Method for preparing low-valence titanium chloride by gaseous TiCl4 molten salt method

Abstract

The invention relates to a method for preparing low-valence titanium chloride from gaseous TiCl4 through a molten salt method, and belongs to the technical field of titanium metallurgy. The low-valence titanium chloride preparation device comprises a TiCl4 gasification unit, an argon current-carrying conveying unit and a molten salt reaction unit, crude titanium and chloride molten salt are added into the molten salt reaction unit, the chloride molten salt is heated to 500-800 DEG C through the molten salt reaction unit, liquid molten salt is kept, and the liquid molten salt is located above a crude titanium solid phase; the method comprises the following steps: heating liquid TiCl4 to the temperature of 150-200 DEG C through a TiCl4 gasification unit, and gasifying the liquid TiCl4 into TiCl4 steam; tiCl4 steam is introduced into liquid molten salt of the molten salt reaction unit at a constant speed through argon flow of the argon current-carrying conveying unit, a gas-solid-liquid three-phase interface reaction system is constructed in a normal-pressure inert atmosphere, and the TiCl4 steam and crude titanium in the liquid molten salt are subjected to a multi-phase reduction reaction at the temperature of 500-800 DEG C to obtain low-valence titanium chlorides (TiCl3 and TiCl2). The method is suitable for providing a stable and efficient low-valence titanium chloride raw material for preparing high-purity metal titanium through a fused salt electrolysis method.

Description

Technical Field

[0001] The invention relates to a method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, belonging to the technical field of titanium metallurgy. Background Art

[0002] Due to its excellent specific strength, corrosion resistance, and biocompatibility, titanium metal is widely used in high-end manufacturing fields such as aerospace, military, chemical, and medical, and is hailed as the "metal of the future." Current industrial production primarily relies on the Kroll process, which uses TiCl4 as the raw material and produces sponge titanium through a magnesium-thermal reduction reaction. Although this process is relatively mature in industry, it suffers from complex procedures, high energy consumption, and severe pollution, making it difficult to meet the urgent demand for green and efficient metallurgical processes. Therefore, the development of new, low-energy, environmentally friendly, and continuously operational titanium extraction and purification technologies has become a research hotspot in this field.

[0003] In recent years, electrochemical titanium extraction and electrolytic refining technology based on molten salt system has developed rapidly. This method can effectively remove impurity elements such as Fe, Cr, O, and N by electrolyzing crude titanium or sponge titanium in molten chloride, thereby preparing high-purity metallic titanium. It has the advantages of short process, low energy consumption, and environmental friendliness, showing good application prospects. However, in actual operation, due to the low-valent titanium ions (Ti 2+ 、Ti 3+ ) concentration is low and unevenly distributed, which leads to the easy generation of metallic titanium doped with impurities during the cathode deposition process, seriously affecting the purity and overall performance of the product.

[0004] Studies have shown that the type, concentration and distribution of low-valent titanium ions are key factors affecting the behavior of titanium electrodeposition and the quality of finished products. 2+ or Ti 3+ The concentration of titanium ions can help improve the nucleation and crystallization behavior of titanium, thereby increasing current efficiency and product density. Currently, common methods for introducing low-valent titanium ions include using crude titanium as a soluble anode or adding titanium-containing salts such as K2TiF6 and TiCl3 to the molten salt system. However, these methods often have problems such as low dissolution efficiency, high risk of impurity introduction, and difficulty in concentration control, making it difficult to achieve precise regulation and stable supply of titanium ions in the molten salt.

