TW201043707A - Device and method for producing high purity metals - Google Patents

Abstract

The present invention relates to a device and method for producing high purity metals applying separation and purification techniques. The device includes a mixing feeder, a heating melting reactor, a liquid-liquid phase separation device and a liquid-gas phase separation device, wherein the mixing feeder and the heating melting reactor mix high purity metal powder with metal halide salts. By removing gaseous impurities, heating to melt the mixture is heated and melted into liquid phase. By utilizing the liquid-liquid separation device, the two phases are initially purified and separated, and the liquid-gas phase separation device then is utilized to perform a gas-liquid purification and separation process for metals and metal halide slats in the pressure reduction and temperature rising manners to obtain high purity metal products that is greater than grade 6N.

Description

201043707 VI. Description of the Invention: [Technical Field] The present invention relates to a device and a method for producing high-purity metal by a separation technique, in particular, a mixture of metal powder and toothed salt, liquid liquid and liquid gas A device and method for separating and purifying to produce high purity metals. [Prior Art] In recent years, due to the rise of the solar energy industry, the demand for the production of solar grade or electronic grade high purity germanium has increased. The method of mass production of high purity Shixi in the industrial sector mainly uses the Siemens gas/child method. However, this practice Knowing the Siemens method is a high-energy, low-efficiency production method that generates more than 100 kilowatt-hours of electricity per kilogram (kwh). The improved Siemens method uses a fluidized bed method, which reduces energy consumption. There are still 1〇2〇% of tantalum powder with a particle size smaller than micrometer. The powder is too oxidized due to excessive surface area and is not easily melted. In order to solve the above-mentioned problem of the application of the conventional method of the Siemens method, there are many prior patents for purifying the technology to obtain the purity of the block, for example, the US invention patent No. 4 '388 '286 "Siliconpurification" case, It is disclosed that the alkali gold-doped toothed salt is mixed with the cerium powder, and the mixture is melted by a high temperature of 141 〇〇 C or higher, and the toothed salt is separated from the hydrazine by standing, and high purity hydrazine is obtained by coldness, but gravity is simply used. Conditions for liquid-liquid two-phase separation must be allowed to stand for a long time, and is not suitable for industrial production. U.S. Patent No. 4,612, Π9, "Process for puriflcation 〇fs〇lid silicc^", which uses a semiconductor body grade stone powder having a particle size of less than 1 mm (mm) mixed with ultrapure sodium fluoride (NaF). Below the dream melting temperature of 13 (8) - 141 (Γ (:, by the sodium fluoride molten salt to remove the impurities on the surface of the powder, after cooling, then acid water cleaning method, remove sodium fluoride to obtain bismuth, this method Since the granules are not melted, the particle size cannot be increased, and it is difficult to recover the 夕 粒径 粒径 粒径 粒径 。 。 。 。 。 。 ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' No. "Ground plus for producing consolidated materials", which uses a semiconductor grade of Shixi powder and a halogenated metal salt, which is mixed and heated to 14 摄-i8 〇〇 ° C, hard and fluorinated 3 201043707 nanomixture In the presence of a liquid-liquid phase, the separation of ruthenium and sodium fluoride into two phases is carried out by using the different specific gravity of the two liquids, and the two solid phases are separated by cooling to room temperature. Using gravity separation method, it must be left standing for a long time In order to reduce the two-phase mixing interface, there are still problems and shortcomings that are not suitable for industrial mass production. [Summary of the Invention] The conventional method or method for purifying high-purity metal by the Siemens method or the fluidized bed method is simply performed by using gravity conditions. The liquid-liquid two-phase separation must be allowed to stand for a long time, and is not suitable for industrial mass production, or the method of removing the metal halide salt by acid water cleaning to obtain the metal, the particle size cannot be increased, and the acid water cleaning method is difficult to recover. The metal powder of i mm © particle size, without industrial use value. Therefore, the object of the present invention is to provide a high-purity metal separation and purification apparatus and method for high-purity metal powder, such as strontium powder, and halogenation. After the metal salt is mixed and melted, the two-phase interface is accelerated to achieve the effect of industrially producing high-purity yttrium, and the gas powder can be completely recovered and purified by using the gas-liquid separation. The high-purity metal of the present invention can be produced. The apparatus comprises: a mixing feeder for supplying a high-purity metal powder and a toothed metal salt feed to form a solid mixture; heating The smelting reactor is connected to the mixing feeder, and the mixed zero-purity high-purity metal powder of the mixed feeder and the self-chemical metal salt mixture are placed in the reactor, and the vacuum is filled with argon (Ar) The inert gas is used to remove the impure gas and the water gas in the reactor cabin, and the mixture is heated to melt by a heater; the liquid phase separation device is connected to the squaring reaction n, and the molten mixture in the hetero-melt reactor is mixed The primary phase of the metal and the metal self-salting salt is subjected to preliminary purification, so that the impurities are discharged along with the metal toothed salt liquid to obtain a mixture of a high concentration of metal and a small amount of a salt of a southern salt; and a gas phase separation device of the y liquid , connecting the liquid phase separation device, preliminarily purifying the high concentration metal with a small amount of the liquid chemical separation liquid, and separating the gas and liquid by heating under reduced pressure to make the toothed salt and the impurity from the molten metal Volatile, accelerate separation of the two-phase mixed interface to obtain your grade high purity metal. 