CN115747527A - Vanadium extraction method of stone coal ore fluidized roasting-pressure leaching based on microwave heating - Google Patents
Vanadium extraction method of stone coal ore fluidized roasting-pressure leaching based on microwave heating Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 140
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 70
- 238000010438 heat treatment Methods 0.000 title claims abstract description 29
- 238000000605 extraction Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 70
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- 239000003795 chemical substances by application Substances 0.000 claims description 9
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- 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 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 4
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- 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
- 238000004519 manufacturing process Methods 0.000 description 2
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- 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
- 230000000191 radiation effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
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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
- Y02P10/20—Recycling
Abstract
A vanadium extraction method of stone coal ore 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, the stone coal particles can absorb microwave energy and convert the microwave energy into heat energy, and the temperature inside and outside the particles is rapidly increased simultaneously. According to the wave-absorbing characteristic difference of each mineral, the vanadium-containing mineral is selectively heated; the fluidized roasting technology ensures that 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 damage and cracks in the particles under the condition that the stone coal material is not sintered is fulfilled. And in the pressure leaching process, the damages and the cracks can enable leachate ions in the solution to efficiently enter the interior of the particles to react, so that liquid-solid contact reaction sites are improved, and the leaching rate is improved. The method is suitable for the refractory stone coal mine, and can realize effective leaching of mica type and illite type refractory stone coal.
Description
Technical Field
The invention relates to the technical field of vanadium extraction, in particular to a vanadium extraction method of stone coal ore fluidization roasting-pressure leaching 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 highly-polluted waste gas and waste water, and can effectively reduce pollution. However, the blank roasting-leaching process has poor leaching effect on refractory stone coal mines in which vanadium exists in the form of similar similarities. 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 comes from heat conduction, convection and radiation, which results in uneven heating inside and outside the material and low heat transfer efficiency. And feeding ore before entering the furnace needs to be pelletized or baked, and cooling and crushing are needed after discharging. On one hand, the gas-solid contact is insufficient and the mass and heat transfer efficiency is low in the reaction process, and on the other hand, the production process is complex, the heat is wasted and the operation cost is high.
And the fluidized roasting technology can be used for strengthening the roasting effect of blank roasting. The fluidized roasting technology also makes a technical breakthrough in the fields of refractory iron ores, iron-manganese ores, stone coal and other various mineral resources, and part of projects are industrially applied. For example, patent CN106868292A "a complex iron ore reinforced separation method based on mineral phase segmentation precise control", patent CN111644267A "a suspension roasting system and method for industrial processing of iron and manganese ores", patent CN111304465A "a method for vanadium-containing stone coal decarburization-crystal breaking roasting reinforced acid leaching vanadium extraction", and patent CN111304464A "method for stone coal vanadium ore multistage roasting reinforced acid mixing curing vanadium extraction". However, these conventional fluidized roasts cannot cause a great deal of effective damage and cracks inside the stone coal particles. On the other hand, when the common microwave roasting is carried out, material particles are stacked, and local overheating sintering is easy to generate. How to cause a large amount of damage and cracks inside stone coal particles under the condition of ensuring no sintering is a difficulty for researching the stone coal roasting technology.
In the blank roasting-leaching process, the leaching process is normal-pressure leaching, and when the stone coal is leached at normal pressure, the leaching efficiency of a roasted product of the stone coal is relatively low, the consumption of a leaching agent is large, and the leaching time is long, so 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 vanadium extraction method of stone coal ore fluidization roasting-pressure leaching based on microwave heating. The invention strengthens the blank roasting effect of the stone coal by microwave heating and fluidized roasting technologies, and achieves the purposes of improving the reaction mass and heat transfer efficiency, improving the heating rate and strengthening the crystal lattice damage of vanadium-containing minerals.
The invention strengthens the leaching efficiency of the roasted product by pressure leaching, and achieves the purposes of reducing the dosage of the leaching solution, shortening the leaching time and improving the vanadium leaching rate. So as to realize the high-efficiency leaching of the mica type and illite type refractory stone coal.
