CN111225988B - Oxygen pressure leaching method of copper sulfide concentrate and copper smelting method - Google Patents
Oxygen pressure leaching method of copper sulfide concentrate and copper smelting method Download PDFInfo
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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
- C22B15/00—Obtaining copper
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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Abstract
An oxygen pressure leaching method of copper sulfide concentrate and a copper smelting method, wherein the copper sulfide concentrate is firstly added with water and ground into ore pulp; adding the first dispersing agent, the first alum precipitating agent, the second-stage supernatant and the ore pulp into the high-pressure kettle, and performing first-stage oxygen pressure leaching to obtain first-stage underflow and first-stage supernatant; then adding the first-stage underflow, the waste electrolyte, the second dispersing agent and the second alum precipitating agent into the high-pressure kettle, and performing second-stage oxygen pressure leaching to obtain second-stage supernatant and second-stage leaching residue; and adding a neutralizing agent into the first-stage supernatant to obtain a neutralized supernatant and neutralized slag, and electrodepositing copper by using the neutralized supernatant. The method ensures high leaching rate of copper and controls the contents of iron and sulfuric acid in the leaching solution.
Description
Technical Field
The invention relates to an oxygen pressure leaching method of copper sulfide concentrate and a copper smelting method, belonging to the technical field of non-ferrous metal hydrometallurgy.
Background
At present, copper sulfide concentrate is smelted by a pyrogenic process, copper in the copper sulfide concentrate is smelted into blister copper, then the blister copper is electrolyzed to obtain cathode copper, sulfur-containing flue gas is sent to produce acid to produce sulfuric acid, copper oxide ore and low-grade copper sulfide ore are produced into electrodeposited copper by hydrometallurgy, namely a leaching-extraction-electrodeposition process, and the sulfuric acid is not produced due to low sulfur content of raw materials. In some areas where copper sulphide concentrate is produced, sulphuric acid cannot be transported, stored and sold due to the weak industrial base around, and thus the process for pyrometallurgically smelting copper sulphide concentrate cannot be implemented. Therefore, the research on the method for producing the sulfur by similar zinc sulfide concentrate oxygen pressure leaching is applied to the hydrometallurgy method of the copper sulfide concentrate, and has very important practical significance. Although the zinc sulfide concentrate oxygen pressure leaching process has been practiced for over thirty years in industrial production, the copper sulfide concentrate oxygen pressure leaching process is only in the experimental research stage, and most of the research work content and the method route have great difference with the industrial production at present. The biggest difficulty of the oxygen pressure leaching process of the copper sulfide concentrate is that the copper leaching needs high temperature, the temperature is increased, the copper leaching rate is high, but the content of iron and sulfuric acid entering the leaching solution is increased, the subsequent procedures adopt a neutralizing agent such as limestone for acid reduction and iron removal, a large amount of neutralized slag is produced to cause copper loss, and the iron in the leaching solution is Fe3+The iron slag filtration performance is also poor. In 2007, Arizona establishes a set of 6.6 ten thousand/a copper oxygen leaching factory, the factory adopts a section of high-temperature high-pressure oxygen leaching process, the produced leaching solution is desiliconized and then carries out copper electrodeposition, most of the produced electro-hydraulic fluid is sent to copper oxide ore heap leaching for deacidification, the heap leaching solution is extracted and purified and then returns to oxygen pressure leaching, and the mixed electro-hydraulic fluid entering the high-pressure kettle is low in acidity. Therefore, the plant completely utilizes the redundant sulfuric acid produced by the oxygen pressure leaching of the copper sulfide concentrate for the heap leaching of the copper oxide ore.
However, in areas where there is not enough copper oxide ore to consume the excess sulfuric acid, it is also difficult to control the contents of iron and sulfuric acid entering the leaching solution to meet the requirements of the subsequent copper electrodeposition process while ensuring the leaching rate of copper.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an oxygen pressure leaching method of copper sulfide concentrate based on the operability of industrial production, so as to control the contents of iron and sulfuric acid in a leaching solution to meet the requirement of subsequent electrodeposition while ensuring the high leaching rate of copper; in addition, the invention also provides a copper smelting method.
