CN112210661A - Method for oxygen-enriched suspension roasting of copper-cobalt sulfide ore - Google Patents
Method for oxygen-enriched suspension roasting of copper-cobalt sulfide ore Download PDFInfo
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- CN112210661A CN112210661A CN202011181605.7A CN202011181605A CN112210661A CN 112210661 A CN112210661 A CN 112210661A CN 202011181605 A CN202011181605 A CN 202011181605A CN 112210661 A CN112210661 A CN 112210661A
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/10—Roasting processes in fluidised form
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- C22B1/00—Preliminary treatment of ores or scrap
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- C22B1/06—Sulfating roasting
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- C22B15/001—Preliminary treatment with modification of the copper constituent
- C22B15/0013—Preliminary treatment with modification of the copper constituent by roasting
- C22B15/0017—Sulfating or sulfiding roasting
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- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/005—Preliminary treatment of ores, e.g. by roasting or by the Krupp-Renn process
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- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
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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
The invention provides an oxygen-enriched suspension roasting method for copper-cobalt sulfide ores, belonging to the cross field of metallurgy and chemical industry. Firstly, mixing copper cobalt sulfide ore with a circulating acid-containing solution to prepare slurry, atomizing the ore slurry into a roasting furnace, and then carrying out adjustable oxygen-enriched suspension roasting to complete a reinforced sulfation process or an oxidation process; flue gas generated by roasting is subjected to an acid making process to obtain finished sulfuric acid and an acid-containing solution; leaching the calcine with sulfuric acid, and extracting the leaching solution to obtain a copper-containing solution and a cobalt-containing solution; electrodepositing the copper-containing solution to obtain cathode copper and acid-containing solution; and recovering cobalt from the cobalt-containing solution to obtain crude cobalt hydroxide. The method solves the problem that the roasting furnace cannot normally operate due to the change of ore components in the roasting process of the copper-cobalt sulfide ore, reduces the cost of preparing acid from flue gas while improving the leaching rate of roasted copper-cobalt metal, recycles acid-containing solution and realizes zero emission of process waste acid.
Description
Technical Field
The invention belongs to the cross field of metallurgy and chemical industry, and particularly relates to a method for oxygen-enriched suspension roasting of copper cobalt sulfide ore.
Background
Copper is an indispensable basic metal in national economic development and is widely applied to the fields of electric power, machinery, traffic, buildings and the like. Cobalt is an important strategic metal, and the rapid development of the ternary battery industry is the main reason for the rapid increase of cobalt demand. The reserves of copper and cobalt in China account for 3.1 percent and 1.1 percent of the reserves of the whole world, and the external dependence degree is as high as 75.0 percent. Congo (gold) copper-cobalt ore reserves are abundant, and become one of the main overseas supply bases of cobalt and copper resources in China.
The cobalt grade of the congo (gold) copper-cobalt ore is high, the cobalt-copper ratio can reach 3:1, but the sulfur grade of the ore is unstable, and the sulfur content of part of resources is low. In addition, local infrastructure falls behind, technical equipment level is low, industrial foundation is weak, technical workers are lacked, partial auxiliary materials cannot be supplied independently and can only be imported, import price is high, various basic conditions required by the traditional pyrometallurgical treatment process are not available locally, and cobalt resources in the copper-cobalt ore cannot be recovered by pyrometallurgical treatment. Therefore, the development of a new technology for the efficient comprehensive utilization of Congo (gold) copper-cobalt ore is very important.
The existing technology for refining congo (gold) copper-cobalt ore mainly comprises roasting-leaching-extracting-electrodeposition technology, and whether the technology can be smoothly carried out depends on the roasting process. Because the sulfur grade of the copper-cobalt ore is unstable and the cobalt content of most of the ore is high, the conventional roasting technology cannot realize the self-heating roasting of the low-sulfur copper-cobalt ore, and the leaching rate of the cobalt after roasting is low.
Chinese patent CN110846496A discloses a sulfating roasting smelting method of sulfur-containing copper-cobalt concentrate, which is characterized in that sodium salt wastewater, high-grade pyrite and copper-cobalt ore are mixed into slurry and then are sent into a fluidized bed furnace through a hose pump for roasting, and roasted sand and smoke dust are subjected to acid leaching. The method realizes the roasting self-heating process by adding high-sulfur ores, but is not suitable for areas lacking of pyrite resources.
