U-shaped distillation equipment for sponge titanium production and use method thereof

Abstract

The invention relates to the technical field of sponge titanium production devices, in particular to U-shaped distillation equipment for sponge titanium production and a use method of the U-shaped distillation equipment. The invention discloses U-shaped distillation equipment for sponge titanium production. The U-shaped distillation equipment comprises a distiller, a condenser and a connecting passage, the distiller comprises a distillation electric furnace and a distillation reactor. The connecting passage comprises a transverse pipe and two vertical pipes connected with the two ends of the transverse pipe; the lower ends of the two vertical pipes are respectively inserted into the distiller and the condenser. The lower end of the vertical pipe inserted into the cold end sealing cover is of a closing-up structure with the diameter gradually reduced from top to bottom, and a heater is arranged between the outer side of the vertical pipe and the hole wall of the center hole. The lower end of the vertical pipe inserted into the cold end sealing cover is provided with the closing-in structure, the cross sectional area of a channel is reduced through the closing-in structure, rapid passing and efficient condensation of substances are facilitated, accumulation and condensation caused by low-speed retention are reduced, and therefore the risk that a connecting channel is blocked is effectively reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of titanium sponge production devices, and in particular to a U-shaped distillation equipment for titanium sponge production and a method of using the same. Background Art

[0002] Titanium and titanium alloys have the characteristics of high specific strength, corrosion resistance, and good high-temperature performance. They are widely used in aerospace, deep-sea exploration, chemical industry, medical and other fields. Sponge titanium is the raw material for the preparation of titanium and titanium alloys. It is produced industrially by reducing TiCl4 by magnesium thermal method and vacuum distilling the reduced product. The production of sponge titanium is to convert ilmenite into titanium tetrachloride, then put it into a sealed stainless steel tank, fill it with argon gas, and react with magnesium metal to obtain "sponge titanium". One of the important stages is distillation.

[0003] At present, the equipment for producing titanium sponge includes "U" type and "I" type equipment. U-type distillation equipment includes distillation reactor, condenser, middle passage and vacuum unit. At present, the distillation method adopted by the inverted U-type furnace is that the reactor and condenser are connected in parallel through the central tube of the passage. Therefore, whether the passage is unobstructed directly affects the distillation effect. The passage blockage is caused by the following reasons: 1. The volatiles cool down too quickly in the middle passage, condense in the middle passage or at the outlet of the cold end passage, and block the passage; 2. The temperature of the cold end cover is low, and the volatiles condense and grow rapidly on the surface of the cover head, blocking the passage; 3. When clearing the passage, it is difficult to thoroughly clean the condensate inside the passage and at the passage mouth, and the passage is blocked for the second time in a short time; 4. The residual amount of magnesium chloride and liquid magnesium is large, and the volatilization amount of the distillate is difficult to match the condensation rate, which is easy to block the passage mouth or the evacuation pipe. How to reduce the frequency of pipe blockage in the distillation stage will not only help to improve the comprehensive indicators of the product, but also improve production efficiency and reduce production costs. This is also a difficult problem that the industry can constantly explore and tackle.

[0004] In order to solve the problem of blockage in the distillation channel, various sponge enterprises have carried out equipment and process research and proposed solutions. The main solutions include the following aspects: (1) Heating the inlet of the distillation reactor of the middle aisle and the condenser; for example, the utility model patent with the publication number CN220907589U provides a heating compensation device for the heater of the U-type furnace sponge titanium production aisle. Through the setting of the vertical tube heater, the outer side of the vertical tube 2 can be heated. At the same time, the heater in the temperature compensation and temperature measuring device is kept at a constant temperature of 800°C for a long time. The auxiliary heater increases the heat radiation area in the vertical tube 2 channel, so that when the impurities magnesium and magnesium chloride in the titanium lump in the reactor are distilled to the cooling kettle, they will not condense and hang on the wall in the vertical tube 2 channel. (2) Add an automatic dredging device to the inlet of the condenser for regular dredging; for example, the invention patent with publication number CN114769237B provides a U-shaped titanium sponge reactor distillation aisle high-efficiency automatic cleaning device, including a shell, a cleaning component and a partition component. The cleaning component is placed on the inner top of the shell. The cleaning component includes a hydraulic cylinder, a first hydraulic connection valve, a push rod, a motor and a high-strength drill. For example, the invention patent application with publication number CN117385197A provides a magnetic fluid sealed aisle dredging device for a titanium sponge distillation process, including a reduction furnace, a distillation furnace, an aisle pipe, a dredging module and a stabilization module. (3) Optimize the distillation reactor and condenser structure. For example, the invention patent application with publication number CN117568627A provides an anti-blocking large cover and its operation method for producing a titanium sponge inverted U-shaped furnace. The large cover head is a cavity structure filled with thermal insulation cotton. The large cover and the aisle center pipe can be heated to reduce the condensation amount of volatiles at the large cover and prevent channel blockage. The invention patent application with publication number CN110714130A provides a device and process for preventing vacuum channel blockage in sponge titanium production, including a condenser, a sieve plate, a reactor, a magnesium chloride tube, a large cover, a large cover riser and a heating furnace. The invention application eliminates the evacuation tube and uses a magnesium chloride tube for evacuation, reduces the large cover welds, and reduces the product air intake rate.

