Method for removing vanadium from petroleum coke for normal-pressure aluminum anode
By mixing petroleum coke with oxidant and acid solution for leaching reaction under normal pressure, the problems of high temperature and high pressure and impurities introduction in the vanadium extraction process in petroleum coke were successfully solved, and efficient and environmentally friendly vanadium removal effect was achieved.
Patent Information
- Application Number
- CN202411811659.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-10
- Publication Date
- 2025-03-07
AI Technical Summary
The vanadium extraction process in the prior art in petroleum coke has problems such as harsh high temperature and high pressure conditions, toxic gases, and the introduction of impurity metal elements, resulting in low devanalysis efficiency and environmental pollution.
Under normal pressure conditions, petroleum coke is mixed with an oxidant and an acid solution to carry out a leaching reaction, and the low-valent oxide of vanadium is oxidized into high-valent oxides, thereby achieving effective removal of vanadium in petroleum coke.
It has achieved efficient removal of vanadium from petroleum coke, with a simple process and low cost, no impurity metal elements introduced, and is environmentally friendly.
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Figure CN119571091A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of vanadium removal, and in particular to a method for removing vanadium from petroleum coke used as an anode for normal pressure aluminum. Background Art
[0002] Prebaked anodes are the most important consumables in aluminum electrolysis production. With the continuous development of aluminum electrolysis technology, the requirements for the quality of carbon anodes are getting higher and higher. Petroleum coke is one of the most important raw materials for the production of carbon anodes. In recent years, due to the deterioration of petroleum coke products and the increase in the content of impurity elements (such as vanadium, sulfur, iron, sodium, calcium, etc.), low-vanadium and low-sulfur petroleum coke that meets the requirements of carbon anode production is increasingly in short supply. Some companies have to use high-vanadium and high-sulfur petroleum coke to produce carbon anodes, but the impurity elements are too high, especially vanadium, which can greatly promote the oxidation of the anode, reduce its physical and chemical properties, and thus lead to a decrease in the quality of the anode. In addition, it enters the electrolyte during the electrolysis process, affecting the aluminum liquid index. Therefore, high-vanadium petroleum coke has great potential for vanadium removal.
[0003] At present, the extraction of vanadium from petroleum coke is mainly based on wet methods, including acid leaching and alkaline leaching. The acid leaching process mainly uses sulfuric acid as the leaching agent, and the vanadium extraction rate is relatively high, but the leaching process needs to be carried out under high temperature and high pressure conditions, the leaching conditions are harsh, and the leaching process produces toxic and harmful gases (SO2, etc.), which have a great impact on the environment; the alkaline leaching process mainly uses sodium hydroxide as the leaching agent, and sodium hypochlorite, potassium hypochlorite, etc. are added as oxidants, which can also achieve a high vanadium extraction rate, but the leaching process introduces a large amount of metallic impurity elements (Na, K, etc.). Once these harmful impurity metals enter the petroleum coke, it is very difficult and cumbersome to remove them later. Therefore, it is urgent to develop a new process for removing vanadium from high-vanadium petroleum coke. Summary of the invention
[0004] The present application provides a method for removing vanadium from petroleum coke used in atmospheric pressure aluminum anodes to solve the following technical problem: how to remove vanadium from petroleum coke.
[0005] The present application provides a method for removing vanadium from petroleum coke used as an anode for atmospheric pressure aluminum, wherein the petroleum coke contains vanadium, comprising the following steps:
[0006] The petroleum coke, oxidant and acid solution are mixed to obtain a mixed material;
[0007] The mixed material is subjected to leaching reaction to obtain devanadiumized petroleum coke.
[0008] Optionally, the molar concentration of hydrogen ions in the mixed material is 0.5 mol / L to 3.5 mol / L.
[0009] Optionally, the molar concentration of the oxidant in the mixed material is 1 mol / L to 3 mol / L.
[0010] Optionally, the acid solution includes at least one of the following: hydrochloric acid, nitric acid and acetic acid.
[0011] Optionally, the oxidant includes at least one of the following: hypochlorous acid, perchloric acid and hydrogen peroxide.
[0012] Optionally, the oxidant is hydrogen peroxide, and the volume fraction of the hydrogen peroxide is 3% to 7%.
[0013] Optionally, the solid-liquid ratio in the mixed material is 1:1 to 1:7.
