CN115043399A - Method for efficiently purifying coal-series graphite - Google Patents
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- CN115043399A CN115043399A CN202210883880.6A CN202210883880A CN115043399A CN 115043399 A CN115043399 A CN 115043399A CN 202210883880 A CN202210883880 A CN 202210883880A CN 115043399 A CN115043399 A CN 115043399A
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Abstract
The invention belongs to the technical field of coal-series graphite purification, and provides a method for efficiently purifying coal-series graphite. According to the invention, the coal-series graphite is subjected to electrochemical oxidation and microwave heating to slightly expand the coal-series graphite, so that the closely associated fine particle impurities in the coal-series graphite are directionally decomposed, a foundation is laid for subsequent ultrasonic separation, the graphite is further expanded through ultrasound, so that the fine particle impurities in the dispersed graphite are further dissociated, and finally the dissociated expanded graphite floats to the upper layer by adopting nano-bubble flotation, while the fine particle impurities are left at the lower layer, so that the high-efficiency purification of the coal-series graphite is realized. The results of the examples show that the fixed carbon content of the coal-based graphite treated by the method provided by the invention is improved from 80.5% to 96.78%, and the recovery rate of the fixed carbon is 93.10%.
Description
Technical Field
The invention relates to the technical field of coal-series graphite purification, in particular to a method for efficiently purifying coal-series graphite.
Background
The coal-based graphite is formed under the thermal contact metamorphism action of coal, coal shale and the like, is one of coal-based nonmetallic minerals, and belongs to a strategic new mineral. The diameter of the coal-series graphite crystal is generally less than 1 μm, and the crystal form can be seen only under an electron microscope. The surface of the coal-based graphite ore is in a soil shape, grey black and steel grey, generally has dull luster, and has dense massive, soil-like, layered and lamellar structures. The grade of the ore is generally high, the fixed carbon content is generally 60-80%, and the small amount reaches more than 90%. For a long time, people only pay attention to the exploitation and processing of the crystalline graphite, neglect the development and utilization of the aphanitic graphite, mainly apply the aphanitic graphite as raw ores and rough processing products, and partially even burn the aphanitic graphite as coal, thereby causing the waste of mineral resources. The efficient purification of the coal-based graphite is the key for realizing the deep processing of the resources and improving the application range, and has important social and economic benefits.
The purification of the coal-based graphite is mainly to improve the purity of the aphanitic graphite and remove non-graphite impurity components such as quartz, silicate minerals, hydroxides of aluminum, magnesium and calcium. These non-graphite minerals tend to be finely granular impregnated in the cryptocrystalline graphite and are difficult to remove by conventional flotation processes. The existing purification method of the cryptocrystalline graphite commonly adopts a physical method and a chemical method, wherein the physical method comprises a flotation method, and the chemical method comprises an acid-base method, an acid leaching method, a chlorination roasting method and the like. However, the traditional flotation process is long in flow, multi-stage ore grinding and multi-stage flotation are often required, the removal effect of fine particle impurities is poor, and although the chemical method has a good purification effect, the product energy consumption is high, the process is complex, the risk of environmental pollution exists, and the large-scale application is difficult. Therefore, a method for purifying coal-based graphite with good purification effect and high purification efficiency is needed to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a method for efficiently purifying coal-based graphite, which has good purification effect and high purification efficiency, and the purified graphite has high fixed carbon content.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a method for efficiently purifying coal-series graphite, which comprises the following steps:
(1) sequentially carrying out electrochemical oxidation and microwave heating on the coal-based graphite to obtain expanded microcrystalline graphite;
(2) mixing the expanded microcrystalline graphite obtained in the step (1) with water, and then carrying out ultrasonic treatment to obtain graphite ore pulp;
(3) and (3) carrying out nano bubble flotation on the graphite ore pulp obtained in the step (2) to obtain graphite concentrate.
Preferably, the particle size of the coal-based graphite in the step (1) is D97 < 0.045 mm.
Preferably, the electrolyte used in the electrochemical oxidation in the step (1) is a sulfuric acid solution; the mass fraction of the sulfuric acid solution is more than or equal to 60 percent; the mass ratio of the coal-based graphite to the sulfuric acid solution is 1: (4-6).
Preferably, the current density of the electrochemical oxidation in the step (1) is 40-60 mA/cm 2 The electrifying time of the electrochemical oxidation is 4.0-6.0 h, and the temperature of the electrochemical oxidation is room temperature.
Preferably, the microwave heating power in the step (1) is 600-1200W, and the microwave heating time is 30-90 s.