[0005] However, in the distillation process, it is difficult to accurately control the condensation process of the volatile vapor in the above-mentioned device, and the anti-blocking effect is difficult to judge. When blocked, the distillation production efficiency is low. Summary of the invention

[0006] In view of this, the present invention proposes a U-shaped distillation device for titanium sponge production and a method of using the same, which can at least solve the technical problems in the prior art that the condensation process of volatile vapor is difficult to control and the anti-blocking effect is difficult to judge.

[0007] The first aspect of the present invention provides a U-shaped distillation equipment for sponge titanium production, including a distiller, a condenser and a connecting passage. The distiller includes a distillation electric furnace and a distillation reactor arranged in the distillation electric furnace, and a hot end cover is arranged on the top of the distiller; a cold end cover is arranged on the top of the condenser, and a central hole that passes through the hot end cover and the cold end cover is arranged on each of the hot end cover and the cold end cover. The connecting passage includes a horizontal tube and two vertical tubes connecting the two ends of the horizontal tube, and the lower ends of the two vertical tubes are respectively inserted into the central holes on the hot end cover and the cold end cover; the lower end of the vertical tube inserted into the cold end cover is a closing structure with a diameter gradually decreasing from top to bottom, and a heater is arranged between the outer side of the vertical tube and the hole wall of the central hole.

[0008] In some embodiments, the diameter of the vertical pipe is 90-120 mm, the diameter of the lower end of the closing structure is 30-60 mm, and the inner angle between the wall surface of the closing structure and the horizontal plane is 120°-150°.

[0009] In some embodiments, the heater includes thermal insulation cotton filled in the center hole, a heating wire arranged in the thermal insulation cotton for heating the lower end of the vertical pipe, and the heater corresponding to the condenser also includes a first thermocouple arranged in the thermal insulation cotton for detecting the heating temperature.

[0010] In some embodiments, the outer periphery of the connecting aisle is also wrapped with a heat preservation layer, and an aisle heater for heating the connecting aisle is arranged inside the heat preservation layer.

[0011] In some embodiments, a cold end thermocouple is disposed on one side of the transverse tube close to the cold end cover, and a hot end thermocouple is disposed on one side of the transverse tube close to the hot end cover.

[0012] In some embodiments, the condenser includes a cooling water jacket and a condensation tank disposed in the cooling water jacket. A horizontally placed partition is disposed at the bottom of the condensation tank. A plurality of air flow holes are distributed on the circumferential edge of the partition.

[0013] In some embodiments, the diameter of the air flow hole is 15-30 mm, and the radial distance from the center of the air flow hole to the wall of the condensation tank is 50-100 mm.

[0014] In some embodiments, a second thermocouple (303) extending into the interior of the condenser tank is also provided on the cold end cover, a water inlet valve is provided at the lower position of the cooling water jacket, a first water outlet valve is provided at 1 / 4 of the height of the cooling water jacket from the bottom surface, and a second water outlet valve is provided at 1 / 2 of the height of the cooling water jacket from the bottom surface.

[0015] In some embodiments, the distillation reactor and the condenser are also provided with a vacuum gauge for detecting the internal pressure. The distillation reactor and the condenser are also provided with a vacuum pipe fitted with the inner wall, the upper end of the vacuum pipe passes through the corresponding cold end cover or hot end cover, and is connected to an external vacuum unit, and the vacuum unit includes a low vacuum unit and a high vacuum unit arranged in parallel.

