Directional purification method and equipment for titanium tetrachloride

Abstract

The invention relates to a directional purification method and equipment for titanium tetrachloride in the field of preparation and purification of integrated circuit raw materials, the directional purification equipment comprises an oxidation device, the oxidation device comprises an oxidation kettle, a pure copper part and a spraying device, the pure copper part and the spraying device are contained in the oxidation kettle, and the spraying device is suspended above the pure copper part; a feeding hole connected with the spraying device is formed in the oxidation kettle, and a first heating device for heating the pure copper workpiece is arranged on the oxidation kettle; the rectifying system comprises a rectifying still, a rectifying tower connected to the top of the rectifying still and a second heating device used for heating the rectifying still, a material pressing opening and an inert gas opening are formed in the rectifying still, and a tower top condensation structure is formed at the top of the rectifying tower; a plurality of tower plates are arranged in the rectifying tower at intervals along the height direction of the rectifying tower. According to the directional purification method and equipment, the purification difficulty of the titanium tetrachloride can be effectively reduced, the production cost is reduced, and the purity of the titanium tetrachloride is effectively improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of integrated circuit raw material preparation and purification, in particular to a directional purification method and equipment for titanium tetrachloride. BACKGROUND

[0002] Titanium tetrachloride is not only an important raw material for the titanium industry, but also widely used in chemical industry, electronics, agriculture and military and other fields. Since the 1950s, it has realized large-scale production, and its influence has penetrated into every corner of modern society, becoming an important force to promote social development. With the vigorous development of China's titanium industry, the supply market of titanium tetrachloride shows great potential. Therefore, while pursuing higher yield, it is particularly important to continuously improve the quality of titanium tetrachloride products. Crude titanium tetrachloride generally contains various impurities, and the requirements for impurities are different according to different downstream industries. The main impurities are vanadium trichloride, silicon tetrachloride, iron trichloride, etc., and other transition metal element impurities such as chromium, manganese, nickel, etc.

[0003] The current mainstream purification methods for titanium tetrachloride are rectification method, adsorption method and vanadium removal method. Among them, the vanadium removal method mainly uses organic mud method and aluminum powder method, but the organic mud method has problems such as sticky residue difficult to handle, carbon pollution, low temperature sensitivity, etc., and the aluminum powder method has problems such as high safety risk, complex process control, high cost of residue vanadium extraction, etc. The rectification method needs more equipment, and its vanadium removal mechanism is to crack at high temperature to form high-activity particles and react with vanadium to increase the boiling point of vanadium impurities for secondary rectification removal, but high-activity particles will also react with iron and other impurities, causing serious equipment scaling. The adsorption method has the problem of high production cost, and the whole process has many steps, which increases the operation cost. Moreover, the existing rectification means mainly uses a packed tower as the rectification equipment, which needs various packings, and new impurities are easily introduced during the rectification process. SUMMARY

[0004] The main purpose of the present application is to provide a directional purification method and equipment for titanium tetrachloride, which aims to solve at least one of the above technical problems.

[0005] In order to achieve the above-mentioned purpose, the present application provides a directional purification equipment for titanium tetrachloride, which comprises: an oxidation device, the oxidation device comprises an oxidation kettle, a pure copper part contained in the oxidation kettle and a spraying device, the spraying device is suspended above the pure copper part, a feed inlet connected with the spraying device is arranged on the oxidation kettle, and a first heating device for heating the pure copper part is arranged on the oxidation kettle; a rectification system, the rectification system comprises a rectification kettle, a rectification tower connected at the top of the rectification kettle and a second heating device for heating the rectification kettle, a pressure port and an inert gas port are formed on the rectification kettle, a tower top condensing structure is formed at the top of the rectification tower, and a plurality of tower plates are arranged in the rectification tower along the height direction.

[0006] In some embodiments of the present application, the pure copper piece is a copper pipe.

[0007] In some embodiments of the present application, the copper pipe is arranged in a spiral manner in the vertical direction in the oxidation kettle.

