A method for controlling solid content of a vanadium removal slurry

Abstract

According to one aspect of the present application, a method for controlling solid content of vanadium-removing slurry is provided, comprising the following steps: adding high-vanadium titanium tetrachloride into a vanadium-removing reactor; adding mixed fatty acid into the vanadium-removing reactor; calculating the discharge amount of vanadium-removing slurry; and controlling the discharge of vanadium-removing slurry from the vanadium-removing reactor according to the calculation result. Through the above-mentioned method for controlling solid content of vanadium-removing slurry, the solid content of vanadium-removing slurry is controlled to fluctuate slightly within the process requirement range by establishing a slurry discharge control model, the first pass yield of refined titanium is improved, the comprehensive utilization of Panxi titanium resources is greatly promoted, and key technical support is provided for large-scale development and utilization of high-titanium blast furnace slag.

Description

Technical Field

[0001] This application generally relates to the technical field of titanium tetrachloride refining, and more specifically, to a method for controlling the solid content of vanadium-removing slurry. Background Technology

[0002] In the selective carbonization-chlorination technology independently developed by Panzhihua Iron and Steel Group, the use of high-titanium blast furnace slag with vanadium-titanium symbiosis as raw material results in crude titanium tetrachloride (TiCl4) containing vanadium oxychloride (VOCl3) impurities exceeding 0.80%, which is more than four times higher than that produced using conventional titanium raw materials. Panzhihua Iron and Steel Group has conducted research on key technologies for efficient refining and vanadium removal using fatty acids as vanadium removal reagents for high-vanadium titanium tetrachloride. During the vanadium removal process, the fluctuating vanadium oxychloride content in the high-vanadium titanium tetrachloride leads to variations in the amount of vanadium removal slurry residue produced after reacting with fatty acid vanadium removal reagents in specific proportions, and also results in variations in the solid content of the crude titanium tetrachloride, causing large fluctuations in the solid content of the vanadium removal slurry generated within the system. In response to fluctuations, the usual practice is to discharge more slurry when the solid content is high and less when the solid content is low. The amount of slurry discharged is controlled based on individual experience, which can easily lead to the solid content of vanadium removal slurry being too low or too high between batches. This makes it difficult to control the solid content of vanadium removal slurry, and the system is prone to blockage and shutdown or substandard quality of refined titanium tetrachloride. The first-pass yield of refined titanium tetrachloride is only 82%.

[0003] Regarding the above-mentioned issues, there is still room for improvement in achieving stable control of the solid content of the vanadium removal slurry during the vanadium removal process of titanium tetrachloride. Summary of the Invention

[0004] To address the aforementioned problems, this disclosure summarizes various aspects of the embodiments and should not be construed as limiting the claims. Other implementations are conceivable based on the technology described herein, as will be apparent to those skilled in the art upon studying the following drawings and detailed descriptions, and these implementations are intended to be included within the scope of this application.

[0005] According to one aspect of the present invention, a method for controlling the solid content of vanadium removal slurry is provided, comprising the following steps:

[0006] High-vanadium titanium tetrachloride was added to the vanadium removal reactor;

[0007] Add mixed fatty acids to the vanadium removal reactor;

[0008] Calculate the discharge volume of vanadium removal slurry;

[0009] The discharge of vanadium removal slurry from the vanadium removal reactor is controlled based on the calculation results.

[0010] In one embodiment, the vanadium removal reactor is a circulating pump tank.

[0011] In another embodiment, calculating the vanadium removal slurry discharge includes:

[0012] A mud discharge control model was established based on the correlation between the amount of crude titanium tetrachloride fed, the amount of refined titanium tetrachloride collected, the impurity content of crude titanium tetrachloride, the density of crude titanium tetrachloride, the density of refined titanium tetrachloride, and the solid content of vanadium removal mud.

[0013] In yet another embodiment, the correlation is determined by the following formula:

[0014]

[0015] Where X represents the hourly discharge volume of vanadium slurry, in kg.

[0016] Y represents the solid content control value of the vanadium removal slurry, in g / L;

[0017] RV represents the mass percentage of vanadium oxychloride in crude titanium tetrachloride;

[0018] D and ρ are the solid content and density of crude titanium tetrachloride, respectively, in g / L and kg / m3.

[0019] L represents the hourly feed rate of crude titanium tetrachloride, expressed in kg.

[0020] γ is a correction coefficient, which is dimensionless.

[0021] In yet another embodiment, the mixed fatty acids are formulated from at least one of oleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, docosahexaenoic acid, and at least one of palmitic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, and arachidic acid.

[0022] In yet another embodiment, a mixed fatty acid is added, and then the temperature inside the vanadium removal reactor is raised to 140-160°C.

[0023] In yet another embodiment, the valves of the slurry tank's diversion pipeline are controlled by a controller that calculates the discharge rate of the vanadium-removing slurry based on a correlation formula.

[0024] In yet another embodiment, fatty acids are fed into the vanadium removal reactor via a vaporization chamber reflux pipe.

