CN115747527B - Vanadium extraction method for stone coal mine fluidization roasting-pressure leaching based on microwave heating - Google Patents
Vanadium extraction method for stone coal mine fluidization roasting-pressure leaching based on microwave heating Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 138
- 239000004575 stone Substances 0.000 title claims abstract description 99
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 63
- 238000010438 heat treatment Methods 0.000 title claims abstract description 23
- 238000000605 extraction Methods 0.000 title claims abstract description 22
- 238000005243 fluidization Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 65
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- 239000000463 material Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910052900 illite Inorganic materials 0.000 claims abstract description 7
- 239000010445 mica Substances 0.000 claims abstract description 7
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 7
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 37
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
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- 229910001456 vanadium ion Inorganic materials 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
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- 229910052742 iron Inorganic materials 0.000 description 2
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
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- 229910052628 phlogopite Inorganic materials 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
A method for extracting vanadium from stone coal mine by fluidization roasting-pressure leaching based on microwave heating belongs to the technical field of vanadium extraction. The vanadium extraction method comprises the processes of preheating roasting, fluidized microwave roasting and pressure leaching. In the fluidized microwave roasting process, stone coal particles can absorb microwave energy and convert the microwave energy into heat energy, and the temperature inside and outside the particles can be quickly raised. According to the difference of wave absorption characteristics of the minerals, the vanadium-containing minerals are selectively heated; the fluidized roasting technology ensures that the gas-solid contact in the roasting process is sufficient, the mass and heat transfer efficiency is high, the flow is simplified, and the aim of generating a large amount of damages and cracks in the particles under the condition that stone coal materials are not sintered is fulfilled. And the damages and cracks can enable leaching solution ions in the solution to efficiently enter the interior of the particles to react in the pressure leaching process, so that the liquid-solid contact reaction sites are improved, and the leaching rate is improved. The method is applicable to refractory stone coal mines, and can realize the effective leaching of mica type refractory stone coal illite type refractory stone coal.
Description
Technical Field
The invention relates to the technical field of vanadium extraction, in particular to a method for extracting vanadium by fluidized roasting-pressure leaching of stone coal mine based on microwave heating.
Background
In the existing stone coal vanadium extraction process, blank roasting-leaching is an environment-friendly and effective stone coal vanadium extraction process. Compared with other additive roasting processes, the blank roasting process has no additive, does not produce high-pollution waste gas and waste water, and can effectively reduce pollution. However, the blank roasting-leaching process has poor leaching effect on refractory stone coal ores in which vanadium exists in a similar form. This is because the conventional blank firing is performed using a flat kiln, a shaft kiln, and a rotary kiln. The heating of the material is derived from heat conduction, convection and radiation, which results in uneven heating of the material inside and outside and low heat transfer efficiency. And the ore feeding before charging is required to be made into balls or baked bricks, and the ore is required to be cooled and crushed after discharging. On the one hand, the gas-solid contact is insufficient in the reaction process, the mass transfer and heat transfer efficiency is low, and on the other hand, the production process is complex, the heat waste and the operation cost are high.
And the fluidized roasting technology can be used for strengthening the roasting effect of blank roasting. The fluidization roasting technology also makes technical breakthroughs in the field of various mineral resources such as refractory iron ores, iron-manganese ores, stone coals and the like, and part of projects have realized industrialized application. The method is characterized in that according to the patent CN106868292A, a complex iron ore reinforced separation method based on ore phase segmentation and accurate regulation is disclosed, CN111644267A, a suspension roasting system and method for industrially treating iron-manganese ore is disclosed, CN111304465A, a vanadium-containing stone coal decarburization-crystal breaking roasting reinforced acid leaching vanadium extraction method is disclosed, and CN111304464A, a stone coal vanadium ore multistage roasting reinforced acid mixing curing vanadium extraction method is disclosed. However, these conventional fluidized roasting cannot cause a great deal of effective damage and cracks to the inside of stone coal particles. On the other hand, during ordinary microwave roasting, material particles are accumulated, and local overheat sintering is extremely easy to generate. How to cause a great deal of damage and cracks inside the stone coal particles under the condition of ensuring that the stone coal particles are not sintered is a difficult point for researching stone coal roasting technology.
In the blank roasting-leaching process, the leaching process is normal pressure leaching, and when the normal pressure leaching is carried out, the leaching efficiency of stone coal roasting products is relatively low, the consumption of leaching agent is large, the leaching time is long, so that the production cost is high.
