CN112978734B - Method for extracting carbon and silicon dioxide from coal gangue - Google Patents
Method for extracting carbon and silicon dioxide from coal gangue Download PDFInfo
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- CN112978734B CN112978734B CN202110295979.XA CN202110295979A CN112978734B CN 112978734 B CN112978734 B CN 112978734B CN 202110295979 A CN202110295979 A CN 202110295979A CN 112978734 B CN112978734 B CN 112978734B
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- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a method for extracting carbon and silicon dioxide from coal gangue, which comprises the following steps: crushing and grinding the coal gangue; carrying out activation treatment on the crushed and ground coal gangue under the condition of supercritical water or subcritical water; separating an organic liquid phase and a solid slag phase from the activated coal gangue through separation equipment; screening the solid slag phase by a shaking table to obtain enriched substances containing carbon and silicon dioxide, silicate and impurities; and (4) electrically separating the enriched substance containing carbon and silicon dioxide to obtain high-grade carbon and silicon dioxide. The carbon and the silicon dioxide separated by the method have high purity, the carbon can be burnt as clean coal, and the pure silicon dioxide is processed into products for sale, so that the method has obvious economic value.
Description
Technical Field
The invention relates to the technical field of extraction of valuable substances in coal gangue minerals, in particular to a method for extracting carbon and silicon dioxide from coal gangue.
Background
China is the largest coal producing country and consuming country in the world, and the national coal yield in 2019 is 38.5 hundred million tons. The coal gangue is a solid waste generated in the production and processing processes of coal, is a coal symbiotic resource, and the production amount of the coal gangue accounts for 10-25% of the coal exploitation amount. With the increasing development of coal mine industry in China, coal gangue has become one of the solid wastes with the largest discharge amount and more serious harm in China.
The coal gangue yield in China is accumulated to exceed 50 hundred million tons, the comprehensive utilization degree of the coal gangue is insufficient, the stacking amount is increased day by day, and the brought environmental problems are increased. A large amount of coal gangue is stacked in the open air, which causes certain pollution to the surrounding environment. For example, a large amount of dust can be generated in the stacking of open-air coal gangue, and the air quality is affected; pyrite and substances with high carbon content in the coal gangue can be spontaneously combusted, and harmful and toxic gases are generated; the waste pile generates a large amount of acid water or water carrying heavy metal ions through solarization, rain, weathering and decomposition, the underground water quality is damaged by infiltration, and the surface water is polluted and the environment is seriously polluted due to outflow. Therefore, it is imperative to explore methods for fully utilizing and high-value utilizing coal gangue, improve the comprehensive utilization rate and utilization value of coal gangue, and discuss the best way of saving coal gangue resources and protecting environment.
At present, coal gangue has multiple uses, such as power generation, building materials, soil improvement, water treatment agents and the like. If the elements are all recycled, the waste ore heap is changed into a product with practical value, so that the utilization rate of the coal gangue ore can be greatly improved, the value of the coal gangue mineral is increased, the waste is changed into valuable, and meanwhile, the coal gangue mineral contributes to environmental protection.
In order to solve the problem of utilization of coal gangue, the existing technology for extracting carbon and silicon dioxide from coal gangue mainly adopts high-temperature thermal activation and auxiliary concentrated acid leaching dissolution (the acid leaching rate is high after high-temperature activation at the temperature of more than 700 ℃), and due to the technical limitations, the energy consumption is high, the resource utilization rate is low, a large amount of waste liquid and waste residue are generated, so that serious secondary pollution is caused, the requirement on corrosion resistance of equipment by high-concentration acid-base treatment is high, and the large-scale industrial application of the technology is restricted.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for extracting carbon and silicon dioxide from coal gangue, which not only achieves a quick, efficient, economic and practical separation process, but also can realize the recovery of carbon and silicon dioxide in the coal gangue and respond to the policy of recycling solid wastes in China.
In order to achieve the purpose, the invention provides a method for extracting carbon and silicon dioxide from coal gangue, which comprises the following steps:
crushing and grinding the coal gangue;
step two, performing activation treatment on the crushed and ground coal gangue under the condition of supercritical water or subcritical water;
step three, separating an organic liquid phase and a solid slag phase from the activated coal gangue through separation equipment;
screening the solid slag phase by a shaking table to obtain enriched substances containing carbon and silicon dioxide, silicate and impurities;
and step five, carrying out electric separation on the enriched substance containing carbon and silicon dioxide to obtain high-grade carbon and silicon dioxide.
Further, the particle size of the crushed and ground coal gangue in the first step is 2 micrometers to 2 millimeters.