4 201043707 The apparatus of the present invention described above, wherein the solid mixture of the high purity metal powder and the toothed metal salt in the mixing feeder can be obtained by reacting a high purity toothed metal with an alkali metal. The above apparatus of the present invention, wherein a solid mixture of the high-purity metal powder and the toothed metal salt in the mixed feeder can be obtained by reacting a high-purity metal halide with an alkaline earth metal. The above apparatus of the present invention, wherein the solid mixture of the high-purity metal powder and the toothed metal salt in the mixing feeder may be composed of a mixture of a semiconductor grade niobium powder and a high-purity halogenated metal salt. Ο

The apparatus of the present invention described above in which the liquid vapor phase separation apparatus is separated is a sputum liquid which can be directly guided to the field of crystal growth, directional solidification or related polysilicon. The method for producing high-purity metal of the present invention comprises the steps of: a) forming a solid mixture of a high-purity metal powder and a metal halide; mixing and adding a high-purity metal powder and a metal toothed salt to the mixed feeder to form a high a solid mixture of a purity metal powder and a metal halide; ' b. evacuating and removing impure gas and moisture, placing a solid mixture of the high purity metal powder of step a and the metal halide salt in a heated melt reactor, repeatedly vacuuming (less than 5 Par) and impure gas to remove the impure gas and water gas in the reactor; heating and melting 'heating the mixture of the metal powder of step b and the metal toothed salt mixture to a molten mixture; d. Metal and metal self-chemical ribbed green, will pour the age of the human body liquid phase liquid separation liquid separation device to separate the pin metal bismuth salt to form a high / long metal and a small amount of self-chemical salt mixture e. Gas-phase separation of metal and metal toothed salt liquid 'Introducing the high concentration of metal in step d with a small amount: 幽 = mixture into the gas-liquid separator, and then using the gas-liquid separation heated under reduced pressure ^ Operation of 'the salt with a gas-volatile gaseous impurities and form a purified liquid metal 5 201043707 f · extraction of high purity metal, high purity liquid metal by the step. The bottom of the liquid gas phase separator of e is extracted to obtain the 6N-stage method of the present invention. The solid mixture of the salt of the step a can be obtained by the high-purity metal. The method of the present invention is as described above. The device for producing high-purity metal of the invention has the advantage that the metal ruthenium can effectively purify the impurities on the surface of the metal powder; oxidation:=

= two impurities and toothed salt separated from the liquid metal to achieve preliminary purification, and then paste the heated album, so that the oxidized carbonized 矽 = 0), self-made slave phosphorus π pure matter late _ impurity purification, and The change of the soap is purely by gravity, and the village is formed to test the two-phase disambiguation to the purpose of mass production. And the final derivative of the apparatus and method of the present invention is pure liquid gold > 1 ' 'Can be directly produced in the high-tech electronics industry or the solar energy industry _ paste product process, the raw material energy consumption and cost. [Embodiment]

First, referring to the first figure, the apparatus 100' for producing high-purity metal of the present invention comprises a mixing feeder 10, which further comprises at least one feeding container 11 and a feed. Controlling the width 12, the feed container u is used to mix the high-purity metal powder with the halogenated metal salt feed to form a solid mixture 200. The formation of the solid mixture 2 (10) can also be obtained by reacting a high-purity metal halide with an alkali metal group metal, or by high purity. The bismuth halide is reacted with an alkaline earth metal, and the feed control valve 12 is coupled to the lower side of the feed vessel ' to control the rotation of the solid mixture 200 in the feed vessel 11 by the feed control valve 12. A heating and melting reactor 20' is connected to the mixing feeder 1A, and the heating and melting reactor 2 further comprises a melting vessel 21, a melting heating device 22 and a melting vessel discharge control valve 23', wherein the melting vessel 21 can It is made of graphite or tantalum carbide (SiC) or other high temperature resistant material. The top of the melting vessel 21 is provided with at least one inlet 6 201043707, 211, vacuum suction port 212 and inert gas inlet 213. The feed of 10. The μ inlet port 211 is controlled by the feed control valve 12, and the two purity metal powders _ in the secretor 11 are input into the ablation container 21, and the vacuum suction port 212 is provided. For the second thing, the internal part of the fusion article 21 is to reduce the air, the inert gas population ^ into the like, the gas, the mixed dance 21 _, the Wei device cry: the mouth 214 'the outside of the melting container 21' coated - The layer melts the containment layer 215' to prevent heat loss from the molten container 2, which melts the outer layer 216' to extract the container 21 or oil. The coolant of the outer layer 216 of the melting container of the clothes 7 may be provided in the water device 22, and the heat storage operation is performed on the