Molten salt chlorination rectification reaction device for enriching and purifying vanadium

Abstract

The invention relates to a fused salt chlorination rectification reaction device for enriching and purifying vanadium. According to the technical scheme, the fused salt chlorination rectification reaction device comprises four parts, namely a fused salt device (2), a chlorination device (4), a condensing device (5) and a high-temperature circulating oil bath device, a fused salt output pipe (14) of the fused salt device (2) is communicated with a fused salt input port (25) of the chlorination device (4) through a first pipeline B, and prepared fused salt is output from the fused salt output pipe (14) and enters the chlorination device (4) from the fused salt input port (25) through the first pipeline B; a gas outlet B (35) of the chlorination device (4) is communicated with a gas inlet C (41) of the collecting tank (44) through a second pipeline B, and the prepared vanadium oxychloride gas flows out of the gas outlet B (35) and enters the condensing device (5) from the gas inlet C (41) through the second pipeline B. The method has the characteristics of high molten salt adaptability, high molten salt preparation efficiency and chlorination efficiency, sufficient reaction, high product purity, economy, safety and easiness in industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of enriching and purifying vanadium, and specifically relates to a molten salt chlorination distillation reaction device for enriching and purifying vanadium. Background Art

[0002] As an important strategic metal, vanadium is widely used in the fields of metallurgy, chemical industry and aerospace industry, and is an indispensable element in modern science. At present, with the gradual development of all-vanadium liquid flow battery, electrode materials, vanadium aluminum alloy, high-purity vanadium and other industries, the market demand for high-purity vanadium products is increasing.

[0003] Chlorination distillation is a method in which vanadium-containing substances react with chlorinating agents under high temperature conditions, and the difference in physical and chemical properties between the generated vanadium oxychloride and the chloride of impurity ions is used to separate vanadium impurities and achieve the purpose of enriching and purifying vanadium. Using low-temperature molten salt as a chlorinating agent is more environmentally friendly than using chlorine as a chlorinating agent, with lower process controllability and easier industrial application.

[0004] However, the devices used in the existing molten salt chlorination distillation process are mostly series reaction devices, which require multiple independent devices such as reactors, multi-stage condensation equipment, receiving tanks, and tail gas treatment equipment to be placed in series, resulting in the device occupying a large space and poor economy; the multi-stage series device requires longer pipelines and more valve connections, which increases the risk of leakage of vanadium trichloride and has poor safety.

[0005] The patented technology of "Molten Salt Chlorination Device" (CN216093563U) designs an integrated chlorination reaction device, which compactly integrates the reaction structure, furnace structure and furnace shell structure into one device, thereby improving the heating efficiency and molten salt chlorination reaction efficiency; however, the reaction device is a closed reaction type, and when the reaction product is a gas, it cannot be well collected; the molten salt preparation and chlorination reaction are in the same device, and the heated and volatilized molten salt will enter the reaction product, reducing the purity of the product; the device lacks a temperature control system and a temperature sensor, and cannot monitor the temperature in the device in real time to adjust the reaction temperature, affecting the reaction efficiency.

[0006] The patented technology of "A chlorination distillation device for extracting cadmium" (CN116479246A) adopts a segmented and regional heating method and a heat preservation layer design, which can effectively control the temperature of the reaction area and form a temperature gradient according to the needs of the reaction, which is conducive to promoting the generation and separation of cadmium chloride. It has a good adaptability effect. However, the device is suitable for chlorination reaction devices with chlorine as the chlorinating agent; when molten salt is used as the chlorinating agent, the equipment is not equipped with a stirring device, which will lead to reduced chlorination efficiency and insufficient reaction.

[0007] The document (Jiang Dandan. Research on the purification process of vanadium pentoxide by low-temperature chlorination of aluminum chloride [D]. University of Chinese Academy of Sciences (Institute of Process Engineering, Chinese Academy of Sciences), 2017.) discloses a process for purifying vanadium pentoxide by low-temperature chlorination of aluminum chloride. The molten salt chlorination distillation reaction device used in this process is a traditional small-scale distillation series reaction device. Multiple independent devices such as distillation flasks, condensers, receiving tanks and tail gas treatment equipment are placed in series, requiring longer pipelines and more valve connections, which increases the risk of leakage of vanadium trichloride and has poor safety. The equipment is not equipped with a stirring device, which will lead to reduced chlorination efficiency and insufficient reaction, making it difficult to industrialize production.

