Method and device for separating vanadium-containing slurry

By heating air in the combustion device and evaporate the vanadium-containing mud, rapid separation of vanadium-containing mud and effective recovery of resources are achieved, and the problems of long separation operation time and failure to effectively recover resources in the prior art are solved.

CN113666417BActive Publication Date: 2025-02-11PANGANG GROUP VANADIUM & TITANIUM RESOURCES CO LTD
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Patent Information

Application Number
CN202111069457.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-09-13
Publication Date
2025-02-11
Estimated Expiration
2041-09-13

AI Technical Summary

Technical Problem

In the prior art, the separation operation and treatment time of vanadium-containing mud is long, and the vanadium-containing substances cannot be effectively recovered, which affects the stable operation of the chlorination refining system and the comprehensive utilization of resources.

Method used

The combustion reaction and liquid evaporation occur in the combustion device using air heated to a predetermined temperature and a mist-shaped vanadium-containing slurry to obtain a gas-solid mixture, and the oxide solids of titanium tetrachloride gas and vanadium are separated to achieve vanadium-containing solids. Rapid separation of mud and efficient recycling of resources.

Benefits of technology

Through rapid combustion reaction, the separation operation time is shortened, and the effective and rapid separation of titanium tetrachloride and vanadium-containing substances is achieved, the rapid treatment of vanadium-containing mud is ensured, and the vanadium-containing substances are effectively recovered and utilized.

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Abstract

The present invention discloses a method and device for separating vanadium-containing mud, the method comprising: sending air heated to a predetermined temperature and mist-like vanadium-containing mud into a combustion device, wherein a combustion reaction and evaporation of liquid in the vanadium-containing mud occur in the combustion device to obtain a gas-solid mixture; and separating the gas-solid mixture to obtain separated gas and separated solid; wherein the combustion reaction comprises the reaction of carbon elements and vanadium elements in the vanadium-containing mud with oxygen in the air, respectively. The present invention can separate and recover titanium tetrachloride and vanadium-containing substances in the vanadium-containing mud, and can shorten the processing time of the separation operation to achieve rapid separation.
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Description

Technical Field

[0001] The invention relates to the technical field of chemical engineering, and in particular to a method and a device for separating vanadium-containing slurry. Background Art

[0002] Titanium tetrachloride is the main raw material for industrial products such as chloride-based titanium dioxide and titanium sponge. There are two main methods for producing titanium tetrachloride in the prior art: boiling chlorination and molten salt chlorination. Both methods involve the reaction of titanium dioxide-containing raw materials with chlorine at high temperatures to produce titanium tetrachloride. The titanium tetrachloride produced by the reaction contains a lot of impurities, mainly VOCl3, FeCl3, etc. It needs to enter the refining system for impurity removal and purification, and the purified vanadium-containing slurry needs to be discharged from the system in a timely manner. In addition, the vanadium-containing slurry contains titanium tetrachloride liquid and vanadium-containing substances, which need to be separated and reused.

[0003] At present, the common separation method is to use an evaporator for evaporation treatment or directly return it to the chlorination furnace. However, the evaporation treatment time of the evaporator is long, the production environment is bad, and it is not conducive to the stable operation of the chlorination refining system; if it is directly returned to the chlorination furnace, the vanadium-containing substances will directly enter the waste slag and cannot be comprehensively recycled.

[0004] Based on this, the existing technology still needs to be improved. Summary of the invention

[0005] The main purpose of the present invention is to provide a method and device for separating vanadium-containing slurry, so as to solve the problems of long separation operation processing time and inability to effectively recover vanadium-containing substances in the prior art.

[0006] According to one aspect of the present invention, a method for separating vanadium-containing mud is proposed, comprising: feeding air heated to a predetermined temperature and mist-like vanadium-containing mud into a combustion device, wherein a combustion reaction and evaporation of liquid in the vanadium-containing mud occur in the combustion device to obtain a gas-solid mixture; and separating the gas-solid mixture to obtain separated gas and separated solid; wherein the combustion reaction includes reactions of carbon element and vanadium element in the vanadium-containing mud with oxygen in the air, respectively.

[0007] According to one embodiment of the present invention, a predetermined amount of the air is first introduced into the combustion device, and then the air and the vanadium-containing slurry are introduced simultaneously.