melting device, and the type of the melting heating device μ is not limited. The peak yak electric heater is taken as an example of 'other equivalent heating device, and the fused mixture of the high-purity metal powder and the metal halide salt is supplied through the inlet port 211 without departing from the invention. Aged mixture. The slewing container discharge control valve 23 is coupled to the output port 14' at the bottom end of the smelting container 21 to control the output control of the mixture formed by the smelting heating device 22 to reduce the thickness of the solid mixture. The liquid phase separation device 30 of the Bayi liquid is connected to the heating and melting reactor 20, and the type of the liquid phase two device 30 is not limited. In the present invention, the separation 1 using gravity separation is taken as an example. Different types, only the functions of which are described herein, can be replaced by an equivalent multi-separator type separator for enhanced liquid-liquid separation. The liquid phase separation device 3 further comprises at least one liquid phase separation container 3, a liquid liquid, a knife-off state heating device 32, a metal halide salt discharge control valve 33, and a liquid-liquid phase separation grain discharge control valve 34. 'The liquid phase separation container 31 may be made of graphite or carbon carbide material or may be formed of other high temperature resistant material lining. The liquid phase separation container 31 is provided with a feed port 311, the inlet port The melted grain discharge control valve 23 of the heating and melting reactor 2 is coupled to the solid mixture 200 to melt the formed 7 201043707 mixture. 312 3_ is provided with at least a metal halide salt liquid outlet from the pure (10) port 313, a hetero-liquid phase separation vessel discharge Ο 出口 outlet 312 and (4); a lower end of the wheel outlet 312 'to make the metal halide salt liquid feeder 31 The school rents the il*s container discharge port 313 to provide the input liquid phase separation ί discharge, the mouth of the eight-year-old metal halide salt and the preliminary purification of the metal liquid 210 points (four) M, Λ, Μ 31 external and coated - The liquid-liquid phase separation container is absolutely: 埶 is ^π/: the liquid-liquid phase separation container 31 is heat-dissipated, and the liquid-liquid phase separation container is divided into... A layer of liquid phase separation vessel is further coated to cool the outer layer 315 to provide 31, and _ cold, and the coolant of the outer layer 315 may be water or oil. The liquid-liquid phase separation container heating device 32 is disposed in the liquid-liquid phase separation container 31 to improve the initial purification of the golden green training and the metal Nanhua salt for the purpose of the separation of the liquid phase separation container. The melt mixed mixed surface is poured, and the material is separated from the liquid surface of the molten metal 21 ,, so that the metal salt solution is discharged corresponding to the gold salt solution outlet 312, and the preliminary purified metal liquid 210 corresponds to the liquid liquid. The phase separation vessel discharge port 313 is rotated, and the liquid phase separation vessel heating device 32 is not limited in type. In the present invention, an electric heater is taken as an example. The metal toothed salt discharge control valve 33 and the liquid phase separation container discharge control valve 34 are respectively connected to the metal halide salt liquid wheel outlet 312 of the liquid phase separation container 31, at least - the liquid phase separation container discharge π 313 phase Linking to provide the metal clearing liquid discharge and the initial, purified metal liquid 210 output. The ι-liquid gas separation device 40' is connected to the liquid phase separation device 3, and the liquid phase separation device 40 further includes a liquid vapor separation vessel 41, a liquid-vapor separation vessel heating device 42, a cooler 43, and a reduced pressure. The device 44 and the liquid-vapor separation container discharge control device, wherein the liquid vapor separation container 41 can be made of graphite or tantalum carbide or by using a high-temperature resistant material liner, and the liquid vapor separation container 41 is provided at the top end. _入^=411, the feed port 411 is connected with the liquid-liquid phase separation container discharge 8 of the liquid-liquid separation device 30, 201043707, port 313, to input the liquid liquid separation device 3, the preliminary purification of the molten metal 2ι The liquid is separated into the inside of the liquid phase separation vessel 41. The liquid vapor phase separation vessel 41 is provided at the top end and is provided with at least one metal halide salt gas discharge port 412 for discharging the metal halide salt gas from the metal halide salt gas discharge port 412. The bottom portion of the liquid vapor phase separation container 41 is provided with at least one The liquid phase separation container discharge port 413' is provided to provide the final purified rain purity liquid phase metal output to the liquid vapor separation container 41 - externally and coated with a liquid phase separation container insulation layer 4 Μ to prevent the liquid phase separation container 41 heat loss, the liquid gas phase separation vessel insulation layer 414 is further coated with a layer of ruthenium liquid gas phase separation vessel to cool the outer layer to provide the liquid gas phase separation vessel Μ externally from the vessel insulation layer 414 for cooling and cooling. The liquid phase separation vessel heating device 42 is disposed inside the liquid-vapor separation container 41 to provide a liquid-gas two-phase separation heating operation for providing the liquid-gas two-phase separation heating operation inside the liquid vapor separation container. The metal halide salt in the initially purified metal liquid 210 is discharged to the metal toothed salt gas discharge port 412 at the top of the liquid vapor phase separation container by the metal halide body, and the purified high-purity metal liquid can be discharged. The liquid phase separation container (4) is outputted from the liquid port 413, and the liquid gas phase separation container is provided with a device 42. The crane is not limited. In the present invention, an electric heater is taken as an example. The cooler 43 is connected to the metal halide salt gas discharge port to cool the metal-salted salt gas outputted from the gold strike-out port 412, and the pressure-reducing device L 1143' is further reduced by the metal salt gas. Pressure, the decompression boot 'is similar to the sample on the date of the present invention. 