[0016] The second aspect of the present invention provides a method for using a U-shaped distillation device for producing sponge titanium, wherein the U-shaped distillation device comprises a distiller, a condenser and a connecting passage, wherein the two ends of the connecting passage are respectively connected to the distiller and the condenser, wherein one end of the connecting passage connected to the distiller is a hot end connecting passage, and one end of the connecting passage connected to the condenser is a cold end connecting passage, wherein a heater is provided in a cold end cover of the condenser; the method for using the device comprises the following steps: S300, distillation stage: control the temperature of the distiller at 800℃-1020℃, wherein the temperature of the distiller is controlled at 800℃~950℃ at a predetermined time before the start of distillation, and a low vacuum unit is used for exhaust; from the predetermined time after the start of distillation to the stage when the distillation reactor is taken out of the furnace, the temperature of the distiller is controlled at 950℃~1020℃, and if the vacuum pipeline pressure is less than or equal to 10Pa, a high vacuum unit is used for exhaust; during the entire distillation process, the temperature of the hot end connecting aisle is controlled at 850℃~900℃, the temperature of the cold end connecting aisle is controlled at 850℃~900℃, and the temperature of the heater in the cold end cover is controlled at 900℃~950℃.

[0017] In some embodiments, the cooling water jacket of the condenser is provided with a water inlet valve, a first water outlet valve, and a second water outlet valve. The water inlet valve is located below the first water outlet valve, and the second water outlet valve is located above the first water outlet valve.

[0018] In step S300, the distillation stage further includes: S301, from the start of vacuum distillation to the time when the condenser temperature is greater than 400°C, close the first water outlet valve, use the water inlet valve to inlet water, and use the second water outlet valve to drain water; When the condenser temperature is 300℃~400℃, open the first water outlet valve, use the water inlet valve to let water in, and the first water outlet valve to drain water; When the condenser temperature is less than or equal to 300℃, reduce the opening of the water inlet valve until it is completely closed, and control the condenser temperature at 250℃~300℃.

[0019] In some embodiments, the U-shaped distillation device further includes a plurality of vacuum pipes respectively inserted into the distiller and the condenser and connected to an external vacuum unit. The method for using the U-shaped distillation device for titanium sponge production further includes: S400, leak detection stage: if the vacuum distillation time is greater than 30h and the vacuum pipeline pressure is greater than 10Pa, perform leak detection on the distillation reactor, condenser and vacuum pipeline.

[0020] In some embodiments, before step S300, the method further includes: S200, assemble U-shaped distillation equipment: weld the distiller and condenser at the preset position, and weld the two horizontal pipe sections of the connecting aisle through flanges, insert the two vertical pipes into the center holes on the hot end cover of the distiller and the cold end cover of the distiller respectively, and then install the aisle heater and insulation layer on the connecting aisle; at this stage, control the pressure of the distillation reactor and condenser at 5~15kPa.

[0021] In some embodiments, before step S200, the method further includes: S100, argon is charged into the distiller, and the charging pressure is controlled to be 30~50kPa, and the residual Mg and MgCl2 in the distiller are discharged and placed in a ladle protected by argon gas, and returned to the magnesium electrolyte refining furnace.

[0022] The beneficial effects of the present invention are as follows: the U-shaped distillation equipment for titanium sponge production of the present invention sets a closing structure at the lower end of the vertical pipe inserted into the cold end cover, and reduces the cross-sectional area of ​​the passage through the closing structure, so that the friction resistance between the volatile vapor and the pipe wall is reduced, which is conducive to the rapid passage and efficient condensation of the material, and reduces the accumulation and condensation caused by low-speed retention, thereby effectively reducing the risk of blockage of the connecting aisle. In addition, when the present application is in use, the gradient temperature control of the aisle heater in the connecting aisle is used to ensure that the volatile vapor passes to the condenser inlet in a gaseous state, thereby preventing the connecting aisle from being blocked. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For ordinary technicians in this field, other embodiments can be obtained based on these drawings without paying creative work.

[0024] Figure 1 A structural cross-sectional view of a U-shaped distillation device for producing titanium sponge provided in one embodiment of the present invention; Figure 2 A schematic diagram of the structure of a heater installed on a cold end cover provided by an embodiment of the present invention; Figure 3 A schematic structural diagram of a partition provided in one embodiment of the present invention.