Preferably, the power of the ultrasound in the step (2) is 100-200W, and the time of the ultrasound is 10-60 min.
Preferably, the mass of the expanded microcrystalline graphite in the step (2) is 3-8% of the total mass of the expanded microcrystalline graphite and the water.
Preferably, the flotation conditions of the nanobubble flotation in the step (3) are as follows: the aeration rate is 0.5-2.0L/min, the ore feeding speed is 0.5-2.0L/min, the thickness of the foam layer is 200-500 mm, the flow rate of flushing water is 0.5-2.0L/min, and the pH value of the graphite ore pulp is 9-10.
Preferably, the reagents used in the nanobubble flotation in the step (3) comprise: 300-700 g/t of collecting agent, 300-700 g/t of foaming agent and 1200-1500 g/t of inhibitor.
Preferably, the flotation times of the nano bubble flotation in the step (3) are 4-6 times.
The invention provides a method for efficiently purifying coal-series graphite, which comprises the following steps: (1) sequentially carrying out electrochemical oxidation and microwave heating on the coal-based graphite to obtain expanded microcrystalline graphite; (2) mixing the expanded microcrystalline graphite obtained in the step (1) with water, and then carrying out ultrasonic treatment to obtain graphite ore pulp; (3) and (3) carrying out nano bubble flotation on the graphite ore pulp obtained in the step (2) to obtain graphite concentrate. According to the invention, the coal-series graphite is subjected to electrochemical oxidation and microwave heating to slightly expand the coal-series graphite, so that the closely associated fine particle impurities in the coal-series graphite are directionally decomposed, a foundation is laid for subsequent ultrasonic separation, the graphite is further expanded through ultrasound, so that the fine particle impurities in the dispersed graphite are further dissociated, and finally the dissociated expanded graphite floats to the upper layer by adopting nano-bubble flotation, while the fine particle impurities are left at the lower layer, so that the high-efficiency purification of the coal-series graphite is realized. The results of the examples show that the fixed carbon content of the coal-based graphite treated by the method provided by the invention is improved from 80.5% to 96.78%, and the recovery rate of the fixed carbon is 93.10%.
Drawings
FIG. 1 is a flow chart of a process for purifying coal-based graphite in example 1 of the present invention.
Detailed Description
The invention provides a method for efficiently purifying coal-series graphite, which comprises the following steps:
(1) sequentially carrying out electrochemical oxidation and microwave heating on the coal-based graphite to obtain expanded microcrystalline graphite;
(2) mixing the expanded microcrystalline graphite obtained in the step (1) with water, and then carrying out ultrasonic treatment to obtain graphite ore pulp;
(3) and (3) carrying out nano bubble flotation on the graphite ore pulp obtained in the step (2) to obtain graphite concentrate.
The source of the coal-based graphite is not particularly limited, and the method for efficiently purifying the coal-based graphite provided by the invention is suitable for various coal-based graphites known to those skilled in the art.
In the present invention, the raw materials used are all commercial products which are conventional in the art, unless otherwise specified.
The invention carries out electrochemical oxidation and microwave heating on the coal-based graphite in sequence to obtain the expanded microcrystalline graphite. The method ensures that the coal-based graphite is subjected to micro-expansion through electrochemical oxidation and microwave heating, thereby realizing the directional 'loosening' of closely associated micro-fine particle impurities in the coal-based graphite and laying a foundation for subsequent ultrasonic separation.
In the present invention, the particle size of the coal-based graphite is preferably D97 < 0.045 mm. In the invention, the granularity of the coal-based graphite is preferably controlled within the range, the granularity of the coal-based graphite is too large, and the dissociation of graphite crystals and fine particle impurities is insufficient; the undersize of the coal-based graphite is not beneficial to subsequent expansion and flotation separation. In the present invention, when the particle size of the coal-based graphite does not satisfy the above conditions, the present invention preferably mechanically dissociates the coal-based graphite. The mechanical dissociation method is not particularly limited in the present invention, and a mechanical dissociation method known to those skilled in the art may be used. In the present invention, the mechanical dissociation is preferably performed by ball milling or roll milling.
The operation of the electrochemical oxidation is not particularly limited in the present invention, and the technical scheme of the electrochemical oxidation known to those skilled in the art may be adopted.
In the present invention, the electrolyte used for the electrochemical oxidation is preferably a sulfuric acid solution; the mass fraction of the sulfuric acid solution is preferably not less than 60%, and more preferably 70-75%. The invention takes sulfuric acid solution as electrolyte, and H ions in the sulfuric acid can oxidize graphite in the electrochemical oxidation process, thereby obtaining expandable graphite, and preparing for subsequent microwave expansion while directionally loosening closely associated micro-fine particle impurities.
