A device and method for beating vanadium removal residue of titanium tetrachloride organic matter

Abstract

The application provides a titanium tetrachloride organic vanadium-removing residue pulping device and method, which comprises the following: a mineral pulp evaporation furnace is vertically connected to the top of a pulping tank through a residue discharge pipe at the bottom; the mineral pulp evaporation furnace can discharge residue into the pulping tank through the residue discharge pipe; a clear liquid tank is used to provide alkali liquor to the pulping tank; a waste gas spraying nipple is arranged at the top of the pulping tank; the inlet of a pulping spraying pump is communicated with the pulping tank, and the outlet is respectively communicated with the residue discharge pipe, the top of the pulping tank and the waste gas spraying nipple; the waste gas spraying nipple and the top of the clear liquid tank are communicated through a first breathing pipe; the outlet of a clear liquid conveying pump is communicated with the pulping tank; the outlet of a first clear liquid spraying pump is communicated with the first breathing pipe; and the outlet of a second clear liquid spraying pump is respectively communicated with the clear liquid tank and a second breathing pipe. The application ensures the environmental protection, safety and high efficiency of titanium tetrachloride organic vanadium-removing residue discharge and collection treatment.

Description

Technical Field

[0001] This invention relates to the field of titanium tetrachloride production technology, and more particularly to a pulping device and method for removing vanadium residue from organic titanium tetrachloride. Background Technology

[0002] Titanium tetrachloride is an important intermediate product in titanium industry production. Based on impurity content, it can be divided into crude titanium tetrachloride and refined titanium tetrachloride. Crude titanium tetrachloride is a primary product obtained by reacting titanium-rich materials, petroleum coke, and chlorine in a chlorination furnace, followed by dust removal, washing, and condensation. It has a relatively high impurity content and is generally referred to as crude titanium tetrachloride. After vanadium removal from crude titanium tetrachloride, or further removal of high-boiling-point and low-boiling-point impurities as needed, pure titanium tetrachloride with a TiCl4 content greater than 99.8% is obtained, which can be used to produce chloride-process titanium dioxide and sponge titanium. Currently, organic vanadium removal processes are commonly used in China to purify crude titanium tetrachloride. The slurry generated during the vanadium removal process needs to be recovered, as it contains more than 90% TiCl4. In addition, the vanadium removal slurry also contains vanadium chloride and chloride oxides, which can be recycled as high-value-added vanadium resources.

[0003] Domestic titanium industry enterprises typically employ electric furnace evaporation to recover vanadium compounds from vanadium removal slurry. This process involves distilling off TiCl4 and its low-boiling-point impurities at temperatures between 130-400℃, recovering them as crude titanium tetrachloride. The remaining dried residue is discharged from the bottom of the furnace and used as a vanadium-containing raw material for further vanadium extraction. The main components of the dried residue include carbonaceous dust, TiO2, FeCl3, and AlCl3. The carbonaceous dust has numerous micropores, which increase its specific surface area, leading to smoldering at around 50℃. Smoldering is a form of solid combustion characterized by slow, invisible combustion, typically producing smoke and a rise in temperature. Furthermore, the carbonaceous dust ignites rapidly upon contact with air at around 100℃. During the discharge of the dried residue from the bottom of the furnace, the residue temperature is generally above 100℃. Using open containers to receive the residue poses a significant safety hazard to production operators, can damage equipment and facilities, and may even cause a fire. Therefore, ensuring the environmental friendliness, safety, and efficiency of the discharge, collection, and treatment of vanadium removal residues from titanium tetrachloride organic matter has become an urgent problem to be solved in the fields of titanium metallurgy and chemical technology. Summary of the Invention

[0004] To ensure the environmental friendliness, safety, and efficiency of the discharge, collection, and treatment of vanadium removal residue from titanium tetrachloride organic matter, this invention proposes a pulping device and method for vanadium removal residue from titanium tetrachloride organic matter.

[0005] The technical means employed in this invention are as follows:

[0006] A slurrying device for removing vanadium residue from titanium tetrachloride organic compounds includes a slurrying tank, a slurry spray pump, a clear liquid tank, a clear liquid transfer pump, a first clear liquid spray pump, and a second clear liquid spray pump.

