CN112080631A - Method for purifying silicon dioxide from tailings - Google Patents
Method for purifying silicon dioxide from tailings Download PDFInfo
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- CN112080631A CN112080631A CN202010766735.0A CN202010766735A CN112080631A CN 112080631 A CN112080631 A CN 112080631A CN 202010766735 A CN202010766735 A CN 202010766735A CN 112080631 A CN112080631 A CN 112080631A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/08—Chloridising roasting
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for purifying silicon dioxide from tailings, which comprises the following steps: a. uniformly mixing tailings, a sodiumizing agent and a chlorinating agent, and then roasting, wherein the mass ratio of the tailings, the sodiumizing agent and the chlorinating agent is 1:0.1-3:0.2-15, the roasting temperature is 800-; b. and (b) adding water into the roasting slag obtained in the step (a) for size mixing, and performing water leaching treatment, wherein the pH value of the solution is 1-2, and the leaching time is 1-2h, so as to obtain a metal leaching solution and silicon dioxide leaching slag. The method has wide adaptability to tailings, simple process flow and high utilization rate of metal elements and silicon-containing components in the tailings, and can realize mine tailless discharge.
Description
Technical Field
The invention belongs to the technical field of tailing treatment, and particularly relates to a method for purifying silicon dioxide from tailings.
Background
Along with the increase of the demand of national economy on mineral products, the development scale of mineral resources in China is unprecedented, but the problem of difficulty in disposal caused by the stock and incremental change of mine tailings comes with the increase. Particularly, with the improvement of the production technology level, the environmental awareness and requirements are raised, and enterprises operating mines in a rough type are difficult to adapt to the requirements of the current society and the market. The reasonable disposal of mine tailings becomes one of important factors restricting the sustainable development of mine enterprises. According to incomplete statistics, the accumulated stockpiling of the tailings in China is nearly 150 hundred million tons, 83 percent of the accumulated stockpiling is the tailings formed by mining iron ores, copper ores and gold ores, and the annual discharge amount is up to more than 15 hundred million tons. In chemical and ferrous metal mines, the amount of tailings accounts for 50 to 80 percent of the amount of ores; in the non-ferrous metal mine, the amount of tailings accounts for 70 to 95 percent of the selected ore; in rare and precious metal mines such as gold, molybdenum, tantalum, niobium and the like, the amount of tailings sometimes reaches up to 99%, and the amount of generated tailings is huge. The large accumulation of the tailings brings a lot of hazards, which not only occupies a large amount of land resources and space, but also generates a lot of secondary hazards, and damages to production, life and ecological environment become severe day by day.
It is known that mine tailings contain a large amount of valuable metals and available resources, and particularly, the mine tailings containing a large amount of metal resources in the last century of extensive operation of enterprises with low production technology level. The tailings are taken as secondary resources for recycling, the recycling of the tailings is highly regarded by mine enterprises, and the comprehensive utilization of the tailings mainly comprises three treatment methods: the method 1 is to take the tailings as secondary metal mineral resources and extract and recover valuable metals in the tailings again; the method 2 is to take the tailings as non-metal mineral resources, and select different methods to recycle the tailings according to different components of the tailings; the method 3 is to use the tailings as raw materials for producing building materials and backfill materials, and the like. Although the method introduced above can partially and effectively recover and utilize metal minerals and non-metal minerals in tailings and can obtain better effects, the three disposal methods still have problems, in method 1, after the secondary metal is recovered, the disposal problem of the non-metal minerals still needs to be faced, and the method is relatively suitable for the situation of high content of the metal minerals; when the method 2 or 3 is adopted for disposal, the problem of limitation of the content of metal minerals in the tailings is faced.
At present, in the tailing resource development and utilization technology, the utilization rate of metals or nonmetal is not high, and the added value of products in the recovery process is not high. The deep processing and high-value utilization of the tailings become the development direction of the current tailings disposal, and are an important way for relieving the environmental pressure of the tailings disposal. The silicate gangue mineral fraction in most ore tailings is large, usually SiO2The high content, often more than 50%, is a kind of potential high silicon chemical raw material with abundant reserves. However, the secondary comprehensive utilization of the tailings containing metal minerals as the raw materials of silicification industry is still very limited due to the difficulty in separating and extracting the residual metal minerals, and especially the application of the tailings in high-purity materials with high added values is limited, such as the preparation of white carbon black, molecular sieves and the like.
