CN114324550B - Method for in-situ development of coal-type key metal mineral products - Google Patents
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Abstract
The invention discloses a method for in-situ development of coal-type key metal mineral products, which can simultaneously realize clean utilization of gasification combustion of coal resources and development of key metal mineral products in coal by combining underground coal gasification and in-situ leaching of key metals.
Description
Technical Field
The invention relates to the field of in-situ development methods of coal-type key metal minerals, in particular to a method for in-situ development of coal-type key metal minerals.
Background
The key metals (critical metals) or key mineral resources (critical minerals) are newly proposed resource concepts in the world, refer to the general names of a class of metal elements and mineral deposits thereof with high risk for the safe supply necessary in the current society, and mainly comprise rare earth, rare, scattered and rare noble metals. Rare earth elements are the lanthanoids of the periodic table of chemical elements-lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), and the elements yttrium (Y) and scandium (Sc) closely related to the lanthanoids together in 17 elements; rare noble elements, platinum (Pt), iridium (Ir), osmium (Os), ruthenium (Ru), rhodium (Rh), palladium (Pd), gold (Au); rare earth elements-rhenium (Re), gallium (Ga), indium (In), thallium (Tl), germanium (Ge), selenium (Se), tellurium (Te), cadmium (Cd); rare elements-lithium (Li), rubidium (Rb), cesium (Cs), francium (Fr), beryllium (Be), strontium (Sr), tantalum (Ta).
The key metal mineral products taking rare, rare and rare earth elements as main bodies have irreplaceable important application in the fields of new materials, new energy sources, information technology and the like. Because coal is an irreplaceable enrichment carrier for a plurality of key metals, and traditional key metal mineral resources in China are increasingly reduced, the worldwide demand is gradually increased, and therefore, the coal-type key metal mineral will become a new important source. The existing coal type key metal development and utilization mainly takes fly ash generated by burning coal as a research object, a large amount of toxic and harmful substances such as sulfur dioxide, smoke dust, radioactive fly ash, carbon monoxide and the like are generated in the coal burning process, then the fly ash is treated by means of high-temperature roasting, acid leaching, alkaline leaching, pressurizing and the like, and the leaching solution containing the key metal is subjected to impurity removal, concentration and other processes for further utilization, so that the process is complicated, a large amount of solid waste residues are generated to occupy land resources to pollute underground water, the cost is high, and meanwhile, serious harm is caused to the environment and human health. In order to solve the problems in the prior art, in view of the fact that the coal seam is an organic mineral deposit with a certain pore structure and permeability, the possibility of leaching key metals enriched in the coal seam exists.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a method for in-situ development of coal-type key metal minerals, which can simultaneously realize clean utilization of gasification combustion of coal resources and development of key metal minerals in coal.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a method for in-situ development of coal-type key metal mineral products, which comprises the following steps:
step one: carrying out a key metal element content test on coal samples acquired from each drilling hole and underground through inductively coupled plasma mass spectrometry to determine an enrichment coefficient CC of key metal elements in coal;
step two: selecting mining areas with the thickness of more than 2m, water-blocking and heat-insulating top and bottom plates, coal beds and surrounding rock dip angles of less than 35 degrees, undeveloped fracture structures, fractured uncut coal beds and surrounding rock cover rocks, poor water enrichment of a mining field aquifer, poor supply conditions, more than or equal to 10 key metal element enrichment coefficients and more than 3 key metal element enrichment typical coal samples as research objects for underground gasification and gasification coal ash leaching;