And the microwave fluidized roasting ingeniously realizes the purpose that a large amount of damage and cracks can be generated inside the particles under the condition that the stone coal material is not sintered. The damages and cracks greatly promote leachate ions in the solution to efficiently enter the particles to react in the pressure leaching process, so that effective liquid-solid contact is realized and the leaching rate is improved. Because the damage and the cracks are small, ions in the leaching liquid cannot enter effectively in the leaching process under normal pressure, and the effect of the cracks generated by microwave roasting can be revealed only through high pressure.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention relates to a vanadium extraction method of stone coal ore fluidization roasting-pressure leaching based on microwave heating, which comprises the following specific embodiments:
s1, a crushing process:
crushing stone coal mine to obtain fine stone coal ore powder with-0.045 mm size of 55-70%;
in S1, the process of crushing the stone coal powder comprises two steps of crushing and grinding. The stone coal feeding granularity 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 fine ore to-0.045 mm which accounts for 55% -70%. The specific grinding fineness is determined according to different ore properties, and the finer the embedding particle size of the vanadium mineral is, the finer the fineness of the crushed product is.
S2, preheating and roasting:
the finely ground stone coal powder ore is preheated, the preheating temperature is 600-700 ℃, the retention time is 25-40 s, and the absorbed water in the materials can be removed in the process. Preheating and roasting the stone coal fine powder, and heating the stone coal fine powder to 400-500 ℃ to obtain preheated stone coal fine powder;
s3, fluidized microwave roasting:
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. Introducing air and O into the bottom of the fluidized microwave roasting device 2 The roasting atmosphere can be adjusted and controlled according to the change of ore feeding property, and the fluidization microwave roasting device adjusts and controls the air flow (5 m) 3 /h～6.5m 3 H) and the power of a microwave heater (25 kW-45 kW) to control the internal temperature of the fluidized microwave roasting device within the range of 850-950 ℃. During the roasting process, carbonaceous, pyrite and other minerals are first oxidized. Secondly, minerals such as kaolinite and dolomite are decomposed. When the temperature of the material reaches the set temperature, the mica minerals are subjected to dehydroxylation reaction, and Al-O octahedrons and Si-O tetrahedrons in crystal lattices are efficiently damaged. Meanwhile, vanadium atoms in the vanadium oxide are more easily dissociated and oxidized in the form of a similar image. According to different properties of the mineral powder, the retention time of the mineral powder in the fluidization microwave roasting process is 28-60 min, and a roasted product is obtained.
S4, pressure leaching:
vanadium ions in the roasted product exist mostly in +4 and +5 valences, and are easily soluble in acids and bases. Thus, the pressure leaching process employs sulfuric acid or sodium hydroxide as a leaching agent. The leaching agent is added with water to prepare leaching solution, the leaching solution reacts with the oxide of the high-valence vanadium to generate vanadium ions to be dissolved out, and then the dissolution of the vanadium in the fine ore is realized. The pressure leaching process comprises the following steps: 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, the leaching solution: 1g of roasted product (1.5-2) mL, leaching temperature of 150-180 ℃, leaching agent mass in the leaching solution accounting for 5-15% of the roasted product mass percent, and leaching time of 1-2 h to obtain vanadium-rich pregnant solution and leaching residue.
By adopting the method for extracting vanadium by fluidized roasting-pressure leaching of stone coal mine based on microwave heating, the leaching rate of vanadium in the stone coal mine can reach 85% -90%, and the leachate obtained after vanadium extraction of the vanadium-rich pregnant solution can be recycled.
The key points of the invention are as follows:
1. the invention strengthens the roasting effect of the stone coal by a microwave heating technology. In the microwave field, the 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 rapidly increased. In addition, according to the difference of wave-absorbing characteristics of various minerals, the vanadium-containing minerals are selectively heated.
2. The invention enhances the leaching efficiency of the roasted product by a pressure leaching technology. The pressure leaching operation can effectively improve the leaching pressure and the leaching temperature, thereby reducing the dosage of the leaching solution, shortening the leaching time and improving the vanadium leaching rate. The leaching effect on the refractory stone coal can be improved, and the effective leaching of the mica type and illite type refractory stone coal can be realized.
