WO2019235098A1 - 金属チタン製造装置及び方法 - Google Patents
金属チタン製造装置及び方法 Download PDFInfo
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- WO2019235098A1 WO2019235098A1 PCT/JP2019/017638 JP2019017638W WO2019235098A1 WO 2019235098 A1 WO2019235098 A1 WO 2019235098A1 JP 2019017638 W JP2019017638 W JP 2019017638W WO 2019235098 A1 WO2019235098 A1 WO 2019235098A1
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- precipitate
- bismuth
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1277—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using other metals, e.g. Al, Si, Mn
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1295—Refining, melting, remelting, working up of titanium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the present disclosure relates to a titanium metal manufacturing apparatus and method. This application claims priority based on Japanese Patent Application No. 2018-108973 for which it applied to Japan on June 6, 2018, and uses the content here.
- Patent Document 1 listed below discloses a titanium production method that can efficiently obtain a titanium alloy, and that can be produced (smelted) at low cost continuously by refining the titanium alloy at a low cost. ing.
- this production method by adding titanium tetrachloride (TiCl 4 ) to a mixture containing bismuth and magnesium to obtain a liquid alloy of bismuth and titanium, the liquid alloy is subjected to distillation treatment.
- Step 2 distillation step for removing components other than titanium as a basic step, a liquid part is segregated between Step 1 and Step 2, and a solid-liquid coexistence portion in which solid and liquid coexist
- separates into is included as an auxiliary process.
- distillation process since it is necessary to input a lot of energy, in order to further reduce the manufacturing cost (smelting cost) of metal titanium, the processing efficiency (distillation) of the distillation process (distillation process) Efficiency) needs to be improved.
- the present disclosure has been made in view of the above-described circumstances, and aims to improve the processing efficiency (distillation efficiency) in the distillation process as compared with the related art.
- a titanium metal production apparatus reduces a titanium-chloride liquid alloy by reducing titanium tetrachloride in the presence of bismuth and magnesium.
- the atmosphere is set so as to evaporate the bismuth preferentially, and then the atmosphere is set so as to evaporate the bismuth forming the precipitate.
- the titanium metal production apparatus further includes a concentrating device that obtains a concentrated intermetallic compound by separating the bismuth incidental to the precipitate from the precipitate, and the distillation device includes:
- the concentrated intermetallic compound may be distilled instead of the precipitate.
- the distillation apparatus has a temperature at or near 800 ° C. as the atmosphere for preferentially evaporating the bismuth incidental to the precipitate. You may set so that.
- the distillation apparatus is configured such that the precipitate has a temperature of 1000 ° C. or a vicinity thereof as an atmosphere for evaporating the bismuth forming the precipitate. May be set.
- the distillation apparatus is configured such that the precipitate has a temperature of 1100 ° C. or a vicinity thereof as an atmosphere for evaporating the bismuth forming the precipitate. May be set.
- the distillation apparatus has a temperature at or near 1000 ° C. as an atmosphere for evaporating the bismuth forming the precipitate. Then, the precipitate may be set to 1100 ° C. or a temperature in the vicinity thereof.
- the distillation apparatus can maintain the structure of titanium contained in the precipitate obtained by the segregation apparatus and is directed from the inside of the precipitate toward the surface thereof.
- the precipitate is heated at a first temperature such that bismuth diffuses from the surface by bismuth diffusion, and then the precipitate is heated at a second temperature higher than the first temperature. May be heated.
- the titanium metal production method includes a reduction step of obtaining a liquid alloy comprising titanium and the bismuth by reducing titanium tetrachloride in the presence of bismuth and magnesium, A segregation step of obtaining a precipitate by subjecting a liquid alloy to segregation; and a distillation step of obtaining a titanium metal by subjecting the precipitate to a distillation treatment.
- priority is given to the bismuth incidental to the precipitate.
- the atmosphere around the precipitate is set so as to evaporate, and then the atmosphere is set so as to evaporate the bismuth forming the precipitate.
- the structure of titanium contained in the precipitate obtained in the segregation step can be maintained, and the inside of the precipitate is directed to the surface thereof.
- the precipitate is heated at a first temperature such that bismuth diffuses from the surface by bismuth diffusion, and then the precipitate is heated at a second temperature higher than the first temperature. May be heated.
