CN110745858A - Method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag - Google Patents
Method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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
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Abstract
The invention discloses a method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag, which can leach copper ions in the copper slag in a short time without introducing new impurity particles by a combined method of oxidation leaching, neutralization precipitation, evaporation and cooling crystallization, successfully separate the copper ions from copper ions in a solution by using the difference of the pH value of heavy metal ion precipitation, control the specific gravity and the cooling temperature of the evaporated solution by using evaporation equipment, and perform evaporation, cooling and crystallization on the purified solution to obtain the high-quality copper sulfate pentahydrate. The method successfully converts the copper slag originally abandoned in the slag yard into the high-quality copper sulfate pentahydrate with higher added value by using a simple, convenient, efficient and low-cost mode. The copper sulfate pentahydrate product prepared by the method reaches the industrial standard YS/t94-2007 first-grade product, and brings good economic and environmental benefits for enterprises.
Description
Technical Field
The invention relates to the technical field of metal smelting, in particular to a method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag.
Background
The conventional treatment method for the residual copper slag after zinc smelting comprises the following steps: high-temperature roasting-conventional leaching, catalyst dissolution, liquid-phase air, oxygen pressure leaching, etc., and the leachate is usually subjected to concentration crystallization treatment. The high-temperature roasting-conventional leaching method has high energy consumption and needs waste gas treatment facilities, the catalyst dissolution method generally introduces new medicament or impurity ions, the reaction rate of the liquid-phase air method is too slow, the pressure required by the oxygen pressure leaching method is high, and the requirement on reaction equipment is high.
The above-mentioned several copper slag treatment methods have the disadvantages of complicated process, high energy consumption, limited application range, complex operation, high treatment cost and low added value.
Disclosure of Invention
The invention aims to provide a method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag, which successfully separates heavy metal ions from copper ions in a solution by using the difference of the pH values of heavy metal ion precipitates through a combined method of oxidation leaching, neutralization precipitation, evaporation and cooling crystallization.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag comprises the following steps:
step one, acid leaching: weighing a certain amount of copper slag, crushing the copper slag, and adding the crushed copper slag into a sulfuric acid solution for dissolving, wherein the mass ratio of the sulfuric acid solution to the copper slag is 2-3: 1; controlling the temperature of the solution to be 60-90 ℃, and carrying out acid leaching reaction for 0.5-2 h to ensure that the metal Cu is2+、Zn2+Part of Cd2+、Fe3+、Fe2+、Co2+、Sb3+Part of Bi3+、Ca2+The ions enter into the sulfuric acid solution;
step two, oxidation and neutralization reaction: adding an oxidant into the solution subjected to the acid leaching reaction in the step one under constant-speed stirring for oxidation reaction for 1.5-3 h, adjusting the pH of the solution to 3-4 by using an alkali liquor with the mass percentage concentration of 10-20%, performing neutralization precipitation reaction for 0.5-2 h, and performing vacuum filtration by using a vacuum pump to obtain a purified filtrate;
step three, evaporation separation: adding the filtrate obtained in the second step into a separation tank, preheating by a plate heat exchanger, and then pumping to an evaporation head tank for evaporation; the specific gravity of the solution after evaporation is controlled to be 1.01g/m3~1.60g/m3;
Step four, cooling and crystallizing: pumping the evaporated liquid prepared in the third step to a water-cooling crystallization tank for cooling crystallization, wherein the water-cooling crystallization tank is cooled by circulating water, and the cooling end point temperature is 5-30 ℃; and (4) separating the cooled slurry by using a centrifugal machine, and then carrying out vacuum filtration for 0.5-1 h to obtain copper sulfate pentahydrate crystals.
Preferably, the copper slag contains 29.22% by mass of Cu, and the copper crop phase analysis shows that the content of oxidized copper is 20.82% by mass and the content of vulcanized copper is 8.4% by mass.
Preferably, the mass percent concentration of the sulfuric acid solution in the first step is 15-30%.
Preferably, the oxidant used in the oxidation reaction in the second step is hydrogen peroxide, an ammonium persulfate solution or a sodium thiosulfate solution.
Preferably, the alkali liquor in the second step is sodium acetate solution or sodium carbonate solution or sodium oxalate solution.
Preferably, the quality of the copper sulfate pentahydrate crystal prepared in the fourth step reaches the first-grade product of the industry standard YS/t 94-2007.