In conclusion, how to effectively extract and separate the metal minerals in the mine tailings and purify the non-metal minerals in the tailings to improve the added economic value of the tailings is a common problem in deep processing of most metal mine tailings. Therefore, there is an urgent need to develop efficient techniques for purifying siliceous base materials and separating and recovering metals from mine tailings.
Disclosure of Invention
The present invention is based on the discovery and recognition by the inventors of the following facts and problems:
deep processing and high-value utilization of tailings are always hot problems. The utilization efficiency of each component in the tailing materials is not high, and the separation and purification of the components are difficult; silicate in most ore sorting tailingsGangue mineral with large SiO content2The content is high, but when the silicon dioxide is used as a silicon chemical raw material, the silicon dioxide is very easily influenced by metal minerals in tailings and is limited, and particularly, the application of the silicon dioxide in preparing high-purity silicon materials is very limited, such as the preparation of white carbon black with higher added value. Although the white carbon black prepared by using tailings is more and more valued, the utilization rate is not high due to the immaturity of the preparation technology.
For the related technology of preparing white carbon black with high added value by tailings, there have been many reports, for example, CN106219558A uses gold tailings, CN106185963A uses copper tailings, CN106219559A uses nickel tailings, and CN106185963A uses graphite tailings as raw materials to prepare white carbon black, in these processes, a mixed acid system containing fluorine acid solution, hydrochloric acid and nitric acid is adopted, and it depends to some extent on hydrofluoric acid or fluosilicic acid to prepare SiO in tailings2The acid dissolution effect is difficult to popularize and apply under the condition that the emission of fluorine ions is strictly regulated. CN102234116A discloses a method for preparing nano white carbon black by using iron tailings, which comprises the steps of firstly carrying out melting roasting treatment on the iron tailings at high temperature by using caustic soda, then adding hydrochloric acid for acidification, and then preparing a nano white carbon black product by using a precipitation method. CN106044790A discloses a method for preparing white carbon black by a precipitation method, which is to purify and prepare white carbon black by using water glass as a raw material and matching with a surfactant.
Therefore, there is an urgent need to develop a tailing treatment method capable of efficiently separating metal minerals in tailings to obtain high-silicon components.
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
Therefore, the embodiment of the invention provides a method for purifying silicon dioxide from tailings, which has wide adaptability to the tailings, simple process flow and high utilization rate of metal elements and silicon-containing components in the tailings and can realize mine tailless discharge.
According to the embodiment of the invention, the method for purifying the silicon dioxide from the tailings comprises the following steps:
a. uniformly mixing the tailings, a sodiumizing agent and a chlorinating agent, and then roasting to obtain roasting smoke and roasting slag;
b. and (b) adding water into the roasting slag obtained in the step (a) for size mixing, and performing water leaching treatment to obtain a metal leaching solution and silicon dioxide leaching slag.
