CN114752761B - Method for reinforcing grinding and leaching efficiency of vanadium shale by utilizing microwaves - Google Patents

Abstract

The invention relates to a method for using microwave to enhance the grinding and leaching efficiency of vanadium shale. The technical solution is to crush and screen the vanadium shale raw ore to obtain vanadium shale raw ore with a particle size of <1.5 mm and a particle size of 1.5 to 10.0 mm. Turn on the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency", feed raw vanadium shale ore with a particle size of 1.5~10.0mm from the feed port at 60~150kg/h, and then press the resulting microwave-treated The vanadium shale:water mass ratio is 1:1~3 for water quenching to obtain water quenching slurry; then the mass ratio of vanadium shale raw ore with a particle size of <1.5mm: vanadium shale raw ore with a particle size of 1.5~10.0mm is: 1:1.5~2, mix the water quenching slurry with the vanadium shale raw ore with a particle size <1.5mm, grind the ore, and the resulting grinding product enters the leaching process. The invention has short processing time, low energy consumption, no carbon emissions, good effects on enhancing the grindability and leaching rate of vanadium shale, simple operation and high processing efficiency, and is suitable for microwave strengthening of the vanadium shale full wet vanadium extraction system.

Description

A method of using microwave to enhance vanadium shale grinding and leaching efficiency

Technical field

The invention belongs to the technical field of vanadium extraction from shale. Specifically, it involves a method of using microwaves to enhance the grinding and leaching efficiency of vanadium shale.

Background technique

Vanadium-containing stone coal (vanadium shale) is an important type of vanadium resource. Vanadium extraction from shale has become an important way and demand guarantee for the development and utilization of vanadium resources in my country. Grinding and leaching of vanadium shale are two important links in the shale vanadium extraction process. The grinding and leaching efficiency jointly determine the comprehensive recovery rate of shale vanadium and the cost of vanadium extraction. As a clean energy source, microwaves have received widespread attention in the field of mining and metallurgy, especially in auxiliary grinding and enhanced leaching.

Junpeng Wang et al. (Junpeng Wang, Tao Jinag, Yajing Liu, and XiangxinXue. Effect of microwave irradiation on the grinding and magnetic separation characteristics of vanadium titano-magnetite[J]. Metallurgical Research&Technology, 2019, 116, 419: 1-10) used microwave strengthening Grinding effect of vanadium titanium magnetite. When the microwave power is 2kW and the processing time is 4 minutes, the grindability (in terms of crushing rate) of vanadium-titanium magnetite is increased by up to about 159.1%. On the one hand, although this method can improve the grindability of vanadium-containing minerals to a certain extent, it requires continuous irradiation for 4 minutes under 2kw conditions, which consumes high energy; and the grinding efficiency is increased by 159.1%, which is not a big improvement. On the other hand, this method is an intermittent microwave treatment. When large quantities of vanadium-containing shale need to be processed, the operation of the device will be more complicated and inefficient. Therefore, the existing microwave-enhanced vanadium-containing mineral grinding technology has technical defects such as high processing energy consumption, small improvement in the grindability of vanadium minerals, complex operations, and low processing efficiency.

Li Yinli et al. (Li Yinli, Song Yonghui, Wang Kopeng, Chen Xiangyang. Research on the vanadium extraction process by microwave leaching from stone coal [J]. Nonferrous Metals (Smelting Section), 2016,03:36-44.) used a microwave solution chemical reactor to extract vanadium containing Research on microwave enhanced leaching of vanadium coal. It was found that when the microwave power was 800W, the microwave irradiation time was 60 minutes, the sulfuric acid concentration was 13%, and the liquid-to-solid ratio was 2:1 (mL/g), the vanadium leaching rate was 83.2%; conventional heating was used under the same leaching conditions. After leaching, a vanadium leaching rate of 73.63% can be obtained. Although this method can obtain a higher vanadium leaching rate, it requires continuous microwave irradiation for 60 minutes, long processing time, high energy consumption, and the leaching rate is less than 10% higher than the conventional method. In addition, the microwave solution chemical reactor is an intermittent processing device and cannot achieve continuous operation. When large quantities of vanadium shale need to be processed, the operation is complicated and inefficient. It shows that the existing microwave enhanced leaching technology has the disadvantages of long processing time, high energy consumption, small improvement in vanadium leaching rate, complex device operation and low efficiency.

Yi-zhongYuan et al. (Yi-zhongYuan, Yi-minZhang, Tao Liu1, and Tie-junChen. Comparison of the mechanisms of microwave roasting and conventional roasting and of their effects on vanadium extraction from stone coal[J]. International Journal of Minerals, Metallurgy and Materials , 2015, 22(5):476-482) The vanadium shale was microwave roasted at 800°C for 30 minutes, and the roasted sample was leached, and a vanadium leaching rate of 84% was obtained; compared with conventional roasting at 900°C for 60 minutes, the vanadium leaching rate rate increased by 13%. Compared with conventional roasting methods, although the roasting temperature and roasting time have been shortened, and the leaching rate has also been improved; however, there are still technical defects such as too high processing temperature, long processing time and high energy consumption; furthermore, the microwave roasting temperature It has far exceeded the combustion temperature of carbon in vanadium shale and will produce large amounts of carbon emissions during processing. In addition, this method is an intermittent microwave treatment. When large quantities of vanadium-containing shale need to be processed, the operation of the device will be more complicated and inefficient. Therefore, the existing technology for enhancing the leaching efficiency of vanadium-containing minerals through microwave roasting has technical flaws such as long microwave treatment time, high treatment energy consumption, large carbon emissions, complex operations, and low treatment efficiency.