[0014] Optionally, the mixed material is reacted, and the reaction parameters of the leaching reaction include: a reaction temperature of 50° C. to 90° C., and a reaction time of 60 min to 180 min.
[0015] Optionally, the vanadium content in the petroleum coke is greater than 0.05%, and the mass of the vanadium in the petroleum coke is greater than 0.05% of the total mass of the petroleum coke.
[0016] Optionally, the particle size of the petroleum coke is not less than 100 mesh.
[0017] Optionally, subjecting the mixed material to a leaching reaction to obtain devanadiumized petroleum coke comprises:
[0018] subjecting the mixed material to a leaching reaction to obtain a reaction mixed solution;
[0019] The reaction mixed solution is subjected to solid-liquid separation to obtain devanadiumized petroleum coke.
[0020] The above technical solution provided by the embodiment of the present invention has the following advantages compared with the prior art:
[0021] The invention discloses a method for removing vanadium from petroleum coke for normal pressure aluminum anodes, and relates to the technical field of vanadium recovery. The method of the invention comprises the following steps: firstly, petroleum coke is mixed with an oxidant and an acid solution in a solid-liquid ratio to obtain a mixed material; the mixed material is subjected to a leaching reaction under normal pressure conditions, and after the reaction is completed, solid-liquid separation is performed to obtain devanadiumized petroleum coke. The vanadium element in the petroleum coke mainly exists in the form of insoluble low-valent oxides (V2O3, VO2). During the leaching process, the low-valent oxides of vanadium are oxidized to high-valent oxides (V2O5) that are easily soluble in acid, thereby achieving effective removal of vanadium from the petroleum coke. The invention is simple to operate, low in cost, and does not introduce impurity metal elements. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] The accompanying drawings herein are incorporated in and constitute a part of the specification, illustrate embodiments consistent with the present application, and together with the description, are used to explain the principles of the present application.
[0023] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.
[0024] Figure 1 The present invention is a schematic flow chart of a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anodes according to some embodiments of the present application. DETAILED DESCRIPTION
[0025] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are 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 making creative work are within the scope of protection of this application.
[0026] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity and should not be understood as a rigid limitation on the scope of the present application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values within the range; for example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which applies regardless of the range; in addition, whenever a numerical range is indicated in this document, it is meant to include any cited numbers (fractions or integers) within the indicated range.
[0027] In this document, the terms including "including" and "including" mean "including but not limited to". Relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. "And / or" describes the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone; where A and B can be singular or plural. "At least one" means one or more, and "plurality" means two or more; "at least one", "at least one of the following" or similar expressions, refers to any combination of these items, including any combination of single or plural items; for example, "at least one of a, b, or c", or "at least one of a, b, and c" can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple. "Parts" such as parts by weight and parts by mass indicate the proportional relationship between the components. In the proportional relationship involved in this article, the parameters that need to be described by proportion should be understood as the first term of the proportional formula in the order of description, and the proportional numbers should be understood as the second term of the proportional formula. For example, if the mass ratio of substance A, substance B and substance C is 1:2:3, then substance A, substance B and substance C should correspond to the proportional numbers in the proportional formula in the order of description, that is, the mass of substance A: the mass of substance B: the mass of substance C = 1:2:3.
[0028] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in this article can be purchased from the market or prepared by existing methods.
[0029] Figure 1 A schematic flow chart of a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anodes according to some embodiments of the present application;
[0030] like Figure 1 As shown, the embodiment of the present application provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, wherein the petroleum coke contains vanadium, including:
[0031] S1, mixing the petroleum coke, oxidant and acid solution to obtain a mixed material;
[0032] S2. subjecting the mixed material to an acid leaching reaction to obtain devanadiumized petroleum coke.
[0033] In the above embodiment, the vanadium element in the petroleum coke mainly exists in the form of insoluble low-valent oxides (V2O3, VO2), the oxidant includes an oxidizing substance, the acidic substance provides hydrogen ions, and the petroleum coke is mixed with the oxidant and the acid solution to carry out a leaching reaction. During the leaching process, the low-valent oxides of vanadium are oxidized to high-valent oxides (V2O5) that are easily soluble in acid, thereby achieving effective removal of vanadium from inferior high-vanadium petroleum coke. Finally, after the reaction is completed, the mixed material is directly subjected to solid-liquid separation to obtain an acid solution containing vanadium elements and devanadiumized petroleum coke.