Further, in the second step, activation treatment is carried out under the condition of supercritical water or subcritical water, the activation temperature is 30-350 ℃, the activation pressure is 1-30MPa, and the activation time is 0.1-3h.
Furthermore, the separation equipment in the third step is any one of a hydraulic cyclone, a solid-liquid separation centrifugal machine and a spiral chute.
Furthermore, the transverse angle of the shaking table in the fourth step is 1-5 degrees, and the longitudinal angle is 1-5 degrees.
Further, in the fourth step, the grade of the enriched substances of carbon and silicon dioxide is 60-90%.
Further, in the fifth step, the method for separating the enriched carbon and the silica is to electrically select and separate the enriched carbon and the enriched silica through an electric separator.
Further, the grade of carbon obtained in the fifth step is 75-90%, and the grade of silicon dioxide carbon is 75-95%.
The invention has the following beneficial effects:
1. the invention provides a method for extracting carbon and silicon dioxide from coal gangue, which comprises the steps of crushing and grinding the coal gangue, and realizing the primary separation of minerals by changing the granularity and microstructure of the minerals in a mechanical way; then activating under subcritical/supercritical water, wherein the effect is to reduce the chemical stability of minerals, the generated crystal form is converted into an amorphous state, aluminum-silicon connection is separated, the activity is improved, an organic liquid phase and a solid slag phase are separated by strong centrifugal acting force of a hydro-cyclone, mineral enrichment is realized, enriched ore of carbon and silicon dioxide, alumina, silicate and a small amount of ferrotitanium are obtained by gravity separation of a table concentrator according to different specific gravities of different minerals; the carbon and silicon dioxide enriched ore is separated and collected through electric separation, and the function is to realize electric separation under an electric field according to different mineral dielectric constants. The carbon and the silicon dioxide separated by the method have higher purity, the carbon can be used as clean coal for combustion, and the pure silicon dioxide is processed into products for sale, so the method has obvious economic value.
2. The invention provides a method for extracting carbon and silicon dioxide from coal gangue, which adopts a novel supercritical hydrothermal activation method as a main activation method, overcomes the defects of the traditional high-temperature activation acid leaching, and has the defects that the main component of the coal gangue is bauxite with aluminosilicate, the silicon and the alumina are difficult to open, and the extraction of SiO2 is difficult. The physicochemical properties of the supercritical (subcritical) water are changed greatly, the density, viscosity and solvation capacity of the solution are changed greatly, and the strong decomposition capacity enables minerals to generate crystal form transformation in hydrothermal solution, and silicon-aluminum connection is opened through chemical reaction and the like, so that the key problem for subsequently extracting silicon dioxide is solved. Compared with the common thermal activation acid leaching, the supercritical activation has the advantages of low reaction temperature, high reaction rate, simple and easily-controlled process and the like.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic structural view of a preferred embodiment of the present invention.
Detailed Description
Embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways, which are defined and covered by the claims.
Example 1
As shown in fig. 1, the gangue is crushed and ground to 74 microns, subcritical activation is performed for 30min at 320 ℃ and 8MPa to obtain activated gangue, most of carbon and silica are exposed after activation, then a hydrocyclone is used for classifying the gangue into an organic liquid phase and a slag phase, the separated organic liquid phase is recycled, the slag phase is subjected to shaking table to obtain enriched ore of carbon and silica and silicate ore, the grade of the enriched ore is 80%, the enriched ore of carbon and silica is subjected to electric separation to obtain high-grade carbon and silica, the grade of carbon is 90%, and the grade of silica is 95%. The finished products of carbon and silica are better obtained under the process conditions.
Example 2
As shown in fig. 1, the gangue ore is crushed and ground to 36 micrometers, subcritical activation is carried out for 30min at 250 ℃ and 20MPa, the activated gangue ore is obtained, most of carbon and silica are exposed after activation, then a hydraulic cyclone is used for classifying the gangue ore into an organic liquid phase and a slag phase, the separated organic liquid phase is recycled, the slag phase is subjected to shaking table to obtain enriched ore of carbon and silica and silicate ore, the grade of the enriched ore is 70%, the enriched ore of carbon and silica is subjected to electric separation to obtain high-grade carbon and silica, the grade of carbon is 80%, and the grade of silica is 90%. The finished products of carbon and silicon dioxide are better obtained under the condition of the process, but the whole process is slow and the workload is increased due to the smaller particle size.