In summary, the existing technology that uses microwaves to enhance vanadium shale grinding and leaching efficiency suffers from long processing time, high energy consumption, large carbon emissions, small improvement in vanadium leaching efficiency, complex device operation, and low processing efficiency. Technical defects.

Contents of the invention

The present invention aims to overcome the shortcomings of the existing technology, and aims to provide a microwave-based microwave oven with short processing time, low energy consumption, no carbon emissions, good effects on enhancing the grindability and leaching rate of vanadium shale, simple device operation and high processing efficiency. Method to enhance the grinding and leaching efficiency of vanadium shale. This method is suitable for microwave strengthening method of vanadium shale full wet vanadium extraction system.

In order to achieve the above object, the specific steps of the technical solution adopted by the present invention are:

Step 1. Crush and screen the vanadium shale raw ore to obtain vanadium shale raw ore with a particle size of <1.5 mm and vanadium shale raw ore with a particle size of 1.5 to 10.0 mm.

Step 2. Use the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" for microwave processing, set the transportation speed of the conveyor belt, turn on the switches of all wave sources in the continuous microwave processing device, and start the conveyor belt .

The raw vanadium shale ore with a particle size of 1.5 to 10.0 mm is fed from the feed port of the continuous microwave treatment device, and the feeding amount is 60 to 150kg/h; from the discharge of the continuous microwave treatment device Microwave-treated vanadium shale is obtained at the mouth.

Step 3: According to the mass ratio of the microwave-treated vanadium shale:water being 1:1 to 3, the microwave-treated vanadium shale is quenched in water to obtain water-quenched slurry.

Then according to the mass ratio of vanadium shale raw ore with a particle size of <1.5mm: vanadium shale raw ore with a particle size of 1.5-10.0mm, the water quenching slurry and the vanadium with a particle size of <1.5mm are The raw shale ore is mixed and ground to obtain a ground product; the ground product enters the subsequent leaching process.

Step 4. After all material processing is completed, turn off the switches with all wave sources and close the material conveyor belt.

The chemical composition of the vanadium shale is: C content is 4-25wt%; V ₂ O ₅ content is ≥0.45wt%.

The microwave power of the wave source is 500-1500W.

The transport speed of the conveyor belt 9 is na~2na/min.

The structure of the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" is: the continuous microwave processing device is composed of a cavity surrounded by 4 rectangular flat plates, 4n wave sources and a material transmission belt; The length × width of the rectangular flat plate = 2na , the height of the upper surface of the conveyor belt from the top of the cavity is 0.52~0.58a, and the width of the conveyor belt is 0.9~0.95a.

The four rectangular flat plates are the top plate, the left plate, the bottom plate and the right plate respectively. The top plate, the left plate, the bottom plate and the right plate are respectively equipped with the top plate wave source, the left plate wave source, the bottom plate wave source and the right plate wave source; Each wave source consists of a magnetron and a waveguide, and the mounting surface of each wave source on a rectangular flat plate is rectangular.

The installation position of each wave source on its corresponding rectangular plate:

For the sake of simplicity of description, it is assumed that the cavity is separated from the intersection of the top plate and the right side plate, so that the cavity is expanded into a plane; and let: the inlet end of the material be the starting edge of each rectangular plate, The dividing line of the top plate is the upper edge line of the cavity expansion surface, that is, the first horizontal line of the cavity expansion surface is the upper edge line of the top plate, and the second horizontal line of the cavity expansion surface is the upper edge line of the left panel. The third horizontal line is the upper edge of the bottom plate, and the fourth horizontal line of the cavity expansion surface is the upper edge of the right plate.

The installation position of the roof wave source on the roof: the first roof wave source is located at a/2 from the starting edge of the roof, the second roof wave source is located at 2a(2-1)+a/2 from the starting edge of the roof, The three top wave sources are located at 2a(3-1)+a/2 from the starting edge of the top plate,..., and so on, the nth top plate wave source is located at 2a(n-1)+a from the starting edge of the top plate. /2; the distance between the center O1 of the mounting surface of each roof wave source and the upper edge of the roof is a/4, and the long side of the mounting surface of each roof wave source is perpendicular to the upper edge of the roof.

The installation position of the left panel wave source on the left panel: the first left panel wave source is located a/2 from the starting edge of the left panel, and the second left panel wave source is located 2a from the starting edge of the left panel (2-1)+a/2, the third left plate wave source is located at 2a (3-1)+a/2 from the starting edge of the left plate,..., and so on, the nth left plate wave source The side panel wave source is located at 2a(n-1)+a/2 from the starting edge of the left panel; the distance between the center O2 of the installation surface of each left panel wave source and the upper edge of the left panel is a/4, The angle θ between the long side of the wave source mounting surface of each left panel and the upper edge of the left panel is 0° to 45°.

The installation position of the base plate wave source on the base plate: the first base plate wave source is located at 3a/2 from the starting edge of the base plate, the second base plate wave source is located at 2a(2-1)+3a/2 from the starting edge of the base plate, the second base plate wave source is located at 2a(2-1)+3a/2 from the starting edge of the base plate, The three bottom plate wave sources are located at 2a(3-1)+3a/2 from the starting edge of the bottom plate,..., and so on, the nth bottom plate wave source is located at 2a(n-1)+3a from the starting edge of the bottom plate. /2; the distance between the center O3 of the mounting surface of each base plate wave source and the upper edge line of the base plate is a/4, and the long side of the installation surface of each base plate wave source is parallel to the upper edge line of the base plate.