3. In the leaching process, acid liquor or alkali liquor can be selected as a leaching agent, so that the method can be better suitable for stone coal raw ores with different properties.
4. The invention strengthens the roasting effect of the stone coal by a fluidized roasting process. The fluidized roasting has the advantages of full gas-solid contact, high mass and heat transfer efficiency, low operation cost, environmental protection and the like, and is a high-efficiency stone coal vanadium extraction process.
Compared with the prior art, the vanadium extraction method of the stone coal ore fluidized roasting-pressure leaching based on microwave heating has the beneficial effects that:
(1): the invention strengthens the roasting effect of the stone coal by microwave heating and fluidization roasting technologies. In the microwave field, the 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 rapidly increased. In addition, according to the difference of wave-absorbing characteristics of various minerals, the vanadium-containing minerals are selectively heated; the fluidized roasting technology has the advantages of full gas-solid contact, high mass and heat transfer efficiency, low operation cost, environmental protection, simplified process and the like in the roasting process.
(2): the pressure leaching operation can effectively improve the leaching pressure and the leaching temperature, thereby reducing the dosage of the leaching solution, shortening the leaching time and improving the vanadium leaching rate. The leaching effect on the refractory stone coal can be improved, and the effective leaching of mica type and illite type refractory stone coal can be realized.
Drawings
FIG. 1 is a schematic flow diagram of a vanadium extraction method based on microwave heating stone coal ore fluidized roasting-pressure leaching.
FIG. 2 is a schematic diagram of a material change of the preheating roasting apparatus.
FIG. 3 is a schematic diagram of the material change of the fluidized microwave roasting apparatus.
Fig. 4 is a schematic diagram of a material change of the pressure leaching device.
Detailed Description
The technical scheme in the patent implementation is clearly and completely described with reference to the attached 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 the application. All other embodiments, which can be derived by a person skilled in the art without making creative efforts, based on the present invention, belong to the protection scope of the present patent.
Example 1:
in the example, the stone coal raw ore is taken from a certain place in Hunan, and the stone coal raw ore comprises the following components in percentage by mass:V 2 O 5 1.32% of C, 0.73% of TFe, 1.12% of SiO 2 The content is 57.61%, and quartz and vanadium-containing phlogopite are main constituent minerals. The vanadium extraction method of stone coal ore fluidized roasting-pressure leaching based on microwave heating has a flow schematic diagram shown in figure 1, and specifically comprises the following steps:
(1) And (3) a crushing process: after the raw ore is crushed and ground by a crusher, the granularity of the product reaches-0.074 mm accounting for 78 percent and-0.045 mm accounting for 69 percent, and the ground stone coal powder ore is obtained.
(2) Preheating and roasting: feeding the finely ground stone coal powder ore into a preheating roasting device. The natural gas is used as fuel to burn, and the interior of the preheating roasting device is heated to 600 ℃. The material flows through the device and is heated to about 400 ℃ by heat conduction, convection and radiation effects, so as to obtain the preheated stone coal fine ore.
(3) Fluidized microwave roasting process: feeding the preheated stone coal fine ore into a fluidized microwave roasting device, adjusting a microwave heater and introducing air quantity to control the temperature in a furnace body to be 910 ℃. The power of the microwave heater is 35kW, and 5.5m of microwave is introduced into the furnace body 3 H mixed gas of air and O in a volume ratio 2 The ratio of (1) is 4, and the reaction is continued for 35min to ensure that the lattice destruction process and the vanadium oxidation process are completely carried out, so as to obtain a roasted product.
(4) And (3) pressure leaching process: weighing sulfuric acid accounting for 8% of the mass fraction of the roasted product, and mixing the sulfuric acid aqueous solution according to the liquid-solid ratio: 1g of roasted product =1.5mL, preparing a sulfuric acid aqueous solution as a sulfuric acid leaching solution, and immersing the roasted product into the 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. The leaching rate of the finally obtained vanadium was 86.07%.