According to the advantages and technical effects brought by the independent claims, 1, in the embodiment of the invention, mine tailing waste is used as a raw material, the raw material is mixed with a chlorinating agent and a sodium treatment agent to carry out sodium treatment-chlorination composite isolation roasting on metal minerals, and the sodium treatment agent and the chlorinating agent are coupled with Cl in a molten state-、Na+Carrying out segregation treatment on metal minerals and metal-containing silicate components in tailings, decomposing a chlorinating agent into chlorine gas in the roasting process, carrying out ion permeation/segregation on heavy metal components in the materials by the chlorine gas so as to convert the heavy metal-containing components into volatile or soluble chloride components, adding a sodiumizing agent to reduce the decomposition temperature of the chlorinating agent so that chlorination segregation roasting can be carried out at the temperature of 800-900 ℃, and sodium ions have strong permeation and corrosion capacities on silicates so as to separate and recover residual or wrapped multiple metal components which are difficult to treat in the tailings from the tailings; 2. in the embodiment of the invention, volatile roasting smoke and segregated roasting slag are obtained after the tailings are subjected to compound segregation roasting by a chlorinating agent and a sodium treatment agent, some volatile metal chlorides enter the smoke to be recovered, the segregated roasting slag is subjected to water leaching treatment after being subjected to size mixing, metal components in the roasting slag can be fully leached in a metal ion form and dissolved in the leaching solution to be recovered, silicon-containing components are left in the leaching slag to obtain purified and enriched silicon dioxide, the content of the silicon dioxide in the leaching slag can reach more than 80%, the content of the metal is low, and the silicon dioxide can be used as a raw material for preparing white carbon black, a molecular sieve and the like; 3. the method of the embodiment of the invention takes the tailings as raw materials, is not limited by the content of metal minerals in the tailings, utilizes the strong segregation and permeability of chloride ions and sodium ions to metal and non-metal minerals to separate metal components and purify silicon-containing components in the tailings in one step, and can effectively recover silicon dioxide while purifying the mine waste tailingsThe method can be used for treating various tailings with high silicon content, and greatly widens the field of secondary processing and utilization of the tailings.
According to the embodiment of the invention, in the step a, the mass ratio of the tailings, the sodium reagent and the chlorinating agent is 1:0.1-3: 0.2-15.
The method for purifying the silicon dioxide from the tailings according to the embodiment of the invention, wherein in the step a, the sodium treatment agent is at least one selected from sodium chloride, sodium sulfate or sodium carbonate; the chlorinating agent is at least one selected from sodium chloride, magnesium chloride or ammonium chloride.
According to the method for purifying the silicon dioxide from the tailings, in the step a, the roasting temperature is 800-900 ℃, and the roasting time is 1-2 h.
According to the method for purifying the silicon dioxide from the tailings, in the step a, the dosage of the chlorinating agent is 2-5 times of the dosage of the sodium reagent.
According to the embodiment of the invention, in the step b, the liquid-solid ratio of the water to the roasting slag is 1: 2-3.
According to the embodiment of the invention, in the step b, the leaching time of the water leaching treatment is 1-2 h.
According to the embodiment of the invention, in the step b, after the calcined slag is added with water and is subjected to size mixing, the pH value of the solution is 1-2.
According to the method for purifying the silicon dioxide from the tailings, provided by the embodiment of the invention, the silica leaching residue obtained in the step b is used for preparing the white carbon black by adopting a liquid phase precipitation method or a gas phase method.
According to the embodiment of the invention, the tailings in the step a are gold tailings, copper tailings, nickel tailings, molybdenum tailings, iron tailings, lead tailings, zinc tailings, sulfur tailings or graphite tailings.
Drawings
FIG. 1 is a flow diagram of a process for purifying silica from tailings in accordance with an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
As shown in fig. 1, a method for purifying silica from tailings according to an embodiment of the present invention includes the following steps:
a. uniformly mixing the tailings, a sodiumizing agent and a chlorinating agent, and then roasting, preferably, the roasting temperature is 800-;
b. and (b) adding water into the roasting slag obtained in the step (a) for size mixing, and performing water leaching treatment to obtain a metal leaching solution and silicon dioxide leaching slag.
