Leaching method of vanadium pentoxide

Abstract

The invention discloses a leaching method of vanadium pentoxide, relates to the technical field of vanadium pentoxide production, and can solve the problem of low concentration of leachate. According to the specific scheme, the method is applied to gradient leaching equipment of vanadium pentoxide, the equipment comprises a plurality of leaching pools, the multiple leaching pools are connected in a closed loop mode, and the method comprises the steps that clinker is added into the current leaching pool, and the clinker is roasted granular vanadium ore; a leaching agent is added into the current leaching pool for leaching treatment, and then leaching liquid and residues are obtained; if the PH value of the leaching solution is smaller than a preset threshold value, the leaching solution is conveyed into the next leaching pool to be used for leaching of the next batch of clinker in the next leaching pool, and the leaching agent is the leaching solution conveyed from the previous leaching pool; and if the PH value of the leaching liquid is equal to or larger than the preset threshold value, a leaching pregnant solution is obtained, and the leaching pregnant solution is conveyed out of the gradient leaching equipment to be used for producing vanadium pentoxide.

Description

Technical Field

[0001] The present application relates to the technical field of vanadium pentoxide production, and in particular to a vanadium pentoxide leaching method. Background Art

[0002] Stone coal vanadium ore is a unique vanadium-containing resource with a wide distribution and rich reserves. It is an important raw material for producing vanadium pentoxide in addition to steel slag vanadium extraction raw materials. At present, the main processes for producing vanadium pentoxide are "ore pre-processing-roasting-leaching-enrichment-impurity removal-vanadium precipitation" and "ore pre-processing-sulfuric acid solution leaching-enrichment-impurity removal-vanadium precipitation". Leaching is an indispensable and important link in the production of vanadium pentoxide, and it is an important link that directly affects the recovery rate and cost of vanadium pentoxide production. At present, the leaching methods of vanadium pentoxide all have the problems of complex processes and low concentration of leaching solution. Summary of the invention

[0003] The present application provides a vanadium pentoxide leaching method, which can improve the problem of low concentration of leaching solution.

[0004] In order to achieve the above objectives, this application adopts the following technical solutions:

[0005] The embodiment of the present application provides a leaching method of vanadium pentoxide, which is applied to a gradient leaching device of vanadium pentoxide, wherein the device comprises a plurality of leaching tanks, and the plurality of leaching tanks are connected in a closed loop, and the method comprises:

[0006] Adding clinker, which is roasted, granulated vanadium ore, to an existing leaching tank;

[0007] Adding a leaching agent into the current leaching tank for leaching treatment to obtain a leaching solution and a residue;

[0008] If the pH of the leachate is less than a preset threshold, the leachate is transported to the next leaching tank for leaching the next batch of clinker in the next leaching tank, and the leachant is the leachate transported from the previous leaching tank;

[0009] If the pH of the leaching solution is equal to or greater than the preset threshold, a leaching precious solution is obtained, and the leaching precious solution is transported out of the gradient leaching equipment to be used for producing vanadium pentoxide.

[0010] As a possible implementation manner, the method further includes:

[0011] If the current leaching tank has been subjected to a preset number of leaching treatments, the residue in the current leaching tank is discharged from the current leaching tank, and a new batch of clinker is added to the current leaching tank.

[0012] As a possible implementation, the step of adding a leaching agent to the current leaching tank for leaching treatment includes:

[0013] The leaching agent is added into the current leaching tank and then allowed to stand and circulate.

[0014] As a possible implementation, the step of adding the leaching agent to the current leaching tank and then placing the leaching agent therein for standing and circulating the leaching agent therein comprises:

[0015] After adding the leaching agent into the current leaching tank, the leaching agent is allowed to stand for a first time, stirred for a second time, and then allowed to stand for the first time.

[0016] As a possible implementation manner, the leaching agent is a dilute sulfuric acid solution, and the preset threshold is 2.

[0017] As a possible implementation manner, the liquid-to-solid ratio of the leaching agent to the clinker is 1:(1-1.15), and the particle size of the vanadium ore is 20-50 mm.

[0018] As a possible implementation manner, the first time is 2.5 to 3.5 hours, and the second time is 5.5 to 6.5 hours.

[0019] As a possible implementation manner, the multiple leaching tanks are connected by pipelines, and a delivery pump is installed on the pipeline.

[0020] As a possible implementation manner, the step of transporting the leaching solution to the next leaching tank includes:

[0021] The delivery pump is used to deliver the leaching solution to the next leaching solution.

