CN115353115A - Low-carbon high-efficiency extraction of high-purity SiO from high-silicon hematite tailings 2 Method (2) - Google Patents
Low-carbon high-efficiency extraction of high-purity SiO from high-silicon hematite tailings 2 Method (2) Download PDFInfo
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Abstract
The invention discloses a method for extracting high-purity SiO from high-silicon hematite tailings with low carbon and high efficiency 2 The preparation concentration is 20-80kg/m 3 Adding a dispersing agent into the ore pulp, and ultrasonically dispersing for 1-4min at the power of 70-200W to effectively disperse quartz and impurity particles; carrying out weak-strong superconducting high-gradient magnetic separation on ore pulp; roasting the magnetically-separated quartz coarse refined powder at 700-900 ℃ for 4-6h, taking out the quartz coarse refined powder, and performing water quenching to crack the quartz surface and expose impurity ions on the surface; pickling the water-quenched quartz coarse refined powder twice, and performing acid leaching to obtain SiO 2 High-purity SiO with content of more than or equal to 99 percent 2 . The invention not only solves the problem of preparing high-purity SiO by the prior art 2 The problems of complex process flow, environmental pollution, high operation cost and the like can be solved, and high-value recycling of useful components in the high-silicon hematite tailings can be realized; prepared high-purity SiO 2 Can effectively solve the problem of shortage of high-silicon quartz mineral resources in China.
Description
Technical Field
The invention belongs to the technical field of cyclic utilization of solid waste resources, and particularly relates to a method for efficiently extracting high-purity SiO from high-silicon hematite tailings with low carbon 2 The method of (1).
Background
Quartz is used as an industrial mineral raw material which is widely applied, has the characteristics of stable chemical property, good insulating property, high temperature resistance and the like, and is widely applied to the fields of glassware, refractory materials, ceramics, semiconductors, solar energy and the like. The main component of natural quartz is SiO 2 Often containing minor amounts of impurities such as: a1 2 O 3 、Na 2 O, caO, mgO, etc., and there are various types. With the rapid development of the technology,the demand of China for high-purity quartz increases year by year and the supply is not in demand. The price of each ton of high-purity quartz raw material with the total impurity content lower than 20ppm reaches tens of thousands yuan or even hundreds of thousands yuan RMB. China needs to import a large amount of high-purity quartz from foreign countries every year, which brings serious pressure to national economy.
Along with the increase of resource demand, mineral resources are continuously developed and utilized, and the quantity of tailings in China is huge. China is a big country for steel production, and millions of tons of residual iron tailings are mined every year. Iron tailings are stacked for a long time, so that a large amount of land is occupied, the environment around a mining area is polluted, a large amount of funds and manpower are needed for repairing and maintaining the mining area, and even accidents such as dam break of the tailings reservoir can occur. Therefore, the search for a suitable method for treating iron ore tailings is urgent. At present, the iron tailings are mainly used for paving, brick making, tailing reclamation vegetation, tailing used as fertilizer, soil improvement agent or ecological protection area building and the like, and the extensive utilization of the iron tailings causes waste of iron tailing resources. It is worth noting that the main mineral in the iron tailings is mainly quartz, the content of the main mineral can reach more than 65%, and the iron tailings also contain a certain amount of CaO and Al 2 O 3 、MgO、Fe 2 O 3 、Fe 3 O 4 And the like. In order to effectively separate, purify and recycle quartz resources in iron tailings, it is urgently needed to provide a method for purifying SiO from high-silicon iron tailings 2 The method for separating and purifying.
CN103058203B discloses a method for simultaneously extracting iron and silicon elements in solid wastes by using a superconducting magnetic separation device, and MD-004 and PFASSB reagents are added to separate and extract Fe by using the superconducting high-gradient magnetic separation device 2 O 3 And SiO 2 . The addition of PFASSB introduces new impurities, resulting in SiO 2 The content is reduced and additional reagent costs are incurred. Because the solid waste contains a large amount of magnetic or weakly magnetic particles, the superconducting high-gradient direct magnetic separation can generate a magnetic flocculation phenomenon, the separation effect is worsened, and the recovery rate of concentrate is reduced. In addition, the invention does not have SiO 2 Coarse refined powder (SiO) 2 Content (wt.)<99%) is further purified to obtain SiO 2 The coarse powder has low yield.
