CN115927859A - Method for recycling valuable metals from nickel matte in copper sulfate circulating leaching - Google Patents
Method for recycling valuable metals from nickel matte in copper sulfate circulating leaching Download PDFInfo
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- CN115927859A CN115927859A CN202211654315.9A CN202211654315A CN115927859A CN 115927859 A CN115927859 A CN 115927859A CN 202211654315 A CN202211654315 A CN 202211654315A CN 115927859 A CN115927859 A CN 115927859A
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Abstract
The invention discloses a method for recovering valuable metals from nickel matte in copper sulfate circulating leaching, wherein the nickel matte mainly comprises 25-35% of Ni, 16-22% of Cu, 16-20% of Fe, 0.34-0.70% of Co and 18-24% of S. The method adopts a sulfuric acid-copper sulfate leaching process, realizes the leaching of nickel and iron by setting the process procedures of normal pressure leaching, pressure replacement, pressure leaching, pressure iron removal, evaporative crystallization and the like and controlling the concentration of copper and acid in different process sections in a system, can separate main metals in nickel matte, and realizes the separation and enrichment of valuable metals and the comprehensive recycling of impurity metals. Finally, nickel and cobalt are separated in the form of coarse nickel and cobalt sulfate crystals, which can be used for connecting the production process of nickel and cobalt sulfate products; copper is separated in the form of copper slag containing precious metals, and the copper smelting and precious metal recovery process can be linked; the iron is separated in the form of ferric oxide, and can be linked with the production process of iron ore concentrate, so that the resource utilization of iron is realized.
Description
Technical Field
The invention belongs to the technical field of nickel pyrometallurgy, and particularly relates to a method for recycling valuable metals from nickel matte in copper sulfate circulating leaching.
Background
In the smelting process of the nickel sulfide ore, nickel sulfide concentrate is smelted by a flash furnace (or a top-blown furnace) to produce low grade nickel matte, the low grade nickel matte is blown by a converter to produce high grade nickel matte, and the main purpose of the process is to remove iron; in the converter blowing process, the iron content in the low nickel matte is required to be blown to be less than 4%, however, the loss of cobalt and part of metals is serious in the blowing process, especially the loss rate of cobalt is up to 50%, and the produced converter slag needs to be depleted in a depletion electric furnace, and the repeated smelting causes repeated material circulation, repeated energy consumption and serious environmental pollution. Research shows that in order to improve the recovery rate of metals such as cobalt and the like and reduce repeated smelting and environmental pollution, a wet process can be adopted to directly treat low grade nickel matte to replace the traditional pyrometallurgical smelting process.
The iron content of the low nickel matte produced by the pyrometallurgical smelting process reaches 27-56%, the low nickel matte is treated by a wet method, the treatment cost is related to the iron content in the raw materials, and generally, the wet treatment cost and the process complexity are increased along with the increase of the iron content in the low nickel matte. Practice proves that in the process of blowing low nickel matte to high nickel matte, when the iron content in nickel matte is 16-20%, the loss rate of cobalt is low. According to the characteristics, the iron in the low grade nickel matte can be blown to 16-20%, and the nickel matte is called medium grade nickel matte, so that not only can most of iron be blown off in the pyrometallurgical smelting process be ensured, but also higher cobalt recovery rate can be ensured. Therefore, the cost and the process treatment difficulty can be correspondingly reduced by adopting the wet process treatment for the medium grade nickel matte.
Disclosure of Invention
Based on the above, the invention provides the method for recycling valuable metals from nickel matte in the copper sulfate cyclic leaching, which has the advantages of simple process and low cost, realizes the separation and enrichment of valuable metals such as nickel, copper and the like by using the cyclic leaching of copper in the raw materials, recycles the sulfuric acid produced by iron removal, and realizes no wastewater and no waste residue discharge in the whole process.