[0022] As a possible implementation, the pipeline is made of organic material, and the delivery pump is a fluorine-lined pump.

[0023] The beneficial effects brought by the technical solution provided by the embodiment of the present application include at least:

[0024] The embodiment of the present application provides a gradient leaching method for vanadium pentoxide. The method is applied to a gradient leaching device for vanadium pentoxide. The device includes multiple leaching tanks, which are connected in a closed loop. During the leaching process, clinker is added to a current leaching tank, and the clinker is granular vanadium ore after roasting. A leaching agent is added to the current leaching tank for leaching treatment to obtain a leachate and a residue. If the pH of the leachate is less than a preset threshold, the leachate is transported to the next leaching tank for leaching of the next batch of clinker in the next leaching tank, and the leaching agent is the leachate transported from the previous leaching tank. If the pH of the leachate is equal to or greater than the preset threshold, a leached precious liquid is obtained, and the leached precious liquid is transported out of the gradient leaching device for the production of vanadium pentoxide. The gradient leaching method of vanadium pentoxide provided in the embodiment of the present application can utilize the inherent characteristics of the material to naturally form a layer filter in the leaching tank, eliminating the forced solid-liquid separation step in the stirring leaching, and reducing the operating cost and investment of the filtration equipment. In addition, the leaching form in which the solid phase material is stationary and the liquid phase is in relative motion reduces the wear and scouring of the equipment by solid particles. The flowing liquid is a sulfuric acid solution without solid particles. The equipment pipeline material is selected from organic pipelines and fluorine-lined pumps, which can effectively solve the corrosion and wear of the equipment. Furthermore, by adopting countercurrent step leaching, a concentration gradient is formed between different pools, overcoming the problem of low concentration of the leachate in stirring leaching. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 A schematic diagram of a gradient leaching device for vanadium pentoxide provided in an embodiment of the present application;

[0026] Figure 2 A flow chart of a gradient leaching method of vanadium pentoxide provided in an embodiment of the present application. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0028] In the following, the terms "first" and "second" are used for descriptive purposes only and are not to be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the embodiments of the present disclosure, unless otherwise specified, "plurality" means two or more.

[0029] Additionally, the use of “based on” or “according to” is meant to be open and inclusive, as a process, step, calculation, or other action “based on” or “according to” one or more conditions or values ​​may, in practice, be based on additional conditions or beyond values.

[0030] Stone coal vanadium ore is a unique vanadium-containing resource with a wide distribution and rich reserves. It is an important raw material for producing vanadium pentoxide in addition to steel slag vanadium extraction raw materials. At present, the main processes for producing vanadium pentoxide are "ore pre-processing-roasting-leaching-enrichment-impurity removal-vanadium precipitation" and "ore pre-processing-sulfuric acid solution leaching-enrichment-impurity removal-vanadium precipitation". Leaching is an indispensable and important link in the production of vanadium pentoxide, and it is an important link that directly affects the recovery rate and cost of vanadium pentoxide production. At present, the main ways to produce vanadium pentoxide leaching are stirred leaching in which the ore powder is processed to a certain fineness and then the leaching medium is added for strong mechanical stirring, and static immersion in the pool (irrigation).

[0031] Among them, stirring leaching is to grind the ore to a certain fineness, add a certain concentration and amount of sulfuric acid solution in the stirring barrel, add mineral powder, use mechanical strong stirring, and use solid-liquid separation equipment to separate the slurry into solid and liquid after the leaching time reaches. At present, the stirring leaching used in the stone coal vanadium extraction industry generally grinds the ore to -200 mesh greater than 90%, and then adds sulfuric acid solution according to the liquid-solid ratio. The concentration of sulfuric acid solution is 5-25%. Use mechanical strong stirring, and the slurry after leaching is separated and washed by a thickener, or by filtering equipment for solid-liquid separation and washing. The stirring tank, stirring shaft, and stirring impeller are made of corrosion-resistant 316L or other corrosion-resistant materials. The service life of the stirring shaft and impeller is generally less than one year.

[0032] Static leaching in a tank (tank) is to put the granular material in a tank (tank), then add 5-25% sulfuric acid solution, and then start soaking. During the soaking process, the liquid penetrates into the solid particles through the pores in the particles, and the valuable elements in the solid are leached into the liquid by diffusion, thereby achieving the purpose of leaching. At present, the leaching tank (tank) of domestic vanadium extraction enterprises is generally 200-500t. Since the solid phase and liquid phase are both in a relatively static state in this leaching method, the leaching cycle is generally 7-10 days.

