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WO2005021807A2 - Systeme, procede et appareil de separation - Google Patents

Systeme, procede et appareil de separation Download PDF

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Publication number
WO2005021807A2
WO2005021807A2 PCT/US2004/028553 US2004028553W WO2005021807A2 WO 2005021807 A2 WO2005021807 A2 WO 2005021807A2 US 2004028553 W US2004028553 W US 2004028553W WO 2005021807 A2 WO2005021807 A2 WO 2005021807A2
Authority
WO
WIPO (PCT)
Prior art keywords
vessel
metal
slurry
salt
liquid metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2004/028553
Other languages
English (en)
Other versions
WO2005021807A3 (fr
Inventor
Donn Reynolds Armstrong
Rirchard P. Anderson
Stanley S. Borys
Lance Jacobsen
Dariusz Kogut
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
International Titanium Powder LLC
Original Assignee
International Titanium Powder LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from PCT/US2003/027647 external-priority patent/WO2004022798A1/fr
Priority claimed from PCT/US2003/027649 external-priority patent/WO2004048622A1/fr
Priority claimed from PCT/US2003/027653 external-priority patent/WO2004028655A2/fr
Priority to US10/570,422 priority Critical patent/US20070180951A1/en
Priority to CNA2004800309734A priority patent/CN1894427A/zh
Priority to EA200600520A priority patent/EA011795B1/ru
Priority to AU2004269422A priority patent/AU2004269422B2/en
Application filed by International Titanium Powder LLC filed Critical International Titanium Powder LLC
Priority to CA002537659A priority patent/CA2537659A1/fr
Priority to JP2006526175A priority patent/JP2007533843A/ja
Publication of WO2005021807A2 publication Critical patent/WO2005021807A2/fr
Publication of WO2005021807A3 publication Critical patent/WO2005021807A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • C22B9/023—By filtering
    • 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
    • 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
    • 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
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04—Refining by applying a vacuum
    • 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

  • This invention relates to a separation system, method and apparatus useful for
  • the present invention provides a system and method for handling the product
  • a slurry is produced which if filtered provides a filter cake in the form of a gel.
  • the slurry has a solids fraction which depends in large part on the amount of excess reductant metal used to control the steady-state temperatures at which the reaction
  • the liquid metal in the gel has to be removed by way of distillation with or without a vacuum or by contact with
  • a hot sweep gas preferably inert to the constituents of the gel with or without a vacuum or any combination thereof.
  • a principal object of the invention is to provide a separation system, method and
  • Another object of the invention is to provide a continuous separation system.
  • the invention consists of certain novel features and a combination of parts hereinafter
  • Figure 1 is a schematic illustration of the separation system of the present invention.
  • FIG. 2 is a schematic view of a system for practicing the method of the present invention
  • FIG. 3 is an enlarged schematic representation of the product filtering disc portion of the system illustrated in Fig. 2shown in longitudinal sectional view;
  • FIG. 4 is a horizontal cross-sectional view of the vessel illustrated in Fig. 3
  • FIG. 5 is an alternate embodiment of the system illustrated in Fig. 2 and
  • FIG. 6 is a schematic representation of a variety of processes and products made by or from powder separated from slurries according to the present invention.
  • FIG. 7 is a graph of pressure rise versus time for a flat plate filter nutsche runs;
  • FIG. 8 shows data for various temperatures as a function of time and pressure;
  • FIG. 9 shows a schematic of the filter trap for the above example
  • FIG. 10 shows a schematic of another embodiment of the filter trap of Fig. 3.
  • FIG. 11 is a schematic diagram showing the two vessels and an embodiment of the
  • FIG. 12 is a schematic of an alternate embodiment of the present invention
  • FIG. 13 is a schematic illustration of yet another embodiment of the present invention
  • FIG. 14 is a schematic representation of a separation system incorporating features of
  • the system 10 of the present invention deals with the separation of a metal, alloy or
  • the product of Armstrong process is a slurry of excess reductant metal, product metal and alloy or ceramic and salt produced from the
  • This slurry has to be separated so that various parts of it can be recycled and the produced metal, alloy or ceramic separated and passivated if necessary.