In the prior art of roasting copper and cobalt sulfide ores, high leaching rate and high SO of roasted metal exist2The acid preparation from the concentration smoke is restricted and difficult to balance. That is, if the metal leaching rate of the calcine is increased, the flue gas SO2The concentration is low, and the acid preparation cost is high; on the contrary, if the high SO is obtained2The leaching rate of calcine metal is reduced when the flue gas is concentrated; the two are restricted and difficult to balance.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides the method for oxygen-enriched suspension roasting of the copper-cobalt sulfide ore, which has high efficiency and simple flow, strengthens the roasting effect of the copper-cobalt ore, and solves the problems of high leaching rate and high SO content of roasted metal after roasting the copper-cobalt ore2The acid preparation from the concentration smoke is restricted and difficult to balance. Meanwhile, the waste acid is recycled, so that the problem of waste acid pollution is solved, and the cost for preparing acid from flue gas is reduced. The method has strong raw material adaptability, and is particularly suitable for treating low-sulfur copper ores or cobalt-rich copper-cobalt ores.
The invention is realized by the following technical scheme:
a method for oxygen-enriched suspension roasting of copper cobalt sulfide ore comprises the following steps:
(1) mixing copper-cobalt sulfide ore with circulating acid-containing solution and fully stirring to prepare ore pulp;
(2) atomizing and spraying the ore pulp into a roasting furnace to perform adjustable oxygen-enriched suspension roasting, and obtaining flue gas and calcine after completing the enhanced sulfation reaction or oxidation reaction;
(3) cooling and purifying the flue gas, and preparing acid to obtain a finished acid and an acid-containing solution; returning the acid-containing solution to the step (1) or the step (2) for recycling;
(4) adding sulfuric acid into the calcine to carry out first-stage leaching, converting sulfate or oxide in the calcine into sulfate ions to be dissolved in acid liquor, and carrying out dense separation to obtain a first-stage leaching solution and a first-stage underflow; adding sulfuric acid into the bottom flow to carry out second-stage leaching, and filtering to obtain second-stage leaching slag and second-stage leaching liquid;
(5) mixing, aging and clarifying the first-stage leachate and the second-stage leachate, and extracting to obtain a copper-containing solution and a cobalt-containing solution; obtaining cathode copper and acid-containing solution after electrodeposition of the copper-containing solution, and returning the acid-containing solution to the step (1) or the step (2) for recycling; and removing iron, precipitating cobalt and precipitating magnesium from the cobalt-containing solution to obtain crude cobalt hydroxide.
Further, in the step (1), the copper-cobalt sulfide ore is low-sulfur copper-cobalt ore or cobalt-rich copper-cobalt ore, and the mass fraction of the main chemical components is as follows: 20-65% of Cu; 0.12-8% of Co; 10-34% of S; 1.5-15% of Fe; 0.14-2.2% of Al; 0.48 to 2.5 percent of Mg.
Further, the acid in the acid-containing solution in the step (1) is sulfuric acid, the concentration of the sulfuric acid is 10-130 g/L, and the concentration of ore pulp after the mineral powder and the acid-containing solution are mixed is 65-75%.
Further, the adjustable oxygen-enriched suspension roasting in the step (2) is carried out, wherein sulfur or granular coal is sprayed in, oxygen-enriched air is blown in or a combination of the sulfur or the granular coal and the oxygen-enriched air is blown in during the roasting process, the roasting temperature is 500-800 ℃, and the roasting time is 4-12 hours. Furthermore, the adding amount of the sulfur or the granulated coal is 0-10% of the dry ore amount; the oxygen volume concentration of the oxygen-enriched air is 21-40%, and the air speed is 0.3-0.8 m/s.