[0008] In summary, the existing chlorination distillation reaction device has the problems of poor adaptability to molten salt, low chlorination efficiency, insufficient reaction, low product purity, difficulty in industrial production and poor safety. Summary of the invention

[0009] The present invention aims to overcome the defects of the prior art and aims to provide a molten salt chlorination distillation reaction device for enriching and purifying vanadium with strong molten salt adaptability, high molten salt preparation efficiency and chlorination efficiency, sufficient reaction, high product purity, economic safety and easy industrial production.

[0010] To achieve the above purpose, the technical solution adopted by the present invention is:

[0011] A molten salt chlorination distillation reaction device for enriching and purifying vanadium, comprising

[0012] The molten salt device is a sandwich tank with stirring, with at least a feeding port A at the top and at least a discharge pipe and a molten salt output pipe at the bottom;

[0013] The chlorination device is a sandwich tank with stirring, the top of which is equipped with at least a molten salt input port, a feed port B and a gas outlet B, and the bottom is equipped with at least a slag discharge pipe;

[0014] a condensing device connected to the gas outlet B and used for condensing the gas evaporated from the chlorination device; and

[0015] The high temperature circulating oil bath device is used to perform oil bath heating on the interlayers of the molten salt device and the chlorination device respectively.

[0016] Furthermore, the molten salt device is composed of a speed regulator A, an agitator A, a body A, a temperature sensor A, a cover plate A and a motor A.

[0017] The body A is a double-layer cylinder, and an interlayer A is provided between the outer wall and the inner wall of the body A. The interlayer A is filled with high-temperature silicone oil, and the high-temperature silicone oil heats the body A. The port of the body A is fixedly connected to the cover plate A by bolts, and a sealing ring is provided between the body A and the cover plate A.

[0018] A feeding port A is provided on one side of the center of the cover A, and a temperature sensor through hole A is provided on the other side of the center of the cover A; the temperature measuring end of the temperature sensor A passes through the temperature sensor through hole A at the lower part of the inner cavity of the body A, and the wiring terminal of the sensor A is externally connected to the speed regulator A. A stirrer through hole A is provided at the center of the cover A, and the lower end of the stirrer A passes through the stirrer through hole A at the lower part of the inner cavity of the body A, and a stirring paddle A is provided at the lower end of the stirrer A, and the upper end of the stirrer A is connected to the output shaft of the motor A through a coupling, and the wiring terminal of the motor A is externally connected to the speed regulator A.

[0019] The upper part of one side of the circular wall outer surface of the body A is provided with an oil outlet of the molten salt device, and the lower part of the other side of the circular wall outer surface of the body A is provided with an oil inlet of the molten salt device; a discharge port is provided at the bottom center of the body A, and the discharge port is equipped with a discharge pipe and a molten salt output pipe, a first discharge valve is provided at the pipe mouth of the discharge pipe, and a second discharge valve is provided at the pipe mouth of the molten salt output pipe. The oil outlet of the molten salt device is connected to the oil bath oil inlet A of the high-temperature circulating oil bath A through the first insulation pipe A, and the oil inlet of the molten salt device is connected to the oil bath oil outlet A of the high-temperature circulating oil bath A through the second insulation pipe A.

[0020] Furthermore, the chlorination device is composed of a speed regulator B, an agitator B, a body B, a cover plate B, a temperature sensor B and a motor B.

[0021] The body B is a double-layer cylinder, with an interlayer B between the outer wall and the inner wall of the body B, and high-temperature silicone oil is contained in the interlayer B, which heats the body B. The port of the body B is fixedly connected to the cover plate B by bolts, and a sealing ring is provided between the body B and the cover plate B.

[0022] One side of the center of the cover plate B is provided with a molten salt input port, an air inlet B and a feed port B in sequence from outside to inside, and the other side of the center of the cover plate B is provided with a temperature sensor through hole B and an air outlet B in sequence from inside to outside; the temperature measuring end of the temperature sensor B passes through the temperature sensor through hole B at the lower part of the inner cavity of the body B, and the wiring terminal of the temperature sensor B is externally connected to the speed regulator B. A stirrer through hole B is provided at the center of the cover plate B, the lower end of the stirrer B passes through the stirrer through hole B at the lower part of the inner cavity of the body B, a stirring paddle B is provided at the lower end of the stirrer B, the upper end of the stirrer B is connected to the output shaft of the motor B through a coupling, and the wiring terminal of the motor B is externally connected to the speed regulator B.

[0023] An oil outlet of the chlorination device is arranged at the upper part of one side of the circular wall outer surface of the body B, and an oil inlet of the chlorination device is arranged at the lower part of the other side of the circular wall outer surface of the body B; a slag discharge pipe is arranged at the bottom center of the body B, and a slag discharge valve is arranged at the pipe mouth of the slag discharge pipe.