Example 3
As shown in fig. 1, the gangue is crushed and ground to 0.15 mm, subcritical activation is performed at 400 ℃ and 15Mpa for 60min to obtain activated gangue, a part of carbon and silicon dioxide are exposed after activation, then hydrocyclones are used for classifying the gangue into an organic liquid phase and a slag phase, the separated organic liquid phase is recycled, the slag phase is subjected to shaking table to obtain enriched ore of carbon and silicon dioxide and silicate ore, the grade of the enriched ore is 60%, the enriched ore of carbon and silicon dioxide is subjected to electric separation to obtain high-grade carbon and silicon dioxide, the grade of carbon is 75%, and the grade of silicon dioxide is 76%. The quality of finished products of carbon and silicon dioxide obtained under the process condition is general, and because the granularity of the mineral is large, part of the mineral cannot be dissociated, and the final grade and yield are influenced.
Comparative example 1: (without supercritical activation step)
The gangue mine is crushed and ground to 36 microns, the gangue mine is directly graded by a hydraulic cyclone without being activated by supercritical water (other steps are the same as the example 1), and the graded slag phase is sorted by a table concentrator, so that the silicon dioxide, the alumina and the silicate are difficult to separate, most of the silicon dioxide exists in a continuous state, the yield of the carbon and silicon dioxide enriched mine is very low and is less than 40%, the carbon grade obtained by subsequently electrically separating the enriched mine is only 35% with a large amount of other impurities, the silicon dioxide grade is only 30%, and most of the silicon dioxide and the alumina and the silicate are not separated with associated impurities. Therefore, the yield and the taste of the process are very low in the later stage of non-supercritical activation, carbon and silicon dioxide cannot be effectively separated, and the economic value is low.
Comparative example 2: (excessive temperature)
Crushing and grinding the coal gangue ore to 36 micrometers, performing subcritical activation for 30min at 450 ℃ and 8MPa to obtain activated coal gangue ore, classifying the coal gangue ore into an organic liquid phase and a slag phase by using a hydraulic cyclone, recovering and treating the separated organic liquid phase, and obtaining enriched ore of carbon and silicon dioxide and alumina and silicate associated ore from the slag phase through a table concentrator, wherein the enriched ore level of the carbon and the silicon dioxide is 85%, and the high-grade carbon and silicon dioxide can be obtained by electrically selecting the enriched ore level of the carbon and the silicon dioxide, wherein the carbon grade is 92% and the silicon dioxide grade is 95%. The silicon-aluminum element separation ratio under the high-temperature condition is good, the electric separation effect is good, but the improvement effect is not obvious compared with the example-I activation condition, and the analysis reason is as follows: when the temperature reaches 373 ℃, the liquid water is converted into water in a supercritical state, the purpose of separating elements such as silicon and aluminum is achieved by utilizing the strong decomposition capacity of supercritical water, minerals such as aluminosilicate are dissociated, and then if the temperature is continuously increased, the water still keeps the supercritical state, and the dissociation effect of the minerals is not greatly improved. Therefore, the improvement of the sorting effect is not obvious, and the temperature is kept below 400 ℃ in practical application from the viewpoint of energy conservation.
Comparative example 3: (too low temperature)
Crushing and grinding the coal gangue ore to 36 micrometers, performing subcritical activation for 30min at 80 ℃ and 20MPa to obtain activated coal gangue ore, then classifying the coal gangue ore into an organic liquid phase and a slag phase by using a hydraulic cyclone, obtaining enriched ore of carbon and silicon dioxide, alumina, silicate and the like from the slag phase through a table concentrator, and obtaining carbon and silicon dioxide from the enriched ore of carbon and silicon dioxide through electric separation, wherein the carbon grade is 60%, the silicon dioxide grade is 50%, and associated aluminate and other minerals with more impurities in the silicon dioxide are not fully dissociated. The temperature has great influence on the activation, the activation effect is not obvious only by increasing the pressure at low temperature, the extracted substance has more accompanying impurities, and the utilization value is low. For analysis reasons, the stability of mineral crystals in the coal gangue is high, the silicon-aluminum connection is not easy to open due to low activation temperature, most minerals are not dissociated, and the purity of electrically-selected silicon dioxide is low.
Comparative example 4: (too low a pressure)
Crushing and grinding the coal gangue ore to 36 micrometers, performing subcritical activation for 30min at 350 ℃ and 3MPa to obtain activated coal gangue ore, then classifying the coal gangue ore into an organic liquid phase and a slag phase by using a hydraulic cyclone, obtaining enriched ore of carbon and silicon dioxide, alumina, silicate and the like from the slag phase through a shaking table, obtaining carbon and silicon dioxide from the enriched ore of carbon and silicon dioxide through electric separation, wherein the carbon grade is 63%, the silicon dioxide grade is 55%, more accompanying impurities are not separated, and separating out impure minerals. The effect is not greatly improved after the high-temperature low-pressure activation, and the extracted substances are accompanied by aluminum salt impurities and are difficult to further separate. The pressure has great influence on the activation, and the activation effect is not obvious by only increasing the temperature under low pressure. The chemical stability of the minerals in the coal gangue is high for analysis reasons, although carbon and aluminosilicate are opened at high temperature, the pressure is not enough, the aluminum and silicon are difficult to be further separated, the acting force cannot meet the requirement of converting the crystal structure of the aluminosilicate minerals, the activation degree is low, and the separation effect is not obvious.
