Method and device for reducing C impurity in titanium sponge

Abstract

The invention relates to the field of titanium sponge production, in particular to a method and a device for reducing C impurities in titanium sponge, comprising a storage tank, the storage tank is connected with a feed pipe, one side of the storage tank is connected with a feed port of a centrifugal machine through a pipeline, a liquid phase outlet of the centrifugal machine is connected with a buffer tank through a pipeline, and one side of the buffer tank is connected with a charging tank through a pipeline; one side of the feeding tank is connected with a feeding pipe, the bottom of the buffer tank and the bottom of the feeding tank are each provided with a material returning opening, the two material returning openings are both connected to a material returning pipe, and the material returning pipe is connected with a feeding pipe; through the operations of centrifugation, standing and material returning, it is guaranteed that the C content in the sponge titanium reaches the 0A-level standard or above, and the problem that the sponge titanium cannot reach the high-end sponge titanium due to the fact that the C impurity exceeds the standard is solved.

Description

Technical Field

[0001] The present invention relates to the field of titanium sponge production, and particularly relates to a method and device for reducing C impurities in titanium sponge. Background Art

[0002] At present, the industrial production of titanium sponge at home and abroad all adopts the Kroll process, that is, liquid magnesium is added to a high-temperature reactor, and then titanium tetrachloride is introduced to react with it to obtain titanium sponge and magnesium chloride. The main raw materials of this reaction are titanium tetrachloride and magnesium. The technical standard of magnesium thermal reduction method for titanium sponge in China requires that the C impurity content of first-class products should not be more than 0.03%. However, for titanium sponge to enter the high-end market, the requirement for C impurities is not more than 0.01%. Even for some special downstream enterprises, the requirement for C content is higher. Therefore, the C impurity element has become one of the main factors affecting the entry of titanium sponge into the high-end market. The C impurities in titanium sponge mainly come from the raw material titanium tetrachloride (accounting for more than 80%), and a small amount comes from the raw material electrolytic magnesium. The reason why C impurities are carried in titanium tetrachloride is that currently, in the process of producing titanium tetrachloride, organic vanadium removal replaces aluminum powder vanadium removal. During the process of organic vanadium removal, C impurities will be introduced into titanium tetrachloride, resulting in a high content of C impurities in titanium sponge.

[0003] According to the observation of the morphology of titanium tetrachloride and the results of infrared detection, the C impurities in titanium tetrachloride mainly exist in the form of solid particles. Therefore, it is necessary to invent a method and device for reducing C impurities in titanium sponge according to this characteristic to solve the problem that titanium sponge cannot enter the high-end market due to high C impurities. Summary of the Invention

[0004] The purpose of the present invention is to provide a method and device for reducing C impurities in titanium sponge, which can effectively reduce the content of C impurities in titanium sponge to solve the defects mentioned in the above background art.

[0005] To achieve the above purpose, the present invention provides the following technical solutions:

[0006] A device for reducing C impurities in titanium sponge includes a storage tank, the storage tank is connected with a feed pipe, one side of the storage tank is connected to the feed inlet of a centrifuge through a pipeline, the liquid phase outlet of the centrifuge is connected to a buffer tank through a pipeline, one side of the buffer tank is connected to a feeding tank through a pipeline, one side of the feeding tank is connected with a feeding pipe, the bottoms of the buffer tank and the feeding tank are respectively provided with return ports, both of the return ports are connected to a return pipe, and the return pipe is connected to the feed pipe.

[0007] As a further improvement, the storage tank, the buffer tank and the feeding tank are respectively connected with argon filling ports; valves are provided on the argon filling ports.

[0008] As a further improvement, valves are respectively provided on the feed pipe, between the storage tank and the feed inlet of the centrifuge, between the liquid phase outlet of the centrifuge and the buffer tank, between the buffer tank and the feeding tank, on the feeding pipe, at the refeeding port, and at one end of the refeeding pipe connected to the feed pipe.

[0009] As a further improvement, the centrifuge is a horizontal filtration centrifuge, and the rotation speed of the centrifuge is 2000 - 3000 revolutions per minute.

[0010] As a further improvement, the solid phase outlet of the centrifuge is hermetically connected to a slag tank, and a valve is provided at the solid phase outlet of the centrifuge.