In order to realize the purpose, the invention adopts the following technical scheme:
a method for recovering valuable metals from nickel matte in copper sulfate circulating leaching comprises the following steps:
a) Leaching under normal pressure: adding water into the nickel matte to pulp, adding the pulp into an atmospheric pressure closed leaching reaction kettle, adding a part of crystallization mother liquor produced in the step e) into the atmospheric pressure closed reaction kettle, controlling the mass ratio of liquid to solid to be 4;
b) Pressure replacement: after the atmospheric leaching reaction is finished, adding the reaction slurry and the copper sulfate solution obtained in the step c) into a pressure reaction kettle, heating to perform pressure displacement leaching, controlling the leaching temperature to be 150-200 ℃ and the time to be 2-6 h, and performing solid-liquid separation after the reaction is finished to obtain a liquid after pressure displacement and displacement slag;
c) Pressure leaching: pulping the replacement slag obtained in the step b) by using evaporative crystallization condensed water obtained in the step e), adding the pulped replacement slag into a pressurized reaction kettle, simultaneously adding part of crystallization mother liquor produced in the step e) into the pressurized reaction kettle, controlling the mass ratio of liquid to solid to be 4 to 1 to 6, heating, introducing oxygen to carry out pressurized leaching, controlling the leaching temperature to be 150 to 180 ℃, the time to be 1 to 3 hours and the oxygen partial pressure to be 0.1 to 0.3MPa, and carrying out solid-liquid separation after the reaction is finished to obtain a copper sulfate solution and copper slag;
d) Pressurizing and deironing: adding the displaced liquid obtained in the step b) into a pressurized reaction kettle, introducing oxygen after the temperature reaches the reaction requirement, performing pressurized iron removal, controlling the iron removal temperature to be 180 to 220 ℃, the time to be 0.5 to 2h and the oxygen partial pressure to be 0.1 to 0.3MPa, and performing solid-liquid separation after the reaction is finished to obtain iron-removed liquid and iron slag;
e) Evaporation and crystallization: evaporating and crystallizing the iron-removed solution obtained in the step d) to obtain crude nickel cobalt sulfate crystals and a crystallization mother solution, wherein one part of the crystallization mother solution returns to the atmospheric pressure leaching process, and the other part returns to the pressure leaching process.
The whole process flow of the invention realizes the recycling of water, the leaching solution (copper sulfate solution) obtained in the pressure leaching process returns to the pressure replacement process, the crystallization mother liquor obtained in the evaporation crystallization process returns to the pressure leaching and normal pressure leaching processes, and the volume balance of the whole process is realized. When the whole process flow is started, newly prepared copper sulfate solution can be added in the pressure replacement process to start reaction, and water can be added in the normal pressure leaching and pressure leaching processes to replace the crystallization mother liquor returned in normal production to start the whole process flow. After the whole process is started, the pressurized leaching solution (copper sulfate solution) returns to the pressurized replacement process, and the crystallization mother liquor returns to the normal pressure leaching and the pressurized leaching, so that the volume balance of the whole process is realized.
Preferably, the medium grade nickel matte is derived from low grade nickel matte produced in the pyrometallurgical smelting of nickel sulfide ores and is blown by a converter to obtain low-iron-content nickel matte, and the main components of the low-iron-content nickel matte comprise the following components in percentage by weight: 25-35% of Ni, 16-22% of Cu, 16-20% of Fe, 0.34-0.70% of Co and 18-24% of S.
Further, the normal pressure leaching time is 2 to 5 hours.
The invention has the beneficial effects that:
1. the invention provides a method for circularly leaching copper sulfate aiming at nickel matte in an intermediate material produced by pyrogenic process smelting of nickel sulfide ores, which can realize separation and enrichment of valuable metals such as nickel, copper and the like and realize resource recycling of iron by utilizing a sulfuric acid-copper sulfate leaching process.
2. The method solves the problem of unbalanced sulfuric acid in the whole process caused by different contents of iron and sulfur in the raw materials through the normal pressure leaching process, and effectively controls the acid balance in the whole process.
3. The method realizes leaching of iron, nickel and cobalt metals in the nickel matte raw material by using copper ions through the pressure replacement-pressure leaching process, and reduces the consumption of sulfuric acid in the whole process.
4. The method can realize the leaching of nickel and iron by controlling the leaching of copper in different process sections in the system and the concentration of copper and sulfuric acid in the solution, thereby achieving the purposes of separating and enriching valuable metals and recycling impurity elements. The recycling of the sulfuric acid produced in the iron removal process is realized in the whole process, compared with the traditional process, the consumption of acid-base reagents can be effectively reduced, and no wastewater or waste residue is discharged in the whole process.
