Preparation method of efficient and stable TiCl4 refined mixed vanadium removal reagent

Abstract

The invention relates to the field of mixed metallurgy, and provides an efficient and stable TiCl4 refining mixed vanadium removal reagent preparation method which comprises the following steps: adding mineral oil into a mixing tank, stirring and heating; adding a dissolution promoter into the mixing tank, and mixing and stirring for a first preset time; adding fatty acid into the mixing tank, and mixing and stirring for a second preset time; and obtaining the mixed vanadium removal reagent from the mixing tank. By utilizing the vanadium removal activity of fatty acid and the dispersity of mineral oil, the two reagents are mixed according to a certain proportion to form the mixed vanadium removal reagent, active carbon particles generated by the mixed vanadium removal reagent in the production process are smaller, the effective vanadium removal surface area is larger, and the purposes of high efficiency and stability are achieved; the problems of low vanadium removal efficiency, short production cycle and large reagent usage amount of the existing fatty acid reagent and mineral oil are solved, so that the titanium tetrachloride refining vanadium removal system can operate economically and stably for a long period.

Description

Technical Field

[0001] The invention relates to the field of mixed metallurgy, and more specifically to a method for preparing an efficient and stable TiCl4 refined mixed vanadium removal reagent. Background Art

[0002] Vanadium removal reagents are used to test the vanadium content in steel. Through specific chemical reactions, the vanadium content in steel can be accurately determined, which is crucial to controlling the quality and performance of steel. It can also remove vanadium ions from wastewater, thereby reducing environmental pollution. Vanadium is a toxic heavy metal element. If it is discharged directly into the environment without treatment, it will cause harm to the ecosystem and human health.

[0003] At present, in industrial production, TiCl4 refining mainly uses chemical methods to remove VOCl3 impurities in crude titanium tetrachloride. The main methods are: copper wire vanadium removal method, aluminum powder vanadium removal method, hydrogen sulfide vanadium removal method and organic vanadium removal method. Among them, aluminum powder vanadium removal method and organic vanadium removal method are mainstream processes. Organic vanadium removal method has the characteristics of low production cost, simple and continuous process. It is an ideal vanadium removal method and the most widely used and largest vanadium removal method. According to the type of vanadium removal reagent, there are two types of organic vanadium removal methods: mineral oil vanadium removal method and fatty acid vanadium removal method.

[0004] However, in production practice, the fatty acid vanadium removal process has problems such as pipe blockage, scaling on the container wall, short production cycle due to adhesion, and high environmental pressure. The mineral oil vanadium removal process has problems such as low vanadium removal efficiency, large amount of vanadium removal reagents used, and unstable quality of refined titanium. Summary of the invention

[0005] In view of this, the present invention proposes a method for preparing an efficient and stable TiCl4 refined mixed vanadium removal reagent to solve the problems of low vanadium removal efficiency, short production cycle and large reagent usage existing in current fatty acid reagents and mineral oils.

[0006] Based on the above purpose, the present invention proposes a method for preparing an efficient and stable TiCl4 refined mixed vanadium removal reagent, comprising the following steps: Add mineral oil to a mixing tank and stir to heat; Adding the solvent into the mixing tank and mixing for a first preset time; Adding fatty acids into the mixing tank and mixing for a second preset time; Obtain the mixed vanadium removal reagent from the mixing tank.

[0007] In some embodiments, the mineral oil accounts for 50% to 55% by mass of the mixed vanadium removal reagent.

[0008] In some embodiments, the mass percentage of the dissolution promoter is 5% to 10% of the mixed vanadium removal reagent.

[0009] In some embodiments, the fatty acid accounts for 40% to 45% of the mixed vanadium removal reagent by weight.

[0010] In some embodiments, the solubilizing agent is an ester organic compound with 5-10 carbon atoms.

[0011] In some embodiments, the fatty acid is an unsaturated fatty acid with 10-30 carbon atoms.

[0012] In some embodiments, the mineral oil is liquid cycloalkanes and aromatic hydrocarbons with a specific gravity of 0.9 kg / L to 1.0 kg / L.