  • a source of, for illustration purposes only, titanium tetrachloride 12 which is introduced into a reactor 15 of the type hereinbefore disclosed in the Armstrong process.
  • a supply tank or reservoir 17 with a supply of titanium tetrachloride 12 which is introduced into a reactor 15 of the type hereinbefore disclosed in the Armstrong process.
  • the slurry product 20 is transferred to a vessel 25 which is in the illustration dome-
  • the vessel 25 having an interior 26 into which the slurry product 20 is introduced.
  • a filter 27, preferably but not necessarily cylindrical, is positioned within the interior 26 and defines an annulus 28, the slurry product 20 being received inside the cylindrical filter 27.
  • An annular heat exchanger 29 is positioned
  • the vessel 25 further includes a moveable bottom closure 30.
  • the collection vessel 35 is positioned below the vessel 25 and is sealed therefrom by the moveable bottom closure 30.
  • the collection vessel 35 has an inwardly sloping bottom surface 36 which leads to a crusher 38 and a valve 39 in the outlet 40 of the collection vessel
  • a vapor conduit 42 interconnects the top of the vessel 25 and particularly the interior 26 thereof with a condenser vessel 45, the condenser vessel having a heat exchange plate 46 connected, as hereinafter described, to an isolated cooling system 60.
  • the isolated heating system 50 includes a head tank 52 for the heating fluid which is
  • the isolating cooling system 60 also is provided with a head tank 62, a pump 63 and a cooler 65 which serves to cool the cooling fluid circulated in an isolated loop to the cooling plates 46 as will be hereinafter set forth.
  • a product conveyor 70 having a baffle or cake spreader 71 extending downwardly toward the conveyor 70.
  • the conveyor 70
  • vessel 35 after removal of the excess reductant metal, is contacted with a counter current flow of gas, preferably but not necessarily oxygen and argon, 77 from a blower 75 in communication with a supply 76 of oxygen and the supply of inert gas such as argon.
  • gas preferably but not necessarily oxygen and argon
  • heat exchanger 79 is in communication with the blower 75 so as to cool the oxygen/argon mixture 77 as it flows in counter current relationship with the produced metal, alloy or ceramic on the conveyor 70, thereby to contact the product particulates with oxygen to inert
  • a back filter valve 91 is provided in order to flush the filter
  • shut-off valves 93 are positioned within the loop, hereinafter to be explained and as required.
  • a vacuum pump 95 is used to draw a
  • Product 20 from the reactor 15 exits through line 110 and enters vessel 25 at the top
  • line 110 is shown entering above the filter 27, preferably the line 110 and filter 27 are positioned so that slurry 20 is introduced below the top of filter 27 or in the center of the filter or both. As described in the previously incorporated patents, the slurry
  • product 20 consists of excess reductant metal, salt formed by the reaction and the product of the reaction which in this specific example is titanium existing as solid particles.
  • the vessel 25 is a filter 27 which occupies a portion of the interior 26 of the vessel 25, the interior optionally being heated with the annular heat exchanger 29.
  • the slurry product 20 is directed to the interior of the filter 27
  • the heat exchange fluid in the plates 32 pass with the heat
  • Heat exchange fluid moves from the heater 55 through the heat exchange plates 32 by means of the pump 53 as the heated heat exchange fluid flows out of the heat exchanger 55 through line 113 and back into the heat exchange plates 32 and/or the annular heat exchanger 29.
  • the heat exchange fluid may or may not be the same as the reductant metal used in the reactor 15. NaK is shown as an example because of the low melting point thereof, but any other suitable heat exchange fluid may be used.
  • Suitable valves 93 control the flow of heat exchange fluid from the heater 55 to either or both of the heat exchanger 29 and plates 32.
  • the plates 32 are relatively close together, on the
  • Exact spacing of the plates 32 depends on a number of factors, including but not limited to, the total surface area of the plates, the heat transfer coefficient of the plates, the amount of
  • reactor 15 is operated, usually up to about two atmospheres.
  • the product slurry 20 enters the inside of filter 27 under elevated pressure and gravity results in the liquid reductant metal
  • Heating fluid liquid or vapor, for instance Na vapor
  • the temperature in vessel 25 is elevated sufficiently to vaporize remaimng liquid metal reductant 18 therein which is drawn off through conduit 42 to the condenser 45.