The installation position of the right plate wave source on the right plate: the first right plate wave source is located 3a/2 from the starting edge of the right plate, and the second right plate wave source is located 2a from the starting edge of the right plate (2-1)+3a/2, the third right plate wave source is located at 2a (3-1)+3a/2 from the starting edge of the right plate,..., and so on, the nth right plate wave source The side panel wave source is located at 2a(n-1)+3a/2 from the starting edge of the right panel; the distance between the center O4 of the mounting surface of each right panel wave source and the upper edge of the right panel is a/4, The angle β between the long side of the wave source mounting surface of each right panel and the upper edge of the right panel is 90°-θ.

The long side l of the rectangle is a/6~a/3.

Due to the adoption of the above technical solution, the present invention has the following beneficial effects:

1. The present invention is based on the simulation and experimental verification of the electromagnetic-thermal-stress composite physical field in the cavity of the microwave processing device, and adopts a "continuous microwave processing device to enhance the grinding and leaching efficiency of vanadium shale" (hereinafter referred to as " Continuous microwave processing device") performs microwave processing. The layout of the cavity and wave sources of the continuous microwave processing device has been optimized, and corresponding n wave sources are regularly installed at different positions and different angles on the four flat outer walls of the cavity, realizing the above-mentioned The optimized distribution of the composite physical field in the cavity gives full play to the induction and strengthening effect of microwave on the heterogeneous dissociation of vanadium shale, which greatly improves the grindability of vanadium shale; in addition, the continuous processing method of multiple wave sources can realize the grinding of vanadium shale in the cavity During the operation in the body, it is subjected to continuous multi-dimensional irradiation, which improves the treatment effect and shortens the treatment cycle.

The present invention can realize efficient pretreatment of vanadium shale within 1 to 2 minutes and below the combustion temperature of carbon, thereby increasing the grindability (in terms of crushing rate) of the vanadium shale by more than 200% and reducing the total energy consumption of grinding. (including microwave pretreatment energy consumption and grinding energy consumption of microwave pretreatment products) has been reduced by more than 40%, with short processing cycle, good processing effect and low energy consumption.

2. The present invention focuses on the interweaving characteristics of pyrite and carbonaceous absorbing materials of vanadium shale, and the fine particles of non-absorbing silicate minerals such as mica and feldspar, as well as the interweaving of vanadium-containing minerals in the processing process. The evolution law of electrical characteristics is based on the simulation of composite physical fields through the "continuous microwave processing device" microwave cavity and n-level (the first wave source of each plate is called the first level, and the first wave source of each plate is The two wave sources are called the second level,..., and so on, the nth wave source of each plate is called the nth level) The special design of the wave source and continuous transmission device, during the preprocessing process, continuously excites multi-level microwaves. The plasmodynamic effect causes the treated vanadium shale to be continuously and alternately subjected to n electromagnetic-thermal-stress composite physical fields in the cavity. The distribution form of this composite physical field greatly strengthens the vanadium-containing mica Al The dehydroxylation reaction of -O(OH) octahedron improves the reactivity of shale vanadium during the acid leaching process, increasing the vanadium leaching rate by more than 15% under the same leaching conditions, which has a significant strengthening effect on the vanadium leaching rate. .

3. The present invention adopts a "continuous microwave processing device" with a multi-level continuous distribution mechanism of n-level wave sources combined with a material transmission belt. During the continuous microwave process of vanadium shale, the irradiation power and irradiation time of each level of wave sources are And the transmission speed of the material conveyor belt is adjusted to implement optimized matching; on the one hand, the operating steps of microwave treatment of vanadium shale are simplified, and batch continuous processing of vanadium shale can be achieved under simple operations; on the other hand, due to the The treated vanadium shale continuously passes through n electromagnetic-thermal-stress composite physical fields. The continuous and alternating radiation can greatly reduce the radiation inhomogeneity in multiple physical fields in the microwave device cavity, within 1 to 2 minutes. It can obtain higher grindability and leaching efficiency of vanadium shale, and has high production efficiency.

4. In the process of in-line microwave treatment of vanadium shale in the present invention, due to the short processing cycle, low overall temperature and no carbon emissions, a "continuous microwave treatment device" can be set up between the vanadium shale crushing process and the grinding process. "; Through simple series combination, the organic combination of grinding process, microwave treatment process and grinding process can be realized, and it is suitable for the full wet vanadium extraction system from vanadium shale.

Therefore, the present invention has the characteristics of short processing time, low energy consumption, no carbon emissions, good effect on enhancing the grindability and leaching rate of vanadium shale, simple operation and high processing efficiency. This method is suitable for full wet extraction of vanadium shale. Microwave strengthening method of vanadium system.

Description of the drawings

Figure 1 is a schematic structural diagram of a continuous microwave treatment device used in the present invention to enhance vanadium shale grinding and leaching efficiency;

Figure 2 is an expanded schematic view of the structure shown in Figure 1.

Detailed ways

The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments, which does not limit the scope of protection:

In order to avoid duplication, the relevant structure of the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" adopted in this specific embodiment will be described in a unified manner as follows, and will not be repeated in the embodiment:

As shown in Figure 1, the four rectangular flat plates are respectively the top plate 1, the left plate 3, the bottom plate 5 and the right plate 7. The top plate 1, the left plate 3, the bottom plate 5 and the right plate 7 are respectively equipped with Top plate wave source 8, left plate wave source 2, bottom plate wave source 4 and right plate wave source 6; each wave source is composed of a magnetron and a waveguide, and the installation surface of each wave source on the rectangular plate is rectangular.