[0033] Agitation leaching is a leaching method currently used to produce vanadium pentoxide. Its advantages are high leaching efficiency and short leaching time, but its disadvantages are that it is leached in a sulfuric acid solution, which places high demands on equipment corrosion protection. The ore powder also causes great wear on the equipment. Under the dual unfavorable conditions of wear and corrosion, it is difficult for the equipment material to achieve long-term use. Due to the influence of the slurry concentration, the concentration of vanadium pentoxide in the leachate is relatively low. After leaching, the slurry is difficult to filter and wash. The tailings are difficult to stack and are not environmentally friendly.

[0034] Static leaching in a pool is to place granular materials in a leaching pool, add a prepared leaching medium (sulfuric acid solution), and use the permeability of the liquid to leach the valuable ions in the solid phase into the liquid phase through the diffusion principle. Compared with stirring leaching, its advantages are simplicity and reliability, reducing the stirring power of stirring leaching, and eliminating the filtration link. At present, domestic companies that use pool leaching generally use single pool leaching, and the disadvantages are low leachate concentration; pH value requires subsequent neutralization treatment, which increases the processing cost; high labor intensity; and difficult discharge.

[0035] In view of the above problems, the present application provides a gradient leaching device for vanadium pentoxide, such as Figure 1 As shown, the gradient leaching equipment includes a plurality of leaching tanks, which are connected in a closed loop. The plurality of leaching tanks are connected by pipelines, and a delivery pump is installed on the pipeline. The pipeline is made of organic materials, and the delivery pump is a fluorine-lined pump.

[0036] Based on the above-mentioned gradient leaching equipment of vanadium pentoxide, the embodiment of the present application provides a gradient leaching method of vanadium pentoxide, such as Figure 2 As shown, the method includes:

[0037] Step 201: Add clinker into a current leaching tank, wherein the clinker is granular vanadium ore after roasting.

[0038] The particle size of the vanadium ore is 20 to 50 mm. The current leaching tank can be any one of a plurality of leaching tanks.

[0039] Step 202: adding a leaching agent to the current leaching tank for leaching treatment to obtain a leaching solution and a residue.

[0040] Wherein, the leaching agent is a dilute sulfuric acid solution, and the liquid-to-solid ratio of the leaching agent to the clinker is 1:(1-1.15).

[0041] The above process of adding a leaching agent to the current leaching tank for leaching treatment may be:

[0042] After adding the leaching agent into the current leaching tank and letting it stand for a first time, the leaching agent is circulated for a second time, and then let it stand for the first time.

[0043] Among them, the first time is 2.5 to 3.5 hours, and the second time is 5.5 to 6.5 hours.

[0044] Step 203: If the pH of the leachate is less than a preset threshold, the leachate is transported to the next leaching tank for use in leaching the next batch of clinker in the next leaching tank, and the leaching agent is the leachate transported from the previous leaching tank.

[0045] The preset threshold value may be 2. The process of conveying the leaching solution to the next leaching tank may be as follows: conveying the leaching solution to the next leaching tank by using a conveying pump.

[0046] Step 204: If the pH of the leaching solution is equal to or greater than the preset threshold, a leaching precious solution is obtained, and the leaching precious solution is transported out of the gradient leaching equipment to be used for producing vanadium pentoxide.

[0047] Optionally, the method further includes: if the current leaching tank has been subjected to a preset number of leaching treatments, the residue in the current leaching tank is discharged from the current leaching tank, and a new batch of clinker is added to the current leaching tank. The preset number of times may be 4 times, and of course the preset number of times may be set according to the application scenario, which is not specifically limited in the present embodiment of the application.

[0048] In the actual implementation process, this application takes a total of 8 leaching pools as an example for explanation, and of course this application does not limit the number of leaching pools. Among them, the precious liquid mentioned below is the leaching precious liquid, the first pool mentioned below is the first leaching pool, and the second pool is the second leaching pool. Of course, this application does not limit the order of the leaching pools, and any leaching pool can be the first leaching pool.

[0049] After the first pool of clinker is loaded, the first pool starts to enter the first 7% dilute sulfuric acid solution for leaching operation. The leaching adopts the operation mode of liquid self-circulation and static leaching. After the liquid is filled, it is soaked for 3 hours, and the liquid starts to circulate itself. After 6 hours of circulation, it is soaked for another 3 hours. If the pH of the first leaching pool is less than 2, the leachate of the first leaching pool is transported to the next leaching pool for leaching the next batch of clinker in the next leaching pool. If the pH of the leachate of the first leaching pool is equal to or greater than 2, a leached precious liquid is obtained, and the leached precious liquid is transported out of the gradient leaching equipment for the production of vanadium pentoxide.