[0024] The oil outlet of the chlorination device is connected to the oil bath oil inlet B of the high-temperature circulating oil bath B through the first insulation pipe B, and the oil inlet of the chlorination device is connected to the oil bath oil outlet B of the high-temperature circulating oil bath B through the second insulation pipe B.

[0025] Furthermore, the condensing device consists of a collecting tank and a condenser.

[0026] The collecting tank is a hollow sphere, a collecting pipe is arranged at the bottom of the hollow sphere, a collecting valve is arranged at the pipe mouth of the collecting pipe, an air inlet C is arranged on the left side of the hollow sphere, and an air outlet C is arranged on the upper part of the hollow sphere.

[0027] The condenser consists of a condenser tube shell, a serpentine condenser tube and an exhaust gas collecting tube, wherein the serpentine condenser tube and the exhaust gas collecting tube are coaxially installed in the condenser tube shell; the lower port of the serpentine condenser tube passes through the lower part of the condenser tube shell, and the lower port of the serpentine condenser tube is the liquid inlet, and the upper port of the serpentine condenser tube passes through the upper part of the condenser tube shell, and the upper port of the serpentine condenser tube is the liquid outlet; the liquid inlet is externally connected to the liquid outlet pipe of the low-temperature coolant circulator, and the liquid outlet is externally connected to the liquid inlet pipe of the low-temperature coolant circulator.

[0028] The gas outlet C of the collecting tank is fixedly connected to the lower end of the condenser tube shell of the condenser.

[0029] The molten salt output pipe of the molten salt device is connected with the molten salt input port of the chlorination device through the first pipeline B, and the prepared molten salt is output from the molten salt output pipe and enters the chlorination device from the molten salt input port through the first pipeline B; the gas outlet B of the chlorination device is connected with the gas inlet C of the collection tank through the second pipeline B, and the prepared vanadium trichloride gas is output from the gas outlet B and enters the condensation device from the gas inlet C through the second pipeline B.

[0030] The inner wall material of the molten salt device is one of quartz material, ceramic material and Hastelloy material.

[0031] The inner wall material of the chlorination device is one of quartz material, ceramic material and Hastelloy material.

[0032] The distance from the lower surface of the stirring paddle A to the bottom of the body A is 0.1 to 0.3 times the height of the inner wall of the body A; the blade radius of the stirring paddle A is 0.4 to 0.6 times the radius of the inner cavity of the body A.

[0033] The distance from the lower surface of the stirring paddle B to the bottom of the body B is 0.1 to 0.2 times the height of the inner wall of the body B; the blade radius of the stirring paddle B is 0.5 to 0.7 times the radius of the inner cavity of the body B.

[0034] The length of the condenser of the condensing device is 3 to 5 times the diameter of the inner cavity of the collecting tank.

[0035] The motor A is located directly above the center of the cover plate A of the molten salt device, and the motor A is fixedly connected to the cover plate A through a support frame.

[0036] The motor B is located directly above the center of the cover plate B of the molten salt device, and the motor B is fixedly connected to the cover plate B through a support frame.

[0037] The seal of the lower end of the agitator A passing through the agitator through hole A is a dynamic seal.

[0038] The seal of the lower end of the agitator B passing through the agitator through hole B is a dynamic seal.

[0039] Due to the adoption of the above technical solution, the present invention has the following positive effects compared with the prior art:

[0040] 1. The structure of the present invention adopts a multifunctional integrated design, that is, the molten salt device, the chlorination device and the condensation device are integrated into one. Compared with the traditional series-connected reaction device, it occupies a small space, uses fewer pipes and valves, is not easy to leak vanadium oxychloride gas, has enhanced safety and is easy for industrial production.

[0041] 2. The molten salt device and chlorination device provided in the present invention can realize the regional heating reaction. Compared with the integrated chlorination reaction device in the prior art, it can prevent the molten salt from partially volatilizing due to heat during the preparation process, and prevent the volatilized chloride from adhering to the inner wall of the chlorination reaction device and entering the vanadium trichloride gas, thereby effectively inhibiting the reduction of the purity of the reaction product. Therefore, the product prepared by the present invention has high purity; in addition, the enrichment and purification of vanadium by chlorination reaction requires a reaction temperature of 170°C to 200°C, and the temperature of molten salt preparation is 100°C to 350°C. The regional heating reaction can avoid the molten salt preparation temperature being limited by the chlorination reaction temperature, and has strong adaptability to molten salt.