Further, the volume fraction of the smoke components in the step (3) is as follows: SO (SO)2 3.5~9%，SO3 0.3~1.5%，CO2 1.0~2.2%， O2 2.8~4.5%，N225.6 to 63.4 percent. The finished product acid is sulfuric acid containing 93-98% of sulfuric acid by mass; the concentration of the acid-containing solution is 10-20 g/L. The cooling and purifying equipment is one or more of a waste heat boiler, a surface cooler, a cyclone dust collector and electric defogging equipment.
Further, the reaction temperature of the sulfuric acid leaching and the second stage leaching in the step (4) is 20-70 ℃, and the reaction time is 1-10 hours. The sulfuric acid used in the first-stage leaching and the second-stage leaching is one or a combination of 93% -98% concentrated sulfuric acid and 10-130 g/L sulfuric acid, namely, concentrated sulfuric acid can be selected for the first-stage leaching and the second-stage leaching, or dilute sulfuric acid can be selected for the first-stage leaching and the second-stage leaching, or concentrated sulfuric acid can be selected for one stage, or dilute sulfuric acid can be selected for the other stage.
The technical scheme of the invention has the following beneficial effects:
(1) the invention solves the problem that the low-sulfur copper-cobalt ore can not be roasted by self-heating in the traditional roasting process.
(2) The leaching rate of copper and cobalt metal is improved, and the economic benefit of the process is further increased.
(3) Solves the problems of high leaching rate and high SO content of calcine metal after roasting copper-cobalt ore2The problem that the acid preparation from the flue gas with concentration is restricted and difficult to balance is solved, and the low-cost acid preparation has wide application prospect.
(4) The acid-containing solution can be recycled in the process, and the waste acid is changed into valuable.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the examples, but the scope of the invention is not limited to the description.
The invention discloses a method for oxygen-enriched suspension roasting of copper sulfide cobalt ore and utilization of waste acid. As shown in figure 1, the method comprises the steps of firstly mixing copper-cobalt sulfide ore with circulating acid-containing solution and fully stirring to prepare ore pulp; atomizing the ore pulp and spraying the ore pulp into a roasting furnace to perform adjustable oxygen-enriched suspension roasting, and obtaining flue gas and roasted sand after completing the enhanced sulfation reaction or oxidation reaction; cooling and purifying the flue gas, and preparing acid to obtain a finished acid and an acid-containing solution. Sulfuric acid leaching is carried out on the calcine, so that sulfate or oxide in the calcine is converted into sulfate ions to be dissolved in acid liquor, and the first-stage leaching liquid and the first-stage underflow are obtained through concentration separation. Adding sulfuric acid into the bottom flow to carry out second-stage leaching, and filtering to obtain second-stage leaching slag and second-stage leaching liquid; and mixing, aging and clarifying the first-stage leachate and the second-stage leachate, and extracting to obtain a copper-containing solution and a cobalt-containing solution. And electrodepositing the copper-containing solution to obtain cathode copper and acid-containing solution. The electrodeposited acid-containing solution and the flue gas acid-containing solution are returned to size mixing or flue gas cooling for cyclic utilization; and removing iron, precipitating cobalt and precipitating magnesium from the cobalt-containing solution to obtain crude cobalt hydroxide.
Example 1
Copper-cobalt ore containing 22.0% of copper, 6.1% of cobalt, 24.0% of sulfur, 13.9% of iron, 0.7% of aluminum and 1.5% of magnesium and acid-containing solution (10 g/L) are mixed into ore pulp with the mass concentration of 65%, and then the ore pulp is sprayed into a roasting furnace for suspension sulfating roasting. The oxygen volume concentration of the air is 30 percent, the gas velocity is 0.3m/s, the roasting temperature is 600 ℃, and the retention time is 8 hours. After the roasting flue gas is subjected to waste heat boiler, cyclone dust collection and electric defogging purification, the volume fraction of the flue gas is as follows: SO (SO)2 4.5%，SO3 0.31%，CO2 1.5%， O23.9%， N254.8 percent, and obtaining 98 percent sulfuric acid after acid preparation. Adding 98% sulfuric acid into the calcine, and reacting for 4 hours at 50 ℃ to obtain leached ore pulp, wherein the leaching rate of copper is 97% and the leaching rate of cobalt is 94%. And (3) carrying out solid-liquid separation and CCD washing on the leached ore pulp by a thickener to obtain a copper-containing solution and a cobalt-containing solution. And (3) extracting and electrodepositing the copper-containing solution to obtain No. 1 cathode copper, and removing iron, precipitating cobalt and precipitating magnesium from the cobalt-containing solution to obtain crude cobalt hydroxide (the cobalt content is more than 38%).