Disclosure of Invention
Aiming at the problems of the existing stone coal blank roasting-leaching process, the invention provides a stone coal mine fluidization roasting-pressure leaching vanadium extraction method based on microwave heating. The invention strengthens the blank roasting effect of stone coal by the microwave heating and fluidization roasting technology, and achieves the purposes of improving the reaction mass and heat transfer efficiency, improving the heating rate and strengthening the damage of vanadium-containing mineral crystal lattices.
The invention strengthens the leaching efficiency of the roasted product by pressure leaching, and achieves the purposes of reducing the leaching liquid dosage, shortening the leaching time and improving the vanadium leaching rate. So as to realize the efficient leaching of the mica type illite type refractory stone coal.
And the microwave fluidization roasting skillfully realizes the purpose that a large amount of damages and cracks can be generated in the particle under the condition that stone coal materials are not sintered. These damages and cracks greatly promote the efficient entry of leachate ions in the solution into the interior of the particles for reaction during the pressure leaching process, thereby realizing effective liquid-solid contact and improving leaching rate. Because of the small damage and cracks, the leaching process at normal pressure cannot effectively enter ions in the leaching solution, and the effect of cracks generated by microwave roasting can be revealed only by high pressure.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention relates to a method for extracting vanadium from stone coal mine through fluidization roasting-pressure leaching based on microwave heating, which comprises the following specific embodiments:
s1, crushing:
Crushing stone coal mine to obtain finely ground stone coal powder ore with the diameter of-0.045 mm accounting for 55% -70%;
In the step S1, the stone coal ore crushing process consists of two working procedures of crushing and grinding. The ore feeding granularity of stone coal is in the range of 8 mm-250 mm. The stone coal mine is crushed to 1 mm-6 mm by a jaw crusher, and then the dry semi-autogenous mill is adopted to grind the powder ore to-0.045 mm accounting for 55% -70%. The specific grinding fineness is determined according to the properties of different ores, and the finer the embedding granularity of vanadium minerals is, the finer the fineness of the crushed products is.
S2, preheating and roasting processes:
The finely ground stone coal powder ore is preheated at 600-700 ℃ for 25-40 s, and the adsorbed water in the material can be removed in the process. Preheating and roasting the stone coal powder to 400-500 ℃ to obtain preheated stone coal powder;
S3, fluidization microwave roasting process:
the preheated stone coal powder ore is directly fed into a fluidized microwave roasting device, and a microwave heater on the outer wall of the device can generate a microwave field to rapidly heat material particles. Air and O 2 are introduced into the bottom of the fluidization microwave roasting device, the roasting atmosphere can be regulated and controlled according to the ore feeding property change, and the fluidization microwave roasting device controls the internal temperature of the fluidization microwave roasting device within the range of 850-950 ℃ by regulating and controlling the air quantity (5 m 3/h～6.5m3/h) and the power of a microwave heater (25-45 kW). In the roasting process, minerals such as carbonaceous and pyrite are oxidized first. Secondly, minerals such as kaolinite, dolomite and the like are decomposed. When the material temperature reaches the set temperature, the mica minerals undergo dehydroxylation reaction, and Al-O octahedron and Si-O tetrahedron in the crystal lattice are efficiently destroyed. Meanwhile, vanadium atoms present therein in a congener form are more easily dissociated and oxidized. According to different mineral powder properties, the retention time of the mineral powder in the fluidized microwave roasting process is 28-60 min, and a roasting product is obtained.
S4, pressurizing and leaching:
Vanadium ions in the roasted product exist in +4 and +5 valences and are easy to dissolve in acid and alkali. Thus, the pressure leaching process uses sulfuric acid or sodium hydroxide as the leaching agent. Adding water into the leaching agent to prepare a leaching solution, and reacting the leaching solution with oxide of high-valence vanadium to generate vanadium ions for leaching, thereby realizing the leaching of vanadium in the powder ore. The pressure leaching process is as follows: immersing the roasted product in the leaching solution, ensuring the pressure in the reaction kettle to be 1.0-1.5 MPa, and according to the liquid-solid ratio, leaching the solution: the roasting product is (1.5-2) mL, the leaching temperature is 150-180 ℃, the mass of the leaching agent in the leaching solution accounts for 5-15% of the mass of the roasting product, and the leaching time is 1-2 h, so that the vanadium-rich noble liquid and the leaching slag are obtained.