[0050] After the loading of clinker in the second tank is completed, the leachate from the first tank is pumped to the second tank for leaching operation; after the leachate from the first tank is transferred to the second tank, the first tank starts to introduce secondary leachate; when the concentration of the leachate from the second tank reaches above 5g / l through leaching and self-circulation, and the PH is about 2, the second tank starts to discharge precious liquid through the bottom liquid pump, and the discharged precious liquid is pumped to the next process; after the discharge of precious liquid is completed, the secondary leachate from the first tank is pumped to the second tank as the primary leachate of the second tank, and after the washing water volume reaches the requirement, the second tank starts static leaching and internal circulation to start washing operation; the first tank starts to introduce tertiary leachate and carry out leaching and internal circulation operations.

[0051] After the loading of clinker in the third tank is completed, the primary leaching agent in the second tank is pumped to the third tank for leaching operation; after the washing water in the second tank is switched to the third tank, the secondary leaching agent starts to enter the second tank; when the concentration of the liquid in the third tank reaches more than 5g / l after leaching and self-circulation, and the ph is about 2, the third tank starts to discharge precious liquid through the bottom water pump, and the leached precious liquid is transported to the next process; after the discharge of precious liquid is completed, the secondary washing water in the second tank is pumped to the third tank as the primary washing water of the third tank. After the washing water volume reaches the requirement, the third tank starts static leaching and the circulation in the tank starts the washing operation.

[0052] The first pool starts to enter four washing waters, and the second pool starts to enter three washing waters, and performs leaching and pool circulation operations. The leaching operations of the fourth, fifth, sixth, seventh, and eighth pools are carried out step by step according to the above steps. The leaching agent used in the leaching pool for newly loaded clinker is the leaching solution of the previous pool, and the leaching solution of the previous pool is used as the leaching agent of the next pool, and leaching and washing operations are carried out in sequence. When the concentration gradient of vanadium pentoxide in the leaching solution of the first pool does not change much (0.25g / l), the leaching and washing operations are completed, and the first pool starts to discharge tailings. The leaching solution of the eighth pool is used as the leaching agent of the first pool, and the eight leaching pools 1-8 are circulated in sequence for leaching and washing operations. The leached tailings produced are sent to the slag plant for temporary storage and treatment via a multi-bucket reclaimer and a belt conveyor. The control valves of the liquids between each leaching pool use electric control valves. The control logic is compiled according to the characteristics of the leaching operation and the process requirements. The start and stop of the pump and the switch of the valve are opened according to the logic.

[0053] The embodiment of the present application provides a gradient leaching method for vanadium pentoxide. The method is applied to a gradient leaching device for vanadium pentoxide. The device includes multiple leaching tanks, which are connected in a closed loop. During the leaching process, clinker is added to a current leaching tank, and the clinker is granular vanadium ore after roasting. A leaching agent is added to the current leaching tank for leaching treatment to obtain a leachate and a residue. If the pH of the leachate is less than a preset threshold, the leachate is transported to the next leaching tank for leaching of the next batch of clinker in the next leaching tank, and the leaching agent is the leachate transported from the previous leaching tank. If the pH of the leachate is equal to or greater than the preset threshold, a leached precious liquid is obtained, and the leached precious liquid is transported out of the gradient leaching device for the production of vanadium pentoxide. The gradient leaching method of vanadium pentoxide provided in the embodiment of the present application can utilize the inherent characteristics of the material to naturally form a layer filter in the leaching tank, eliminating the forced solid-liquid separation step in the stirring leaching, and reducing the operating cost and investment of the filtration equipment. In addition, the leaching form in which the solid phase material is stationary and the liquid phase is in relative motion reduces the wear and scouring of the equipment by solid particles. The flowing liquid is a sulfuric acid solution without solid particles. The equipment pipeline material is selected from organic pipelines and fluorine-lined pumps, which can effectively solve the corrosion and wear of the equipment. Furthermore, by adopting countercurrent step leaching, a concentration gradient is formed between different pools, overcoming the problem of low concentration of the leachate in stirring leaching.

[0054] In addition, the solid material and liquid flow directions of the present invention are reversed, and the characteristic of alkaline substances in the solid material consuming sulfuric acid is utilized to make the pH values ​​between different pools form a gradient from low to high, and the excess H + By consuming the solid clinker in the pool, the pH value of the leachate required by the subsequent process is achieved, eliminating the process of adjusting the pH, saving the consumption cost of the neutralizer, and reducing the loss of vanadium pentoxide during neutralization. Through multiple leaching and multiple washing, the leaching rate of vanadium pentoxide is effectively improved and the consumption of leaching agent is reduced. The introduction of an automatic control system realizes fully automatic operation and improves operating efficiency. Fully closed-loop circulation achieves zero wastewater discharge. The solid material is granular and relatively environmentally friendly.