In the present invention, the mass ratio of the coal-based graphite to the sulfuric acid solution is preferably 1: (4-6), more preferably 1: (4-5). The invention preferably controls the mass ratio of the coal-based graphite to the sulfuric acid solution within the range, and when the dosage of the sulfuric acid solution is too small, the oxidation is insufficient, which is not beneficial to the subsequent full expansion; when the amount of the sulfuric acid solution is too large, the swelling effect cannot be improved and the cost is increased.
In the invention, the current density of the electrochemical oxidation is preferably 40-60 mA/cm 2 More preferably 50 to 60mA/cm 2 . In the invention, the electrifying time of the electrochemical oxidation is preferably 4.0-6.0 h, and more preferably 5.0-6.0 h. In the present invention, the temperature of the electrochemical oxidation is preferably room temperature. The current density and the electrifying time of the electrochemical oxidation are preferably controlled within the ranges, so that the full expansion of graphite is facilitated, the graphite is better dispersed, and the excellent purification effect is finally achieved.
The operation of the microwave heating is not particularly limited in the present invention, and the technical scheme of microwave heating known to those skilled in the art can be adopted.
In the invention, the power of the microwave heating is preferably 600-1200W, and more preferably 900-1200W; the time for microwave heating is preferably 30-90 s, and more preferably 30-60 s. The invention further expands the coal-based graphite by microwave heating, thereby realizing the further dissociation of graphite crystals and micro-fine particle impurities in the coal-based graphite.
After the expanded microcrystalline graphite is obtained, the expanded microcrystalline graphite is mixed with water and then subjected to ultrasonic treatment to obtain graphite pulp. The invention further expands the graphite through ultrasound, thereby further dissociating and dispersing micro-fine particle impurities in the graphite and improving the purification effect.
The operation of the ultrasound is not particularly limited in the present invention, and the technical scheme of ultrasound known to those skilled in the art may be adopted.
In the invention, the power of the ultrasonic wave is preferably 100-200W, and more preferably 150-200W; the time of the ultrasonic treatment is preferably 10-60 min, and more preferably 20-60 min. The invention preferably controls the power and time of the ultrasonic within the above range, and ensures the full dispersion of graphite and fine particle impurities.
In the present invention, the mass of the expanded microcrystalline graphite is preferably 3 to 8%, more preferably 5 to 8%, of the total mass of the expanded microcrystalline graphite and water. The invention preferably controls the dosage of the expanded microcrystalline graphite and the water in the range, and the content of the expanded microcrystalline graphite is too high to be beneficial to dispersion; the content of the expanded microcrystalline graphite is too low, the water consumption is large, and the separation efficiency is influenced.
After obtaining the graphite ore pulp, the invention carries out nano-bubble flotation on the graphite ore pulp to obtain graphite concentrate. The invention leads the graphite to float to the upper layer through the flotation of the nano bubbles, and the micro-fine particle impurities are left at the lower layer, thereby realizing the high-efficiency purification of the coal-based graphite.
In the present invention, the flotation conditions of the nanobubble flotation are preferably: the aeration rate is 0.5-2.0L/min, the ore feeding speed is 0.5-2.0L/min, the thickness of the foam layer is 200-500 mm, the flow rate of flushing water is 0.5-2.0L/min, and the pH value of the graphite ore pulp is 9-10. The flotation conditions are preferably adopted for nano-bubble flotation, so that the flotation process can be better controlled, and graphite is brought to a foam layer by bubbles; the larger the aeration quantity is, the more bubbles are, the more matters float, but impurities can be entrained, and the purification effect is influenced.
In the invention, the pH regulator for regulating the pH value of the graphite ore pulp is preferably calcium oxide and/or sodium carbonate, and more preferably calcium oxide. The invention can prevent pyrite in graphite from floating up by adjusting the pH value of the graphite ore pulp, thereby adjusting the electrical property of minerals.
In the invention, based on the usage amount of the graphite ore pulp, the reagents used for the nanobubble flotation preferably comprise: 300-700 g/t of collecting agent, 300-700 g/t of foaming agent and 1200-1500 g/t of inhibitor, and more preferably 500-700 g/t of collecting agent, 500-700 g/t of foaming agent and 1300-1500 g/t of inhibitor. The invention preferably controls the dosage of the medicament used for the nano bubble flotation in the range, thereby not only ensuring the flotation effect, but also not wasting raw materials.