  • the conduit 42 is required to be relatively large in diameter to permit rapid evacuation of the interior 26 of the vessel 25. Because the pressure drop between the vessel 25 and the condenser 45, during vaporization of
  • the reductant metal 18 is low, the specific volume is high and the mass transfer low, requiring a large diameter conduit 42. Boiling the reductant metal on the shell side is accomplished by
  • the annular heat exchanger 29 is optionally operated to maintain the expressed liquid
  • the cooling system 60 is operated in a closed loop and maintained at a temperature sufficiently low that reductant metal vapor introduced into the condenser 45 condenses and flows out of the condenser, as will be disclosed.
  • the cooling system 60 includes a cooler 65 as previously described and the pump 62.
  • cooling system 60 may be the same or may be different, as the systems 50 and 60 can be maintained separately or intermixed.
  • Both the vessel 25 and the condenser 45 are operated at least part of the time under a protective atmosphere of argon or other suitable inert gas from the argon supply 85, the pressure of which is monitored by the transducer 86, the (argon) supply inert gas 85 being connected to the condenser 45 by a line 117, the condenser 45 also being in communication
  • heating system 50 and the cooling system 60 is provided with its own pump, respectively 53 and 63.
  • the heating and cooling fluid may, preferably be NaK due to its lower melting point, but not necessarily, and as an alternative could be the
  • closure 30 is opened, the dry cake falls from the filter 27 into the collection vessel 35
  • the titanium powder is passivated and cooled.
  • the conveyor 70 is positioned in Fig. 1 horizontally, it may be advantageous to have the conveyor move upwardly at a slant as a safety measure in the event that closure 30 fails, then excess reductant metal would not flow toward a water wash.
  • Cooling and passivating is accomplished in the cooler 79 with blower 75 which blows
  • Oxygen is conducted to the system from a supply thereof 76 through a valve 93 and line 122 and is generally maintained
  • a filter backwash valve 91 is positioned so that the filter 27 can be backwashed when required if it becomes clogged or otherwise requires backwashing.
  • Symbol 100 is used to denote that parallel systems identical or similar to all or a
  • the present invention provides a separation system, apparatus and method which permits the separation to be either continuous or in sequential batches so rapidly switched by appropriate valving as to be as continuous as required.
  • the object of the invention is to provide a separation apparatus, system and method which allows the reactor(s) 15 in a commercial plant to operate continuously or in economic
  • the heating mechanism shown is by fluid heat exchange, but heaters could also be electric or other equivalent means, all of which are incorporated herein.
  • the bottom closure 30 is shown as hinged and is available commercially. The closure 30 may be clamped when shut and hydraulically moved to the open position; however, sliding closures such as gate valves are available and incorporated herein.
  • the reactor 20 is shown separate from the vessel 25, the invention includes engineering changes within the skill of the art, such as but not limited to incorporating reactor 20 into vessel 25. Although not shown in Fig. 1, it is contemplated that the slurry as it forms a cake on the filter may be agitated and the cake may be broken to facilitate distillation and/or transfer.
  • vessel 35 is illustrated in one embodiment, the vessel 35 could easily be designed as a pipe or the like. Also, the crusher 38 could be located in vessel 25 or intermediate vessel 25 and vessel 35. Moreover, the cake forming on the filter 27 may be broken up prior to or during or subsequent to removal of the liquid metal therefrom. Similarly, when referring to an inert environment, the invention includes a vacuum as well as an inert gas. An important feature of the invention is the separation of vessels 25 and 35 so the environments of each remain separate. That way, no oxygen can contaminate either vessel.
  • a reactor 15 producing 2 million pounds per year of titanium powder or alloy powder requires two vessels 25, each roughly 14' high and 7' in diameter with appropriate valving, so that the reactor 15 would operate continuously and when one vessel 25 was filled, the slurry product from the reactor would switch automatically to the second vessel 25.