- distillation efficiency distillation efficiency
- FIG. 1 is a system configuration diagram of a titanium metal manufacturing apparatus according to an embodiment of the present disclosure. It is a flowchart which shows operation
- the titanium metal production apparatus includes a reduction furnace 1, a Bi supply apparatus 2, a TiCl 4 supply apparatus 3, an Mg supply apparatus 4, an MgCl 2 recovery apparatus 5, a segregation apparatus 6, and a concentration apparatus 7. , A distillation device 8 and an exhaust device 9 are provided.
- the reduction furnace 1, the Bi supply device 2, the TiCl 4 supply device 3, the Mg supply device 4, and the MgCl 2 recovery device 5 constitute the reduction device of the present disclosure. That is, the reduction furnace 1, Bi supply device 2, TiCl 4 supply device 3, Mg supply device 4 and MgCl 2 recovery device 5 have an overall function in the presence of bismuth (Bi) X 1 and magnesium (Mg) X 3.
- the reduction furnace 1 reduces the titanium tetrachloride in the presence of bismuth X1 and magnesium X3 at a temperature (reduction temperature) higher than any melting point of bismuth X1 and magnesium X3.
- This is a heating furnace for producing magnesium chloride (MgCl 2 ) X5.
- the reduction temperature is 900 ° C., for example. This reduction temperature may be adjusted as appropriate.
- the liquid state Bi-Ti liquid alloy X4 and the liquid are obtained by adding the liquid state titanium tetrachloride X2 to the liquid state bismuth X1 and magnesium X3.
- the state of magnesium chloride X5 is produced.
- Such reduction reactor 1, a Bi-Ti liquid alloy X4 is one of the products supplied to the segregated unit 6, and supplies the magnesium chloride X5 is the other product MgCl 2 recovery device 5.
- the Bi supply device 2 is a bismuth supply source that supplies the reduction furnace 1 with bismuth X1, which is one of the raw materials for the reduction treatment.
- the TiCl 4 supply device 3 is a titanium tetrachloride supply source that supplies titanium tetrachloride X2 that is one of the raw materials for the reduction treatment to the reduction furnace 1.
- the Mg supply device 4 is a magnesium supply source that supplies magnesium X3, which is one of the raw materials for the reduction treatment, to the reduction furnace 1.
- the MgCl 2 recovery device 5 is a device that recovers magnesium chloride X5 that is one of the products from the reduction furnace 1.
- the segregation apparatus 6 is an apparatus that obtains a solid-liquid mixture by subjecting the Bi—Ti liquid alloy X4 to segregation. That is, the segregation apparatus 6 maintains the Bi-Ti liquid alloy X4 at a predetermined segregation temperature, for example, 500 ° C., thereby providing a Bi—Ti liquid alloy (Ti 8 Bi) having a higher titanium concentration than the Bi—Ti liquid alloy X4. 9 liquid alloy) is selectively precipitated to form a solid-liquid mixture composed of Ti 8 Bi 9 intermetallic compound (solid phase, precipitate) and bismuth alloy X7 (liquid phase) having a high bismuth concentration.
- a predetermined segregation temperature for example, 500 ° C.
- 9 liquid alloy is selectively precipitated to form a solid-liquid mixture composed of Ti 8 Bi 9 intermetallic compound (solid phase, precipitate) and bismuth alloy X7 (liquid phase) having a high bismuth concentration.
- the segregation device 6 provides the concentration device 7 with a mixture X6 containing a relatively large amount of Ti 8 Bi 9 among the solid-liquid mixture, and provides the bismuth alloy X7 with the reduction furnace 1.
- bismuth solid or liquid
- Ti 8 Bi 9 crystals solid
- the concentration device 7 is a device that obtains the concentrated intermetallic compound X9 by separating bismuth incidental to the mixture X6 from the mixture X6.
- the concentrating device 7 includes at least a concentrating furnace 7a, an Ar gas supply device 7b, and a drive source 7c.
- the concentrating furnace 7a is a bottomed cylindrical container that contains the mixture X6 and holds it in a predetermined atmosphere, and is installed in such a posture that its axis is in the vertical direction.
- Such a concentration furnace 7a includes a perforated drum for accommodating the mixture X6, a receiving container for accommodating the perforated drum, a heater provided in the receiving container, a heat insulating member, and the like.