By adopting the vanadium extraction method based on fluidized roasting and pressure leaching of the stone coal mine by microwave heating, the leaching rate of vanadium in the stone coal mine can reach 85% -90%, and the obtained leaching liquid can be recycled after vanadium extraction of the vanadium-rich noble liquid.
The key points of the invention are as follows:
1. The invention strengthens the roasting effect of stone coal by a microwave heating technology. In the microwave field, stone coal particles can absorb microwave energy and convert the microwave energy into heat energy, so that the temperature inside and outside the particles can be quickly raised. In addition, the vanadium-containing minerals will be selectively heated according to the differences in the wave-absorbing characteristics of the respective minerals.
2. The invention strengthens the leaching efficiency of the roasted product by the pressure leaching technology. The pressure leaching operation can effectively improve the leaching pressure and the leaching temperature, thereby reducing the leaching liquid dosage, shortening the leaching time and improving the vanadium leaching rate. The leaching effect on refractory stone coal can be improved, and the effective leaching of mica type refractory stone coal and illite type refractory stone coal can be realized.
3. The leaching process can select acid liquor or alkali liquor as a leaching agent, and can be better suitable for stone coal raw ores with different properties.
4. The invention strengthens the roasting effect of stone coal by a fluidized roasting process. The fluidized roasting has the advantages of sufficient gas-solid contact, high mass and heat transfer efficiency, low operation cost, environmental protection and the like, and is an efficient stone coal vanadium extraction process.
Compared with the prior art, the vanadium extraction method based on fluidized roasting-pressure leaching of stone coal mine by microwave heating has the beneficial effects that:
(1): the invention strengthens the roasting effect of stone coal by microwave heating and fluidization roasting technology. In the microwave field, stone coal particles can absorb microwave energy and convert the microwave energy into heat energy, so that the temperature inside and outside the particles can be quickly raised. In addition, according to the difference of wave absorption characteristics of the minerals, the vanadium-containing minerals are selectively heated; the fluidized roasting technology ensures that the roasting process has the advantages of sufficient gas-solid contact, high mass and heat transfer efficiency, low operation cost, environmental protection, simplified flow and the like.
(2): The pressure leaching operation can effectively improve the leaching pressure and the leaching temperature, thereby reducing the leaching liquid dosage, shortening the leaching time and improving the vanadium leaching rate. The leaching effect on refractory stone coal can be improved, and the effective leaching of mica type refractory stone coal and illite type refractory stone coal can be realized.
Drawings
FIG. 1 is a schematic flow chart of a method for extracting vanadium from stone coal mine by fluidized roasting-pressure leaching based on microwave heating.
FIG. 2 is a schematic diagram of the material change of the preheat roasting apparatus.
Fig. 3 is a schematic diagram of material change of a fluidized microwave roasting device.
Fig. 4 is a schematic diagram of the material change of the pressure leaching device.
Detailed Description
The technical scheme in the implementation of the patent is clearly and completely described with reference to the accompanying drawings. It should be noted that the examples described herein are for further explanation and illustration only and are not intended to limit the scope of their application. All other embodiments, which can be obtained by a person skilled in the art without making any inventive effort, are within the scope of protection of the present patent.
Example 1:
In the example, the raw stone coal ore is taken from a certain place in Hunan, and the raw stone coal ore contains the following components in percentage by mass: v 2O5 content 1.32%, C content 0.73%, TFe content 1.12%, siO 2 content 57.61%, quartz and vanadium-containing phlogopite are main constituent minerals. The flow diagram of the vanadium extraction method based on fluidized roasting and pressure leaching of stone coal mine by microwave heating is shown in figure 1, and the method is specifically developed according to the following steps:
(1) Crushing: after the raw ore passes through a crusher and is ground, the granularity of the product reaches 78 percent of-0.074 mm and 69 percent of-0.045 mm, and the ground stone coal powder ore is obtained.
(2) And (3) preheating and roasting: and feeding the finely ground stone coal powder ore into a preheating roasting device. The natural gas is burned as fuel to heat the interior of the preheating roasting device to 600 ℃. The material flows through the device, is heated to about 400 ℃ by the effects of heat conduction, convection and radiation, and the preheated stone coal powder ore is obtained.