5. The method can convert nickel, copper, cobalt and noble metals into crude nickel cobalt sulfate crystals and copper slag enriched with noble metals; the iron is converted into the iron slag mainly existing in the form of ferric oxide, and the iron slag can be used as a raw material for producing iron ore concentrate, so that the resource recycling of the iron is realized.
Drawings
FIG. 1 is a process flow diagram of the method for recovering valuable metals from nickel matte in the copper sulfate circulating leaching process.
Detailed Description
The process of the present invention will be described in detail with reference to specific examples.
Example 1
The mass percentages of the main elements of the nickel matte in the example are shown in table 1.
TABLE 1 main element content (wt%) of icy nickel in example 1
The specific implementation process comprises the following steps:
1) Pulping the nickel matte in the table 1 by using water, adding the slurried nickel matte into an atmospheric pressure closed leaching reaction kettle, adding part of crystallization mother liquor produced in the evaporation and crystallization process into the atmospheric pressure closed leaching reaction kettle, controlling the liquid-solid volume mass ratio to be 5, and carrying out atmospheric pressure leaching, wherein the leaching temperature is controlled to be 85 ℃, the leaching time is 2.5 hours, and the leaching end point pH is 1.68;
2) And pumping the normal-pressure reaction slurry and the pressure leached copper sulfate solution into a pressure reaction kettle, performing pressure displacement leaching, and controlling the leaching temperature to be 150 ℃ and the leaching time to be 5 hours. After the reaction is finished, carrying out solid-liquid separation to obtain pressurized displacement liquid and displacement slag;
3) Pulping the replacement slag by using evaporation crystallization condensed water, adding the pulp into a pressurized reaction kettle, adding a certain amount of crystallization mother liquor (the rest of the crystallization mother liquor required by atmospheric pressure leaching), controlling the liquid-solid volume mass ratio to be 5, heating, introducing oxygen, and carrying out pressurized leaching, wherein the leaching temperature is controlled to be 180 ℃, the time is 2 hours, and the oxygen partial pressure is 0.1MPa. After the reaction is finished, carrying out solid-liquid separation to obtain a copper sulfate leaching solution and copper slag containing noble metals;
4) And adding the displaced liquid into a pressurized reaction kettle, and controlling the temperature to be 190 ℃, the reaction time to be 1h and the oxygen partial pressure to be 0.1MPa to perform pressurized iron removal. After the reaction is finished, carrying out solid-liquid separation to obtain iron-removed liquid and iron slag;
5) And evaporating and crystallizing the iron-removed solution to obtain crude nickel cobalt sulfate crystals and a crystallization mother solution, wherein one part of the crystallization mother solution returns to the atmospheric pressure leaching process, and the other part of the crystallization mother solution returns to the pressure leaching process.
The main ingredients of the crude nickel cobalt sulfate crystal, copper slag and iron slag are shown in the table 2.
Table 2 example 1 major output composition (%)
Example 2
The mass percentages of the main elements of the nickel matte in the example are shown in Table 3.
Table 3 main element content (%) -of nickel matte in example 2
The specific implementation process comprises the following steps:
1) Adding water into the nickel matte shown in the table 3 for slurrying, adding the slurried nickel matte into an atmospheric pressure closed leaching reaction kettle, adding part of crystallization mother liquor produced in the evaporation crystallization process into the atmospheric pressure closed leaching reaction kettle, controlling the liquid-solid volume mass ratio to be 4;
2) And pumping the normal-pressure reaction slurry and the pressure leached copper sulfate solution into a pressure reaction kettle, performing pressure displacement leaching, and controlling the leaching temperature to be 180 ℃ and the leaching time to be 3 hours. After the reaction is finished, carrying out solid-liquid separation to obtain pressurized displacement liquid and displacement slag;
3) Pulping the replacement slag by adopting evaporation crystallization condensed water, adding the pulp into a pressurized reaction kettle, adding a certain amount of crystallization mother liquor (the rest of the crystallization mother liquor required by atmospheric pressure leaching), controlling the liquid-solid volume-mass ratio to be 4, heating, introducing oxygen for pressurized leaching, and controlling the leaching temperature to be 150 ℃, the time to be 3 hours and the oxygen partial pressure to be 0.1MPa. After the reaction is finished, carrying out solid-liquid separation to obtain a copper sulfate leaching solution and copper slag containing noble metals;
4) And adding the displaced liquid into a pressurized reaction kettle, and controlling the temperature to be 180 ℃, the time to be 0.5h and the oxygen partial pressure to be 0.3MPa to perform pressurized iron removal. After the reaction is finished, carrying out solid-liquid separation to obtain iron-removed liquid and iron slag;
5) And evaporating and crystallizing the iron-removed solution to obtain crude nickel cobalt sulfate crystals and a crystallization mother solution, returning one part of the crystallization mother solution to the normal-pressure leaching process, and returning the other part of the crystallization mother solution to the pressure leaching process.