[0042] 3. In the present invention, agitators A and agitators B are correspondingly provided in the molten salt device and the chlorination device. The corresponding agitators A and B are driven by motors A and B to increase the contact area between the molten salt and the molten salt, and between the vanadium-containing raw material and the molten salt, thereby improving the molten salt preparation efficiency and the chlorination efficiency and making the reaction more complete.

[0043] Therefore, the present invention has the characteristics of strong adaptability to molten salt, high molten salt preparation efficiency and chlorination efficiency, sufficient reaction, high product purity, economic safety and easy industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 It is a structural schematic diagram of the present invention;

[0045] Figure 2 It is an enlarged schematic diagram of a molten salt device 2 in the present invention;

[0046] Figure 3 It is an enlarged schematic diagram of a high-temperature circulating oil bath A1 in the present invention;

[0047] Figure 4 It is an enlarged schematic diagram of a chlorination device 4 in the present invention;

[0048] Figure 5 It is an enlarged schematic diagram of another high-temperature circulating oil bath B3 in the present invention;

[0049] Figure 6 It is an enlarged schematic diagram of a condensing device 5 in the present invention. DETAILED DESCRIPTION

[0050] The present invention is further described below in conjunction with the accompanying drawings and specific embodiments, but is not intended to limit the scope of protection thereof.

[0051] Example 1

[0052] A molten salt chlorination distillation reaction device for enriching and purifying vanadium. The molten salt chlorination distillation reaction device for enriching and purifying vanadium is as follows Figure 1 As shown, it includes four parts: a molten salt device 2, a chlorination device 4, a condensation device 5 and a high-temperature circulating oil bath device; the high-temperature circulating oil bath device includes a high-temperature circulating oil bath A1 and a high-temperature circulating oil bath B3.

[0053] The molten salt device 2 is a sandwich tank with a stirring function, with at least a feeding port A7 disposed on the top and at least a discharge pipe 12 and a molten salt output pipe 14 disposed on the bottom.

[0054] The chlorination device 4 is a sandwich tank with a stirring function, and is at least provided with a molten salt input port 25, a feed port B23 and a gas outlet B35 on the top, and at least provided with a slag discharge pipe 30 on the bottom.

[0055] A condensation device 5, connected to the gas outlet B35, for condensing the gas evaporated from the chlorination device 4; and

[0056] The high temperature circulating oil bath device is used to perform oil bath heating on the interlayers of the molten salt device 2 and the chlorination device 4 respectively.

[0057] The structure of the molten salt device 2 is as follows Figure 2 As shown: It consists of a speed regulator A6, an agitator A10, a body A11, a temperature sensor A17, a cover A18 and a motor A19.

[0058] like Figure 2 As shown, the body A11 is a double-layer cylinder, and an interlayer A9 is provided between the outer wall and the inner wall of the body A11. The interlayer A9 is filled with high-temperature silicone oil, and the high-temperature silicone oil heats the body A11. The port of the body A11 is fixedly connected to the cover plate A18 by bolts, and a sealing ring is provided between the body A11 and the cover plate A18.

[0059] like Figure 2As shown, a feeding port A7 is provided on one side of the center of the cover A18, and a temperature sensor through hole A is provided on the other side of the center of the cover A18; the temperature measuring end of the temperature sensor A17 passes through the temperature sensor through hole A at the lower part of the inner cavity of the body A11, and the wiring terminal of the sensor A17 is externally connected to the speed regulator A6. A stirrer through hole A is provided at the center of the cover A18, and the lower end of the stirrer A10 passes through the stirrer through hole A at the lower part of the inner cavity of the body A11, and a stirring paddle A is provided at the lower end of the stirrer A10, and the upper end of the stirrer A10 is connected to the output shaft of the motor A19 through a coupling, and the wiring terminal of the motor A19 is externally connected to the speed regulator A6.

[0060] like Figure 2 As shown, an oil outlet 8 of a molten salt device is provided at the upper part of one side of the circular wall outer surface of the main body A11, and an oil inlet 16 of a molten salt device is provided at the lower part of the other side of the circular wall outer surface of the main body A11; a discharge port is provided at the bottom center of the main body A11, and a discharge pipe 12 and a molten salt output pipe 14 are installed at the discharge port, a first discharge valve 13 is provided at the pipe mouth of the discharge pipe 12, and a second discharge valve 15 is provided at the pipe mouth of the molten salt output pipe 14.