[0005] Therefore, there is an urgent need to develop a molten salt electrolysis method with a reasonable structure, safe operation and high reaction efficiency to achieve the efficient preparation and precise control of low-valent titanium chloride in molten salt. Summary of the Invention

[0006] In view of the insufficient reaction between TiCl4 and titanium metal, 3+ or Ti 2+The present invention solves the technical problems of low generation rate, large fluctuation of product concentration, and difficulty in meeting the requirements of electrolyte component stability and controllability in the process of high-purity titanium refining. The present invention proposes a method for preparing low-valent titanium chloride by gaseous TiCl4 molten salt method, which gasifies TiCl4 into TiCl4 vapor and carries it into the chloride molten salt containing crude titanium through carrier gas argon to react with crude titanium metal in situ, so that TiCl4 is rapidly generated and stably exists in the molten salt system. 3+ or Ti 2+ , thereby achieving efficient regulation of the concentration and type of low-valent titanium ions, providing high-quality precursor conditions for subsequent electrochemical refining or deposition processes.

[0007] A method for preparing low-valent titanium chloride by a gaseous TiCl4 molten salt method, using a low-valent titanium chloride preparation device, the low-valent titanium chloride preparation device comprising a TiCl4 gasification unit, an argon carrier flow transport unit and a molten salt reaction unit; The specific steps of the method are as follows: S1. Adding crude titanium and chloride molten salt to a molten salt reaction unit, heating the chloride molten salt to 500-800°C through the molten salt reaction unit to maintain the liquid molten salt, with the liquid molten salt located above the crude titanium solid phase; the initial crystallization temperature of the chloride molten salt is 450-750°C, and the heating temperature of the chloride molten salt is higher than the initial crystallization temperature of the chloride molten salt; S2. The liquid TiCl4 is heated to a temperature of 150-200°C by a TiCl4 gasification unit to be gasified into TiCl4 vapor; S3. TiCl4 vapor is uniformly introduced into the liquid molten salt of the molten salt reaction unit through the argon flow of the argon carrier flow transport unit, and a gas-solid-liquid three-phase interface reaction system is constructed in an inert atmosphere at normal pressure. The TiCl4 vapor undergoes a multiphase reduction reaction with the crude titanium in the liquid molten salt at a temperature of 500-800°C to obtain low-valent titanium chloride.

[0008] Preferably, the chloride molten salt in step S1 is one or more of NaCl, KCl, MgCl2, CaCl2 or LiCl.

[0009] Preferably, the crude titanium is sponge titanium or scrap titanium.

[0010] Preferably, in step S3, the argon flow rate is 3-10 mL / min.

[0011] Preferably, the TiCl4 gasification unit includes a heating device 2 and a TiCl4 storage tank 3. The TiCl4 storage tank 3 is placed in the heating zone of the heating device 2. A temperature sensor I is provided on the inner side wall of the TiCl4 storage tank 3. The temperature sensor I is externally connected to a temperature controller I. The temperature controller I is electrically connected to the heater of the heating device 2. The top cover of the TiCl4 storage tank 3 is provided with a carrier gas inlet and a TiCl4 vapor outlet. The TiCl4 storage tank 3 is filled with liquid TiCl4. The argon carrier flow delivery unit includes an argon tube 1, a TiCl4 vapor delivery tube 4, a gas flow control valve 5 and a gas delivery tube 6, the two ends of the argon tube 1 are respectively A end and B end, the A end of the argon tube 1 is externally connected to the carrier gas tank, the B end of the argon tube 1 passes through the carrier gas inlet of the top cover of the TiCl4 storage tank 3 and extends downward to above the liquid TiCl4, the argon tube 1 is provided with a flow meter, the two ends of the TiCl4 vapor delivery tube 4 are respectively A' end and B' end, the A' end of the TiCl4 vapor delivery tube 4 is connected to the TiCl4 vapor outlet of the top cover of the TiCl4 storage tank 3, the B' end of the TiCl4 vapor delivery tube 4 is connected to the gas inlet of the gas flow control valve 5, the two ends of the gas delivery tube 6 are respectively A" end and B" end, and the A" end of the gas delivery tube 6 is connected to the gas outlet of the gas flow control valve 5; The molten salt reaction unit includes a heating furnace body 7 and a molten salt reactor 8. The molten salt reactor 8 is filled with crude titanium 9 and chloride molten salt 10. The molten salt reactor 8 is placed in the heating zone of the heating furnace body 7. A gas through hole is opened in the center of the top cover of the heating furnace body 7. The B" end of the gas pipe 6 passes through the gas through hole and extends downward into the crude titanium 9. A temperature sensor II is provided on the inner side wall of the molten salt reactor 8. The temperature sensor II is externally connected to a temperature controller II, and the temperature controller II is electrically connected to the heater of the heating furnace body 7.