[0013] In some embodiments, the temperature at which the mineral oil and the solubilizing agent are mixed is 60°C to 80°C.

[0014] In some embodiments, the temperature range of sufficient mixing after adding fatty acid is 40°C to 120°C.

[0015] In some embodiments, the first preset time is 3 hours to 5 hours, and the second preset time is 1 hour to 3 hours.

[0016] The present invention has at least the following beneficial technical effects: The invention provides a method for preparing an efficient and stable TiCl4 refined mixed vanadium removal reagent, the method comprising: adding mineral oil into a mixing tank, stirring and heating; adding a solvent into the mixing tank, mixing and stirring for a first preset time; adding fatty acid into the mixing tank, mixing and stirring for a second preset time; obtaining the mixed vanadium removal reagent from the mixing tank.

[0017] The invention utilizes the vanadium removal activity of fatty acid and the dispersibility of mineral oil, mixes the two reagents in a certain ratio to form a mixed vanadium removal reagent, and during the production process, the activated carbon particles generated by the mixed vanadium removal reagent are smaller, and the effective vanadium removal surface area is larger, so as to achieve the purpose of high efficiency and stability, solve the problems of low vanadium removal efficiency, short production cycle and large reagent usage existing in the current fatty acid reagent and mineral oil, and make the titanium tetrachloride refined vanadium removal system economical, stable and long-term operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the following specific embodiments, they are used to explain the present invention but do not constitute a limitation of the present invention. In the accompanying drawings: Figure 1 A flow chart of a method for preparing an efficient and stable TiCl4 refined mixed vanadium removal reagent according to an embodiment of the present invention is shown. DETAILED DESCRIPTION

[0019] The specific implementation of the present disclosure is described in detail below in conjunction with the accompanying drawings. It should be understood that the specific implementation described herein is only used to illustrate and explain the present disclosure, and is not used to limit the present disclosure.

[0020] In addition, reference to "embodiments" herein means that a particular feature, structure, or characteristic described in conjunction with the embodiments may be included in at least one embodiment of the present invention. The appearance of the phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0021] It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical terms and scientific terms) used herein have the same meaning as the general understanding of those skilled in the art to which this application belongs. It should also be understood that terms such as those defined in general dictionaries should be understood to have the same meaning as in the context of the prior art, and will not be interpreted with an idealized or overly formal meaning unless specifically defined as in the embodiments of this application.

[0022] The present invention proposes a method for preparing a highly efficient and stable TiCl4 refined mixed vanadium removal reagent. Figure 1 , including the following steps: Add mineral oil to a mixing tank and stir to heat; Adding the solvent into the mixing tank and mixing for a first preset time; Adding fatty acids into the mixing tank and mixing for a second preset time; Obtain the mixed vanadium removal reagent from the mixing tank.

[0023] The present invention utilizes the principle that fatty acid reagents have high vanadium removal efficiency, but fatty acid molecules are prone to polymerization reactions, resulting in high viscosity and easy scaling; mineral oil vanadium removal reagents have low vanadium removal efficiency, but are easy to disperse. According to the characteristics of these two reagents in the vanadium removal reaction process, the vanadium removal activity of fatty acids and the dispersibility of mineral oil are utilized, and the two reagents are mixed in a certain proportion to form a mixed vanadium removal reagent. In the production process, the activated carbon particles generated by the mixed vanadium removal reagent are smaller, and the effective vanadium removal surface area is larger, thereby achieving the purpose of high efficiency and stability.

[0024] The highly efficient and stable TiCl4 refined mixed vanadium removal reagent prepared by the present invention mainly comprises three components: fatty acid, mineral oil and a solvent promoter; the preparation steps of the mixed vanadium removal reagent are: firstly, the mineral oil and the solvent promoter are fully mixed to form a reagent a, and then the reagent a and the fatty acid are fully mixed to form a target mixed vanadium removal reagent.

