Device and method for collecting crude titanium tetrachloride

By designing two leaching towers and a device that separates the circulating pump tank, the gas channel and overflow partition are used to achieve full mixing of liquid and flue gas, which solves the problems of string material risks and insufficient energy utilization in the leaching system, and improves the problem of The collection efficiency and temperature control accuracy of titanium tetrachloride are obtained.

CN119289716APending Publication Date: 2025-01-10PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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Patent Information

Application Number
CN202411498831.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-24
Publication Date
2025-01-10

AI Technical Summary

Technical Problem

In the existing titanium chloride metallurgy process, the leaching system has problems such as risk of stringing materials and underutilizing energy, which affects the collection efficiency and temperature control of titanium tetrachloride.

Method used

A device consisting of two leaching towers and a separate circulation pump tank is designed, and the two leaching towers are connected through a gas channel, and an overflow partition and a liquid pump are provided in the circulation pump tank, using a triangular box and a guide. The flow structure realizes full mixing of liquid and flue gas and temperature regulation to avoid the phenomenon of stringing materials.

Benefits of technology

It improves the collection efficiency and temperature control accuracy of titanium tetrachloride, reduces the liquid temperature, enhances the heat exchange ability, avoids the risk of stringing, and improves the efficiency of the overall process.

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Abstract

The invention discloses a device and a method for collecting crude titanium tetrachloride, and belongs to the technical field of titanium chlorination metallurgy. The device comprises a first leaching tower, a second leaching tower, a gas channel and a circulating pump tank. The gas channel is arranged between the first leaching tower and the second leaching tower; the circulating pump tank is divided into a first circulating pump tank and a second circulating pump tank by an overflow partition plate, the overflow partition plate is a hollow partition plate, the first circulating pump tank and the second circulating pump tank are respectively communicated with the first leaching tower and the second leaching tower, and a submerged pump and a heat exchanger are respectively arranged at the bottoms of the first circulating pump tank and the second circulating pump tank; an overflow opening is formed in the side wall of the first circulating pump groove or the second circulating pump groove. The temperature of the titanium tetrachloride liquid in the second leaching tower is not increased due to material mixing of the circulating pump groove after the liquid is leached by the device; liquid in the second circulating pump tank with relatively low temperature overflows into the first circulating pump tank, so that the temperature of the liquid in the first circulating pump tank can be reduced, and the heat exchange capacity of the first leaching tower is improved.
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Description

Technical Field

[0001] The invention relates to the field of titanium chloride metallurgy, in particular to a collecting device and a method for preparing titanium tetrachloride from titanium-containing materials. Background Art

[0002] As the preferred engineering process for high-grade titanium dioxide raw materials, the chlorination process of titanium dioxide technology has been rapidly developed and expanded in China in recent years. Titanium-containing materials react with chlorine in a chlorination furnace to generate titanium tetrachloride mixed flue gas, which is then eluted and separated in multiple stages to obtain crude titanium tetrachloride. Usually, the titanium tetrachloride liquid collected in the circulation tank is used to spray the high-temperature titanium tetrachloride flue gas after heat exchange and cooling in a heat exchanger. In the high-temperature section, the high-boiling solid matter in the flue gas is reduced and separated; in the low-temperature section, the flue gas is condensed to obtain crude titanium tetrachloride liquid with a low solid content. In order to ensure the highest possible efficiency in the collection of titanium tetrachloride and reduce the loss of titanium tetrachloride, the last stage of cooling often uses frozen brine to further reduce the temperature of titanium tetrachloride.

[0003] In the actual production process, the elution system can be composed of a one-to-one and completely independent elution tower and a circulation pump tank. The elution liquid is stored in an independent or shared storage tank below the circulation pump tank. Alternatively, two or more elution towers can be arranged in parallel to correspond to the same circulation pump tank, and the elution liquid is mixed in the circulation pump tank and then enters the storage tank. The operation and control of a completely independent system is relatively simple, but the footprint is large. Two or more elution towers sharing a circulation pump tank can reduce the footprint, but there is a risk of cross-contamination. In addition, the temperature of the liquid after cooling by the frozen brine in the last stage is relatively low, and the energy is not fully utilized.

[0004] Therefore, it is necessary to design an efficient leaching system that can more easily regulate the temperature of liquid and flue gas without cross-contamination. Summary of the invention

[0005] In view of the above problems, the present invention provides a device and method for collecting crude titanium tetrachloride.