According to the phase analysis result of the raw material copper slag, the specific weight of the copper in the sulfide state in the copper slag is large, and the copper sulfate cannot be completely leached by directly using a sulfuric acid solution, so that the copper in the sulfide state needs to be oxidized into copper in an oxidation state in advance, then the copper oxide is subjected to acid leaching to enable metal copper ions in the copper oxide to enter the solution, after the pH value of the copper oxide is adjusted by alkali liquor, the rest heavy metal ions are neutralized and precipitated, and then the filtrate after evolution is obtained through suction filtration.
The invention can leach copper ions in copper slag in a short time without introducing new impurity particles by a combined method of oxidation leaching, neutralization precipitation, evaporation and cooling crystallization, successfully separate the copper ions from the copper ions in the solution by using the difference of the pH value of heavy metal ion precipitation, control the specific gravity and the cooling temperature of the evaporated solution by using evaporation equipment, and perform evaporation cooling crystallization on the purified solution to obtain the high-quality copper sulfate pentahydrate.
The method has the advantages that the copper slag originally abandoned in the slag yard can be successfully converted into the high-quality copper sulfate pentahydrate with higher added value by a simple, convenient, efficient and low-cost mode. The copper sulfate pentahydrate product prepared by the method reaches the industrial standard YS/t94-2007 first-grade product, and brings good economic and environmental benefits for enterprises.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag comprises the following steps:
step one, acid leaching: balanceTaking a certain amount of copper slag, crushing the copper slag, adding the crushed copper slag into a sulfuric acid solution with the mass percentage concentration of 15% for dissolution, wherein the mass ratio of the sulfuric acid solution to the copper slag is 2: 1; controlling the temperature of the solution at 60 ℃, and carrying out acid leaching reaction for 0.5h to ensure that the metal Cu is2+、Zn2+Part of Cd2+、Fe3+、Fe2+、Co2+、Sb3+Part of Bi3+、Ca2+The ions enter into the sulfuric acid solution;
step two, oxidation and neutralization reaction: adding hydrogen peroxide into the solution obtained after the acid leaching reaction in the step one under constant-speed stirring for carrying out oxidation reaction for 1.5h, adjusting the pH of the solution to 3 by using a sodium carbonate solution with the mass percentage concentration of 10%, carrying out neutralization precipitation reaction for 0.5h, and carrying out vacuum filtration by using a vacuum pump to obtain a purified filtrate;
step three, evaporation separation: adding the filtrate obtained in the second step into a separation tank, preheating by a plate heat exchanger, and then pumping to an evaporation head tank for evaporation; the specific gravity of the solution after evaporation is controlled to be 1.08g/m3;
Step four, cooling and crystallizing: pumping the evaporated liquid prepared in the third step to a water-cooling crystallization tank for cooling crystallization, wherein the water-cooling crystallization tank is cooled by circulating water, and the cooling end point temperature is 10 ℃; and separating the cooled slurry by using a centrifugal machine, and vacuumizing and filtering for 0.5h to obtain copper sulfate pentahydrate crystals. The quality of the copper sulfate pentahydrate crystal prepared in the step four reaches the first-grade product of the industry standard YS/t 94-2007.
The copper slag contains 29.22% of Cu by mass, and the copper crop phase analysis shows that the content of oxidized copper is 20.82% by mass and the content of vulcanized copper is 8.4% by mass.
The indexes of the prepared blue copperas and impurities are shown in table 1
TABLE 1
Example 2
A method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag comprises the following steps:
step one, acid leaching: weighing a certain amount of copper slag, crushing the copper slag, adding the crushed copper slag into a sulfuric acid solution with the mass percentage concentration of 20% for dissolution, wherein the mass ratio of the sulfuric acid solution to the copper slag is 2.3: 1; controlling the temperature of the solution at 70 ℃, and carrying out acid leaching reaction for 1h to ensure that the metal Cu is2+、Zn2+Part of Cd2+、Fe3+、Fe2+、Co2+、Sb3+Part of Bi3+、Ca2+The ions enter into the sulfuric acid solution;
step two, oxidation and neutralization reaction: adding a sodium thiosulfate solution into the solution obtained after the acid leaching reaction in the step one under constant-speed stirring for carrying out oxidation reaction for 2 hours, adjusting the pH of the solution to 3.3 by using a sodium oxalate solution with the mass percentage concentration of 13%, carrying out neutralization precipitation reaction for 1 hour, and carrying out vacuum filtration by using a vacuum pump to obtain a purified filtrate;
step three, evaporation separation: adding the filtrate obtained in the second step into a separation tank, preheating by a plate heat exchanger, and then pumping to an evaporation head tank for evaporation; the specific gravity of the solution after evaporation is controlled to be 1.2g/m3;
Step four, cooling and crystallizing: pumping the evaporated liquid prepared in the third step to a water-cooling crystallization tank for cooling crystallization, wherein the water-cooling crystallization tank is cooled by circulating water, and the cooling end point temperature is 15 ℃; and (4) separating the cooled slurry by using a centrifugal machine, and performing vacuum filtration for 1h to obtain copper sulfate pentahydrate crystals. The quality of the copper sulfate pentahydrate crystal prepared in the step four reaches the first-grade product of the industry standard YS/t 94-2007.
