Low-chlorine high-porosity titanium sponge production device and use method

Abstract

The application discloses a low-chlorine high-porosity titanium sponge production device and a use method thereof. The production device comprises a reactor and a condenser which are connected through a pipeline. An upwardly-extending pore-forming assembly is arranged at the middle lower part of the reactor. The pore-forming assembly comprises a conical top and a straight section. A plurality of split leaves are arranged at the bottom of the pore-forming assembly. A discharge pipe is arranged at the bottom of the reactor and is connected with a feeding port of a ladle. A shut-off valve is arranged between the reactor and the condenser. The application sets the disconnectable valve at the passageway of the distiller and the condenser, realizes the quick disconnection of the distiller and the condenser, provides equipment conditions for judging the vacuum distillation end point by using the 'pressure rising method', and improves the mass transfer efficiency of Mg / MgCl2 at the central part of the titanium lump by additionally arranging the pore-forming equipment on the titanium lump.

Description

Technical Field

[0001] This invention relates to the technical field of sponge titanium production methods, and in particular to a low-chlorine, high-porosity sponge titanium production apparatus and its usage method. Background Technology

[0002] Titanium sponge is a crucial basic material for the preparation of titanium and titanium alloys, and it is an important raw material for the manufacture of aerospace, shipbuilding, chemical, and biomedical equipment. The properties of titanium sponge directly affect the properties of titanium and titanium alloys. Chlorine impurities in titanium sponge have a significant impact on the corrosiveness of titanium and titanium alloy materials; therefore, it is necessary to strictly control the vacuum distillation process of titanium sponge to obtain products with chlorine impurity content meeting requirements.

[0003] For example, Chinese patent application publication number CN 114703380 A proposes a method for producing ultra-low chlorine content sponge titanium, which uses argon purging to remove chlorine from the sponge titanium agglomerate produced by distillation. During the distillation process, argon gas is introduced into the reactor through an argon gas inlet to control the chlorine impurity content.

[0004] Chinese patent CN 219824312 U discloses a vacuum distillation device for sponge titanium with controllable chlorine content. It precisely controls the temperature and vacuum level at each stage of the distillation process through a vacuum pump and distillation components, thereby improving distillation efficiency, greatly reducing the chlorine content in the finished sponge titanium product, and improving product quality. The rectifier components ensure uniform and rapid heating around the reactor, achieving uniform distillation operation.

[0005] Chinese patent application publication number CN 118421973 A proposes a method for reducing the chlorine content of sponge titanium products. It further removes chlorine impurities from sponge titanium by water washing, drying, and vacuum degassing to solve the problem of excessive chlorine in sponge titanium.

[0006] Chinese patent application publication number CN 121294886 A proposes a method for reducing the chlorine content of sponge titanium by re-heating and vacuum distillation.

[0007] To address the issues of low efficiency in the vacuum distillation process of titanium sponge and the difficulty in preparing titanium sponge with low chlorine content, the following patent provides a solution to enhance the vacuum distillation process.

[0008] For example, Chinese patent application publication number CN 115679123 A proposes a composite sponge titanium reduction discharge process, which reduces the amount of material to be vacuum distilled by discharging the remaining Mg / MgCl2 in the container after the reduction reaction.

[0009] Chinese patent application publication number CN 117385195 A proposes a production apparatus for high-stability, low-packaging-density sponge titanium. When producing sponge titanium using the magnesothermic reduction method, a large-diameter central titanium rod is installed in the center of the flange at the top of the reduction distillation furnace before the reduction reaction. During the distillation process, a high-frequency induction heater is installed at the original location of the large-diameter central titanium rod to heat the titanium mass from the center.

[0010] Existing technologies do not offer feasible solutions to the problem of residual low-valent titanium chlorides such as titanium dichloride and titanium trichloride generated during the reduction process affecting vacuum distillation efficiency and the chlorine content of the finished sponge titanium product. In addition, the residual Mg / MgCl2 is not effectively removed before distillation, resulting in a high distillation load and long time. Furthermore, the accuracy of determining the endpoint of vacuum distillation is poor, and the separation of chlorine impurities is insufficient.