[0006] In order to solve at least one of the above technical problems, the present invention adopts the following technical solution: According to one aspect of the present invention, there is provided a device for collecting crude titanium tetrachloride, comprising: A first elution tower, wherein a first elution tower gas inlet and a first spray port are provided at one end of the first elution tower; A second elution tower, wherein one end of the second elution tower is provided with a second elution tower gas inlet and a second spray port; A gas channel, which is arranged between the first elution tower and the second elution tower and is used to connect the first elution tower and the second elution tower; A circulating pump tank, the circulating pump tank is divided into a first circulating pump tank and a second circulating pump tank by an overflow partition, the overflow partition is set as a hollow partition, the first circulating pump tank and the second circulating pump tank are respectively connected to the first elution tower and the second elution tower, and a submersible pump and a heat exchanger are respectively arranged at the bottom of the first circulating pump tank and the second circulating pump tank, and an overflow port is arranged on the side wall of the first circulating pump tank or the second circulating pump tank; The liquids in the first circulation pump tank and the second circulation pump tank are pumped out by their respective submersible pumps and cooled by their respective heat exchangers before entering the first elution tower and the second elution tower respectively through the first spray port and the second spray port.

[0007] According to one embodiment of the present invention, the rear side of the circulation pump tank is vertically connected to the first elution tower and the second elution tower through a triangular box.

[0008] According to an embodiment of the present invention, a liquid guide structure is provided on the inclined surface of the triangular box body, and the guide structure includes at least one guide plate extending in a fan shape along the inclined surface of the box body toward two ends of the circulation pump groove.

[0009] According to one embodiment of the present invention, the number of guide plates is 2 to 10.

[0010] According to one embodiment of the present invention, the gas channel is located 100-500 mm below the first elution tower and the second elution tower.

[0011] According to one embodiment of the present invention, the gas channel is configured as a herringbone channel with an angle of 90-150 degrees and an operation port at the top.

[0012] According to one embodiment of the present invention, the height of the overflow baffle is 1 / 2 to 6 / 7 of the diameter of the circulation pump tank, and is 200 mm to 400 mm higher than the height of the overflow port on the outside of the circulation pump tank.

[0013] According to one embodiment of the present invention, the outside of the overflow port is connected to the storage tank.

[0014] According to another aspect of the present invention, there is provided a method for collecting crude titanium tetrachloride using the above-mentioned device, comprising the following steps: The liquid in the first circulating pump tank S1 is pumped to the heat exchanger by the submerged pump at the bottom of the circulating pump tank, and after cooling, it is sprayed to the first elution tower to generate heat exchange with the gas phase titanium tetrachloride entering the gas inlet of the first elution tower; The S2 liquid flows down the first elution tower to the first circulation pump tank, and the uncondensed gas phase enters the second elution tower through the gas channel, is pumped out by the submerged pump of the second circulation pump tank, and is cooled by the heat exchanger to exchange heat with the liquid in the second circulation pump tank; After the low-temperature liquid in the second circulating pump tank S3 accumulates to the height of the overflow partition, it overflows into the first circulating pump tank, further reducing the temperature of the liquid in the first circulating pump tank, and finally enters the storage tank through the overflow port outside the circulating pump tank.

[0015] According to a method for collecting crude titanium tetrachloride in one embodiment of the present invention, in step S2, the rear side of the circulation pump tank is vertically connected to the first elution tower and the second elution tower through a triangular box body, and a guide structure is provided inside the triangular box body. The liquid flows down along the first elution tower to the triangular box body, and enters the circulation pump tank along the guide structure for mixing.

[0016] Preferably, the flow guide structure inside the triangular box body may include at least one flow guide plate extending in a fan shape along the inclined surface of the triangular box body toward the two ends of the circulation pump groove.

[0017] Due to the adoption of the above technical solution, the liquid after titanium tetrachloride elution will not further cause the temperature of titanium tetrachloride liquid in the second elution tower to rise due to the cross-contamination of the first circulation pump tank and the second circulation pump tank, thereby affecting the temperature of titanium tetrachloride liquid at the outlet of the heat exchanger and the efficiency of eluting and collecting flue gas; at the same time, the relatively low-temperature second circulation pump tank liquid overflows into the first circulation pump tank, which can further reduce the temperature of the liquid in the first circulation pump tank and improve the heat exchange capacity of the first elution tower. Correspondingly, the method of the present invention has the same benefits. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] 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.