The copper slag contains 29.22% of Cu by mass, and the copper crop phase analysis shows that the content of oxidized copper is 20.82% by mass and the content of vulcanized copper is 8.4% by mass.
The indexes of the prepared blue copperas and impurities are shown in Table 2
TABLE 2
Example 3
A method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag comprises the following steps:
step one, acid leaching: weighing a certain amount of copper slag, crushing the copper slag, adding the crushed copper slag into a sulfuric acid solution with the mass percentage concentration of 25% for dissolution, wherein the mass ratio of the sulfuric acid solution to the copper slag is 2.5: 1; controlling the temperature of the solution to be 80 ℃, and carrying out acid leaching reaction for 1.5h to ensure that the metal Cu is2+、Zn2+Part of Cd2+、Fe3+、Fe2+、Co2+、Sb3+Part of Bi3+、Ca2+The ions enter into the sulfuric acid solution;
step two, oxidation and neutralization reaction: adding hydrogen peroxide into the solution obtained after the acid leaching reaction in the step one under constant-speed stirring for carrying out oxidation reaction for 2.5 hours, adjusting the pH of the solution to 3.5 by using a sodium carbonate solution with the mass percentage concentration of 16%, carrying out neutralization precipitation reaction for 1.5 hours, and carrying out vacuum filtration by using a vacuum pump to obtain a purified filtrate;
step three, evaporation separation: adding the filtrate obtained in the second step into a separation tank, preheating by a plate heat exchanger, and then pumping to an evaporation head tank for evaporation; the specific gravity of the solution after evaporation is controlled to be 1.4g/m3;
Step four, cooling and crystallizing: pumping the evaporated liquid prepared in the third step to a water-cooling crystallization tank for cooling crystallization, wherein the water-cooling crystallization tank is cooled by circulating water, and the cooling end point temperature is 20 ℃; and after cooling, separating the slurry by using a centrifugal machine, and then carrying out vacuum filtration for 0.8h to obtain copper sulfate pentahydrate crystals. The quality of the copper sulfate pentahydrate crystal prepared in the step four reaches the first-grade product of the industry standard YS/t 94-2007.
The copper slag contains 29.22% of Cu by mass, and the copper crop phase analysis shows that the content of oxidized copper is 20.82% by mass and the content of vulcanized copper is 8.4% by mass.
The indexes of the prepared blue copperas and impurities are shown in Table 3
TABLE 3
Example 4
A method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag comprises the following steps:
step one, acid leaching: weighing a certain amount of copper slag, crushing the copper slag, adding the crushed copper slag into a sulfuric acid solution with the mass percentage concentration of 30% for dissolution, wherein the mass ratio of the sulfuric acid solution to the copper slag is 3: 1; controlling the temperature of the solution to be 85 ℃, and carrying out acid leaching reaction for 2 hours to ensure that the metal Cu is2+、Zn2+Part of Cd2+、Fe3+、Fe2+、Co2+、Sb3+Part of Bi3+、Ca2+The ions enter into the sulfuric acid solution;
step two, oxidation and neutralization reaction: adding hydrogen peroxide into the solution obtained after the acid leaching reaction in the step one under constant-speed stirring for carrying out oxidation reaction for 3 hours, adjusting the pH of the solution to 4 by using a sodium acetate solution with the mass percentage concentration of 20%, carrying out neutralization precipitation reaction for 2 hours, and carrying out vacuum filtration by using a vacuum pump to obtain a purified filtrate;
step three, evaporation separation: adding the filtrate obtained in the second step into a separation tank, preheating by a plate heat exchanger, and then pumping to an evaporation head tank for evaporation; the specific gravity of the solution after evaporation is controlled to be 1.6g/m3;
Step four, cooling and crystallizing: pumping the evaporated liquid prepared in the third step to a water-cooling crystallization tank for cooling crystallization, wherein the water-cooling crystallization tank is cooled by circulating water, and the cooling end point temperature is 30 ℃; and (4) separating the cooled slurry by using a centrifugal machine, and performing vacuum filtration for 1h to obtain copper sulfate pentahydrate crystals. The quality of the copper sulfate pentahydrate crystal prepared in the step four reaches the first-grade product of the industry standard YS/t 94-2007.