[0034] The advantages of this method are:
[0035] The raw materials are simple: only two substances are needed: oxidant and acidic substance to dissolve and react vanadium in petroleum coke;
[0036] The process is simple: only one-step reaction is required, that is, the oxidant, acid solution and petroleum coke need to be mixed and reacted directly. After the reaction, only solid-liquid separation is required to obtain the vanadium-containing acid solution and the devanadiumized petroleum coke, thereby achieving the removal of vanadium from the petroleum coke.
[0037] As an optional implementation manner, the molar concentration of hydrogen ions in the mixed material is 0.5 mol / L to 3.5 mol / L.
[0038] In the above embodiment, the reason for controlling the molar concentration of hydrogen ions in the mixed material to be 0.5mol / L to 3.5mol / L is to ensure that the solution in the mixed material is always acidic and to maximize the removal of vanadium. The concentration of hydrogen ions will affect the rate and effect of the acidolysis reaction, so it needs to be controlled within an appropriate range. If the molar concentration of hydrogen ions exceeds 3.5mol / L, it is easy to cause waste of acidic substances. If the molar concentration of hydrogen ions is lower than 0.5mol / L, it will affect the removal efficiency of vanadium. Exemplarily, the molar concentration of hydrogen ions in the mixed material is 0.5mol / L, 1.0mol / L, 1.5mol / L, 2.0mol / L, 2.5mol / L, 3.0mol / L or 3.5mol / L.
[0039] As an optional implementation manner, the molar concentration of the oxidant in the mixed material is 1 mol / L to 3 mol / L.
[0040] In the above embodiment, the reason for controlling the molar concentration of the oxidant in the mixture to be 1 mol / L to 3 mol / L is to ensure that the low-valent oxides of vanadium in the petroleum coke are completely reacted, thereby facilitating the extraction of vanadium in the petroleum coke. If the concentration of the oxidant exceeds 3 mol / L, it may cause waste of the oxidant; if the concentration of the oxidant is lower than 1 mol / L, the vanadium trioxide in the petroleum coke may not react completely. Exemplarily, the molar concentration of the oxidant in the mixture may be 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L or 3 mol / L.
[0041] As an optional implementation, the acid solution includes at least one of the following: hydrochloric acid, nitric acid and acetic acid.
[0042] In the above-mentioned embodiment, the acid solution can be selected from hydrochloric acid, nitric acid or acetic acid, etc. These acids are acidic and can effectively carry out acidolysis reaction. The acid solution prepared by using one or more of hydrochloric acid, nitric acid and acetic acid can provide hydrogen ions to participate in the reaction. Since it is necessary to use excessive acid during the reaction, it is also necessary to consider the problem of excess acid treatment after the reaction. Hydrochloric acid and acetic acid can be directly volatilized by evaporation, while others require other treatment methods. Therefore, hydrochloric acid and acetic acid are more preferred acids. In addition, since acetic acid may be oxidized into carbon dioxide and water in the presence of a strong oxidant, hydrochloric acid is the best choice.
[0043] As an optional embodiment, the oxidant includes at least one of the following: hypochlorous acid, perchloric acid and hydrogen peroxide.
[0044] In the above embodiment, the oxidant may be hypochlorous acid, perchloric acid or hydrogen peroxide, etc., which have strong oxidizing properties and can effectively oxidize vanadium. The function of the oxidant is to oxidize low-valent oxides into vanadium pentoxide, so any oxidant that can achieve this purpose belongs to the protection scope of this application.
[0045] As an optional implementation manner, the oxidant is hydrogen peroxide, and the volume fraction of the hydrogen peroxide is 3% to 7%.
[0046] When the oxidant is hydrogen peroxide, its volume fraction should be controlled between 3% and 7% to ensure the oxidation effect.
[0047] In the above embodiment, hydrogen peroxide is selected as the oxidant for the following reasons:
[0048] 1) Hydrogen peroxide does not contain other elements, avoiding subsequent impurity element treatment;
[0049] 2) Hydrogen peroxide is highly safe, low-cost, and suitable for industrial promotion and application;
[0050] 3) When hydrogen peroxide has not reacted completely, it can be directly decomposed by heating to reduce the subsequent processing procedures.