(3) Fluidized microwave roasting process: the preheated stone coal powder ore is fed into a fluidized microwave roasting device, and the temperature in the oven body is controlled to be 910 ℃ by adjusting a microwave heater and the ventilation quantity. The power of the microwave heater is 35kW, mixed gas of 5.5m 3/h is introduced into the furnace body, wherein the ratio of air to O 2 is 4:1 according to the volume ratio, and the reaction is continued for 35min to ensure the complete lattice damage process and the oxidation process of vanadium, so as to obtain a roasting product.
(4) Pressure leaching process: weighing sulfuric acid with the mass fraction of 8% of the baked product, and mixing the sulfuric acid with the aqueous solution of liquid-solid ratio: roasting product=1.5ml:1g, preparing sulfuric acid aqueous solution, immersing the roasting product into sulfuric acid leaching solution, wherein the pressure in a reaction kettle in the leaching process is 1.2MPa, the leaching temperature is 160 ℃, and the leaching time is 1h. Finally, the leaching rate of the obtained vanadium is 86.07 percent.
Example 2:
In the example, stone coal raw ore is taken from a place of Shaanxi, and the stone coal comprises the following components in percentage by mass: v 2O5 content 1.02%, C content 0.16%, TFe content 1.38%, siO 2 content 72.56%, quartz and vanadium-containing illite are the main mineral constituents, wherein vanadium minerals are mainly assigned to illite in the same manner as in the category, and the content is 92%. The vanadium extraction method based on fluidized roasting and pressure leaching of stone coal mine by microwave heating is developed according to the following steps:
(1) Crushing: after the raw ore is crushed by a jaw crusher and a lattice overflow ball mill, the granularity of the product reaches 86 percent of-0.074 mm and 70 percent of-0.045 mm, and the finely ground stone coal powder ore is obtained.
(2) And (3) preheating and roasting: the finely ground stone coal powder ore is fed into a preheating roasting device of a fluidized microwave roasting system. The coke oven gas is burned as fuel to heat the interior of the preheating roasting device to 635 ℃. The material flow is heated to about 450 ℃ by the device, and the preheated stone coal powder ore is obtained.
(3) Fluidized microwave roasting process: the preheated stone coal powder ore is fed into a fluidized microwave roasting device, and the temperature in the oven body is controlled to be 950 ℃ by adjusting a microwave heater and the ventilation quantity. The power of the microwave heater is 40kW, mixed gas of 6.2m 3/h is introduced into the furnace body, wherein the ratio of air to O 2 is 3:1 according to the volume ratio, and the reaction is continued for 60min to ensure the complete lattice damage process and the oxidation process of vanadium, so as to obtain a roasting product.
(4) Pressure leaching process: weighing sulfuric acid with the mass fraction of 13% of the baked product, and mixing the sulfuric acid with the aqueous solution of liquid-solid ratio: roasting product = 2ml:1g, preparing sulfuric acid aqueous solution, immersing the roasting product into sulfuric acid leaching solution, wherein the pressure in a reaction kettle in the leaching process is 1.5MPa, the leaching temperature is 180 ℃, and the leaching time is 1.5h. The leaching rate of the finally obtained vanadium is 89.28%.
Example 3:
In the example, stone coal raw ore is taken from a certain Gansu province, and the raw ore contains the following components in percentage by mass: v 2O5 content 1.83%, C content 1.59%, TFe content 1.43%, siO 2 content 58.51%, quartz and vanadium-containing phlogopite are the main constituent minerals. The vanadium extraction method based on fluidized roasting and pressure leaching of stone coal mine by microwave heating is developed according to the following steps:
(1) Crushing: after the raw ore passes through a crusher and is ground, the granularity of the product reaches 75 percent of-0.074 mm and 67 percent of-0.045 mm, and the ground stone coal powder ore is obtained.
(2) And (3) preheating and roasting: and feeding the finely ground stone coal powder ore into a preheating roasting device. The natural gas is burned as fuel to heat the interior of the preheating roasting device to 600 ℃. The material flows through the device, is heated to about 415 ℃ by the effects of heat conduction, convection and radiation, and the preheated stone coal powder ore is obtained.
(3) Fluidized microwave roasting process: the preheated stone coal powder ore is fed into a fluidized microwave roasting device, and the temperature in the oven body is controlled to be 910 ℃ by adjusting a microwave heater and the ventilation quantity. The power of the microwave heater is 38kW, mixed gas of 5.5m 3/h is introduced into the furnace body, wherein the ratio of air to O 2 is 3:1 according to the volume ratio, and the reaction is continued for 28min to ensure the complete lattice damage process and the oxidation process of vanadium, so as to obtain a roasting product.