For the sake of simplicity of description, it is assumed that the cavity shown in Figure 1 is separated from the intersection of the top plate 1 and the right side plate 7, so that the cavity shown is expanded into the plan view shown in Figure 2; and let: the inlet end of the material is each The starting edge of a rectangular flat plate, the dividing line of top plate 1 is the upper edge line of the cavity development surface, that is, the first horizontal line of the cavity development surface is the upper edge line of top plate 1, and the second horizontal line of the cavity development surface is the left The upper edge of the side plate 3 and the third horizontal line of the cavity development surface are the upper edge of the bottom plate 5 , and the fourth horizontal line of the cavity development surface is the upper edge of the right side panel 7 .

The grinding equipment, leaching equipment and leaching system used in this example are the same as those in Comparative Example 1.

Comparative example 1

Crush 10kg of vanadium shale raw ore to 0~10mm and directly grind it with slurry. The grinding equipment used is a ball mill with a power of 1000W and a single processing capacity of 1kg; the leaching equipment of the grinding product is a magnetic stirrer, and the leaching system is: H ₂ The dosage of SO ₄ is 35wt.%, the leaching time is 8 hours, the leaching temperature is 95°C, the dosage of CaF ₂ is 5wt.%, and the liquid-to-solid ratio is 1.5mL/g.

Example 1

A method of using microwave to enhance the grinding and leaching efficiency of vanadium shale. The steps of the method described in this embodiment are:

Step 1. Crush and screen the vanadium shale raw ore to obtain vanadium shale raw ore with a particle size of <1.5 mm and vanadium shale raw ore with a particle size of 1.5 to 10.0 mm.

Step 2. Use the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" for microwave processing, set the transportation speed of the conveyor belt 9, turn on the switches of all wave sources in the continuous microwave processing device, and start Conveyor belt 9.

The raw vanadium shale ore with a particle size of 1.5 to 10.0 mm is fed from the feed port of the obtained continuous microwave treatment device, and the feeding amount is 60kg/h; it is obtained from the outlet of the continuous microwave treatment device. Microwave treated vanadium shale.

Step 3: According to the mass ratio of the microwave-treated vanadium shale:water being 1:1, the microwave-treated vanadium shale is quenched in water to obtain water-quenched slurry.

Then according to the mass ratio of vanadium shale raw ore with a particle size of <1.5mm: vanadium shale raw ore with a particle size of 1.5-10.0mm being 1:1.5, the water quenching slurry is mixed with the vanadium shale with a particle size of <1.5mm The raw ore is mixed and ground to obtain a ground product; the ground product enters the subsequent leaching process.

Step 4. After all material processing is completed, turn off the switches with all wave sources and close the material conveyor belt (9).

The chemical composition of the vanadium shale is: C content is 4wt%; V ₂ O ₅ content is 0.45wt%.

This example has been tested: the grindability of vanadium shale (based on crushing rate) is 0.1501, an increase of 185.9%; the grinding time is 17min; the energy consumption is 0.3266kw·h/Kg (including: microwave processing energy consumption is 0.0443kw ·h/Kg; grinding energy consumption is 0.2833kw·h/Kg), a decrease of 48.42%; the leaching rate of grinding products is 73.01%, an increase of 15.14%.

This embodiment describes a continuous microwave treatment device that enhances vanadium shale grinding and leaching efficiency. As shown in Figure 1, the continuous microwave processing device is composed of a cavity surrounded by four rectangular flat plates, 4×n wave sources and a material transmission belt 9. The length × width of the rectangular flat plate = 2na The height of the surface from the top of the cavity is 0.55a, the width of the conveyor belt 9 is 0.92a; the transport speed of the conveyor belt 9 is 1.5na/min.

In this embodiment: n=5; the microwave power of the wave source is 500W.

The installation position of each wave source on its corresponding rectangular plate:

The installation position of the top plate wave source 8 on the top plate 1 is shown in Figure 2: the first top plate wave source 8 is located a/2 from the starting edge of the top plate 1, and the second top plate wave source 8 is located 2a+ from the starting edge of the top plate 1 At a/2, the third roof wave source 8 is located at 4a+a/2 from the starting edge of top plate 1, the fourth roof wave source 8 is located at 6a+a/2 from the starting edge of top plate 1, and the fifth The top plate wave source 8 is located at 8a+a/2 from the starting edge of the top plate 1. The distance between the center O1 of the mounting surface of each roof wave source 8 and the upper edge of the roof 1 is a/4, and the long side of the mounting surface of each roof wave source 8 is perpendicular to the upper edge of the roof 1 .

The installation position of the left panel wave source 2 on the left panel 3 is shown in Figure 2: the first left panel wave source 2 is located a/2 from the starting edge of the left panel 3, and the second left panel wave source 2 Located at 2a+a/2 from the starting edge of left panel 3, the third left panel wave source 2 is located at 4a+a/2 from the initial edge of left panel 3, and the fourth left panel wave source 2 It is located at 6a+a/2 from the starting edge of left plate 3, and the fifth left plate wave source 2 is located at 8a+a/2 from the starting edge of left plate 3. The distance between the center O2 of the mounting surface of each left panel wave source 2 and the upper edge of the left panel 3 is a/4, and the distance between the long side of the mounting surface of each left panel wave source 2 and the upper edge of the left panel 3 is The angle θ is 30°.