step three: performing underground gasification simulation experiments in a laboratory, performing coal sample gasification under the condition of oxygen-enriched air and a certain air inflow, increasing oxygen concentration in the gasification process until unburned carbon disappears, obtaining gasified coal ash after the coal sample is fully burned, observing the morphology of the gasified coal ash by using a scanning electron microscope, and transiting the morphology of the gasified coal ash from complex multiple holes to homogenization and singleization;
step four: the gasified coal ash comprises aluminosilicate amorphous glass bodies and mineral phases, the mineral composition in the gasified coal ash is measured by an X-ray diffractometer, the mineral composition comprises mullite, quartz and anorthite, and the key metal elements are supposed to be wrapped in the glass bodies or the crystal lattices of the mineral crystals;
step five: sequentially adding deionized water, 0.5-2mol/L ammonium acetate and 2-5mol/L hydrochloric acid/sodium hydroxide into gasified coal ash by adopting a progressive chemical extraction method, circularly leaching, oscillating and centrifuging to obtain water-soluble, ion-exchanged, glassy and mineral-phase products, digesting the mineral-phase products by nitric acid and hydrofluoric acid, and testing the element content in the products by using an inductively coupled plasma mass spectrometry to finally determine that key metal elements in the gasified coal ash are mainly in the glassy state, and then the content in the water-soluble and ion-exchanged states is lower;
step six: adding sodium carbonate as a roasting aid, mixing the sodium carbonate with gasified coal ash at a ratio of 1:1, roasting at a temperature of at least 900 ℃, converting mullite, quartz and anorthite into soluble aluminosilicate, and carrying out acid leaching on the roasted clinker and 3-5mol/L hydrochloric acid at a temperature of 80-150 ℃ for 1-3h at a ratio of 1g:10-15 ml;
step seven: according to the simulation situation of the earlier stage laboratory, in-situ drilling is carried out in a coal mine area, the in-situ drilling comprises an inlet drilling hole, an outlet drilling hole and a coal seam gasification channel, an ignition rod is sent into the coal seam gasification channel in advance, 30% -80% oxygen-enriched air gasifying agent is injected through each inlet drilling hole by utilizing a gasifying agent device, a gasifying ignition device enters the coal seam through the inlet drilling hole, coal is gasified and combusted through ignition, the temperature reaches at least 600 ℃, and CO in the outlet gas is obtained 2 A ratio of more than 20% indicates successful gasification ignition;
step eight: the synthesis gas of the combustible gas and the non-combustible gas generated by underground coal gasification is discharged through an outlet drill hole, the synthesis gas is separated by utilizing the existing gas separation device, and the separated combustible gas is reused;
step nine: feeding sodium carbonate as a roasting auxiliary agent through an inlet drill hole, roasting ash samples at a high temperature after combustion, inputting 3-5mol/L hydrochloric acid to leach key metal elements according to the conditions in the step six, and fully leaching key metals through a plurality of circulating leaching processes;
step ten: after the leaching process is finished, the existing extracting device is conveyed into a coal seam position through an outlet drilling hole, and leaching liquid containing key metals is extracted and conveyed to a leaching liquid treatment plant through the outlet drilling hole to recycle the key metal elements in the leaching liquid;
step eleven: sampling by multiple drilling holes, testing the pH value of underground reaction residues, injecting a neutralizer through an inlet drilling hole, and extracting residual liquid through an outlet drilling hole after reaction until the tested underground residues meet the non-toxic and non-corrosive requirements of industrial solid waste discharge.
Preferably, in the first step, the enrichment coefficient CC of the key metal element in the coal is determined compared with the background value of the world coal, cc=element content in the coal/element content in the world coal.
Preferably, in the third step, the oxygen-enriched air with the oxygen concentration of 40% -80% and the air inflow of 15-20Nm 3 Gasification of coal sample at/h to produce CO 2 、N 2 、CO、H 2 A small amount of CH 4 Wherein CO accounts for 14-26% of the total amount of the gas, H 2 The ratio is 22-30%, CH 4 Duty ratio of0.9% -1.2%, with the increase of the oxygen concentration, unburned carbon disappears, and the coal sample burns more fully.