[0008] In some embodiments of the present application, the copper pipe is tilted at an angle after being spiraled in the oxidation kettle.

[0009] In some embodiments of the present application, the oxidation kettle is provided with a water inlet towards the pure copper piece.

[0010] In some embodiments of the present application, the tower plate is a quartz sieve tower plate.

[0011] In some embodiments of the present application, the number of tower plates is 10-20.

[0012] According to another aspect of the present application, there is provided a method for directional purification of titanium tetrachloride, which utilizes the directional purification device described above to purify titanium tetrachloride, comprising the following steps: heating the pure copper piece, preheating the crude titanium tetrachloride, and then sending it to the spraying device through the feeding port, so that the crude titanium tetrachloride is sprayed on the surface of the pure copper piece by the spraying device; the titanium tetrachloride after contacting the surface of the pure copper piece is pressed into the rectification kettle through the pressing port, and under the inert atmosphere, the rectification kettle temperature is controlled at 120-145°C, the rectification tower temperature is controlled at 130-140°C, the reflux ratio is controlled at 2:1-10:1, the pressure is controlled at 7x10 4 -9.5x10 4 Pa, and the front and rear fractions are intercepted, and the middle fraction is taken.

[0013] In some embodiments of the present application, before the titanium tetrachloride is pressed into the rectification kettle, inert gas is first introduced into the rectification kettle and the rectification tower for purging until the dew point temperature in the rectification kettle and the rectification tower is -100°C; then the rectification kettle and the rectification tower are washed with pure water and dried, and the drying temperature is 120°C.

[0014] In some embodiments of the present application, the rectification purification process is as follows: first, the titanium tetrachloride is warmed in the rectification kettle, and when it is near the boiling point temperature interval of low-boiling-point impurities, inert gas is introduced to blow out the low-boiling-point impurities contained in the titanium tetrachloride; then the titanium tetrachloride is continuously warmed, and when it is at 136°C, the fraction is distilled out, and the 10% front fraction is discarded; then high-boiling-point impurities are separated from the titanium tetrachloride by total reflux; finally, the final product is taken at 1 / 3 of the rectification tower, and the 40-60% middle fraction is taken.

[0015] The embodiment of the present application provides a directional purification method and equipment of titanium tetrachloride, the directional purification method and equipment can effectively change vanadium impurities in the titanium tetrachloride into high-boiling vanadium impurities based on an oxidation device, the pure copper parts in the oxidation kettle are convenient to clean, the introduction of impurities can be reduced, under the inert atmosphere, the titanium tetrachloride treated by the oxidation device is subjected to rectification and purification by controlling parameters such as the rectification kettle temperature, the rectification tower temperature, the reflux ratio and the pressure, the impurities can be removed in a targeted manner, and by using the tray-type rectification tower and cooperating with the inert gas, new impurities can be effectively avoided in the rectification process, so that high-purity titanium tetrachloride is finally obtained, the purification difficulty of the titanium tetrachloride is effectively reduced, the production cost is reduced, and the purity of the titanium tetrachloride is effectively improved, so that the purity of the final product meets the production requirements under the minimum production cost. BRIEF DESCRIPTION OF DRAWINGS

[0016] Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The detailed description is made with reference to the accompanying drawings.

[0017] Figure 1 Fig. 1 is a schematic diagram of the overall structure of the directional purification equipment of titanium tetrachloride of the present application;

[0018] Figure 2 Fig. 2 is a schematic diagram of the structure of the oxidation device of the present application;

[0019] Figure 3 Fig. 3 is a schematic diagram of the structure of the rectification system of the present application.

[0020] In the drawings, various reference numerals represent the following: 1, oxidation kettle; 2, pure copper part; 3, spraying device; 4, feed inlet; 5, rectification kettle; 6, rectification tower; 7, pressure feed port; 8, inert gas port; 9, tower top condensation structure; 10, water inlet; 11, gas inlet; 12, discharge port; 13, kettle body; 14, flange; 15, kettle cover; 16, condenser pipe; 17, reflux pipe. DETAILED DESCRIPTION

[0021] It should be clear that the described embodiments are only some of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of protection of the present application. Those of ordinary skill in the art will easily identify multiple non-critical parameters, which can be changed or modified, and the results are basically the same.

