CN113943004A - Method for comprehensively recycling copper-nickel sulfide ore smelting slag - Google Patents
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Abstract
The invention relates to a method for comprehensively utilizing smelting slag of copper-nickel sulfide ore in a recycling manner, which comprises the following steps: s1, mixing, grinding and roasting the smelting slag of the copper-nickel sulfide ore and an activating assistant (sodium hydroxide/sodium carbonate) to obtain active clinker, and collecting furnace gas generated by roasting in the process; s2, leaching the active clinker with water to obtain water leaching residues and water leaching solution; s3, carbonizing and decomposing the water extract, and filtering to obtain silica gel and filtrate; concentrating the filtrate, and then applying to S1; s4, purifying and burning the roasting furnace gas, introducing water to obtain sulfuric acid, adjusting the concentration to a proper value, and leaching the water leaching residue to obtain acid leaching residue and filtrate A; s5, heating and aging the filtrate A to obtain silica gel and filtrate B; s6, mixing the silica gels generated in S3 and S5, adding water, pulping and drying to obtain a white carbon black product; and S7, adjusting the pH value of the filtrate B to 1.5-4.0 to obtain ferric hydroxide and filtrate C. The method reduces the pollution of the solid wastes of mineral products to the environment on one hand, and fully utilizes the smelting slag to produce white carbon black and ferric hydroxide products with wide application value on the other hand, thereby creating considerable economic benefits.
Description
Technical Field
The invention relates to the technical field of treatment of mineral waste residues, in particular to a method for comprehensively recycling smelting slag of copper-nickel sulfide ore.
Background
Nickel metal has the advantages of good magnetism, corrosion resistance, plasticity and the like, and is widely applied to the fields of military, aerospace, aviation and the like (Xieje et al, 2018; Roxianping et al, 2013). With the rapid development of the industrialization process, the nickel consumption in China is increasing (Mayufang, 2019). A large amount of smelting slag is produced in the smelting process of copper and nickel, taking Jinchuan company as an example, the Jinchuan company currently discharges 160 ten thousand tons of nickel smelting slag and 90 thousand tons of copper smelting slag every year. Since the start of the smelting technology in 1963, about 3300 ten thousand tons of nickel-copper smelting slag is accumulated and stockpiled up to the end of 2012. In these slags, iron is 30-50%, Ni0.02% -0.5%, Cu0.1% -1%, Co0.0% -0.2% (Wangshou et al, 2015). Although the metallurgical slag contains about 40% of Fe, the comprehensive utilization of the metallurgical slag is difficult. Firstly, the artificial silicate mineral cannot be enriched by mineral separation methods such as magnetic separation and the like; secondly, Fe exists in the slag in the form of ferric silicate, and the problems of easy generation of foam slag, difficult control of furnace conditions and high energy consumption exist in reduction; meanwhile, S contained in the slag is a harmful element in the steel and iron process.
In addition, the existing copper-nickel sulfide ore smelting slag recovery process (wet leaching, flotation and heavy-flotation) has the problems of large slag discharge amount, serious environmental pollution, low comprehensive utilization rate and the like. Therefore, in order to solve the problems of environmental pollution, resource waste, land occupation and the like of the copper-nickel sulfide ore smelting slag in China and realize harmless utilization and high value-added utilization of the copper-nickel sulfide ore smelting slag in China, a method for efficiently recycling the copper-nickel sulfide ore smelting slag is urgently needed to be developed.