Preferably, in the step six, the leaching effect of the key metal elements such as lithium, gallium and rare earth can reach more than 80 percent; the mechanism is as follows: na (Na) 2 CO 3 →Na 2 O+CO 2 ↑
3Al 2 O 3 ·2SiO 2 +4SiO 2 +3Na 2 O→6NaAlSiO 4 。
The invention has the beneficial effects that: the method combines underground coal gasification and in-situ key metal leaching, can realize clean utilization of gasification combustion of coal resources and development of key metal minerals in coal, fully realizes the utilization value of the coal resources, solves the problem of development and utilization of coal seams which are not suitable for underground mining, accords with the concept of green mines, and greatly reduces harm to environment and human health.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a method for in-situ development of coal-type key metal minerals provided by an embodiment of the invention;
reference numerals illustrate:
a. a gasifying agent device; b. a leaching solution storage device; c. drilling an inlet; d. extraction means; e. drilling an outlet; f. a gas separation device; g. a power plant; h. a leachate treatment plant;
1. a gasifying agent; 2. gasifying coal ash; 3. synthesis gas; 4. leaching liquid; 5. leaching liquid of key metals.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1, a method for in-situ development of coal-type key metal minerals comprises the following steps:
step one: carrying out a key metal element content test on coal samples acquired from each drilling hole and underground through inductively coupled plasma mass spectrometry (ICP-MS), and determining an enrichment coefficient CC of key metal elements in coal compared with a world coal background value, wherein the enrichment coefficient CC of key metal elements in coal=the element content in coal/the average value of the element content in world coal;
step two: selecting mining areas with the thickness of more than 2m, water-blocking and heat-insulating top and bottom plates, coal beds and surrounding rock dip angles of less than 35 degrees, undeveloped fracture structures, fractured uncut coal beds and surrounding rock cover rocks, poor water enrichment of a mining field aquifer, poor supply conditions, more than or equal to 10 key metal element enrichment coefficients and more than 3 key metal element enrichment typical coal samples as research objects for underground gasification and gasification coal ash leaching;
step three: in laboratory, the simulated experiment of underground gasification is carried out, and the oxygen-enriched air with oxygen concentration of 40% -80% and air inflow of 15-20Nm 3 Gasification of coal sample at/h to produce CO 2 、N 2 、CO、H 2 A small amount of CH 4 Wherein CO accounts for 14-26% of the total amount of the gas, H 2 The ratio is 22-30%, CH 4 The ratio of the oxygen to the unburned carbon is 0.9-1.2%, and the unburned carbon disappears and the coal sample burns more fully along with the increase of the oxygen concentration; observing the morphology of gasified coal ash 2 by using a scanning electron microscope, and transiting the morphology of gasified coal ash 2 from complex porous to homogeneous and single;
step four: the gasified coal ash 2 comprises aluminosilicate amorphous glass bodies and mineral phases, the mineral composition in the gasified coal ash 2 is measured by an X-ray diffractometer, the mineral composition comprises mullite, quartz and anorthite, and the key metal elements are supposed to be wrapped in the glass bodies or the crystal lattices of the mineral crystals;
step five: sequentially adding deionized water, 0.5-2mol/L ammonium acetate and 2-5mol/L hydrochloric acid/sodium hydroxide into gasified coal ash 2 by adopting a progressive chemical extraction method, circularly leaching, oscillating and centrifuging to obtain water-soluble, ion-exchanged, glassy and mineral-phase products, digesting the mineral-phase products by nitric acid and hydrofluoric acid, testing the element content in the products by using inductively coupled plasma mass spectrometry (ICP-MS), and finally determining that key metal elements in gasified coal ash 2 are mainly in a glassy state, and then in a mineral-phase state, the content in the water-soluble and ion-exchanged states is lower;