[0025] Fatty acids and mineral oils can work synergistically to improve the vanadium removal efficiency. Mineral oil can be used as a carrier or auxiliary agent in the process of fatty acid vanadium removal to enhance the vanadium removal effect. Fatty acids and mineral oils show different characteristics in the vanadium removal process. By using them in combination, their respective advantages can be fully utilized to make up for each other's shortcomings. Fatty acids have high vanadium removal performance, while mineral oils have good stability and low cost characteristics.

[0026] In some embodiments, see Figure 1 , the mass percentage of the mineral oil accounts for 50% to 55% of the mixed vanadium removal reagent.

[0027] Mineral oil is highly safe and easy to transport and store. At the same time, mineral oil shows good stability in the vanadium removal process and is not prone to chemical reactions that lead to equipment corrosion or blockage. The cost of mineral oil is relatively low. Using mineral oil as a vanadium removal reagent can reduce production costs to a certain extent and improve the economic benefits of the enterprise. Mineral oil can dissolve a variety of chemical substances. When used as a solvent or dispersant, it helps to evenly disperse other ingredients in the reagent and improve the stability and uniformity of the reagent. The use of mineral oil is relatively simple and does not require complex equipment and operating procedures. This helps to simplify the production process and improve production efficiency.

[0028] In some embodiments, see Figure 1 The mass percentage of the dissolution promoter is 5% to 10% of the mixed vanadium removal reagent.

[0029] A chaotropic agent can significantly lower the solubility threshold of the solute, making it easier for mineral oils and fatty acids that are difficult to dissolve in the solvent. This is especially important for mineral oils and fatty acids that have low solubility and are difficult to dissolve directly in water. By using a chaotropic agent, you can ensure that these substances are evenly distributed in the solution. During the dissolution process, the solution may be unstable due to particle aggregation, precipitation or denaturation. It helps the solute to be better dispersed in the solvent by interacting with the solute molecules and breaking the intermolecular interaction forces, thereby enhancing the uniformity and stability of the solution.

[0030] In some embodiments, see Figure 1 The mass percentage of the fatty acid is in the range of 40% to 45% of the mixed vanadium removal reagent.

[0031] Unsaturated fatty acids have a faster vanadium removal rate, and the vanadium removal efficiency increases with the increase of unsaturation. This means that under the same conditions, the use of unsaturated fatty acids can reduce the vanadium content in TiCl4 faster. As natural organic matter, fatty acids are widely available and renewable, and are more environmentally friendly than some chemical vanadium removal agents. At the same time, the use of fatty acids will not cause serious environmental pollution to the subsequent production process.

[0032] In some embodiments, see Figure 1 , the solubilizing agent is an ester organic substance with 5-10 carbon atoms.

[0033] Due to their specific chemical structure, ester organic compounds often have good solubility properties. When used as a cosolvent, they can effectively lower the solubility threshold of the solute, making it easier for substances that are originally insoluble or slightly soluble in the solvent to dissolve in the solvent. Esters of 5-10 carbon atoms can be used for many different types of solutes due to their moderate carbon chain length.

[0034] Ester organic compounds usually have high chemical stability and are not easily decomposed under normal conditions. They can maintain their solvent-promoting properties for a long time, thereby ensuring the stability and durability of the solution.

[0035] In some embodiments, see Figure 1 , the type of fatty acid is an unsaturated fatty acid with 10-30 carbon atoms.

[0036] The types with chain lengths between 10 and 30 carbons have excellent vanadium removal performance due to their unique chemical structure. These fatty acid molecules can effectively interact with vanadium ions, thereby precipitating or reducing them from solution. Compared with other types of vanadium removal agents, unsaturated fatty acids can reduce the vanadium content more quickly, making the vanadium removal process more efficient.

[0037] By adjusting the structure and type of unsaturated fatty acids, the vanadium removal rate and the amount of residue can be effectively controlled. For example, unsaturated fatty acids with different chain lengths and different saturation levels will show different performances in the vanadium removal process. The most suitable fatty acid type and ratio can be selected to achieve the best vanadium removal effect.