[0011] In view of this, improvements should be made to the existing technology. Summary of the Invention

[0012] The main objective of this invention is to provide a low-chlorine, high-porosity sponge titanium production apparatus. By installing a disconnectable valve on the connecting pipe between the distiller and condenser, the distiller and condenser can be quickly disconnected, providing the equipment conditions for determining the endpoint of vacuum distillation using the "pressure rise method". By installing a discharge pipe detachably connected to the ladle at the bottom of the reactor, residual Mg / MgCl2 melt in the reactor can be discharged in advance before distillation, reducing the vacuum distillation load. At the same time, by adding a pore-forming component to the titanium agglomerate, the mass transfer efficiency of Mg / MgCl2 in the central part of the titanium agglomerate is improved.

[0013] According to one aspect of the present invention, a low-chlorine, high-porosity sponge titanium production apparatus is provided, comprising a reactor and a condenser connected by a pipeline, wherein an upwardly extending pore-forming component is provided in the lower middle part of the reactor, the pore-forming component includes a conical apex and a straight section, and a plurality of lobes are provided at the bottom of the pore-forming component, a discharge pipe is provided at the bottom of the reactor, the discharge pipe is connected to the feed inlet of a lifting bag, and an isolation valve is provided between the reactor and the distiller.

[0014] According to one embodiment of the present invention, the height ratio of the pore-forming component to the reactor is 0.65 to 0.8:1.

[0015] According to one embodiment of the present invention, the ratio of the straight section of the pore-forming component to the height of the reactor is 0.5 to 0.6:1.

[0016] According to one embodiment of the present invention, multiple leaflets are at 90° to each other and are connected by a connecting pipe.

[0017] According to one embodiment of the present invention, the connecting pipe is a hollow steel pipe with a diameter of 10~20cm.

[0018] According to one embodiment of the present invention, the reactor is provided with an argon filling port and an argon venting port, and a volatile storage tank is provided at the outlet of the argon venting port.

[0019] According to one embodiment of the present invention, a reduction furnace is provided outside the reactor, and the reduction furnace includes multiple sections from bottom to top, wherein the heating range of the first section located at the top is 750~1020°C.

[0020] According to one embodiment of the present invention, a thermocouple is provided on the condenser, and an automatic flow control valve is provided at the cooling water inlet of the condenser.

[0021] According to another aspect of the present invention, a method of using a low-chlorine, high-porosity sponge titanium production apparatus is provided, comprising the following steps: S1. Place the pore-forming component in the reactor, add liquid magnesium and titanium tetrachloride to the reactor for reduction, and after the reduction is completed, heat the reactor to 850~880℃ and hold for 2~3 hours. S2. Argon gas is introduced into the upper space of the reactor to discharge the free liquid magnesium and MgCl2 remaining at the bottom of the reactor into the lifting bag. The lifting bag is protected by argon gas, and the pressure of the lifting bag is 1~3 kPa. S3. After the residual Mg / MgCl2 is discharged, the reactor is used as a distillation apparatus for distillation. The distillation apparatus and condenser are connected by an isolation valve and the vacuum system is started. The temperature of the first section is raised to 900~1020℃, and argon gas is introduced through the argon filling port to purge the titanium block. S4. Then, heat the other zones of the reduction furnace to 950~1020℃; S5. When the distillation time is ≥12h / t, close the isolation valve between the distiller and the condenser. If the pressure rise of the distiller - the pressure rise of the airtightness is ≤0.2Pa / min, then the product is discharged from the furnace; otherwise, it is discharged from the furnace after 13h / t.

[0022] According to one embodiment of the present invention, during the vacuum distillation process, the condensation temperature is monitored by a thermocouple, and cooling water is injected from the bottom of the condenser and flows out from the upper valve; the cooling water inlet valve has an automatic adjustment function, and when the condenser temperature drops at a rate ≤2℃ / h or rises, the cooling water flow rate is automatically increased; if the condenser temperature drops at a rate ≥5℃ / h, the cooling water flow rate is decreased.