[0025] In another embodiment, the high-vanadium titanium tetrachloride is produced by low-temperature chlorination, and the flow rate of the high-vanadium titanium tetrachloride input into the titanium tetrachloride circulation pump tank is 7-8 t / h, and the amount of mixed fatty acids added is 0.04-0.08 t / h.

[0026] In yet another embodiment, the initial vanadium-removing titanium tetrachloride slurry in the titanium tetrachloride circulating pump tank is continuously discharged through a slurry discharge pipe and fed into a titanium tetrachloride mud transfer tank.

[0027] The method for stabilizing the solid content of high-vanadium slurry provided by this invention establishes a slurry discharge control model, which controls the solid content of vanadium-removing slurry within the range of process requirements with slight fluctuations, thereby improving the first-pass yield of refined titanium, greatly promoting the comprehensive utilization of titanium resources in the Panzhihua-Xichang region, and providing key technical support for the large-scale development and utilization of high-titanium blast furnace slag. Attached Figure Description

[0028] To better understand this application, reference can be made to the embodiments shown in the following figures. Components in the figures are not necessarily drawn to scale, and related elements may be omitted, or in some cases the scale may have been enlarged to emphasize and clearly illustrate the novel features described herein. Additionally, as is known in the art, system components may be arranged differently. Furthermore, in the figures, the same reference numerals denote corresponding parts throughout several views.

[0029] Figure 1 This is a schematic flowchart of a method for controlling the solid content of vanadium-removing slurry according to an embodiment of the present invention. Detailed Implementation

[0030] The following describes embodiments of this disclosure. However, it should be understood that the disclosed embodiments are merely examples, and other embodiments may take various alternative forms. The drawings are not necessarily drawn to scale; certain functions may be exaggerated or minimized to show detail of particular components. Therefore, the specific structural and functional details disclosed herein should not be construed as limiting, but merely as a representative basis for teaching those skilled in the art to use this application in various ways. As will be understood by those skilled in the art, various features shown and described with reference to any of the drawings may be combined with features shown in one or more other drawings to produce embodiments not explicitly shown or described. The combinations of features shown provide representative embodiments for typical applications. However, various combinations and modifications of features consistent with the teachings of this disclosure may be desirable for certain particular applications or implementations.

[0031] As mentioned in the background section, the inventors of this invention realized that the existing method of handling the solid content fluctuations of vanadium removal slurry in titanium tetrachloride removal operations based on individual experience could be further improved. Figure 1The flowchart shown illustrates a method for controlling the solid content of vanadium removal slurry. The preparation process begins at box 105, followed by the addition of high-vanadium titanium tetrachloride to the vanadium removal reactor at box 110. In one or more embodiments of the invention, the vanadium removal reactor can be a circulating pump tank. In one or more embodiments of the invention, the flow rate of high-vanadium titanium tetrachloride input into the titanium tetrachloride circulating pump tank is 7-8 t / h. In this step, the high-vanadium titanium tetrachloride is produced by low-temperature chlorination, and the impurity in the high-vanadium titanium tetrachloride is vanadium oxychloride.

[0032] Next, at frame 115, a mixed fatty acid is added to the vanadium removal reactor. In one or more embodiments of the present invention, the mixed fatty acid may be formulated from at least one of oleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, and docosahexaenoic acid, as well as at least one of palmitic acid, octanoic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, and arachidic acid. After the mixed fatty acid is added to the vanadium removal reactor, the temperature of the vanadium removal reactor is raised to between 140-160°C by a heating device. Furthermore, in one or more embodiments of the present invention, the mixed fatty acid is input into the vanadium removal reactor through the reflux pipe of the vaporization chamber of the carbon tetrachloride vanadium removal device. In one or more embodiments of the present invention, the amount of mixed fatty acid added is 0.04-0.08 t / h. In one embodiment, the mixed fatty acid is formulated from oleic acid and palmitic acid. The vanadium removal effect of the mixed fatty acid is mainly achieved through the carbon-carbon double bonds, α-H, and carboxyl groups in the mixed fatty acid; therefore, the amount of mixed fatty acid added is controlled by adjusting the molar amounts of carbon-carbon double bonds, α-H, and carboxyl groups. The molar ratio of carbon-carbon double bonds to α-H and carboxyl groups in the mixed fatty acids is: carbon-carbon double bonds : (α-H and carboxyl groups) = 0.6 to 0.75. In one embodiment, the molar ratio of carbon-carbon double bonds to α-H and carboxyl groups in the mixed fatty acids is: carbon-carbon double bonds : (α-H and carboxyl groups) = 0.7.

[0033] The process continues to frame 120, where the vanadium removal slurry discharge rate is calculated. Specifically, in one or more embodiments of the present invention, a slurry discharge rate control model is established based on the correlation between the crude titanium tetrachloride feed rate, the refined titanium tetrachloride collection rate, the impurity content of crude titanium tetrachloride, the density of crude titanium tetrachloride, the density of refined titanium tetrachloride, and the solid content of the vanadium removal slurry. The correlation between multiple parameters is determined by the following formula:

[0034] Where X represents the hourly discharge volume of vanadium slurry, in kg.

