Method for using vanadium precipitation agent for vanadium-containing mother liquor at normal temperature

Abstract

The invention discloses a use method of a vanadium-containing mother liquor vanadium precipitation agent at normal temperature, and belongs to the technical field of non-ferrous metallurgy. The use method comprises the following steps that S1, a vanadium precipitation agent solution is prepared; s2, preparing a vanadium precipitate through the vanadium precipitation agent solution obtained in the step S1; and S3, drying and calcining the vanadium precipitate obtained in S2 to obtain a vanadium pentoxide product. According to the use method of the vanadium-containing mother liquor vanadium precipitation agent at the normal temperature, vanadium precipitation can be carried out at the normal temperature, the vanadium precipitation time can be shortened to be within 5 min, the production efficiency is greatly improved, and the vanadium recovery rate and the purity of a vanadium product are remarkably improved through participation of the vanadium precipitation agent.

Description

Technical Field

[0001] The invention relates to the technical field of nonferrous metallurgy, and in particular to a method for using a vanadium-containing mother liquor vanadium precipitation agent at room temperature. Background Art

[0002] Vanadium is a rare metal element with excellent physical and chemical properties. It has a high melting point and boiling point, good ductility and toughness, and high corrosion resistance to hydrochloric acid, dilute sulfuric acid, alkaline solution and seawater. With the development of modern industry, the demand for vanadium in various fields continues to grow, especially in the steel industry, chemical industry, aerospace and other fields. At present, the main raw material used in the vanadium extraction industry is vanadium-containing converter slag produced after vanadium-titanium magnetite is smelted in blast furnace and converter.

[0003] Based on this, the current vanadium extraction processes mainly include sodium roasting-water leaching process and calcium roasting-acid leaching process. In order to extract vanadium from the leaching solution, the mainstream process cannot do without adding ammonium salts, high-temperature hydrolysis and other processes, which are inevitably accompanied by low production efficiency, large energy consumption for heating, and the generation of ammonia nitrogen wastewater. In addition, the traditional vanadium precipitation process also has problems such as low purity and recovery rate. Summary of the invention

[0004] The purpose of the present invention is to provide a method for using a vanadium-containing mother liquor vanadium precipitation agent at room temperature, which can be used to precipitate vanadium at room temperature and shorten the vanadium precipitation time to within 5 minutes, thereby greatly improving production efficiency. Through the participation of the vanadium precipitation agent, the recovery rate of vanadium and the purity of the vanadium product are significantly improved.

[0005] To achieve the above object, the present invention provides a method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature, comprising the following steps:

[0006] S1, preparing a vanadium precipitation agent solution;

[0007] S2, preparing vanadium precipitate by using the vanadium precipitant solution obtained in S1;

[0008] S3, drying and calcining the vanadium precipitate obtained in S2 to obtain a vanadium pentoxide product.

[0009] Preferably, the specific operation of S2 is: adding the vanadium precipitant solution obtained in S1 to the vanadium leaching mother solution while it is hot and stirring evenly, adding acid solution to adjust the pH to react and obtain vanadium precipitate.

[0010] Preferably, the specific operation of S2 is: adding the vanadium precipitant solution obtained in S1 to the vanadium leaching mother solution while it is hot and stirring evenly, adding acid solution to adjust the pH to react and obtain vanadium precipitate.

[0011] Preferably, the mass ratio of the vanadium precipitant to the clean water in S1 is 1:20-50.

[0012] Preferably, the mass ratio of the vanadium precipitant to the clean water in S1 is 1:25-30.

[0013] Preferably, the mass ratio of the weight of the vanadium precipitant in S2 to the vanadium element in the vanadium leaching mother liquor is 0.9-1.3, the stirring speed is 300-400rpm, the acid solution is one or both of acetic acid and sulfuric acid, the pH is adjusted to 2-5, and the reaction time is 1-10min.

[0014] Preferably, the TV concentration of the vanadium leaching mother solution in S2 is 0.1-100 g / L.

[0015] Preferably, the mass ratio of the weight of the vanadium precipitant in S2 to the mass ratio of the vanadium element in the vanadium leaching mother solution is 1-1.2, the pH is adjusted to 3-3.5, and the reaction time is 3-5 min.

[0016] Preferably, the calcination temperature in S3 is 550-600° C. and the calcination time is 2-3 h.

[0017] Preferably, the reaction of S2 is carried out at room temperature, which ranges from 0 to 50°C.