[0023] In a low-chlorine, high-porosity sponge titanium production apparatus according to an embodiment of the present invention, a disconnectable valve is installed in the passageway between the distiller and the condenser to achieve rapid disconnection between the distiller and the condenser, providing equipment conditions for determining the endpoint of vacuum distillation using the "pressure rise method"; at the same time, by adding pore-forming equipment to the titanium mass, the mass transfer efficiency of Mg / MgCl2 in the central part of the titanium mass is improved. Attached Figure Description

[0024] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some implementation examples of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 A schematic diagram of the reduction reaction apparatus of a low-chlorine, high-porosity sponge titanium production device according to an exemplary embodiment of the present invention is shown. Figure 2 A schematic diagram of the structure of a vacuum distillation apparatus for producing low-chlorine, highly porous sponge titanium according to an exemplary embodiment of the present invention is shown. Figure 3 A cross-sectional view of a pore-forming component of a low-chlorine, high-porosity sponge titanium production apparatus according to an exemplary embodiment of the present invention is shown. Figure 4 A schematic diagram of the pore-forming component of a low-chlorine, high-porosity sponge titanium production apparatus according to an exemplary embodiment of the present invention is shown. In the diagram: 101. Argon filling port; 102. Argon venting port; 103. Volatile substance storage tank; 201. Feed inlet; 202. Discharge pipe; 203. Lifting bag; 204. Reactor; 205. Condenser; 206. Thermocouple; 207. Vacuum gauge; 208. Isolation valve; 209. Vacuum system; 210. Cooling water inlet valve; 211. Cooling water outlet valve; 301. Reduction furnace; 302. Section 1; 303. Section 2; 304. Section 3; 305. Section 4; 306. Section 5; 307. Section 6; 401. Hole forming component; 402. Leaf segmentation. Detailed Implementation

[0026] The following detailed description of the embodiments is intended to exemplify the principles of the present invention, but should not be construed as limiting the scope of the invention. The present invention can be implemented in many different forms and is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

[0027] These embodiments are provided to make this disclosure thorough and complete, and to fully express the scope of the invention to those skilled in the art. It should be noted that, unless otherwise specifically stated, the relative arrangement of components and steps, material composition, numerical expressions, and values ​​set forth in these embodiments should be interpreted as merely exemplary and not as limiting.

[0028] It should be noted that, in the description of this invention, unless otherwise stated, "a plurality of" means two or more; the terms "upper," "lower," "left," "right," "inner," and "outer," etc., indicating orientation or positional relationships, are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0029] It should also be noted that, in the description of this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this invention depending on the specific circumstances. When a specific device is described as being located between a first device and a second device, an intermediary device may or may not be present between the specific device and the first or second device.

[0030] All terms used in this invention have the same meaning as understood by one of ordinary skill in the art to which this disclosure pertains, unless otherwise specifically defined. It should also be understood that terms defined in general dictionaries should be interpreted as having meanings consistent with their meanings in the context of the relevant art, and not as idealized or highly formalized, unless expressly defined herein.

[0031] Techniques, methods, and equipment known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and equipment should be considered part of the specification.

[0032] like Figure 1 and 2 As shown, the present invention provides a low-chlorine, high-porosity sponge titanium production apparatus, which includes a reactor 204 and a condenser 205 connected by pipes. A pore-forming component 401 extending upward is provided in the lower middle part of the reactor 204. The pore-forming component 401 includes a conical apex and a straight section. Multiple lobes 402 are provided at the bottom of the pore-forming component 401. A discharge pipe 202 is provided at the bottom of the reactor 204. The discharge pipe 202 is connected to the feed inlet of the lifting bag 203. An isolation valve 208 is provided between the reactor 204 and the distiller.

[0033] According to an embodiment of the present invention, the low-chlorine, high-porosity sponge titanium production apparatus achieves rapid disconnection between the distiller and condenser 205 by installing a disconnectable valve in the passageway of the distiller and condenser 205, providing equipment conditions for determining the endpoint of vacuum distillation using the "pressure rise method"; at the same time, by adding pore-forming equipment to the titanium agglomerate, the mass transfer efficiency of Mg / MgCl2 in the central part of the titanium agglomerate is improved.