[0011] A method for reducing C impurities in titanium sponge by using the device for reducing C impurities in titanium sponge as described above, the method comprising the following steps:

[0012] S1, Unifiedly store refined titanium tetrachloride in the storage tank;

[0013] S2, Centrifuge the refined titanium tetrachloride in S1 by the centrifuge to remove solid particle impurities in the refined titanium tetrachloride solution;

[0014] S3, The refined titanium tetrachloride centrifuged in S2 enters the buffer tank and is statically stored for 4d - 6d. After the static storage ends, part of the refined titanium tetrachloride is returned to the storage tank through the refeeding port at the bottom of the buffer tank. After the refeeding ends, the remaining refined titanium tetrachloride in the buffer tank is transported to the feeding tank;

[0015] S4, First, let the refined titanium tetrachloride stand in the feeding tank. After the standing ends, part of the refined titanium tetrachloride is returned to the storage tank through the refeeding port at the bottom of the feeding tank. After the refeeding ends, the refined titanium tetrachloride in the feeding tank can be fed into the reduction furnace through the feeding pipe.

[0016] As a further improvement, the storage tank, the buffer tank, and the feeding tank are respectively filled with argon for protection, and the argon filling pressure is 20 - 30 kPa.

[0017] As a further improvement, the refeeding amount of the refined titanium tetrachloride to the storage tank in step S3 is 10% - 15% of the total amount of the refined titanium tetrachloride in the buffer tank.

[0018] As a further improvement, the refeeding amount of the refined titanium tetrachloride to the storage tank in step S4 is 3% - 5% of the total amount of the refined titanium tetrachloride in the feeding tank.

[0019] As a further improvement, the standing time of the refined titanium tetrachloride in step S4 is 1 - 3h.

[0020] Compared with the prior art, the beneficial effects of the present invention are:

[0021] 1. In the present invention, a centrifuge is provided. Since the C impurities in refined titanium tetrachloride mainly exist in the form of solid particles, the filtration function of the centrifuge can effectively remove most of the solid particle impurities.

[0022] 2. After titanium tetrachloride passes through the centrifuge in the present invention, a buffer tank is provided. The buffer tank is provided with a return port, and the feeding tank is also provided with a return port, in order to further ensure the quality of refined titanium tetrachloride and avoid introducing C impurities into titanium sponge.

[0023] 3. In the present invention, by filling with argon for protection, hydrolysis of titanium tetrachloride can be avoided, and new impurities can be prevented from being introduced.

[0024] 4. In the present invention, the return ratio of the buffer tank is controlled at 10 - 15%, and the return ratio of the feeding tank is controlled at 3 - 5%. This not only ensures that titanium tetrachloride with C impurities is returned to the storage tank for reprocessing, but also avoids the problem of excessive return amount causing excessive load on the centrifuge.

[0025] 5. Through the operations of centrifugation, standing, and return in the present invention, the C content in titanium sponge is ensured to reach above the 0A level standard, solving the problem that titanium sponge cannot meet the requirements of high-end titanium sponge due to excessive C impurities. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0027] Figure 1 It is a schematic structural diagram of an embodiment of the present invention;

[0028] Figure 2 It is a flowchart of the method for reducing C impurities in an embodiment of the present invention.

[0029] In the figure: 1 - storage tank; 2 - feed pipe; 3 - valve 1; 4 - pipeline 1; 5 - centrifuge; 6 - valve 2; 7 - liquid phase outlet; 8 - solid phase outlet; 9 - pipeline 3; 10 - buffer tank; 11 - valve 3; 12 - pipeline 4; 13 - feeding tank; 14 - valve 4; 15 - feeding pipe; 16 - valve 5; 17 - return port; 18 - return pipe; 19 - valve 6; 20 - valve 7; 21 - valve 8; 22 - argon filling port 1; 23 - argon filling valve 1; 24 - argon filling port 2; 25 - argon filling valve 2; 26 - argon filling port 3; 27 - argon filling valve 3; 28 - slag tank; 29 - valve 9. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0030] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the scope of protection of the present invention.