Example 2:
in the example, the stone coal raw ore is taken from somewhere in Shaanxi, and the stone coal comprises the following components in percentage by mass: v 2 O 5 1.02% of C, 1.38% of TFe, siO 2 The content is 72.56%, quartz and vanadium-containing illite are main mineral compositions, wherein the vanadium mineral is mainly represented in the illite in a similar manner, and the content is 92%. Based on microwave plusThe vanadium extraction method of the hot stone coal ore fluidized roasting-pressure leaching is developed according to the following steps:
(1) And (3) crushing: after the raw ore is combined and crushed by a jaw crusher and a lattice overflow ball mill, the granularity of the product reaches-0.074 mm accounting for 86 percent and-0.045 mm accounting for 70 percent, and the ground stone coal powder ore is obtained.
(2) Preheating and roasting: feeding the finely ground stone coal powder ore into a preheating roasting device of a fluidized microwave roasting system. The coke oven gas is used as fuel to burn, and the interior of the preheating roasting device is heated to 635 ℃. The material flow through the apparatus is heated to about 450 c to obtain preheated stone coal fines.
(3) Fluidized microwave roasting process: feeding the preheated stone coal fine ore into a fluidized microwave roasting device, adjusting a microwave heater and introducing air quantity to control the temperature in the furnace body to be 950 ℃. The power of the microwave heater is 40kW, and 6.2m of microwave is introduced into the furnace body 3 H mixed gas of air and O in a volume ratio 2 The reaction is continued for 60min to ensure that the crystal lattice destruction process and the vanadium oxidation process are completely carried out, and a roasted product is obtained.
(4) And (3) a pressure leaching process: weighing sulfuric acid accounting for 13% of the mass fraction of the roasted product, and mixing the sulfuric acid aqueous solution according to the liquid-solid ratio: 1g of roasted product =2mL, preparing a sulfuric acid aqueous solution as a sulfuric acid leaching solution, and immersing the roasted product into the 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 percent.
Example 3:
in the example, the stone coal raw ore is taken from a place in Gansu, and the raw ore comprises the following components in percentage by mass: v 2 O 5 1.83% of C, 1.59% of TFe, 1.43% of SiO 2 The content is 58.51 percent, and quartz and vanadium-containing phlogopite are main constituent minerals. The vanadium extraction method of stone coal ore fluidization roasting-pressure leaching based on microwave heating is developed according to the following steps:
(1) And (3) crushing: after the raw ore is crushed and ground by a crusher, the granularity of the product reaches-0.074 mm and accounts for 75 percent, and-0.045 mm and accounts for 67 percent, and the ground stone coal powder ore is obtained.
(2) Preheating and roasting: feeding the finely ground stone coal powder ore into a preheating roasting device. Natural gas is used as fuel for combustion, and the interior of the preheating roasting device is heated to 600 ℃. The material flows through the device and is heated to 415 ℃ by heat conduction, convection and radiation effects, and the preheated stone coal fine ore is obtained.
(3) Fluidized microwave roasting process: feeding the preheated stone coal fine ore into a fluidized microwave roasting device, adjusting a microwave heater and introducing air quantity to control the temperature in the furnace body to be 910 ℃. The power of the microwave heater is 38kW, and 5.5m of microwave is introduced into the furnace body 3 H mixed gas of air and O in a volume ratio 2 The reaction is continued for 28min to ensure that the lattice destruction process and the vanadium oxidation process are completely carried out, and a roasted product is obtained.
(4) And (3) pressure leaching process: weighing sulfuric acid accounting for 13% of the mass fraction of the roasted product, and mixing the sulfuric acid aqueous solution according to the liquid-solid ratio: 1g of roasted product =2mL, preparing a sulfuric acid aqueous solution as a sulfuric acid leaching solution, and immersing the roasted product into the 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. The leaching rate of the finally obtained vanadium is 92.26 percent. The result shows that the fluidized microwave roasting and pressurizing leaching process can effectively improve the vanadium leaching effect of the refractory stone coal.