[0051] As an optional implementation, the solid-liquid ratio in the mixed material is 1:1 to 1:7, that is, in the mixed material, the ratio of the mass of petroleum coke to the total mass of the oxidant and the acid solution is controlled to be 1:1 to 1:7.
[0052] In the above embodiment, the reason for controlling the solid-liquid ratio in the mixed material to be 1:1 to 1:7 is that petroleum coke is hydrophobic, and its contact area with the solution needs to be guaranteed to achieve the dissolution reaction. If the mass ratio of the mass of petroleum coke to the solution exceeds 1:1, the surface of the petroleum coke may not be completely in contact with the solution, reducing the efficiency of the dissolution reaction; if the mass ratio of the mass of petroleum coke to the solution is less than 1:7, the amount of petroleum coke is too small, wasting the solution. Exemplarily, the solid-liquid ratio in the mixed material can be 1:1, 1:2, 1:3, 1:4, 1:5, 1:6 or 1:7.
[0053] As an optional implementation, the parameters of the leaching reaction include: a reaction temperature of 50° C. to 90° C., and a reaction time of 60 min to 180 min.
[0054] In the above embodiment, the reaction temperature is controlled to be 50°C to 90°C because increasing the temperature is conducive to the reaction. When the temperature is lower than 50°C, the reaction rate and the vanadium dissolution rate are both low; however, when the temperature is higher than 90°C, the oxidant and the acid in the mixture may volatilize or even decompose. Exemplarily, the reaction temperature may be 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C or 90°C.
[0055] There is a certain relationship between the reaction time and the reaction temperature. When the reaction temperature is high, the reaction speed is fast and the reaction time is short; when the reaction temperature is low, the reaction time is long. Exemplarily, the reaction time can be 60 min, 70 min, 80 min, 90 min, 100 min, 110 min, 120 min, 130 min, 140 min, 150 min, 160 min, 170 min or 180 min.
[0056] As an optional implementation, the vanadium content in the petroleum coke is greater than 0.05%.
[0057] In the above embodiment, the vanadium content in the petroleum coke is controlled to be greater than 0.05%. The reason is that if the vanadium content in the petroleum coke is low, it does not need to be removed and can be used for the preparation of aluminum anodes.
[0058] As an optional implementation, the particle size of the petroleum coke is not less than 100 mesh.
[0059] In the above embodiment, the particle size of petroleum coke is controlled to be not less than 100 meshes, the purpose of which is to ensure the dissolution efficiency and reaction efficiency. The carbon content in petroleum coke is too high. If the particle size exceeds 100 meshes, most of the vanadium elements in the petroleum coke will be wrapped by carbon and cannot react, thereby reducing the reaction efficiency.
[0060] As an optional embodiment, the mixed material is subjected to a leaching reaction to obtain devanadiumized petroleum coke, comprising:
[0061] subjecting the mixed material to a leaching reaction to obtain a reaction mixed solution;
[0062] The reaction mixed solution is subjected to solid-liquid separation to obtain devanadiumized petroleum coke.
[0063] The present application is further described below in conjunction with specific examples. The experimental methods in the following examples where specific conditions are not specified are usually measured in accordance with national standards / industry standards; if there are no corresponding national standards / industry standards, they are measured in accordance with common international standards, conventional conditions or conditions recommended by the manufacturer.
[0064] The petroleum coke used in the following examples and comparative examples has a vanadium content of 0.065% and a particle size of 200 meshes.
[0065] Example 1
[0066] This embodiment provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, comprising the following steps:
[0067] S1, taking 100 g of high-vanadium petroleum coke, adding hydrogen peroxide and hydrochloric acid solution as devanadium agents and stirring evenly to obtain a mixed material;
[0068] The concentration of hydrochloric acid in the mixture is 0.5 mol / L, the volume fraction of hydrogen peroxide is 3%, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:1;
[0069] S2, reacting the mixture in step S1 at 50° C., stirring at 400 rpm, and reacting for 60 min. After the reaction is completed, naturally cooling to room temperature is performed, and devanadiumized petroleum coke is obtained after solid-liquid separation.
[0070] The devanadiumized petroleum coke is analyzed by element content, and the vanadium removal rate is calculated to be 51.2%. The devanadiumized petroleum coke can be used as a raw material for carbon anode for aluminum.