[0008] According to one embodiment of the present invention, the predetermined temperature is above 400° C.; and / or the mass ratio of the air fed into the combustion device to the vanadium-containing slurry is 1 to 1.5:1.

[0009] According to one embodiment of the present invention, the vanadium-containing slurry includes titanium tetrachloride liquid, and the method further includes: sending the separated gas to a chlorination condensation system to collect titanium tetrachloride.

[0010] According to one embodiment of the present invention, the separated solid includes vanadium oxide, and the method further includes: sending the separated solid to a production system of ferrovanadium products.

[0011] According to another aspect of the present invention, a vanadium-containing mud separation device is proposed, comprising: an air heating device, provided with a first air inlet and a first air outlet, the first air outlet discharges air heated to a predetermined temperature; a combustion device, provided with a second air inlet, a vanadium-containing mud inlet and a gas-solid mixture outlet, the second air inlet is connected to the first air outlet, a spray device is provided at the vanadium-containing mud inlet, a combustion reaction and evaporation of the liquid in the vanadium-containing mud occur in the combustion device; a gas-solid separation device, provided with a gas-solid mixture inlet, a gas outlet and a solid outlet, the gas-solid mixture inlet is connected to the gas-solid mixture outlet.

[0012] According to one embodiment of the present invention, the second air inlet is opened before the vanadium-containing slurry inlet.

[0013] According to one embodiment of the present invention, the mass ratio of the air entering from the second air inlet to the vanadium-containing slurry entering from the vanadium-containing slurry inlet is 1-1.5:1.

[0014] According to one embodiment of the present invention, the gas outlet is connected to a chlorination condensation system; and / or the solid outlet is connected to a vanadium slag collection device.

[0015] According to one embodiment of the present invention, a fan is provided at the first air inlet; and / or the gas-solid separation device is a cyclone dust collector.

[0016] In the vanadium-containing mud separation method according to an embodiment of the present invention, when the hot air heated to a predetermined temperature and the mist-like vanadium-containing mud contact in the combustion device, a combustion reaction occurs, and the combustion reaction includes the reaction of the carbon element and the vanadium element in the vanadium-containing mud with the oxygen in the hot air, respectively, so that on the one hand, the liquid (such as titanium tetrachloride liquid) in the vanadium-containing mud can be evaporated to form gas through the heat release of the combustion reaction and the heat provided by the hot air, and on the other hand, the vanadium element in the vanadium-containing mud is oxidized to vanadium oxide, which exists in solid form. After that, by separating the gas-solid mixture, a gas containing titanium tetrachloride and a solid containing vanadium oxide can be obtained respectively, thereby separating the titanium tetrachloride and the vanadium-containing substance in the vanadium-containing mud, and the vanadium-containing substance is separated in the form of vanadium oxide, which is convenient for recycling. In addition, the combustion reaction is carried out at an extremely fast speed, which is conducive to shortening the time of the separation operation, realizing the effective and rapid separation of titanium tetrachloride and vanadium-containing substances, and ensuring that the vanadium-containing mud is quickly processed. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 A schematic diagram of a vanadium-containing slurry separation device according to an exemplary embodiment of the present invention is shown. DETAILED DESCRIPTION

[0019] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the embodiments of the present invention are further described in detail below in combination with specific embodiments and with reference to the accompanying drawings.

[0020] It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are for distinguishing two non-identical entities with the same name or non-identical parameters. It can be seen that "first" and "second" are only for the convenience of expression and should not be understood as limitations on the embodiments of the present invention. The subsequent embodiments will not explain this one by one.

[0021] Figure 1 A schematic diagram of a vanadium-containing slurry separation device according to an exemplary embodiment of the present invention is shown. Figure 1 As shown, the vanadium-containing mud separation device includes:

[0022] The air heating device 10 is provided with a first air inlet 12 and a first air outlet 14, and the first air outlet 14 discharges air heated to a predetermined temperature;

[0023] A combustion device 20 is provided with a second air inlet 22, a vanadium-containing slurry inlet 24 and a gas-solid mixture outlet 26, wherein the second air inlet 22 is connected to the first air outlet 14, a spray device 21 is provided at the vanadium-containing slurry inlet 24, and a combustion reaction and evaporation of liquid in the vanadium-containing slurry occur in the combustion device 20; and

[0024] The gas-solid separation device 30 is provided with a gas-solid mixture inlet 32 ​​, a gas outlet 34 and a solid outlet 36 . The gas-solid mixture inlet 32 ​​is connected to the gas-solid mixture outlet 26 .