- the perforated drum included in the concentrating furnace 7a can be rotated by a driving source 7c.
- the Ar gas supply device 7b is a device that supplies Ar gas X8 to the concentration furnace 7a.
- the Ar gas supply device 7b supplies the Ar gas X8 to the concentration furnace 7a
- the inside of the concentration furnace 7a becomes an Ar gas atmosphere (inert gas atmosphere).
- the drive source 7c is a rotational power source for rotating the mixture X6 in the concentration furnace 7a. That is, this drive source 7c rotates the mixture X6 accommodated in the perforated drum by rotationally driving the perforated drum accommodated in the concentration furnace 7a.
- the concentrating device 7 configured in this manner applies centrifugal force to the mixture X6 by rotating the perforated drum while heating the mixture X6 accommodated in the perforated drum by the heater in an Ar gas atmosphere.
- a concentrator 7 functions as a kind of centrifugal separator, and separates liquid-phase bismuth and solid-phase Ti 8 Bi 9 crystals into solid-liquid by applying centrifugal force to the mixture X6.
- the concentration device 7 removes most of the liquid phase bismuth from the mixture X6 by such centrifugation, and obtains an alloy having a higher titanium concentration than the mixture X6, that is, the concentrated intermetallic compound X9, and supplies it to the distillation device 8. Supply.
- the centrifugal force is a kind of inertial force as is well known.
- the distillation apparatus 8 is an apparatus that obtains metallic titanium by subjecting the concentrated intermetallic compound X9 to a distillation process, which is a kind of purification process. That is, the distillation apparatus 8 heats the concentrated intermetallic compound X9 to a predetermined distillation temperature in a reduced-pressure atmosphere, thereby selectively vaporizing bismuth forming the concentrated intermetallic compound X9 to obtain titanium metal.
- the distillation temperature is 1000 ° C., for example.
- such a distillation apparatus 8 is a kind of purification apparatus.
- the exhaust device 9 is a vacuum pump that exhausts the internal gas of the distillation device 8 to the outside.
- the exhaust device 9 supplies bismuth X10 obtained by the exhaust process of the exhaust device 9 to the reduction furnace 1.
- the inside of the distillation apparatus 8 becomes a reduced pressure atmosphere by the operation of the exhaust apparatus 9.
- the titanium metal manufacturing apparatus configured as described above is controlled in an integrated manner by the control device 10. That is, the Bi supply device 2, TiCl 4 supply device 3, Mg supply device 4, MgCl 2 recovery device 5, segregation device 6, concentration device 7, distillation device 8, and exhaust device 9 described above are operated by the control device 10. Is appropriately controlled to perform a series of manufacturing processes as described below.
- the titanium metal manufacturing apparatus in the present embodiment includes a control device 10.
- the control device 10 includes a computer, and the computer includes a CPU (Central Processing Unit), a storage device, an input / output device, and the like.
- CPU Central Processing Unit
- the storage device includes one or more of a volatile memory such as a RAM (Random Access Memory), a nonvolatile memory such as a ROM (Read Only Memory), an HDD (Hard Disk Drive), and an SSD (Solid State Drive). .
- the input / output device includes a Bi supply device 2, a TiCl 4 supply device 3, an Mg supply device 4, an MgCl 2 recovery device 5, a segregation device 6, a concentration device 7, a distillation device 8, and an exhaust device 9 in a wired or wireless manner. (Measurement data such as temperature and pressure) is exchanged.
- FIG. 1 shows that the control device 10 is connected to the distillation device 8 only by wire or wirelessly for simplification, the control device 10 is connected to each device.
- the computer can perform a predetermined function based on a program or the like stored in the storage device.
- the control device 10 is provided by a computer provided separately for each of the Bi supply device 2, the TiCl 4 supply device 3, the Mg supply device 4, the MgCl 2 recovery device 5, the segregation device 6, the concentration device 7, the distillation device 8, and the exhaust device 9. May be configured.
- a reduction process (reduction process) is performed by a reduction device (step S1). That is, in the reduction apparatus, the atmospheric temperature of the reduction furnace 1 is set to a predetermined reduction temperature, the Bi supply apparatus 2 supplies bismuth X1 to the reduction furnace 1, and the TiCl 4 supply apparatus 3 supplies titanium tetrachloride X2 to the reduction furnace. 1 and the Mg supply device 4 supplies magnesium X3 to the reduction furnace 1.