[0025] Description of reference numerals: 100. distiller; 101. distillation furnace; 102. distillation reactor; 103. furnace heating wire; 104. hot end cover; 105. condenser; 106. cooling water jacket; 107. condenser tank; 201. connecting passage; 202. hot end thermocouple; 203. cold end thermocouple; 204. insulation layer; 301. heater; 302. cold end cover; 303. second thermocouple; 304. vacuum pipe; 305. water inlet valve; 306. first water outlet valve; 307. second water outlet valve; 401. partition; 402. air flow hole; 501. first thermocouple; 502. heating wire; 503. insulation cotton. DETAILED DESCRIPTION

[0026] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the embodiments of the present invention are further described in detail below in combination with specific embodiments and with reference to the accompanying drawings.

[0027] It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are for distinguishing two non-identical entities with the same name or non-identical parameters. It can be seen that "first" and "second" are only for the convenience of expression and should not be understood as limitations on the embodiments of the present invention. The subsequent embodiments will not explain this one by one.

[0028] refer to Figure 1 In a first aspect, the present invention provides a U-shaped distillation equipment for sponge titanium production, which includes a distiller 100, a condenser 105 and a connecting passage 201. The distiller 100 includes a distillation furnace 101 and a distillation reactor 102 arranged in the distillation furnace 101. The distillation furnace 101 is provided with an electric furnace heating wire 103 for heating the distillation reactor 102. A hot end cover 104 is provided on the top of the distiller 100. A cold end cover 302 is provided on the top of the condenser 105. Both the hot end cover 104 and the cold end cover 302 are provided with a center hole that passes through from top to bottom. The connecting passage 201 includes a horizontal tube and two vertical tubes connecting the two ends of the horizontal tube. The lower ends of the two vertical tubes are respectively inserted into the center holes on the hot end cover 104 and the cold end cover 302. Specifically, as Figure 1 As shown, the horizontal pipe consists of two sections connected by flanges, and each section of the horizontal pipe is welded to a vertical pipe. Figure 2 As shown, the lower end of the vertical tube inserted into the cold end cover 302 is a closing structure with a diameter gradually decreasing from top to bottom, and a heater 301 is arranged between the outer side of the vertical tube and the hole wall of the center hole. The heater 301 is used to heat the gas entering the connecting passage 201 and the condenser 105.

[0029] Compared with the prior art, the present invention sets a closing structure at the lower end of the vertical pipe inserted into the cold end cover 302, and reduces the cross-sectional area of ​​the passage through the closing structure. According to the continuity equation (law of conservation of mass), under the condition of constant flow of incompressible fluid, the flow rate is inversely proportional to the flow area, so the speed of Mg and MgCl2 in the condenser 105 is accelerated. In the condenser 105, when Mg and MgCl2 move at high speed, the friction resistance with the pipe wall is reduced due to the thinning of the dynamic boundary layer, which is conducive to the rapid passage and efficient condensation of the material, and reduces the accumulation and condensation caused by low-speed retention, thereby effectively reducing the risk of blockage of the connecting passage 201.

[0030] In some embodiments, Figure 2 As shown, the diameter of the vertical pipe is 90-120 mm, the diameter of the lower end of the closing structure is 30-60 mm, and the inner angle α between the wall surface of the closing structure and the horizontal plane is 120°-150°. The smaller inlet diameter and the inclined closing structure help to increase the flow rate of the gas, reduce the accumulation of materials at the inlet of the condenser 105, and reduce the risk of blockage.

[0031] In some embodiments, Figure 3 As shown, the heater 301 includes a heat-insulating cotton 503 filled in the center hole, a heating wire 502 arranged in the heat-insulating cotton 503 for heating the lower end of the vertical pipe, and the heater 301 corresponding to the condenser 105 also includes a first thermocouple 501 arranged in the heat-insulating cotton 503 for detecting the heating temperature. The heat-insulating cotton 503 filled in the center hole can effectively reduce heat loss and improve heating efficiency. The heating wire 502 fits tightly to the lower end of the vertical pipe to ensure uniform heat transfer and rapid temperature rise. The first thermocouple 501 built into the heat-insulating cotton 503 can accurately monitor the heating temperature and achieve precise temperature control. According to the temperature information fed back by the first thermocouple 501, the heater 301 can automatically adjust the power to maintain the set temperature range. The first thermocouple 501 is preferably a K-type thermocouple, the heating wire 502 is made of NiCr alloy, preferably Ni20Cr80; the heat-insulating cotton material is preferably aluminum silicate fiber cotton.