In the prior art, the preparation method of the high-purity quartz sand generally adopts the processes of crushing, ultrasonic scrubbing, multiple magnetic separation, microwave heating acid leaching, flotation, drying and the like, so that the iron element impurity in the prepared high-purity quartz sand can be reduced to be below 0.35mg/kg, but the flotation can generate wastewater and pollute the environment. Aiming at the purification method of the high-purity quartz sand tailings, the processes of ore grinding, strong magnetic separation, acid leaching, calcination, water quenching, cleaning and the like are generally adopted, and a leaching agent, such as a mixture of oxalic acid and thiocyanic acid, needs to be added in the acid leaching stage of the process, so that the process is complex in component, complex to operate and high in cost; the temperature setting during the calcination process is complex; the water quenching process has strict requirements on the temperature of cooling water, so the industrial production and operation cost is high.
In conclusion, the prior art has the problems of complex process flow, environmental pollution, high operation cost and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to solve the technical problem of high-purity SiO 2 Complex process flow, environmental pollution, high operation cost and the like in the preparation process. Meanwhile, the technology overcomes the magnetic flocculation phenomenon generated by superconducting high-gradient direct magnetic separation, and solves the problem of how to recycle the quartz component in the high-silicon hematite tailings. In addition, the produced high-purity quartz can effectively relieve the problem of shortage of quartz mineral resources in China.
In order to realize the purpose, the invention provides a method for extracting high-purity SiO from high-silicon hematite tailings with low carbon and high efficiency 2 The method comprises the following steps:
(1) grinding hematite tailings, adding water to prepare the hematite tailings with the concentration of 20-80kg/m 3 The ore pulp can be added with a dispersing agent and ultrasonically dispersed for 1-4min under the condition that the ultrasonic power is 70-200W, so that quartz and impurity particles in the ore pulp are effectively dispersed.
(2) Magnetic separation: carrying out weak-strong superconducting high-gradient magnetic separation on the ore pulp dispersed in the step (1) to obtain quartz coarse refined powder, wherein SiO (silicon dioxide) of the quartz coarse refined powder 2 The content is less than 99 percent.
(3) High-temperature water quenching: roasting the quartz coarse refined powder subjected to magnetic separation in the step (2) at the high temperature of 700-900 ℃ for 4-6h, and then performing water quenching.
(4) Fine purification: performing acid leaching and purification twice on the quartz coarse refined powder subjected to water quenching in the step (3), wherein primary acid washing is performed by using acid washing liquid under the conditions that the stirring speed is 120-160r/min, the temperature is 25-60 ℃, and the liquid-solid ratio is 10-15 1ml/g, and the time is 4-6h; performing secondary fine purification by performing secondary acid leaching on the leaching solution for 6-8h under the conditions that the stirring speed is 200-220r/min, the temperature is 60-80 ℃, and the liquid-solid ratio is 5-6; in order to ensure that there is sufficient H in the solution during the quartz leaching process + And complexing ions with impurities, and supplementing leachate with the solid-liquid volume of 2-5% after the second acid leaching into the reaction device every 1 h. Pickling to obtain SiO 2 High-purity SiO with mass content of 99 percent 2 。
SiO in the hematite tailings in the step (1) 2 The mass content is more than 80 percent, and the grinding is carried out until the 325-mesh passing rate is more than 80 percent; the intensity of the low-intensity magnetic separation of the superconducting high-gradient magnetic separation in the step (2) is 0.5-0.8T, and the intensity of the high-intensity magnetic separation is 4.1-5.0T. The pickling solution for the first pickling in the step (4) is a mixture of 0.5mol/L hydrofluoric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid; and (4) the leachate obtained in the second acid leaching is a mixture of 2mol/L sulfuric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid.
High-purity SiO 2 Extracting high-purity SiO from the high-silicon hematite tailings 2 The method (1) is carried out; the SiO 2 The mass content is more than or equal to 99 percent. Low-carbon and high-efficiency extraction of high-purity SiO from high-silicon hematite tailings 2 The method is applied to the recovery and utilization of the high-silicon hematite tailings.
In the above technical scheme, preferably, the concentration of the ore pulp prepared from the hematite tailings is 30-70%, and the hematite tailings are subjected to ultrasonic dispersion under the condition that the ultrasonic power is 80-120W.