The installation position of the base plate wave source 4 on the base plate 5 is shown in Figure 2: the first base plate wave source 4 is located 3a/2 from the starting edge of the base plate 5, and the second base plate wave source 4 is located 2a+ from the starting edge of the base plate 5 At 3a/2, the third base plate wave source 4 is located at 4a+3a/2 from the starting edge of base plate 5, and the fourth base plate wave source 4 is located at 6a+3a/2 from the starting edge of base plate 5, and the 5th A base plate wave source 4 is located at 8a+3a/2 from the starting edge of the base plate 5. The distance between the center O3 of the mounting surface of each bottom plate wave source 4 and the upper edge of the bottom plate 5 is a/4, and the long side of the mounting surface of each bottom plate wave source 4 is parallel to the upper edge of the bottom plate 5 .

The installation position of the right plate wave source 6 on the right plate 7 is shown in Figure 2. The second right plate wave source 6 is located at 2a+3a/2 from the starting edge of the right plate 7. The third right plate wave source 6 is located at 2a+3a/2 from the starting edge of the right plate 7. Wave source 6 is located at 4a+3a/2 from the starting edge of right plate 7. The wave source 6 of the fourth right plate is located at 6a+3a/2 from the starting edge of right plate 7. The fifth right plate The wave source 6 is located at 8a+3a/2 from the starting edge of the right side plate 7. The distance between the center O4 of the mounting surface of each right panel wave source 6 and the upper edge of the right panel 7 is a/4, and the distance between the long side of the mounting surface of each right panel wave source 6 and the upper edge of the right panel 7 is Angle β is 60°.

The long side of the rectangle is l=a/6.

Example 2

A method of using microwave to enhance the grinding and leaching efficiency of vanadium shale. The steps of the method described in this embodiment are:

Step 1. Crush and screen the vanadium shale raw ore to obtain vanadium shale raw ore with a particle size of <1.5 mm and vanadium shale raw ore with a particle size of 1.5 to 10.0 mm.

Step 2. Use the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" for microwave processing, set the transportation speed of the conveyor belt 9, turn on the switches of all wave sources in the continuous microwave processing device, and start Conveyor belt 9.

The raw vanadium shale ore with a particle size of 1.5 to 10.0 mm is fed from the feed port of the continuous microwave treatment device, and the feeding amount is 100kg/h; from the outlet of the continuous microwave treatment device, Obtain microwave-treated vanadium shale.

Step 3: According to the mass ratio of the microwave-treated vanadium shale:water being 1:1.2, the microwave-treated vanadium shale is quenched in water to obtain water-quenched slurry.

Then according to the mass ratio of vanadium shale raw ore with a particle size of <1.5mm: vanadium shale raw ore with a particle size of 1.5-10.0mm being 1:1.8, the water quenching slurry is mixed with the vanadium shale with a particle size of <1.5mm The raw ore is mixed and ground to obtain a ground product; the ground product enters the subsequent leaching process.

Step 4. After all material processing is completed, turn off the switches with all wave sources and close the material conveyor belt (9).

The chemical composition of the vanadium shale is: C content is 15wt%; V ₂ O ₅ content is 0.74wt%.

This example has been tested: the grindability of vanadium shale (based on crushing rate) is 0.1678, an increase of 236.3%; the grinding time is 12min; the energy consumption is 0.3333kw·h/Kg (including: microwave processing energy consumption is 0.1333kw ·h/Kg; grinding energy consumption is 0.2kw·h/Kg), a decrease of 47.37%; the leaching rate of grinding products is 83.32%, an increase of 24.45%.

This embodiment describes a continuous microwave treatment device that enhances vanadium shale grinding and leaching efficiency. As shown in Figure 1, the continuous microwave processing device is composed of a cavity surrounded by four rectangular flat plates, 4×n wave sources and a material transmission belt 9. The length × width of the rectangular flat plate = 2na The height from the top of the cavity is 0.58a, the width of the conveyor belt 9 is 0.9a; the transport speed of the conveyor belt 9 is na/min.

In this embodiment: n=10; the microwave power of the wave source is 1000W.

The installation position of each wave source on its corresponding rectangular plate:

The installation position of the top plate wave source 8 on the top plate 1 is shown in Figure 2: the first top plate wave source 8 is located a/2 from the starting edge of the top plate 1, and the second top plate wave source 8 is located 2a+ from the starting edge of the top plate 1 At a/2, the third roof wave source 8 is located at 4a+a/2 from the starting edge of top plate 1,..., and so on, the 10th roof wave source 8 is located at 18a+a from the starting edge of top plate 1 /2 places. The distance between the center O1 of the mounting surface of each roof wave source 8 and the upper edge of the roof 1 is a/4, and the long side of the mounting surface of each roof wave source 8 is perpendicular to the upper edge of the roof 1 .

The installation position of the left panel wave source 2 on the left panel 3 is shown in Figure 2: the first left panel wave source 2 is located a/2 from the starting edge of the left panel 3, and the second left panel wave source 2 Located at 2a+a/2 from the starting edge of left plate 3, the third left plate wave source 2 is located at 4a+a/2 from the starting edge of left plate 3,..., and so on, the third The 10 left plate wave sources 2 are located at 18a+a/2 from the starting edge of the left plate 3. The distance between the center O2 of the mounting surface of each left panel wave source 2 and the upper edge of the left panel 3 is a/4, and the distance between the long side of the mounting surface of each left panel wave source 2 and the upper edge of the left panel 3 is The angle θ is 0° to 45°.