Disclosure of Invention
Technical problem to be solved
In view of the defects and shortcomings of the prior art, the invention provides a method for comprehensively recycling the smelting slag of copper-nickel sulfide ore, which can separate and extract iron elements in the smelting slag of copper-nickel sulfide ore into iron hydroxide products and silicon into white carbon black, and simultaneously recycle sulfur in tailings and prepare sulfuric acid for application in the process, thereby realizing the high-efficiency recycling of the smelting slag of copper-nickel sulfide ore and reducing the emission of pollutants.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the invention provides a method for comprehensively utilizing smelting slag of copper-nickel sulfide ore as resources, which comprises the following steps:
s1, mixing and grinding the smelting slag of the copper-nickel sulfide ore and the activating auxiliary agent according to the mass ratio of 1:0.5-1.5 to 200-mesh and 300-mesh, then carrying out aerobic roasting to obtain active clinker, and collecting furnace gas generated by roasting; the activating auxiliary agent is sodium carbonate or sodium hydroxide;
s2, mixing the active clinker with water, and stirring and leaching to obtain water leaching residues and a water leaching solution; the water extract contains sodium silicate; the water-immersed slag contains metal salt, silicate, metal hydroxide and metal oxide which can not be dissolved in alkali solution;
s3, slowly introducing carbon dioxide into the water extract of S2 for carbonation decomposition, filtering/centrifuging after decomposition to obtain silica gel and Na2CO3Filtering the solution; na (Na)2CO3Concentrating the filtrate, and then applying the concentrated filtrate to S1 as an activating auxiliary ingredient;
s4, dedusting, purifying and fully burning the furnace gas collected in the S1, collecting the furnace gas with water to obtain sulfuric acid, adjusting the sulfuric acid to obtain a 1.5-5.5mol/L dilute sulfuric acid solution, mixing the dilute sulfuric acid solution with the water leaching residue of the S3, and stirring and leaching to obtain acid leaching residue and filtrate A; silicate contained in the water leaching slag reacts with sulfuric acid solution to generate silicic acid which enters the filtrate A, and some metal hydroxides and metal oxides have double decomposition reaction with dilute sulfuric acid to enable part of metal elements to enter the filtrate A;
s5, heating and aging the filtrate A, and filtering/centrifugally separating to obtain silica gel and filtrate B;
s6, mixing the silica gels of S3 and S5, adding water for pulping, and performing spray drying at 80-100 ℃ to obtain a white carbon black product;
s7, adjusting the pH value of the filtrate B to 1.5-4.0, and then carrying out centrifugal separation to obtain ferric hydroxide and filtrate C.
According to the preferred embodiment of the present invention, in S1, the baking temperature is 600-900 ℃ and the baking time is 20-60 min.
According to the preferred embodiment of the invention, in S2, the active clinker is mixed with water according to the solid-to-liquid ratio of 1:5-15, the agitation leaching temperature is 25-90 ℃, and the agitation time is 5-20 min.
According to the preferred embodiment of the present invention, the end point of the carbonation decomposition reaction in S3 is that the pH value of the aqueous leach solution reaches 6-8.
According to a preferred embodiment of the invention, in S4, the furnace gas is dedusted by a deduster, cooled and dried, and then fully combusted, and the combustion product is introduced into water to obtain a sulfuric acid solution.
According to the preferred embodiment of the invention, in S4, dilute sulfuric acid solution and water leaching slag are mixed according to the solid-to-liquid ratio of 1:5-10, and stirred and leached for 3-15min at the temperature of 25-85 ℃;
the method for adjusting the concentration of the sulfuric acid solution comprises the following steps: adding concentrated sulfuric acid/evaporating concentration to increase concentration or adding water to dilute to decrease concentration to obtain 1.5-5.5mol/L dilute sulfuric acid solution.
According to the preferred embodiment of the present invention, in S5, the heating and aging temperature is 50-90 deg.C for 2-10h to fully precipitate the silica gel.
According to a preferred embodiment of the present invention, in S6, the silica gel collected in S3 and S5 is washed to neutrality with water, the washed gel is prepared into slurry with solid content of 10-40 wt%, preferably 25-35 wt%, and the slurry is spray dried at 80-100 deg.c to obtain the silica white product.
According to a preferred embodiment of the present invention, in S7, sodium hydroxide solution is added dropwise to slowly adjust the pH of filtrate B to 1.5-4.0 (preferably, pH 2-3.7), and filtration/centrifugation is performed to obtain an iron hydroxide product; wherein the mass concentration of the sodium hydroxide solution is 5-20%.