[0035] Y represents the solid content control value of the vanadium removal slurry, in g / L;

[0036] RV represents the mass percentage of vanadium oxychloride in crude titanium tetrachloride;

[0037] D and ρ are the solid content and density of crude titanium tetrachloride, respectively, in g / L and kg / m3.

[0038] L represents the hourly feed rate of crude titanium tetrachloride, expressed in kg.

[0039] γ is a correction coefficient, which is dimensionless.

[0040] The correction coefficient γ is an empirical coefficient, and its value range is related to the content of vanadium oxychloride in crude titanium tetrachloride, typically between 0.3 and 0.9. The empirical correspondence is shown in the table below:

[0041]

[0042] After establishing the aforementioned correlation and building an external discharge control model based on it, at box 125, the valves of the slurry tank's diversion pipeline are controlled by a controller according to the calculation results of the model, thereby achieving stable and effective control over the discharge volume of the vanadium-removing slurry. The vanadium-removing slurry can be continuously discharged through the discharge pipeline and fed into the titanium tetrachloride slurry transfer tank.

[0043] Subsequently, the entire method for controlling the solid content of vanadium removal slurry ends at frame 130.

[0044] In this application, the use of antonymous conjunctions is intended to include the conjunction itself. The use of definite or indefinite articles is not intended to indicate cardinality. Specifically, references to “the” object or to “a” and “one” objects are intended to indicate one of a plurality of such objects. Furthermore, the conjunction “or” may be used to convey simultaneous features rather than mutually exclusive schemes. In other words, the conjunction “or” should be understood as including “and / or”. The term “including” is inclusive and has the same scope as “contains”.

[0045] The above embodiments are possible examples of implementation methods of this application, and are provided only to enable those skilled in the art to clearly understand the principles of this application. Those skilled in the art should understand that the above discussion of any embodiment is merely exemplary and is not intended to imply that the scope of the embodiments disclosed in this application (including the claims) is limited to these examples; under the overall concept of this application, the technical features of the above embodiments or different embodiments can also be combined with each other, producing many other variations of different aspects of the embodiments of this application as described above, which are not provided in the specific implementation for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the embodiments of this application should be included within the scope of protection claimed by this application.

Claims

1. A method for controlling the solid content of vanadium-removing slurry, characterized in that, High-vanadium titanium tetrachloride was added to the vanadium removal reactor; Mixed fatty acids are added to the vanadium removal reactor; Calculate the discharge rate of vanadium removal slurry; The discharge of the vanadium removal slurry from the vanadium removal reactor is controlled based on the calculation results; The calculation of the vanadium removal slurry discharge includes: A mud discharge control model was established based on the correlation between crude titanium tetrachloride feed rate, refined titanium tetrachloride collection rate, crude titanium tetrachloride impurity content, crude titanium tetrachloride density, refined titanium tetrachloride density and vanadium removal mud solid content. The correlation is determined by the following formula: Where X represents the hourly discharge volume of vanadium slurry, in kg. Y represents the solid content control value of the vanadium removal slurry, in g / L; R V The mass percentage of vanadium oxychloride in crude titanium tetrachloride; D and ρ represent the solid content and density of crude titanium tetrachloride, respectively, in g / L and kg / m³. 3 ; L represents the hourly feed rate of crude titanium tetrachloride, expressed in kg. γ is a correction coefficient, which is dimensionless.

2. The method for controlling the solid content of vanadium-removing slurry according to claim 1, characterized in that, The vanadium removal reactor is a circulating pump tank.

3. The method for controlling the solid content of vanadium-removing slurry according to claim 1, characterized in that, The mixed fatty acids are formulated from at least one of oleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid, and docosahexaenoic acid, as well as at least one of palmitic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, and arachidic acid.

4. The method for controlling the solid content of vanadium-removing slurry according to claim 1, characterized in that, The mixed fatty acids are added, and then the temperature inside the vanadium removal reactor is maintained at 100–130°C.

5. The method for controlling the solid content of vanadium-removing slurry according to claim 1, characterized in that, The valves of the slurry tank's diversion pipeline are controlled by the controller based on the correlation formula, which calculates the discharge rate of the vanadium-removing slurry.

6. The method for controlling the solid content of vanadium-removing slurry according to claim 1, characterized in that, The fatty acids are fed into the vanadium removal reactor through a reflux pipe in the vaporization chamber.

7. The method for controlling the solid content of vanadium-removing slurry according to claim 2, characterized in that, The high-vanadium titanium tetrachloride is produced by low-temperature chlorination, and the flow rate of the high-vanadium titanium tetrachloride input into the circulating pump tank is 6-10 t / h, and the amount of mixed fatty acids added is 0.02-0.08 t / h.

8. The method for controlling the solid content of vanadium-removing slurry according to claim 7, characterized in that, The initial vanadium-removing titanium tetrachloride slurry in the circulating pump tank is continuously discharged through the slurry discharge pipe and fed into the titanium tetrachloride mud transfer tank.

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