The installation position of the base plate wave source 4 on the base plate 5 is shown in Figure 2: the first base plate wave source 4 is located 3a/2 from the starting edge of the base plate 5, and the second base plate wave source 4 is located 2a+ from the starting edge of the base plate 5 At 3a/2, the third base plate wave source 4 is located at 4a+3a/2 from the starting edge of base plate 5,..., and so on, the 10th base plate wave source 4 is located at 18a+3a from the starting edge of base plate 5 /2 places. The distance between the center O3 of the mounting surface of each bottom plate wave source 4 and the upper edge of the bottom plate 5 is a/4, and the long side of the mounting surface of each bottom plate wave source 4 is parallel to the upper edge of the bottom plate 5 .

The installation position of the right plate wave source 6 on the right plate 7 is shown in Figure 2: the first right plate wave source 6 is located 3a/2 from the starting edge of the right plate 7, and the second right plate wave source 6 It is located at 2a+3a/2 from the starting edge of the right plate 7, and the third right plate wave source 6 is located at 4a+3a/2 from the starting edge of the right plate 7,..., and so on. The 10 right plate wave sources 6 are located at 18a(n-1)+3a/2 from the starting edge of the right plate 7. The distance between the center O4 of the mounting surface of each right panel wave source 6 and the upper edge of the right panel 7 is a/4, and the distance between the long side of the mounting surface of each right panel wave source 6 and the upper edge of the right panel 7 is Angle β is 45°.

The long side of the rectangle is l=a/4.

Example 3

A method of using microwave to enhance the grinding and leaching efficiency of vanadium shale. The steps of the method described in this embodiment are:

Step 1. Crush and screen the vanadium shale raw ore to obtain vanadium shale raw ore with a particle size of <1.5 mm and vanadium shale raw ore with a particle size of 1.5 to 10.0 mm.

Step 2. Use the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" for microwave processing, set the transportation speed of the conveyor belt 9, turn on the switches of all wave sources in the continuous microwave processing device, and start Conveyor belt 9.

The raw vanadium shale ore with a particle size of 1.5 to 10.0 mm is fed from the feed port of the continuous microwave treatment device, and the feeding amount is 150kg/h; from the outlet of the continuous microwave treatment device That is, microwave-treated vanadium shale is obtained.

Step 3: According to the mass ratio of the microwave-treated vanadium shale:water being 1:3, the microwave-treated vanadium shale is quenched in water to obtain water-quenched slurry.

Then according to the mass ratio of vanadium shale raw ore with a particle size of <1.5 mm: vanadium shale raw ore with a particle size of 1.5 to 10.0 mm, the water is quenched with the vanadium shale with a particle size of <1.5 mm. The raw ore is mixed and ground to obtain a ground product; the ground product enters the subsequent leaching process.

Step 4. After all material processing is completed, turn off the switches with all wave sources and close the material conveyor belt (9).

The chemical composition of the vanadium shale is: C content is 25wt%; V ₂ O ₅ content is 1.25wt%.

This example has been tested: the grindability of vanadium shale (based on crushing rate) is 0.1577, an increase of 216%; the grinding time is 16.5min; the energy consumption is 0.3665kw·h/Kg (including: microwave treatment energy consumption is 0.0083 kw·h/Kg; grinding energy consumption is 0.3999kw·h/Kg), a decrease of 40.78%; the leaching rate of grinding products is 76.19%, an increase of 18.39%.

This embodiment describes a continuous microwave treatment device that enhances vanadium shale grinding and leaching efficiency. As shown in Figure 1, the continuous microwave processing device is composed of a cavity surrounded by four rectangular flat plates, 4×n wave sources and a material transmission belt 9. The length × width of the rectangular flat plate = 2na The height from the top of the cavity is 0.52a, the width of the conveyor belt 9 is 0.95a; the transport speed of the conveyor belt 9 is 2na/min.

In this embodiment: n=3.

The microwave power of the wave source is 1500W.

The installation position of each wave source on its corresponding rectangular plate:

The installation position of the top plate wave source 8 on the top plate 1 is shown in Figure 2: the first top plate wave source 8 is located a/2 from the starting edge of the top plate 1, and the second top plate wave source 8 is located 2a+ from the starting edge of the top plate 1 At a/2, the third top plate wave source 8 is located at 4a/2 from the starting edge of the top plate 1. The distance between the center O1 of the mounting surface of each roof wave source 8 and the upper edge of the roof 1 is a/4, and the long side of the mounting surface of each roof wave source 8 is perpendicular to the upper edge of the roof 1 .

The installation position of the left panel wave source 2 on the left panel 3 is shown in Figure 2: the first left panel wave source 2 is located a/2 from the starting edge of the left panel 3, and the second left panel wave source 2 It is located at 2a+a/2 from the starting edge of left plate 3, and the third left plate wave source 2 is located at 4a+a/2 from the starting edge of left plate 3. The distance between the center O2 of the mounting surface of each left panel wave source 2 and the upper edge of the left panel 3 is a/4, and the distance between the long side of the mounting surface of each left panel wave source 2 and the upper edge of the left panel 3 is Angle θ is 0°.

The installation position of the base plate wave source 4 on the base plate 5 is shown in Figure 2: the first base plate wave source 4 is located 3a/2 from the starting edge of the base plate 5, and the second base plate wave source 4 is located 2a+ from the starting edge of the base plate 5 At 3a/2, the third base plate wave source 4 is located at 4a+3a/2 from the starting edge of the base plate 5. The distance between the center O3 of the mounting surface of each bottom plate wave source 4 and the upper edge of the bottom plate 5 is a/4, and the long side of the mounting surface of each bottom plate wave source 4 is parallel to the upper edge of the bottom plate 5 .