- Bi—Ti indicates a Bi—Ti liquid alloy X4 made of titanium and bismuth.
- the supply amount of each raw material supplied to the reduction furnace 1, that is, the supply amount of bismuth X1, titanium tetrachloride X2 and magnesium X3 to the reduction furnace 1 is the mole of each raw material in the reduction reaction represented by the above formula (1). It is set as appropriate based on the ratio.
- the Bi—Ti liquid alloy X4 and the magnesium chloride X5 exist as liquids in the reduction furnace 1, but both are separated into two layers due to the difference in specific gravity. That is, the Bi—Ti liquid alloy X4 has a relatively large specific gravity, and thus becomes a lower layer liquid product in the reduction furnace 1. On the other hand, since magnesium chloride X5 has a relatively small specific gravity, it becomes an upper liquid product in the reduction furnace 1.
- the lower Bi—Ti liquid alloy X4 is taken out from the bottom of the reduction furnace 1 and supplied to the segregation device 6, and the upper magnesium chloride X5 is taken out from the middle part of the reduction furnace 1 and recovered in the MgCl 2 recovery device 5. Is done.
- a segregation process is subsequently performed by the segregation apparatus 6 (step S2). That is, the segregation apparatus 6 performs a segregation process on the Bi—Ti liquid alloy X4.
- the Bi—Ti liquid alloy X4 has a segregation temperature of 500 ° C. and the Ti 8 Bi 9 intermetallic compound when the titanium concentration in the Bi—Ti liquid alloy X4 is 47 at% or less. Precipitates.
- Ti 8 Bi 9 intermetallic compounds are obtained as precipitates, but the present invention is not limited to this, and other Bi—Ti intermetallic compounds (for example, Ti 3 Bi) are obtained.
- the segregation temperature and atomic composition percentage may be adjusted so that 2 ) is obtained as a precipitate.
- This Ti 8 Bi 9 intermetallic compound is a precipitate of the Bi—Ti liquid alloy X4, and is a solid substance whose titanium concentration is higher than that of the Bi—Ti liquid alloy X4. Further, since this Ti 8 Bi 9 intermetallic compound has a lower density than the Bi—Ti liquid alloy X4, it floats in the Bi—Ti liquid alloy X4 and becomes a floating body. That is, in the segregation apparatus 6, the Bi—Ti liquid alloy X 4 is exposed to a predetermined segregation temperature, whereby a solid-liquid mixture (mixture X 6) composed of Ti 8 Bi 9 intermetallic compound (solid phase) and bismuth (liquid phase). Is generated.
- This metal titanium production apparatus subsequently performs a distillation process (distillation process) using the distillation apparatus 8. That is, the distillation apparatus 8 selectively vaporizes bismuth forming the concentrated intermetallic compound X9 by placing the concentrated intermetallic compound X9 under a predetermined distillation temperature and a reduced-pressure atmosphere, thereby obtaining metallic titanium.
- the titanium metal production apparatus first depressurizes the inside of the distillation apparatus 8 as a distillation step (step S3). That is, in the titanium metal production apparatus, the inside of the distillation apparatus 8 in which the concentrated intermetallic compound X9 is stored is placed under a reduced-pressure atmosphere of, for example, 10 Pa or less by the exhaust apparatus 9. You may adjust the pressure in the distillation apparatus 8 suitably.
- a titanium metal manufacturing apparatus raises the temperature inside the distillation apparatus 8 to 800 degreeC or its vicinity (1st temperature) as a distillation process (step S4).
- the internal temperature of the distillation apparatus 8 By raising the internal temperature of the distillation apparatus 8 to 800 ° C. or in the vicinity thereof, the internal temperature of the concentrated intermetallic compound X9 gradually increases, and bismuth incidental to the concentrated intermetallic compound X9 starts to evaporate. That is, the distillation apparatus 8 sets an atmosphere (atmosphere around the precipitate) so as to preferentially evaporate bismuth incidental to the precipitate.
- the bismuth evaporated from the inside of the concentrated intermetallic compound X9 is released as a gas from the surface of the concentrated intermetallic compound X9.