The copper slag contains 29.22% of Cu by mass, and the copper crop phase analysis shows that the content of oxidized copper is 20.82% by mass and the content of vulcanized copper is 8.4% by mass.
The indexes of the prepared blue copperas and impurities are shown in Table 4
TABLE 4
Claims (6)
1. A method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag is characterized by comprising the following steps: it comprises the following steps:
step one, acid leaching: weighing a certain amount of copper slag, crushing the copper slag, and adding the crushed copper slag into a sulfuric acid solution for dissolving, wherein the mass ratio of the sulfuric acid solution to the copper slag is 2-3: 1; controlling the temperature of the solution to be 60-90 ℃, and carrying out acid leaching reaction for 0.5-2 h to ensure that the metal Cu is2+、Zn2+Part of Cd2+、Fe3+、Fe2+、Co2+、Sb3+Part of Bi3+、Ca2+The ions enter into the sulfuric acid solution;
step two, oxidation and neutralization reaction: adding an oxidant into the sulfuric acid solution subjected to the acid leaching reaction for oxidation reaction for 1.5-3 hours under constant-speed stirring, adjusting the pH of the solution to 3-4 by using an alkali liquor with the mass percentage concentration of 10-20%, performing neutralization precipitation reaction for 0.5-2 hours, and performing vacuum filtration by using a vacuum pump to obtain a purified filtrate;
step three, evaporation separation: adding the filtrate obtained in the second step into a separation tank, preheating by a plate heat exchanger, and then pumping to an evaporation head tank for evaporation; the specific gravity of the solution after evaporation is controlled to be 1.01g/m3~1.60g/m3;
Step four, cooling and crystallizing: pumping the evaporated liquid prepared in the third step to a water-cooling crystallization tank for cooling crystallization, wherein the water-cooling crystallization tank is cooled by circulating water, and the cooling end point temperature is 5-30 ℃; and (4) separating the cooled slurry by using a centrifugal machine, and then carrying out vacuum filtration for 0.5-1 h to obtain copper sulfate pentahydrate crystals.
2. The method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag as claimed in claim 1, wherein the method comprises the following steps: the copper slag contains 29.22% of Cu by mass, and the copper crop phase analysis shows that the content of oxidized copper is 20.82% by mass and the content of vulcanized copper is 8.4% by mass.
3. The method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag as claimed in claim 1, wherein the method comprises the following steps: the mass percentage concentration of the sulfuric acid solution in the first step is 15-30%.
4. The method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag as claimed in claim 1, wherein the method comprises the following steps: and the oxidant used in the oxidation reaction in the second step is hydrogen peroxide or an ammonium persulfate solution or a sodium thiosulfate solution.
5. The method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag as claimed in claim 1, wherein the method comprises the following steps: and in the second step, the alkali liquor is sodium acetate solution, sodium carbonate solution or sodium oxalate solution.
6. The method for preparing high-quality copper sulfate pentahydrate by using zinc smelting copper slag as claimed in claim 1, wherein the method comprises the following steps: the quality of the copper sulfate pentahydrate crystal prepared in the fourth step reaches the first-grade product of the industry standard YS/t 94-2007.
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Cited By (2)
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CN114107670A (en) * | 2021-11-24 | 2022-03-01 | 白银有色集团股份有限公司 | Method for recovering copper sulfate crystals from waste copper slag |
CN115612848A (en) * | 2022-10-27 | 2023-01-17 | 昆明理工大学 | Method for reducing copper content in zinc purification slag by ultrasonically activating persulfate |
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CN102815740A (en) * | 2012-08-03 | 2012-12-12 | 西北矿冶研究院 | Production method for improving copper sulfate grade |
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CN102815740A (en) * | 2012-08-03 | 2012-12-12 | 西北矿冶研究院 | Production method for improving copper sulfate grade |
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巫旭等: "铜渣生产硫酸铜的试验研究", 《矿冶》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114107670A (en) * | 2021-11-24 | 2022-03-01 | 白银有色集团股份有限公司 | Method for recovering copper sulfate crystals from waste copper slag |
CN115612848A (en) * | 2022-10-27 | 2023-01-17 | 昆明理工大学 | Method for reducing copper content in zinc purification slag by ultrasonically activating persulfate |
CN115612848B (en) * | 2022-10-27 | 2024-05-24 | 昆明理工大学 | Method for reducing copper content in zinc purification slag by ultrasonic activation of persulfate |
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