  • the fill time for each vessel 25 is the same or somewhat longer than the deliquor,
  • the invention as disclosed permits continuous production and separation of metal or ceramic
  • vessels 25 and related equipment would probably be between 2 and 3 times the number of
  • the system 10A includes a reactor 11 such as, but not limited to the type shown in the Armstrong Process, including a nozzle 12 through which
  • liquid metal flows and having a housing 14 surrounding the nozzle.
  • a gas inlet 15 serves to introduce gas from a source 16 thereof into the liquid metal thereby producing an exothermic
  • reaction may be a slurry of a liquid reducing metal, such as sodium, having dispersed therein particles of the element or alloy produced, such as titanium or an alloy thereof, and the
  • reaction product from the gas which may be sodium chloride or combination of chloride salts, as in the case of sodium and titanium tetrachloride.
  • the slurry leaves the reactor housing 14 through an outlet 18 and is introduced into a receiving vessel 20 having near the top thereof a dome portion 21 and a cylindrical portion 22 terminating in a frustoconical portion 23 having a discharge outlet 25 at the bottom thereof terminating in a circular flange 26.
  • a motor 30 may be mounted at the top of the vessel 20 connected to an output shaft 31 having an agitator 32 at the bottom of the cylindrical portion 22 or the frustoconical portion
  • Indexing filter system 35 is in communication with the vessel 20 and more particularly includes a housing 36, having a top 37, a cylindrical side wall
  • the housing 38 provided with opposed upper apertures 39 and opposed lower apertures 41.
  • An index drive 45 includes a motor 46 having an output shaft 47 in communication
  • An aperture 49A is provided in the cylindrical wall 38 to accommodate the axle 49.
  • An indexing disc 55 is rotatably mounted on the axle 49, the disc having a plurality of longitudinally spaced apart chambers 56 therein, six such chambers being shown for purposes
  • a filter 60 preferably but not necessary a metal wedge wire, is positioned in exit
  • conduit 65 has a collar 61 maintained in sealing contact with the disc 55 through a spring and pin arrangement 62.
  • the chambers 56 in the disc 55 are also in contact with a collar and spring and pin arrangement in communication with an inlet conduit 63 so as to provide a
  • a T-shaped conduit 66 having flanges and seals 67 connecting the outlet
  • a sealing flange 26A (Fig. 2) with the usual seals (not shown) to provide a suitable connection between the vessel 20 and the indexing filter system 35.
  • Compaction ram assembly 70 is mounted to the housing 36 of the indexing filter system 35 and includes a piston rod 71 having mounted thereon a piston 72.
  • the piston rod 71 is surrounded by a bellows seal 73 and is connected at one end to a suitable drive or motor
  • a discharge ram assembly 80 is mounted to the housing 36 including a similar piston
  • the discharge ram assembly 80 is rotated for clarity but may be positioned anywhere around the housing 36 in which a chamber 56 is positioned during the
  • system 10A of the present invention may also include two or more compaction ram
  • the discharge ram assembly 80 further includes, as did the compaction ram assembly 70, collars 86 and springs and retaining pins 87 to ensure a
  • a cake breaker 93 which may be in the form of a stationary grid or flexible members is positioned at the end of the distillation system 95, as will be explained and for a purpose hereinafter described.
  • a distillation system 95 is in communication with the outlet conduit 90 of the
  • indexing filter system 35 and includes a longitudinally extending conveyor 96 in a container
  • the distillation system 95 is in communication with a condenser assembly 100 by means of one more tubes 101 extending from the container 98 to a condenser containerl03, it being understood that the condenser container 103 is shown for purposes of illustration as an elongated container but may be of any size or shape as dete ⁇ iiined.
  • the condenser container 103 is also connected by
  • a conduit 102 provides communication
  • a distillation vacuum pump 106 having connected thereto a distillation vacuum pump 106 and an outlet pipe 107.
  • a pumpl08 pumps liquid metal from the supply vessel 105 through a conduit 109 to a liquid metal accumulation tank 115.
  • the tank 115 also receives liquid metal from a head tank 110 in
  • a heat exchanger 112 may be in heat exchange relationship with the outlet conduit 65 if heat is needed to be added or removed from the liquid metal exiting the indexing filter system 35, as
  • a vessel 120 is positioned in communication with the distillation system 95 and
  • valve 121 the vessel 120 being in communication with a pump 122 which in turn is in communication with a vessel 125 or lock hopper which is also provided with a valve 126 at the bottom thereof.