According to the advantages and technical effects brought by the independent claims, 1, in the embodiment of the invention, mine tailing waste is used as a raw material, the raw material is mixed with a chlorinating agent and a sodium treatment agent to carry out sodium treatment-chlorination composite isolation roasting on metal minerals, and the sodium treatment agent and the chlorinating agent are coupled with Cl in a molten state-、Na+Carrying out segregation treatment on metal minerals and metal-containing silicate components in tailings, decomposing a chlorinating agent into chlorine gas in the roasting process, carrying out ion permeation/segregation on heavy metal components in the materials by the chlorine gas so as to convert the heavy metal-containing components into volatile or soluble chloride components, adding a sodiumizing agent to reduce the decomposition temperature of the chlorinating agent so that chlorination segregation roasting can be carried out at the temperature of 800-900 ℃, and sodium ions have strong permeation and corrosion capacities on silicates so as to separate and recover residual or wrapped multiple metal components which are difficult to treat in the tailings from the tailings; 2. in the embodiment of the invention, the tailings are subjected to composite segregation roasting by a chlorinating agent and a sodium treatment agent to obtainVolatile roasting smoke and segregated roasting slag are obtained, some volatile metal chlorides enter the smoke to be recovered, the segregated roasting slag is subjected to water leaching after size mixing, metal components in the roasting slag can be fully leached and dissolved in the leachate in the form of metal ions to be recovered, silicon-containing components are left in the leaching slag to obtain purified and enriched silicon dioxide, the content of the silicon dioxide in the leaching slag can reach more than 80%, the content of the metal is low, and the silicon-containing components can be used as raw materials for preparing white carbon black, molecular sieves, ceramics, building materials and the like; 3. the method provided by the embodiment of the invention takes tailings as a raw material, is not limited by the content of metal minerals in the tailings, utilizes the strong segregation and permeability of chloride ions and sodium ions to metal and non-metal minerals to separate metal components and purify silicon-containing components in the tailings in one step, can effectively recover metal elements such as gold, copper, iron, nickel, potassium and the like in the tailings while purifying silicon dioxide from mine waste tailings, successfully avoids the technical short plate limited by the residual metal minerals in deep processing and utilization of the tailings, purifies and enriches high-silicon raw materials suitable for preparing white carbon black, can be used for treating various tailings with high silicon content, and greatly widens the field of secondary processing and utilization of the tailings.
According to the method for purifying the silicon dioxide from the tailings, in the step a, the mass ratio of the tailings, the sodium reagent and the chlorinating agent is 1:0.1-3:0.2-15, and preferably, the dosage of the chlorinating agent is 2-5 times that of the sodium reagent. In the embodiment of the invention, the mass ratio of the tailings, the sodium treatment agent and the chlorinating agent is optimized, the recovery rate of metals in the tailings and the purity of silicon dioxide can be effectively improved, the dosage of the chlorinating agent is further optimized to be 2-5 times of that of the sodium treatment agent, the chlorinating agent can fully react with heavy metal components, so that the heavy metal components are completely separated, the metal content in the purified silicon dioxide leaching residue is reduced, and the recovery rate of the metal components is improved, the dosage of the chlorinating agent is slightly more than that of the sodium treatment agent, and residual acid components on the surface of the roasting residue are facilitated, so that the pH value of the solution after size mixing in the subsequent step is acidic, and the metal leaching is facilitated, but the buffering effect is achieved due to the partial sodium treatment agent in the process, and the acidity of the solution after size mixing is not too high.
The method for purifying the silicon dioxide from the tailings according to the embodiment of the invention, wherein in the step a, the sodium treatment agent is at least one selected from sodium chloride, sodium sulfate or sodium carbonate; the chlorinating agent is at least one selected from sodium chloride, magnesium chloride or ammonium chloride. The chlorinating agent and the sodium treatment agent adopted in the embodiment of the invention are conventional raw materials, and the raw materials are low in cost and easy to obtain and are suitable for application.
According to the method for purifying the silicon dioxide from the tailings, in the step b, preferably, the liquid-solid ratio of the water to the roasting slag is 1:2-3, and the pH value of the solution after the water is added into the roasting slag for size mixing is 1-2; the leaching time of the water leaching treatment is 1-2 h. In the embodiment of the invention, the pH value of the solution after size mixing is controlled to be 1-2, the solution is acidic, the metal elements in the roasting slag can be leached and dissolved into the leaching solution, and the silicon-containing components are remained in the leaching slag and purified and enriched into the silicon dioxide leaching slag.
According to the method for purifying the silicon dioxide from the tailings, provided by the embodiment of the invention, the silica leaching residue obtained in the step b is used for preparing the white carbon black by adopting a liquid phase precipitation method or a gas phase method. The content of silicon dioxide in the leaching slag obtained by the embodiment of the invention can reach more than 80%, the surface area of the leaching slag after roasting is greatly improved by segregation roasting, and the leaching slag containing silicon dioxide is favorable for being used as a raw material for preparing the white carbon black subsequently. The leaching residue obtained in the embodiment can also be used for producing materials such as ceramics, building materials, molecular sieves and the like.