[0032] In some embodiments, the outer periphery of the connecting aisle 201 is further wrapped with an insulation layer 204, and an aisle heater 301 for heating the connecting aisle 201 is disposed in the insulation layer 204. The insulation layer 204 can effectively reduce the heat loss to the environment through the outer wall of the connecting aisle 201. The aisle heater 301 ensures that the temperature of the connecting aisle 201 is maintained at a stable level to avoid affecting the distillation effect due to temperature fluctuations.

[0033] In some embodiments, a cold end thermocouple 203 is provided on one side of the transverse tube close to the cold end cover 302 (cold end connection passage), and a hot end thermocouple 202 is provided on one side of the transverse tube close to the hot end cover 104 (hot end connection passage). The cold end thermocouple 203 and the hot end thermocouple 202 can monitor the temperature change during the distillation process in real time to ensure that the distillation process is carried out within a suitable temperature range. According to the data fed back by the thermocouple, the heating power can be automatically adjusted to maintain the stability of the distillation process.

[0034] In some embodiments, the condenser 105 includes a cooling water jacket 106 and a condensation tank 107 disposed in the cooling water jacket 106; a horizontally placed partition 401 is disposed at the bottom of the condensation tank 107, and specifically, the partition 401 is supported by a bracket below. A plurality of air flow holes 402 are distributed on the circumferential edge of the partition 401. The air flow holes 402 on the partition 401 increase the contact area between the volatile vapor and the inner wall of the condensation tank 107, thereby improving the condensation efficiency and strengthening the cooling effect of the volatile vapor on the wall. The design of the air flow holes 402 helps the condensed gas to be evenly distributed in the condensation tank 107, avoiding the problem of local overheating or insufficient condensation.

[0035] In some embodiments, the diameter of the airflow hole 402 is 15-30 mm, and the radial distance from the center of the airflow hole 402 to the wall of the condensation tank 107 is 50-100 mm. By properly adjusting the size and number of the airflow holes 402, the condensation rate of the steam can be controlled, thereby affecting the purity and quality of the product.

[0036] In some embodiments, the cold end cover 302 is further provided with a second thermocouple 303 extending into the interior of the condensing tank 107, a water inlet valve 305 is provided at the lower position of the cooling water jacket 106, a first water outlet valve 306 is provided at 1 / 4 of the cooling water jacket 106, and a second water outlet valve 307 is provided at 1 / 2 of the cooling water jacket 106. According to the temperature of the condensing tank 107 detected by the second thermocouple 303, the opening and closing degree of the water inlet valve 305, as well as the opening and closing of the first water outlet valve 306 and the second water outlet valve 307 are appropriately adjusted, so that the flow rate and flow velocity of the cooling medium can be adjusted, which is suitable for condensing volatile vapors of different temperatures.

[0037] In some embodiments, the distillation reactor 102 and the condenser 105 are also provided with a vacuum gauge for detecting the internal pressure. The distillation reactor 102 and the condenser 105 are also provided with a vacuum pipe 304 that fits the inner wall. The upper end of the vacuum pipe 304 passes through the corresponding cold end cover 302 or the hot end cover 104, and is connected to the external vacuum unit (not shown in the figure). The vacuum unit includes a low vacuum unit and a high vacuum unit arranged in parallel. Specifically, the vacuum pump of the low vacuum unit is a slide valve pump; the vacuum pump of the high vacuum unit is a combination of a second slide valve pump and an oil booster pump. Different vacuum units have different working pressures, among which the working pressure range of the low vacuum unit is 50~101325Pa, with high working pressure and large exhaust volume, but relatively low pumping speed, which is mainly used for preliminary vacuum establishment and rapid exhaust under atmospheric pressure. The vacuum unit of the high vacuum unit has a low working pressure (0.1Pa~50Pa), a small exhaust volume, and a high pumping speed, which is suitable for maintaining a low-pressure high vacuum environment. The present application uses a built-in vacuum pipe 304 to connect with the vacuum pipeline of the vacuum unit for evacuation.