[0007] The slurry evaporator is vertically connected to the top of the pulping tank via a slag discharge pipe at the bottom, and a slag discharge valve is installed on the slag discharge pipe; the slurry evaporator can discharge residue into the pulping tank through the slag discharge pipe; the clear liquid tank is used to supply alkali solution to the pulping tank;

[0008] The top of the pulping tank is equipped with a waste gas spray section; the inlet of the pulping spray pump is connected to the pulping tank, and the outlet is connected to the slag discharge pipe, the top of the pulping tank, and the waste gas spray section through the first pulping spray pipe, the second pulping spray pipe, and the third pulping spray pipe, respectively; the waste gas spray section is connected to the top of the clear liquid tank through a first breather pipe;

[0009] The inlets of the clear liquid transfer pump, the first clear liquid spray pump, and the second clear liquid spray pump are respectively connected to the bottom of the clear liquid tank; the outlet of the clear liquid transfer pump is connected to the top of the pulping tank through a clear liquid transfer pipe; the outlet of the first clear liquid spray pump is connected to the inlet of the first breathing pipe through a first clear liquid spray pipe; the outlet of the second clear liquid spray pump is connected to the top of the clear liquid tank and the inlet of the second breathing pipe through a second clear liquid spray pipe and a third clear liquid spray pipe, respectively; the waste gas in the clear liquid tank enters the waste gas scrubbing system through the second breathing pipe.

[0010] Furthermore, it also includes an alkali pipe for replenishing alkali solution to the clear liquid tank and a new water pipe for replenishing new water to the clear liquid tank; the alkali pipe is connected to the top of the clear liquid tank; the new water pipe is connected to the second breathing pipe through 3-4 equally spaced spray branch pipes, and is evenly distributed in the middle and outlet end of the second breathing pipe, and a spiral nozzle is provided at the outlet end of the spray branch pipe.

[0011] Furthermore, the bottom of the pulping tank is provided with a liquid outlet, and the inlet of the pulping spray pump is connected to the liquid outlet through a pipe; the bottom surface inside the pulping tank is a 5-10° downward slope facing the side where the liquid outlet is located, and the bottom of the slope is lower than the liquid outlet. The sloped bottom design facilitates the discharge of slurry in the pulping tank; the outlet of the pulping spray pump is also provided with a slurry discharge pipe, which is used to discharge the uniformly mixed slurry inside the pulping tank into a collection container.

[0012] Furthermore, the outlet of the first slurry spray pipe is connected to the middle of the slag discharge pipe, and a nozzle is provided at the outlet end of the first slurry spray pipe.

[0013] Furthermore, the outlet of the second pulping spray pipe is provided with 3-4 spray branch pipes extending into the pulping tank, and they are evenly distributed in the middle area of ​​the top of the pulping tank; the outlet end of the spray branch pipe is provided with a nozzle.

[0014] Furthermore, the exhaust gas spray section is located at the top of the pulping tank near the edge of the tank wall; the inner diameter of the exhaust gas spray section is 200-400mm; the exhaust gas spray section is used to draw out the exhaust gas in the pulping tank to ensure that the pulping tank is under negative pressure; the outlet of the third pulping spray pipe is connected to the outlet of the exhaust gas spray section, and a nozzle is provided at the outlet end of the third pulping spray pipe.

[0015] Furthermore, the outlet of the first clear liquid spray pipe is connected to the first breathing pipe through 2-4 spray branch pipes arranged at equal intervals; a nozzle is provided at the outlet end of the spray branch pipe; the first breathing pipe is provided with a horizontal section and a vertical section from the inlet end to the outlet end, the horizontal section is inclined at 5-15° relative to the horizontal direction, and one end of the horizontal section near the outlet end of the first breathing pipe is lower than the other end.

[0016] Furthermore, the second clear liquid spray pipe is provided with 3-4 spray branch pipes extending into the clear liquid tank, and evenly distributed in the middle area of ​​the top of the clear liquid tank; the outlet end of the spray branch pipe is provided with a nozzle.

[0017] Furthermore, the outlet of the third clear liquid spray pipe is connected to the second breathing pipe through 2-4 spray branch pipes arranged at equal intervals; a nozzle is provided at the outlet end of the spray branch pipe; the second breathing pipe is inclined at 5-15° relative to the horizontal direction, and the outlet end of the second breathing pipe is higher than the inlet end.