According to the method for purifying the silicon dioxide from the tailings, after the volatile roasting flue gas obtained in the step a is treated by water or alkali liquor absorption liquid, the volatile roasting flue gas and the leachate produced in the step b can be subjected to metal single or combined recovery treatment, preferably, the metal components are recovered in a precipitation mode by adjusting the pH value of the solution to 7-8, the used metal element precipitation regulator is sodium hydroxide, carbon dioxide, sodium carbonate, magnesium carbonate, calcium carbonate and the like, the metal components are precipitated and recovered to obtain metal-containing mixed precipitate and high salt solution, and the metal-containing mixed precipitate is used as a subsequent metal raw material, wherein the recovery rate of the metal elements in the tailings in the embodiment of the invention can reach more than 95%. And (c) concentrating the obtained high-salt-content solution, and distilling under reduced pressure to obtain salt products, wherein the obtained salt products can be preferably returned to the step a to be used as a sodium reagent and a chlorinating agent. The method of the embodiment of the invention relieves the influence pressure of tailing disposal on the environment, the purified silicon dioxide-containing component can be used for preparing white carbon black, the separated and recovered metal component can be used for subsequent metal processing, the high-salt backwater generated in the process can be returned to the process to be used as a chlorinating agent or a sodium treatment agent for continuous use, and the tailless treatment is really realized.
According to the method for purifying the silicon dioxide from the tailings, the tailings in the step a are gold tailings, copper tailings, nickel tailings, molybdenum tailings, iron tailings, lead tailings, zinc tailings, sulfur tailings or graphite tailings, and preferably, the content of the silicon dioxide in the tailings is more than 40% (by mass). According to the method provided by the embodiment of the invention, the tailings are used as the raw material, the limitation of the content of metal minerals in the tailings is avoided, the strong segregation and permeability of chloride ions and sodium ions to metal and non-metal minerals is utilized, the metal components are separated and the silicon-containing components in the tailings are purified in one step, the silicon material purification and metal recovery rate is high, the application range is wide, and the secondary processing and utilization range of the tailings is greatly widened.
The present invention will be described in detail with reference to examples.
Example 1
The Au content in a certain gold tailing is 0.28g/t, the Cu, Pb, Zn, Fe and S contents are 0.3%, 0.04%, 0.06%, 3.0% and 1.2% respectively, and SiO2、MgO、CaO、Al2O3The contents of the lead, copper, lead and zinc minerals are respectively 68.3%, 2.3%, 1.2%, 1.3% and 8.9%, the silicon-containing minerals in the tailings are mainly quartz, the copper, lead and zinc minerals have extremely fine occurrence and high content, and the copper, lead and zinc minerals are difficult to be secondarily processed into materials with high added values by adopting the conventional process.
As shown in figure 1, gold tailings are ground to-0.074 mm, sodium chloride is adopted as a chlorinating agent and a sodium treatment agent, and the ratio of the gold tailings: uniformly mixing sodium chloride at a mass ratio of 1:4, placing in a flue gas recoverable device, performing segregation roasting at 850 deg.C for 2 hr to obtain segregation roasting residue and roasting flue gas, wherein more than 99% of gold, copper, zinc,Lead, zinc and aluminum are collected in the flue gas, so that the separation, volatilization and separation of precious metals are realized; cooling the segregated roasting slag, mixing the cooled segregated roasting slag with a liquid-solid ratio of 1:2, adjusting the pH to 1.2, stirring and leaching the separated metal at normal temperature for 1h, dissolving more than 98 percent of iron and more than 70 percent of magnesium and calcium in tailings into the leaching solution to realize acid leaching separation of non-volatile chlorinated metal, leaving silicon-containing components in the leaching slag, and adding SiO into the leaching solution2The content reaches 93 percent, and the total component content of heavy metals in the leaching residue<0.01 percent, and then adopting sodium hydroxide to dissolve and prepare sodium silicate, and then adopting precipitation method to prepare white carbon black and white carbon black SiO2The purity is over 99 percent, and the specific surface area measured by a BET method reaches 320m2The comprehensive silicon utilization rate reaches 84% (namely the ratio of the total amount of the prepared white carbon black product to the mass of silicon dioxide in tailings); the flue gas is treated by an alkaline aqueous solution and then mixed with the leaching solution to recover metal components, the metal components are subjected to size mixing and precipitation to recover metal elements, in addition, in the process of preparing sodium silicate by dissolving leaching residues by using sodium hydroxide, a residue phase with higher calcium and magnesium contents can be obtained after the sodium hydroxide is leached, and the total metal recovery rate in the embodiment reaches more than 97%.