[0025] The air heating device 10 may be any device capable of heating air, and a heating component is provided in the air heating device 10 to heat the air. The first air inlet 12 may be connected to the atmosphere to input air to be heated into the air heating device 10. A fan 11 may be provided at the first air inlet 12 to send external air into the air heating device 10 through the first air inlet 12. The air heating device 10 heats the air input from the first air inlet 12 to a predetermined temperature, and then the air heated to the predetermined temperature is discharged from the first air outlet 14 and enters the combustion device 20 through the second air inlet 22.

[0026] The spray device 21 provided in the combustion device 20 can form the vanadium-containing mud into a mist form, and then the mist-containing vanadium-containing mud is sent into the combustion device 20 through the vanadium-containing mud inlet 24, and contacts with the air heated to a predetermined temperature entering the combustion device 20 through the second air inlet 22, so as to initiate a combustion reaction. Since the vanadium-containing mud is in a mist form and the air is heated to a predetermined temperature, the two can be directly burned after contact without other auxiliary operations. In one embodiment of the present invention, the predetermined temperature is above 400°C to ensure that the air at this temperature can be quickly and effectively burned after contacting the mist-containing vanadium mud. The second air inlet 22 and the vanadium-containing mud inlet 24 can be arranged at the lower part of the combustion device 20, and the gas-solid mixture outlet 26 can be arranged at the upper part of the combustion device 20. During the combustion and evaporation process, the gas-solid mixture outlet 26 can be kept in an open state, so that the entire separation process of the vanadium-containing mud can be carried out continuously. In an embodiment of the present invention, the spray device 21 includes a plurality of spray holes, the aperture of which is 3 to 5 mm, suitable for inputting a desired amount of vanadium-containing mud.

[0027] The combustion reaction may include the reaction of the carbon element and the vanadium element in the vanadium-containing slurry with the oxygen in the air respectively. The vanadium-containing slurry may be a slurry produced by refining titanium tetrachloride using organic matter. The vanadium-containing slurry is a solid-liquid mixture, wherein the liquid contains titanium tetrachloride liquid; the solid contains carbon element from organic matter, and also contains vanadium chloride (such as VCl3) and / or vanadium chloride oxide (VOCl2) generated by the refining process of VOCl3 impurities in crude titanium tetrachloride, and may also contain FeCl3 and the like. The carbon element undergoes a rapid and violent oxidation reaction with oxygen in the air heated to a predetermined temperature to generate CO2 and release a large amount of heat. The vanadium chloride and / or vanadium chloride oxide also undergo a violent oxidation reaction with oxygen to generate vanadium oxide (mainly V2O5) and release a large amount of heat. The titanium tetrachloride liquid in the vanadium-containing slurry evaporates into a gaseous form through the heat released by the combustion reaction and the heat provided by the air heated to a predetermined temperature. After the combustion reaction and the evaporation of the liquid, a gas-solid mixture is formed in the combustion device 20, wherein the gas components are mainly TiCl4, CO2, N2, etc., and the solid substances are mainly V2O5, FeCl3, etc. The combustion reaction proceeds very quickly, usually in seconds, which can greatly shorten the processing time and improve the efficiency compared with the evaporation treatment method of the prior art (usually takes several days).

[0028] In one embodiment of the present invention, the second air inlet 22 is opened before the vanadium-containing mud inlet 24, that is, a predetermined amount of heated hot air can be first introduced into the combustion device 20, and then the hot air and the vanadium-containing mud are simultaneously introduced. Thus, firstly, the temperature in the cavity of the combustion device 20 can be raised to, for example, above 300° C. by adding hot air, and then the vanadium-containing mud can be directly evaporated and burned after entering.