step six: adding sodium carbonate as a roasting auxiliary agent, mixing the sodium carbonate with gasified coal ash at a ratio of 1:1, roasting at a temperature of at least 900 ℃, converting mullite, quartz and anorthite into soluble aluminosilicate, and carrying out acid leaching on the roasted clinker and 3-5mol/L hydrochloric acid at a temperature of 80-150 ℃ for 1-3 hours according to a ratio of 1g:10-15ml, wherein the leaching effect of the key metal elements such as lithium, gallium and rare earth can reach more than 80%; the mechanism is as follows: na (Na) 2 CO 3 →Na 2 O+CO 2 ↑
3Al 2 O 3 ·2SiO 2 +4SiO 2 +3Na 2 O→6NaAlSiO 4 ；
Step seven: according to the simulation situation of the prior laboratory, in-situ drilling is carried out in a coal mine area, the in-situ drilling comprises an inlet drilling hole c, an outlet drilling hole e and a coal seam gasification channel, an ignition rod is sent into the coal seam gasification channel in advance, 30% -80% oxygen-enriched air gasifying agent 1 is injected through each inlet drilling hole c by utilizing a gasifying agent device a, a gasifying ignition device enters the coal seam through the inlet drilling holes c, coal is gasified and combusted through ignition, the temperature reaches at least 600 ℃, and CO in the outlet gas is obtained 2 A ratio of more than 20% indicates successful gasification ignition;
step eight: the synthesis gas 3 of the combustible gas and the non-combustible gas generated by underground coal gasification is discharged through an outlet drill hole e, the synthesis gas 3 is separated by utilizing the existing gas separation device f, and the separated combustible gas is sent to a power plant g for recycling;
step nine: sodium carbonate serving as a roasting auxiliary agent is fed through an inlet drill hole c, coal ash is roasted and gasified at a high temperature after combustion, 3-5mol/L hydrochloric acid is input for leaching key metal elements according to the conditions in the step six, and the purpose of fully leaching the key metal is achieved through a plurality of circulating leaching processes;
step ten: after the leaching process is finished, the existing extracting device d is sent to the position of the coal seam through an outlet drilling e, and the leaching liquid 5 containing the key metals is extracted and conveyed to a leaching liquid treatment plant h through the outlet drilling e to recycle the key metal elements in the leaching liquid;
step eleven: sampling by multiple drilling holes, testing the pH value of the underground reaction residues, injecting a neutralizing agent through an inlet drilling hole c, and extracting residual liquid through an outlet drilling hole e after reaction until the tested underground residues meet the non-toxic and non-corrosive requirements of industrial solid waste discharge.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (4)
1. The in-situ development method of the coal-type key metal mineral products is characterized by comprising the following steps of:
step one: carrying out a key metal element content test on coal samples acquired from each drilling hole and underground through inductively coupled plasma mass spectrometry to determine an enrichment coefficient CC of key metal elements in coal;
step two: selecting mining areas with the thickness of more than 2m, water-blocking and heat-insulating top and bottom plates, coal beds and surrounding rock dip angles of less than 35 degrees, undeveloped fracture structures, fractured uncut coal beds and surrounding rock cover rocks, poor water enrichment of a mining field aquifer, poor supply conditions, more than or equal to 10 key metal element enrichment coefficients and more than 3 key metal element enrichment typical coal samples as research objects for underground gasification and gasification coal ash leaching;
step three: performing underground gasification simulation experiments in a laboratory, performing coal sample gasification under the condition of oxygen-enriched air and a certain air inflow, increasing oxygen concentration in the gasification process until unburned carbon disappears, obtaining gasified coal ash after the coal sample is fully burned, observing the morphology of the gasified coal ash by using a scanning electron microscope, and transiting the morphology of the gasified coal ash from complex multiple holes to homogenization and singleization;
step four: the gasified coal ash comprises aluminosilicate amorphous glass bodies and mineral phases, the mineral composition in the gasified coal ash is measured by an X-ray diffractometer, the mineral composition comprises mullite, quartz and anorthite, and the key metal elements are supposed to be wrapped in the glass bodies or the crystal lattices of the mineral crystals;