[0018] This invention also provides a method for pulping vanadium removal residue from titanium tetrachloride organic compounds, employing the aforementioned pulping device, specifically including the following steps:

[0019] A. Add alkali solution (30% NaOH solution) to the clear liquid tank through the alkali solution pipe, and then add fresh water to the clear liquid tank through the fresh water pipe. The volume ratio of alkali solution to fresh water is 1:1 to 2:1.

[0020] B. Start the second clear liquid spray pump to circulate the alkaline solution and fresh water in the clear liquid tank through the second and third clear liquid spray pipes, and mix the alkaline solution and fresh water in the clear liquid tank evenly.

[0021] C. Start the clear liquid transfer pump to transfer the alkaline solution that is evenly mixed with fresh water to the pulping tank. The ratio of the volume of alkaline solution added to the pulping tank to the volume of residue discharged from the slurry evaporator in each batch is 10:1.

[0022] D. Start the first clear liquid spray pump to circulate and spray alkaline solution through the first breathing tube;

[0023] E. Start the pulping spray pump, and simultaneously circulate alkaline solution through the first pulping spray pipe, the second pulping spray pipe and the third pulping spray pipe to spray alkaline solution onto the slag discharge pipe, the top of the pulping tank and the exhaust gas spray section.

[0024] F. Open the slag discharge valve of the slurry evaporator and discharge a batch of residue into the pulping tank to mix thoroughly with the alkali solution;

[0025] G. Close the slag discharge valve of the slurry evaporator. After the slurry spray pump has been running for 1-2 hours, open the valve on the slurry discharge pipe to transfer the evenly mixed slurry in the slurry tank to the collection container. This completes the slurry treatment of one batch of residue. The next batch of residue will be slurryed through the cyclic step AG.

[0026] Compared with the prior art, the present invention has the following advantages:

[0027] The titanium tetrachloride organic vanadium removal residue pulping device and method provided by the present invention can mix the residue of the slurry evaporator with alkaline solution under closed conditions to form a slurry. The carbon-containing dust generated during the pulping process is fully washed to prevent combustion due to contact with air. At the same time, it reduces the deposition and adhesion of carbon-containing dust in the breathing pipe, stabilizes the air pressure of the pulping device, greatly reduces the labor intensity of manually cleaning the breathing pipe, and significantly improves the on-site working environment and safety control level.

[0028] Based on the above reasons, this invention can be widely promoted in the field of titanium tetrachloride production. Attached Figure Description

[0029] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0030] Figure 1 This is a schematic diagram of the overall process flow of the vanadium removal residue pulping device of the present invention.

[0031] Figure 2 This is a partial process flow diagram of the pulping tank of the present invention.

[0032] Figure 3 This is a partial process flow diagram of the clear liquid tank of the present invention.

[0033] In the diagram: 1. Slurry evaporator; 11. Slag discharge valve; 12. Slag discharge pipe; 2. Slurry tank; 21. Slurry spray pump; 22. First slurry spray pipe; 23. First breathing pipe; 24. Second slurry spray pipe; 25. Third slurry spray pipe; 26. Waste gas spray section; 27. Slurry discharge pipe; 28. Agitator; 3. Clarified liquid tank; 31. Clarified liquid transfer pump; 32. Clarified liquid transfer pipe; 33. First clear liquid spray pump; 34. First clear liquid spray pipe; 35. Second clear liquid spray pump; 36. Second clear liquid spray pipe; 37. Third clear liquid spray pipe; 38. Second breathing pipe; 4. Alkali solution pipe; 5. Fresh water pipe. Detailed Implementation

[0034] It should be noted that, unless otherwise specified, the embodiments and features described in the present invention can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0035] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0036] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of exemplary embodiments according to the invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0037] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps set forth in these embodiments do not limit the scope of the invention. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following figures denote similar items; therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.

[0038] In the description of this invention, it should be understood that the orientation or positional relationship indicated by directional terms such as "front, back, up, down, left, right", "horizontal, vertical, horizontal" and "top, bottom" is generally based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing this invention and simplifying the description. Unless otherwise stated, these directional terms do not indicate or imply that the device or element referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the scope of protection of this invention. The directional terms "inner" and "outer" refer to the inner and outer contours relative to the outline of each component itself.