[0022] The following description refers to the accompanying drawings. Unless otherwise noted, like elements in different drawings have the same or similar reference numerals. The following description of illustrative embodiments is not meant to limit or restrict the scope of the application. Rather, the following description is merely an example embodiment of the application, which is consistent with some aspects of the application as detailed in the appended claims.

[0023] In the description of the present application, it should be understood that the terms "first", "second" and the like are used to describe various elements, but not necessarily indicate or imply relative importance. The above terms can be understood by those of ordinary skill in the art according to the specific meaning in the present application. In addition, in the description of the present application, "a plurality of" means two or more, unless otherwise specified. The association between the associated objects is described, which means that there can be three relationships, for example, A and / or B, which means that there are three cases of A alone, A and B together, and B alone. The character " / " generally represents an "or" relationship between the associated objects before and after it.

[0024] Unless otherwise specified in the examples, the techniques or conditions are carried out according to the techniques or conditions described in the literature in the art or according to the product instructions. Unless otherwise specified, the reagents or instruments used are conventional products that can be purchased through regular channels. The experimental methods in the following examples are conventional methods, unless otherwise specified. The test materials used in the following examples are commercially available products, unless otherwise specified.

[0025] The current mainstream purification methods of titanium tetrachloride are rectification, adsorption and vanadium removal. For example, high-boiling-point impurities such as iron are removed by rectification, and then the titanium tetrachloride after removing high-boiling-point substances is added to an organic vanadium removal agent to remove vanadium, and then secondary rectification is carried out, but this method requires more equipment, because the mechanism of vanadium removal is that high-activity microparticles are generated by cracking at high temperature and react with vanadium to increase the boiling point of vanadium impurities, and then secondary rectification is carried out, but high-activity microparticles also react with impurities such as iron, resulting in serious scaling of the equipment. Alternatively, two-stage liquid-phase adsorption devices, rectification units and precision filtration units are used to remove organic matter, metal ions and non-metal ion impurities by two-stage liquid-phase adsorption, then the product components are further purified by the packed column rectification unit, and finally the particle content in the product is effectively reduced by the precision filtration unit, but this method has high production cost, and the process has many steps, which increases the operation cost.

[0026] Therefore, the present application provides a directional purification method and device for titanium tetrachloride, which can effectively reduce the purification difficulty of titanium tetrachloride, reduce the production cost, and effectively improve the purity of titanium tetrachloride.

[0027] The embodiments of the present application disclose a directional purification device for titanium tetrachloride. As shown in Figures 1-3As shown, the directional purification equipment of titanium tetrachloride includes an oxidation device and a rectification system; the oxidation device includes an oxidation kettle 1, a pure copper part 2 contained in the oxidation kettle 1, and a spraying device 3 suspended above the pure copper part 2, the oxidation kettle 1 is provided with a feeding port 4 connected with the spraying device 3, and the oxidation kettle 1 is provided with a first heating device for heating the pure copper part 2; the rectification system includes a rectification kettle 5, a rectification tower 6 connected at the top of the rectification kettle 5, and a second heating device for heating the rectification kettle 5, the rectification kettle 5 is formed with a pressure port 7 and an inert gas port 8, the top of the rectification tower 6 is formed with a tower top condensation structure 9, and a plurality of tower plates are arranged in the rectification tower 6 along the height direction thereof.