In order to solve the technical problems, the technical scheme of the invention is as follows:
an oxygen pressure leaching method of copper sulfide concentrate, comprising the steps of:
s1, adding water into the copper sulfide concentrate to grind the copper sulfide concentrate into ore pulp;
s2, adding the first dispersing agent, the first alum settling agent, the secondary supernatant and the ore pulp obtained in the S1 into the autoclave to obtain the initial acid concentration (namely H)2SO4The concentration of the first slurry) is 50-70 g/L, then oxygen is introduced into the high-pressure kettle, first-stage oxygen pressure leaching is carried out under the conditions that the temperature is 135-145 ℃ and the pressure is 1.3-1.5 MPa, after the reaction is finished, the temperature and the pressure are reduced, solid-liquid separation is carried out, and first-stage underflow and first-stage supernatant are obtained;
wherein, generally, the adding amount of the first dispersing agent is 3-5 kg/t-concentrate (namely, after each ton of copper sulfide concentrate is ground into pulp, 3-5 kg of the first dispersing agent is added into the corresponding pulp), the adding amount of the first alum settling agent is 25-30 kg/t-concentrate, preferably, the adding amount of the first dispersing agent is 3.5-4.5 kg/t-concentrate, and the adding amount of the first alum settling agent is 26-28 kg/t-concentrate; h in first-stage supernatant2SO4Cu at a concentration of 25 to 35g/L2+The concentration of Fe is 90-100 g/L3+The concentration is 8-14 g/L;
s3, adding the first-stage underflow, the waste electrolyte, the second dispersing agent and the second alum precipitating agent into a high-pressure kettle to obtain second slurry with the initial acid concentration of 100-130 g/L, introducing oxygen into the high-pressure kettle, performing second-stage oxygen pressure leaching under the conditions that the temperature is 165-175 ℃ and the pressure is 1.4-1.6 MPa, cooling and depressurizing after the reaction is finished, and performing solid-liquid separation to obtain second-stage supernatant and second-stage leaching residue;
wherein, H in the waste electric hydrops2SO4The concentration is 160-180 g/L, preferably 165-175 g/L;generally, the addition amount of the second dispersing agent is 5-7 kg/t-concentrate, and the addition amount of the second alum settling agent is 30-35 kg/t-concentrate; preferably, the addition amount of the second dispersing agent is 5.5-6.5 kg/t-concentrate, and the addition amount of the second alum settling agent is 32-34 kg/t-concentrate;
adding a neutralizing agent into the first-stage supernatant, reacting to obtain neutralized slurry with the pH value of 2.5-3.5, and then carrying out solid-liquid separation to obtain neutralized supernatant and neutralized slag.
In the present invention, Cu in the supernatant is neutralized2+The concentration of Fe is 90-100 g/L3+The concentration is less than or equal to 2g/L, the pH value is 2.5-3.5, and the requirements of the copper electrodeposition process on the components of the novel electrodeposition liquid can be met.
In the invention, two-stage countercurrent oxygen pressure leaching is adopted, acid is reduced at medium temperature and pressure in one stage, copper is leached at high temperature and pressure in the second stage, wherein the supernatant of the second stage returns to the oxygen pressure leaching in the first stage to provide acid for the oxygen pressure leaching reaction in the first stage, the acid is consumed in a reaction system, the copper leached in the oxygen pressure leaching in the second stage is accumulated in a leaching solution and enters the supernatant of the first stage, the temperature and the pressure adopted in the oxygen pressure leaching in the first stage are relatively low, and the leaching rate of iron is low; meanwhile, in the two-stage oxygen pressure leaching process, an alum precipitating agent is added to inhibit the leaching of iron. Therefore, the high leaching rate of copper can be ensured, and the contents of iron and sulfuric acid in the leaching solution can be effectively controlled. In addition, in the two-stage oxygen pressure leaching reaction process, the required acid is mainly provided by the waste electrolyte.