[0039] For ease of description, spatial relative terms such as "above," "over," "on the upper surface of," "above," etc., are used herein to describe the spatial positional relationship of a device or feature as shown in the figures to other devices or features. It should be understood that spatial relative terms are intended to encompass different orientations in use or operation besides the orientation of the device as described in the figures. For example, if the device in the figures is inverted, a device described as "above" or "above" other devices or structures would subsequently be positioned as "below" or "under" other devices or structures. Thus, the exemplary term "above" can include both "above" and "below." The device may also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatial relative descriptions used herein will be interpreted accordingly.

[0040] Furthermore, it should be noted that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore should not be construed as limiting the scope of protection of this invention.

[0041] Example 1

[0042] like Figure 1 As shown, the present invention provides a slurrying device for removing vanadium residue from titanium tetrachloride organic matter, including a slurrying tank 2, a slurry spray pump 21, a clear liquid tank 3, a clear liquid transfer pump 31, a first clear liquid spray pump 33, and a second clear liquid spray pump 35.

[0043] The slurry evaporator 1 is vertically connected to the top of the pulping tank 2 via a slag discharge pipe 12 at the bottom; the slurry evaporator 1 can discharge residue into the pulping tank 2 through the slag discharge pipe 12; the clear liquid tank 3 is used to supply alkaline solution to the pulping tank 2;

[0044] The top of the pulping tank 2 is provided with an exhaust gas spray section 26; the inlet of the pulping spray pump 21 is connected to the pulping tank 2, and the outlet is connected to the slag discharge pipe 12, the top of the pulping tank 2 and the exhaust gas spray section 26 through the first pulping spray pipe 22, the second pulping spray pipe 24 and the third pulping spray pipe 25 respectively; the exhaust gas spray section 26 is connected to the top of the clear liquid tank 3 through the first breather pipe 23;

[0045] The inlets of the clear liquid transfer pump 31, the first clear liquid spray pump 33, and the second clear liquid spray pump 35 are respectively connected to the bottom of the clear liquid tank 3; the outlet of the clear liquid transfer pump 31 is connected to the top of the pulping tank 2 through the clear liquid transfer pipe 32; the outlet of the first clear liquid spray pump 33 is connected to the inlet of the first breathing pipe 23 through the first clear liquid spray pipe 34; the outlet of the second clear liquid spray pump 35 is connected to the top of the clear liquid tank 3 and the inlet of the second breathing pipe 38 through the second clear liquid spray pipe 36 and the third clear liquid spray pipe 37 respectively; the waste gas in the clear liquid tank 3 enters the waste gas scrubbing system through the second breathing pipe 38.

[0046] Furthermore, a slag discharge valve 11 is installed on the slag discharge pipe 12.

[0047] Furthermore, it also includes an alkali pipe 4 for replenishing the clear liquid tank 3 with alkali solution (30% NaOH solution) and a new water pipe 5 for replenishing the clear liquid tank 3 with new water; the alkali pipe 4 is connected to the top of the clear liquid tank 3, and the alkali solution provided by the alkali pipe 4 comes from the alkali pipe network; the new water pipe 5 is connected to the second breathing pipe 38, and the new water provided by the new water pipe 5 comes from the new water pipe network.

[0048] Furthermore, the waste gas scrubbing system is used to deeply scrub the waste gas after it has been treated by the pulping device of the present invention, so as to ensure that the treated waste gas can meet the emission standards. The waste gas scrubbing system can adopt equipment with good absorption effect for HCl and Cl2 gases in the prior art.

[0049] Furthermore, after liquid is introduced into the pulping tank 2 and the clear liquid tank 3, a liquid phase zone and a gas phase zone located above the liquid phase zone are formed; the outlets of the slag discharge pipe 12, the second pulping spray pipe 24, and the clear liquid conveying pipe 32 are all connected to the gas phase zone located at the top of the pulping tank 2; the exhaust gas spray section 26 is used to connect the gas phase zones in the pulping tank 2 and the clear liquid tank 3; the outlets of the alkali pipe 4 and the second clear liquid spray pipe 36, as well as the inlet of the second breathing pipe 38, are all connected to the gas phase zone located at the top of the clear liquid tank 3.