Example 2
The tailings obtained by sulfuration-flotation of certain mixed copper and copper ores contain 0.3 percent and 3.5 percent of Cu and Fe and K2The content of O is 5.2 percent, and the main silicon-containing components in the tailings are potassium feldspar and SiO2The content is 55 percent, the copper mineral is wrapped by limonite or feldspar, and the conventional method is difficult to separate copper from potassium.
As shown in fig. 1, the copper tailings were ground to-0.074 mm, and the weight ratio of copper tailings: sodium sulfate: uniformly mixing sodium chloride according to a mass ratio of 1:0.2:3, placing the mixture in a device capable of recycling flue gas, carrying out segregation roasting at 800 ℃ for 1h to obtain segregation roasting slag and roasting flue gas, and recovering 95% of copper and 83% of aluminum in tailings after segregation and volatilization in the flue gas; cooling the segregated roasting slag, mixing the cooled segregated roasting slag with a liquid-solid ratio of 1:3, adjusting the pH to 1.5, stirring and leaching at normal temperature to separate iron metal for 1h, dissolving more than 98% of iron and nearly 80% of potassium in tailings into leaching liquid to realize acid leaching separation of non-volatile chlorinated metal, leaving most silicon-containing components in the leaching slag, and preparing SiO2The content reaches 91 percent, and the total component content of heavy metal in the leaching residue<0.05％，Then sodium silicate is prepared by adopting sodium hydroxide to dissolve, then white carbon black is prepared by adopting a gas phase method, and obtained white carbon black SiO2The purity is over 99.5 percent, and the specific surface area measured by a BET method reaches 332m2The comprehensive silicon utilization rate reaches 88 percent; the flue gas is treated by alkaline water solution and then is subjected to size mixing and precipitation to recover copper, leaching solution is crystallized to extract potassium, the comprehensive recovery rate of copper reaches 95%, and the recovery rate of potassium is 80.2%.
Example 3
The nickel and copper contents in certain copper-nickel tailings are 0.25 percent and 0.21 percent, and the silicon-containing minerals in the tailings mainly comprise silicic acid minerals containing Mg, such as serpentine, talc, chlorite and the like, MgO and SiO2The contents are respectively 30.9% and 53.2%, and the gangue mineral has complex composition and large metal residue, and is difficult to be used for material preparation.
As shown in figure 1, the copper-nickel tailings are ground to-0.074 mm, and the weight ratio of the copper-nickel tailings: sodium carbonate: uniformly mixing ammonia chloride according to the mass ratio of 1:2:10, placing the mixture in a device capable of recycling flue gas, carrying out segregation roasting at 900 ℃ for 1.5 hours to obtain segregation roasting slag and roasting flue gas, and collecting 95% of copper and 93% of nickel in tailings after segregation and volatilization in the flue gas; cooling the segregated roasting slag, mixing the cooled segregated roasting slag with a liquid-solid ratio of 1:2 to obtain a solution with the pH of 1.0, stirring and leaching the solution at normal temperature to separate soluble components, realizing acid leaching separation of non-volatile soluble metal elements into the leaching solution, wherein the leaching slag basically exists in porous high-silicon components, SiO is2The content reaches 83 percent, and the total content of heavy metal in the leaching residue<0.05 percent, adopting sodium hydroxide to dissolve to prepare sodium silicate, then adopting a precipitation method to prepare white carbon black, and obtaining the white carbon black SiO2The purity reaches 99 percent, and the specific surface area measured by a BET method reaches 210m2The comprehensive silicon utilization rate reaches 88 percent; the method comprises the following steps of treating the flue gas with an aqueous alkali solution, recovering metal components, recovering copper and nickel through size mixing and precipitation, carrying out size mixing on a high-magnesium leaching solution, crystallizing and precipitating in the form of a basic magnesium carbonate precursor, and carrying out reduction roasting to prepare high-purity magnesium oxide powder, wherein the recovery rate of copper and nickel is more than 95% and the recovery rate of magnesium is more than 90%.