The main ingredients of the crude nickel cobalt sulfate crystal, copper slag and iron slag are shown in Table 4.
Table 4 example 2 major output composition (%)
Example 3
The mass percentages of the main elements of the nickel matte in the present example are shown in table 5.
Table 5 main element content (%) -of nickel matte in example 3
The specific implementation process comprises the following steps:
1) Adding water into the nickel matte shown in the table 5 for slurrying, adding the slurried nickel matte into an atmospheric pressure closed leaching reaction kettle, adding part of crystallization mother liquor obtained in the evaporation crystallization process into the atmospheric pressure closed leaching reaction kettle, controlling the liquid-solid volume mass ratio to be 6;
2) Adding the normal-pressure reaction slurry and the pressure leached copper sulfate solution into a pressure reaction kettle, carrying out pressure displacement leaching, controlling the leaching temperature to be 180 ℃ and the leaching time to be 3 hours. After the reaction is finished, carrying out solid-liquid separation to obtain pressurized displacement liquid and displacement slag;
3) Pulping the replacement slag by adopting evaporation crystallization condensed water, adding the pulp into a pressurized reaction kettle, adding a certain amount of crystallization mother liquor (the rest of the crystallization mother liquor required by atmospheric pressure leaching), controlling the liquid-solid volume-mass ratio to be 6, heating, introducing oxygen for pressurized leaching, and controlling the leaching temperature to be 180 ℃, the time to be 1.5h and the oxygen partial pressure to be 0.3MPa. After the reaction is finished, carrying out solid-liquid separation to obtain a copper sulfate leaching solution and copper slag containing noble metals;
4) And adding the displaced liquid into a pressurized reaction kettle, and controlling the temperature to be 200 ℃, the time to be 1h and the oxygen partial pressure to be 0.2MPa to perform pressurized iron removal. After the reaction is finished, carrying out solid-liquid separation to obtain iron-removed liquid and iron slag;
5) And evaporating and crystallizing the iron-removed solution to obtain crude nickel cobalt sulfate crystals and a crystallization mother solution, returning one part of the crystallization mother solution to the normal-pressure leaching process, and returning the other part of the crystallization mother solution to the pressure leaching process.
The main ingredients of the crude nickel cobalt sulfate crystal, copper slag and iron slag are shown in Table 6.
Table 6 example 3 major product composition (%)
Example 4
The mass percentages of the main elements of nickel matte in this example are shown in table 7.
Table 7 main element content (%) -of nickel matte in example 4
The specific implementation process comprises the following steps:
1) Adding water into the nickel matte shown in the table 7 for slurrying, adding the slurried nickel matte into an atmospheric pressure closed leaching reaction kettle, adding part of crystallization mother liquor obtained in the evaporation crystallization process into the atmospheric pressure closed reaction kettle, controlling the liquid-solid volume mass ratio to be 4;
2) Adding the normal pressure reaction slurry and the copper sulfate solution subjected to pressure leaching into a pressure reaction kettle, performing pressure displacement leaching, and controlling the leaching temperature to be 160 ℃ and the leaching time to be 5 hours. After the reaction is finished, carrying out solid-liquid separation to obtain pressurized displacement liquid and displacement slag;
3) And pulping the replacement slag by adopting evaporative crystallization condensed water, adding the pulp into a pressurized reaction kettle, adding a certain amount of crystallization mother liquor (the rest of the crystallization mother liquor required by atmospheric pressure leaching), controlling the liquid-solid volume-mass ratio to be 4, heating, introducing oxygen for pressurized leaching, and controlling the leaching temperature to be 170 ℃, the time to be 2 hours and the oxygen partial pressure to be 0.2MPa. After the reaction is finished, carrying out solid-liquid separation to obtain a leached copper sulfate solution and copper slag containing noble metals;
4) And adding the displaced liquid into a pressurized reaction kettle, and controlling the temperature to be 215 ℃, the time to be 2 hours and the oxygen partial pressure to be 0.1MPa to perform pressurized iron removal. After the reaction is finished, carrying out solid-liquid separation to obtain iron-removed liquid and iron slag;
5) And evaporating and crystallizing the iron-removed solution to obtain crude nickel cobalt sulfate crystals and a crystallization mother solution, wherein one part of the crystallization mother solution returns to the atmospheric pressure leaching process, and the other part of the crystallization mother solution returns to the pressure leaching process.