[0071] Example 2
[0072] This embodiment provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, comprising the following steps:
[0073] S1, taking 100 g of high-vanadium petroleum coke, adding hydrogen peroxide and hydrochloric acid solution as devanadium agents and stirring evenly to obtain a mixed material;
[0074] The concentration of hydrochloric acid in the mixture is 1.5 mol / L, the volume fraction of hydrogen peroxide is 5%, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:3;
[0075] S2, reacting the mixture at 60° C., stirring at 400 rpm, and reacting for 90 min. After the reaction is completed, naturally cooling to room temperature is performed, and after solid-liquid separation, a vanadium-containing acid solution and devanadiumized petroleum coke are obtained.
[0076] The devanadiumized petroleum coke is analyzed by element content, and the vanadium removal rate is calculated to be 56.9%. The devanadiumized petroleum coke can be used as a raw material for carbon anode for aluminum.
[0077] Example 3
[0078] This embodiment provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, comprising the following steps:
[0079] S1, taking 100 g of high-vanadium petroleum coke, adding hydrogen peroxide and hydrochloric acid solution as devanadium agents and stirring evenly to obtain a mixed material;
[0080] The concentration of hydrochloric acid in the mixture is 2.5 mol / L, the volume fraction of hydrogen peroxide is 5%, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:3;
[0081] S2, reacting the mixture at 70° C., stirring at 400 rpm, and reacting for 120 min. After the reaction is completed, naturally cooling to room temperature is performed, and after solid-liquid separation, a vanadium-containing acid solution and devanadiumized petroleum coke are obtained.
[0082] The devanadiumized petroleum coke is analyzed by element content, and the vanadium removal rate is calculated to be 60.2%. The devanadiumized petroleum coke can be used as a raw material for carbon anode for aluminum.
[0083] Example 4
[0084] This embodiment provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, comprising the following steps:
[0085] S1, taking 100 g of high-vanadium petroleum coke, adding hydrogen peroxide and hydrochloric acid solution as devanadium agents and stirring evenly to obtain a mixed material;
[0086] The concentration of hydrochloric acid in the mixture is 2.5 mol / L, the volume fraction of hydrogen peroxide is 5%, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:5;
[0087] S2, reacting the mixed material in step S2 at 80° C., stirring at 400 rpm, and reacting for 150 min. After the reaction is completed, naturally cooling to room temperature is performed, and after solid-liquid separation, a vanadium-containing acid solution and devanadiumized petroleum coke are obtained.
[0088] The devanadiumized petroleum coke is analyzed by element content, and the vanadium removal rate is calculated to be 64.7%. The devanadiumized petroleum coke can be used as a raw material for carbon anode for aluminum.
[0089] Example 5
[0090] This embodiment provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, comprising the following steps:
[0091] S1, taking 100 g of high-vanadium petroleum coke, adding hydrogen peroxide and hydrochloric acid solution as devanadium agents and stirring evenly to obtain a mixed material;
[0092] The concentration of hydrochloric acid in the mixture is 2.5 mol / L, the volume fraction of hydrogen peroxide is 5%, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:7;
[0093] S2, reacting the mixture at 90° C., stirring at 400 rpm, and reacting for 180 min. After the reaction is completed, naturally cooling to room temperature is performed, and after solid-liquid separation, a vanadium-containing acid solution and devanadiumized petroleum coke are obtained.
[0094] The devanadiumized petroleum coke is analyzed by element content, and the vanadium removal rate is calculated to be 67.3%. The devanadiumized petroleum coke can be used as a raw material for carbon anode for aluminum.
[0095] Example 6
[0096] This embodiment provides a method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, comprising the following steps:
[0097] S1, taking 100 g of high-vanadium petroleum coke, adding hydrogen peroxide and hydrochloric acid solution as devanadium agents and stirring evenly to obtain a mixed material;
[0098] The concentration of hydrochloric acid in the mixture is 3.5 mol / L, the volume fraction of hydrogen peroxide is 7%, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:7;
[0099] S2, reacting the mixture at 90° C., stirring at 400 rpm, and reacting for 180 min. After the reaction is completed, naturally cooling to room temperature is performed, and after solid-liquid separation, a vanadium-containing acid solution and devanadiumized petroleum coke are obtained.