  • the vessel or lock hopper 125 through valve 126 is in communication
  • a passivation system 130 which includes a containment vessel 131, a conveyor 132 in communication with a gas inlet conduit 133 and a gas outlet conduit 134 in communication with a pump 135.
  • the passivation system 130 has an outlet 136, all for a purpose hereinafter set forth.
  • Operation of the system 10A is as follows.
  • a supply of gas 16 is brought to temperature in a boiler which is meant to be included in the vessel 16 and is transmitted
  • Liquid metal pump 105 provides a continuous flow of liquid metal to the nozzle 12 and the amount of liquid metal
  • ram assembly 70 is actuated and the piston 72 drives forwardly into the chamber 56 compressing the material in the conduit 66 thereby expressing liquid metal through the filter 60 until a cake is formed in which most of the liquid metal has been expressed and there remains what could be categorized as wet cake particulate salt and particulate titanium. This cake has sufficient integrity to hold its shape but at the same time still contains some liquid
  • liquid metal which exits the indexing filter system 35 through the outlet conduit 65 is then recycled to the head tank 110 and moved via the pump 108 back to the nozzle 12 in the reactor 11.
  • the motor therefor 74 withdraws the piston 72 and the indexing disc 55 is rotated by the index drive mechanism 45 so as to advance the next chamber 56 into position for
  • the chamber 56 after compaction until the next chamber is in alignment with the compaction ram 70, at which time the aligned chamber 56 fills with the slurry and is thereafter compacted or compressed.
  • the discharge ram assembly 80 is in alignment or in registry with another chamber 56 of the indexing disc 55 and when the chamber 56 which has the compressed or compacted
  • seals are not necessarily perfect in the real world and although the sealing mechanism in the conduits are intended to provide a seal for the liquid metal, some inevitably may escape and is collected within the
  • compaction ram assembly 70 and one discharge ram assembly 80 it is well within the skill of the art to include more than one compaction and/or discharge ram assembly 70, 80.
  • the particulates from the cake are heated by virtue of the heat exchanger 97, which may be via conduction, convection, induction heating or any other suitable commercial method of heating the powder or particulates moved by the conveyor 96 through the cake breaker 93 to the vessel 120.
  • the cake breaker 93 is shown schematically and may be a fixed series of wires or a variety of other mechanical mechanisms which breaks
  • Liquid metal which is vaporized in the distillation system 95 is collection and transmitted via conduits 101 into the condenser assembly 100 and container 103 which is maintained at a sufficiently low temperature to
  • a valve 121 exists between the vessel 120 and the vessel or lock hopper 125.
  • pump 122
  • the particulates move in countercurrent relation to the passivation material but may not be required to do so.
  • the passivation material may not be required to do so.
  • passivation fluid is a gas containing a small percentage such as 0.2% by volume oxygen and
  • FIG. 5 there is shown an alternate embodiment of the present invention in which like numbers have been applied to like parts.
  • the principal difference in the embodiment of Fig. 5 is that the indexing disc 55 as well as the indexing filter system 35
  • the discharge ram assembly 80 is actuated to move the cake into the distillation system 95.
  • the discharge ram assembly 80 is actuated to move the cake into the distillation system 95.
  • the chambers 56 would be 10 inches in diameter and 6 inches in length. Preferably there are 6 such chambers in each disc 55 based calculations that the slurry and/or
  • the indexing disc 55 will be indexed approximately every 11 seconds based on the above-
  • ejected by the compaction ram assembly 80 will be about 1.5 inches thick and have a solids composition between about 64 and 65 percent by weight.
  • Fig. 6 there is disclosed a schematic representation of the various components
  • the reduction box is
  • the separation is as previously described herein along with the passivation.
  • the passivated material then is transmitted to a wash and dry assembly 140 in which the salt product, in this specific example, sodium chloride, is removed from the product particulates, in the example titanium or titanium alloy powder.
  • the salt product in this specific example, sodium chloride
  • the schematic shows that the powder may be melted to form an ingot or other solid product by a variety of methods such as casting or transmitted to a powder metallurgy process which includes, but is not limited to, for
  • the product may also be produced by cold spraying the metal powder in a gas jet or subjecting the metal powder to a laser or spheridizing the metal powder by plasma.