In the technical scheme, preferably, the first fine purification is performed by pickling with pickling solution under the conditions that the stirring speed is 130-150r/min, the temperature is 30-60 ℃, the liquid-solid ratio is 13; and carrying out secondary acid leaching on the secondary fine purification under the conditions that the stirring speed is 210r/min, the temperature is 70 ℃, the liquid-solid ratio is 6.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts the superconducting coupling acid leaching technology to solve the problem of high-purity SiO 2 In the preparation process, the problems of complex process flow, environmental pollution, high operation cost and the like in the prior art are solved, and the high-purity SiO is prepared from the high-silicon hematite tailings 2 A new technology is provided; meanwhile, the recovery and utilization of valuable components of the high-silicon hematite tailings are developed, the tailings are recycled to the maximum extent, and remarkable economic and social benefits can be brought to enterprises and society.
(2) SiO in the prepared high-purity quartz 2 The grade is up to more than 99 percent, the method meets the standard of refined quartz sand, and can effectively relieve the problem of shortage of high-silicon quartz mineral resources in China.
(3) Compared with the conventional electromagnetism, the superconducting high-intensity magnetic purification method saves energy by about 90 percent, and is a low-carbon separation and purification technology.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples. In the embodiment, the chemical component analysis adopts an inductively coupled plasma mass spectrometer ICP-MS to measure the content of impurity elements in raw materials (hematite tailings) and products (high-purity quartz), and then adopts a subtraction method to calculate SiO 2 And (4) content. The method is exemplified by the red iron tailings of Anemata Fermentata, and the gradual purification is described through the following experimental process, so that the high-purity SiO with the content of not less than 99 percent is finally obtained 2 And (5) producing the product. The chemical composition of the feedstock (hematite tailings) in examples 1-3 is shown in table 1.
TABLE 1 hematite tailings chemical composition (wt%)
Example 1
(1) Ultrasonic dispersion: grinding the hematite tailings to reach the passing rate of 85 percent of 325 meshes, and preparing the concentration of 50kg/m by using clear water 3 The pulp of (2) is 100W strips at the ultrasonic powerUltrasonic dispersion is carried out for 4min under the part, so that quartz and impurity particles in the ore pulp are effectively dispersed.
(2) Magnetic separation: performing weak magnetic separation on the ore pulp dispersed in the step (1) at 0.5T through superconducting high-gradient magnetic separation equipment, performing strong magnetic separation at 5.0T, and performing magnetic separation to obtain SiO in the quartz coarse refined powder 2 The content is 95.201%;
(3) high-temperature water quenching: and (3) roasting the quartz coarse refined powder subjected to magnetic separation in the step (2) at a high temperature of 800 ℃ for 5 hours, taking out the quartz coarse refined powder, and putting the quartz coarse refined powder into tap water for water quenching to enable the surface of quartz to generate cracks and expose impurity ions on the surface.
(4) Fine purification: performing acid leaching and refining twice on the quartz coarse refined powder subjected to water quenching in the step (3), wherein primary acid pickling is performed by using an acid pickling solution under the conditions that the stirring speed is 140r/min, the temperature is 50 ℃, and the liquid-solid ratio is 13 1ml/g, and the time is 6h; wherein the acid washing solution is a mixture obtained by mixing 0.5mol/L hydrofluoric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid according to the volume ratio of 1.
Secondary fine purification: and performing secondary acid leaching on the quartz powder subjected to primary fine purification for 8 hours under the conditions that the stirring speed is 210r/min, the temperature is 70 ℃, and the liquid-solid ratio is 6 2 (ii) a The leaching solution is a mixture obtained by mixing 2mol/L sulfuric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid according to a volume ratio of 1. In order to ensure that there is sufficient H in the solution during the quartz leaching process + And impurity complex ions, and adding leachate with the solid-liquid volume of 5% after the second acid leaching into the reaction device every 1 h.
Finally obtained high-purity SiO 2 Measurement of high purity SiO by chemical analysis (ICP-MS) 2 The content of impurity elements is calculated by adopting a differential subtraction method 2 Content) measuring SiO 2 The content reaches 99.154 percent.
Example 2
(1) Ultrasonic dispersion: grinding the hematite tailings to reach a passing rate of 89% of 325 meshes, and preparing the concentration of 20kg/m by using clear water 3 The ore pulp of (2); adding a dispersant sodium hexametaphosphate into the red iron tailings, wherein the mass ratio of the sodium hexametaphosphate to the red iron tailings is 40g/t; then carrying out ultrasonic treatment for 4min under the condition that the ultrasonic power is 70W to ensure that the ore pulp is in the state ofThe quartz is effectively dispersed with the foreign particles.
