulfuric acid 1m3And activating for 4 hours.
S2, adding 10m of water into the slurry obtained in the step S13Heating the mixture to 75 ℃,and reacting for 12 h. After the reaction, the diluted slurry is filtered to remove waste residues by a solid-liquid separation device, so that a cobalt-nickel-containing solution is obtained, the cobalt recovery rate is 95.5%, and the nickel recovery rate is 96.3%.
Example 6
S1, adding 1200kg of tungsten scrap smelting slag (the mass content of cobalt oxide is 15 percent, the mass content of nickel oxide is 8 percent) into 75 percent concentrated sulfuric acid with the mass fraction of 1.45m3And activating for 18 h.
S2, adding 6m of water into the slurry obtained in the step S13Heating to 90 ℃ and reacting for 12 h. After the reaction, the diluted slurry is filtered to remove waste residues by a solid-liquid separation device, so that a cobalt-nickel-containing solution is obtained, the cobalt recovery rate is 96.5%, and the nickel recovery rate is 96.6%.
Comparative example 1
Tungsten scrap slag was treated in the same manner as in example 6, except that 30% by mass of sulfuric acid was used and the conditions were not changed to obtain a cobalt-nickel-containing solution with a cobalt recovery rate of 50% and a nickel recovery rate of 60%.
Comparative example 2
Tungsten scrap slag was processed as in example 1 except that the reaction was diluted with water at room temperature without heating and under otherwise constant conditions to obtain a cobalt-nickel containing solution with a cobalt recovery of 65% and a nickel recovery of 68%.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (9)
1. A method for recovering cobalt and nickel from tungsten scrap smelting slag is characterized by comprising the following steps:
(1) mixing tungsten waste smelting slag with an activating agent for activation treatment so as to obtain activated slurry;
(2) mixing the activated slurry with water to obtain a diluted slurry;
(3) and carrying out solid-liquid separation treatment on the diluted slurry so as to obtain a cobalt-nickel containing solution.
2. The method according to claim 1, wherein in step (1), the content of cobalt oxide and nickel oxide in the tungsten scrap smelting slag is 5-45 wt% and 2-20 wt%.
3. The method according to claim 1, wherein in step (1), the activating agent is concentrated sulfuric acid.
4. The method of claim 3, wherein the concentrated sulfuric acid has a concentration of 60 to 98 wt%.
5. The method according to claim 1, wherein in step (1), the solid-to-liquid ratio of the activation treatment is 1: (0.5-2) for 4-24 h.
6. The method according to claim 1, wherein in step (1), the solid-to-liquid ratio of the activation treatment is 1: (1-1.5) for 8-16 h.
7. The method according to claim 1, wherein in the step (2), the liquid-solid ratio of the added amount of the water to the tungsten scrap smelting slag is (3-10): 1.
8. the method according to claim 1 or 7, wherein in the step (2), the mixing temperature is 60-100 ℃ and the mixing time is 1-12 h.
9. The method of claim 7, wherein in the step (2), the mixing temperature is 80-90 ℃ and the mixing time is 4-8 h.
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| CN201910871112.7A CN110629033A (en) | 2019-09-16 | 2019-09-16 | Method for recovering cobalt and nickel from tungsten waste smelting slag |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113373315A (en) * | 2021-05-18 | 2021-09-10 | 厦门嘉鹭金属工业有限公司 | Method for efficiently recovering cobalt and nickel in tungsten slag |
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| CN103898327B (en) * | 2014-01-23 | 2016-06-01 | 广西有色金属集团汇元锰业有限公司 | A kind of manganese cobalt nickel waste residue extracts the method for nickel |
| CN105803212A (en) * | 2016-03-15 | 2016-07-27 | 中南大学 | Method for recycling cobalt from oxidized and deposited cobalt residues |
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2019
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| CN1510151A (en) * | 2002-12-26 | 2004-07-07 | 中国科学院过程工程研究所 | Cobalt slag containing treating method |
| CA2682532A1 (en) * | 2007-03-30 | 2008-10-09 | Paul Wurth S.A. | Method for recovering molybdenium, nickel, cobalt or their mixtures from used or regenerated catalysts |
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| CN103898327B (en) * | 2014-01-23 | 2016-06-01 | 广西有色金属集团汇元锰业有限公司 | A kind of manganese cobalt nickel waste residue extracts the method for nickel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113373315A (en) * | 2021-05-18 | 2021-09-10 | 厦门嘉鹭金属工业有限公司 | Method for efficiently recovering cobalt and nickel in tungsten slag |
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