Comparative example 1
The same procedure as in example 2 was repeated, except that sodium sulfate was not added during the isolation firing at 1000 ℃.
The leaching residue obtained by the method of comparative example 1 contains 84% of silicon dioxide, 0.4% of total heavy metal and white carbon SiO2The purity is 97% (the purity is too low, and the white carbon black product is not qualified), and the specific surface area is 270m by the BET method2The comprehensive silicon utilization rate is 81 percent, the comprehensive copper recovery rate is 92 percent, and the potassium recovery rate is 65 percent.
Comparative example 2
The same procedure as in example 2 was followed, except that sodium sulfate was not added during the isolation calcination.
The leaching residue obtained by the method of comparative example 2 contains 76% of silicon dioxide, 1.2% of total heavy metal and SiO 22The purity is 95 percent (the purity is too low and is not qualified white carbon black products), and the specific surface area is 230m by the BET method2The comprehensive silicon utilization rate is 77 percent, the comprehensive copper recovery rate is 87 percent, and the potassium recovery rate is 58 percent.
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for purifying silicon dioxide from tailings is characterized by comprising the following steps:
a. uniformly mixing the tailings, a sodiumizing agent and a chlorinating agent, and then roasting to obtain roasting smoke and roasting slag;
b. and (b) adding water into the roasting slag obtained in the step (a) for size mixing, and performing water leaching treatment to obtain a metal leaching solution and silicon dioxide leaching slag.
2. A method for purifying silicon dioxide from tailings according to claim 1, wherein in the step a, the mass ratio of the tailings, the sodium reagent and the chlorinating agent is 1:0.1-3: 0.2-15.
3. A method for purifying silica from tailings according to claim 1, wherein in the step a, the sodium treatment agent is at least one selected from sodium chloride, sodium sulfate or sodium carbonate; the chlorinating agent is at least one selected from sodium chloride, magnesium chloride or ammonium chloride.
4. The method for purifying silica from tailings as claimed in claim 1, wherein the calcination temperature in step a is 800-.
5. A process for purifying silica from tailings according to claim 1 or 2, wherein in the step a, the dosage of the chlorinating agent is 2 to 5 times of the dosage of the sodifying agent.
6. A method for purifying silica from tailings as claimed in claim 1, wherein the liquid-solid ratio of water to calcine slag in the step b is 1: 2-3.
7. A process for purifying silica from tailings as claimed in claim 1, wherein the leaching time of the water leaching treatment in step b is 1-2 h.
8. A method for purifying silica from tailings as claimed in claim 1, wherein in the step b, the pH of the solution after the calcine slag is added with water and is subjected to size mixing is 1-2.
9. The method for purifying silica from tailings according to claim 1, wherein the silica leaching residue obtained in the step b is prepared into the silica by a liquid phase precipitation method or a gas phase method.
10. A process for purifying silica from tailings as claimed in claim 1, wherein the tailings in step a are gold tailings, copper tailings, nickel tailings, molybdenum tailings, iron tailings, lead tailings, zinc tailings, sulfur tailings or graphite tailings.
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| CN113979441A (en) * | 2021-10-29 | 2022-01-28 | 凯盛石墨碳材料有限公司 | Method for recycling graphite solid waste |
| CN115316508A (en) * | 2022-10-13 | 2022-11-11 | 天津冶建特种材料有限公司 | Feed additive containing silicon dioxide and preparation method thereof |
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