[0029] In one embodiment of the present invention, the mass ratio of the hot air entering from the second air inlet 22 to the vanadium-containing mud entering from the vanadium-containing mud inlet 24 is 1 to 1.5: 1, so as to ensure that the oxygen in the hot air fully reacts with the carbon element in the vanadium-containing mud and ensure that the combustion reaction is fully carried out at a certain intensity. Among them, the mass of the air can be calculated based on the volume and density of the air. The amount of air and vanadium-containing mud added can be controlled by, for example, a volume flow meter and / or a mass flow meter. For example, the amount of air added can be controlled by a volume flow meter, and the mass of the air can be converted into the volume and density of the air. An air flow regulating unit can be provided between the first air outlet 14 and the second air inlet 22; the spray device 21 can be provided with a spray flow regulating unit, and the spray flow regulating unit can adjust the spray flow by changing the pressure and / or the nozzle aperture.

[0030] The gas-solid separation device 30 can be any device that can be used to separate gas-solid mixtures. In one embodiment, the gas-solid separation device 30 is a cyclone dust collector, which uses the centrifugal force in a high-speed rotating airflow to separate solid matter from the gas. The separated gas contains TiCl4, CO2, N2, etc. The gas outlet 34 can be further connected to a chlorination condensation system to collect titanium tetrachloride in the gas by condensation elution. The separated solid contains V2O5, FeCl3, etc. The solid outlet 36 can be further connected to a vanadium slag collection device 40 through a rotary valve. By opening the rotary valve, the separated solid in the gas-solid separation device 30 enters the vanadium slag collection device 40 for storage, and after being stored to a certain amount, it is sent to a vanadium processing system to produce ferrovanadium and other products as raw materials, such as 50 ferrovanadium with a vanadium content of about 50%.

[0031] According to another aspect of the present invention, a method for separating vanadium-containing slurry is provided, comprising:

[0032] sending air heated to a predetermined temperature and a mist-like vanadium-containing slurry into a combustion device, wherein a combustion reaction and evaporation of liquid in the vanadium-containing slurry occur in the combustion device to obtain a gas-solid mixture; and

[0033] Separating the gas-solid mixture to obtain separated gas and separated solid;

[0034] The combustion reaction includes the reaction of the carbon element and the vanadium element in the vanadium-containing slurry with the oxygen in the air respectively.

[0035] In the vanadium-containing mud separation method according to an embodiment of the present invention, when the hot air heated to a predetermined temperature and the mist-like vanadium-containing mud contact in the combustion device, a combustion reaction occurs, and the combustion reaction includes the reaction of the carbon element and the vanadium element in the vanadium-containing mud with the oxygen in the hot air, respectively, so that on the one hand, the liquid (such as titanium tetrachloride liquid) in the vanadium-containing mud can be evaporated to form gas through the heat release of the combustion reaction and the heat provided by the hot air, and on the other hand, the vanadium element in the vanadium-containing mud is oxidized to vanadium oxide, which exists in solid form. After that, by separating the gas-solid mixture, a gas containing titanium tetrachloride and a solid containing vanadium oxide can be obtained respectively, thereby separating the titanium tetrachloride and the vanadium-containing substance in the vanadium-containing mud, and the vanadium-containing substance is separated in the form of vanadium oxide, which is convenient for recycling. In addition, the combustion reaction is carried out at an extremely fast speed, which is conducive to shortening the time of the separation operation, realizing the effective and rapid separation of titanium tetrachloride and vanadium-containing substances, and ensuring that the vanadium-containing mud is quickly processed.

[0036] In one embodiment, a predetermined amount of air is first introduced into the combustion device, and then the air and the vanadium-containing slurry are introduced simultaneously. Thus, the temperature in the cavity of the combustion device can be raised to above 300° C. by the addition of hot air, and then the vanadium-containing slurry can be directly evaporated and burned after entering.

[0037] In one embodiment of the present invention, the predetermined temperature is above 400° C. to ensure that the air at this temperature can burn quickly and effectively after contacting the misty vanadium-containing slurry.

[0038] In one embodiment of the present invention, the mass ratio of the air fed into the combustion device to the vanadium-containing slurry is 1-1.5:1, thereby ensuring that the oxygen in the hot air fully reacts with the carbon element in the vanadium-containing slurry and that the combustion reaction is fully carried out at a certain intensity.

[0039] In one embodiment of the present invention, the vanadium-containing slurry includes titanium tetrachloride liquid, and the method further includes: sending the separated gas to a chlorination condensation system to collect titanium tetrachloride.

[0040] In one embodiment of the present invention, the separated solid includes vanadium oxide, and the method further includes: sending the separated solid to a production system of ferrovanadium products.