[0012] The beneficial effects of the present invention are: (1) The present invention uses gaseous TiCl4 to directly react with metallic titanium in molten salt. The reaction is violent and the conversion rate is fast. High concentrations of divalent and trivalent titanium ions can be generated in a short time, significantly improving the efficiency of raw material preparation. (2) The present invention achieves the continuous generation and stable existence of low-valent titanium ions by regulating the TiCl4 gasification temperature, the conveying air flow rate and the crude titanium ratio, thereby meeting the dynamic demand for titanium source concentration in the subsequent molten salt electrolysis process; (3) The present invention constructs a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. TiCl4 vapor undergoes a multiphase reduction reaction with crude titanium in liquid molten salt to obtain low-valent titanium chloride, which can avoid a complex vacuum system, simplify the operation process, and reduce equipment costs and operating risks. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 This is a schematic diagram of a device for preparing low-valent titanium chloride; In the figure, 1-argon pipe, 2-heating device, 3-TiCl4 storage tank, 4-TiCl4 steam transmission pipe, 5-gas flow control valve, 6-gas transmission pipe, 7-heating furnace body, 8-molten salt process reactor, 9-crude titanium, 10-chloride molten salt. DETAILED DESCRIPTION

[0014] The present invention will be further described in detail below in conjunction with specific embodiments, but the protection scope of the present invention is not limited to the contents described above.

[0015] The method for preparing low-valent titanium chloride by a gaseous TiCl4 molten salt method according to an embodiment of the present invention adopts a low-valent titanium chloride preparation device, which includes a TiCl4 gasification unit, an argon carrier flow delivery unit and a molten salt reaction unit; The TiCl4 gasification unit includes a heating device 2 and a TiCl4 storage tank 3. The TiCl4 storage tank 3 is placed in the heating zone of the heating device 2. The inner wall of the TiCl4 storage tank 3 is provided with a temperature sensor I. The temperature sensor I is externally connected to a temperature controller I. The temperature controller I is electrically connected to the heater of the heating device 2. The top cover of the TiCl4 storage tank 3 is provided with a carrier gas inlet and a TiCl4 vapor outlet. The TiCl4 storage tank 3 is filled with liquid TiCl4. The argon carrier flow delivery unit includes an argon tube 1, a TiCl4 vapor delivery tube 4, a gas flow control valve 5 and a gas delivery tube 6, the two ends of the argon tube 1 are respectively A end and B end, the A end of the argon tube 1 is externally connected to the carrier gas tank, the B end of the argon tube 1 passes through the carrier gas inlet of the top cover of the TiCl4 storage tank 3 and extends downward to above the liquid TiCl4, the argon tube 1 is provided with a flow meter, the two ends of the TiCl4 vapor delivery tube 4 are respectively A' end and B' end, the A' end of the TiCl4 vapor delivery tube 4 is connected to the TiCl4 vapor outlet of the top cover of the TiCl4 storage tank 3, the B' end of the TiCl4 vapor delivery tube 4 is connected to the gas inlet of the gas flow control valve 5, the two ends of the gas delivery tube 6 are respectively A" end and B" end, and the A" end of the gas delivery tube 6 is connected to the gas outlet of the gas flow control valve 5; The molten salt reaction unit includes a heating furnace body 7 and a molten salt reactor 8. The molten salt reactor 8 is filled with crude titanium 9 and chloride molten salt 10. The molten salt reactor 8 is placed in the heating zone of the heating furnace body 7. A gas through hole is opened in the center of the top cover of the heating furnace body 7. The B" end of the gas pipe 6 passes through the gas through hole and extends downward into the crude titanium 9. A temperature sensor II is provided on the inner side wall of the molten salt reactor 8. The temperature sensor II is externally connected to a temperature controller II, and the temperature controller II is electrically connected to the heater of the heating furnace body 7.