[0031] As Figure 1 shown, a device for reducing C impurities in titanium sponge includes a storage tank 1. A feed pipe 2 is connected to the top of the storage tank 1, and a valve 3 is provided on the feed pipe 2. The middle part of one side of the storage tank 1 is connected to the feed port of a centrifuge 5 through a pipeline 4, and a valve 6 is provided on the pipeline 4. The centrifuge 5 also has a liquid phase outlet 7 and a solid phase outlet 8. The liquid phase outlet 7 is connected to the top of a buffer tank 10 through a pipeline 9, and a valve 11 is provided on the pipeline 9. The middle part of one side of the buffer tank 10 is connected to the top of a feeding tank 13 through a pipeline 12, and a valve 14 is provided on the pipeline 12. The middle part of one side of the feeding tank 13 is connected to a feeding pipe 15, and a valve 16 is provided on the feeding pipe 15.

[0032] The bottom of the feeding tank 13 and the bottom of the buffer tank 10 are respectively provided with a return port 17. Both return ports are connected to a return pipe 18. One end of the return pipe 18 is connected to the feed pipe 2 downstream of the valve 3. A valve 19 is provided on the return port 17 at the bottom of the feeding tank 13, a valve 20 is provided on the return port 17 at the bottom of the buffer tank 10, and a valve 21 is provided at the end where the return pipe 18 is connected to the feed pipe 2. By setting the return port 17, the titanium tetrachloride containing C impurities deposited at the bottom of the feeding tank 13 and the buffer tank 10 is returned to the storage tank 1 for reprocessing.

[0033] In addition, an argon filling port 22 is connected to the feed pipe 2 downstream of the valve 3, and an argon filling valve 23 is provided on the argon filling port 22; an argon filling port 24 is connected to the pipeline 9 downstream of the valve 11, and an argon filling valve 25 is provided on the argon filling port 24; an argon filling port 26 is provided on the pipeline 12 downstream of the valve 14, and an argon filling valve 27 is provided on the argon filling port 26.

[0034] The solid phase outlet 8 of the centrifuge 5 is hermetically connected to a slag tank 28, and a valve 29 is provided at the solid phase outlet 8 of the centrifuge 5. In this embodiment, the centrifuge 5 is a horizontal filtration centrifuge, and the rotation speed of the centrifuge 5 is 2000 - 3000 revolutions per minute.

[0035] As Figure 2 shown, a method for reducing C impurities in titanium sponge using the above device for reducing C impurities in titanium sponge includes the following steps:

[0036] S1, The purchased refined titanium tetrachloride or self-produced refined titanium tetrachloride is uniformly stored in the storage tank 1;

[0037] S2. Centrifuge the refined titanium tetrachloride in S1 by centrifuge 5 to remove solid particle impurities in the refined titanium tetrachloride solution;

[0038] S3. The refined titanium tetrachloride centrifuged in S2 enters buffer tank 10 and is stored statically for 4d - 6d; after the static storage ends, part of the refined titanium tetrachloride is returned to storage tank 1 through the return port at the bottom of buffer tank 10, and the return amount of the refined titanium tetrachloride to storage tank 1 is 10% - 15% of the total amount of the refined titanium tetrachloride in buffer tank 10; after the return ends, the remaining refined titanium tetrachloride in buffer tank 10 is transported to charging tank 13;

[0039] S4. The refined titanium tetrachloride is first stored statically in charging tank 13 for 1 - 3h; after the static storage ends, part of the refined titanium tetrachloride is returned to storage tank 1 through return port 17 at the bottom of charging tank 13, and the return amount of the refined titanium tetrachloride to storage tank 1 is 3% - 5% of the total amount of the refined titanium tetrachloride in charging tank 13; after the return ends, the refined titanium tetrachloride in charging tank 13 can be fed into the reduction furnace through feed pipe 15.

[0040] During the operation of the system, argon is filled into storage tank 1, buffer tank 10, and charging tank 13 respectively through argon filling port 1, argon filling port 2, and argon filling port 3 for argon protection, and the argon filling pressure is 20 - 30 kPa.

[0041] Comparative example: The purchased refined titanium tetrachloride or the self-produced refined titanium tetrachloride is directly stored in storage tank 1, and storage tank 1 is directly connected to charging tank 13 through a pipeline. The refined titanium tetrachloride is not centrifugally filtered by centrifuge 5 and does not have static return in buffer tank 10 and charging tank 13, and directly enters charging tank 13 through storage tank 1 and then enters the reduction furnace. The following table is used to compare the C impurities contained in the titanium sponge produced by using this embodiment and the titanium sponge produced by the comparative example.