- the distillation apparatus 8 (distillation process) of the present embodiment can maintain the structure of titanium contained in the precipitate (Ti 8 Bi 9 intermetallic compound in the present embodiment) obtained by the segregation apparatus 6 (segregation process).
- the bismuth diffuses from the inside of the precipitate toward the surface thereof, so that the evaporation of bismuth from the surface is maintained (the temperature in the embodiment is 800 ° C. or the vicinity thereof).
- the bismuth content on the surface is appropriately maintained.
- the diffusion of bismuth from the inside of the precipitate toward the surface and the evaporation of bismuth from the surface are appropriately performed. Maintained.
- titanium contained in the precipitate is not melted and the metal structure can be maintained. Therefore, the bismuth is continuously evaporated from the precipitate, so that the precipitate gradually has a large number of holes. It changes into a porous state. Through these holes, diffusion and evaporation of bismuth from the inside of the precipitate can be further promoted.
- the first temperature may be appropriately adjusted according to the pressure in the distillation apparatus 8 and the like.
- a titanium metal manufacturing apparatus raises the temperature inside the distillation apparatus 8 to 1000 degreeC or its vicinity (2nd temperature) as a distillation process (step S5). That is, the distillation apparatus 8 sets the atmosphere so as to evaporate the bismuth forming the precipitate after setting the atmosphere so as to preferentially evaporate bismuth incidental to the precipitate as described above. At this time, since the vapor pressure of bismuth is extremely higher than the vapor pressure of titanium, it is considered that the evaporation of bismuth from Ti 8 Bi 9 in the concentrated intermetallic compound X9 is selectively promoted. For this reason, an increase in the melting point is expected by increasing the titanium concentration of the porous concentrated intermetallic compound X9.
- the structure can be distilled at a higher temperature while maintaining the strength without melting or collapsing.
- the precipitation is performed at a second temperature higher than the first temperature (in this embodiment, 1000 ° C. or a temperature in the vicinity thereof, or 1100 ° C. or a temperature in the vicinity thereof).
- the product is further heated.
- a metal titanium manufacturing apparatus raises the temperature inside the distillation apparatus 8 to 1100 degreeC or its vicinity as a distillation process (step S6). Thereby, the distillation apparatus 8 completely evaporates the bismuth which the concentration intermetallic compound X9 contains, and obtains metallic titanium.
- the bismuth (gas phase) acquired by the exhaust device 9 from the distillation device 8 is supplied to the reduction furnace 1 as shown in FIG.
- bismuth (liquid phase) contained in the solid-liquid mixture of the segregation apparatus 6 is supplied to the reduction furnace 1 as shown in FIG.
- bismuth incidental to the concentrated intermetallic compound X9 is preferentially evaporated to form a porous structure on the surface of the concentrated intermetallic compound X9, and thereafter
- the bismuth contained in Ti 8 Bi 9 is evaporated.
- bismuth evaporated inside can be discharged through the pores of the porous structure, and the processing efficiency (distillation efficiency) in the distillation process can be improved as compared with the conventional case.
- the titanium concentration in each step when the above-described steps S4 to S6 are performed is the temperature condition 1
- the titanium concentration when the distillation at 1100 ° C. is performed three times without performing the step S5 is the temperature condition 2.
- a graph is shown in FIG. In this figure, in the temperature condition 1, the titanium concentration in the finally obtained metal was 97.80%, and in the temperature condition 2, the titanium concentration in the finally obtained metal was 81.76%. That is, by performing step S5 of performing distillation at 1000 ° C., the porous structure can be prevented from collapsing to promote the evaporation of bismuth and the purity of titanium can be increased.
- the titanium metal production apparatus includes the concentration device 7 that concentrates the mixture X6 by solid-liquid separation, but the present disclosure is not limited thereto.
- the titanium metal production apparatus does not include the concentrating device 7, and the mixture X6 may be directly distilled in the distillation device.
- the titanium metal production apparatus includes the segregation apparatus 6 that generates the mixture X6 composed of the Bi 8 Ti 9 intermetallic compound (solid phase) and bismuth (liquid phase) from the Bi—Ti liquid alloy X4.
- the present disclosure is not limited to this.