[0019] Figure 1 This is a schematic diagram of the structure of a device for collecting crude titanium tetrachloride according to one embodiment of the present invention; Figure 2 for Figure 1 A schematic diagram of the structure of a triangular box located at the rear side of a circulating pump tank in a device for collecting crude titanium tetrachloride; Figure 3 for Figure 1 Schematic diagram of gas heat exchange in the device for collecting crude titanium tetrachloride.

[0020] The reference numerals are as follows: 1. First circulation pump tank; 2. Second circulation pump tank; 3. First elution tower; 4. Second elution tower; 5. First elution tower gas inlet; 6. Second elution tower gas inlet; 7. Triangular box; 8. Guide plate; 9. Gas channel; 10. Operation port; 11. First spray port; 12. Second spray port; 13. Overflow port; 14. Overflow baffle. DETAILED DESCRIPTION

[0021] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0022] 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.

[0023] According to one aspect of the present invention, a device for collecting crude titanium tetrachloride is provided. Figure 1 As shown, the device for collecting crude titanium tetrachloride mainly comprises: A first leaching tower 3, one end of which is provided with a first leaching tower gas inlet 5 and a first spray port 11; A second elution tower 4, one end of which is provided with a second elution tower gas inlet 6 and a second spray port 12; A gas channel, which is arranged between the first elution tower 3 and the second elution tower 4 and is used to connect the first elution tower 3 and the second elution tower 4; The circulating pump tank is divided into a first circulating pump tank 1 and a second circulating pump tank 2 by an overflow partition 14. The overflow partition 14 is a hollow partition. The first circulating pump tank 1 and the second circulating pump tank 2 are connected to the first elution tower 3 and the second elution tower 4 respectively, and a submersible pump and a heat exchanger are respectively arranged at the bottom of the circulating pump tank. The side wall of the first circulating pump tank 1 or the second circulating pump tank 2 is provided with an overflow port 13; the overflow port 13 is connected to the storage tank to collect the elution liquid. Figure 1 In the illustrated embodiment, the overflow port 13 is disposed on the outer side wall of the first circulation pump tank 1 .

[0024] Based on the above structure, the liquid in the first circulation pump tank 1 and the second circulation pump tank 2 are pumped out by their respective submersible pumps, cooled by the heat exchanger, and enter the first elution tower 3 and the second elution tower 4 through the first spray port 11 and the second spray port 12 respectively.

[0025] According to the crude titanium tetrachloride collection device of the present invention, after the liquid in the first circulation pump tank 1 is pumped to the heat exchanger for cooling by the submerged pump below it, the flue gas generated is sprayed to enter the first leaching tower 3, and the solids such as high-boiling point chlorides in the flue gas and part of the cooled titanium tetrachloride enter the first circulation pump tank 1, and the uneluted gas phase enters the second leaching tower 4 through the gas channel 9. Similarly, after the liquid in the second circulation pump tank 2 is pumped to the heat exchanger for cooling by the submerged pump below it, the flue gas generated is sprayed to enter the second leaching tower 4, and the cooled titanium tetrachloride in the flue gas enters the second circulation pump tank 2. When the liquid in the second circulation pump tank 2 accumulates to the height of the overflow partition 14, it will cause overflow, causing the liquid in the second circulation pump tank 2 to overflow to the first circulation pump tank 1. Finally, when the liquid in the first circulation pump tank 1 accumulates to the height of the overflow port 13, it will flow out from the overflow port 13 to the storage tank.

[0026] like Figure 2 As shown, in the embodiment of the present invention, in order to make the newly rinsed liquid and the liquid in the circulating pump tank mix more fully, a triangular box is provided at the rear side of the circulating pump tank, which is vertically connected to the bottom of the first elution tower 3 and the second elution tower 4, and a liquid guide structure is provided inside. The guide structure may include at least one guide plate 8 extending in a fan shape toward both ends of the circulating pump tank along the inclined surface of the box.

[0027] Preferably, the number of the guide plates 8 can be set to 2 to 10.

[0028] In order to ensure better collection of crude titanium tetrachloride, it is necessary to further comprehensively regulate the number and shape of the guide plates 8, the gas channels, and the specifications of the heat insulation plates.