[0042] Category Number of furnaces C content in titanium sponge / % This example 10 furnaces 0.007 Comparative example 10 furnaces 0.026

[0043] Through the comparative experiment, it is found that by centrifugally filtering with centrifuge 5 and having static return in buffer tank 10 and charging tank 13, the effect of removing C impurities in the refined titanium tetrachloride is obvious, and the C content of the produced titanium sponge can be at 0A level or above.

[0044] The above shows and describes the basic principle, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The above embodiments and the descriptions in the specification are only preferred examples of the present invention and are not used to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed. The scope of protection claimed by the present invention is defined by the appended claims and their equivalents.

Claims

1. A device for reducing C impurities in titanium sponge, characterized by: It includes a storage tank, which is connected to a feed pipe. One side of the storage tank is connected to a feed port of a centrifuge through a pipeline. The liquid phase outlet of the centrifuge is connected to a buffer tank through a pipeline. One side of the buffer tank is connected to a feeding tank through a pipeline. One side of the feeding tank is connected to a feeding pipe. Return ports are respectively provided at the bottom of the buffer tank and the bottom of the feeding tank. Both return ports are connected to the return pipe. The return pipe is connected to the feed pipe.

2. The device for reducing C impurities in titanium sponge according to claim 1, characterized in that: The storage tank, the buffer tank and the feeding tank are respectively connected with argon filling ports; and a valve is arranged on the argon filling port.

3. The device for reducing C impurities in titanium sponge according to claim 1, characterized in that: Valves are respectively provided on the feed pipe, between the storage tank and the feed port of the centrifuge, between the liquid phase outlet of the centrifuge and the buffer tank, between the buffer tank and the feeding tank, on the feeding pipe, at the return port and at one end of the return pipe connected to the feed pipe.

4. The device for reducing C impurities in titanium sponge according to claim 1, characterized in that: The centrifuge is a horizontal filtering centrifuge, and the rotation speed of the centrifuge is 2000-3000 rpm.

5. The device for reducing C impurities in titanium sponge according to claim 1, characterized in that: The solid phase outlet of the centrifuge is sealed and connected with a slag tank, and a valve is arranged at the solid phase outlet of the centrifuge.

6. A method for reducing C impurities in titanium sponge using the device for reducing C impurities in titanium sponge according to any one of claims 1 to 5, characterized in that: The method comprises the following steps: S1, the refined titanium tetrachloride is uniformly stored in the storage tank; S2, centrifuging the refined titanium tetrachloride in S1 by the centrifuge to remove solid particle impurities in the refined titanium tetrachloride solution; S3, the refined titanium tetrachloride centrifuged in S2 enters the buffer tank and is stored for 4d-6d. After the standing, part of the refined titanium tetrachloride is returned to the storage tank through the return port at the bottom of the buffer tank. After the return, the remaining refined titanium tetrachloride in the buffer tank is transported to the feeding tank; S4, the refined titanium tetrachloride is first allowed to stand in the feeding tank, and after the standing is completed, part of the refined titanium tetrachloride is returned to the storage tank through the return port at the bottom of the feeding tank. After the return is completed, the refined titanium tetrachloride in the feeding tank can be fed to the reduction furnace through the feeding pipe.

7. A method for reducing C impurities in titanium sponge according to claim 6, characterized in that: The storage tank, the buffer tank and the feeding tank are respectively filled with argon for protection, and the argon filling pressure is 20-30 kPa.

8. A method for reducing C impurities in titanium sponge according to claim 6, characterized in that: In step S3, the amount of refined titanium tetrachloride returned to the storage tank is 10%-15% of the total amount of refined titanium tetrachloride in the buffer tank.

9. A method for reducing C impurities in titanium sponge according to claim 6, characterized in that: In step S4, the amount of refined titanium tetrachloride returned to the storage tank is 3%-5% of the total amount of refined titanium tetrachloride in the feeding tank.

10. A method for reducing C impurities in titanium sponge according to claim 6, characterized in that: The time for the refined titanium tetrachloride to stand in step S4 is 1-3 hours.

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