[0028] In the present application, when impurities need to be removed from the crude titanium tetrachloride, the first heating device is used to heat the pure copper part 2 to a certain temperature and maintain the temperature, then the crude titanium tetrachloride to be treated is preheated, and then the crude titanium tetrachloride is sent to the spraying device 3 through the feeding port 4, so that the crude titanium tetrachloride is sprayed on the surface of the pure copper part 2 through the spraying device 3, the vanadium impurities in the crude titanium tetrachloride react to become high-boiling vanadium impurities, and then the titanium tetrachloride after contacting the surface of the pure copper part 2 is pressed into the rectification kettle 5 through the pressure port 7, under the inert gas atmosphere, by controlling the temperature of the rectification kettle 5, the temperature of the rectification tower 6, the reflux ratio, and the pressure and other parameters, rectification and purification are carried out, impurities are removed, and by using the tower plate type rectification tower 6, in combination with the inert gas, new impurities are effectively avoided in the rectification process, so that high-purity titanium tetrachloride is finally obtained, the directional purification equipment of the present application effectively reduces the purification difficulty of titanium tetrachloride, reduces the production cost, and effectively improves the purity of titanium tetrachloride, so that the purity of the final product meets the production requirements at the lowest production cost.

[0029] In some embodiments of the present application, the crude titanium tetrachloride sprayed by the spraying device 3 should correspond to the position of the pure copper part 2 as much as possible, so that the crude titanium tetrachloride can contact the surface of the pure copper part 2 as much as possible, and ensure that the vanadium impurities in the crude titanium tetrachloride are fully converted into high-boiling vanadium impurities.

[0030] In some embodiments of the present application, as shown in Figure 2 The pure copper part 2 is a copper pipe.

[0031] In the present embodiment, the pure copper part 2 is a copper pipe, which has good structural strength and good pressure resistance, and based on its smooth surface, the crude titanium tetrachloride can be in contact with the surface of the copper pipe as much as possible, thereby improving the effect of converting vanadium impurities in the crude titanium tetrachloride into high-boiling vanadium impurities.

[0032] Furthermore, the copper tubes are arranged vertically in a spiral manner inside the oxidation reactor 1, similar to a spring shape. By spiraling the copper tubes, the overall area of ​​pure copper that can contact the crude titanium tetrachloride can be further increased, ensuring that the crude titanium tetrachloride sprayed from top to bottom is in full contact with the pure copper.

[0033] Furthermore, after the copper tube is coiled inside the oxidation reactor 1, it is tilted at a certain angle. By tilting the coiled copper tube, the vertical projection area of ​​the copper tube can be increased, and a stepped structure can be formed. This can significantly reduce the difficulty of contact between the crude titanium tetrachloride sprayed by the spraying device 3 and the pure copper workpiece 2. With the control of the spraying speed, the contact efficiency and contact effect between the crude titanium tetrachloride and the pure copper workpiece 2 can be further improved. It can also further increase the operating range of the spraying and improve the processing efficiency of crude titanium tetrachloride.

[0034] In some embodiments of the present invention, multiple copper tubes may be installed in the oxidation reactor 1. The multiple copper tubes are arranged in a spiral manner and nested from the outside to the inside. The number of copper tubes includes, but is not limited to, two, three, four, five, etc., to further improve the treatment effect and efficiency of crude titanium tetrachloride.

[0035] In some embodiments of the present invention, the copper tube can exist with any curvature, and in addition to coiling, it can also be arranged in a way such as bending or spiraling.

[0036] When multiple copper tubes are arranged in a spiral manner, the multiple spiral copper tubes can be arranged at intervals, and the multiple spiral copper tubes can be arranged in a staggered manner.

[0037] In some embodiments of the present invention, the pure copper component 2 can be in the form of copper tube, copper mesh, copper sheet, etc.

[0038] In some embodiments of the present invention, the copper content of the pure copper component 2 is preferably 99.7% to 99.95%.

[0039] In some embodiments of the present invention, the first heating device (not shown) is included, but is not limited to, disposed on the side wall of the oxidation reactor 1 or inside a copper tube. The first heating device includes, but is not limited to, electric heating or heat transfer by a working fluid.

[0040] In some embodiments of the present invention, the spraying device 3 includes, but is not limited to, a spraying structure such as a hollow disc or annular tube, and multiple spraying nozzles are evenly opened at the positions corresponding to the pure copper parts 2 in the hollow disc or annular tube.