[0016] Example 1: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Crude titanium (sponge titanium) and 300 g of molten chloride salt (a NaCl-KCl mixed salt with a mass ratio of 1:1) are added to a molten salt reaction unit. The molten chloride salt is heated to 750°C in the molten salt reaction unit to maintain the molten salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (sponge titanium) is added in an amount of 8 wt% of the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 150°C and vaporized into TiCl4 vapor by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit via an argon flow (flow rate of 3 mL / min) from an argon carrier flow transport unit, establishing a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. The TiCl4 vapor and crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at 750°C for 16 minutes to produce low-valent titanium chlorides (TiCl3 and TiCl2). The total amount of TiCl4 vapor introduced was 16 wt% of the mass of the chloride molten salt. The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+ The concentration of Ti was 0.21 mol / L; Ti was detected by hydrogen titration. 2+ The concentration is 0.03 mol / L.

[0017] Example 2: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Add crude titanium (scrap titanium, titanium content 96 wt.%) and 300 g of molten chloride salt (a NaCl-KCl mixed salt with a mass ratio of 1:1) to a molten salt reaction unit. Heat the molten chloride salt to 720°C in the molten salt reaction unit to maintain the molten chloride salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (scrap titanium) is added in an amount of 10 wt.% based on the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 180°C and vaporized into TiCl4 vapor by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit through an argon flow (flow rate of 5 mL / min) from an argon carrier flow transport unit, establishing a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. The TiCl4 vapor and crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at 720°C for 3 minutes to produce low-valent titanium chlorides (TiCl3 and TiCl2). The total amount of TiCl4 vapor introduced was 5 wt% of the mass of the chloride molten salt. The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+The concentration of Ti was 0.06 mol / L; Ti was detected by hydrogen titration 2+ The concentration is 0.34 mol / L.

[0018] Example 3: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Crude titanium (sponge titanium) and 300 g of molten chloride salt (a LiCl-KCl mixed salt with a mass ratio of 1:1) are added to a molten salt reaction unit. The molten chloride salt is heated to 520°C in the molten salt reaction unit to maintain the molten salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (sponge titanium) is added in an amount of 10 wt % based on the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 200°C and vaporized into TiCl4 vapor by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit through an argon flow (flow rate of 10 mL / min) from an argon carrier flow transport unit, establishing a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. The TiCl4 vapor and the crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at a temperature of 520°C for 6 minutes to obtain low-valent titanium chlorides (TiCl3 and TiCl2); the total amount of TiCl4 vapor introduced was 20 wt% of the mass of the chloride molten salt; The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+ The concentration of Ti was 0.24 mol / L; Ti was detected by hydrogen titration. 2+ The concentration is 0.04mol / L.

[0019] Example 4: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Crude titanium (sponge titanium) and 300 g of molten chloride salt (MgCl2-LiCl-KCl mixed salt with a mass ratio of 1:1:1) are added to a molten salt reaction unit. The molten chloride salt is heated to 570°C in the molten salt reaction unit to maintain the molten chloride salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (sponge titanium) is added in an amount of 10 wt% of the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 160°C and vaporized into TiCl4 vapor by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit through an argon flow (flow rate of 3 mL / min) from an argon carrier flow transport unit, establishing a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. The TiCl4 vapor and crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at 570°C for 50 minutes to obtain low-valent titanium chlorides (TiCl3 and TiCl2). The total amount of TiCl4 vapor introduced was 50 wt% of the mass of the chloride molten salt. The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+ The concentration of Ti was 0.16 mol / L; Ti was detected by hydrogen titration. 2+ The concentration is 0.18mol / L.