In the present invention, the collector is preferably diesel and/or kerosene, more preferably diesel. In the invention, the collector has the function of increasing the hydrophobicity of graphite and improving the flotation recovery rate.
In the present invention, the frother is preferably No. two oil and/or octanol, more preferably No. two oil. In the present invention, the foaming agent can increase the mechanical strength of the bubbles, prevent the bubbles from merging, control the floating rate of the bubbles, and change the distribution state of the bubbles.
In the present invention, the inhibitor is preferably sodium hexametaphosphate and/or water glass, more preferably sodium hexametaphosphate. In the invention, the inhibitor has the functions of adsorbing silicate minerals with the same acid radicals, forming hydrophilic films on the surfaces of inorganic minerals in graphite, increasing the hydrophilicity of the inorganic minerals, and inhibiting the floatability of the minerals.
In the invention, the flotation times of the nano bubble flotation are preferably 4-6 times, and more preferably 5-6 times. In the invention, a foaming agent is preferably added during the 2 nd-6 th nanometer bubble flotation; the foaming agent is preferably No. two oil and/or secondary octanol; the addition amount of the foaming agent is preferably 300-700 g/t.
After the nano-bubble flotation is finished, the product obtained by the nano-bubble flotation is preferably dried to constant weight to obtain graphite concentrate. In the present invention, the drying temperature and time are not particularly limited, and the product may be dried to a constant weight.
The method comprises the steps of firstly carrying out electrochemical oxidation and microwave heating on the coal-based graphite to enable the coal-based graphite to be micro-expanded, so that the micro-fine particle impurities closely associated in the coal-based graphite are directionally loosened, laying a foundation for subsequent ultrasonic separation, further expanding the graphite through ultrasound, further dissociating and dispersing the micro-fine particle impurities in the graphite, and finally floating the dissociated expanded graphite to an upper layer and leaving the micro-fine particle impurities at a lower layer through nano-bubble flotation, so that the high-efficiency purification of the coal-based graphite is realized.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Mechanically dissociating the crushed coal-based graphite raw ore by using a roller mill to obtain ore grinding graphite with the granularity D97 less than 0.045 mm;
(2) performing electrochemical oxidation on the ore grinding graphite obtained in the step (1), wherein sulfuric acid with the mass fraction of 70% is used as an electrolyte, and the mass ratio of the ore grinding graphite to a sulfuric acid solution is 1: 5, controlling the current density to be 50mA/cm at room temperature 2 Electrifying for 5.0h, then washing with water, and drying to constant weight to obtain graphite oxide;
(3) carrying out microwave heating on the graphite oxide obtained in the step (2), wherein the microwave power is 900W, and the heating time is 60s, so as to obtain expanded microcrystalline graphite;
(4) preparing the expanded microcrystalline graphite obtained in the step (3) and water into ore pulp with the mass concentration of 5%, and performing ultrasonic dispersion with the ultrasonic power of 150W for 20min to obtain graphite ore pulp;
(5) and (4) carrying out nano bubble flotation on the graphite ore pulp obtained in the step (4), wherein the flotation conditions are as follows: the aeration quantity is 1.0L/min, the ore feeding speed is 1.0L/min, the thickness of a foam layer is 300mm, the washing water is 1.0L/min, and the pH value is adjusted to 9.5 by calcium oxide; the medicament is as follows: 500g/t of diesel oil, 500g/t of second oil and 1300g/t of sodium hexametaphosphate to obtain flotation coarse ore;
(6) collecting the flotation coarse ore obtained in the step (5), carrying out concentration for 5 times according to the same flotation conditions in the step (4), and supplementing second oil in the subsequent concentration process, wherein the using amount is 500g/t, so as to obtain flotation concentrate;
(7) and (4) drying the flotation concentrate obtained in the step (6) to constant weight to obtain a final product.
Fig. 1 is a process flow diagram of purifying coal-based graphite in this embodiment, in which coal-based graphite is first mechanically dissociated to dissociate graphite into small particles; and then performing electrochemical oxidation and microwave heating to expand the graphite, directionally loosening micro-fine particle impurities closely associated in the coal-based graphite, further expanding the graphite through ultrasound, further dissociating and dispersing the micro-fine particle impurities in the graphite, and finally floating the dissociated expanded graphite to an upper layer and leaving the micro-fine particle impurities on a lower layer by adopting nano-bubble flotation, thereby realizing the high-efficiency purification of the coal-based graphite.