[0061] like Figure 1 , Figure 2 and Figure 3 As shown, the oil outlet 8 of the molten salt device is connected to the oil bath oil inlet A20 of the high-temperature circulating oil bath A1 through the first insulation pipe A, and the oil inlet 16 of the molten salt device is connected to the oil bath oil outlet A21 of the high-temperature circulating oil bath A1 through the second insulation pipe A.

[0062] The structure of the chlorination device 4 is as follows Figure 4 As shown: It consists of a speed regulator B36, an agitator B28, a body B29, a cover plate B34, a temperature sensor B33 and a motor B22.

[0063] like Figure 4 As shown, the body B29 is a double-layer cylinder, and an interlayer B27 is provided between the outer wall and the inner wall of the body B29. The interlayer B27 is filled with high-temperature silicone oil, and the high-temperature silicone oil heats the body B29. The port of the body B29 is fixedly connected to the cover plate B34 by bolts, and a sealing ring is provided between the body B29 and the cover plate B34.

[0064] like Figure 4As shown, one side of the center of the cover plate B34 is provided with a molten salt input port 25, an air inlet B24 and a feed port B23 from outside to inside, and the other side of the center of the cover plate B34 is provided with a temperature sensor through hole B and an air outlet B35 from inside to outside; the temperature measuring end of the temperature sensor B33 passes through the temperature sensor through hole B at the lower part of the inner cavity of the body B29, and the connection terminal of the temperature sensor B33 is externally connected to the speed regulator B36. A stirrer through hole B is provided at the center of the cover plate B34, and the lower end of the stirrer B28 passes through the stirrer through hole B at the lower part of the inner cavity of the body B29, and a stirring paddle B is provided at the lower end of the stirrer B28. The upper end of the stirrer B28 is connected to the output shaft of the motor B22 through a coupling, and the connection terminal of the motor B22 is externally connected to the speed regulator B36.

[0065] like Figure 4 As shown, an oil outlet 26 of a chlorination device is provided at the upper part of one side of the circular wall outer surface of the body B29, and an oil inlet of a chlorination device is provided at the lower part of the other side of the circular wall outer surface of the body B29; a slag discharge pipe 30 is provided at the bottom center of the body B29, and a slag discharge valve 31 is provided at the mouth of the slag discharge pipe 30.

[0066] like Figure 1 , Figure 4 and Figure 5 As shown, the oil outlet 26 of the chlorination device is connected to the oil bath oil inlet B37 of the high-temperature circulating oil bath B3 through the first insulation pipe B, and the oil inlet 32 ​​of the chlorination device is connected to the oil bath oil outlet B38 of the high-temperature circulating oil bath B3 through the second insulation pipe B.

[0067] The condensing device 5 has a structure as follows Figure 6 As shown: it consists of a collecting tank 44 and a condenser 39.

[0068] like Figure 6 As shown, the collecting tank 44 is a hollow sphere, a collecting pipe 42 is provided at the bottom of the hollow sphere, a collecting valve 43 is provided at the mouth of the collecting pipe 42, an air inlet C41 is provided on the left side of the hollow sphere, and an air outlet C45 is provided on the upper part of the hollow sphere.

[0069] like Figure 6 As shown, the condenser 39 is composed of a condenser tube shell 46, a serpentine condenser tube 47 and an exhaust gas collecting tube 40, wherein the serpentine condenser tube 47 and the exhaust gas collecting tube 40 are coaxially installed in the condenser tube shell 46; the lower port of the serpentine condenser tube 47 passes through the lower part of the condenser tube shell 46, and the lower port of the serpentine condenser tube 47 is a liquid inlet, and the upper port of the serpentine condenser tube 47 passes through the upper part of the condenser tube shell 46, and the upper port of the serpentine condenser tube 47 is a liquid outlet; the liquid inlet is externally connected to the liquid outlet pipe of the low-temperature coolant circulator, and the liquid outlet is externally connected to the liquid inlet pipe of the low-temperature coolant circulator.

[0070] like Figure 6As shown, the gas outlet C45 of the collecting tank 44 is fixedly connected to the lower end of the condenser tube shell 46 of the condenser 39 .

[0071] like Figure 1 , Figure 2 , Figure 4 and Figure 6 As shown, the molten salt output pipe 14 of the molten salt device 2 is connected with the molten salt input port 25 of the chlorination device 4 through the first pipeline B, and the prepared molten salt flows out from the molten salt output pipe 14 and enters the chlorination device 4 from the molten salt input port 25 through the first pipeline B; the gas outlet B35 of the chlorination device 4 is connected with the gas inlet C41 of the collection tank 44 through the second pipeline B, and the prepared vanadium trichloride gas is output from the gas outlet B35 and enters the condensation device 5 from the gas inlet C41 through the second pipeline B.