Example 4:
(1) And (3) a crushing process: the crushing process of the stone coal mine consists of two working procedures of crushing and grinding. The feeding granularity of the 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 mill the fine ore to-0.045 mm accounting for 55% -70%, so as to obtain the finely ground stone coal fine ore. The specific grinding fineness is determined according to different ore properties, and the finer the embedding particle size of the vanadium mineral is, the finer the fineness of the crushed product is.
(2) Preheating and roasting: the finely ground stone coal fine ore enters a preheating roasting device of a fluidized microwave roasting system, and the material change of the preheating roasting device is shown in figure 2. The lower part of the preheating roasting device is provided with a combustion station, combustible gas such as natural gas, coke oven gas and the like is mixed and combusted with air, and the internal temperature of the preheating roasting device is heated to 650 ℃. The stone coal fine ore is preheated in the process of flowing through the preheating roasting device. The retention time is 25 s-40 s, and the absorbed water in the material can be removed in the process. After preheating and roasting, the stone coal ore powder is heated to 420 ℃, and the preheated stone coal fine powder is obtained.
(3) Fluidized microwave roasting process: the preheated stone coal fine 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 heat the material particles rapidly. Introducing air and O into the bottom of the fluidized microwave roasting device 2 The roasting atmosphere can be adjusted and controlled according to the change of the feeding property. The device regulates and controls the air flow (6.5 m) 3 H) and microwave heater power (30 kW) to control the internal temperature of the apparatus within 950 ℃. During the roasting process, carbonaceous, pyrite and other minerals are first oxidized. Secondly, minerals such as kaolinite and dolomite are decomposed. When the temperature of the material reaches the set temperature, the mica minerals are subjected to dehydroxylation reaction, and Al-O octahedrons and Si-O tetrahedrons in crystal lattices are efficiently damaged. Meanwhile, vanadium atoms in the vanadium oxide are more easily dissociated and oxidized in the form of a similar image. According to different properties of the mineral powder, the retention time of the mineral powder in the fluidization microwave roasting process is 30min, and a roasted product is obtained.
(4) And (3) pressure leaching process: vanadium ions in the roasted product exist mostly in +4 and +5 valences, and are easily soluble in acids and bases. Thus, the pressure leaching process employs sodium hydroxide as the leaching agent. The leaching solution reacts with the oxide of high-valence vanadium to generate vanadium ions for dissolution, so that the dissolution of vanadium in the fine ore is realized, and a material change diagram of the adopted pressure leaching device is shown in figure 4. Weighing sodium hydroxide according to the mass fraction of 10 percent of the roasted product, and mixing the following components in percentage by liquid-solid ratio: 1g of roasted product =1.8mL, preparing a sodium hydroxide aqueous solution as a sodium hydroxide leaching solution, immersing the roasted product in sodium hydroxide, wherein the leaching process ensures that the pressure in a reaction kettle is 1.3MPa, the leaching temperature is 180 ℃, the leaching time is 1h, the leaching rate of vanadium in the obtained stone coal can reach 89.2%, and the leaching solution obtained after vanadium extraction of the vanadium-rich pregnant solution can be recycled.
Example 5:
the difference from example 1 is that: the temperature in the preheating roasting device is 658 ℃, the temperature in the fluidization microwave roasting device is 934 ℃, and the air quantity is 5.8m 3 The other conditions were kept constant. Finally, the total vanadium leaching rate was 88.67%.
Example 6:
the difference from example 2 is that: the temperature in the preheating roasting device is 686 ℃, the temperature in the fluidization microwave roasting device is 920 ℃, and the air quantity is 6.2m 3 The other conditions were kept constant. 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 ℃, and the gas amount is 5.1m 3 H, other conditions were kept constant. Finally, the total vanadium leaching rate was 87.54%.
Example 8:
the difference from example 4 is that: the temperature in the preheating roasting device is 700 ℃, the temperature in the fluidization microwave roasting device is 918 ℃, and the gas amount is 6.3m 3 The other conditions were kept constant. Finally, the total vanadium leaching rate was 85.84%.