The main ingredients of the crude nickel cobalt sulfate crystals, copper slag and iron slag are shown in Table 8.
Table 8 example 4 main product composition (%)
Aiming at the nickel matte produced by pyrometallurgical smelting, the invention provides a full-wet treatment process with simple process and low cost, which utilizes the cyclic leaching of copper in raw materials to realize the separation and enrichment of valuable metals such as nickel, copper and the like, recycles sulfuric acid produced by iron removal, and realizes no wastewater and no waste residue discharge in the full process.
Claims (3)
1. A method for recovering valuable metals from nickel matte in copper sulfate circulating leaching is characterized by comprising the following steps:
a) Leaching under normal pressure: adding water into the nickel matte to pulp, adding the pulp into an atmospheric pressure closed leaching reaction kettle, adding a part of crystallization mother liquor produced in the step e) into the atmospheric pressure closed reaction kettle, controlling the mass ratio of liquid to solid to be 4;
b) Pressure replacement: after the atmospheric pressure leaching reaction is finished, adding the reaction slurry and the copper sulfate solution obtained in the step c) into a pressurized reaction kettle, heating to carry out pressurized displacement leaching, controlling the leaching temperature to be 150-200 ℃ and the time to be 2-6 h, and carrying out solid-liquid separation after the reaction is finished to obtain a pressurized displacement liquid and displacement slag;
c) Pressure leaching: pulping the replacement slag obtained in the step b) by using evaporative crystallization condensed water obtained in the step e), adding the pulped replacement slag into a pressurized reaction kettle, simultaneously adding part of crystallization mother liquor produced in the step e) into the pressurized reaction kettle, controlling the mass ratio of liquid to solid to be 4 to 1 to 6, heating, introducing oxygen to carry out pressurized leaching, controlling the leaching temperature to be 150 to 180 ℃, the time to be 1 to 3 hours and the oxygen partial pressure to be 0.1 to 0.3MPa, and carrying out solid-liquid separation after the reaction is finished to obtain a copper sulfate solution and copper slag;
d) Pressurizing and deironing: adding the displaced liquid obtained in the step b) into a pressurized reaction kettle, introducing oxygen after the temperature reaches the reaction requirement, performing pressurized iron removal, controlling the iron removal temperature to be 180 to 220 ℃, the time to be 0.5 to 2h and the oxygen partial pressure to be 0.1 to 0.3MPa, and performing solid-liquid separation after the reaction is finished to obtain iron-removed liquid and iron slag;
e) Evaporation and crystallization: evaporating and crystallizing the iron-removed solution obtained in the step d) to obtain crude nickel cobalt sulfate crystals and a crystallization mother solution, wherein one part of the crystallization mother solution returns to the atmospheric pressure leaching process, and the other part returns to the pressure leaching process.
2. The method for recovering valuable metals from nickel matte in copper sulfate circulating leaching, as claimed in claim 1, wherein the nickel matte is derived from low-iron nickel matte obtained by converting low-nickel matte produced in the pyrometallurgical smelting of nickel sulfide ores through a converter, and the main components of the nickel matte comprise, by weight: 25-35% of Ni, 16-22% of Cu, 16-20% of Fe, 0.34-0.70% of Co and 18-24% of S.
3. The method for recovering valuable metals from nickel matte in copper sulfate circulating leaching process as claimed in claim 1, wherein the atmospheric leaching time is 2 to 5 hours.
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