In S1, the solid content of the ore pulp is 60-70wt%, preferably 63-68 wt%.
Further, in S1, the ore is ground through a sand mill, a stirring grinding disc of the sand mill can enable the grinding medium to be in full contact with the material, and further the grinding medium is 0.8-1 mm zirconium beads, is large in specific surface area and can fully grind the material.
In S1, the ore particles with the particle size less than 15 μm in the ore pulp account for more than 90wt% of the total amount of the minerals, and preferably account for more than 90wt% of the total amount of the minerals. Ensuring certain granularity condition, improving reaction efficiency and further improving leaching rate. In general, the mineral is understood to be a copper sulphide concentrate, and when a neutralisation slag is added, the mineral is understood to be a mixture of neutralisation slag and copper sulphide concentrate.
In S2, the reaction time of the first-stage oxygen pressure leaching is 1.5-2.5h, preferably 1.8-2.3 h.
In S2, in the first-stage oxygen pressure leaching reaction, the oxygen partial pressure in the autoclave is 0.9-1.1MPa, preferably 0.95-1.05 MPa.
In S3, the reaction time of the two-stage oxygen pressure leaching is 2.5 to 3.5 hours, preferably 2.8 to 3.3 hours.
In S3, the partial pressure of oxygen in the autoclave is 0.8-1.0MPa, preferably 0.85-0.95MPa, during the second-stage oxygen pressure leaching reaction.
Through reasonable regulation and control of reaction time, high completion degree of leaching reaction can be ensured, leaching time can be shortened, and time waste is avoided. By controlling the oxygen partial pressure, the requirements of the oxygen pressure leaching reaction process on the reaction conditions can be ensured, and the oxygen pressure leaching reaction can be efficiently carried out.
In S3, the neutralizing agent is limestone and/or copper calcine, preferably the neutralizing agent is copper calcine, neutralized slag obtained by neutralization reaction is sent to S1 for grinding and pulping, further, the mass ratio of the neutralized slag to the copper sulfide concentrate can be set according to needs, and in general, the neutralized slag and the copper sulfide concentrate can be mixed in any proportion. Further, in the copper calcine, the copper content is 18-25 wt%, the iron content is 25-35 wt%, the sulfur content is 4-6 wt%, and the balance is gangue.
The neutralizing agent is limestone, and the generated bottom flow can be subjected to filter pressing to obtain neutralized slag which can be treated in a piling mode and the like.
In S3, the waste electrolyte is copper electrodeposition waste liquid, wherein Cu2+Concentration not higher than 40g/L, Fe3+The concentration is not higher than 2 g/L.
In the invention, the dispersant and the alum precipitating agent can be both commonly used in the wet smelting and leaching treatment process of nonferrous metals, and further, the dispersant can be lignosulfonate and the alum precipitating agent can be ammonium salt or alkali.
In the invention, the solid-liquid separation process can be carried out by adopting a thickener.
In the present invention, the concentration of oxygen introduced into the autoclave is not less than 99%.
The oxygen pressure leaching method of the invention can be suitable for leaching treatment of copper sulfide concentrates of different grades.
Based on the same inventive concept, the invention also provides a copper smelting method, which comprises the steps of leaching copper sulfide concentrate according to the oxygen pressure leaching method to obtain a neutralized supernatant; and then taking the neutralized supernatant as electro-deposition liquid, and electro-depositing to obtain electro-deposited copper and copper electro-deposition waste liquid.
Further, in the electrodeposition process, the current density is controlled to be 160-180A/m2The electrodeposition cycle was 7 days.