'Other equivalents are arranged: metal ί: the fan of the invention'. The gold salt gas is controlled under reduced pressure and the material is controlled. The valve 45 is connected to the liquid-phase separation container to discharge the read gas phase (4) control 45 open, _j, and the high-purity molten metal 2H) after the 41 (10) is output. The first embodiment of the second dispensing port is not the first embodiment of the present invention, and the steps include: forming a high-purity gold threat and metal salt reduction with the knife (3〇〇), mixing and adding 9 201043707 Purifying the metal powder and the metal halide salt into the mixed feeder 10 to form a solid mixture 200 of the high-purity metal powder and the self-chemical metal salt; (310) evacuating and removing the impurity gas and the water gas' A solid mixture 200 of the purity metal powder and the self-chemical metal salt is introduced into the heating and melting reactor 20 via the mixing feeder 1 and heated to 100-100 Torr. (:, and repeatedly vacuuming to less than 5 Par ' and filling the inert gas into the heating melt reactor 2〇 to remove the impure gas and water gas in the heating and melting reactor 20; (320) heating and melting 'continuous use of heating Melt reactor 2 加热 heating the metal powder of step 31 () and the metal salt mixture to melt to form a mixed liquid output; 〇 (330) metal is separated from the metal halide salt liquid phase, and the mixture of step 320 is input into the liquid liquid. The phase separation device 30' preliminarily separates the metal from the metal halide salt by the liquid phase separation device 30 to form a mixed solution of a high concentration metal and a small amount of a halogenated salt; (340) Gas phase separation of the metal and the metal halide salt solution. The high concentration metal and a small amount of the halogenated salt mixture are introduced into the gas phase separator 40, and then the gas-liquid separation and purification operation by the reduced pressure heating is performed to volatilize the gaseous salt of the southern salt and the impurity to form a high purity purified liquid phase. (350) Extraction of high-purity metal 'The 6N-grade high-purity liquid phase metal is extracted from the bottom of the liquid phase separator 4 of step 35. 〇Please refer to the third figure as the life of the invention. A second embodiment of the method of high purity metal, wherein a purification embodiment for use in a semiconductor crucible is shown, the step comprising: (400) reacting a high purity metal with an alkali gold metal to obtain a high purity metal powder and a toothing a solid mixture of metal salts, such as an alkali metal group of liquid sodium, and a halogenated compound such as a silicon tetrafluoride (SiF4) gas, which is reacted in a feed feeder 11 of a mixed feeder to produce a high-purity stone. The solid mixture of the metal salt powder of the sulphate and the sulphate is 200', and its reaction formula is siF4(g) + 4Na(lBu(s) + 4NaF(s), or 'solid sulphur hexahydrate (s〇dium fluorosiiieate, Na2SiF6) is reacted with the alkali metal of liquid sodium in the feed vessel U of the mixing feeder 10 to produce a solid mixture of high purity cerium and sodium fluoride southing metal salt powder, which is reversed. 201043707 The formula is Na2SiF0(s)+4Na (1SiSi(s)+6NaF(s), and the solid state of sodium hexafluoroantimonate is not limited, such as a ruthenium compound with ruthenium tetrafluoride gas and The reaction of solid sodium fluoride gives 'the reaction formula is SiF4(g) + 2 NaF(s) - Na2SiF6(s) 〇(410) Vacuum and remove the impure gas and moisture, and the solid mixture 200 of the high-purity cerium powder and the metal halide salt of step 4 is fed into the heating and melting reactor 20 via the mixing feeder 1 and heated to Celsius loo-9. 〇〇°c, and repeatedly vacuuming to less than 5 Par, and then filling the inert gas of argon gas into the heating and melting reactor 2〇 to repeatedly carry out the purification gas, water vapor and volatile impurities; (420) heating and melting 'Continuously use the heating and melting reactor 2〇 to heat the solid mixture 200 of step 41〇, and continue to heat up until both mixtures are liquefied, taking sodium fluoride and cesium as an example, the heating temperature can be 1400-155 degrees Celsius (TC, temperature rise rate Can take 5-15 ° C / min. (degrees / minute) until molten into a mixture output; (430) metal and metal toothed salt liquid phase separation, step 42 〇 sodium fluoride and strontium melt mixture The molten liquid container discharge control opening 23 is turned into the liquid phase separation container 31 of the liquid phase separation device 30, and the liquid phase separation device 3 is used to initially separate the stone and the sodium fluoride to form a high concentration 矽. Mix with a small amount of sodium fluoride The liquid 'the self-chemical salt and the liquid impurity can be controlled to be discharged through the metal self-salt salt discharge control 33; (440) the metal and the metal toothed salt liquid gas phase separation 'the high concentration of the high concentration of the step 430 sputum and a small amount The sodium fluoride mixed liquid is introduced into the liquid vapor phase separation vessel 41 of the gas phase separator 40 by the liquid phase separation container discharge control valve 34, and the liquid vapor phase separation vessel 41 is combined with the liquid vapor phase separation vessel heating device. 42, using a reduced-pressure heating method, so that a liquid substance such as a low boiling point of sodium fluoride is first volatilized and separated, and the effect of purifying the sputum liquid to separate the impurity is achieved, and the cooler 43 and the pressure reducing device 44 can avoid the high-temperature steam of the sodium fluoride directly. discharge. (45〇) extracting high-purity metal, and the liquid-gas phase separation container discharge control valve 45 at the bottom of the liquid phase separator 4 of step 450 is opened and controlled to obtain a 6N-class high-purity