Comparative example 5: (excessive pressure)
Crushing and grinding the coal gangue ore to 36 micrometers, performing supercritical activation at 350 ℃ and 25Mpa for 30min to obtain activated coal gangue ore, dissociating most of the activated ore, classifying the activated ore into an organic liquid phase and a slag phase by using a hydraulic cyclone, obtaining enriched ore of carbon and silicon dioxide, alumina, silicate and ore containing a small amount of ferrotitanium by using the slag phase through a table concentrator, and obtaining high-grade carbon and silicon dioxide by electrically selecting the enriched ore of carbon and silicon dioxide, wherein the carbon grade is 95%, and the silicon dioxide grade is 95%. The extraction effect of each element is obvious and the separation is comparatively better under the supercritical condition, but the promotion effect is not obvious compared with the activation condition of the embodiment 2, and the analysis reason is that when the pressure reaches 22.5MPa, the liquid water is converted into the water in the supercritical state, and the purpose of separating elements such as silicon aluminum and the like is achieved by utilizing the strong decomposition capacity of the supercritical water to dissociate minerals such as aluminosilicate and the like, and then if the pressure is continuously promoted, the water still keeps the supercritical state, and the mineral dissociation effect is not greatly promoted. Therefore, the improvement on the sorting effect is not obvious, and the pressure is kept below 20MPa in practical application from the viewpoint of protecting equipment.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for extracting carbon and silicon dioxide from coal gangue is characterized by comprising the following steps:
crushing and grinding the coal gangue;
step two, performing activation treatment on the crushed and ground coal gangue under the condition of supercritical water or subcritical water;
step three, separating an organic liquid phase and a solid slag phase from the activated coal gangue through separation equipment;
screening the solid slag phase by a shaking table to obtain enriched substances containing carbon and silicon dioxide, silicate and impurities;
step five, carrying out electric separation on the enriched substance containing carbon and silicon dioxide to obtain high-grade carbon and silicon dioxide;
in the second step, activation treatment is carried out under the condition of supercritical water or subcritical water, the activation temperature is 250-400 ℃, the activation pressure is 8-20MPa, and the activation time is 0.1-3h;
the grade of carbon obtained in the fifth step is 75-90%, and the grade of silicon dioxide carbon is 75-95%.
2. The method for extracting carbon and silica from coal gangue as claimed in claim 1, wherein the particle size of the coal gangue crushed and ground in the first step is 2 μm to 2 mm.
3. The method for extracting carbon and silica from coal gangue as claimed in claim 1, wherein the separation equipment in the third step is any one of a hydrocyclone, a solid-liquid separation centrifuge and a spiral chute.
4. The method for extracting carbon and silica from coal gangue as claimed in claim 1, wherein the transverse angle of the table in the fourth step is 1-5 ° and the longitudinal angle is 1-5 °.
5. The method for extracting carbon and silica from coal gangue as claimed in claim 1, wherein the enriched grade of carbon and silica in the fourth step is 60-90%.
6. The method for extracting carbon and silica from coal gangue as claimed in claim 1, wherein the enriched carbon and silica separation method in the fifth step is electro-mechanical separation by an electric separator.
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| CN114212797B (en) * | 2021-12-03 | 2023-07-18 | 内蒙古科技大学 | Method for extracting liquid silica gel from coal gangue |
| CN114247572A (en) * | 2021-12-03 | 2022-03-29 | 内蒙古科技大学 | Device and method for separating coal from coal gangue in grading manner |
| CN114247552B (en) * | 2021-12-03 | 2023-07-21 | 内蒙古科技大学 | Beneficiation process for coal gangue by utilizing chromaticity difference |
| CN114249454A (en) * | 2021-12-03 | 2022-03-29 | 内蒙古科技大学 | Cleaning method for slime water |
| CN114247554A (en) * | 2021-12-03 | 2022-03-29 | 内蒙古科技大学 | Method for selecting valuable minerals in coal gangue |
| CN114247553B (en) * | 2021-12-03 | 2024-03-12 | 内蒙古科技大学 | Comprehensive separation method for gangue minerals |
| CN114247725B (en) * | 2021-12-03 | 2023-07-18 | 内蒙古科技大学 | Method for activating coal gangue through subcritical/supercritical water oxidation |
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