The main reactions involved in the present invention are as follows:
CuFeS2+O2+2H2SO4→CuSO4+FeSO4+2S0+2H2O (1)
2FeSO4+0.5O2+H2SO4→Fe2(SO4)3+H2O (2)
Fe2(SO4)3+3H2O→Fe2O3+3H2SO4 (3)
3Fe2(SO4)3+2(A)OH+10H2O→2(A)Fe3(SO4)2(OH)6+5H2SO4 (4)
wherein A is selected from Na+、K+、NH4 +(ii) a The reactions (1), (2), (3) and (4) mainly occur in the oxygen pressure leaching process.
Compared with the prior art, the invention has the following beneficial effects:
(1) materials such as copper sulfide concentrate and the like are fully ground into ore pulp, so that the leaching efficiency and the leaching rate are improved.
(2) Two-stage countercurrent oxygen pressure leaching is adopted, waste electrolyte is directly leached out to obtain a first-stage underflow in the second-stage oxygen pressure leaching, and a first-stage supernatant component (H) is produced after first-stage oxygen pressure leaching deacidification of a second-stage supernatant2SO4Cu at a concentration of 25 to 35g/L2+At a concentration of90～100g/L，Fe3+The concentration is 8-14 g/L), and after the first-stage supernatant is subjected to neutralization treatment, the obtained neutralized supernatant can meet the component requirements (Cu) of the traditional copper electrodeposition novel liquid2+The concentration of Fe is 90-100 g/L3+The concentration is 2g/L, and the pH is 2.5-3.5).
(3) The iron is removed under the condition of high temperature and high acid, and the iron is directly deposited in the autoclave in the form of alum slag, so that the problem of high iron content in the supernatant fluid obtained by copper oxygen pressure leaching is solved.
(4) The first-stage supernatant is neutralized by a neutralizing agent, so that part of impurities such as iron, arsenic and the like in the solution can be removed in addition to the sulfuric acid, solvent extraction is not needed, the impurity content is further reduced, the requirements of the working condition of the electrodeposited copper can be met, and the process flow and equipment configuration are simplified.
(5) The leaching rate of copper can be improved by two-stage countercurrent oxygen pressure leaching, the total leaching rate of copper in the two-stage oxygen pressure leaching can reach more than 90 percent, and the supernatant in one stage has low acid and iron, the used neutralization dosage is small, the slag amount is small, and the copper loss is small. And (4) carrying out flotation on copper which is not leached in the second-stage leaching residue to recover copper and sulfur.
(6) The waste electrolyte generated by smelting can be effectively utilized, the production cost can be reduced, and the resource recycling is realized.
Drawings
FIG. 1 is a flow chart of a copper smelting process of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
100g of copper sulfide concentrate (containing Cu22.81wt% and Fe27.22wt%) is ground until the granularity of 90% of the concentrate is less than 15 mu m, and ore pulp is obtained. Adding the second-stage supernatant, 0.4g of dispersant, 2.5g of alum precipitating agent and ore pulp into an autoclave, controlling the liquid-solid ratio to be 4:1, introducing oxygen, controlling the temperature to be 135 ℃ and the pressure to be 1.3MPa, carrying out first-stage oxygen pressure leaching, reacting for 2h, obtaining 370mL of first-stage supernatant and first-stage underflow, wherein the first-stage supernatant contains 90.78g/L of Cu and 90.81g/L, H g of Fe10.8178 g/L2SO428 g/L. Sending the generated first-stage underflow into a second-stage autoclave, and adding waste electrolyte, 0.6g of dispersing agent and precipitated alum3g of agent, controlling the liquid-solid ratio to be 4:1, introducing oxygen, controlling the temperature to be 165 ℃ and the pressure to be 1.4MPa, carrying out two-stage oxygen pressure leaching, reacting for 2.5h, and generating 70g of two-stage leaching residue (containing Cu3.1wt% and Fe33.7wt%), the total leaching rate of two-stage copper is 90.49%, and the total leaching rate of iron is 13.34%.