  • the metal powder may be formed into a foam and
  • the powder may be pressed onto a mandrel and thereafter rolled into a thin wall tube.
  • powder product may be formed by drawing or extruding the metal powder, hi the event that product morphology such as the packing fraction, mean size or size distribution needs to be
  • Attriting mechanism may be used to change the morphology of the powder, including the packing fraction or reducing the overall size distribution of the powder.
  • P-trap is the pressure above the filter (assume downstream pressure remains constant) as the run progressed.
  • Flow 2 is the Na flow rate and the V reactor shows when the product
  • the trap was designed to allow distillation through the filter into the bottom of the trap to utilize the full trap diameter for vapor movement.
  • the trap also
  • the distillation times can be decreased from about (22 or 28) hours to about (9 to 11 ) hours. This is of significant importance in the design of plants by simplifying designs, reducing collection tanks, valves,
  • crumbling the filter cake into small quantities such as less than about five centimeters in diameter and preferably in the range of from about two to about five centimeters in diameter,
  • positive pressure such as, but not limited to, psig with a heated or hot inert gas, such as but
  • a transfer mechanism 10E which includes a double walled conduit including an outer conduit wall 11 having a liquid outlet 12
  • cylindrical wall 11 is an inner tube or conduit 15 having a portion 16 which is solid and a portion 17 which is apertured and maybe a mesh of any suitable size.
  • the inner tube or conduit 15 having a portion 16 which is solid and a portion 17 which is apertured and maybe a mesh of any suitable size.
  • conduit 15 may either be cylindrical as illustrated in Fig. 1 or conical as will be explained, the inner conduit 15 has a discharge end 18 thereof which opens into a vacuum chamber 25 and
  • a feed screw 30 is positioned within the inner conduit 15 and includes a rotatable
  • the thread 32 may have a constant or a variable pitch.
  • the pitch is the distance between adjacent threads and the variable pitch may preferably be a progressive pitch in which the pitch decreases from the vessel 20 toward the container or vessel 25, for a purpose hereinafter
  • mechanism 10E is used in conjunction with a material made by the Armstrong Process. More
  • the slurry discussed herein will be a combination of liquid sodium, sodium chloride particles and particles of titanium and/or a
  • the vessel or container 20 preferably operated under an inert atmosphere
  • the wall of the cylinder or tube 16 diminishes as material is moved by the feed screw 30 from container or vessel 20 to container or vessel 25.
  • the slurry is concentrated and reaches the portion 16, the solid portion 16 of the inner tube or conduit 15, a seal is established between the vessel 25 and the vessel 20 which houses the slurry from the reactor.
  • the formation of a seal by the transfer mechanism 10 is a critical aspect of the present invention because separation of liquid sodium and salt from the desired particles of the
  • vacuum chamber or a vessel 25 and the Armstrong reactor itself may be an inerted vessel such as with argon. Accordingly, it is important for a seal to be formed between the two
  • the transfer mechanism 10F has a housing 15A
  • conical in shape and the screw 30 therein may or may not be a progressive pitch screw.
  • screw threads in the embodiment illustrated in Fig. 12 may not need to be closer together, that is the pitch need not be diminished in order to reduce the volume of the material between
  • FIG. 13 there is shown another embodiment of the present invention 10G
  • shank 3 IB of the screw 3 OB is conical in shape with the larger end of the cone being adjacent the vessel 25B and with the pitch between adjacent threads 32B being constant
  • the invention includes movement and concentration of material from one
  • containers may be connected pipes or vessels, and the environments may be vacuums, inerted atmospheres or otherwise.
  • FIG. 14 there is shown a separation schematic which is a combination of
  • a reactor to produce by exothermic reaction, in one instance, a slurry of a metal powder, salt particles, and excess reductant metal.