(III) advantageous effects
(1) The invention provides a method for comprehensively recycling copper-nickel sulfide ore smelting slag, which takes copper-nickel sulfide ore smelting slag as a raw material, and can separate, extract and convert silicon in the copper-nickel sulfide ore smelting slag into a white carbon black product and iron into an iron hydroxide product by combining roasting with sodium hydroxide/sodium carbonate and the like, leaching with water, leaching with acid and the like step by step, simultaneously collect furnace gas generated by roasting the smelting slag, obtain sulfuric acid by purifying and oxidizing the furnace gas, and reuse the sulfuric acid into the acid leaching procedure of the method, thereby reducing the emission of acidic gas or polluted smoke dust, reducing the acid leaching cost, realizing the efficient recycling of the copper-nickel sulfide ore smelting slag and generating considerable economic benefits.
(2) Compared with the prior art of flotation, gravity separation-flotation, direct acid leaching and the like, the method has the advantages of high comprehensive utilization rate and no environmental pollution. The invention realizes the reduction and resource treatment of the smelting slag of the copper-nickel sulfide ore, and reduces the pollution of the accumulation to the environment; meanwhile, the smelting slag of the copper-nickel sulfide ore is converted into a white carbon black product and an iron hydroxide product with wide application value, so that the high added value conversion of the waste slag is realized.
(3) The method has the advantages of simple process, no special requirement on equipment, low energy consumption, easy realization of industrialization and the like, simultaneously conforms to the environmental protection requirement (no discharge of poisonous and harmful solid wastes, furnace gas and smoke dust, and poisonous and harmful solutions and gases such as acidity, alkalinity, heavy metals and the like), and opens up a new way for the high-efficiency resource utilization of the smelting slag of the copper-nickel sulfide ore.
Drawings
Fig. 1 is a flow chart of the method for comprehensively utilizing the smelting slag of the copper-nickel sulfide ore as resources.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
As shown in fig. 1, the flow chart of the method for comprehensively utilizing the smelting slag of the copper-nickel sulfide ore as resources comprises the following processing procedures:
(1) mixing and grinding the smelting slag of the copper-nickel sulfide ore and the activating auxiliary agent according to the mass ratio of 1:0.5-1.5 to 200-mesh and 300-mesh, then carrying out aerobic roasting at the temperature of 600-mesh and 900 ℃ for 20-60min to obtain active clinker, and collecting furnace gas generated by roasting; the activating assistant is sodium carbonate or sodium hydroxide.
(2) Mixing the raw materials according to a solid-to-liquid ratio of 1:5-15, and leaching at 25-90 deg.C for 5-20min under stirring to obtain water leaching residue and water leaching solution; the water extract contains sodium silicate; the water-immersed slag contains metal salts, silicates, metal hydroxides and metal oxides which are insoluble in alkali solution.
(3) Slowly introducing carbon dioxide into the water extract obtained in step (2) for carbonation decomposition until pH is 6-8, filtering/centrifuging to obtain silica gel and Na2CO3Filtering the solution; na (Na)2CO3The filtrate is concentrated and then is used as an activating auxiliary ingredient in S1.
(4) Dedusting the furnace gas collected in the step (1) by using a dust remover, cooling and drying, then fully burning, introducing a combustion product into water to obtain a sulfuric acid solution, measuring the concentration of the sulfuric acid solution, adjusting the concentration to 1.5-5.5mol/L of a dilute sulfuric acid solution according to the condition, mixing the dilute sulfuric acid solution with the water leaching residue in the step (3) according to a solid-to-liquid ratio of 1:5-10, and stirring and leaching at the temperature of 25-85 ℃ for 3-15min to obtain acid leaching residue and filtrate A; silicate contained in the water leaching slag reacts with sulfuric acid solution to generate silicic acid which enters the filtrate A, and some metal hydroxides and metal oxides have double decomposition reaction with dilute sulfuric acid to enable part of metal elements to enter the filtrate A.
The method for adjusting the concentration of the sulfuric acid solution comprises the following steps: adding concentrated sulfuric acid/evaporating concentration to increase concentration or adding water to dilute to decrease concentration to obtain 1.5-5.5mol/L dilute sulfuric acid solution.
(5) And (3) heating the filtrate A in the step (4) to 50-90 ℃, aging for 2-10h to ensure that the silica gel is fully precipitated, and filtering/centrifuging to obtain the silica gel and filtrate B.
