Preparation method of vanadium pentoxide and vanadium pentoxide product
By adjusting the concentration and pH of the vanadium pentoxide enrichment solution, and combining heating, stirring, filtration, and calcination, the problems of long process routes, high vanadium loss, and high energy consumption in existing processes have been solved, achieving efficient and low-cost vanadium pentoxide preparation.
Patent Information
- Application Number
- CN202411489226.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-24
- Publication Date
- 2025-01-07
AI Technical Summary
The existing process for preparing high-purity vanadium pentoxide is relatively long, involves many vanadium loss stages, has high energy and reagent consumption, generates a large amount of ammonia nitrogen wastewater, and has high costs.
After adjusting the concentration and pH of the vanadium pentoxide enrichment solution, two impurity removal processes were performed, including heating and stirring and filtration. Subsequently, vanadium precipitation and calcination to remove ammonia were carried out to obtain high-purity vanadium pentoxide.
The process route was shortened, vanadium loss was reduced, energy and reagent consumption were lowered, ammonia nitrogen wastewater generation was reduced, and preparation efficiency and recovery rate were improved.
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Figure CN119263346A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of vanadium pentoxide production, and in particular to a preparation method of vanadium pentoxide and a vanadium pentoxide product. Background Art
[0002] Vanadium has many excellent physical and chemical properties and is widely used in metallurgy, electronics, chemical industry and other industries. About 85% of it is used for smelting ferrovanadium as an alloy additive, mainly in the form of vanadium pentoxide.
[0003] At present, the process route for preparing high-purity vanadium pentoxide is generally "enriched liquid adjustment---heating---impurity removal---vanadium precipitation---washing---ammonium metavanadate heating and alkaline dissolution---PH adjustment---secondary impurity removal---filtration---secondary vanadium precipitation---washing---calcination". The current preparation method has a long process route and many vanadium loss links. Summary of the invention
[0004] The present application provides a method for preparing vanadium pentoxide and a vanadium pentoxide product, which can improve the preparation efficiency of vanadium pentoxide and the recovery rate of vanadium pentoxide.
[0005] In order to achieve the above purpose, this application adopts the following technical solutions:
[0006] In a first aspect of the embodiments of the present application, a method for preparing vanadium pentoxide is provided, the method comprising:
[0007] obtaining a vanadium pentoxide enriched solution;
[0008] After pre-treating the enriched solution, a first enriched solution is obtained, wherein the pre-treatment includes concentration adjustment and pH value adjustment;
[0009] After sequentially performing a first impurity removal treatment and a second impurity removal treatment on the first enriched liquid, a target enriched liquid is obtained;
[0010] The target vanadium pentoxide is obtained by extraction from the target enriched solution.
[0011] As a possible implementation manner, the pretreatment is concentration adjustment, and the pretreatment of the enriched solution includes:
[0012] The concentration of vanadium pentoxide in the enriched solution is treated to be 35-45 g / L.
[0013] As a possible implementation, the pretreatment is pH adjustment, and the pretreatment of the enriched liquid includes:
[0014] The pH value of the enriched solution is adjusted to 8.7-9.3.
[0015] As a possible implementation manner, performing a first impurity removal treatment on the first enriched liquid includes:
[0016] The first enriched solution is heated to 60-70° C., a first impurity remover is added, and the mixture is stirred at 62-67° C. for 1.5-2.5 hours and then the heating is stopped to obtain a first solution;
[0017] The first solution is filtered through a membrane plate and frame filter to obtain a first impurity-removed liquid.
[0018] As a possible implementation manner, the first impurity remover is a polymer containing polyacrylamide, and the added amount of the first impurity remover is 0.5 times the weight of vanadium pentoxide in the enriched solution.
[0019] As a possible implementation manner, performing a second impurity removal treatment on the first impurity removal liquid includes:
[0020] The second impurity remover is added to the first impurity remover at room temperature, and stirred for 0.5 to 1.5 hours, and allowed to stand for 3.5 to 4.5 hours to obtain the target enriched liquid; wherein the second impurity remover is a mixture of polyaluminium chloride, polyferric chloride and a non-ionic flocculant.
[0021] As a possible implementation method, the step of extracting the target vanadium pentoxide from the target enriched solution comprises:
[0022] The target enriched liquid is sequentially subjected to vanadium precipitation treatment, calcination treatment and deammoniation treatment to obtain the target vanadium pentoxide.
[0023] As a possible implementation method, the target enriched solution is subjected to vanadium precipitation treatment and calcination and deamination treatment in sequence to obtain the target vanadium pentoxide, comprising:
[0024] Adding a vanadium precipitant to the target enriched solution, stirring for 1 to 2 hours, and then filtering to obtain a filter cake, wherein the filter cake is ammonium metavanadate;
[0025] The filter cake is subjected to calcination and deammoniation treatment to obtain the target vanadium pentoxide.