II 201043707 Liquid, which can be directly supplied to the use of long crystal or directional solidification or solar industry polycrystalline raw materials. The solid mixture 200 in the above step 400 can be mixed with a high-purity alkali metal or alkaline earth-like tooth powder by using a semiconductor-grade niobium powder having a particle diameter of less than 1 mm to form a reactant composition, and the purification step of the above steps 400 to 450 can be used. The tantalum powder particles having a particle size of less than 丨 mm are completely recovered and purified. Hereinafter, a number of operation examples will be further enumerated to further explain the operating conditions and technical connotations of the present invention, wherein: (Operation Example 1) 半导体 Add semiconductor grade Shishi powder and sodium fluoride powder in a ratio of 1:1-1:4. The melt reactor 20 is heated, evacuated to below 1 〇Par, filled with argon to } bar, and liquid-liquid separation device 30 is heated to 1400-16 Torr. (:, the liquid-gas phase separation device is heated to a temperature of 1450 - 160 ° C (TC, the decompression device 44 produces 1 - lOOKpa vacuum. (Operation 2) 矽 and sodium fluoride powder produced by the reaction of cesium fluoride with sodium, The solid mixture 200 in which the hydrazine is mixed with the sodium fluoride powder is added to the heating and melting reactor 20, and the remaining separation and purification procedures and conditions are the same as in the operation example 1. The high-purity mash products purified by the two operation examples are ICP 〇MaM^UCTIVELY COUPLED PLASMA-MASS, inductively coupled plasma mass spectrometry), the results are as follows: Item \ Operation Example 1 (ppb) Example 2 (ppb) Li7 <1 <1 Na23 9.468 74.216 Mg24 1.322 4.812 A127 2.502 6.986 Ga71 <1 <1 Ini 15 <1 <1 Bal38 <1 <1 12 201043707

From the above analysis, it is found that the product obtained by the purification of the device and method of the present invention has the same purity as that of the 6N-grade high-purity Shixi product X which can be used in the industrial grade. The invention discloses a device and a method for producing high-purity metal, and the invention is a method for producing a high-purity metal, which is a disclosure of a hybrid embodiment of the present invention, which is not a secret (this). The technical features and methods of the invention are subject to modification and equivalent modifications without departing from the spirit and scope of the invention. The definition of these ranges will be defined by the scope of the patent application. BRIEF DESCRIPTION OF THE DRAWINGS The first figure is a schematic view of the structure of a device for producing high-purity metal according to the present invention; 13 201043707

The second figure is a flow chart of the second embodiment of the method of the first embodiment of the method for producing high purity metal of the present invention. The third figure shows the production of high purity metal according to the invention.

Ο 100 11 20 211 213 215 22 30 311 313 315 33 40 411 413 415 43 45 300 [Main component symbol description] Device feed container heating melt reactor inlet inlet inert gas inlet melting vessel insulation layer melting heating device liquid phase Separation device inlet liquid liquid phase separation container discharge port liquid phase separation container cooling outer layer metal toothed salt discharge control valve liquid gas separation device inlet port liquid phase separation container discharge port liquid phase separation container cooling outer layer Coolant liquid vapor phase separation vessel discharge control valve forms a solid mixture of high purity metal powder bundle and nanochemical metal salt 10 Mixing feeder 12 Feed control valve 21 Melting vessel 212 Vacuum suction port 214 Output port 216 layer melting vessel cooling Outer layer 23 smelting vessel discharge control valve 31 liquid phase separation vessel 312 metal halide salt liquid wheel outlet 314 liquid phase separation vessel insulation layer 32 liquid phase separation vessel heating device 34 liquid phase separation vessel discharge control valve 41 liquid Gas phase separation vessel 412 metal halide salt gas discharge port 414 liquid gas phase separation vessel heat insulation layer 42 liquid gas phase separation vessel heating device 44 Pressing device 200 solid mixture 310 vacuuming and removing impure gas and water gas 320 340 400 metal and metal toothed salt liquid liquid phase separation extracting high purity metal vacuuming and removing impure gas and water gas heating melting 33 () metal and metal halogenation Gas phase separation of salt solution 35 〇 high-purity functionalized metal and gold-receiving metal anti-410 should obtain high-purity metal powder and _ metal salt solid mixture 201043707 420 heated smelting 430 metal and metal toothed salt liquid phase separation 440 Metal and Metal Deuterated Salt Liquid Phase Separation 450 Extraction of High Purity Metal 210 Metal Liquid ❹ 〇15

Claims (1)