[0038] The second aspect of the present invention provides a method for using the U-shaped distillation device for producing the above-mentioned titanium sponge, comprising the following steps: S300, distillation stage: the temperature of the distiller 100 is controlled at 800℃-1020℃, wherein the temperature of the distiller 100 is controlled at 800℃~950℃ at a predetermined time before the start of distillation (10h before the start of distillation), and a low vacuum unit is used for exhaust; from the predetermined time after the start of distillation (for example, 10h after the start of distillation) to the stage when the distillation reactor 102 is taken out of the furnace, the temperature of the distiller 100 is controlled at 950℃~1020℃, if the pressure of the vacuum pipe 304 is less than or equal to 10Pa, and the temperature of the condenser 100 is less than or equal to 500℃, the high vacuum unit is started for exhaust; during the whole distillation process, the temperature of the hot end connecting aisle is controlled at 850℃~900℃, the temperature of the cold end connecting aisle is controlled at 850℃~900℃, and the temperature of the heater 301 in the cold end cover 302 is controlled at 900℃~950℃. The two ends of the connecting passage 201 are respectively connected to the distiller 100 and the condenser 105, the hot end connecting passage is the end connecting the connecting passage 201 and the distiller 100, the cold end connecting passage is the end connecting the connecting passage 201 and the condenser 105, and the heater in the cold end cover 302 is the heater 301 in the cold end cover 302 of the condenser 105. Specifically, for example, 10 hours before distillation, the temperature of the distillation electric furnace 101 is first increased to 800°C, the temperature of the hot end connecting passage is controlled to be 850°C (measured by the hot end thermocouple 202 of the first aspect embodiment), the temperature of the cold end connecting passage is 850°C (measured by the cold end thermocouple 203 of the first aspect embodiment), and the temperature of the heater 301 in the cold end cover 302 is 880°C (measured by the thermocouple in the cold end cover 302). After the high vacuum unit is started, the temperature of the distillation furnace 101 is controlled at 950℃~1020℃, the temperature of the hot end connecting aisle is controlled at 850℃~900℃, the temperature of the cold end connecting aisle is controlled at 850℃~900℃, and the temperature of the heater 301 in the cold end cover 302 is controlled at 880~900℃.

[0039] The present application ensures that the volatile steam reaches the inlet of the condenser 105 in a gaseous form by controlling the temperature of the aisle heater 301 in the connecting aisle 201 with a gradient, thereby preventing the connecting aisle 201 from being blocked.

[0040] In some embodiments, in step S300, the distillation stage further includes: From the start of vacuum distillation to the time when the temperature of the condenser 105 is greater than 400°C, the first water outlet valve 306 is closed, water is introduced through the water inlet valve 305, and water is discharged through the second water outlet valve 307; at this time, a large amount of cooling water flows, which can quickly cool the volatile gas.

[0041] When the temperature of the condenser 105 is 300° C. to 400° C., the first water outlet valve 306 is opened, water is introduced through the water inlet valve 305 , and the first water outlet valve 306 is used to discharge water; When the temperature of the condenser 105 is less than or equal to 300°C, the opening of the water inlet valve 305 is reduced until it is completely closed, and the temperature of the condenser 105 is controlled at 250°C to 300°C.

[0042] By monitoring the temperature of the condenser 105, when the temperature in the condenser 105 is too low, the cooling intensity of the condenser 105 is reduced; after the reduction is completed, the residual Mg and MgCl2 in the distiller 100 are discharged from the distillation reactor 102 to improve the vacuum distillation efficiency.

[0043] In some embodiments, the method for using the U-type distillation apparatus for titanium sponge production further includes: S400, leak detection stage: if the vacuum distillation time is greater than 30 hours, and the pressure of the vacuum pipe 304 is greater than 10Pa, the distiller 100, the condenser 105, and the vacuum pipe 304 are leak-checked. Specifically, for example, in the distillation stage, if the low vacuum pumping is greater than 10 hours, the pressure of the vacuum pipe 304 is less than or equal to 10Pa, and the temperature of the condenser 105 is less than or equal to 500°C, the vacuum unit composed of the oil booster pump and the slide valve pump is started to pump air; after 20 hours of distillation, if the pressure of the vacuum pipe 304 is still greater than 10Pa, it indicates that there may be a leak, and the distiller 100 and the condenser 105 need to be leak-checked.

[0044] In some embodiments, before step S300, the method further includes: S200, assemble the U-shaped distillation equipment: weld the distiller 100 and the condenser 105 at the preset position, and weld the two horizontal pipe sections connecting the aisle 201 through flanges, insert the two vertical pipes into the center holes on the hot end cover 104 and the cold end cover 302 respectively, and then install the aisle heater 301; in this stage, the pressure of the distillation reactor 102 and the condenser 105 is controlled at 5 to 15 kPa, and the distiller 100 and the condenser 105 are kept in a positive pressure state to prevent the sponge titanium from being contaminated by the air.