[0026] As a possible implementation, the vanadium precipitating agent is ammonium chloride or ammonium sulfate, and the added amount of the vanadium precipitating agent is 2 to 2.5 times the weight of vanadium pentoxide in the enriched solution.
[0027] In a second aspect of the embodiments of the present application, a vanadium pentoxide product is provided. The vanadium pentoxide product is prepared by the method for preparing vanadium pentoxide in the first aspect of the embodiments of the present application.
[0028] The beneficial effects brought by the technical solution provided by the embodiment of the present application include at least:
[0029] The method for preparing vanadium pentoxide provided in the embodiment of the present application is as follows: obtaining a vanadium pentoxide enriched solution; pre-treating the enriched solution to obtain a first enriched solution, wherein the pre-treatment includes concentration adjustment and pH value adjustment; performing a first impurity removal treatment and a second impurity removal treatment on the first enriched solution in sequence to obtain a target enriched solution; and extracting the target vanadium pentoxide from the target enriched solution. Compared with the existing process for producing high-purity vanadium pentoxide, the method for preparing vanadium pentoxide provided in the present application has a shorter process line, a reduced vanadium loss link, and at the same time reduces the entire process of secondary dissolution, reduces energy consumption and reagent consumption, and also reduces the amount of ammonia nitrogen wastewater generated compared with the traditional process. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 This is a flow chart of a method for preparing vanadium pentoxide provided in an embodiment of the present application. DETAILED DESCRIPTION
[0031] 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.
[0032] 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.
[0033] 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.
[0034] Vanadium has many excellent physical and chemical properties and is widely used in metallurgy, electronics, chemical industry and other industries. About 85% of it is used for smelting ferrovanadium as an alloy additive, mainly in the form of vanadium pentoxide.
[0035] At present, in the stone coal vanadium extraction industry, there is no process for using vanadium enriched liquid (resin analytical liquid, stripping enriched liquid) to achieve a production line with a production quality level of 99.0% or more of high-purity vanadium pentoxide at one time. The existing technical route is to use an impurity remover (generally magnesium chloride, aluminum chloride, and polymerized magnesium salt or aluminum salt) to remove some impurities in the enriched liquid under certain temperature and pH conditions, and then add ammonium chloride or ammonium sulfate to precipitate ammonium metavanadate or ammonium polyvanadate. The quality level of the precipitated ammonium metavanadate or ammonium polyvanadate is generally below 98.5%. To produce high-purity vanadium pentoxide, it is also necessary to heat and dissolve the precipitated ammonium metavanadate (or ammonium polyvanadate) in an alkaline solution for a second time, then add an impurity remover to remove impurities and filter, and then add ammonium chloride or sulfuric acid to the filtrate to precipitate vanadium for a second time, and then wash the precipitated ammonium metavanadate with deionized water, filter, and calcine to obtain high-purity vanadium pentoxide.
[0036] At present, the process route for preparing high-purity vanadium pentoxide is generally "enriched liquid adjustment---heating---impurity removal-vanadium precipitation---washing---ammonium metavanadate heating and alkaline dissolution---PH value adjustment---secondary impurity removal---filtration---secondary vanadium precipitation---washing---calcination". The current preparation method process route is relatively long and there are many vanadium loss links. In addition, during the purification process, there are two heating, impurity removal, filtration, and vanadium precipitation, which consumes high power, vanadium precipitation agent, and impurity removal agent. During the purification process, ammonium metavanadate must undergo alkaline dissolution and pH adjustment, which consumes alkali and acid. The amount of ammonia nitrogen wastewater generated in the entire purification process is large, which increases the cost of wastewater treatment, and the operating cost and production cost of purification are high.
[0037] Based on the above problems, the present application provides a method for preparing vanadium pentoxide, such as Figure 1 As shown, the method comprises the following steps:
[0038] Step 101: Obtain a vanadium pentoxide enriched solution.
[0039] Step 102: Pre-treat the enriched solution to obtain a first enriched solution, wherein the pre-treatment includes concentration adjustment and pH value adjustment.
[0040] Optionally, the above process may be: firstly adjusting the concentration of vanadium pentoxide in the enriched solution to 35-45 g / L, and then adjusting the pH value of the enriched solution to 8.7-9.3.
[0041] Specifically, the concentration of vanadium pentoxide in the enriched solution can be adjusted by increasing the mass of the solute, reducing the volume of the solvent, evaporating the solvent, raising or lowering the temperature, ion exchange, and the like.
[0042] The pH value of the enrichment solution can be adjusted to 8.7-9.3 by diluting with water, adding alkaline substances, adding acidic substances, ventilation, using ion exchange resins, etc.