(6) And (3) combining the silica gels obtained in the step (3) and the step (5), washing with water to be neutral, adding water, pulping into slurry with the solid content of 10-40 wt%, preferably 25-35 wt%, and performing spray drying at 80-100 ℃ to obtain the white carbon black product.
(7) And (3) adjusting the pH of the filtrate B obtained in the step (5) to 1.5-4.0 (more preferably, pH 2-3.7) by using a sodium hydroxide solution with the mass concentration of 5-20%, and then filtering/centrifuging to obtain an iron hydroxide product and a filtrate C. Wherein, in the process of precipitating the ferric hydroxide, slowly dropwise adding a sodium hydroxide solution and slowly stirring uniformly, simultaneously monitoring the pH of the filtrate B by using a pH test electrode, beginning precipitating when the pH reaches 1.5, stopping dropwise adding the sodium hydroxide when the pH is 3.7, filtering, obtaining a ferric hydroxide product with the purity of more than 89%, and keeping metal elements such as magnesium, aluminum and the like in the filtrate C. And further dropwise adding a sodium hydroxide solution into the filtrate C to obtain aluminum hydroxide, magnesium hydroxide and the like.
SiO in the white carbon black product prepared by the method2The content is more than 92 wt%, and the BET specific surface area is more than 220m2The oil absorption value is more than 3.4mL/g, and the requirement of the white carbon black HB/T3061 is met; therefore, the white carbon black-containing white carbon black can be used for replacing carbon black for rubber reinforcement, such as pesticides, efficient spraying fertilizers and the like, white carbon black is used as a carrier or a diluent/disintegrant, daily chemical products (transparent colorful and opaque toothpaste using white carbon black as a filler and an abrasive, the toothpaste has good flexibility and dispersibility, is smooth, soft and good in abrasiveness and does not abrade a toothpaste tube body, can keep the stability of the drug property of the medicinal toothpaste), a cementing agent, an anti-caking agent and a papermaking filler, and can also be used in various industries such as fire-fighting agents, feeds, cosmetics, flatting agents, pigments, paints and the like. The ferric hydroxide product obtained by the method can be used for preparing pigments and medicines, can be used as a water purifying agent, and can also be used as an arsenic antidote and the like.
The following are preferred embodiments of the present invention.
Example 1
SiO in the smelting slag of the copper-nickel sulfide ore of the embodiment233.67% of Fe2O344.96% of the total content, 12.23% of MgO and SO3The content is 1.45%.
The embodiment provides a method for resource utilization of the copper-nickel sulfide ore smelting slag, which comprises the following main process lines:
(1) mixing the smelting slag of the copper-nickel sulfide ore with sodium carbonate according to the mass ratio of 1:1.5, grinding to 200 meshes, then carrying out aerobic roasting at 650 ℃ for 60min to obtain active clinker, and collecting furnace gas generated by roasting.
(2) Mixing the active clinker with water according to a solid-to-liquid ratio of 1:5, heating to 90 ℃, and leaching for 5min under stirring to obtain water leaching residues and water leaching solution; the water extract contains sodium silicate; the water-immersed slag contains metal salts, silicates, metal hydroxides and metal oxides which are insoluble in alkali solution.
(3) Slowly introducing carbon dioxide into the water extract obtained in the step (2) for carbonation decomposition until the pH is 6.0, and performing centrifugal separation to obtain silica gel and Na2CO3Filtering the solution; na (Na)2CO3The filtrate is concentrated and then is used as an activating auxiliary ingredient in S1.
(4) Dedusting the furnace gas collected in the step (1) by using a dust remover, cooling and drying, then fully burning, introducing the combustion product into water to obtain a sulfuric acid solution, measuring the concentration of the sulfuric acid solution, adjusting to obtain a dilute sulfuric acid solution of 5.5mol/L according to the condition, mixing the dilute sulfuric acid solution and the water leaching residue in the step (3) according to the solid-to-liquid ratio of 1:5, and stirring and leaching for 15min at the temperature of 25 ℃ to obtain acid leaching residue and filtrate A. In the process, silicate contained in the water leaching slag reacts with sulfuric acid solution to generate silicic acid which enters the filtrate A, and meanwhile, some metal hydroxides and metal oxides react with dilute sulfuric acid to generate double decomposition reaction so that part of metal elements enter the filtrate A.