[0034] In this invention, reactor 204 serves as both a reduction reactor 204 and a distillation reactor 204, and is connected to condenser 205 by the opening and closing of isolation valve 208.

[0035] The top of the reactor 204 is provided with a feeding port 201 for feeding materials.

[0036] In some specific embodiments, the ratio of the height (H2) of the pore-forming component 401 to the height (H3) of the reactor 204 is 0.65 to 0.8:1.

[0037] Based on the above embodiments, the ratio of the straight section (H1) of the hole forming component 401 to the height of the reactor 204 is 0.5~0.6:1.

[0038] The ratio of the transverse width (D2) to the diameter (D1) of reactor 204 is 0.5~0.6:1.

[0039] These proportional parameters divide the sponge titanium accumulated in reactor 204 into 4 groups of petals, with the top of the pore-forming component 401 exposed at the very top of the titanium mass.

[0040] like Figure 3 and 4 As shown, in some specific embodiments, multiple leaflets 402 are at 90° to each other, and the leaflets 402 are connected by connecting pipes.

[0041] Specifically, there are four leaflets 402, and the hole-forming assembly 401 is connected to the four leaflets 402 by welding.

[0042] By adding a pore-forming component to the titanium agglomerate, the agglomerate is divided into four parts due to the difference in expansion coefficients between the pore-forming component and the titanium agglomerate. During vacuum distillation, the volatilization area of ​​the titanium agglomerate increases, and the resistance to the diffusion and migration of Mg and MgCl2 in the central pores of the titanium agglomerate to the surface decreases. Therefore, the pore-forming component improves the mass transfer efficiency of Mg / MgCl2 in the central part of the titanium agglomerate.

[0043] Based on the above embodiments, the connecting pipe is a hollow steel pipe with a diameter of 10~20cm.

[0044] Based on the above embodiments, a vacuum gauge 207 is provided on the reactor 204.

[0045] In some specific embodiments, reactor 204 is provided with an argon filling port 101 and an argon venting port 102, and a volatile matter storage tank 103 is provided at the outlet of the argon venting port 102. The volatile matter storage tank 103 is used to store TiCl2 and TiCl3.

[0046] Based on the above embodiments, the isolation valve 208 is a pneumatic valve that can be remotely controlled.

[0047] Based on the above embodiments, a reduction furnace 301 is provided outside the reactor 204. The reduction furnace 301 has a heating function and includes 6 zones from bottom to top, wherein the heating range of the first zone 302 located at the top is 750~1020℃.

[0048] The six partitions, from bottom to top, are partition 1 (302), partition 2 (303), partition 3 (304), partition 4 (305), partition 5 (306), and partition 6 (307).

[0049] In some specific embodiments, a thermocouple 206 is provided on the condenser 205, and a cooling water inlet and a cooling water outlet are provided on the condenser 205. A cooling water inlet valve 210 is provided on the cooling water inlet, and a cooling water outlet valve 211 is provided on the cooling water outlet. The cooling water inlet valve 210 is an automatic flow control valve.

[0050] Based on the above embodiments, the discharge pipe 202 is a magnesium chloride discharge pipe 202, which extends into the bottom of the reactor 204 and is connected to the feed inlet of the lifting bag 203. The lifting bag 203 has an argon protection function.

[0051] The present invention also provides a method of using a low-chlorine, high-porosity sponge titanium production apparatus, which includes the following steps: S1. Place the hole-forming component 401 in the reactor 204, add liquid magnesium and titanium tetrachloride to the reactor 204 for reduction, and after the reduction is completed, heat the reactor 204 to 850~880℃ and hold for 2~3 hours. S2. Argon gas is introduced into the upper space of reactor 204 to discharge the free liquid magnesium and MgCl2 remaining at the bottom of reactor 204 into the lifting bag 203. The lifting bag 203 is protected by argon gas, and the pressure of the lifting bag 203 is 1~3 kPa. S3. After the residual Mg / MgCl2 is discharged, the reactor 204 is used as a distillation apparatus for distillation. The distillation apparatus is connected to the condenser 205 through the isolation valve 208 and the vacuum system 209 is started to raise the temperature of the first section 302 to 900~1020℃ and argon gas is introduced through the argon filling port 101 to purge the titanium block. S4. Then, heat the other zones of the reduction furnace 301 to 950~1020℃; S5. When the distillation time is ≥12h / t, close the isolation valve 208 between the distiller and the condenser 205. If the pressure rise of the distiller - the pressure rise of the airtightness is ≤0.2Pa / min, then the product is discharged from the furnace; otherwise, it is discharged from the furnace after 13h / t.

