CN113981242A - Method for displacement copper deposition in nickel chloride solution by using activating agent - Google Patents
Method for displacement copper deposition in nickel chloride solution by using activating agent Download PDFInfo
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- CN113981242A CN113981242A CN202111310058.2A CN202111310058A CN113981242A CN 113981242 A CN113981242 A CN 113981242A CN 202111310058 A CN202111310058 A CN 202111310058A CN 113981242 A CN113981242 A CN 113981242A
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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
- C22B23/0423—Halogenated 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
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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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
- C22B23/0469—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods by chemical substitution, e.g. by cementation
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Abstract
The invention discloses a method for replacing and depositing copper in a nickel chloride solution by using an active agent, which relates to the technical field of copper removal and is used for solving the problems of large amount of copper deposition slag, high loss of noble metals and harsh preparation conditions in the copper removal process method in the prior art, and comprises the following steps: slurrying nickel concentrate and water according to the volume ratio of 1:3-5, heating to 80-85 ℃ for chlorine leaching, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 480-500mV, and separating after filtering to obtain a nickel chloride solution; heating the nickel chloride solution to 60-65 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 3-4:1 and the mass ratio of the copper content in the nickel concentrate to the copper chloride solution of 3-4:1, adjusting the pH to 0.5-2, stirring uniformly, and then heating to 85-90 ℃ for displacement copper precipitation reaction for 3-4 h. The method can be used for removing copper and iron from goethite directly, so that the amount of copper deposition slag is smaller, the loss of noble metal is less, and the preparation condition is simpler and more convenient.
Description
Technical Field
The invention relates to the technical field of copper removal, in particular to the technical field of a method for carrying out displacement copper deposition in a nickel chloride solution by utilizing an active agent.
Background
The copper removing process in hydrometallurgy mainly comprises a nickel concentrate and anode mud method, an active nickel sulfide method and an H2The method comprises an S method, a nickel thiosulfate method and the like, wherein nickel concentrate and anode mud can achieve the purpose of supplementing nickel ions, but the amount of copper precipitation slag is large, and the loss of precious metals is large; the active nickel sulfide is used for copper deposition, so that the amount of copper deposition slag can be greatly reduced, the loss of noble metals is less, partial Pb, Zn and As can be removed, meanwhile, the copper slag treatment process is short, but the active nickel sulfide prepared on site is easy to inactivate, and the production cost of the electrolytic nickel is increased; while adopting the domestic mature H2S removal of copper, control of redox potential from-50 to-80 mV inhibits Ni2+And Co2+The impurities such As Pb, Zn, As and the like can be partially removed while the impurities enter the copper-removing slag due to precipitation, but H2S has high toxicity and high requirement on the tightness of equipment, and is suitable for treating low-concentration Cu2+A solution; the copper removal by using the nickel thiosulfate has the advantages of less introduced impurities, no pollution, complete copper removal and the like, but the preparation condition of the nickel thiosulfate is harsh, and the nickel thiosulfate in the solution is unstable, is easy to decompose and is difficult to realize in industrial application.
Aiming at the chlorine leaching process, the metal ions of nickel, copper, iron and cobalt are selectively leached under the condition of 480-500mV of oxidation-reduction potential, and the metal ions are subjected to leachingThe nickel chloride solution obtained by separation after filtration has an initial pH value less than 0.6 and contains a large amount of Fe3+While the goethite iron removal process requires Fe3+Less than or equal to 1g/L and the pH value is between 2.0 and 2.5, so that the nickel chloride solution can not be directly used for removing iron from goethite.
In conclusion, the copper removal process method in the prior art has the problems of difficult nickel supplement, large copper deposition amount, more precious metal loss, easy inactivation of the prepared active nickel sulfide and harsh preparation conditions. In addition, the initial pH of the nickel chloride solution in the chlorination system is less than 0.6, a large amount of alkali is consumed to adjust the pH to 2-2.5, goethite iron removal is carried out, the production cost is increased, and meanwhile, the iron in the nickel chloride solution is Fe3+Fe is required for removing iron from goethite3+Will be reduced to Fe2+In order to solve the technical problems, a method for replacing and precipitating copper in a nickel chloride solution by using an active agent is provided.