(2) Magnetic separation: performing low-intensity magnetic separation on the ore pulp dispersed in the step (1) at 0.8T through superconducting high-gradient magnetic separation equipment, performing high-intensity magnetic separation at 4.1T, and performing magnetic separation to obtain SiO in the quartz coarse refined powder 2 The content is 96.102%;
(3) high-temperature water quenching: and (3) roasting the quartz coarse powder subjected to magnetic separation in the step (2) at a high temperature of 700 ℃ for 4 hours, taking out the quartz coarse powder, and putting the quartz coarse powder into tap water for water quenching to enable the surface of the quartz to generate cracks and expose impurity ions on the surface.
(4) Fine purification: carrying out acid leaching and refining twice on the quartz coarse refined powder subjected to water quenching in the step (3), wherein primary acid washing is carried out on the quartz coarse refined powder by using an acid washing solution under the conditions that the stirring speed is 120r/min, the temperature is 25 ℃, and the liquid-solid ratio is 15 1ml/g, and the time is 4h; the acid washing solution is a mixture obtained by mixing 0.5mol/L hydrofluoric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid according to a volume ratio of 1.
Secondary fine purification: and carrying out secondary acid leaching on the primarily purified quartz powder for 8 hours under the conditions that the stirring speed is 200r/min, the temperature is 60 ℃, and the liquid-solid ratio is 6 2 (ii) a The leaching solution is a mixture obtained by mixing 2mol/L sulfuric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid according to a volume ratio of 1. In order to ensure that there is sufficient H in the solution during the quartz leaching process + And impurity complex ions, and adding leachate with the solid-liquid volume of 2% after the second acid leaching into the reaction device every 1 h.
Finally obtained high-purity SiO 2 Measurement of high purity SiO by chemical analysis (ICP-MS) 2 The content of impurity elements in the SiO is calculated by adopting a differential subtraction method 2 Content) measuring SiO 2 The content reaches 99.691%.
Example 3
(1) Ultrasonic dispersion: grinding the hematite tailings to reach the passing rate of 90 percent of 325 meshes, and preparing the concentration of 80kg/m by using clear water 3 Adding a dispersant of sodium hexametaphosphate into the ore pulp, wherein the mass ratio of the sodium hexametaphosphate to the hematite tailings is 50g/t; then carrying out ultrasonic treatment for 1min under the condition that the ultrasonic power is 200W, so that quartz and impurity particles in ore pulp are effectively dispersed。
(2) Magnetic separation: performing low-intensity magnetic separation on the ore pulp dispersed in the step (1) at 0.6T by using superconducting high-gradient magnetic separation equipment, performing high-intensity magnetic separation at 4.8T, and performing magnetic separation on SiO in quartz coarse refined powder 2 The content is 96.301%;
(3) high-temperature water quenching: and (3) roasting the quartz coarse powder subjected to magnetic separation in the step (2) at a high temperature of 900 ℃ for 6 hours, taking out the quartz coarse powder, and putting the quartz coarse powder into tap water for water quenching to enable the surface of the quartz to generate cracks and expose impurity ions on the surface.
(4) Fine purification: carrying out acid leaching and refining twice on the quartz coarse refined powder subjected to water quenching in the step (3), wherein primary acid washing is carried out on the quartz coarse refined powder subjected to water quenching in the step (3) by using an acid washing solution under the conditions that the stirring speed is 160r/min, the temperature is 60 ℃, and the liquid-solid ratio is 10 1ml/g, and the time is 6h; the pickling solution is a mixture obtained by mixing 0.5mol/L hydrofluoric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid according to a volume ratio of 1.
Secondary fine purification: and carrying out secondary acid leaching on the primarily purified quartz powder for 6 hours under the conditions that the stirring speed is 220r/min, the temperature is 80 ℃, and the liquid-solid ratio is 5 2 (ii) a The leaching solution is a mixture obtained by mixing 2mol/L sulfuric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid according to a volume ratio of 1. In order to ensure that there is sufficient H in the solution during the quartz leaching process + And impurity complex ions, and adding leachate with the solid-liquid volume of 5 percent after the second acid leaching into the reaction device every 1 hour.