[0072] The inner wall of the molten salt device 2 is made of quartz material.

[0073] The inner wall of the chlorination device 4 is made of quartz material.

[0074] like Figure 2 As shown, the distance from the lower surface of the stirring paddle A to the bottom of the body A11 is 0.1 times the height of the inner wall of the body A11; the blade radius of the stirring paddle A is 0.4 times the radius of the inner cavity of the body A11.

[0075] like Figure 4 As shown, the distance from the lower surface of the stirring paddle B to the bottom of the body B29 is 0.1 times the height of the inner wall of the body B29; the blade radius of the stirring paddle B is 0.5 times the radius of the inner cavity of the body B29.

[0076] like Figure 6 As shown, the length of the condenser 39 of the condensing device 5 is three times the diameter of the inner cavity of the collecting tank 44 .

[0077] like Figure 1 and Figure 2 As shown, the motor A19 is located directly above the center of the cover A18 of the molten salt device 2, and the motor A19 is fixedly connected to the cover A18 through a support frame.

[0078] like Figure 1 and Figure 4 As shown, the motor B22 is located directly above the center of the cover plate B34 of the molten salt device 2, and the motor B22 is fixedly connected to the cover plate B34 through a support frame.

[0079] like Figure 2 As shown, the seal of the lower end of the agitator A10 passing through the agitator through hole A is a dynamic seal.

[0080] like Figure 4 As shown, the seal of the lower end of the agitator B28 passing through the agitator through hole B is a dynamic seal.

[0081] Example 2

[0082] A molten salt chlorination distillation reaction device for enriching and purifying vanadium. The molten salt chlorination distillation reaction device described in this embodiment is the same as that in embodiment 1 except for the following technical parameters:

[0083] The inner wall of the molten salt device 2 is made of ceramic material.

[0084] The inner wall of the chlorination device 4 is made of ceramic material.

[0085] The distance from the lower surface of the stirring paddle A to the bottom of the body A11 is 0.2 times the height of the inner wall of the body A11; the blade radius of the stirring paddle A is 0.5 times the radius of the inner cavity of the body A11.

[0086] The distance from the lower surface of the stirring paddle B to the bottom of the body B29 is 0.15 times the height of the inner wall of the body B29; the blade radius of the stirring paddle B is 0.6 times the radius of the inner cavity of the body B29.

[0087] The length of the condenser 39 of the condensing device 5 is 4 times the diameter of the inner cavity of the collecting tank 44 .

[0088] Example 3

[0089] A molten salt chlorination distillation reaction device for enriching and purifying vanadium. The molten salt chlorination distillation reaction device described in this embodiment is the same as that in embodiment 1 except for the following technical parameters:

[0090] The inner wall material of the molten salt device 2 is Hastelloy alloy.

[0091] The inner wall material of the chlorination device 4 is Hastelloy alloy.

[0092] The distance from the lower surface of the stirring paddle A to the bottom of the body A11 is 0.3 times the height of the inner wall of the body A11; the blade radius of the stirring paddle A is 0.6 times the radius of the inner cavity of the body A11.

[0093] The distance from the lower surface of the stirring paddle B to the bottom of the body B29 is 0.2 times the height of the inner wall of the body B29; the blade radius of the stirring paddle B is 0.7 times the radius of the inner cavity of the body B29.

[0094] The length of the condenser 39 of the condensing device 5 is 5 times the diameter of the inner cavity of the collecting tank 44 .

[0095] Compared with the prior art, this specific implementation has the following positive effects:

[0096] 1. This specific implementation method adopts a multifunctional integrated design in structure, that is, the molten salt device 2, the chlorination device 4 and the condensation device are integrated into one. Compared with the traditional series-connected reaction device, it occupies a small space, uses fewer pipes and valves, is not easy to leak vanadium trichloride gas, has enhanced safety and is easy for industrial production.

[0097] 2. The molten salt device 2 and chlorination device 4 provided in this specific embodiment can realize the heating reaction in different regions. Compared with the integrated chlorination reaction device in the prior art, it can prevent the molten salt from partially volatilizing due to heat during the preparation process, and prevent the volatilized chloride from adhering to the inner wall of the chlorination reaction device and entering the vanadium trichloride gas, thereby effectively inhibiting the reduction of the purity of the reaction product. Therefore, the product prepared in this specific embodiment has high purity; in addition, the enrichment and purification of vanadium by chlorination reaction requires a reaction temperature of 170°C to 200°C, and the temperature of molten salt preparation is 100°C to 350°C. The heating reaction in different regions can avoid the molten salt preparation temperature being limited by the chlorination reaction temperature, and has strong adaptability to molten salt.