Disclosure of Invention
The invention aims to: aiming at solving the problems of difficult nickel supplement, large copper deposition amount, more precious metal loss, harsh preparation conditions, low pH value of nickel chloride solution and Fe in the solution in the prior art copper removal process method3+The invention provides a method for replacing and copper-depositing in nickel chloride solution by using an active agent, wherein the nickel chloride solution produced by separation after filtration is subjected to replacement and copper-depositing reaction, other impurity metal ions cannot be introduced into the added nickel concentrate and anode mud, 99.96% of copper ions in the nickel chloride solution can be removed, the effects of improving the pH value of the solution, reducing alkali consumption and supplementing nickel ions can be achieved, the iron removal of goethite can be directly carried out, the copper removal by the method can also ensure that the amount of copper-deposited slag is smaller, the loss of precious metals is less, and the preparation condition is simpler and more convenient.
The invention specifically adopts the following technical scheme for realizing the purpose:
a method for displacement copper deposition in a nickel chloride solution by using an active agent comprises the following steps:
slurrying nickel concentrate and water according to the volume ratio of 1:3-5, heating to 80-85 ℃ for chlorine leaching, raising the temperature to 110 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 480-;
heating the nickel chloride solution to 60-65 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 3-4:1 and the mass ratio of the copper content in the nickel concentrate to the copper chloride solution of 3-4:1, adjusting the pH to 0.5-2, stirring uniformly, and then heating to 85-90 ℃ for displacement copper precipitation reaction for 3-4 h.
And (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
The invention has the following beneficial effects:
(1) according to the method, the nickel chloride solution produced by separation after filtration is subjected to displacement copper precipitation reaction, other impurity metal ions cannot be introduced into the added nickel concentrate and the anode mud, 99.96% of copper ions in the nickel chloride solution can be removed, the effects of improving the pH value of the solution, reducing alkali consumption and supplementing nickel ions can be achieved, goethite iron removal can be directly performed, copper removal can be performed by the method, the amount of copper precipitation slag is smaller, the loss of precious metals is less, and the preparation condition is simpler and more convenient.
(2) In the invention, after the replacement copper precipitation reaction is finished, the solid-liquid separation is carried out, the copper precipitation slag is returned to the chlorination leaching process for continuous leaching, and the liquid after copper precipitation is subjected to iron removal by carrying out goethite method, so that the copper in the copper precipitation slag can be further removed, the copper can be removed as much as possible, and meanwhile, the useful metal iron in the solution after copper precipitation can be removed for utilization.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention.
A method for displacement copper deposition in a nickel chloride solution by using an active agent comprises the following steps:
slurrying nickel concentrate and water in a volume ratio of 1:3-5, heating to 80-85 ℃ for chlorine leaching, raising the temperature to 110 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 480-500mV, and filtering and separating to produce a nickel chloride solution;
heating the nickel chloride solution to 60-65 ℃, and then mixing the nickel concentrate with the anode mud according to the mass ratio of 3-4: 1. adding nickel concentrate and anode mud into the nickel concentrate and the nickel chloride solution according to the mass ratio of copper content of 3-4:1, adjusting pH to 0.5-2, uniformly stirring, and then heating to 85-90 ℃ for displacement copper precipitation reaction for 3-4 h;
and (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
Wherein, the nickel chloride solution is provided by a workshop, and the chemical components of the nickel chloride solution are shown in the table 1 after being filtered and separated.
TABLE 1 Nickel chloride solution chemical composition (g/L)
| Element(s) | Ni | Cu | Fe | Co |
| Content (wt.) | 184.05 | 26.55 | 19.20 | 1.82 |
Reaction time, pH, nickel concentrate adding amount, anode mud adding amount, activity of nickel concentrate and anode mud and reaction temperature influence copper removal efficiency, and specific influence conditions of the reaction time, the pH, the nickel concentrate adding amount, the anode mud adding amount, the activity of nickel concentrate and anode mud and the reaction temperature on the copper removal efficiency are respectively tested.