[0041] The present invention proposes a drying and separation process for refining vanadium-containing sludge from titanium tetrachloride, which can provide an efficient evaporation separation method, realize the effective and rapid separation of titanium tetrachloride and vanadium-containing substances, ensure the rapid treatment of the vanadium-containing sludge, and effectively recover the vanadium-containing substances in the vanadium-containing sludge, and has great promotion prospects in the titanium tetrachloride production industry.

[0042] It should be particularly pointed out that the various components or steps in the above-mentioned embodiments can be cross-linked, replaced, added, or deleted with each other. Therefore, the combinations formed by these reasonable arrangements and combinations should also fall within the scope of protection of the present invention, and the scope of protection of the present invention should not be limited to the embodiments.

[0043] The above are exemplary embodiments disclosed in the present invention. The order disclosed in the above embodiments of the present invention is for description only and does not represent the advantages and disadvantages of the embodiments. However, it should be noted that the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope disclosed in the embodiments of the present invention (including the claims) is limited to these examples. Various changes and modifications may be made without departing from the scope defined in the claims. The functions, steps and / or actions of the method claims according to the disclosed embodiments described herein do not need to be performed in any particular order. In addition, although the elements disclosed in the embodiments of the present invention may be described or required in individual form, they may also be understood as multiple unless explicitly limited to the singular.

[0044] A person skilled in the art should understand that the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope of the disclosure of the embodiments of the present invention (including the claims) is limited to these examples; under the concept of the embodiments of the present invention, the technical features in the above embodiments or different embodiments can also be combined, and there are many other changes in different aspects of the embodiments of the present invention as described above, which are not provided in detail for the sake of simplicity. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the embodiments of the present invention should be included in the protection scope of the embodiments of the present invention.

Claims

1. A method for separating vanadium-containing slurry, comprising: sending air heated to a predetermined temperature and a mist-like vanadium-containing slurry into a combustion device, wherein a combustion reaction and evaporation of liquid in the vanadium-containing slurry occur in the combustion device to obtain a gas-solid mixture; and Separating the gas-solid mixture to obtain separated gas and separated solid; The combustion reaction includes the reaction of the carbon element and the vanadium element in the vanadium-containing slurry with the oxygen in the air respectively; The predetermined temperature is above 400° C., so that the mass ratio of the air fed into the combustion device to the vanadium-containing slurry is 1 to 1.5:

1.

2. The method according to claim 1, characterized in that First, a predetermined amount of the air is fed into the combustion device, and then the air and the vanadium-containing slurry are fed into the combustion device simultaneously.

3. The method according to claim 1, characterized in that The vanadium-containing slurry includes titanium tetrachloride liquid, and the method further includes: sending the separated gas to a chlorination condensation system to collect titanium tetrachloride.

4. The method according to claim 1, characterized in that: The separated solids include vanadium oxides, and the method further includes: sending the separated solids to a production system of ferrovanadium products.

5. A vanadium-containing slurry separation device, comprising: an air heating device having a first air inlet and a first air outlet, wherein the first air outlet discharges air heated to a predetermined temperature; A combustion device, provided with a second air inlet, a vanadium-containing mud inlet and a gas-solid mixture outlet, wherein the second air inlet is connected to the first air outlet, a spray device is provided at the vanadium-containing mud inlet, and a combustion reaction and evaporation of liquid in the vanadium-containing mud occur in the combustion device; as well as A gas-solid separation device, provided with a gas-solid mixture inlet, a gas outlet and a solid outlet, wherein the gas-solid mixture inlet is connected to the gas-solid mixture outlet; Wherein, the predetermined temperature is above 400° C.; and the mass ratio of the air entering from the second air inlet to the vanadium-containing slurry entering from the vanadium-containing slurry inlet is 1 to 1.5:

1.

6. The device according to claim 5, characterized in that The second air inlet is opened before the vanadium-containing slurry inlet.

7. The device according to claim 5, characterized in that The gas outlet is connected to a chlorination condensation system; and / or the solid outlet is connected to a vanadium slag collection device.

8. The device according to claim 5, characterized in that A fan is provided at the first air inlet; and / or the gas-solid separation device is a cyclone dust collector.

Citation Information

Patent Citations

  • Drying method of titanium tetrachloride settling mud

    CN102092783A

  • Vanadium-containing slurry separation device

    CN216155497U