(5) And (3) heating the filtrate A in the step (4) to 90 ℃, aging for 2h to ensure that the silica gel is fully precipitated, and filtering/centrifuging to obtain the silica gel and a filtrate B.
(6) And (3) combining the silica gels obtained in the step (3) and the step (5), washing with water to be neutral, adding water, pulping into slurry with the solid content of 30 wt%, and performing spray drying at 100 ℃ to obtain the white carbon black product.
SiO in the white carbon black product prepared by the method2The content was 92.3% by weight, the BET specific surface area was about 222m2/g，The oil absorption value is 3.45mL/g, and the requirement of the white carbon black HB/T3061 is met.
(7) Slowly dropwise adding a sodium hydroxide solution with the mass concentration of 5% into the filtrate B in the step (5), adjusting the pH to 3.7, stopping dropwise adding, and filtering/centrifuging to obtain an iron hydroxide product and a filtrate C, wherein the purity of the iron hydroxide product reaches 89.05%.
Example 2
SiO in the smelting slag of the copper-nickel sulfide ore of the embodiment233.67% of Fe2O344.96% of the total content, 12.23% of MgO and SO3The content is 1.45%.
The embodiment provides a method for resource utilization of the copper-nickel sulfide ore smelting slag, which comprises the following main process lines:
(1) mixing and grinding the smelting slag of the copper-nickel sulfide ore and sodium hydroxide to 250 meshes according to the mass ratio of 1:0.5, then carrying out aerobic roasting at 900 ℃ for 20min to obtain active clinker, and collecting furnace gas generated by roasting.
(2) Mixing the active clinker with water according to a solid-to-liquid ratio of 1:15, and stirring and leaching for 20min at 30 ℃ to obtain water leaching residues and water leaching liquid; the water extract contains sodium silicate; the water-immersed slag contains metal salts, silicates, metal hydroxides and metal oxides which are insoluble in alkali solution.
(3) Slowly introducing carbon dioxide into the water extract obtained in the step (2) for carbonation decomposition until the pH is 7.0, and filtering to obtain silica gel and Na2CO3Filtering the solution; na (Na)2CO3The filtrate is concentrated and then is used as an activating auxiliary ingredient in S1.
(4) Dedusting the furnace gas collected in the step (1) by using a dust remover, cooling and drying, then fully combusting, introducing the combustion product into water to obtain a sulfuric acid solution, measuring the concentration of the sulfuric acid solution, adjusting the concentration to obtain a 1.5mol/L dilute sulfuric acid solution according to the condition, mixing the dilute sulfuric acid solution and the water leaching residue in the step (3) according to the solid-to-liquid ratio of 1:5, and stirring and leaching at the temperature of 85 ℃ for 5min to obtain acid leaching residue and filtrate A. In the process, silicate contained in the water leaching slag reacts with sulfuric acid solution to generate silicic acid which enters the filtrate A, and some metal hydroxides and metal oxides have double decomposition reaction with dilute sulfuric acid to enable part of metal elements to enter the filtrate A.
(5) And (3) heating the filtrate A in the step (4) to 50 ℃, aging for 9 hours to ensure that the silica gel is fully precipitated, and filtering/centrifuging to obtain the silica gel and a filtrate B.
(6) And (3) combining the silica gels obtained in the step (3) and the step (5), washing with water to be neutral, adding water, pulping into slurry with the solid content of 25 wt%, and performing spray drying at 80 ℃ to obtain the white carbon black product.
SiO in the white carbon black product prepared by the method2The content was 92.7% by weight and the BET specific surface area was about 229m2The oil absorption value is 3.51mL/g, and the requirement of the white carbon black HB/T3061 is met.