Example 2
Copper-cobalt ore containing 51.8% of copper, 0.12% of cobalt, 14.9% of sulfur, 1.52% of iron, 0.72% of aluminum and 1.12% of magnesium and acid-containing solution (50 g/L) are mixed into ore pulp with the mass concentration of 75%, and then the ore pulp is sprayed into a roasting furnace to be suspended and sulfated and roasted with dry powder sulfur. The oxygen concentration of air is 38% by volume,the gas velocity is 0.4m/s, the roasting temperature is 700 ℃, and the retention time is 6 h. After the roasting flue gas is subjected to waste heat boiler, cyclone dust collection and electric defogging purification, the volume fraction of the flue gas is as follows: SO (SO)2 8.1%，SO3 0.36%，CO2 1.44%， O2 3.24%， N226.84 percent, and obtaining 98 percent sulfuric acid after acid preparation. Adding 98% sulfuric acid into the calcine, and reacting for 5 hours at 60 ℃ to obtain leached ore pulp, wherein the leaching rate of copper is 98% and the leaching rate of cobalt is 50%. And (3) carrying out solid-liquid separation and CCD washing on the leached ore pulp by a thickener to obtain a copper-containing solution and a cobalt-containing solution. And (3) extracting and electrodepositing the copper-containing solution to obtain No. 1 cathode copper, and removing iron, precipitating cobalt and precipitating magnesium from the cobalt-containing solution to obtain crude cobalt hydroxide (the cobalt content is more than 34%).
Example 3
Copper-cobalt ore containing 15.7% of copper, 4.7% of cobalt, 39.1% of sulfur, 21.3% of iron, 0.7% of aluminum and 1.5% of magnesium and acid-containing solution (70 g/L) are mixed into ore pulp with the mass concentration of 65%, and then the ore pulp is sprayed into a roasting furnace for suspension sulfating roasting. The oxygen volume concentration of the air is 21 percent, the gas velocity is 0.3m/s, the roasting temperature is 650 ℃, and the retention time is 8 hours. After the roasting flue gas is subjected to waste heat boiler, cyclone dust collection and electric defogging purification, the volume fraction of the flue gas is as follows: SO (SO)2 5.3%，SO3 0.5%，CO2 1.2%， O24.1%， N236.6 percent, and obtaining 98 percent sulfuric acid after acid preparation. Adding 98% sulfuric acid into the calcine, and reacting for 6 hours at 50 ℃ to obtain leached ore pulp, wherein the leaching rate of copper is 97% and the leaching rate of cobalt is 91%. And (3) carrying out solid-liquid separation and CCD washing on the leached ore pulp by a thickener to obtain a copper-containing solution and a cobalt-containing solution. And (3) extracting and electrodepositing the copper-containing solution to obtain No. 1 cathode copper, and removing iron, precipitating cobalt and precipitating magnesium from the cobalt-containing solution to obtain crude cobalt hydroxide (the cobalt content is more than 38%).
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. The method for oxygen-enriched suspension roasting of copper cobalt sulfide ore is characterized by comprising the following steps of:
(1) mixing copper-cobalt sulfide ore with circulating acid-containing solution and fully stirring to prepare ore pulp;
(2) atomizing and spraying the ore pulp into a roasting furnace to perform adjustable oxygen-enriched suspension roasting, and obtaining flue gas and calcine after completing the enhanced sulfation reaction or oxidation reaction;
(3) cooling and purifying the flue gas, and preparing acid to obtain a finished acid and an acid-containing solution; returning the acid-containing solution to the step (1) for pulping or returning the acid-containing solution to the cooling flue gas in the step;
(4) adding sulfuric acid into the calcine to carry out first-stage leaching, converting sulfate or oxide in the calcine into sulfate ions to be dissolved in acid liquor, and carrying out dense separation to obtain a first-stage leaching solution and a first-stage underflow; adding sulfuric acid into the bottom flow to carry out second-stage leaching, and filtering to obtain second-stage leaching slag and second-stage leaching liquid;
(5) mixing, aging and clarifying the first-stage leachate and the second-stage leachate, and extracting to obtain a copper-containing solution and a cobalt-containing solution; obtaining cathode copper and acid-containing solution after electrodeposition of the copper-containing solution, and returning the acid-containing solution to the step (1) for pulping or to the step (3) for cooling flue gas; and removing iron, precipitating cobalt and precipitating magnesium from the cobalt-containing solution to obtain crude cobalt hydroxide.