First, the influence of the reaction time on the copper removal efficiency
Taking 3000ml of nickel chloride solution, slowly raising the temperature to 60-65 ℃, adding nickel concentrate and anode mud, raising the temperature to 85-90 ℃, and inspecting the influence of different reaction times on the copper removal effect under the conditions that the mass ratio of the nickel concentrate to the anode mud is 3-4:1, the mass ratio of the copper content in the nickel concentrate to the nickel chloride solution is 3-4:1, the reaction temperature is 85-90 ℃, and the pH value is 0.6, wherein the results are shown in table 2, and table 2 shows the change situation of the copper ion content in the solution under different reaction times.
TABLE 2 influence of reaction time on copper removal efficiency (g/L)
As can be seen from Table 2, the copper removal reaction time is 3-4h, and the copper removal effect is optimal.
Second, the influence of pH on the copper removal efficiency
Taking 3000ml of nickel chloride solution, slowly raising the temperature to 60-65 ℃, adding nickel concentrate and anode mud, raising the temperature to 85-90 ℃, and adding a catalyst into the mixture when the mass ratio of the active nickel concentrate to the anode mud is 3-4: 1. cu in nickel concentrate and nickel chloride solution2+3-4 of mass ratio: 1. the effect of different pH values on the copper removal effect was examined under the conditions of a reaction temperature of 85-90 ℃ and a reaction time of 3-4h, and the results are shown in Table 3, wherein Table 3 shows the content of copper ions in the solution under different reaction pH values.
TABLE 3 influence of pH on the copper removal efficiency (g/L)
As can be seen from Table 3, the copper removal effect is the best under the condition that the pH value for copper removal is 0.6.
Thirdly, the influence of the adding amount of the nickel concentrate on the copper removal efficiency
Taking 3000ml of nickel chloride solution, slowly raising the temperature to 60-65 ℃, adding nickel concentrate and anode mud, raising the temperature to 85-90 ℃, reacting at 85-90 ℃, and reacting anode mud and Cu2+The content ratio is 1: 1. the influence of the addition amount of different nickel concentrates on the copper removal effect is examined under the conditions that the reaction time is 3-4h and the pH value is 0.6, the result is shown in table 4, and the table 4 shows the content of copper ions in the solution under different reaction nickel concentrate use amounts.
TABLE 4 influence of the nickel concentrate addition on the copper removal (g/L)
As can be seen from Table 4, the nickel concentrate was mixed with Cu in consideration of the cost2+The copper removal effect is optimal under the condition that the content ratio is 4: 1.
Fourthly, the influence of the adding amount of the anode mud on the copper removal efficiency
Taking 3000ml of nickel chloride solution, slowly raising the temperature to 60-65 ℃, adding nickel concentrate and anode mud, raising the temperature to 85-90 ℃, and adding the nickel concentrate and Cu2+The content ratio is 4: 1. the effect of different anode mud dosages on the copper removal effect is examined under the conditions that the reaction temperature is 85-90 ℃, the reaction time is 3-4h and the reaction pH is 0.6, the result is shown in table 5, and the table 5 shows the content of copper ions in the solution under different anode mud dosages.
TABLE 5 influence of the amount of sludge added on the copper removal efficiency (g/L)
As can be seen from Table 5, the anode slime was mixed with Cu2+The copper removal effect is optimal under the condition that the content ratio is 4: 1.
Influence of activity of nickel concentrate and anode mud on copper removal efficiency
Taking 3000ml of nickel chloride solution, slowly raising the temperature to 60-65 ℃, adding nickel concentrate and anode mud, raising the temperature to 85-90 ℃, and adding a catalyst in a mass ratio of active nickel concentrate to anode mud of 4: 1. cu in nickel concentrate and nickel chloride solution2+And (4) mass ratio: 1. the effect of the activity of different nickel concentrates and anode slime on the copper removal effect is examined under the conditions of the reaction temperature of 85-90 ℃, the reaction time of 3-4h and the pH value of 0.6, the result is shown in table 6, and the table 6 shows the content of copper ions in the solution under different activities of the nickel concentrates and the anode slime.