The installation position of the right plate wave source 6 on the right plate 7 is shown in Figure 2: the first right plate wave source 6 is located 3a/2 from the starting edge of the right plate 7, and the second right plate wave source 6 It is located at 2a+3a/2 from the starting edge of the right plate 7, and the third right plate wave source 6 is located at 4a4+3a/2 from the starting edge of the right plate 7. The distance between the center O4 of the mounting surface of each right panel wave source 6 and the upper edge of the right panel 7 is a/4, and the distance between the long side of the mounting surface of each right panel wave source 6 and the upper edge of the right panel 7 is Angle β is 90°.

The long side of the rectangle is l=a/3.

Compared with the existing technology, this specific implementation method has the following positive effects:

1. This specific implementation method is based on the simulation and experimental verification of the electromagnetic-thermal-stress composite physical field in the cavity of the microwave processing device, and adopts a "continuous microwave processing device that enhances the grinding and leaching efficiency of vanadium shale" (hereinafter Referred to as "continuous microwave processing device") for microwave processing. The layout of the cavity and wave sources of the continuous microwave processing device has been optimized, and corresponding n wave sources are regularly installed at different positions and different angles on the four flat outer walls of the cavity, realizing the above-mentioned The optimized distribution of the composite physical field in the cavity gives full play to the induction and strengthening effect of microwave on the heterogeneous dissociation of vanadium shale, which greatly improves the grindability of vanadium shale; in addition, the continuous processing method of multiple wave sources can realize the grinding of vanadium shale in the cavity During the operation in the body, it is subjected to continuous multi-dimensional irradiation, which improves the treatment effect and shortens the treatment cycle.

This specific implementation can achieve efficient pretreatment of vanadium shale within 1 to 2 minutes and below the combustion temperature of carbon, thereby increasing the grindability (in terms of crushing rate) of vanadium shale by more than 200%, and at the same time increasing the total grinding time. Energy consumption (including microwave pretreatment energy consumption and grinding energy consumption of microwave pretreatment products) is reduced by more than 40%, with short processing cycle, good processing effect and low energy consumption.

2. This specific embodiment is aimed at the interweaving characteristics of pyrite and carbonaceous absorbing materials of vanadium shale, intertwined with fine particles of non-absorbing silicate minerals such as mica and feldspar, and the processing of vanadium-containing minerals. The evolution law of dielectric properties in the process is based on the simulation of composite physical fields. Through the "continuous microwave processing device" microwave cavity and n-level (the first wave source of each plate is called the first level, each plate The second wave source is called the second stage,..., and so on, the nth wave source of each plate is called the nth stage) The special design of the wave source and continuous transmission device, during the preprocessing process, continuously excites multiple stages Microwaves have a mass-dynamic effect, causing the treated vanadium shale to be continuously and alternately subjected to n electromagnetic-thermal-stress composite physical fields in the cavity. The distribution form of this composite physical field greatly strengthens the vanadium-containing shale. The dehydroxylation reaction of mica Al-O(OH) octahedron improves the reactivity of shale vanadium during the acid leaching process, increasing the vanadium leaching rate by more than 15% under the same leaching conditions, which has a significant impact on the vanadium leaching rate. Strengthening effect.

3. This specific implementation adopts a "continuous microwave processing device" with a multi-level continuous distribution mechanism of n-level wave sources combined with the material conveyor belt (9). During the continuous microwave process of vanadium shale, the irradiation of all levels of wave sources is The power, irradiation time and transmission speed of the material conveyor belt (9) are adjusted to achieve optimal matching; on the one hand, the operating steps of microwave treatment of vanadium shale are simplified, and batch continuous batching of vanadium shale can be realized under simple operations. processing; on the other hand, since the processed vanadium shale continuously passes through n electromagnetic-thermal-stress composite physical fields, the continuous and alternating radiation energy can greatly reduce the radiation inconsistency in multiple physical fields in the microwave device cavity. Uniformity, high grindability and leaching efficiency of vanadium shale can be obtained within 1 to 2 minutes, and the production efficiency is high.

4. In this specific embodiment, during the on-line microwave treatment of vanadium shale, due to the short processing cycle, low overall temperature and no carbon emissions, a "continuous microwave" can be set up between the vanadium shale crushing process and the grinding process. "Processing device"; it can realize the organic combination between the grinding process, the microwave treatment process and the grinding process through a simple series combination, and is suitable for the full wet vanadium extraction system from vanadium shale.

Therefore, this specific embodiment has the characteristics of short processing time, low energy consumption, no carbon emissions, good effect on enhancing the grindability and leaching rate of vanadium shale, simple operation and high processing efficiency. This method is suitable for fully wet vanadium shale. Microwave strengthening method for vanadium system.

Claims (4)