[0038] As natural organic compounds, unsaturated fatty acids are generally biodegradable. Using such substances as vanadium removal agents can reduce environmental pollution. Compared with traditional chemical vanadium removal methods, unsaturated fatty acid vanadium removal produces less waste, and these wastes are easier to handle. This helps reduce the impact of the vanadium removal process on the environment and is in line with the current concept of green chemistry and sustainable development.

[0039] In some embodiments, see Figure 1The types of mineral oil are liquid cycloalkanes and aromatic hydrocarbons with a specific gravity of 0.9kg / L~1.0kg / L.

[0040] Liquid cycloalkanes and aromatic hydrocarbons, as the main components of mineral oil, can effectively interact with vanadium ions, helping to precipitate or reduce vanadium ions from the solution, thereby achieving efficient vanadium removal. Mineral oil-based vanadium removal agents have faster vanadium removal speed and higher vanadium removal efficiency.

[0041] Liquid cycloalkanes and aromatic hydrocarbons have good compatibility and stability. They can be effectively mixed with other additives or solvents when preparing vanadium removal reagents and remain stable for a long time, which helps to ensure the performance and effect of vanadium removal reagents, thereby improving the reliability and accuracy of vanadium removal.

[0042] The vanadium removal effect can be controlled by adjusting its ratio, temperature, pH value and other conditions. Selecting the most suitable vanadium removal conditions to achieve the best vanadium removal effect makes the mineral oil-based vanadium removal reagent widely applicable in various application scenarios.

[0043] In some embodiments, see Figure 1 The temperature at which the mineral oil and the solvent are mixed is 60°C to 80°C.

[0044] At a temperature of 60°C to 80°C, the molecular movement speed of mineral oil and solvent-promoting agents increases, which helps to accelerate the dissolution and mixing process of the two. It can also reduce the viscosity of the solution, making it easier for mineral oil and solvent-promoting agents to penetrate and fuse with each other. High-temperature mixing helps to ensure that mineral oil and solvent-promoting agents are evenly distributed in the solution, avoiding local concentrations that are too high or too low. Even mixing can improve the performance and effect of vanadium removal agents.

[0045] Improving the reaction activity between mineral oil and vanadium ions and accelerating the vanadium removal reaction will help achieve a higher vanadium removal efficiency in a shorter time, and will facilitate the precipitation or reduction reaction between the active ingredients in the mineral oil and the vanadium ions, thereby more effectively removing vanadium from the solution.

[0046] Reduce the possibility of decomposition of mineral oil and solvent during mixing, which helps maintain the stability and durability of the vanadium removal agent. Prevent unnecessary precipitation of mineral oil and solvent during mixing, which helps maintain the clarity and transparency of the solution, thereby improving the vanadium removal effect.

[0047] In some embodiments, see Figure 1 After adding fatty acids, the temperature range for thorough mixing is 40℃~120℃.

[0048] The molecular movement speed of fatty acid, mineral oil and solvent is accelerated, which is conducive to the full mixing and uniform distribution among them, which can ensure that each component in the vanadium removal reagent reaches the best ratio and distribution state in the solution.

[0049] As the temperature increases, the viscosity of the solution decreases, and lower viscosity helps improve mixing efficiency and mixing uniformity.

[0050] The temperature range of 40℃~120℃ is relatively wide, which can adapt to different working environments and conditions, making the vanadium removal reagents have good adaptability and reliability in a variety of application scenarios. The wide temperature range allows researchers to choose the most suitable mixing temperature according to specific needs, which helps to improve the flexibility and customizability of vanadium removal reagents.

[0051] The temperature range of 40℃~120℃ is moderate and easy to control by heating or cooling equipment, making the mixing process more controllable and stable. Compared with higher or lower temperature ranges, the mixing temperature of 40℃~120℃ can reduce energy consumption, help reduce production costs and improve economic benefits.

[0052] In some embodiments, see Figure 1 , the first preset time is 3h~5h, and the second preset time is 1h~3h.

[0053] The mixed reagent of the present invention has a larger effective vanadium removal surface area, a higher vanadium removal efficiency, and can operate stably for a long time for more than 6 months.