[0045] In some embodiments, before step S200, the method further includes: S100, argon is charged into the distillation reactor 102, and the charging pressure is controlled to be 30-50 kPa, and the residual Mg and MgCl2 in the distillation reactor 102 are discharged and placed in a ladle protected by argon gas, and returned to the magnesium electrolyte refining furnace.

[0046] Taking a 10-ton U-shaped furnace as an example, when the total distillation time is greater than 135h, and the temperature of the condenser 105 is lower than 300°C, the pressure of the distillation reactor 102 is lower than 10Pa. If the temperature of the condenser 105 is greater than 350°C, and the pressure of the distillation reactor 102 is greater than 10Pa, and the total distillation time reaches 145h, it is removed from the furnace. The distillation electric furnace 101 is powered off, the aisle heater 301 is powered off, the vacuum valve at the front end of the vacuum unit is closed, and the distillation reactor 102 and the condenser 105 are pressurized to a pressure of 15 to 35kPa, and the vacuum unit is closed. Then, the aisle heater 301 is disassembled, and the flanges of the distillation reactor 102 and the condenser 105 connecting the aisle 201 are cut. After the cutting is completed, the distillation reactor 102 is hoisted into the condenser 105 for cooling, and the pressure is controlled at 15 to 35kPa, and the condenser 105 is transferred to reduction production.

[0047] The technical features of the above embodiments may be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0048] The above-mentioned embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent of the present application shall be subject to the attached claims.

Claims

1. A U-shaped distillation device for producing titanium sponge, comprising a distiller (100), a condenser (105) and a connecting passage (201), characterized in that: The distiller (100) comprises a distillation furnace (101) and a distillation reactor (102) arranged in the distillation furnace (101), and a hot end cover (104) is arranged on the top of the distiller (100); a cold end cover (302) is arranged on the top of the condenser (105), and the hot end cover (104) and the cold end cover (302) are both provided with a central hole that passes through from top to bottom; the connecting passage (201) comprises a horizontal tube and two vertical tubes connecting the two ends of the horizontal tube, and the lower ends of the two vertical tubes are respectively inserted into the central holes on the hot end cover (104) and the cold end cover (302); the lower end of the vertical tube inserted into the cold end cover (302) is a closing structure with a diameter that gradually decreases from top to bottom, and a heater (301) is arranged between the outer side of the vertical tube and the hole wall of the central hole.

2. The U-shaped distillation equipment for titanium sponge production according to claim 1, characterized in that: The diameter of the vertical pipe is 90-120 mm, the diameter of the lower end of the closing structure is 30-60 mm, and the inner angle between the wall surface of the closing structure and the horizontal plane is 120°-150°.

3. The U-shaped distillation equipment for titanium sponge production according to claim 1, characterized in that: The heater (301) comprises thermal insulation cotton (503) filled in the central hole, and a heating wire (502) arranged in the thermal insulation cotton (503) for heating the lower end of the vertical pipe. The heater (301) corresponding to the condenser (105) further comprises a first thermocouple (501) arranged in the thermal insulation cotton (503) for detecting the heating temperature.

4. The U-shaped distillation equipment for titanium sponge production according to claim 1, characterized in that: The outer periphery of the connecting passage (201) is also wrapped with a heat-insulating layer (204), and a passage heater (301) for heating the connecting passage (201) is arranged in the heat-insulating layer (204).

5. The U-shaped distillation equipment for titanium sponge production according to claim 1, characterized in that: A cold end thermocouple (203) is provided on one side of the transverse tube close to the cold end cover (302), and a hot end thermocouple (202) is provided on one side of the transverse tube close to the hot end cover (104).

6. The U-shaped distillation equipment for titanium sponge production according to claim 1, characterized in that: The condenser (105) comprises a cooling water jacket (106) and a condensation tank (107) arranged in the cooling water jacket (106); a horizontally placed partition (401) is arranged at the bottom of the condensation tank (107); and a plurality of air flow holes (402) are distributed on the circumferential edge of the partition (401).

7. The U-shaped distillation equipment for titanium sponge production according to claim 6, characterized in that: The diameter of the air flow hole (402) is 15-30 mm, and the radial distance from the center of the air flow hole (402) to the tank wall of the condensation tank (107) is 50-100 mm.