[0050] Furthermore, the bottom of the pulping tank 2 is provided with a liquid outlet, and the inlet of the pulping spray pump 21 is connected to the liquid outlet through a pipe; the bottom surface inside the pulping tank 2 is a sloped downward at 5-10° towards the side where the liquid outlet is located, and the bottom of the sloped surface is lower than the liquid outlet. The sloped bottom surface design can facilitate the discharge of slurry in the pulping tank 2; the outlet of the pulping spray pump 21 is also provided with a slurry discharge pipe 27, which is used to discharge the uniformly mixed slurry inside the pulping tank 2 into a collection container.

[0051] Furthermore, the pulping tank 2 is equipped with a stirrer 28, which has 1-2 layers of blades. The specific number of blade layers can be determined according to the height of the pulping tank 2. In this embodiment, the stirrer 28 has 2 layers of blades. During the pulping process, the stirrer 28 operates continuously, which can prevent the mud from settling at the bottom of the pulping tank 2 and also accelerate the mixing efficiency of the vanadium removal residue and the alkaline solution.

[0052] Furthermore, the top of the pulping tank 2 is equipped with a level gauge, a pressure gauge, and a thermocouple for monitoring the liquid level, pressure, and temperature, respectively. Based on the monitoring results of the level gauge, the operator can be reminded that a certain amount of alkali solution has been added or a certain amount of slurry has been discharged. When the pressure gauge detects that the pressure has reached the upper limit of the control, the operator can be reminded to stop discharging slag into the pulping tank 2 to ensure operational safety. When the thermocouple detects that the temperature exceeds room temperature and continues to rise, the operator can be reminded that vanadium slag has been discharged into the pulping tank 2.

[0053] Furthermore, the outlet of the first slurry spray pipe 22 is connected to the middle of the slag discharge pipe 12, and a nozzle is provided at the outlet end of the first slurry spray pipe 22. This allows the vanadium removal residue to be pre-mixed with the alkaline solution during the slag discharge process and reduces the temperature of the vanadium removal residue. To prevent the nozzle from being blocked or burned by the mud, the nozzle structure can be a stainless steel spiral type, or other nozzles that are resistant to solid particles and high temperature can be selected.

[0054] Furthermore, the outlet of the second pulping spray pipe 24 is provided with 3-4 spray branch pipes extending into the pulping tank 2, and they are evenly distributed in the middle area of ​​the top of the pulping tank 2. The specific number of spray branch pipes is determined according to the diameter of the pulping tank 2. In this embodiment, 4 spray branch pipes are provided. The outlet end of the spray branch pipe is provided with a stainless steel spiral nozzle, which can make the vanadium removal residue and alkaline solution fully mixed in the pulping tank 2, reducing the amount of carbon-containing dust entering the first breathing pipe 23.

[0055] Furthermore, the exhaust gas spray section 26 is located at the top of the pulping tank 2 near the edge of the tank wall; the inner diameter of the exhaust gas spray section 26 is 200-400mm; the exhaust gas spray section 26 is used to draw out the exhaust gas in the pulping tank 2, ensuring that the pulping tank 2 is under negative pressure; the outlet of the third pulping spray pipe 25 is connected to the outlet of the exhaust gas spray section 26, and the outlet end of the third pulping spray pipe 25 is equipped with a stainless steel spiral nozzle, which can pre-wash the carbonaceous dust carried in the exhaust gas discharged from the pulping tank 2.

[0056] Furthermore, the bottom of the clear liquid tank 3 is provided with three liquid outlets, each of which is connected to the inlet of the clear liquid transfer pump 31, the first clear liquid spray pump 33 and the second clear liquid spray pump 35 through a pipe. This can fully utilize the spraying function and effect of the three pumps in the clear liquid tank 3. The top of the clear liquid tank 3 is provided with a liquid level gauge, and the operator can determine the amount of alkali solution or fresh water to be added or discharged based on the liquid level monitoring results.