[0055] In another embodiment of the present application, a computer-readable storage medium is provided, on which a computer program is stored. When the computer program is executed by a processor, the steps of the gradient leaching method of vanadium pentoxide in the embodiment of the present application are implemented.

[0056] In another embodiment of the present application, a computer program product is provided. The computer program product includes computer instructions. When the computer instructions execute the various steps of the gradient leaching method of vanadium pentoxide in the method flow shown in the above method embodiment.

[0057] In the above embodiments, it can be implemented in whole or in part by software, hardware, firmware or any combination thereof. When implemented using a software program, it can be implemented in whole or in part in the form of a computer program product. The computer program product includes one or more computer instructions. When loading and executing computer execution instructions on a computer, the process or function according to the embodiment of the present application is generated in whole or in part. The computer can be a general-purpose computer, a special-purpose computer, a computer network, or other programmable devices. Computer instructions can be stored in a computer-readable storage medium, or transmitted from one computer-readable storage medium to another computer-readable storage medium. For example, computer instructions can be transmitted from a website site, computer, server or data center by wired (e.g., coaxial cable, optical fiber, digital subscriber line (digital subscriber line, DSL)) or wireless (e.g., infrared, wireless, microwave, etc.) mode to another website site, computer, server or data center. The computer-readable storage medium can be any available medium that a computer can access or a data storage device such as a server, data center, etc. that contains one or more servers that can be integrated with a medium. The available medium may be a magnetic medium (eg, a floppy disk, a hard disk, a magnetic tape), an optical medium (eg, a DVD), or a semiconductor medium (eg, a solid state disk (SSD)).

[0058] The technical features of the above embodiments may be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0059] The above embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent of the present application shall be subject to the attached claims.

Claims

1. A gradient leaching method for vanadium pentoxide, characterized in that: The method is applied to a gradient leaching device for vanadium pentoxide, the device comprising a plurality of leaching tanks, the plurality of leaching tanks being connected in a closed loop, and the method comprising: Adding clinker, which is roasted, granulated vanadium ore, to an existing leaching tank; Adding a leaching agent into the current leaching tank for leaching treatment to obtain a leaching solution and a residue; If the pH of the leachate is less than a preset threshold, the leachate is transported to the next leaching tank for leaching the next batch of clinker in the next leaching tank, and the leachant is the leachate transported from the previous leaching tank; If the pH of the leaching solution is equal to or greater than the preset threshold, a leaching precious solution is obtained, and the leaching precious solution is transported out of the gradient leaching equipment to be used for producing vanadium pentoxide.

2. The method according to claim 1, characterized in that The method further comprises: If the current leaching tank has been subjected to a preset number of leaching treatments, the residue in the current leaching tank is discharged from the current leaching tank, and a new batch of clinker is added to the current leaching tank.

3. The method according to claim 1, characterized in that The step of adding a leaching agent to the current leaching tank for leaching treatment comprises: The leaching agent is added into the current leaching tank and then allowed to stand and circulate.

4. The method according to claim 3, characterized in that The step of adding the leaching agent to the current leaching tank and then placing the leaching agent in a static state and circulating the leaching agent in a circulating state comprises: After adding the leaching agent into the current leaching tank and letting it stand for a first time, the leaching agent is circulated for a second time, and then let it stand for the first time.

5. The method according to claim 1, characterized in that The leaching agent is a dilute sulfuric acid solution, and the preset threshold is 2.

6. The method according to claim 5, characterized in that The liquid-to-solid ratio of the leaching agent to the clinker is 1:(1-1.15), and the particle size of the vanadium ore is 20-50 mm.

7. The method according to claim 4, characterized in that The first time is 2.5 to 3.5 hours, and the second time is 5.5 to 6.5 hours.

8. The method according to claim 1, characterized in that The multiple leaching tanks are connected by pipelines, and a delivery pump is installed on the pipeline.

9. The method according to claim 6, characterized in that The step of transporting the leaching solution to the next leaching tank comprises: The delivery pump is used to deliver the leaching solution to the next leaching solution.

10. The method according to claim 8, characterized in that The pipeline is made of organic materials, and the delivery pump is a fluorine-lined pump.

Images