[0043] It is understandable that if the concentration in the enriched solution is too high, impurities are easily encapsulated during the vanadium precipitation process, which is not conducive to the purity of the product. Therefore, the concentration of vanadium pentoxide in the enriched solution needs to be adjusted to 35-45 g / L.
[0044] Step 103: performing a first impurity removal treatment and a second impurity removal treatment on the first enriched solution in sequence to obtain a target enriched solution.
[0045] Optionally, the process of performing the first impurity removal treatment on the first enriched liquid may be:
[0046] The first enriched liquid is heated to 60-70° C., a first impurity remover is added, and the first solution is obtained after stirring at 62-67° C. for 1.5-2.5 hours and then the heating is stopped; the first solution is filtered using a diaphragm plate and frame filter to obtain a first impurity-removed liquid.
[0047] Wherein, the first impurity remover is a polymer containing polyacrylamide, and the added amount of the first impurity remover is 0.5 times the weight of vanadium pentoxide in the enriched solution.
[0048] Optionally, performing a second impurity removal treatment on the first impurity removal liquid comprises:
[0049] A second impurity remover is added to the first impurity remover at room temperature, and stirred for 0.5 to 1.5 hours. After standing for 3.5 to 4.5 hours, the target enriched liquid is filtered using a diaphragm plate and frame filter; wherein the second impurity remover is a mixture of polyaluminium chloride, polyferric chloride and a non-ionic flocculant.
[0050] Step 104: extracting the target vanadium pentoxide from the target enriched solution.
[0051] Optionally, the target enriched liquid is sequentially subjected to vanadium precipitation treatment and calcination and deammoniation treatment to obtain the target vanadium pentoxide.
[0052] Specifically, a vanadium precipitant can be added to the target enriched solution, and the mixture is stirred for 1 to 2 hours and then filtered to obtain a filter cake, wherein the filter cake is ammonium metavanadate; and the filter cake is calcined and deaminated to obtain the target vanadium pentoxide.
[0053] Wherein, the vanadium precipitating agent is ammonium chloride or ammonium sulfate, and the added amount of the vanadium precipitating agent is 2 to 2.5 times the weight of vanadium pentoxide in the enriched solution.
[0054] Optionally, the deamination treatment can be performed by heating the ammonium metavanadate to 500-550° C. in an electrically heated rotary kiln.
[0055] The method for preparing vanadium pentoxide provided in the embodiment of the present application is as follows: obtaining a concentrated solution of vanadium pentoxide; pre-treating the concentrated solution to obtain a first concentrated solution, wherein the pre-treatment includes concentration adjustment and pH value adjustment; performing a first impurity removal treatment and a second impurity removal treatment on the first concentrated solution in sequence to obtain a target concentrated solution; extracting the target vanadium pentoxide from the target concentrated solution. The process route of the method for preparing vanadium pentoxide provided in the present application is "enriched solution concentration adjustment---pH value adjustment---heating---impurity removal---stirring reaction---solid-liquid separation---ammonium metavanadate washing---ammonium metavanadate calcination". Compared with the existing process for producing high-purity vanadium pentoxide, the process route is shorter, the vanadium loss link is reduced, and the entire process of secondary dissolution is reduced, which reduces energy consumption and reagent consumption. In addition, the amount of ammonia nitrogen wastewater generated is also reduced compared with the traditional process.
[0056] The present application also provides a vanadium pentoxide product, which is prepared by the above-mentioned vanadium pentoxide preparation method. The vanadium pentoxide preparation method comprises:
[0057] obtaining a vanadium pentoxide enriched solution;
[0058] After pre-treating the enriched solution, a first enriched solution is obtained, wherein the pre-treatment includes concentration adjustment and pH value adjustment;
[0059] After sequentially performing a first impurity removal treatment and a second impurity removal treatment on the first enriched liquid, a target enriched liquid is obtained;
[0060] The target vanadium pentoxide is obtained by extraction from the target enriched solution.
[0061] In one embodiment, the pretreatment is concentration adjustment, and the pretreatment of the enriched solution includes:
[0062] The concentration of vanadium pentoxide in the enriched solution is analyzed to be 35 to 45 g / L.
[0063] In one embodiment, the pretreatment is pH adjustment, and the pretreatment of the enriched solution comprises:
[0064] The pH value of the enriched solution is adjusted to 8.7-9.3.
[0065] In one embodiment, the first enriched liquid is subjected to a first impurity removal treatment, comprising:
[0066] The first enriched solution is heated to 60-70° C., a first impurity remover is added, and the mixture is stirred at 62-67° C. for 1.5-2.5 hours and then the heating is stopped to obtain a first solution;
[0067] The first solution is filtered through a membrane plate and frame filter to obtain a first impurity-removed liquid.