[0057] Furthermore, the outlet of the first clear liquid spray pipe 34 is connected to the first breathing pipe 23 through 2-4 spray branch pipes arranged at equal intervals. The number of spray branch pipes is determined according to the length of the first breathing pipe 23. In this embodiment, 3 spray branch pipes are provided. A stainless steel spiral nozzle is provided at the outlet end of the spray branch pipe. The first breathing pipe 23 is provided with a horizontal section and a vertical section from the inlet end to the outlet end. The horizontal section is inclined at 5-15° relative to the horizontal direction, and one end of the horizontal section near the outlet end of the first breathing pipe 23 is lower than the other end. This can ensure that the alkaline solution and carbon-containing dust in the first breathing pipe 23 can flow smoothly to the pulping tank 2.

[0058] Furthermore, the second clear liquid spray pipe 36 is provided with 3-4 spray branch pipes extending into the clear liquid tank 3, and evenly distributed in the middle area of ​​the top of the clear liquid tank 3. The specific number of spray branch pipes is determined according to the diameter of the clear liquid tank 3. In this embodiment, 4 spray branch pipes are provided. The outlet end of the spray branch pipe is provided with a stainless steel spiral nozzle, which can make the alkaline solution and fresh water fully mixed in the clear liquid tank 3, and at the same time further spray and wash the carbon-containing dust entering the clear liquid tank 3, reducing its entry into the second breathing pipe 38.

[0059] Furthermore, the outlet of the third clear liquid spray pipe 37 is connected to the second breathing pipe 38 through 2-4 equally spaced spray branch pipes. The number of spray branch pipes is determined according to the number of bends in the second breathing pipe 38, and 1-2 spray branch pipes can be set at each bend. In this embodiment, 2 spray branch pipes are set. The outlet end of the spray branch pipe is equipped with a stainless steel spiral nozzle, which can further spray and wash the carbon-containing dust escaping from the clear liquid tank 3, further reducing its entry into the exhaust gas scrubbing system. The second breathing pipe 38 is set at an inclination of 5-15° relative to the horizontal direction, and the outlet end of the second breathing pipe 38 is higher than the inlet end, which can ensure that the alkaline solution, fresh water and carbon-containing dust in the second breathing pipe 38 can flow back smoothly to the clear liquid tank 3.

[0060] Furthermore, the new water pipe 5 is connected to the second breathing pipe 38 through 3-4 equally spaced spray branch pipes, which are evenly distributed in the middle and outlet of the second breathing pipe 38. The number of spray branch pipes is determined according to the length of the second breathing pipe 38. In this embodiment, there are 4 spray branch pipes, and a spiral nozzle is provided at the outlet of the spray branch pipe. This design can clean the carbon-containing dust attached to the second breathing pipe 38 while adding new water to the clear liquid tank 3.

[0061] This invention also provides a method for pulping vanadium removal residue from titanium tetrachloride organic compounds, employing the aforementioned pulping device, specifically including the following steps:

[0062] A. Add alkali solution (30% NaOH solution) to the clear liquid tank 3 through the alkali solution pipe 4, and then add fresh water to the clear liquid tank 3 through the fresh water pipe 5. During the process of adding fresh water, the inner wall of the second breathing tube 38 is cleaned through the spray branch pipe set on the fresh water pipe 5. The volume ratio of alkali solution to fresh water is 1:1 to 2:1. In this embodiment, it is controlled at 1:1.

[0063] B. Start the second cleaning liquid spray pump 35 to circulate the alkaline solution and fresh water in the cleaning liquid tank 3 through the second cleaning liquid spray pipe 36 and the third cleaning liquid spray pipe 37, so that the alkaline solution and fresh water in the cleaning liquid tank 3 are mixed evenly for 1-2 hours. After that, the second cleaning liquid spray pump 35 continues to run to ensure that the exhaust gas entering the cleaning liquid tank 3 and the second breathing pipe 38 can be continuously sprayed through the second cleaning liquid spray pipe 36 and the third cleaning liquid spray pipe 37. According to the actual alkaline solution flow requirements for washing carbon dust in each part, adjust the valve opening on the first cleaning liquid spray pipe 34 and the second cleaning liquid spray pipe 36 respectively.

[0064] C. Start the clear liquid transfer pump 31 to transfer the alkaline solution, which is mixed evenly with the fresh water, to the pulping tank 2. The volume ratio of the alkaline solution added to the pulping tank 2 to the volume of the residue discharged from the slurry evaporator 1 in each batch is about 10:1. This ensures that the residue and alkaline solution maintain good fluidity after mixing, avoiding blockage of pipes and nozzles. At the same time, it also controls the pH value of the slurry in the pulping tank 2 to be between 9 and 10.