[0041] In some embodiments of the present invention, such as Figure 2 As shown, the oxidation reactor 1 is provided with a water inlet 10 facing the pure copper component 2.

[0042] In the embodiment, when the surface of the pure copper part 2 is deactivated, the surface of the pure copper part 2 can be cleaned by introducing pure water into the oxidation kettle 1 through the water inlet 10, so that the pure copper part 2 can be efficiently reused, without repeatedly taking out the pure copper part 2, the operation is simple, and the way of introducing impurities is reduced.

[0043] In some embodiments of the present application, as shown in Figure 2 The oxidation kettle 1 is provided with an air inlet 11. Preferably, the air inlet 11 is arranged at the top of the oxidation kettle 1, and a plurality of inlets are arranged to facilitate production.

[0044] In some embodiments of the present application, as shown in Figure 2 The bottom of the oxidation kettle 1 is provided with a discharge port 12, which facilitates the transfer of the reacted crude titanium tetrachloride. The discharge port 12 can be used to collect the reacted crude titanium tetrachloride, or the reacted crude titanium tetrachloride can be continuously discharged during spraying.

[0045] In some embodiments of the present application, the oxidation kettle 1 preferably adopts a steel-lined fluorine container.

[0046] In some embodiments of the present application, as shown in Figure 2 The oxidation kettle 1 includes a kettle body 13 and a kettle cover 15 which is detachably connected to the top opening of the kettle body 13 through a flange 14. The pure copper part 2 can be detachably installed in the kettle body 13 through a support or the like structure. The spraying device 3, the feed inlet 4, the water inlet 10, the air inlet 11 and the like structure can be arranged on the kettle cover 15. By removing the kettle cover 15, the pure copper part 2 can be easily replaced or cleaned.

[0047] In some embodiments of the present application, the tower plate is a quartz sieve tower plate.

[0048] In the embodiment, by using the quartz sieve tower plate, new impurities can be further avoided in the rectification process.

[0049] Preferably, the quartz sieve tower plate is made of high-purity quartz with a purity of more than 99.995%.

[0050] Further, the number of tower plates is 10-20, which improves the separation effect while reducing the production cost.

[0051] In some embodiments of the present application, the second heating device (not shown) includes but is not limited to being arranged at the bottom of the rectification kettle 5 or the side wall of the rectification kettle 5. The second heating device includes but is not limited to using electric heating or using a working medium for heat transfer.

[0052] In some embodiments of the present application, the directional purification device further comprises a tail gas absorption system (not shown) connected to the rectification kettle 5 and the rectification tower 6 to ensure pressure balance of the rectification system and collect other blown gases.

[0053] Specifically, the tail gas absorption system can be arranged at the gas escape outlet of the overhead condensation structure, and the tail gas absorption system extracts the gas at a slight negative pressure.

[0054] In some embodiments of the present application, the discharge port 12 of the oxidation kettle 1 and the pressure port 7 of the rectification kettle 5 can be connected by a pipeline and the treated crude titanium tetrachloride is transferred by pumping, or the discharge port 12 is arranged higher than the pressure port 7 to transfer the treated crude titanium tetrachloride by natural gravity, or the discharge port 12 is not directly connected to the pressure port 7 to transfer the treated crude titanium tetrachloride by a container.

[0055] In some embodiments of the present application, as shown in Figure 3 The overhead condensation structure 9 comprises a condensation pipe 16 and a reflux pipe 17, and a condenser (not shown) arranged on the condensation pipe 16 and a reflux pump (not shown) arranged on the reflux pipe 17, the condensate is collected through the outlet of the condensation pipe 16, and the condensate is partially or completely refluxed to the rectification tower 6 through the reflux pipe 17 and the reflux pump.

[0056] The present embodiment also proposes a directional purification method of titanium tetrachloride, which utilizes the above-mentioned directional purification device to purify titanium tetrachloride, and the directional purification method comprises the following steps:

[0057] S1, heating the pure copper parts and preheating the crude titanium tetrachloride to improve the vanadium removal effect.