  • the reactor is operated under an inert atmosphere, as taught in the Armstrong Patents, and the slurry produced is transferred to a first vessel, also operated under an inert atmosphere and /or vacuum, as will be explained since the separation process may include portions thereof at either or both positive or negative pressure, that is the first vessel is inerted. It is very important to prevent oxygen contamination of the first vessel during the processing of the
  • a second vessel which may be a tank or a pipe or any container operated under an inert atmosphere and/or vacuum into which the treated slurry( either wet or dry and either metal powder or a combination of metal powder and salt
  • Fig.l there is shown an apparatus in which the slurry is heated in the first vessel to remove excess liquid metal as both liquid and as vapor.
  • the dried cake is transferred to a
  • the first vessel can be used to treat the slurry by heating to produce either metal powder alone or in combination with salt particles.
  • the first vessel in system 10A can include a sequential indexing
  • the first vessel of Fig.14 is a combination of receiving vessel 20 and indexing filter system 35 which produces a sequence of squeezed cakes to a second vessel or distillation system 95, as previously described.
  • Fig.14 may be disposed horizontally as the distillation system 95 in system 10A illustrated in
  • Figs. 2-6 may or may not have a conveyor therein, all depending on engineering considerations within the skill of the art.
  • material in the second container which is now dry, but may be either metal powder alone or a combination of metal
  • powder and salt is moved one way or another through a lock, as illustrated, or a seal or a valve or any comparable mechanism from the inerted condition of the second container to
  • the lock mechanism maybe the variable pitch screw of Fig. 11 or the variations thereof in Figs. 12 and
  • the treatment of the slurry in the first vessel under an inert atmosphere or vacuum or combinations thereof may produce a wet or dry cake of metal
  • Heaters either internal or external or both, and/or hot inert sweep gases may be used at either positive or negative pressures or combinations of both positive and negative pressures with either the heaters or sweep gas or both to move material, either excess reductant metal alone or a combination of reductant metal and salt, out of the first vessel.
  • the second container may employ a hot
  • inert sweep gas or other mechanism to isolate the metal powder from unwanted constituents. Thereafter, transfer is made to the conveyor, or alternate mechanism, for additional treatment or handling. Passivation with an inert gas having a small amount of oxygen after cooling may be employed, as previously described, followed by a water wash and drying before packaging. Alternately, if both the reductant metal and the salt are removed in the first vessel and/or the second container, the water washing and/or passivation may not be required, resulting perhaps in lower oxygen contamination and/or expense. While there has been disclosed what is considered to be the preferred embodiment of the present invention, it is understood that various changes in the details may be made without departing from the spirit, or sacrificing any of the advantages of the present invention.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un système, un procédé et un appareil permettant de traiter une suspension boueuse de métal liquide et de particules solides au moyen de diverses combinaisons de distillation sous vide et de transfert sous vide avec un gaz inerte chaud. L'invention concerne également divers mécanismes permettant de sceller des chambres rendues inertes ou des chambres à vide afin d'empêcher toute infiltration d'oxygène.
PCT/US2004/028553 2003-09-02 2004-09-02 Systeme, procede et appareil de separation Ceased WO2005021807A2 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
JP2006526175A JP2007533843A (ja) 2003-09-03 2004-09-02 分離システム、方法および装置
CA002537659A CA2537659A1 (fr) 2003-09-02 2004-09-02 Systeme, procede et appareil de separation
US10/570,422 US20070180951A1 (en) 2003-09-03 2004-09-02 Separation system, method and apparatus