- the titanium metal production apparatus does not include the segregation apparatus 6, and the Bi—Ti liquid alloy X4 may be directly distilled in the distillation apparatus.
- the concentration device 7 that applies centrifugal force (inertial force) to the mixture X6 is used, but the present disclosure is not limited thereto.
- a dynamic inertia force for example, it is conceivable to stop (stop) the mixture X6 while moving the mixture X6 in a predetermined direction at a predetermined speed.
- a filter using a filter, a vacuum dehydrator, a belt press, or the like may be used.
- the concentration temperature is, for example, 500 ° C., but the present disclosure is not limited to this.
- the concentration temperature may be in the range of 425 to 930 ° C. as the maximum width, and more preferably in the range of 425 to 700 ° C.
- the distillation temperature is changed to 800 ° C, 1000 ° C, and 1100 ° C as an example, but the present disclosure is not limited thereto.
- the distillation temperature may be changed depending on the situation. That is, step S5 should just be set to a temperature higher than step S4, and step S6 should just be set to a temperature higher than step S5.
- step S5 should just be set to a temperature higher than step S4
- step S6 should just be set to a temperature higher than step S5.
- distillation apparatus 8 (distillation step) of the above embodiment distillation is performed at three different temperatures. However, distillation may be performed at two different temperatures, or at four or more different temperatures.
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Abstract
Description
本願は、2018年6月6日に日本に出願された特願2018-108973号に基づき優先権を主張し、その内容をここに援用する。
制御装置10はコンピュータから構成されており、このコンピュータは、CPU(中央処理装置)、記憶装置、及び入出力装置等を備える。記憶装置は、RAM(Random Access Memory)等の揮発性メモリ、ROM(Read Only Memory)等の不揮発性メモリ、HDD(Hard Disk Drive)、及びSSD(Solid State Drive)等のうちの1以上を含む。入出力装置は、有線または無線でBi供給装置2、TiCl4供給装置3、Mg供給装置4、MgCl2回収装置5、偏析装置6、濃縮装置7、蒸留装置8及び排気装置9と信号やデータ(温度や圧力等の計測データ)のやり取りを行う。図1においては、簡略化のため制御装置10が蒸留装置8のみに有線または無線で接続されていることを示しているが、制御装置10は各装置に接続されている。コンピュータは、記憶装置に保存されたプログラム等に基づいて所定の機能を果たすことができる。なお、Bi供給装置2、TiCl4供給装置3、Mg供給装置4、MgCl2回収装置5、偏析装置6、濃縮装置7、蒸留装置8及び排気装置9に各別に設けられたコンピュータによって制御装置10が構成されてもよい。
TiCl4+Bi+2Mg→Bi-Ti+2MgCl2 (1)