[0058] S2, feeding the preheated crude titanium tetrachloride into the spraying device through the feed port, so that the crude titanium tetrachloride is sprayed on the surface of the pure copper parts through the spraying device.

[0059] S3, the titanium tetrachloride after contacting the surface of the pure copper parts is pressed into the rectification kettle through the pressure port.

[0060] S4, under an inert atmosphere, the rectification kettle is controlled at a temperature of 120-145℃, the rectification tower is controlled at a temperature of 130-140℃, the reflux ratio is controlled at 2:1-10:1, and the pressure is controlled at 7×10 4 -9.5×10 4 Pa, and the front and rear fractions are intercepted, and the middle fraction is taken.

[0061] The purification method of the present application removes impurities according to the different boiling points of titanium tetrachloride and metal ion impurities, under the protection of high-purity inert gas, ensures the pressure balance of the system through the tail gas absorption device, removes impurities through the control of the tower kettle temperature, the tower column temperature, the reflux ratio and the overall system pressure, and obtains the final product by intercepting the front and rear fractions and taking the middle fraction.

[0062] In the rectification process, the titanium tetrachloride in the rectification kettle is heated and evaporated, and the vapor rises through the rectification tower, condenses into liquid at the top of the tower, and according to the different boiling points of impurities, low-boiling-point impurities such as silicon tetrachloride are first heated and evaporated, and high-boiling-point impurities such as iron are left as the rear fraction in the rectification kettle. The overall rectification tower temperature is controlled at about the boiling point of titanium tetrachloride. Because high-boiling-point impurities theoretically will not evaporate (in fact, due to the height of the rectification tower and other problems, a small amount of evaporation will occur), the middle fraction is intercepted.

[0063] Through the above rectification process, vanadium, chromium, manganese, iron, cobalt, nickel, silicon and other impurities in titanium tetrachloride can be removed, so that the vanadium, chromium, manganese, iron, cobalt, nickel, silicon and other impurities are less than 1 ppm, and the product meeting the production demand is obtained at a lower production cost and a simpler operation.

[0064] In some embodiments of the present application, the crude titanium tetrachloride contacts the surface of the pure copper part to react as follows:

[0065] Vanadyl trichloride + copper → vanadyl dichloride + cuprous chloride

[0066] In the present application, based on the directional oxidation of vanadium element by high-purity copper redox, the low-boiling-point vanadium impurity vanadyl trichloride (boiling point 127℃) close to the boiling point of titanium tetrachloride (boiling point 136℃) is changed into vanadyl dichloride precipitation, which is attached to the pure copper part together with cuprous chloride precipitation, so as to achieve the purpose of removing vanadium impurities in crude titanium tetrachloride.

[0067] In some embodiments of the present application, before the titanium tetrachloride is pressed into the rectification kettle, the purified inert gas is first introduced into the rectification kettle and the rectification tower for purging; then the rectification kettle and the rectification tower are washed with pure water and dried, and the drying temperature is 120℃, and the pure water is preferably ultrapure water.

[0068] In some embodiments of the present application, the rectification and purification process is as follows:

[0069] First, the titanium tetrachloride is heated in the rectification kettle, and the inert gas is introduced into the rectification kettle at 105℃-125℃ to perform low-temperature gas chasing. The low-boiling-point impurities contained in the titanium tetrachloride, such as silicon tetrachloride (boiling point 57.6℃), are blown out by the inert gas, that is, the low-boiling-point impurities contained in the titanium tetrachloride are blown out by the inert gas while the titanium tetrachloride is kept in a slight boiling state, and the gas blown out can be blown into the tail gas absorption device.

[0070] After the inert gas purging for several hours, the low boiling point impurities are effectively removed, then the titanium tetrachloride is continuously heated, when the temperature reaches 136℃, the distillate is distilled out, and the first 10% of the distillate is discarded.

[0071] Then the high boiling point impurities such as iron trichloride (boiling point 315℃) and high boiling point vanadium impurities are separated from the titanium tetrachloride by total reflux.