Example 2
100g of copper sulfide concentrate (containing Cu22.81wt% and Fe27.22wt%) is ground until the granularity of 90% of the concentrate is less than 15 mu m, and ore pulp is obtained. Adding the second-stage supernatant, 0.5g of dispersant, 3g of alum precipitating agent and ore pulp into an autoclave, controlling the liquid-solid ratio to be 4:1, introducing oxygen, controlling the temperature to be 140 ℃ and the pressure to be 1.4MPa, carrying out first-stage oxygen pressure leaching, reacting for 2.5h to generate a first-stage supernatant 367mL and a first-stage underflow, wherein the first-stage supernatant contains 92.34g/L of Cu and 13.84g/L, H of FeC2SO430 g/L. And (2) sending the generated first-stage underflow into a second-stage autoclave, adding waste electrolyte, 0.7g of dispersing agent and 3.5g of alum precipitating agent, controlling the liquid-solid ratio to be 4:1, introducing oxygen, controlling the temperature to be 170 ℃, the pressure to be 1.5MPa and the reaction time to be 3h, and performing second-stage oxygen pressure leaching to generate 68g of second-stage leaching residue (containing 2.6 wt% of Cu2 and Fe33.1wt%), the total leaching rate of the two-stage copper to be 92.25% and the total leaching rate of the iron to be 17.31%.
Comparative example 1
100g of copper sulfide concentrate (containing Cu22.81wt% and Fe27.22wt%) is ground until the granularity of 90% of the concentrate is less than 15 mu m, and ore pulp is obtained. The ore pulp is mixed with a leaching agent (the concentration of sulfuric acid is 160g/L, the content of copper is 40g/L, and the content of iron is 2g/L), a proper amount of dispersing agent is added, the mixture is divided into two groups, and primary oxygen pressure leaching is carried out, and the specific test conditions and results are shown in Table 1.
Table 1 comparative example 1 first stage oxygen pressure leaching parameters and results
As can be seen from Table 1, the leachate obtained by the first-stage oxygen pressure leaching has high acid content and high iron content, and the higher the temperature is, the higher the acid content and the iron content in the leachate are, and the comparison shows that the leaching rate of iron in the comparative example is far beyond that of iron in the application.
Comparative example 2
100g of copper sulfide concentrate (containing Cu22.81wt% and Fe27.22wt%) is ground until the granularity of 90% of the concentrate is less than 15 mu m, and ore pulp is obtained. Mixing the ore pulp with a leaching agent (the concentration of sulfuric acid is 40g/L, the content of copper is 70g/L, and the content of iron is 35g/L), adding a proper amount of a dispersing agent and an alum settling agent, dividing into two groups, and carrying out primary oxygen pressure leaching, wherein the specific test conditions and results are shown in Table 2.
Table 2 comparative example 2 first stage oxygen pressure leaching parameters and results
As can be seen from table 2, the addition of the alum-precipitating agent can effectively reduce the iron content in the leaching solution, but the leaching rate of copper is also reduced, which is not favorable for obtaining high leaching rate of copper. By regulating and controlling relevant process parameters of the two-stage oxygen pressure leaching, the method can reduce the leaching rate of iron and obtain high leaching rate of copper, thereby effectively solving the contradiction.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (12)
1. The oxygen pressure leaching method of the copper sulfide concentrate is characterized by comprising the following steps of:
s1, adding water into the copper sulfide concentrate, and grinding the copper sulfide concentrate into ore pulp with solid content of 60-70 wt%;
wherein the content of Fe in the copper sulfide concentrate is 27.22 wt%;
s2, adding the first dispersing agent, the first alum settling agent, the second-stage supernatant and the ore pulp obtained in the S1 into a high-pressure kettle to obtain first slurry with the initial acid concentration of 50-70 g/L, introducing oxygen into the high-pressure kettle, performing first-stage oxygen pressure leaching at the temperature of 135-145 ℃ and under the pressure of 1.3-1.5 MPa, cooling and depressurizing after the reaction is finished, and performing solid-liquid separation to obtain first-stage underflow and first-stage supernatant;