(7) Slowly dropwise adding a sodium hydroxide solution with the mass concentration of 20% into the filtrate B in the step (5), adjusting the pH to 3.5, stopping dropwise adding, and filtering/centrifuging to obtain an iron hydroxide product and a filtrate C, wherein the purity of the iron hydroxide product reaches 90.18%.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A method for comprehensively utilizing smelting slag of copper-nickel sulfide ore as resources is characterized by comprising the following steps:
s1, mixing and grinding the smelting slag of the copper-nickel sulfide ore and the activating auxiliary agent according to the mass ratio of 1:0.5-1.5 to 200-mesh and 300-mesh, then carrying out aerobic roasting to obtain active clinker, and collecting furnace gas generated by roasting; the activating auxiliary agent is sodium carbonate or sodium hydroxide;
s2, mixing the active clinker with water, and stirring and leaching to obtain water leaching residues and a water leaching solution; the water extract contains sodium silicate; the water-immersed slag contains metal salt, silicate, metal hydroxide and metal oxide which can not be dissolved in alkali solution;
s3, slowly introducing carbon dioxide into the water extract of S2 for carbonation decomposition, filtering/centrifuging after decomposition to obtain silica gel and Na2CO3Filtering the solution; na (Na)2CO3Concentrating the filtrate, and then applying the concentrated filtrate to S1 as an activating auxiliary ingredient;
s4, dedusting, purifying and fully burning the furnace gas collected in the S1, collecting the furnace gas with water to obtain sulfuric acid, adjusting the sulfuric acid to obtain a 1.5-5.5mol/L dilute sulfuric acid solution, mixing the dilute sulfuric acid solution with the water leaching residue of the S3, and stirring and leaching to obtain acid leaching residue and filtrate A; silicate contained in the water leaching slag reacts with sulfuric acid solution to generate silicic acid which enters the filtrate A, and some metal hydroxides and metal oxides have double decomposition reaction with dilute sulfuric acid to enable part of metal elements to enter the filtrate A;
s5, heating and aging the filtrate A, and filtering/centrifugally separating to obtain silica gel and filtrate B;
s6, mixing the silica gels of S3 and S5, adding water for pulping, and performing spray drying at 80-100 ℃ to obtain a white carbon black product;
s7, the pH of the filtrate B was adjusted to 1.5 to 4.0, and the filtrate was centrifuged to obtain iron hydroxide and filtrate C.
2. The method as claimed in claim 1, wherein the calcination temperature in S1 is 600-900 ℃ and the calcination time is 20-60 min.
3. The method as claimed in claim 1, wherein in S2, active clinker is mixed with water at a solid-to-liquid ratio of 1:5-15, and the agitation leaching temperature is 25-90 ℃ and the agitation time is 5-20 min.
4. The method of claim 1, wherein the carbonation decomposition reaction is terminated at a point where the aqueous leach solution has a pH of 6 to 8 at S3.
5. The method of claim 1, wherein in S4, the furnace gas is dedusted by a deduster, cooled, dried, and then fully combusted, and the combustion product is introduced into water to obtain sulfuric acid solution.
6. The method as claimed in claim 5, wherein in S4, the dilute sulfuric acid solution and the water leaching slag are mixed according to a solid-to-liquid ratio of 1:5-10, and stirred and leached for 3-15min at a temperature of 25-85 ℃;
7. the method of claim 1, wherein the heating and aging at S5 is carried out at 50-90 deg.C for 2-10h to precipitate the silica gel sufficiently.
8. The method of claim 1, wherein in S6, the silica gel collected in S3 and S5 is washed to neutrality with water, the washed gel is prepared into slurry with solid content of 10-40 wt% by adding water, and the slurry is spray dried at 80-100 ℃ to obtain the white carbon black product.
9. The method as claimed in claim 1, wherein in S7, sodium hydroxide solution is added dropwise to slowly adjust the pH of the filtrate B to 2-3.7, and iron hydroxide product is obtained after filtration and separation; wherein the mass concentration of the sodium hydroxide solution is 5-20%.
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Cited By (2)
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| CN115583655A (en) * | 2022-11-03 | 2023-01-10 | 陕西煤业化工技术研究院有限责任公司 | Method for fractional extraction, utilization and conversion of high-calcium and high-iron gasification furnace slag elements |
| CN118006919A (en) * | 2024-04-10 | 2024-05-10 | 矿冶科技集团有限公司 | Method for improving copper sulfide ore leaching effect through cooperative treatment |
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