TABLE 6 influence of the activity of the nickel concentrate and of the sludge on the copper removal efficiency (g/L)
As can be seen from Table 6, the activity of the nickel concentrate and the anode slime is kept higher within 72h, and the copper removal effect is optimal.
Sixthly, the influence of the reaction temperature on the copper removal efficiency
Taking 3000ml of nickel chloride solution, slowly raising the temperature to 60-65 ℃, adding nickel concentrate and anode mud, and adding the nickel concentrate and the anode mud into the active nickel concentrate: the mass ratio of the anode mud is 4: 1. nickel concentrate and Cu2+The content ratio is 4: 1. the effect of different reaction temperatures on the copper removal effect was examined under the conditions of a reaction pH of 0.6 and a reaction time of 3-4h, and the results are shown in Table 7, in which the content of copper ions in the solution was found at different reaction temperatures in Table 7.
TABLE 7 influence of reaction temperature on copper removal efficiency (g/L)
As can be seen from Table 7, the effect of removing copper is the best when the reaction temperature is 85-90 ℃.
In summary, by comparing conditions such as reaction time, pH, the usage amount of the nickel concentrate and the anode mud, the activity of the nickel concentrate and the anode mud, reaction temperature and the like, it is determined that the nickel concentrate and the anode mud keep higher activity within 72h, and meanwhile, the mass ratio of the nickel concentrate to the anode mud is 4: 1. cu in nickel concentrate and nickel chloride solution2+The mass ratio of the contents is 4: 1. the copper removal effect of the nickel chloride solution is optimal under the process conditions that the reaction temperature is 85-90 ℃, the reaction time is 3-4h and the pH value of the solution is 0.6.
Example 1
As shown in fig. 1, this embodiment provides a method for displacement deposition of copper in nickel chloride solution by using an active agent, which includes the following steps:
slurrying nickel concentrate and water in a volume ratio of 1:3, heating to 80 ℃ for chlorine leaching, raising the temperature to 100 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 480mV, filtering and separating to obtain a nickel chloride solution;
heating the nickel chloride solution to 60 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 3:1 and the mass ratio of the copper content in the nickel concentrate to the copper content in the nickel chloride solution of 3-4:1, adjusting the pH to 0.5, uniformly stirring, and then heating to 85 ℃ for displacement copper precipitation reaction for 3 hours;
and (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
The copper removal after the reaction is shown in table 8:
TABLE 8 copper deposition by displacement of nickel chloride solution test results (g/L)
| Element(s) | Ni | Cu | Fe |
| Concentration (g/L) | 180.27 | 0.069 | 19.20 |
Example 2
As shown in fig. 1, this embodiment provides a method for displacement deposition of copper in nickel chloride solution by using an active agent, which includes the following steps:
slurrying nickel concentrate and water according to the volume ratio of 1:4, heating to 82 ℃ for chlorine leaching, raising the temperature to 105 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 490mV, filtering and separating to produce a nickel chloride solution;
heating the nickel chloride solution to 63 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 3.5:1 and the mass ratio of the copper content in the nickel concentrate to the copper chloride solution of 3.5:1, adjusting the pH to 0.6, uniformly stirring, and then heating to 88 ℃ for displacement copper precipitation reaction for 3.5 hours;
and (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
The copper removal after the reaction is complete is shown in table 9:
TABLE 9 copper deposition by displacement of nickel chloride solution test results (g/L)
| Element(s) | Ni | Cu | Fe |
| Concentration (g/L) | 186.35 | 0.056 | 20.23 |
Example 3
As shown in fig. 1, this embodiment provides a method for displacement deposition of copper in nickel chloride solution by using an active agent, which includes the following steps:
slurrying nickel concentrate and water in a volume ratio of 1:5, heating to 85 ℃ for chlorine leaching, raising the temperature to 110 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 500mV, and filtering to separate out a nickel chloride solution;