言い換えれば、本実施形態の蒸留装置8(蒸留工程)は、偏析装置6(偏析工程)で得た析出物(本実施形態ではTi8Bi9金属間化合物)に含まれるチタンの構造を維持でき、且つ上記析出物内部からその表面に向けてビスマスが拡散することで当該表面からのビスマスの蒸発が維持されるような第1の温度(本実施形態では800℃またはその近傍の温度)で上記析出物を加熱する。上記第1の温度による加熱では、析出物内部からその表面に向かうビスマスの拡散が維持されるため、析出物の表面からビスマスが蒸発しても当該表面でのビスマスの含有量は適切に維持される。言い換えれば、析出物の表面でチタンの含有量が高くなりチタンが膜状になることを防止できるため、析出物内部からその表面に向かうビスマスの拡散と当該表面からのビスマスの蒸発とが適切に維持される。さらに、上記第1の温度による加熱では、析出物に含まれるチタンが融解せず、その金属構造を維持できるため、析出物からビスマスが蒸発し続けることで、次第に析出物は多数の孔を備える多孔質状に変化する。これらの孔を介することで、さらに析出物内部からのビスマスの拡散及び蒸発を促進することができる。なお、蒸留装置8内の圧力等に応じて、第1の温度は適宜調整してもよい。
言い換えれば、上記第1の温度による加熱の後に、上記第1の温度よりも高い第2の温度(本実施形態では1000℃もしくはその近傍の温度、または1100℃もしくはその近傍の温度)で上記析出物をさらに加熱する。上述したように、析出物からビスマスが蒸発することで、当該析出物におけるチタンの含有量は増加し、よって析出物の融点の上昇が期待される。このため、上記第1の温度よりも高い第2の温度で析出物を加熱しても、そこに含まれるチタンの金属構造を維持しつつ、析出物内部から表面に向かうビスマスの拡散及び表面からの蒸発をさらに促進することができる。よって、析出物におけるビスマスの含有量を効果的に減少させることができる。上記第2の温度は、析出物の融点の上昇に応じて適宜選択すればよい。
(1)上記実施形態では、金属チタン製造装置は、混合物X6を固液分離することで濃縮する濃縮装置7を備えるが、本開示はこれに限定されない。金属チタン製造装置は、濃縮装置7を備えず、蒸留装置において、混合物X6を直接蒸留してもよい。
2 Bi供給装置
3 TiCl4供給装置
4 Mg供給装置
5 MgCl2回収装置
6 偏析装置
7 濃縮装置
7a 濃縮炉
7b Arガス供給装置
7c 駆動源
8 蒸留装置
9 排気装置
Claims (9)
- ビスマスとマグネシウムとの存在下で四塩化チタンを還元処理することにより、チタン及び前記ビスマスからなる液体合金を得る還元装置と、
前記液体合金を偏析処理することにより析出物を得る偏析装置と、
前記析出物を蒸留処理して金属チタンを得る蒸留装置と、
を備え、
前記蒸留装置は、前記析出物に付帯する前記ビスマスを優先的に蒸発させるように雰囲気を設定し、その後に前記析出物を形成する前記ビスマスを蒸発させるように雰囲気を設定する、金属チタン製造装置。 - 前記析出物に付帯する前記ビスマスを前記析出物から分離することにより濃縮金属間化合物を得る濃縮装置をさらに備え、
前記蒸留装置は、前記析出物に代えて前記濃縮金属間化合物を蒸留処理する、請求項1に記載の金属チタン製造装置。 - 前記蒸留装置は、前記析出物に付帯する前記ビスマスを優先的に蒸発させるための雰囲気として前記析出物が800℃またはその近傍の温度となるように設定する、請求項1または2に記載の金属チタン製造装置。
- 前記蒸留装置は、前記析出物を形成する前記ビスマスを蒸発させるための雰囲気として前記析出物が1000℃またはその近傍の温度となるように設定する、請求項3に記載の金属チタン製造装置。
- 前記蒸留装置は、前記析出物を形成する前記ビスマスを蒸発させるための雰囲気として前記析出物が1100℃またはその近傍の温度となるように設定する、請求項3に記載の金属チタン製造装置。
- 前記蒸留装置は、前記析出物を形成する前記ビスマスを蒸発させるための雰囲気として、前記析出物が1000℃またはその近傍の温度となるように設定し、その後、前記析出物が1100℃またはその近傍の温度となるように設定する、請求項3に記載の金属チタン製造装置。
- 前記蒸留装置は、前記偏析装置で得た前記析出物に含まれるチタンの構造を維持でき、且つ前記析出物内部からその表面に向けてビスマスが拡散することで当該表面からのビスマスの蒸発が維持されるような第1の温度で前記析出物を加熱し、その後、前記第1の温度よりも高い第2の温度で前記析出物を加熱する、請求項1に記載の金属チタン製造装置。
- ビスマスとマグネシウムとの存在下で四塩化チタンを還元処理することにより、チタン及び前記ビスマスからなる液体合金を得る還元工程と、
前記液体合金を偏析処理することにより析出物を得る偏析工程と、
前記析出物を蒸留処理して金属チタンを得る蒸留工程と、
を有し、
前記蒸留工程では、前記析出物に付帯する前記ビスマスを優先的に蒸発させるように前記析出物回りの雰囲気を設定し、その後に前記析出物を形成する前記ビスマスを蒸発させるように前記雰囲気を設定する、金属チタン製造方法。 - 前記蒸留工程では、前記偏析工程で得た前記析出物に含まれるチタンの構造を維持でき、且つ前記析出物内部からその表面に向けてビスマスが拡散することで当該表面からのビスマスの蒸発が維持されるような第1の温度で前記析出物を加熱し、その後、前記第1の温度よりも高い第2の温度で前記析出物を加熱する、請求項8に記載の金属チタン製造方法。
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