201043707 VII. Patent application scope: 1 'A device for producing high-purity metal, comprising: a mixing feeder for supplying a high-purity metal powder and a toothed metal salt feed to form a solid mixture; a heating and smelting reactor, Connecting the mixed feeder, placing the solid high-purity metal powder of the mixed feeder and the toothed metal salt mixture in the reactor, and removing the impurity gas in the reactor cabin by repeatedly pumping and filling the inert gas And the water gas 'and use a heater to heat the mixture to melt; a liquid phase liquid separation device, which is connected to the heating and melting reactor, and the metal in the molten molten liquid in the hot melt reactor and the metal toothed salt are subjected to two phases. Preliminary purification and separation, so that impurities are discharged with the metal self-chemical salt solution to obtain a mixture of a high concentration of metal and a small amount of a halogenated salt; and a liquid phase gas separation device, which is connected to a liquid phase separation device to separate the liquid phase a preliminary mixture of a high concentration of metal and a small amount of a mixture of toothed salts, using gas-liquid separation under reduced pressure to make halogenated salts and impurities Volatile molten metal, to accelerate the separation to obtain a two-phase interfacial mixing 6N grade high purity metal. 2. The apparatus for producing high purity metal according to claim 1, wherein the solid mixture in the mixing feeder is obtained from a high purity deuterated metal and a gold metal. 3. The apparatus for producing high-purity metal according to claim 2, wherein the high-purity metal halide and the alkali metal group are high-purity antimony tetrafluoride and sodium. 4. The apparatus for producing high purity metal according to the scope of the invention, wherein the solid mixture in the mixing feeder is obtained by reacting a high purity deuterated metal with a soil of a soil test group. 5. The apparatus for producing high-purity metal according to claim 1, wherein the high-purity powder is ruthenium. / 6. The apparatus for producing high-purity metal according to claim 1, wherein the mixed feeder comprises: 'at least one feed container' for mixing high-purity metal powder with a toothed metal salt feed In 16 201043707 solid mixture; and - feed control, linked below the feed container, J ^ from the output of the solid mixture in the feed container. He paste control 7. The heating for producing high-purity metal as described in claim 1, the melt reactor comprises: /, a dry '-melting vessel, a joint mixing contact, and (10) a high-purity metal powder. a solid mixture is input, and a bottom of the melting vessel is provided with a round of outlets; a molten wire is disposed on the miscellaneous rib, and the squeaking operation 'slow-heating device provides a solid mixture of the high-purity gold halide metal salt in the input molten vessel to be heated and smelted into a mixed liquid; /, - the molten container is discharged The material control side 'connects to the bottom of the smelting vessel to control the output of the mixture formed by the heating and solid mixture of the molten heating device = 8. The production is high as described in claim 7 A device for purifying metal, wherein a top of the molten container is provided with a feed port that connects the mixed feeder. 9. If you apply for a high-purity metal device in the form of a special item (4), the top of the device is provided with a vacuum evacuation port. The vacuum pumping port provides a vacuuming operation inside the refining vessel. 10. The apparatus for producing high-purity metal according to claim 7, wherein the top of the melting vessel is provided with an inert gas inlet for inputting an inert gas. The apparatus for producing high-purity metal according to the first aspect of the invention, wherein the inert gas input to the heating and melting reactor is argon. /, 12. For the apparatus for producing high-purity metal according to item 7 of the patent application, the inert gas of the pot into the smelting vessel is argon. VIII. 13. For the production of high-purity metal equipment as described in item 7 of the patent scope, in which 1 the Rongrong Rongke Department is coated with a layer of molten Rongwei heat layer to prevent the Rongrong Rong from dissipating heat. The apparatus for producing high-purity metal according to the thirteenth aspect of the invention, wherein: 17 201043707 the outer covering layer of the molten container insulation layer-layer melting container 15. The sorghum production of the sorghum container as described in claim 14 The coolant of the outer layer is water. The apparatus of X, wherein the application of the high-purity coolant of the molten container described in the item 14 of the scope is oil. In the eighth device, 17. The high-purity production device described in claim 7 is an electric heater. The apparatus, wherein, the production of the high purity as described in the patent application, the liquid phase separation apparatus comprises: , a device, wherein, the liquid liquid is separated from the container, and the liquid liquid phase separation container is at the top of the liquid Twisting and melting anti-depot connection "to form a mixture of the solid mixture to form a genus Nan servant, Shizhaoshan | I Shaozhan this liquid, side and at least the phase separation container outlet is located in the metal toothing The lower end of the salt liquid outlet is: U == liquid phase separation container outlet port provides input liquid respectively = device · such as σ liquid metal halide salt liquid and the first her metal liquid separation and discharge; ο U phase silk green Adding the recording, the phase of the ribs of the cake phase, the preliminary purification of the metal liquid and the gold (4) test of the mixture of the liquid mixture and the gold (4) test, two phases of the two = heating operation 'to make the liquid phase separation of the fine mixture of the message After the operation, the metal halide salt solution is separated from the liquid surface of the molten metal; and... the metal self-reserving side and the phase separation are separated (4) the control side, respectively, and the metal toothed salt of the liquid phase separation container The liquid outlet and the liquid phase separation container outlet are connected to provide separately The metal is discharged from the salt liquid and the preliminary purification of the metal liquid wheel. 