step five: sequentially adding deionized water, 0.5-2mol/L ammonium acetate and 2-5mol/L hydrochloric acid/sodium hydroxide into gasified coal ash by adopting a progressive chemical extraction method, circularly leaching, oscillating and centrifuging to obtain water-soluble, ion-exchanged, glassy and mineral-phase products, digesting the mineral-phase products by nitric acid and hydrofluoric acid, and testing the element content in the products by using an inductively coupled plasma mass spectrometry to finally determine that key metal elements in the gasified coal ash are mainly in the glassy state, and then the content in the water-soluble and ion-exchanged states is lower;
step six: adding sodium carbonate as a roasting aid, mixing the sodium carbonate with gasified coal ash at a ratio of 1:1, roasting at a temperature of at least 900 ℃, converting mullite, quartz and anorthite into soluble aluminosilicate, and carrying out acid leaching on the roasted clinker and 3-5mol/L hydrochloric acid at a temperature of 80-150 ℃ for 1-3h at a ratio of 1g:10-15 ml;
step seven: according to the simulation situation of the earlier stage laboratory, in-situ drilling is carried out in a coal mine area, the in-situ drilling comprises a plurality of inlet drilling holes, outlet drilling holes and a coal seam gasification channel, an ignition rod is sent into the coal seam gasification channel in advance, 30% -80% oxygen-enriched air gasifying agent is injected through each inlet drilling hole, a gasification ignition device enters the coal seam through the inlet drilling holes, coal is gasified and combusted through ignition, the temperature reaches at least 600 ℃ and CO in outlet gas 2 A ratio of more than 20% indicates successful gasification ignition;
step eight: the synthesis gas of the combustible gas and the non-combustible gas generated by underground coal gasification is discharged through an outlet drill hole, the synthesis gas is separated by utilizing the existing gas separation device, and the separated combustible gas is reused;
step nine: feeding sodium carbonate as a roasting auxiliary agent through an inlet drill hole, roasting ash samples at a high temperature after combustion, inputting 3-5mol/L hydrochloric acid to leach key metal elements according to the conditions in the step six, and fully leaching key metals through a plurality of circulating leaching processes;
step ten: after the leaching process is finished, the existing extracting device is conveyed into a coal seam position through an outlet drilling hole, and leaching liquid containing key metals is extracted and conveyed to a leaching liquid treatment plant through the outlet drilling hole to recycle the key metal elements in the leaching liquid;
step eleven: sampling by multiple drilling holes, testing the pH value of underground reaction residues, injecting a neutralizer through an inlet drilling hole, and extracting residual liquid through an outlet drilling hole after reaction until the tested underground residues meet the non-toxic and non-corrosive requirements of industrial solid waste discharge.
2. The method for in-situ development of coal-type key metal minerals of claim 1, wherein: in step one, compared with the background value of the world coal, the enrichment coefficient CC of key metal elements in the coal is determined, wherein CC=the element content in the coal/the element content in the world coal.
3. The method for in-situ development of coal-type key metal minerals of claim 1, wherein: in the third step, the oxygen-enriched air with the oxygen concentration of 40% -80% and the air inflow of 15-20Nm 3 Gasification of coal sample at/h to produce CO 2 、N 2 、CO、H 2 A small amount of CH 4 Wherein CO accounts for 14-26% of the total amount of the gas, H 2 The ratio is 22-30%, CH 4 The ratio of the oxygen to the unburned carbon is 0.9-1.2%, and the unburned carbon disappears and the coal sample burns more fully along with the increase of the oxygen concentration.
4. The method for in-situ development of coal-type key metal minerals of claim 1, wherein: in the sixth step, the leaching effect of the key metal elements such as lithium, gallium and rare earth can reach more than 80 percent; the mechanism is as follows：Na 2 CO 3 →Na 2 O+CO 2 ↑
3Al 2 O 3 ·2SiO 2 +4SiO 2 +3Na 2 O→6NaAlSiO 4 。
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