heating the nickel chloride solution to 65 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 4:1 and the mass ratio of the copper content in the nickel concentrate to the copper chloride solution of 4:1, adjusting the pH to 2, uniformly stirring, and heating to 90 ℃ to perform displacement copper precipitation reaction for 4 hours;
and (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
The copper removal after the reaction is completed is shown in table 10:
TABLE 10 results of nickel chloride solution displacement copper deposition experiments (g/L)
| Element(s) | Ni | Cu | Fe |
| Concentration (g/L) | 190.21 | 0.098 | 19.98 |
Example 4
As shown in fig. 1, this embodiment provides a method for displacement deposition of copper in nickel chloride solution by using an active agent, which includes the following steps:
slurrying nickel concentrate and water according to the volume ratio of 1:4, heating to 82 ℃ for chlorine leaching, raising the temperature to 105 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 490mV, filtering and separating to produce a nickel chloride solution;
heating the nickel chloride solution to 63 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 4:1 and the mass ratio of the copper content in the nickel concentrate to the copper content in the nickel chloride solution of 4:1, adjusting the pH to 0.6, uniformly stirring, and then heating to 88 ℃ for displacement copper deposition reaction for 4 hours;
and (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
The copper removal after the reaction is completed is shown in table 11:
TABLE 11 copper deposition by displacement of nickel chloride solution test results (g/L)
| Element(s) | Ni | Cu | Fe |
| Concentration (g/L) | 188.69 | 0.008 | 19.29 |
The copper content of the solution after copper removal is less than 0.01g/L, the pH value is raised to 2.0-2.5, the residue after copper displacement precipitation is washed by water with the pH value of 2.0 contains 28.93 percent of copper and 18.72 percent of nickel, and meanwhile, the residue after copper displacement precipitation can be returned to chlorination leaching for chlorine selective leaching of Cu2+And Ni2+The noble metal and the sulfur are inhibited in the slag, thereby achieving the purpose of enriching the noble metal.
According to the tests, the nickel chloride solution obtained after filtering and separating is subjected to displacement copper precipitation reaction, other impurity metal ions cannot be introduced into the added nickel concentrate and the anode mud, 99.96% of copper ions in the nickel chloride solution can be removed, the effects of improving the pH value of the solution, reducing alkali consumption and supplementing nickel ions can be achieved, goethite iron removal can be directly performed, copper can be removed by the method, the copper precipitation slag amount is smaller, the loss of precious metals is less, and the preparation conditions are simpler and more convenient.
Claims (2)
1. A method for replacing and depositing copper in a nickel chloride solution by utilizing an active agent is characterized by comprising the following steps: the method comprises the following steps:
slurrying nickel concentrate and water according to the volume ratio of 1:3-5, heating to 80-85 ℃ for chlorine leaching, raising the temperature to 110 ℃ along with the reaction, selectively leaching nickel, copper, iron and cobalt metal ions under the condition of an oxidation-reduction potential of 480-;
heating the nickel chloride solution to 60-65 ℃, adding the nickel concentrate and the anode mud according to the mass ratio of the nickel concentrate to the anode mud of 3-4:1 and the mass ratio of the copper content in the nickel concentrate to the copper chloride solution of 3-4:1, adjusting the pH to 0.5-2, stirring uniformly, and then heating to 85-90 ℃ for displacement copper precipitation reaction for 3-4 h.
2. The method for displacement copper deposition in nickel chloride solution by using the active agent as claimed in claim 1, wherein: and (3) after the replacement copper precipitation reaction is finished, carrying out solid-liquid separation, returning the copper precipitation slag to the chlorination leaching process for continuous leaching, and removing iron from the copper precipitation liquid by a goethite method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114836625A (en) * | 2022-05-30 | 2022-08-02 | 金川镍钴研究设计院有限责任公司 | Method for extracting nickel and cobalt from magnetic steel waste |
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Application publication date: 20220128 |