[0072] Finally, the 40-60% of the middle distillate is taken out as the final product.

[0073] By using the purification method of the present application, the high purity titanium tetrachloride obtained has vanadium, chromium, manganese, iron, cobalt and nickel in the middle distillate lower than the detection limit by ICP-MS detection.

[0074] In some embodiments of the present application, the inert gas used for purging and providing an inert atmosphere includes but is not limited to argon, helium, nitrogen, etc., and argon is preferably used.

[0075] The above is only the preferred specific embodiment of the present application, but the protection scope of the present application is not limited thereto, any changes or replacements easily thought of by those skilled in the art within the technical scope disclosed by the present application should be covered within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A directional purification device for titanium tetrachloride, characterized in that, include: An oxidation device, comprising an oxidation kettle, a pure copper component housed within the oxidation kettle, and a spraying device, wherein the spraying device is suspended above the pure copper component, the oxidation kettle is provided with a feed inlet connected to the spraying device, and the oxidation kettle is provided with a first heating device for heating the pure copper component. A distillation system, comprising a distillation kettle, a distillation column connected to the top of the distillation kettle, and a second heating device for heating the distillation kettle, wherein the distillation kettle has a feed inlet and an inert gas inlet, the distillation column has a top condenser structure, and the distillation column has multiple trays spaced apart along its height.

2. The directional purification equipment for titanium tetrachloride according to claim 1, characterized in that, The pure copper component is a copper tube.

3. The directional purification equipment for titanium tetrachloride according to claim 2, characterized in that, The copper tubes are arranged in a spiral manner along the vertical direction inside the oxidation reactor.

4. The directional purification equipment for titanium tetrachloride according to claim 3, characterized in that, The copper tube is coiled inside the oxidation reactor and then tilted at a certain angle.

5. The directional purification equipment for titanium tetrachloride according to claim 1, characterized in that, The oxidation reactor is provided with a water inlet facing the pure copper component.

6. The directional purification equipment for titanium tetrachloride according to claim 1, characterized in that, The tray is a quartz sieve tray.

7. The directional purification equipment for titanium tetrachloride according to claim 1, characterized in that, The number of trays is 10-20.

8. A method for the directional purification of titanium tetrachloride, comprising purifying titanium tetrachloride using the directional purification equipment as described in any one of claims 1-7, characterized in that, Includes the following steps: The pure copper parts are heated, and the crude titanium tetrachloride is preheated and then fed to the spraying device through the feed port, so that the crude titanium tetrachloride is sprayed onto the surface of the pure copper parts through the spraying device. Titanium tetrachloride, after being in contact with the surface of the pure copper part, is forced into the distillation vessel through the feed port. Under an inert atmosphere, the distillation vessel temperature is controlled at 120℃-145℃, the distillation column temperature at 130℃-140℃, the reflux ratio at 2:1-10:1, and the pressure at 7×10⁻⁶. 4 -9.5×10 4 Distillation and purification were carried out at Pa, and the first and last fractions were separated, while the middle fraction was collected.

9. The targeted purification method according to claim 8, characterized in that, Before the titanium tetrachloride is pressed into the distillation kettle, inert gas is first introduced into the distillation kettle and distillation column for purging until the dew point temperature in the distillation kettle and distillation column is -100°C; then the distillation kettle and distillation column are washed with pure water and dried at a drying temperature of 120°C.

10. The targeted purification method according to claim 8, characterized in that, The distillation and purification process is as follows: First, heat titanium tetrachloride in a distillation vessel. When the temperature is near the boiling point of the low-boiling-point impurities, introduce an inert gas to blow out the low-boiling-point impurities contained in the titanium tetrachloride. The titanium tetrachloride was then heated to 136°C, at which point the fraction was distilled off, and 10% of the first fraction was discarded. Then, high-boiling-point impurities were separated from titanium tetrachloride by total reflux; Finally, the final product, consisting of 40-60% middle fraction, is collected at the condenser at the top of the column.

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