[0020] Example 5: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Add crude titanium (scrap titanium material, titanium content 92 wt.%) and 300 g of molten chloride salt (MgCl2-NaCl-KCl mixed salt with a mass ratio of 1:1:1) to a molten salt reaction unit. Heat the molten chloride salt to 620°C in the molten salt reaction unit to maintain the molten chloride salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (scrap titanium material) is added in an amount of 8 wt.% based on the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 175°C and vaporized into TiCl4 steam by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit through an argon flow (flow rate of 6 mL / min) from an argon carrier flow transport unit, establishing a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. The TiCl4 vapor and the crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at 620°C for 30 minutes to obtain low-valent titanium chlorides (TiCl3 and TiCl2); the total amount of TiCl4 vapor introduced was 60 wt% of the mass of the chloride molten salt; The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+ The concentration of Ti was 0.21 mol / L; Ti was detected by hydrogen titration. 2+ The concentration is 0.09mol / L.

[0021] Example 6: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Crude titanium (sponge titanium) and 300 g of molten chloride salt (a NaCl-CaCl mixed salt with a mass ratio of 1:1) are added to a molten salt reaction unit. The molten chloride salt is heated to 780°C in the molten salt reaction unit to maintain the molten salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (sponge titanium) is added in an amount of 8 wt% of the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 200°C and vaporized into TiCl4 vapor by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit via an argon flow (flow rate of 4 mL / min) from an argon carrier flow transport unit, establishing a gas-solid-liquid three-phase interface reaction system in an inert atmosphere at normal pressure. The TiCl4 vapor and crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at 780°C for 3 minutes to produce low-valent titanium chlorides (TiCl3 and TiCl2). The total amount of TiCl4 vapor introduced was 4 wt% of the mass of the chloride molten salt. The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+ The concentration of Ti was 0.06 mol / L; Ti was detected by hydrogen titration 2+ The concentration is 0.27mol / L.

[0022] Example 7: A method for preparing low-valent titanium chloride using a gaseous TiCl4 molten salt method, the specific steps are as follows: S1. Crude titanium (sponge titanium) and 300 g of molten chloride salt (a LiCl-NaCl-KCl mixed salt with a mass ratio of 1:1:1) are added to a molten salt reaction unit. The molten chloride salt is heated to 500°C in the molten salt reaction unit to maintain the molten salt in a liquid state, with the liquid molten salt located above the crude titanium solid phase. The crude titanium (sponge titanium) is added in an amount of 15 wt % based on the mass of the molten chloride salt. S2. The liquid TiCl4 is heated to a temperature of 180°C and vaporized into TiCl4 vapor by a TiCl4 gasification unit; S3. TiCl4 vapor was uniformly introduced into the liquid molten salt of the molten salt reaction unit through an argon flow (flow rate of 3 mL / min) from an argon carrier flow transport unit, and a gas-solid-liquid three-phase interface reaction system was established in an inert atmosphere at normal pressure. The TiCl4 vapor and the crude titanium in the liquid molten salt underwent a heterogeneous reduction reaction at 500°C for 10 minutes to obtain low-valent titanium chlorides (TiCl3 and TiCl2). The total amount of TiCl4 vapor introduced was 10 wt% of the mass of the chloride molten salt. The chloride molten salt sample after the reaction was sampled and analyzed, and the Ti content in the molten salt was measured by ammonium ferric sulfate titration method. 3+The concentration of Ti was 0.02 mol / L; Ti was detected by hydrogen titration 2+ The concentration is 0.31mol / L.

[0023] The above describes the specific embodiments of the present invention in detail, but the present invention is not limited to the above embodiments. Various changes can be made within the knowledge of ordinary technicians in this field without departing from the scope of the present invention.