2. The method according to claim 1, wherein the copper-cobalt sulfide ore in the step (1) is low-sulfur copper-cobalt ore or cobalt-rich copper-cobalt ore, and the mass fraction of the main chemical components is as follows: 20-65% of Cu; 0.12-8% of Co; 10-34% of S; 1.5-15% of Fe; 0.14-2.2% of Al; 0.48 to 2.5 percent of Mg.
3. The method of claim 1, wherein the acid in the acid-containing solution in the step (1) is sulfuric acid with a concentration of 10-130 g/L, and the mass concentration of ore pulp after the ore powder and the acid-containing solution are mixed is 65-75%.
4. The method of claim 1, wherein in the step (2), the adjustable oxygen-enriched suspension roasting is carried out, sulfur or granular coal is sprayed in, oxygen-enriched air is blown in or a combination of the sulfur and the granular coal is blown in during the roasting process, the roasting temperature is 500-800 ℃, and the roasting time is 4-12 hours.
5. The method of claim 4, wherein the sulfur or coal pellets are added in an amount of 0 to 10% of the dry ore content; the oxygen volume concentration of the oxygen-enriched air is 21-40%, and the air speed is 0.3-0.8 m/s.
6. The method of claim 1, wherein the volume fraction of smoke constituents in step (3) is: SO (SO)2 3.5~9%，SO3 0.3~1.5%，CO2 1.0~2.2%， O2 2.8~4.5%， N2 25.6~63.4%。
7. The method of claim 1, wherein the finished acid in step (3) is sulfuric acid containing 93-98% by mass of sulfuric acid; the concentration of the acid-containing solution is 10-20 g/L.
8. The method of claim 1, wherein the cooling and purifying equipment in step (3) is one or more of a waste heat boiler, a surface cooler, a cyclone dust collector and an electric defogging device.
9. The method as claimed in claim 1, wherein the reaction temperature of the first stage leaching and the second stage leaching in the step (4) is 20-70 ℃, and the reaction time is 1-10 h; the sulfuric acid used in the first stage leaching and the second stage leaching is one or a combination of 93% -98% concentrated sulfuric acid and 10-130 g/L sulfuric acid.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114457243A (en) * | 2021-12-09 | 2022-05-10 | 华刚矿业股份有限公司 | Oxygen-enriched roasting method of high-copper low-sulfur copper sulfide concentrate and cathode copper |
| CN114657372A (en) * | 2022-03-01 | 2022-06-24 | 中国恩菲工程技术有限公司 | Method for extracting copper element and cobalt element from low-grade copper sulfide cobalt concentrate |
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| CN106916946A (en) * | 2017-03-30 | 2017-07-04 | 浙江华友钴业股份有限公司 | A kind of high-sulfur cobalt copper mine handling process of inexpensive leaching rate high |
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2020
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| CN108374083A (en) * | 2017-08-23 | 2018-08-07 | 赣州腾远钴业新材料股份有限公司 | A kind of new process of sulfating roasting cobalt copper sulfide ore |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114457243A (en) * | 2021-12-09 | 2022-05-10 | 华刚矿业股份有限公司 | Oxygen-enriched roasting method of high-copper low-sulfur copper sulfide concentrate and cathode copper |
| CN114657372A (en) * | 2022-03-01 | 2022-06-24 | 中国恩菲工程技术有限公司 | Method for extracting copper element and cobalt element from low-grade copper sulfide cobalt concentrate |
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Application publication date: 20210112 |