wherein, H in the first stage supernatant2SO4Cu at a concentration of 25 to 35g/L2+The concentration of Fe is 90-100 g/L3+The concentration is 8-14 g/L;
s3, adding the first-stage underflow, the waste electrolyte, the second dispersing agent and the second alum precipitating agent into a high-pressure kettle to obtain second slurry with the initial acid concentration of 100-130 g/L, introducing oxygen into the high-pressure kettle, performing second-stage oxygen pressure leaching at the temperature of 165-170 ℃ and under the pressure of 1.4-1.6 MPa, cooling and depressurizing after the reaction is finished, and performing solid-liquid separation to obtain second-stage supernatant and second-stage leaching residue;
wherein the waste electrolyte is copper electrodeposition waste liquid, Cu2+Concentration not higher than 40g/L, Fe3+Concentration not higher than 2g/L, H in waste electric liquid2SO4The concentration is 160-180 g/L;
adding a neutralizing agent into the first-stage supernatant, reacting to obtain neutralized slurry with the pH value of 2.5-3.5, and then carrying out solid-liquid separation to obtain neutralized supernatant and neutralized slag;
wherein Cu in the supernatant is neutralized2+The concentration of Fe is 90-100 g/L3+The concentration is less than or equal to 2g/L, and the pH value is 2.5-3.5; the addition amount of the first dispersing agent is 3-5 kg/t-concentrate, and the addition amount of the first alum settling agent is 25-30 kg/t-concentrate; the addition amount of the second dispersing agent is 5-7 kg/t-concentrate, and the addition amount of the second alum settling agent is 30-35 kg/t-concentrate.
2. The process of oxygen pressure leaching of copper sulphide concentrate according to claim 1, wherein the ore pulp contains more than 90% by weight of the total amount of minerals with a particle size of less than 15 μm in S1.
3. The method of oxygen pressure leaching of copper sulfide concentrate according to claim 1, wherein in S2, the reaction time of the first stage of oxygen pressure leaching is 1.5-2.5 hours.
4. The method of oxygen pressure leaching of copper sulfide concentrate according to claim 3, wherein the reaction time of the first stage of oxygen pressure leaching is 1.8-2.3 hours.
5. The oxygen pressure leaching method of copper sulfide concentrate according to claim 1, wherein in the step S2, the partial pressure of oxygen in the autoclave is 0.9 to 1.1MPa during the first stage of the oxygen pressure leaching reaction.
6. The method of oxygen pressure leaching of copper sulfide concentrate according to claim 1, wherein the first dispersant and the second dispersant are both lignosulfonates; the first alum precipitating agent is ammonium salt or alkali, and the second alum precipitating agent is ammonium salt or alkali.
7. The method of oxygen pressure leaching of copper sulfide concentrate according to claim 1, wherein in S3, the reaction time of the second stage oxygen pressure leaching is 2.5-3.5 hours.
8. The method of oxygen pressure leaching of copper sulfide concentrate according to claim 7, wherein the secondary oxygen pressure leaching reaction time is 2.8-3.3 hours.
9. The oxygen pressure leaching method of copper sulfide concentrate according to claim 1, wherein in the second oxygen pressure leaching reaction in S3, the partial pressure of oxygen in the autoclave is 0.8-1.0 MPa.
10. The process of oxygen pressure leaching of copper sulphide concentrate according to claim 1, wherein in S3 the neutralising agent is limestone and/or copper calcine and the neutralised slag obtained from the neutralisation reaction is fed to S1 for grinding and pulping.
11. The method of oxygen pressure leaching of copper sulfide concentrate according to claim 10, wherein the neutralizing agent is copper calcine.
12. A copper smelting process, characterized in that copper sulphide concentrate is subjected to a leaching process by the oxygen pressure leaching process according to any one of claims 1-11 to obtain a neutralized supernatant; and then taking the neutralized supernatant as electro-deposition liquid, and electro-depositing to obtain electro-deposited copper and copper electro-deposition waste liquid.
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| WO2020062145A1 (en) | 2020-04-02 |
| CN111225988A (en) | 2020-06-02 |
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