(4) Pressure leaching process: weighing sulfuric acid with the mass fraction of 13% of the baked product, and mixing the sulfuric acid with the aqueous solution of liquid-solid ratio: roasting product = 2ml:1g, preparing sulfuric acid aqueous solution, immersing the roasting product into sulfuric acid leaching solution, wherein the pressure in a reaction kettle in the leaching process is 1.5MPa, the leaching temperature is 150 ℃, and the leaching time is 1h. Finally, the leaching rate of the obtained vanadium is 92.26 percent. This shows that the fluidized microwave roasting and pressurizing leaching process can raise the vanadium leaching effect of refractory stone coal effectively.
Example 4:
(1) Crushing: the stone coal mine crushing process consists of two working procedures of crushing and grinding. The ore feeding granularity of stone coal is in the range of 8 mm-250 mm. Crushing stone coal mine to 1-6 mm by a jaw crusher, and grinding the powder ore to-0.045 mm accounting for 55-70% by adopting a dry semi-autogenous mill to obtain the ground stone coal powder ore. The specific grinding fineness is determined according to the properties of different ores, and the finer the embedding granularity of vanadium minerals is, the finer the fineness of the crushed products is.
(2) And (3) preheating and roasting: the finely ground stone coal powder ore enters a preheating roasting device of a fluidization microwave roasting system, and the material change of the preheating roasting device is shown in figure 2. The lower part of the preheating and roasting device is provided with a combustion station, and combustible gas such as natural gas, coke oven gas and the like is mixed with air for combustion to heat the internal temperature of the preheating and roasting device to 650 ℃. The stone coal dust ore is preheated in the process of flowing through the preheating roasting device. The retention time is 25-40 s, and the adsorbed water in the material can be removed in the process. And preheating and roasting the stone coal powder, and heating the stone coal powder to 420 ℃ to obtain the preheated stone coal powder.
(3) Fluidized microwave roasting process: the preheated stone coal powder ore is directly fed into a fluidized microwave roasting device, and the material change schematic diagram is shown in figure 3. The microwave heater on the outer wall of the fluidized microwave roasting device can generate a microwave field to rapidly heat the material particles. Air and O 2 are introduced into the bottom of the fluidized microwave roasting device, and the roasting atmosphere can be regulated and controlled according to the mineral feeding property change. The internal temperature of the device is controlled within 950 ℃ by regulating and controlling the air quantity (6.5 m 3/h) and the power (30 kW) of the microwave heater. In the roasting process, minerals such as carbonaceous and pyrite are oxidized first. Secondly, minerals such as kaolinite, dolomite and the like are decomposed. When the material temperature reaches the set temperature, the mica minerals undergo dehydroxylation reaction, and Al-O octahedron and Si-O tetrahedron in the crystal lattice are efficiently destroyed. Meanwhile, vanadium atoms present therein in a congener form are more easily dissociated and oxidized. According to different mineral powder properties, the retention time of the mineral powder in the fluidized microwave roasting process is 30min, and a roasting product is obtained.
(4) Pressure leaching process: vanadium ions in the roasted product exist in +4 and +5 valences and are easy to dissolve in acid and alkali. Thus, the pressure leaching process uses sodium hydroxide as the leaching agent. The leaching solution reacts with the oxide of the high-valence vanadium to generate vanadium ions for leaching, thereby realizing the leaching of vanadium in the powder ore, and the material change diagram of the adopted pressure leaching device is shown in figure 4. Weighing sodium hydroxide according to the mass fraction of 10% of the baked product, and mixing the sodium hydroxide aqueous solution according to the liquid-solid ratio: roasting product = 1.8ml:1g, preparing sodium hydroxide aqueous solution, as sodium hydroxide leaching solution, immersing the roasting product into sodium hydroxide, ensuring the pressure in a reaction kettle to be 1.3MPa in the leaching process, wherein the leaching temperature is 180 ℃, leaching for 1h, obtaining leaching rate of vanadium in stone coal to be 89.2%, and recycling the leaching solution obtained after vanadium extraction of vanadium-rich noble liquid.
Example 5:
The same as in example 1, except that: the temperature in the preheating roasting device is 658 ℃, the temperature in the fluidization microwave roasting device is 934 ℃, the air quantity is 5.8m 3/h, and other conditions are kept unchanged. Finally, the total leaching rate of vanadium was 88.67%.