Example 2
The difference from example 1 is that the mass ratio of the coal-based graphite to the sulfuric acid solution in step (2) is 1: 4;
the rest of the procedure was the same as in example 1.
Example 3
The difference from example 1 is that the flotation conditions in step (5) are: the aeration quantity is 1.5L/min, the ore feeding speed is 1.5L/min, the thickness of a foam layer is 400mm, the rinsing water is 1.5L/min, and the pH value is adjusted to 10 by calcium oxide;
the rest of the procedure was the same as in example 1.
Example 4
The difference from example 1 is that the pharmaceutical agent in step (5) is: 700g/t of diesel oil, 700g/t of second oil and 1500g/t of sodium hexametaphosphate;
the rest of the procedure was the same as in example 1.
Example 5
The difference from example 1 is that the pharmaceutical agent in step (5) is: 300g/t of diesel oil, 300g/t of second oil and 1200g/t of sodium hexametaphosphate;
the rest of the procedure was the same as in example 1.
Example 6
The difference from embodiment 1 is that the parameters in step (6) are changed to: the dosage of the second oil is 300 g/t;
the rest of the procedure was the same as in example 1.
Comparative example 1
The difference from the embodiment 1 is that the parameters of the step (1) are changed as follows: controlling the granularity to be-0.074 mm;
the rest of the procedure was the same as in example 1.
Comparative example 2
The difference from example 1 is that the mass ratio of the coal-based graphite to the sulfuric acid solution in step (2) is 1: 1;
the rest of the procedure was the same as in example 1.
Comparative example 3
The difference from example 1 is that the number of culling of step (6) is 2.
The fixed carbon content of the final products obtained in the above examples 1-6 and comparative examples 1-3 was analyzed by GB/T3521-2008 "graphite chemistry analysis method", and the results are shown in Table 1.
TABLE 1 fixed carbon content of the raw materials and products prepared in examples 1-6 and comparative examples 1-3
The embodiment and the comparative example show that the method for efficiently purifying the coal-based graphite has good purification effect and high purification efficiency, and the purified graphite has high fixed carbon content, so that the fixed carbon content of the coal-based graphite treated by the method provided by the invention is increased from 80.5% to 96.78%, and the recovery rate of the fixed carbon is 93.10%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for efficiently purifying coal-based graphite comprises the following steps:
(1) sequentially carrying out electrochemical oxidation and microwave heating on the coal-based graphite to obtain expanded microcrystalline graphite;
(2) mixing the expanded microcrystalline graphite obtained in the step (1) with water, and then carrying out ultrasonic treatment to obtain graphite ore pulp;
(3) and (3) carrying out nano bubble flotation on the graphite ore pulp obtained in the step (2) to obtain graphite concentrate.
2. The method of claim 1, wherein the particle size of the coal-based graphite in step (1) is D97 < 0.045 mm.
3. The method according to claim 1, wherein the electrolyte used in the electrochemical oxidation in step (1) is a sulfuric acid solution; the mass fraction of the sulfuric acid solution is more than or equal to 60 percent; the mass ratio of the coal-based graphite to the sulfuric acid solution is 1: (4-6).
4. The method according to claim 1 or 3, wherein the current density of the electrochemical oxidation in the step (1) is 40 to 60mA/cm 2 The electrifying time of the electrochemical oxidation is 4.0-6.0 h, and the temperature of the electrochemical oxidation is room temperature.
5. The method according to claim 1, wherein the power of the microwave heating in the step (1) is 600-1200W, and the time of the microwave heating is 30-90 s.
6. The method according to claim 1, wherein the power of the ultrasound in the step (2) is 100-200W, and the time of the ultrasound is 10-60 min.
7. The method according to claim 1, wherein the mass of the expanded microcrystalline graphite in the step (2) is 3-8% of the total mass of the expanded microcrystalline graphite and the water.
8. The method according to claim 1, wherein the flotation conditions for nanobubble flotation in step (3) are: the aeration rate is 0.5-2.0L/min, the ore feeding speed is 0.5-2.0L/min, the thickness of the foam layer is 200-500 mm, the flow rate of flushing water is 0.5-2.0L/min, and the pH value of the graphite ore pulp is 9-10.
9. The method according to claim 1 or 8, wherein the agent for nanobubble flotation in step (3) comprises: 300-700 g/t of collecting agent, 300-700 g/t of foaming agent and 1200-1500 g/t of inhibitor.
10. The method according to claim 1, wherein the flotation times of the nanobubble flotation in the step (3) are 4-6 times.
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