Comparative example 1:
the difference from example 1 is that, by using atmospheric leaching, the leaching solution ions can not effectively enter the microcracks inside the particles, and the total leaching rate of vanadium is only 75.64%.
Comparative example 2:
the difference from example 1 is that, in comparison with the blank calcination-pressure leaching, there are not much micro-cracks in the interior of the granule and the liquid-solid reaction is not sufficient. The final vanadium leaching rate is only 80.58%.
Claims (10)
1. A vanadium extraction method of stone coal ore fluidized roasting-pressure leaching based on microwave heating is characterized by comprising the following steps: preheating roasting, fluidized microwave roasting and pressure leaching.
2. The method for extracting vanadium by fluidized roasting-pressure leaching of stone coal ore based on microwave heating according to claim 1, characterized in that, before preheating roasting, the stone coal ore is crushed to obtain-0.045 mm of 55% -70% of ground stone coal fine ore, and then preheating roasting is carried out.
3. The method for extracting vanadium by fluidized roasting-pressure leaching of stone coal ore based on microwave heating as claimed in claim 2, wherein the process of crushing the stone coal ore comprises two steps of crushing and grinding.
4. The method for extracting vanadium from stone coal ore by fluidized roasting-pressure leaching based on microwave heating as claimed in claim 3, wherein the crushing process comprises: crushing the stone coal mine to 1-6 mm by a jaw crusher to obtain fine ore; the ore grinding process comprises the following steps: the powder ore is ground to-0.045 mm and accounts for 55-70% by adopting a dry semi-autogenous grinding machine.
5. The method for extracting vanadium by fluidized roasting-pressure leaching of stone coal ore based on microwave heating as claimed in claim 1, wherein in the preheating roasting process, the stone coal ore powder is heated to 400-500 ℃ to obtain preheated stone coal fine ore.
6. The method for extracting vanadium through fluidized roasting-pressure leaching of stone coal ores based on microwave heating as claimed in claim 5, wherein the preheating roasting is as follows: the finely ground stone coal powder ore is preheated, the preheating temperature is 600-700 ℃, and the retention time is 25-40 s.
7. The method for extracting vanadium from stone coal ore by fluidized roasting-pressure leaching based on microwave heating as claimed in claim 1, wherein the fluidized microwave roasting is: directly feeding the preheated stone coal fine ore into a fluidized microwave roasting device, generating a microwave field by a microwave heater to rapidly heat material particles, and introducing air and O into the bottom of the fluidized microwave roasting device 2 Regulating roasting atmosphere according to ore feeding property change, and controlling fluidization by regulating gas flow and microwave heater powerThe internal temperature of the microwave roasting device is within the range of 850-950 ℃, and the retention time of the mineral powder is 28-60 min, so that a roasted product is obtained.
8. The method for extracting vanadium by fluidized roasting-pressure leaching of stone coal ore based on microwave heating as claimed in claim 7, wherein the gas amount is regulated to 5m 3 /h～6.5m 3 The power of the microwave heater is 25 kW-45 kW.
9. The method for extracting vanadium through fluidized roasting-pressure leaching of stone coal ores based on microwave heating as claimed in claim 1, wherein the pressure leaching is as follows: sulfuric acid or sodium hydroxide is used as a leaching agent, the leaching agent is added with water to prepare a leaching solution, a roasted product is immersed in the leaching solution, the pressure in a reaction kettle is ensured to be 1.0-1.5 MPa, and the leaching solution is prepared by the following steps: 1g of roasted product (1.5-2) mL, leaching temperature of 150-180 ℃, leaching agent in the leaching solution accounting for 5-15% of the roasted product by mass percent, and leaching time of 1-2 h to obtain vanadium-rich pregnant solution and leaching residue.
10. The method for extracting vanadium by fluidized roasting-pressure leaching of stone coal mine based on microwave heating according to any one of claims 1 to 9, wherein the vanadium extraction method by fluidized roasting-pressure leaching of stone coal mine based on microwave heating enables the leaching rate of vanadium in stone coal mine to reach 85% -90%.
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