[0065] D. Start the first clear liquid spray pump 33 to circulate and spray alkaline solution onto the first breathing tube 23;

[0066] E. Start the pulping spray pump 21, and simultaneously circulate alkaline solution through the first pulping spray pipe 22, the second pulping spray pipe 24 and the third pulping spray pipe 25 to spray alkaline solution onto the slag discharge pipe 11, the top of the pulping tank 2 and the exhaust gas spray section 26. Adjust the valve openings on the first pulping spray pipe 22, the second pulping spray pipe 24 and the third pulping spray pipe 25 according to the actual alkaline solution flow requirements for washing carbon dust in each part.

[0067] F. Open the slag discharge valve 11 of the slurry evaporator 1 to discharge a batch of residue into the pulping tank 2 and mix it thoroughly with the alkali solution; the agitator 28 can be started for stirring.

[0068] G. Close the slag discharge valve 11 of the slurry evaporator 1. After the slurry spray pump 21 has been running for 1-2 hours, open the valve on the slurry discharge pipe 27 to transport the evenly mixed slurry in the slurry tank 2 to the collection container. This completes the slurry treatment of one batch of residue. The next batch of residue will be slurryed through the cyclic step AG.

[0069] Furthermore, the procedure also includes the following steps: after pulping is completed, every 1-2 days, open the spray branch pipes on the first pulping spray pipe 22, the second pulping spray pipe 24, the third pulping spray pipe 25, the first clear liquid spray pipe 34, the second clear liquid spray pipe 36, and the third clear liquid spray pipe 37, and check and clean the stainless steel spiral nozzles on each spray branch pipe.

[0070] The titanium tetrachloride organic vanadium removal residue pulping device and method provided by the present invention can mix the residue of the slurry evaporator with alkaline solution under closed conditions to form a slurry. The carbon-containing dust generated during the pulping process is fully washed to prevent combustion due to contact with air. At the same time, it reduces the deposition and adhesion of carbon-containing dust in the breathing pipe, stabilizes the air pressure of the pulping device, greatly reduces the labor intensity of manually cleaning the breathing pipe, and significantly improves the on-site working environment and safety control level.

[0071] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A pulping device for removing vanadium residue from organic compounds using titanium tetrachloride, characterized in that, It includes a pulping tank, a pulping spray pump, a clear liquid tank, a clear liquid transfer pump, a first clear liquid spray pump, and a second clear liquid spray pump; The slurry evaporator is vertically connected to the top of the pulping tank via a slag discharge pipe at the bottom, and a slag discharge valve is installed on the slag discharge pipe; the slurry evaporator can discharge residue into the pulping tank through the slag discharge pipe; the clear liquid tank is used to supply alkali solution to the pulping tank; The top of the pulping tank is equipped with a waste gas spray section; the inlet of the pulping spray pump is connected to the pulping tank, and the outlet is connected to the slag discharge pipe, the top of the pulping tank, and the waste gas spray section through the first pulping spray pipe, the second pulping spray pipe, and the third pulping spray pipe, respectively; the waste gas spray section is connected to the top of the clear liquid tank through a first breather pipe; The inlets of the clear liquid transfer pump, the first clear liquid spray pump, and the second clear liquid spray pump are respectively connected to the bottom of the clear liquid tank; the outlet of the clear liquid transfer pump is connected to the top of the pulping tank through a clear liquid transfer pipe; the outlet of the first clear liquid spray pump is connected to the inlet of the first breathing pipe through a first clear liquid spray pipe; the outlet of the second clear liquid spray pump is connected to the top of the clear liquid tank and the inlet of the second breathing pipe through a second clear liquid spray pipe and a third clear liquid spray pipe, respectively; the waste gas in the clear liquid tank enters the waste gas scrubbing system through the second breathing pipe.

2. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, It also includes an alkali pipe for replenishing alkali solution to the clear liquid tank and a new water pipe for replenishing new water to the clear liquid tank; the alkali pipe is connected to the top of the clear liquid tank; the new water pipe is connected to the second breathing pipe through 3-4 spray branch pipes that are equidistantly arranged and are evenly distributed in the middle and outlet end of the second breathing pipe, and the outlet end of the spray branch pipe is provided with a spiral nozzle.

3. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The bottom of the pulping tank is provided with a liquid outlet, and the inlet of the pulping spray pump is connected to the liquid outlet through a pipe; the bottom surface of the pulping tank is a 5-10° downward slope facing the side where the liquid outlet is located, and the bottom of the slope is lower than the liquid outlet. The sloped bottom design facilitates the discharge of slurry in the pulping tank; the outlet of the pulping spray pump is also provided with a slurry discharge pipe, which is used to discharge the uniformly mixed slurry in the pulping tank into a collection container.

4. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The outlet of the first slurry spray pipe is connected to the middle of the slag discharge pipe, and a nozzle is provided at the outlet end of the first slurry spray pipe.

5. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The outlet of the second pulping spray pipe is provided with 3-4 spray branch pipes extending into the pulping tank, and they are evenly distributed in the middle area of ​​the top of the pulping tank; the outlet end of the spray branch pipe is provided with a nozzle.

6. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The exhaust gas spray section is located at the top of the pulping tank near the edge of the tank wall; the inner diameter of the exhaust gas spray section is 200-400mm; the exhaust gas spray section is used to draw out the exhaust gas in the pulping tank to ensure that the pulping tank is under negative pressure; the outlet of the third pulping spray pipe is connected to the outlet of the exhaust gas spray section, and the outlet end of the third pulping spray pipe is provided with a nozzle.

7. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The outlet of the first clear liquid spray pipe is connected to the first breathing pipe through 2-4 spray branch pipes arranged at equal intervals; a nozzle is provided at the outlet end of the spray branch pipe; the first breathing pipe is provided with a horizontal section and a vertical section from the inlet end to the outlet end, the horizontal section is inclined at 5-15° relative to the horizontal direction, and the end of the horizontal section near the outlet end of the first breathing pipe is lower than the other end.

8. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The second clear liquid spray pipe is provided with 3-4 spray branch pipes extending into the clear liquid tank and evenly distributed in the middle area of ​​the top of the clear liquid tank; the outlet end of the spray branch pipe is provided with a nozzle.

9. The titanium tetrachloride organic vanadium removal residue pulping device according to claim 1, characterized in that, The outlet of the third clear liquid spray pipe is connected to the second breathing pipe through 2-4 spray branch pipes arranged at equal intervals; a nozzle is provided at the outlet end of the spray branch pipe; the second breathing pipe is inclined at 5-15° relative to the horizontal direction, and the outlet end of the second breathing pipe is higher than the inlet end.

10. A method for pulping vanadium-removing residue from titanium tetrachloride organic compounds, characterized in that, The pulping device described in claim 3 specifically includes the following steps: A. Add alkali solution to the clear liquid tank through the alkali solution pipe, and then add fresh water to the clear liquid tank through the fresh water pipe. The volume ratio of alkali solution to fresh water is 1:1 to 2:

1. B. Start the second clear liquid spray pump to circulate the alkaline solution and fresh water in the clear liquid tank through the second and third clear liquid spray pipes, and mix the alkaline solution and fresh water in the clear liquid tank evenly. C. Start the clear liquid transfer pump to transfer the alkaline solution that is evenly mixed with fresh water to the pulping tank. The ratio of the volume of alkaline solution added to the pulping tank to the volume of residue discharged from the slurry evaporator in each batch is 10:

1. D. Start the first clear liquid spray pump to circulate and spray alkaline solution through the first breathing tube; E. Start the pulping spray pump, and simultaneously circulate alkaline solution through the first pulping spray pipe, the second pulping spray pipe and the third pulping spray pipe to spray alkaline solution onto the slag discharge pipe, the top of the pulping tank and the exhaust gas spray section. F. Open the slag discharge valve of the slurry evaporator and discharge a batch of residue into the pulping tank to mix thoroughly with the alkali solution; G. Close the slag discharge valve of the slurry evaporator. After the slurry spray pump has been running for 1-2 hours, open the valve on the slurry discharge pipe to transfer the evenly mixed slurry in the slurry tank to the collection container. This completes the slurry treatment of one batch of residue. The next batch of residue will be slurryed through the cyclic step AG.

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