Claims

1. A method for preparing low-valent titanium chloride by a gaseous TiCl4 molten salt method, characterized in that: A low-valent titanium chloride preparation device is used, which includes a TiCl4 gasification unit, an argon carrier flow transport unit and a molten salt reaction unit; The specific steps of the method are as follows: S1. Adding crude titanium and chloride molten salt to a molten salt reaction unit, heating the chloride molten salt to 500-800°C through the molten salt reaction unit to maintain the liquid molten salt, with the liquid molten salt located above the crude titanium solid phase; the initial crystallization temperature of the chloride molten salt is 450-750°C, and the heating temperature of the chloride molten salt is higher than the initial crystallization temperature of the chloride molten salt; S2. The liquid TiCl4 is heated to a temperature of 150-200°C by a TiCl4 gasification unit to be gasified into TiCl4 vapor; S3. TiCl4 vapor is uniformly introduced into the liquid molten salt of the molten salt reaction unit through the argon flow of the argon carrier flow transport unit, and a gas-solid-liquid three-phase interface reaction system is constructed in an inert atmosphere at normal pressure. The TiCl4 vapor undergoes a multiphase reduction reaction with the crude titanium in the liquid molten salt at a temperature of 500-800°C to obtain low-valent titanium chloride.

2. The method for preparing low-valent titanium chloride by the gaseous TiCl4 molten salt method according to claim 1, characterized in that: Step S1. The chloride molten salt is one or more of NaCl, KCl, MgCl2, CaCl2 or LiCl.

3. The method for preparing low-valent titanium chloride by the gaseous TiCl4 molten salt method according to claim 1, characterized in that: The crude titanium is sponge titanium or scrap titanium.

4. The method for preparing low-valent titanium chloride by the gaseous TiCl4 molten salt method according to claim 1, characterized in that: Step S3: The argon flow rate is 3-10 mL / min.

5. The method for preparing low-valent titanium chloride by the gaseous TiCl4 molten salt method according to claim 1, characterized in that: The TiCl4 gasification unit comprises a heating device (2) and a TiCl4 storage tank (3). The TiCl4 storage tank (3) is placed in the heating zone of the heating device (2). A temperature sensor I is provided on the inner wall of the TiCl4 storage tank (3). The temperature sensor I is externally connected to a temperature controller I. The temperature controller I is electrically connected to the heater of the heating device (2). A carrier gas inlet and a TiCl4 vapor outlet are provided on the top cover of the TiCl4 storage tank (3). The TiCl4 storage tank (3) is filled with liquid TiCl4. The argon carrier flow delivery unit comprises an argon pipe (1), a TiCl4 vapor delivery pipe (4), a gas flow control valve (5) and a gas delivery pipe (6), wherein the two ends of the argon pipe (1) are respectively an A end and a B end, the A end of the argon pipe (1) is externally connected to a carrier gas tank, the B end of the argon pipe (1) passes through the carrier gas inlet of the top cover of the TiCl4 storage tank (3) and extends downward to above the liquid TiCl4, the argon pipe (1) is provided with a flow meter, the two ends of the TiCl4 vapor delivery pipe (4) are respectively an A' end and a B' end, the A' end of the TiCl4 vapor delivery pipe (4) is connected to the TiCl4 vapor outlet of the top cover of the TiCl4 storage tank (3), the B' end of the TiCl4 vapor delivery pipe (4) is connected to the gas inlet of the gas flow control valve (5), the two ends of the gas delivery pipe (6) are respectively an A" end and a B" end, and the A" end of the gas delivery pipe (6) is connected to the gas outlet of the gas flow control valve (5); The molten salt reaction unit comprises a heating furnace body (7) and a molten salt reactor (8). The molten salt reactor (8) is filled with crude titanium (9) and chloride molten salt (10). The molten salt reactor (8) is placed in the heating zone of the heating furnace body (7). A gas through hole is opened in the center of the top cover of the heating furnace body (7). The B" end of the gas pipe (6) passes through the gas through hole and extends downward into the crude titanium (9). A temperature sensor II is provided on the inner wall of the molten salt reactor (8). The temperature sensor II is externally connected to a temperature controller II. The temperature controller II is electrically connected to the heater of the heating furnace body (7).

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