[0052] In one specific embodiment, during the vacuum distillation process, the condensation temperature is monitored by thermocouple 206, and cooling water is injected from the bottom of condenser 205 and flows out from the upper valve; the cooling water inlet valve 210 has an automatic adjustment function, which automatically increases the cooling water flow rate when the temperature of condenser 205 drops at a rate ≤2℃ / h or rises; and decreases the cooling water flow rate if the temperature of condenser 205 drops at a rate ≥5℃ / h.

[0053] This method involves purging and replacing the reduced product with argon gas to remove the TiCl2 and TiCl3 generated during reduction from the reactor. The reducer temperature is then controlled in stages to fully reduce the titanium dichloride and titanium trichloride adhering to the reactor walls. High-temperature constant temperature control of the distiller and the removal of Mg / MgCl2 further reduce the TiCl2 and TiCl3 within the reactor and remove any remaining free Mg / MgCl2, thus reducing the distillation load. Intelligent control of the condenser's cooling intensity improves vacuum distillation efficiency, while a pressure rise method is used to assess the amount of MgCl2 volatilized at the end of distillation, ensuring the stable production of low-chloride-content sponge titanium.

[0054] One specific application of this invention is as follows: S1: The pore-forming component is placed in the reactor before the addition of titanium tetrachloride. 22 tons of liquid magnesium are added to the reactor, followed by batches of TiCl4, with a total addition of 40 tons of TiCl4. After reduction, the temperature of section 1 is raised to 850~880℃ and held for 2~3 hours. S2: Argon gas is introduced into the upper space of the reactor to replace the atmosphere. The argon filling port is opened and the pressure relief valve is opened to enrich the volatilized TiCl2 and TiCl3 in the volatile storage tank.

[0055] S3: Heat the first to sixth sections of the electric furnace to 850℃ and hold for 2 hours. Then connect the MgCl2 flask to the magnesium chloride discharge pipe, fill the upper space of the reactor with argon, and control the pressure at 40 kPa. The remaining free liquid magnesium and MgCl2 at the bottom of the reactor are discharged into the flask, and the pressure in the upper space of the flask is controlled at 1~3 kPa.

[0056] S4: The distiller and condenser are connected by an isolation valve; and the vacuum system is started. Then, the first section is heated to 900~1020℃ and argon gas is introduced through the argon filling port to purge the titanium block. S5: Increase the temperature of the other zones of the electric furnace to 950~1020℃; S6: When the distillation time is 120h, close the isolation valve between the still and the condenser. When the pressure rise of the still - the airtightness pressure rise is 0.2Pa / min, then proceed with the discharging.

[0057] S7: During the vacuum distillation process, the condenser temperature is monitored by thermocouples inside the condenser. Cooling water is injected from the bottom valve of the condenser and flows out from the top valve. The cooling water inlet valve has an automatic adjustment function. When the condenser temperature drops at a rate ≤2℃ / h or rises, the cooling water flow rate is automatically increased; if the condenser temperature drops at a rate ≥5℃ / h, the cooling water flow rate is decreased.

[0058] The titanium sponge produced using this method can have its chloride content stably controlled at 0.030% or below, and the encapsulation density of the finished titanium sponge can reach 1.50 g / cm³. 3 the following.