[0029] like Figure 1-3 As shown, the gas channel can be set as a herringbone channel, located 100~500mm below the first elution tower and the second elution tower, with a channel angle of 90~150°. In order to further prevent the eluted liquid from flowing between the first elution tower and the second elution tower, an operation port can be set at the top of the gas channel to clean the solid phase deposited at both ends of the gas channel, so as to ensure the purity of the gas inside the device and the rapid progress of the subsequent reaction, and also improve the working efficiency inside the device to a certain extent.

[0030] The height of the overflow baffle 14 can be set to 1 / 2 to 6 / 7 of the diameter of the circulation tank, and is 200 mm to 400 mm higher than the overflow port 13 of the circulation pump tank.

[0031] According to another aspect of the present invention, the present invention also provides a method for collecting crude titanium tetrachloride, which generally comprises the following steps: S1, the liquid in the first circulating pump tank 1 is pumped to the heat exchanger by the liquid pump at the bottom of the circulating pump tank, and the flue gas after cooling is sprayed to the first elution tower 3 to generate heat exchange with the gas phase titanium tetrachloride entering the inlet of the first elution tower 3; S2, the liquid goes down along the first elution tower 3 to the first circulation pump tank 1, and the uncondensed gas phase enters the second elution tower 4 through the gas channel to perform heat exchange with the liquid in the second circulation pump tank 4 after being cooled by the heat exchanger; S3. After the low-temperature liquid in the second circulation pump tank accumulates to the height of the overflow partition 14, it overflows into the first circulation pump tank, further reducing the temperature of the liquid in the first circulation pump tank, until the liquid water level in the first circulation pump tank reaches the height of the overflow port 13, and then flows out through the overflow port 13 of the first circulation pump tank into the storage tank.

[0032] Preferably, according to the method for collecting crude titanium tetrachloride described in the above embodiment, in order to ensure more sufficient mixing, in step S2 of the present method, a triangular box can be set on the rear side of the circulation pump tank, which is vertically connected with the first elution tower and the second elution tower through the triangular box, and a guide structure is provided inside the triangular box. The liquid can flow down along the first elution tower to the triangular box and enter the circulation pump tank through the guide structure for mixing.

[0033] The present invention is further described below in conjunction with a specific production example.

[0034] According to the crude titanium tetrachloride collection device of one embodiment of the present invention, the first circulation pump tank 1 and the second circulation pump tank 2 are set to have a diameter of 3m and a length of 7m, the internal overflow baffle 14 is 2.5m high, the overflow port 13 is 2.3m high, and the guide plates 8 inside the triangular box are set to 4. When the liquid temperature in the first circulation pump tank 1 is 60°C, the liquid temperature in the second circulation pump tank is -15°C, and the temperature of the titanium tetrachloride mixed gas is 95°C, the titanium tetrachloride mixed gas enters the first leaching tower 3 from the first leaching tower gas inlet 5, and the titanium tetrachloride liquid in the first circulation pump tank 1 is pumped to the heat exchanger by the submerged pump to reduce its temperature to 40°C. The flue gas generated in this process is sprayed into the first leaching tower 3 through the first spray port 11 to exchange heat with the 90°C titanium tetrachloride mixed gas, and the liquid titanium tetrachloride flows into the triangular box and flows into the first circulation pump tank 1 along the guide plate 8 inside it; the uncondensed 40°C flue gas in the first leaching tower 3 enters the second leaching tower 4 through the gas channel 9; similarly, the first After the titanium tetrachloride liquid in the second circulation pump tank 2 is pumped to the heat exchanger by the submersible pump, the temperature is reduced to -23°C, and the flue gas generated is sprayed to the second spray port 12 to enter the second leaching tower 4 for heat exchange with the 40°C titanium tetrachloride mixed gas, and the liquid titanium tetrachloride flows into the triangular box 7 and enters the second circulation pump tank 2 along the guide plate 8; the -15°C titanium tetrachloride liquid in the second circulation pump tank 4 overflows to the first circulation pump tank 1 through the 2.5m overflow baffle 14 between the first circulation pump tank 1 and the second circulation pump tank 2, and mixes with the 60°C liquid to further reduce the liquid temperature of the first circulation pump tank 1, until the accumulated liquid in the first circulation pump tank 1 reaches the height of the overflow port 13, and flows out to the storage tank through the overflow port 13.