[0018] Therefore, the present invention adopts the method of using the above-mentioned vanadium-containing mother solution vanadium precipitation agent at room temperature, which has the following beneficial effects:

[0019] (1) Vanadium precipitation can be carried out at room temperature, and the precipitation time can be shortened to within 5 minutes, greatly improving production efficiency;

[0020] (2) The participation of vanadium precipitation agent significantly improves the recovery rate of vanadium and the purity of vanadium products. The residual vanadium content of vanadium precipitation wastewater produced by the calcium roasting-acid leaching process is about 0.2g / L, while the residual vanadium content of vanadium precipitation wastewater produced by the present invention is less than 0.05g / L, which improves the vanadium recovery rate of enterprises. The purity of vanadium products produced by the sodium roasting-water leaching process and the calcium roasting-acid leaching process is usually about 95%-98%. The present invention can increase the purity of vanadium products to 99.8%;

[0021] (3) No ammonium salt is added during the entire vanadium precipitation process, and no ammonia nitrogen wastewater is generated, which reduces the cost of vanadium precipitation wastewater treatment.

[0022] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 The present invention is a flow chart of an embodiment of a method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature. DETAILED DESCRIPTION

[0024] The technical solution of the present invention is further described below through the accompanying drawings and embodiments.

[0025] Unless otherwise defined, technical or scientific terms used in the present invention shall have the common meanings understood by one having ordinary skills in the field to which the present invention belongs.

[0026] like Figure 1 As shown, the present invention provides a method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature, comprising the following steps:

[0027] S1. Prepare a vanadium precipitating agent solution: add a vanadium precipitating agent into clean water, heat it to boiling and dissolve it to obtain a vanadium precipitating agent solution.

[0028] The mass ratio of the vanadium precipitant to the clean water is 1:20-50, and preferably the mass ratio of the vanadium precipitant to the clean water is 1:25-30.

[0029] S2. Prepare vanadium precipitate by using the vanadium precipitate solution obtained in S1: add the vanadium precipitate solution obtained in S1 into the vanadium leaching mother liquor while it is hot and stir evenly, add acid solution to adjust the pH to react and obtain vanadium precipitate. The reaction of S2 is carried out at room temperature, and the room temperature range is 0-50°C.

[0030] The mass ratio of the weight of the vanadium precipitating agent to the vanadium element in the vanadium leaching mother solution is 0.5-1.3, the stirring speed is 300-400rpm, the acid solution is one or both of acetic acid and sulfuric acid, the pH is adjusted to 2-5, the reaction time is 1-10min, and the TV concentration of the vanadium leaching mother solution is 0.1-100g / L. Preferably, the mass ratio of the weight of the vanadium precipitating agent to the vanadium element in the vanadium leaching mother solution is 1-1.2, the pH is adjusted to 3-3.5, and the reaction time is 3-5min.

[0031] S3, drying and calcining the vanadium precipitate obtained in S2 to obtain a vanadium pentoxide product, the calcination temperature is 550-600°C, and the calcination time is 2-3h.

[0032] Vanadate ions (such as VO4 3- 、HVO4 2- 、H2VO4 -) is widely present in vanadium leaching solution within a certain pH range. Organic amine compounds represented by melamine (including fatty amines, alcohol amines, amides, alicyclic amines, aromatic amines, naphthyl amines and other amines) have amino groups (-NH2) or similar group structures. These groups contain lone pairs of electrons and can form stable complexes with vanadate ions through coordination. The complex formed often has a low solubility. After reaching supersaturation in the solution, it will precipitate in the form of precipitation. The solubility of the complex is closely related to the chemical properties of the complex, the acidity and alkalinity of the solution (pH), temperature and other conditions. By adjusting these parameters, the precipitation of vanadium can be promoted. Different types of organic amine compounds may form different complexes with vanadate ions due to their differences in structure and functional groups, and the efficiency and effect of precipitation are also different. For example, melamine has a unique triazine structure, which can provide multiple amino groups to complex with vanadate, thereby significantly improving the precipitation efficiency.

[0033] In summary, organic amine compounds represented by melamine react with vanadate ions in the vanadium leaching solution through complexation to form low-solubility complex precipitates. This process is of great significance in the extraction and recovery of vanadium resources due to its strong selectivity and simple operation.

[0034] Example 1

[0035] The present invention provides a method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature, comprising the following steps:

[0036] S1. Take 2.496 g of vanadium precipitant and add it to 60 ml of water and boil to dissolve to obtain a vanadium precipitant solution.