19. The device for producing high-purity metal according to claim 18 of the patent application, wherein the liquid liquid phase separation container is provided with a human mouth, the person material Oral connection plus recording and thawing reaction 20. The device for producing high-purity metal according to claim 18 of the patent scope, the liquid-liquid phase separation container is coated with a liquid-liquid phase separation container, and the heat of the liquid phase separation container is lost. . The apparatus for producing high-purity metal according to claim 20, wherein the liquid-phase separation container insulation layer is externally coated with a liquid-liquid phase separation container to cool the outer layer. 22. The apparatus for producing high-purity metal according to claim 21, wherein the coolant for cooling the outer layer of the liquid phase separation container is water. 23. The apparatus for producing high purity metal according to claim 21, wherein the coolant for cooling the outer layer of the liquid phase separation container is oil. 24. The apparatus for producing high purity metal according to claim 18, wherein the liquid phase separation vessel heating device is an electric heater. 25. The apparatus for producing high-purity metal according to claim 1, wherein the liquid vapor separation apparatus comprises: a liquid-phase gas separation container, and the top end is connected to the liquid-liquid separation device to input the The liquid liquid of the liquid phase separation device is initially purified, and the liquid vapor phase separation container is provided at the top of the container and is provided with at least one metal halide salt gas discharge port for discharging the metal_salt gas, and at least one bottom end of the liquid gas phase separation container is provided. The liquid gas phase separation container discharge port is provided to provide a final purified high purity liquid phase metal output; a liquid phase gas separation barn heating device is disposed inside the liquid phase gas separation container to provide the inside of the liquid phase gas separation container The preliminary purification of the metal liquid is used for the liquid-phase two-phase separation heating operation; 'to make the metal halide salt gas halogenated salt gas decompress and then discharge a cooler' to connect the metallized salt gas discharge port body discharge port output The metal_salt gas is cooled; a decompression device is connected to the cooler to regenerate the metal toothed salt; and the liquid is disordered from the control side, and the connection is exhausted. Vapor liquid separation vessel discharge control valve Pirates Tu port in the high purity metal in the vessel after the purification Kawasaki out. ^The liquid phase separation of the liquid 26. The high-purity residual gas phase separation vessel described in the scope of claim 2S is provided with a "manual port 19 201043707 device". 27. The apparatus for producing high-purity metal according to claim 25, wherein the liquid vapor phase separation vessel is externally coated with a heat insulating layer of the liquid phase gas separation container to prevent heat loss of the gas phase separation vessel. 28. The apparatus for producing high-purity metal according to claim 25, wherein the liquid phase separation container insulation layer is externally coated with a liquid vapor phase separation container to cool the outer layer. 29. The apparatus for producing a high-purity metal according to claim 28, wherein the coolant for cooling the outer layer of the liquid phase separation container is water. 30. The apparatus for producing high-purity metal according to claim 28, wherein the coolant of the liquid-phase phase separation trough cooling outer layer is oil. 31. The apparatus for producing high-purity metal according to claim 25, wherein the liquid phase separation vessel heating device is an electric heater. The device for producing high-purity metal according to claim 25, wherein the pressure reducing device is a vacuuming device. 33. A method for producing high purity metal, the steps comprising: (A) forming a solid mixture of a high purity metal powder and a toothed metal salt, mixing and adding a high purity metal powder and a metal toothed salt to a mixed feeder Forming a solid mixture of a high-purity metal powder and a metal halide; (B) evacuating and removing the impure gas and moisture, and placing a solid mixture of the human high-purity metal powder and the metal halide salt through the mixed feeder a heating and melting reactor, heated by the heating and melting reactor, and repeatedly vacuumed, and then filled with an inert gas to the heating and melting reactor to remove the impure gas and water gas in the heating and melting reactor; (C) heating Melting 'continuously using a heated melt reactor to heat the metal powder of step b and the metal halide salt mixture to melt to a mixed liquid output; (D) metal and metal are separated from the liquid phase by a salt liquid, and the mixture of step c is input into a liquid a liquid phase separation device for separating a metal from a metal halide salt by the liquid phase separation device 20 201043707 forming a high concentration metal and a small amount of toothing (E) metal-metallized salt liquid gas phase separation, the high concentration of the metal of step D and a small amount of halogenated salt mixture is introduced into a gas-liquid phase separation device, and then separated and purified by gas-liquid separation under reduced pressure. Action, the i-salt and impurities are volatilized and discharged to form a high-purity purified liquid phase metal; and (F) extracting a high-purity metal' is extracted from the bottom of the liquid phase separator of step E to obtain a 6N-grade 13⁄4 purity liquid phase. metal. 