[0035] 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.

[0036] 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.

[0037] 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 device for collecting crude titanium tetrachloride, characterized in that: include: A first elution tower (3), wherein a first elution tower gas inlet (5) and a first spray port (11) are provided at one end of the first elution tower (3); A second elution tower (4), wherein one end of the second elution tower (4) is provided with a second elution tower gas inlet (6) and a second spray port (12); A gas channel (9), the gas channel being arranged between the first elution tower (3) and the second elution tower (4) and being used to connect the first elution tower (3) and the second elution tower (4); A circulation pump tank, wherein an overflow baffle (14) is provided inside the circulation pump tank so as to separate the circulation pump tank into a first circulation pump tank (1) and a second circulation pump tank (2), wherein the overflow baffle (14) is a hollow baffle, wherein the first circulation pump tank (1) and the second circulation pump tank (2) are respectively connected to the first elution tower (3) and the second elution tower (4), and a submersible pump and a heat exchanger are respectively provided at the bottom of the circulation pump tank, and an overflow port (13) is provided on the side wall of the first circulation pump tank (1) or the second circulation pump tank (2); The liquid in the first circulation pump tank (1) and the second circulation pump tank (2) is pumped out by respective submersible pumps and cooled by a heat exchanger before entering the first elution tower (3) and the second elution tower (4) through the first spray port (11) and the second spray port (12) respectively.

2. The device for collecting crude titanium tetrachloride according to claim 1, characterized in that: The rear side of the circulation pump tank is vertically connected to the first elution tower (3) and the second elution tower (4) through a triangular box (7).

3. The device for collecting crude titanium tetrachloride according to claim 2, characterized in that: A liquid guide structure is provided on the inner inclined surface of the triangular box body (7), wherein the guide structure comprises at least one guide plate (8) extending in a fan shape toward two ends of the circulation pump groove along the inclined surface of the triangular box body.

4. The device for collecting crude titanium tetrachloride according to claim 3, characterized in that: The number of the guide plates (8) is 2 to 10.

5. The device for collecting crude titanium tetrachloride according to claim 1, characterized in that: The gas channel (9) is located 100 to 500 mm below the first elution tower (3) and the second elution tower (4).

6. The device for collecting crude titanium tetrachloride according to claim 5, characterized in that: The gas channel (9) is configured as a herringbone channel with an angle of 90 to 150 degrees, and an operation port (10) is provided at the top.

7. The device for collecting crude titanium tetrachloride according to claim 1, characterized in that: The height of the overflow baffle (14) is 1 / 2 to 6 / 7 of the diameter of the circulation pump tank, and is 200 mm to 400 mm higher than the height of the overflow port (13) outside the circulation pump tank.

8. The device for collecting crude titanium tetrachloride according to claim 1, characterized in that: The overflow port (13) is connected to the storage tank on the outside.

9. A method for collecting crude titanium tetrachloride, characterized in that: The method comprises performing the following steps based on the device for collecting crude titanium tetrachloride according to any one of claims 1 to 8: S1, the liquid in the first circulation pump tank (1) is pumped to the heat exchanger by the submerged pump at the bottom of the circulation pump tank, and after cooling, it is sprayed to the first elution tower (3) to generate heat exchange with the gas phase titanium tetrachloride entering the gas inlet (5) of the first elution tower; S2, the liquid flows down the first elution tower (3) to the first circulation pump tank (1), the uncondensed gas phase enters the second elution tower (4) through the gas channel (9), is pumped out by the submerged pump of the second circulation pump tank (2), is cooled by the heat exchanger, and then exchanges heat with the liquid in the second circulation pump tank (2); S3, after the low-temperature liquid in the second circulation pump tank (2) accumulates to the height of the overflow baffle (14), it overflows into the first circulation pump tank (1), further reducing the temperature of the liquid in the first circulation pump tank (1), and finally enters the storage tank through the overflow port (13) outside the circulation pump tank.

10. The method for collecting crude titanium tetrachloride according to claim 9, characterized in that: In step S2, the rear side of the circulation pump tank is vertically connected to the first elution tower (3) and the second elution tower (4) through a triangular box (7), and a flow guide structure is provided inside the triangular box (7). The liquid flows down along the first elution tower (3) to the triangular box (9) and enters the circulation pump tank along the flow guide structure for mixing.