[0098] 3. In this specific embodiment, agitators A10 and B28 are correspondingly provided in the molten salt device 2 and the chlorination device 4. The corresponding agitators A10 and B28 are driven by motors A19 and B22 to increase the contact area between the molten salt and the molten salt, and between the vanadium-containing raw material and the molten salt, thereby improving the molten salt preparation efficiency and the chlorination efficiency and making the reaction more complete.

[0099] Therefore, the present specific implementation mode has the characteristics of strong adaptability to molten salt, high molten salt preparation efficiency and chlorination efficiency, sufficient reaction, high product purity, economic safety and easy industrial production.

Claims

1. A molten salt chlorination distillation reaction device for enriching and purifying vanadium, characterized in that: include The molten salt device (2) is a sandwich tank with a stirring function, with at least a feeding port A (7) arranged at the top and at least a discharge pipe (12) and a molten salt output pipe (14) arranged at the bottom; The chlorination device (4) is a sandwich tank with a stirring function, the top of which is at least provided with a molten salt input port (25), a feed port B (23) and a gas outlet B (35), and the bottom of which is at least provided with a slag discharge pipe (30); A condensation device (5), connected to the gas outlet B (35), for condensing the gas evaporated from the chlorination device (4); as well as The high-temperature circulating oil bath device is used to perform oil bath heating on the interlayers of the molten salt device (2) and the chlorination device (4).

2. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 1, characterized in that: The molten salt device (2) is composed of a speed regulator A (6), an agitator A (10), a body A (11), a temperature sensor A (17), a cover plate A (18) and a motor A (19); The body A (11) is in a double-layer cylindrical shape, and an interlayer A (9) is provided between the outer wall and the inner wall of the body A (11), and the interlayer A (9) is filled with high-temperature silicone oil, and the high-temperature silicone oil heats the body A (11); the port of the body A (11) is fixedly connected to the cover plate A (18) by bolts, and a sealing ring is provided between the body A (11) and the cover plate A (18); A feeding port A (7) is provided on one side of the center of the cover plate A (18), and a temperature sensor through hole A is provided on the other side of the center of the cover plate A (18); a temperature measuring end of the temperature sensor A (17) passes through the temperature sensor through hole A at the lower part of the inner cavity of the body A (11), and a connection terminal of the sensor A (17) is externally connected to a speed regulator A (6); a stirrer through hole A is provided at the center of the cover plate A (18), and a lower end of the stirrer A (10) passes through the stirrer through hole A at the lower part of the inner cavity of the body A (11), and a stirring paddle A is provided at the lower end of the stirrer A (10), and an upper end of the stirrer A (10) is connected to an output shaft of a motor A (19) through a coupling, and a connection terminal of the motor A (19) is externally connected to a speed regulator A (6); An oil outlet (8) of a molten salt device is provided at the upper portion of one side of the circular wall outer surface of the body A (11), and an oil inlet (16) of a molten salt device is provided at the lower portion of the other side of the circular wall outer surface of the body A (11); a discharge port is provided at the center of the bottom of the body A (11), and a discharge pipe (12) and a molten salt output pipe (14) are installed at the discharge port; a first discharge valve (13) is provided at the pipe mouth of the discharge pipe (12), and a second discharge valve (15) is provided at the pipe mouth of the molten salt output pipe (14).

3. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 2, characterized in that: The chlorination device (4) is composed of a speed regulator B (36), a stirrer B (28), a body B (29), a cover plate B (34), a temperature sensor B (33) and a motor B (22); The body B (29) is in a double-layer cylindrical shape. An interlayer B (27) is provided between the outer wall and the inner wall of the body B (29). High-temperature silicone oil is contained in the interlayer B (27). The high-temperature silicone oil heats the body B (11). The port of the body B (29) is fixedly connected to the cover plate B (34) by bolts. A sealing ring is provided between the body B (29) and the cover plate B (34). A molten salt input port (25), an air inlet B (24) and a feeding port B (23) are sequentially arranged on one side of the center of the cover plate B (34) from outside to inside, and a temperature sensor through hole B and an air outlet B (35) are sequentially arranged on the other side of the center of the cover plate B (34) from inside to outside; a temperature measuring end of the temperature sensor B (33) passes through the temperature sensor through hole B at the lower part of the inner cavity of the body B (29), and a connection terminal of the temperature sensor B (33) is externally connected to a speed regulator B (36); a stirrer through hole B is arranged at the center of the cover plate B (34), a lower end of the stirrer B (28) passes through the stirrer through hole B at the lower part of the inner cavity of the body B (29), a stirring paddle B is arranged at the lower end of the stirrer B (28), an upper end of the stirrer B (28) is connected to an output shaft of a motor B (22) through a coupling, and a connection terminal of the motor B (22) is externally connected to a speed regulator B (36); An oil outlet (26) for a chlorination device is provided at the upper portion of one side of the circular wall outer surface of the body B (29), and an oil inlet (32) for a chlorination device is provided at the lower portion of the other side of the circular wall outer surface of the body B (29); a slag discharge pipe (30) is provided at the center of the bottom of the body B (29), and a slag discharge valve (31) is provided at the pipe mouth of the slag discharge pipe (30).

4. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 3, characterized in that: The condensing device (5) is composed of a collecting tank (44) and a condenser (39); The collecting tank (44) is a hollow sphere, a collecting pipe (42) is provided at the bottom of the hollow sphere, a collecting valve (43) is provided at the pipe mouth of the collecting pipe (42), an air inlet C (41) is provided on the left side of the hollow sphere, and an air outlet C (45) is provided on the upper part of the hollow sphere; The condenser (39) is composed of a condenser tube shell (46), a serpentine condenser tube (47) and an exhaust gas collecting tube (40), wherein the serpentine condenser tube (47) and the exhaust gas collecting tube (40) are coaxially installed in the condenser tube shell (46); the lower port of the serpentine condenser tube (47) passes through the lower part of the condenser tube shell (46), and the lower port of the serpentine condenser tube (47) is a liquid inlet; the upper port of the serpentine condenser tube (47) passes through the upper part of the condenser tube shell (46), and the upper port of the serpentine condenser tube (47) is a liquid outlet; the liquid inlet is externally connected to the liquid outlet pipe of the low-temperature coolant circulator, and the liquid outlet is externally connected to the liquid inlet pipe of the low-temperature coolant circulator; The gas outlet C (45) of the collecting tank (44) is fixedly connected to the lower end of the condenser tube shell (46) of the condenser (39).

5. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 4, characterized in that: The high temperature circulating oil bath device comprises a high temperature circulating oil bath A (1) and a high temperature circulating oil bath B (3); The oil outlet (8) of the molten salt device is connected to the oil bath oil inlet (20) of the high-temperature circulating oil bath A (1) through the first insulation pipe A, and the oil inlet (16) of the molten salt device is connected to the oil bath oil outlet (21) of the high-temperature circulating oil bath A (1) through the second insulation pipe A; The oil outlet (26) of the chlorination device is communicated with the oil bath oil inlet (37) of the high-temperature circulating oil bath B (3) through the first insulation pipe B, and the oil inlet (32) of the chlorination device is communicated with the oil bath oil outlet (38) of the high-temperature circulating oil bath B (3) through the second insulation pipe B.

6. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 5, characterized in that: The molten salt output pipe (14) of the molten salt device (2) is connected to the molten salt input port (25) of the chlorination device (4) through a first pipe B, and the prepared molten salt is output from the molten salt output pipe (14) and enters the chlorination device (4) from the molten salt input port (25) through the first pipe B; the gas outlet B (35) of the chlorination device (4) is connected to the gas inlet C (41) of the collection tank (44) through a second pipe B, and the prepared vanadium oxychloride gas is output from the gas outlet B (35) and enters the condensation device (5) from the gas inlet C (41) through the second pipe B.

7. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to any one of claims 1 to 6, characterized in that: The inner wall materials of the molten salt device (2) and the chlorination device (4) are both one of quartz material, ceramic material and Hastelloy material.

8. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 6, characterized in that: The distance from the lower surface of the stirring paddle A to the bottom of the body A (11) is 0.1 to 0.3 times the height of the inner wall of the body A (11); the blade radius of the stirring paddle A is 0.4 to 0.6 times the radius of the inner cavity of the body A (11).

9. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 6, characterized in that: The distance from the lower surface of the stirring paddle B to the bottom of the body B (29) is 0.1 to 0.2 times the height of the inner wall of the body B (29); the blade radius of the stirring paddle B is 0.5 to 0.7 times the radius of the inner cavity of the body B (29).

10. The molten salt chlorination distillation reaction device for enriching and purifying vanadium according to claim 6, characterized in that: The length of the condenser (39) of the condensation device (5) is 3 to 5 times the diameter of the inner cavity of the collection tank (44).

Images