[0100] The devanadiumized petroleum coke is analyzed by element content, and the vanadium removal rate is calculated to be 69.3%. The devanadiumized petroleum coke can be used as a raw material for carbon anode for aluminum.
[0101] Comparative Example 1
[0102] This comparative example provides a method for removing vanadium from petroleum coke for aluminum anodes, comprising the following steps:
[0103] S1, taking 100 g of high-vanadium petroleum coke, adding hydrochloric acid solution as a devanadium agent thereto and stirring evenly to obtain a mixed material;
[0104] The concentration of hydrochloric acid in the mixed material is 2.5 mol / L, and the solid-liquid ratio of the inferior high-vanadium petroleum coke to the devanadium agent in this embodiment is 1:3;
[0105] S2, reacting the mixture at 35° C., stirring at 400 rpm, and reacting for 120 min. After the reaction is completed, naturally cooling to room temperature is performed, and after solid-liquid separation, a vanadium-containing acid solution and devanadiumized petroleum coke are obtained.
[0106] The devanadiumized petroleum coke was analyzed by element content, and the vanadium removal rate was calculated to be 6.3%. The devanadiumized petroleum coke cannot be used as a raw material for carbon anodes for aluminum.
[0107] From the devanadium results of the above examples and comparative examples, it can be seen that in Examples 1 to 6, the devanadium method provided in the present application is adopted, and the oxidant and acid solution are used to carry out the devanadium reaction on the high-vanadium petroleum coke, and the final vanadium removal rate reaches more than 50%, and the highest can reach more than 69%, and the devanadium effect is good. In the comparative example, only the acid solution is used to carry out the devanadium reaction on the high-vanadium petroleum coke, and the final vanadium removal rate is only 6.3%, and the devanadium effect is extremely poor. The devanadium petroleum coke obtained cannot meet the requirements of petroleum coke for carbon anode for aluminum.
[0108] In summary, the method for devanadiumizing petroleum coke for atmospheric pressure aluminum anode provided in the embodiments of the present application can be used to devanadiumize petroleum coke, and the vanadium oxides in the petroleum coke can be effectively recovered, and the removal rate can reach more than 69%. At the same time, the process is simple and has great potential for industrial application.
[0109] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. It will be apparent to those skilled in the art that various modifications to these embodiments are possible, and the general principles defined in the present application can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown in the present application, but will conform to the widest range consistent with the principles and novel features applied for by the present application.
Claims
1. A method for removing vanadium from petroleum coke for atmospheric pressure aluminum anode, wherein the petroleum coke contains vanadium, comprising the following steps: The petroleum coke, oxidant and acid solution are mixed to obtain a mixed material; The mixed material is subjected to leaching reaction to obtain devanadiumized petroleum coke.
2. The method according to claim 1, wherein the molar concentration of hydrogen ions in the mixed material is 0.5 mol / L to 3.5 mol / L.
3. The method according to claim 1, wherein the molar concentration of the oxidant in the mixed material is 1 mol / L to 3 mol / L.
4. The method according to claim 1, wherein the acid solution comprises at least one of the following: hydrochloric acid, nitric acid and acetic acid; and the oxidant comprises at least one of the following: hypochlorous acid, perchloric acid and hydrogen peroxide.
5. The method according to claim 1, wherein the oxidant is hydrogen peroxide, and the volume fraction of the hydrogen peroxide is 3% to 7%.
6. The method according to claim 1, wherein the solid-liquid ratio in the mixed material is 1:1 to 1:
7.
7. According to the method of claim 1, the mixed material is reacted, and the reaction parameters of the leaching reaction include: The reaction temperature is 50°C to 90°C, and the reaction time is 60min to 180min.
8. The method according to claim 1, wherein the mass of vanadium in the petroleum coke is greater than 0.05% of the total mass of the petroleum coke.
9. The method according to claim 1, wherein the particle size of the petroleum coke is not less than 100 mesh.
10. The method according to claim 1, wherein the mixed material is subjected to a leaching reaction to obtain devanadiumized petroleum coke, comprising: subjecting the mixed material to a leaching reaction to obtain a reaction mixed solution; The reaction mixed solution is subjected to solid-liquid separation to obtain devanadiumized petroleum coke.