Example 6:
The same as in example 2, except that: the temperature in the preheating roasting device is 686 ℃, the temperature in the fluidization microwave roasting device is 920 ℃, the air quantity is 6.2m 3/h, and other conditions are kept unchanged. Finally, the total leaching rate of vanadium was 89.54%.
Example 7:
The difference from example 3 is that: the temperature in the preheating roasting device is 700 ℃, the temperature in the fluidization microwave roasting device is 942 ℃, the air quantity is 5.1m 3/h, and other conditions are kept unchanged. Finally, the total leaching rate of vanadium was 87.54%.
Example 8:
The same as in example 4, except that: the temperature in the preheating roasting device is 700 ℃, the temperature in the fluidized microwave roasting device is 918 ℃, the air quantity is 6.3m 3/h, and other conditions are kept unchanged. Finally, the total leaching rate of vanadium was 85.84%.
Comparative example 1:
The difference from example 1 is that by atmospheric leaching, the leaching solution ions cannot effectively enter the microcracks in the particles, and the total leaching rate of vanadium is only 75.64%.
Comparative example 2:
the difference from example 1 is that the blank roasting-pressure leaching is adopted, compared with the method that a large number of microcracks are not formed in the particles, and the liquid-solid reaction is insufficient. The total leaching rate of the final vanadium is only 80.58%.
Claims (3)
1. The vanadium extraction method for stone coal mine fluidization roasting-pressure leaching based on microwave heating is characterized by comprising the following steps of: preheating roasting, fluidized microwave roasting and pressure leaching;
The stone coal is mica type illite type refractory stone coal, wherein the content of C is 0.16%, 0.73% or 1.59% by mass;
before preheating roasting, crushing stone coal ore to obtain ground stone coal powder ore with the particle size of-0.045 mm accounting for 55% -70%, and then preheating roasting;
The stone coal mine crushing process comprises two working procedures of crushing and grinding;
the crushing procedure is as follows: crushing stone coal mines to 1-6 mm by a jaw crusher to obtain fine ores; the ore grinding process comprises the following steps: grinding the powder ore to-0.045 mm accounting for 55% -70% by adopting a dry semi-autogenous mill;
In the preheating roasting process, firstly, the interior of a preheating roasting device is heated to 600-700 ℃, and stone coal powder is heated to 400-500 ℃ under the effects of heat conduction, convection and radiation, so as to obtain preheated stone coal powder;
Fluidized microwave roasting is as follows: directly feeding the preheated stone coal powder ore into a fluidization microwave roasting device, generating a microwave field by a microwave heater to rapidly heat material particles, so that the stone coal material is damaged and cracked in the particles under the condition of not sintering, introducing air and O 2 into the bottom of the fluidization microwave roasting device, regulating and controlling roasting atmosphere according to the change of ore feeding property, controlling the internal temperature of the fluidization microwave roasting device to 950 ℃ by regulating and controlling the gas quantity and the power of the microwave heater to 5m 3/h~6.5m3/h, controlling the power of the microwave heater to 25 kW-45 kW, and controlling the retention time of mineral powder to 28 min-60 min to obtain a roasting product;
In the pressure leaching process, a roasting product is immersed in a leaching solution, the pressure in a reaction kettle is ensured to be 1.0-1.5 MPa, the leaching solution is 1g of the roasting product (1.5-2) mL, the leaching temperature is 150-180 ℃, the mass of a leaching agent in the leaching solution accounts for 5-15% of the mass of the roasting product, and the leaching time is 1-2 h, so that vanadium-rich noble liquid and leaching slag are obtained.
2. The vanadium extraction method based on fluidized roasting-pressure leaching of stone coal mine by microwave heating according to claim 1, wherein the pressure leaching is: sulfuric acid or sodium hydroxide is used as a leaching agent, and water is added into the leaching agent to prepare leaching liquid.
3. The vanadium extraction method based on fluidized roasting and pressure leaching of the stone coal mine by microwave heating according to claim 1, wherein the vanadium extraction method based on fluidized roasting and pressure leaching of the stone coal mine by microwave heating is characterized in that the leaching rate of vanadium in the stone coal mine reaches 85% -90%.
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| WO2021056110A1 (en) * | 2019-09-25 | 2021-04-01 | 9203-5468 Quebec Inc. Dba Nmr360 | Process for the recovery of vanadium oxides from various materials |
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