[0059] The above are exemplary embodiments disclosed in this invention. The order of the disclosed embodiments is merely for descriptive purposes and does not represent the superiority or inferiority of the embodiments. However, it should be noted that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the disclosed embodiments of this invention (including the claims) is limited to these examples. Various changes and modifications can be made without departing from the scope defined by the claims. The functions, steps, and / or actions of the methods according to the disclosed embodiments described herein do not need to be performed in any particular order. Furthermore, although the elements disclosed in the embodiments of this invention may be described or claimed individually, they may be understood as multiple unless explicitly limited to a singular.

[0060] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the invention (including the claims) is limited to these examples. Within the framework of the invention, technical features of the above embodiments or different embodiments can be combined, and many other variations of the different aspects of the invention as described above exist, which are not provided in the details for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the invention should be included within the protection scope of the invention.

Claims

1. A low-chlorine, high-porosity sponge titanium production apparatus, comprising a reactor and a condenser connected by pipes, characterized in that, The reactor is equipped with a pore-forming assembly extending along the height of the reactor. The pore-forming assembly includes a conical apex and a straight section. The pore-forming assembly includes a central tube and multiple lobes fixed to the outer wall of the central tube and arranged circumferentially. A discharge pipe is provided at the bottom of the reactor. The discharge pipe is detachably connected to the feed inlet of the lifting bag to discharge residual Mg and MgCl2 in the reactor. An isolation valve is provided on the pipeline between the reactor and the condenser.

2. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 1, characterized in that, The height ratio of the pore-forming component to the reactor is 0.65~0.8:

1.

3. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 1, characterized in that, The ratio of the straight section of the pore-forming component to the height of the reactor is 0.5~0.6:1, and the ratio of the transverse width of the straight section of the pore-forming component to the diameter of the reactor is 0.5~0.6:

1.

4. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 1, characterized in that, The included angle between adjacent lobes is 90°.

5. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 4, characterized in that, The central tube is a hollow steel tube with a diameter of 10-20cm.

6. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 1, characterized in that, The reactor is equipped with an argon filling port and an argon venting port, and the argon venting port is connected to a volatile storage tank.

7. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 1, characterized in that, The reactor is equipped with a reduction furnace outside, which includes multiple sections from bottom to top, wherein the heating range of the first section at the bottom is 750~1020℃.

8. The low-chlorine, high-porosity sponge titanium production apparatus according to claim 1, characterized in that, The condenser is equipped with a thermocouple, and the cooling water inlet of the condenser is equipped with an automatic flow control valve.

9. A method of using the low-chlorine, high-porosity sponge titanium production apparatus as described in any one of claims 1-8, characterized in that, Includes the following steps: S1. Place the pore-forming component in the reactor, add liquid magnesium and titanium tetrachloride to the reactor for reduction, and after the reduction is completed, heat the reactor to 850~880℃ and hold for 2~3 hours. S2. Argon gas is introduced into the upper space of the reactor to discharge the free liquid magnesium and MgCl2 remaining at the bottom of the reactor into the lifting bag. The lifting bag is protected by argon gas, and the pressure of the lifting bag is 1~3 kPa. S3. After the residual Mg and MgCl2 are discharged, the reactor is used as a distillation apparatus for distillation. The distillation apparatus and condenser are connected by an isolation valve and the vacuum system is started. The temperature of the first section is raised to 900~1020℃, and argon gas is introduced through the argon filling port to purge the titanium block. S4. Then, heat the other zones of the reduction furnace to 950~1020℃; S5. When the distillation time is ≥12h / t, close the isolation valve between the distiller and the condenser. When the pressure rise of the distiller - the pressure rise of the airtightness is ≤0.2Pa / min, then the product is discharged from the furnace. Otherwise, continue distilling until the preset maximum distillation time is reached before discharging.

10. The method of using the low-chlorine, high-porosity sponge titanium production apparatus according to claim 9, characterized in that, During vacuum distillation, the condensation temperature is monitored by thermocouples. Cooling water is injected from the bottom of the condenser and flows out from the upper outlet valve. The cooling water inlet valve has an automatic adjustment function. When the condenser temperature drops at a rate ≤2℃ / h or rises, the cooling water flow rate is automatically increased. If the condenser temperature drops at a rate ≥5℃ / h, the cooling water flow rate is decreased.

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