[0037] S2. Take the vanadium leaching mother liquor with TV=20.8g / L and pH=2.68. At room temperature, add the above vanadium precipitant solution to 100ml of the vanadium leaching mother liquor, add sulfuric acid to adjust the pH to 3.5, stir continuously at 300rpm for 5min, filter and obtain vanadium precipitate.

[0038] S3. calcining the dried vanadium precipitate at 600° C. for 2 h to obtain a vanadium pentoxide product.

[0039] The purity of the prepared vanadium pentoxide is 99.23%, and the vanadium recovery rate is 99.85%.

[0040] Example 2

[0041] The present invention provides a method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature, comprising the following steps:

[0042] S1. Take 4.455 g of vanadium precipitant and add it to 125 ml of water and boil to dissolve to obtain a vanadium precipitant solution.

[0043] S2. Take the vanadium leaching mother liquor with TV=40.5g / L and pH=2.53. At room temperature, add the above vanadium precipitant solution to 100ml of the vanadium leaching mother liquor, add sulfuric acid to adjust the pH to 3.3, stir at 300rpm for 5min, filter and obtain vanadium precipitate.

[0044] S3. calcining the dried vanadium precipitate at 600° C. for 2 h to obtain a vanadium pentoxide product.

[0045] The purity of the prepared vanadium pentoxide is 99.16%, and the vanadium recovery rate is 99.76%.

[0046] Example 3

[0047] The present invention provides a method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature, comprising the following steps:

[0048] S1. Take 20.9 g of vanadium precipitant and add it to 400 ml of water, boil and dissolve to obtain a vanadium precipitant solution.

[0049] S2. Take the vanadium leaching mother liquor with TV=0.38g / L and pH=2.30, add the above vanadium precipitant solution into 50L of vanadium leaching mother liquor with a temperature of 40°C, add sulfuric acid to adjust the pH to less than 4, stir continuously at 300rpm for 3min, filter and obtain vanadium precipitate.

[0050] S3. calcining the dried vanadium precipitate at 600° C. for 2 h to obtain a vanadium pentoxide product.

[0051] The purity of the prepared vanadium pentoxide is 98.95%, and the vanadium recovery rate is 99.12%.

[0052] Therefore, the present invention adopts the method of using the above-mentioned vanadium-containing mother liquor vanadium precipitation agent at room temperature, vanadium precipitation can be carried out at room temperature, and the vanadium precipitation time can be shortened to within 5 minutes, which greatly improves the production efficiency. Through the participation of the vanadium precipitation agent, the vanadium recovery rate and the purity of the vanadium product are significantly improved.

[0053] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solution of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solution to deviate from the spirit and scope of the technical solution of the present invention.

Claims

1. A method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature, characterized in that: The following steps are involved: S1, preparing a vanadium precipitation agent solution; S2, preparing vanadium precipitate by using the vanadium precipitant solution obtained in S1; S3, drying and calcining the vanadium precipitate obtained in S2 to obtain a vanadium pentoxide product.

2. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 1, characterized in that: The specific operation of S1 is: adding the vanadium precipitating agent into clean water, heating it to boiling and dissolving it to obtain a vanadium precipitating agent solution.

3. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 1, characterized in that: The specific operation of S2 is: adding the vanadium precipitant solution obtained in S1 into the vanadium leaching mother solution while it is hot and stirring evenly, adding acid solution to adjust the pH to react and obtain vanadium precipitate.

4. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 2, characterized in that: The mass ratio of vanadium precipitant to clean water in S1 is 1:20-50.

5. The method for using the vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 4, characterized in that: The mass ratio of vanadium precipitant to clean water in S1 is 1:25-30.

6. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 3, characterized in that: The mass ratio of the weight of the vanadium precipitant in S2 to the mass ratio of the vanadium element in the vanadium leaching mother liquor is 0.5-1.3, the stirring speed is 300-400rpm, the acid solution for adjusting pH is one or both of acetic acid and sulfuric acid, the pH is adjusted to 2-5, and the reaction time is 1-10min.

7. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 6, characterized in that: The TV concentration of the vanadium leaching mother solution in S2 is 0.1-100 g / L.

8. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 1, characterized in that: The mass ratio of the weight of the vanadium precipitant in S2 to the mass ratio of the vanadium element in the vanadium leaching mother solution is 1-1.2, the pH is adjusted to 3-3.5, and the reaction time is 3-5 minutes.

9. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 1, characterized in that: The calcination temperature in S3 is 550-600°C and the calcination time is 2-3h.

10. The method for using a vanadium-containing mother solution vanadium precipitation agent at room temperature according to claim 1, characterized in that: The reactions of S2 are all carried out at room temperature, ranging from 0 to 50°C.

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