8. The U-shaped distillation equipment for titanium sponge production according to claim 6, characterized in that: The cold end cover (302) is also provided with a second thermocouple (303) extending into the interior of the condensing tank (107); a water inlet valve (305) is provided at the lower position of the cooling water jacket (106); a first water outlet valve (306) is provided at a height of 1 / 4 of the bottom surface of the cooling water jacket (106); and a second water outlet valve (307) is provided at a height of 1 / 2 of the bottom surface of the cooling water jacket (106).

9. The U-shaped distillation equipment for titanium sponge production according to claim 8, characterized in that: The distillation reactor (102) and the condenser (105) are also provided with a vacuum gauge for detecting the internal pressure; the distillation reactor (102) and the condenser (105) are also provided with a vacuum pipe (304) in contact with the inner wall, the upper end of the vacuum pipe (304) passes through the corresponding cold end cover (302) or hot end cover (104), and is connected to an external vacuum unit, wherein the vacuum unit includes a low vacuum unit and a high vacuum unit arranged in parallel.

10. A method for using a U-shaped distillation device for titanium sponge production, characterized in that: The U-shaped distillation equipment comprises a distiller, a condenser and a connecting passage, the two ends of the connecting passage are respectively connected to the distiller and the condenser, the end of the connecting passage connected to the distiller is a hot end connecting passage, the end of the connecting passage connected to the condenser is a cold end connecting passage, and a heater is arranged in the cold end cover of the condenser; the method of use The following steps are involved: S300, distillation stage: control the temperature of the distiller at 800℃-1020℃, wherein the temperature of the distiller is controlled at 800℃~950℃ at a predetermined time before the start of distillation, and a low vacuum unit is used for exhaust; from the predetermined time after the start of distillation to the stage when the distillation reactor is taken out of the furnace, the temperature of the distiller is controlled at 950℃~1020℃, and if the vacuum pipeline pressure is less than or equal to 10Pa, a high vacuum unit is used for exhaust; during the entire distillation process, the temperature of the hot end connecting aisle is controlled at 850℃~900℃, the temperature of the cold end connecting aisle is controlled at 850℃~900℃, and the temperature of the heater in the cold end cover is controlled at 900℃~950℃.

11. The method for using the U-shaped distillation equipment for titanium sponge production according to claim 10, characterized in that: The cooling water jacket of the condenser is provided with a water inlet valve, a first water outlet valve, and a second water outlet valve, wherein the water inlet valve is located below the first water outlet valve, and the second water outlet valve is located above the first water outlet valve; In step S300, the distillation stage further includes: S301, from the start of vacuum distillation to the time when the condenser temperature is greater than 400°C, close the first water outlet valve, use the water inlet valve to inlet water, and use the second water outlet valve to drain water; When the condenser temperature is 300℃~400℃, open the first water outlet valve, use the water inlet valve to let water in, and the first water outlet valve to drain water; When the condenser temperature is less than or equal to 300℃, reduce the opening of the water inlet valve until it is completely closed, and control the condenser temperature at 250℃~300℃.

12. The method for using the U-shaped distillation equipment for titanium sponge production according to claim 10, characterized in that: The U-shaped distillation equipment further includes a plurality of vacuum pipes respectively inserted into the distiller and the condenser and connected to an external vacuum unit, and the method of use further includes: S400, leak detection stage: If the vacuum distillation time is greater than 30h and the vacuum pipeline pressure is greater than 10Pa, perform leak detection on the distiller, condenser and vacuum pipeline.

13. The method for using the U-shaped distillation equipment for titanium sponge production according to claim 10, characterized in that: Before step S300, the method further includes: S200, assemble U-shaped distillation equipment: weld the distiller and condenser at the preset position, and weld the two horizontal pipe sections of the connecting aisle through flanges, insert the two vertical pipes into the center holes on the hot end cover of the distiller and the cold end cover of the condenser respectively, and then install the aisle heater and insulation layer on the connecting aisle; at this stage, control the pressure of the distillation reactor and condenser at 5~15kPa.

14. The method for using the U-shaped distillation equipment for titanium sponge production according to claim 13, characterized in that: Before step S200, the method further includes: S100, argon is charged into the distiller, and the charging pressure is controlled to be 30~50kPa, and the residual Mg and MgCl2 in the distiller are discharged and placed in a ladle protected by argon gas, and returned to the magnesium electrolyte refining furnace.

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