[0068] In one embodiment, the first impurity remover is a polymer comprising polyacrylamide, and the amount of the first impurity remover added is 0.5 times the weight of vanadium pentoxide in the enriched solution.
[0069] In one embodiment, the first impurity-removing liquid is subjected to a second impurity-removing treatment, comprising:
[0070] The second impurity remover is added to the first impurity remover at room temperature, and stirred for 0.5 to 1.5 hours, and allowed to stand for 3.5 to 4.5 hours to obtain the target enriched liquid; wherein the second impurity remover is a mixture of polyaluminium chloride, polyferric chloride and a non-ionic flocculant.
[0071] In one embodiment, the step of extracting target vanadium pentoxide from the target enriched solution comprises:
[0072] The target enriched liquid is sequentially subjected to vanadium precipitation treatment and calcination and deammoniation treatment to obtain the target vanadium pentoxide.
[0073] In one embodiment, the target enriched solution is sequentially subjected to vanadium precipitation treatment and calcination and deamination treatment to obtain the target vanadium pentoxide, comprising:
[0074] Adding a vanadium precipitant to the target enriched solution, stirring for 1 to 2 hours, and then filtering to obtain a filter cake, wherein the filter cake is ammonium metavanadate;
[0075] The filter cake is subjected to calcination and deammoniation treatment to obtain the target vanadium pentoxide.
[0076] In one embodiment, the vanadium precipitating agent is ammonium chloride or ammonium sulfate, and the amount of the vanadium precipitating agent added is 2 to 2.5 times the weight of vanadium pentoxide in the enriched solution.
[0077] The technical features of the above embodiments may be arbitrarily combined. 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.
[0078] 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 method for preparing vanadium pentoxide, characterized in that: The method comprises: obtaining a vanadium pentoxide enriched solution; After pre-treating the enriched solution, a first enriched solution is obtained, wherein the pre-treatment includes concentration adjustment and pH value adjustment; After sequentially performing a first impurity removal treatment and a second impurity removal treatment on the first enriched liquid, a target enriched liquid is obtained; The target vanadium pentoxide is obtained by extraction from the target enriched solution.
2. The method according to claim 1, characterized in that: The pretreatment is concentration adjustment, and the pretreatment of the enriched solution includes: The concentration of vanadium pentoxide in the enriched solution is adjusted to 35-45 g / L.
3. The method according to claim 1, characterized in that The pretreatment is pH adjustment, and the pretreatment of the enriched liquid includes: The pH value of the enriched solution is adjusted to 8.7-9.
3.
4. The method according to claim 1, characterized in that: The first enriched liquid is subjected to a first impurity removal treatment, comprising: The first enriched solution is heated to 60-70° C., a first impurity remover is added, and the mixture is stirred at 62-67° C. for 1.5-2.5 hours and then the heating is stopped to obtain a first solution; The first solution is filtered through a membrane plate and frame filter to obtain a first impurity-removed liquid.
5. The method according to claim 4, characterized in that The first impurity remover is a polymer containing polyacrylamide, and the added amount of the first impurity remover is 0.5 times the weight of vanadium pentoxide in the enriched solution.
6. The method according to claim 5, characterized in that The first impurity-removing liquid is subjected to a second impurity-removing treatment, comprising: The second impurity remover is added to the first impurity remover at room temperature, and stirred for 0.5 to 1.5 hours, and allowed to stand for 3.5 to 4.5 hours to obtain the target enriched liquid; wherein the second impurity remover is a mixture of polyaluminium chloride, polyferric chloride and a non-ionic flocculant.
7. The method according to any one of claims 1 to 6, characterized in that: The step of extracting target vanadium pentoxide from the target enriched solution comprises: The target enriched liquid is sequentially subjected to vanadium precipitation treatment and calcination and deammoniation treatment to obtain the target vanadium pentoxide.
8. The method according to claim 7, characterized in that The target enriched solution is sequentially subjected to vanadium precipitation treatment and calcination and deamination treatment to obtain the target vanadium pentoxide, comprising: Adding a vanadium precipitant to the target enriched solution, stirring for 1 to 2 hours, and then filtering to obtain a filter cake, wherein the filter cake is ammonium metavanadate; The filter cake is subjected to calcination and deammoniation treatment to obtain the target vanadium pentoxide.
9. The method according to claim 8, characterized in that The vanadium precipitating agent is ammonium chloride or ammonium sulfate, and the added amount of the vanadium precipitating agent is 2 to 2.5 times the weight of vanadium pentoxide in the enriched solution.
10. A vanadium pentoxide product, characterized in that: The vanadium pentoxide product is prepared by the vanadium pentoxide preparation method according to any one of claims 1 to 9.
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