CNA2004800309734A CN1894427A (zh) 2003-09-02 2004-09-02 分离系统、方法与设备
EA200600520A EA011795B1 (ru) 2003-09-03 2004-09-02 Способ выделения металлического порошка из суспензии и система для его осуществления
AU2004269422A AU2004269422B2 (en) 2003-09-02 2004-09-02 Separation system, method and apparatus

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
USPCT/US03/27649 2003-09-02
US49985703P 2003-09-03 2003-09-03
US60/499,857 2003-09-03
USPCT/US03/27647 2003-09-03
PCT/US2003/027647 WO2004022798A1 (fr) 2002-09-07 2003-09-03 Dispositif a vis utilise pour transferer de la boue reactionnelle contenant du ti dans une enceinte sous vide
PCT/US2003/027653 WO2004028655A2 (fr) 2002-09-07 2003-09-03 Appareil et procede de traitement d'un gateau au moyen d'un filtre
USPCT/US03/27653 2003-09-03
PCT/US2003/027649 WO2004048622A1 (fr) 2002-11-20 2003-09-03 Systeme permettant la separation d'une poudre metallique dans une suspension et procede

Publications (2)

Publication Number Publication Date
WO2005021807A2 true WO2005021807A2 (fr) 2005-03-10
WO2005021807A3 WO2005021807A3 (fr) 2005-04-28

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Country Link
AU (1) AU2004269422B2 (fr)
CA (1) CA2537659A1 (fr)
WO (1) WO2005021807A2 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005028145A3 (fr) * 2003-09-15 2005-12-22 Int Titanium Powder Llc Procede, dispositif et systeme pour la separation de sel/poudre metallique
WO2008013518A1 (fr) * 2005-07-21 2008-01-31 International Titanium Powder, Llc. Alliage de titane
US8322046B2 (en) 2003-12-22 2012-12-04 Zhaolin Wang Powder formation by atmospheric spray-freeze drying
CN114438345A (zh) * 2022-01-29 2022-05-06 安徽理工大学 一种用于镁热法制海绵钛蒸馏工艺的终点判断装置与方法
CN115116638A (zh) * 2021-03-19 2022-09-27 中国核工业二三建设有限公司 一种钠钾合金冷却剂管道系统拆除及后处理方法

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2003273279B2 (en) 2002-09-07 2007-05-03 Cristal Us, Inc. Process for separating ti from a ti slurry
AU2003263082A1 (en) 2002-10-07 2004-05-04 International Titanium Powder, Llc. System and method of producing metals and alloys
US9127333B2 (en) 2007-04-25 2015-09-08 Lance Jacobsen Liquid injection of VCL4 into superheated TiCL4 for the production of Ti-V alloy powder
WO2014209173A1 (fr) * 2013-06-28 2014-12-31 Общество с ограниченной ответственностью "Современные химические и металлургические технологии" Procédé de production de titane par réduction à partir de tétrachlorure de titane

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3867515A (en) * 1971-04-01 1975-02-18 Ppg Industries Inc Treatment of titanium tetrachloride dryer residue
US4379718A (en) * 1981-05-18 1983-04-12 Rockwell International Corporation Process for separating solid particulates from a melt
US5437854A (en) * 1994-06-27 1995-08-01 Westinghouse Electric Corporation Process for purifying zirconium tetrachloride
US6409797B2 (en) * 1994-08-01 2002-06-25 International Titanium Powder Llc Method of making metals and other elements from the halide vapor of the metal
UA78623C2 (en) * 2002-11-20 2007-04-10 Int Titanium Powder Llc Method of separating, meant for separation of metal powder from a slurry (variants) and separating system for realization the same

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005028145A3 (fr) * 2003-09-15 2005-12-22 Int Titanium Powder Llc Procede, dispositif et systeme pour la separation de sel/poudre metallique
US8322046B2 (en) 2003-12-22 2012-12-04 Zhaolin Wang Powder formation by atmospheric spray-freeze drying
WO2008013518A1 (fr) * 2005-07-21 2008-01-31 International Titanium Powder, Llc. Alliage de titane
US9630251B2 (en) 2005-07-21 2017-04-25 Cristal Metals Inc. Titanium alloy
CN115116638A (zh) * 2021-03-19 2022-09-27 中国核工业二三建设有限公司 一种钠钾合金冷却剂管道系统拆除及后处理方法
CN115116638B (zh) * 2021-03-19 2023-10-20 中国核工业二三建设有限公司 一种钠钾合金冷却剂管道系统拆除及后处理方法
CN114438345A (zh) * 2022-01-29 2022-05-06 安徽理工大学 一种用于镁热法制海绵钛蒸馏工艺的终点判断装置与方法
CN114438345B (zh) * 2022-01-29 2023-06-27 安徽理工大学 一种用于镁热法制海绵钛蒸馏工艺的终点判断装置与方法

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AU2004269422B2 (en) 2009-09-10
CA2537659A1 (fr) 2005-03-10
AU2004269422A1 (en) 2005-03-10
WO2005021807A3 (fr) 2005-04-28

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