34. The method for producing a high-purity metal according to claim 33, wherein the high purity metal powder and the metal halide salt of the step A are hair and sodium fluoride. 35. The method for producing high-purity metal according to claim 33, wherein the heating and melting reactor of the step B is heated at a temperature of 1 〇〇 - 9 〇〇 ° c 〇 36. The method of producing high purity metal according to item 33, wherein the heating and melting reactor of the step B is repeatedly evacuated to 5 par. 37. The method for producing a two-purity metal according to claim 33, wherein the liquid phase separator of the step E is extracted at the bottom to obtain a 6N-grade high-purity liquid phase metal as a mash. 38. A method for producing high-purity metal's steps comprising: · 〇 (A1) to obtain a solid mixture of a high-purity metal powder and a toothed metal salt by reacting a high-purity metal halide with an alkali metal group, to a purity of 豳The metal reacts with the metallurgical group metal to form a solid mixture of the high-purity metal powder and the self-chemical metal salt, and is added to a mixed feeder; σ (Β1) is vacuumed and the impure gas and water gas are removed. a solid mixture of the powder and the toothed metal salt is fed into a heated melt reactor via a mixing feeder and heated by the heated melt reactor and vacuumed repeatedly, and then filled with an inert gas to the heated melt reactor to remove Heating the impure gas and water gas in the melt reactor; (C1) heating and melting, continuously heating the metal powder of the step with the metal 21 201043707 halogenated salt mixture to melt into a mixed liquid output by using a heating melt reactor; (D1) metal and metal The liquid phase separation of the salt liquid is carried out, and the mixed liquid of the step C1 is input into a liquid phase liquid separation device, and the liquid and metal teeth are separated by the liquid phase separation device. The salt is initially separated to form a mixture of a high concentration metal and a small amount of a halogenated salt; (E1) the metal is separated from the metal toothed salt liquid by gas phase, and the high concentration metal of step D1 and a small amount of the toothed salt mixture are introduced into a gas phase separation. The device uses the gas-liquid separation and purification operation of the reduced pressure heating to volatilize the halogenated salt and the impurity to form a high-purity purified liquid phase metal; and O (F1) extracts the high-purity metal, and is separated from the liquid phase of the step E1. A 6N grade high purity liquid phase metal is obtained by extracting the bottom of the apparatus. 39. The method of producing a high-purity metal according to claim 38, wherein the high-purity metal of the step A1 and the metal of the gold-receiving group are tetrafluoride. 40. The method for producing a high-purity metal according to claim 38, wherein the high-purity metal halide and the alkali metal group in the step A1 are sodium and sodium hexafluoroantimonate. The method for producing a high-purity metal according to claim 40, wherein the sodium hexafluoroantimonate is composed of ruthenium tetrafluoride and sodium fluoride. 42. The method for producing a high-purity metal according to claim 38, wherein the heating and melting reactor of the step B1 is heated at a temperature of 1 to 9 Torr. Hey. 43. The method of producing high purity metal according to claim 38, wherein the heating and melting reactor of step B1 is repeatedly evacuated to 5Par. 44. The method for producing a high-purity metal according to claim 38, wherein the liquid phase separator of the step E1 is bottom-extracted to obtain a 61-grade high-purity liquid phase metal as a mash. 45. A method for producing a high-purity metal, the steps comprising: (A2) reacting a high-purity functionalized metal with an alkaline earth metal to obtain a solid mixture of a high-purity metal powder and a metal halide, and drawing the metal with high purity The alkaline earth metal reacts to form a solid mixture of the high-purity metal powder and the toothed metal salt, and is added to a mixed 22 201043707 feeder; (B2) vacuuming and removing the impurity gas and moisture, and the high-purity metal powder of step A2 is a solid mixture of a halogenated metal salt is fed into a heated melt reactor via a mixing feeder, heated by the heated melt reactor, and vacuumed repeatedly, and then filled with an inert gas to the heated melt reactor to remove the heat. Impure gas and water gas in the melt reactor; (C2) heating and melting 'continuous use of heating, the melt reactor heats the metal powder of step B2 and the metal halide salt mixture to melt into a mixture liquid; 〇(D2) metal and Liquid phase separation of the metal toothed salt liquid, the liquid of the step 匚2 is input into a liquid phase separation device, and the liquid phase separation device is used to transfer the metal to the gold The halogenated salt is initially separated to form a mixture of a high concentration metal and a small amount of the toothed salt; (E2) the metal is separated from the metal self-chemical salt liquid, and the high concentration metal and a small amount of the halogenated salt mixture are introduced into the gas phase. Separating device, using gas-liquid separation and purification operation under reduced pressure, volatilizing halogenated salt and impurities to form high-purity purified liquid metal; and (F2) extracting high-purity metal, separating from liquid phase in step E2 The bottom of the apparatus is extracted to obtain a g 6N grade high purity liquid phase metal. 46. The method for producing a high-purity metal according to claim 45, wherein the heating and melting reactor of the step B2 is heated at a temperature of 100 to 900 ° C. 47. The method of producing high purity metal according to claim 45, wherein the heating and melting reactor of step B2 is repeatedly evacuated to 5 Par. 48. The method for producing a high-purity metal according to claim 45, wherein the liquid phase separator of the step E2 is extracted at the bottom to obtain a 6N-grade high-purity liquid phase metal as a mash. twenty three