Finally obtained high-purity SiO 2 Measurement of high purity SiO by chemical analysis (ICP-MS) 2 The content of impurity elements in the SiO is calculated by adopting a differential subtraction method 2 Content) of SiO 2 The content reaches 99.712%.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (7)
1. High-purity SiO extracted from high-silicon hematite tailings 2 The method of (a), characterized in that the method comprises the steps of:
(1) ultrasonic dispersion: grinding hematite tailings, and adding water to obtain the hematite tailings with the concentration of 20-80kg/m 3 The ore pulp is subjected to ultrasonic dispersion for 1-4min under the condition that the ultrasonic power is 70-200W;
(2) magnetic separation: carrying out weak-strong superconducting high-gradient magnetic separation on the ore pulp dispersed in the step (1) to obtain quartz coarse refined powder;
(3) high-temperature water quenching: roasting the quartz coarse refined powder subjected to magnetic separation in the step (2) at a high temperature of 700-900 ℃ for 4-6h, and then performing water quenching;
(4) fine purification: carrying out acid leaching and refining twice on the quartz coarse refined powder subjected to water quenching in the step (3), wherein primary refining is carried out by using a pickling solution under the conditions that the stirring speed is 120-160r/min, the temperature is 25-60 ℃, and the liquid-solid ratio is 10-15 ml/g, and the time is 4-6h; performing secondary fine purification by performing secondary acid leaching on the leachate at the stirring speed of 200-220r/min, the temperature of 60-80 ℃ and the liquid-solid ratio of 5-6 of 1ml/g for 6-8h, and supplementing the leachate with the solid-liquid volume of 2-5% after the secondary acid leaching every 1 h; obtaining high-purity SiO after acid leaching 2 。
2. The method for extracting high-purity SiO from high-silicon hematite tailings in claim 1 2 The method of (2), characterized by: siO of the hematite tailings in the step (1) 2 The mass content is more than 80 percent.
3. The method for extracting high-purity SiO from high-silicon hematite tailings in claim 1 2 The method of (2), characterized by: grinding the hematite tailings in the step (1) to a passage rate of 325 meshes of more than 80%.
4. The method for extracting high-purity SiO from high-silicon hematite tailings in claim 1 2 The method of (2), characterized by: the superconducting high-gradient magnetic separation of the step (2)The low-intensity magnetic separation intensity is 0.5-0.8T, and the high-intensity magnetic separation intensity is 4.1-5.0T.
5. The method for extracting high-purity SiO from high-silicon hematite tailings in claim 1 2 The method of (2), characterized by: the pickling solution for the first pickling in the step (4) is a mixture of 0.5mol/L hydrofluoric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid; and (4) leaching solution of the second acid leaching is a mixture of 2mol/L sulfuric acid, 3mol/L hydrochloric acid solution and 2mol/L nitric acid.
6. High-purity SiO 2 The method is characterized in that the high-purity SiO is extracted from the high-silicon hematite tailings of any one of claims 1 to 5 2 The method of (1); the SiO 2 The mass content is more than or equal to 99 percent.
7. Use of the method of claim 1 in the recovery and utilization of high silicon hematite tailings.
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| PCT/CN2022/115158 WO2024036664A1 (en) | 2022-08-17 | 2022-08-26 | Method for low-carbon efficient extraction of high-purity sio2 from high-silicon hematite tailings |
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|---|---|---|---|---|
| CN110510620A (en) * | 2019-09-11 | 2019-11-29 | 江苏凯达石英股份有限公司 | The method of purification of glass sand tailing |
| CN114588999A (en) * | 2022-03-08 | 2022-06-07 | 北京科技大学 | Low-carbon green preparation of high-purity SiO from iron tailings2Method |
| CN114620733A (en) * | 2022-03-08 | 2022-06-14 | 北京科技大学 | Superconductive high-strength magnetic coupling quartz ore low-carbon green SiO2Method for fine purification |
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| CA1184740A (en) * | 1981-05-27 | 1985-04-02 | Martin L.G. Gerritse | Process for obtaining high purity silica |
| CN106064819A (en) * | 2016-06-01 | 2016-11-02 | 安徽晶晶石英科技有限公司 | A kind of quartz deposit prepares the method for glass sand |
| CN114671440A (en) * | 2022-03-08 | 2022-06-28 | 北京科技大学 | Superconducting high-gradient magnetic separation high-silicon solid waste low-carbon green preparation of high-purity SiO2Method (2) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110510620A (en) * | 2019-09-11 | 2019-11-29 | 江苏凯达石英股份有限公司 | The method of purification of glass sand tailing |
| CN114588999A (en) * | 2022-03-08 | 2022-06-07 | 北京科技大学 | Low-carbon green preparation of high-purity SiO from iron tailings2Method |
| CN114620733A (en) * | 2022-03-08 | 2022-06-14 | 北京科技大学 | Superconductive high-strength magnetic coupling quartz ore low-carbon green SiO2Method for fine purification |
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