[0054] In some embodiments, the main implementation equipment includes: a mixing tank with heating and stirring, an oleic acid storage tank, a mineral oil storage tank, and a butyl valerate storage tank. Follow the steps below: Open the valve of the mineral oil storage tank, introduce 550kg of mineral oil into the mixing tank and then close the valve; turn on the agitator speed to 5r / min, turn on the heating device to heat the mineral oil to 70°C; open the valve of the butyl valerate storage tank, introduce 50kg of butyl valerate reagent into the mixing tank and then close the valve; maintain the temperature and stirring speed, and mix thoroughly for 5h; open the valve of the oleic acid storage tank, introduce 400kg of oleic acid into the mixing tank and then close the valve; maintain the temperature and stirring speed, and mix thoroughly for 3h; stop heating and stirring, and the preparation of the mixed vanadium removal reagent is completed.

[0055] After the reaction is completed, the mixture is cooled to room temperature, and the solid product is separated from the liquid product by centrifugation, filtration or sedimentation. The separated solid product is purified to remove unreacted raw materials and other impurities, and the purified product is dried to remove residual moisture and solvent.

[0056] The composition of the vanadium removal reagent is analyzed by chemical analysis methods (such as infrared spectroscopy, nuclear magnetic resonance, etc.) to ensure that it meets the predetermined quality standards.

[0057] The performance of the vanadium removal reagent was tested, such as vanadium removal efficiency and stability, to evaluate its effect in practical application. The experimental results show that the reagent dosage of the present invention is less, only 0.3 kg of mixed reagent is needed for each kilogram of vanadium trichloride, and the cost of vanadium removal is lower, which can reduce the cost by 10% to 15%. It is estimated that after the use of this technology, the dosage of vanadium removal reagent will be reduced by 10%, the production cycle will be increased to 6 months, and the annual saving of raw materials is expected to generate benefits of 600,000 yuan, and the production cycle will be increased to generate benefits of 700,000 yuan, with a total economic benefit of 1.3 million yuan.

[0058] Store the vanadium removal reagent in a dry, cool, well-ventilated place, away from direct sunlight and high temperatures, and ensure that the storage container is well sealed to prevent air and moisture from entering. According to the specific application scenario and needs, add the vanadium removal reagent to the solution to be treated in an appropriate proportion. Promote the reaction of the vanadium removal reagent with the vanadium ions in the solution by stirring, heating, etc. After the reaction is completed, separate the solid product from the solution by filtration, centrifugation, etc. to remove the vanadium in the solution.

[0059] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0060] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0061] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A method for preparing an efficient and stable TiCl4 refined mixed vanadium removal reagent, characterized in that: The following steps are involved: Add mineral oil to a mixing tank and stir to heat; Adding the solvent into the mixing tank and mixing for a first preset time; Adding fatty acids into the mixing tank and mixing for a second preset time; Obtain the mixed vanadium removal reagent from the mixing tank.

2. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The mass percentage of the mineral oil accounts for 50% to 55% of the mixed vanadium removal reagent.

3. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The mass percentage of the dissolution promoter is 5% to 10% of the mixed vanadium removal reagent.

4. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The mass percentage of the fatty acid in the mixed vanadium removal reagent is in the range of 40% to 45%.

5. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The solubilizing agent is an ester organic substance with 5 to 10 carbon atoms.

6. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The fatty acid is an unsaturated fatty acid with 10 to 30 carbon atoms.

7. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The types of mineral oil are liquid cycloalkanes and aromatic hydrocarbons with a specific gravity of 0.9kg / L~1.0kg / L.

8. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The temperature at which the mineral oil and the solvent-promoting agent are mixed is 60° C. to 80° C.

9. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: After adding fatty acids, the temperature range for thorough mixing is 40°C to 120°C.

10. The method for preparing the highly efficient and stable TiCl4 refined mixed vanadium removal reagent according to claim 1, characterized in that: The first preset time is 3h~5h, and the second preset time is 1h~3h.

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