1. A method of using microwaves to enhance vanadium shale grinding and leaching efficiency, characterized in that the specific steps of the method are: Step 1. Crush and screen the vanadium shale raw ore to obtain vanadium shale raw ore with a particle size of <1.5 mm and vanadium shale raw ore with a particle size of 1.5 to 10.0 mm; Step 2. Use the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" for microwave processing, set the transportation speed of the conveyor belt (9), and turn on the switches of all wave sources in the continuous microwave processing device , start the conveyor belt (9); The raw vanadium shale ore with a particle size of 1.5 to 10.0 mm is fed from the feed port of the continuous microwave treatment device, and the feeding amount is 60 to 150kg/h; from the discharge of the continuous microwave treatment device Microwave-treated vanadium shale is readily available; Step 3. According to the mass ratio of the microwave-treated vanadium shale:water being 1:1 to 3, the microwave-treated vanadium shale is quenched in water to obtain water quenching slurry; Then according to the mass ratio of vanadium shale raw ore with a particle size of <1.5mm: vanadium shale raw ore with a particle size of 1.5-10.0mm, the water quenching slurry and the vanadium with a particle size of <1.5mm are Shale raw ore is mixed and ground to obtain ground products; the ground products enter the subsequent leaching process; Step 4. After all material processing is completed, turn off the switches with all wave sources and close the material conveyor belt (9); The structure of the "continuous microwave processing device to enhance vanadium shale grinding and leaching efficiency" is: the continuous microwave processing device is a cavity surrounded by 4 rectangular plates, 4n wave sources and a material transmission belt ( 9) Composition; the length × width of the rectangular plate = 2na × a, each rectangular plate is evenly equipped with n wave sources, 4n wave sources are the same, n is a natural number from 2 to 10; installed horizontally in the cavity There is a material conveyor belt (9), the height of the upper surface of the conveyor belt (9) from the top of the cavity is 0.52~0.58a, and the width of the conveyor belt (9) is 0.9~0.95a; The four rectangular flat plates are the top plate (1), the left plate (3), the bottom plate (5) and the right plate (7); the top plate (1), the left plate (3), the bottom plate (5) and the right plate (7) The top plate wave source (8), the left plate wave source (2), the bottom plate wave source (4) and the right plate wave source (6) are installed in sequence; each wave source consists of a magnetron and a waveguide Composed, the mounting surface of each wave source on a rectangular flat plate is rectangular; The installation position of each wave source on its corresponding rectangular plate: For the sake of simplicity of description, it is assumed that the cavity is separated from the intersection of the top plate (1) and the right plate (7), so that the cavity is expanded into a plane; and let: the inlet end of the material is each rectangle The starting edge of the flat plate and the dividing line of the top plate (1) are the upper edge lines of the cavity development surface, that is, the first horizontal line of the cavity development surface is the upper edge line of the top plate (1), and the second horizontal line of the cavity development surface is is the upper edge line of the left side panel (3), the third horizontal line on the cavity expansion surface is the upper edge line of the bottom plate (5), and the fourth horizontal line on the cavity expansion surface is the upper edge line of the right side panel (7); The installation position of the roof wave source (8) on the roof (1): the first roof wave source (8) is located a/2 away from the starting edge of the roof (1), and the second roof wave source (8) is located 1 distance away from the top plate (1) ) at 2a(2-1)+a/2 from the starting side, the third top plate wave source (8) is located at 2a(3-1)+a/2 from the starting side of the top plate (1),..., By analogy, the nth roof wave source (8) is located at 2a(n-1)+a/2 from the starting edge of the roof (1); the center O1 of the installation surface of each roof wave source (8) is in contact with the roof ( The distance between the upper edge of 1) is a/4, and the long side of the installation surface of each roof wave source (8) is perpendicular to the upper edge of the roof (1); The installation position of the left panel wave source (2) on the left panel (3): the first left panel wave source (2) is located a/2 from the starting edge of the left panel (3), the second left panel The plate wave source (2) is located at 2a(2-1)+a/2 from the starting edge of the left plate (3), and the third left plate wave source (2) is located from the starting edge of the left plate (3) 2a(3-1)+a/2 of /2; the distance between the center O2 of the mounting surface of each left panel wave source (2) and the upper edge of the left panel (3) is a/4, and the long side of the mounting surface of each left panel wave source (2) The angle θ with the upper edge of the left panel (3) is 0° to 45°; The installation position of the bottom plate wave source (4) on the bottom plate (5): the first bottom plate wave source (4) is located 3a/2 from the starting edge of the bottom plate (5), and the second bottom plate wave source (4) is located 5 ) at 2a(2-1)+3a/2 from the starting side, the third bottom plate wave source (4) is located at 2a(3-1)+3a/2 from the starting side of the bottom plate (5),..., By analogy, the nth base plate wave source (4) is located at 2a(n-1)+3a/2 from the starting edge of the base plate (5); the center O3 of the installation surface of each base plate wave source (4) is in contact with the base plate ( The distance between the upper edge of 5) is a/4, and the long side of the installation surface of each bottom plate wave source (4) is parallel to the upper edge of the bottom plate (5); The installation position of the right plate wave source (6) on the right plate (7): the first right plate wave source (6) is located 3a/2 from the starting edge of the right plate (7), the second right The plate wave source (6) is located at 2a(2-1)+3a/2 from the starting edge of the right plate (7), and the third right plate wave source (6) is located from the starting edge of the right plate (7) 2a(3-1)+3a/2,..., and so on, the nth right plate wave source (6) is located at 2a(n-1)+3a from the starting edge of the right plate (7) /2; the distance between the center O4 of the mounting surface of each right plate wave source (6) and the upper edge of the right plate (7) is a/4, and the long side of the mounting surface of each right plate wave source (6) The angle with the upper edge of the right panel (7) is 90°-θ. 2. The method of using microwave to enhance the grinding and leaching efficiency of vanadium shale according to claim 1, characterized in that the chemical composition of the vanadium shale is: C content is 4-25wt%; V ₂ O ₅ content ≥ 0.45wt%. 3. The method of using microwave to enhance vanadium shale grinding and leaching efficiency according to claim 1, characterized in that the microwave power of the wave source is 500-1500W. 4. The method of using microwaves to enhance vanadium shale grinding and leaching efficiency according to claim 1, characterized in that the long side l of the rectangle is a/6 to a/3.