JP2007533843A - Separation system, method and apparatus - Google Patents

Abstract

Systems, methods, and apparatus for processing liquid metal and solid particle slurries are disclosed using various combinations of vacuum distillation and hot inert gas transfer. Various mechanisms are disclosed for inerting or sealing the vacuum chamber to prevent oxygen ingress.

Description

Detailed Description of the Invention

RELATED APPLICATIONS This application is subject to US Provisional Patent Application No. 60 / 499,857 (2002 September) in accordance with Section 119 (e) of Title 35 USC and any other applicable United States Patent Law provisions. Filed on March 3rd, title of invention “SEPARATION SYSTEM, METHOD AND APPARATUS”), and PCT application number PCT / US03 / 027649 (filed September 2, 2003, title of invention “separation” "SEPARATION SYSTEM AND PROCESS", by Richard Armstrong and Lance Jacobsen), and US Provisional Application No. 60 / 497,192 (filed Aug. 22, 2003, entitled "Indexing Separation System ( INDEXING SEPARATION SYSTEM) "by William A. Ernst), and PCT Patent Application No. PCT / US03 / 027653 (filed September 3, 2003, Title of the invention "FILTER CAKE TREATMENT APPARATUS AND METHOD", by Richard Anderson, Donn Armstrong and Lance Jacobsen), and PCT Application No. PCT / US03 / 027647 (filed September 3, 2003, Claims the benefit of the priority of the title "FILTER EXTRACTION MECHANISM", by Richard Anderson, Donn Armstrong and Lance Jacobsen.

BACKGROUND OF THE INVENTION The present invention is an Armstrong method disclosed and claimed in US Pat. Nos. 5,779,761, 5,958,106 and 6,409,797. The disclosures of each of the above patents are incorporated herein by reference, with regard to separation systems, methods and apparatus useful for separating the slurry produced by

  Various metals that control the reaction temperature are disclosed in the Armstrong process, but at present the most industrially (or commercially) process is the titanium tetrachloride to obtain the product titanium or the chloride mixture to obtain the alloy. In order to absorb the heat of reaction during the exothermic reaction of the halide gas, an excessive amount of reducing agent metal such as sodium is used. If an excess of liquid reducing agent metal is used, the reaction product produces elemental or alloy powders to be produced, particulate salts, and excess reducing agent metal. The scope of the invention extends beyond the Armstrong process products to any slurry comprised of liquid metal and particulate material that must be separated from the liquid metal and subsequently processed. It should be understood. For the sake of brevity, the exothermic reduction of titanium tetrachloride with sodium that produces titanium particles, sodium chloride particles and excess sodium shall be described, but is not limited thereto.

  When industrializing the Armstrong process, it is particularly required to quickly handle the product obtained from the Armstrong reactor. This is because the product is produced so quickly that its continuous processing becomes extremely important. The present invention is based on the Armstrong process so that an Armstrong reactor can be operated continuously to produce elemental metals or alloys at 2,000,000,000 pounds / year while using a single separation vessel and system for the reactor. Systems and methods for handling manufactured products are provided. This means that the Armstrong reactor can be operated economically in 24 hours a day, 7 days a week to obtain a metal or alloy or any material produced by the Armstrong process, This is important because it is applied to handle other slurries.

  In producing a metal or alloy or other elemental metal as described in the above-referenced patent, a slurry is formed, which when filtered produces a filter cake in the form of a gel. The slurry has a solid fraction that is predominantly due to excess reducing agent metal, which is used to control the steady state temperature at which the reaction proceeds. When liquid metal is extracted through a filter to form a filter cake, the gel is formed and particles are not settle from it unless the gel is broken, such as by mechanical failure or other means. When a gel is formed, the gel includes metal particles formed during reduction, salt particles formed during reduction, and liquid metal interstitial between them. The liquid metal in the gel can be distilled by distillation with or without vacuum (or reduced pressure), or by contact with hot sweep gas with or without vacuum (preferably inert to the components of the gel) or their It must be removed by any combination.

SUMMARY OF THE INVENTION The main objective of the present invention is to provide a separation system, method and apparatus for the Armstrong process disclosed in US Pat. Nos. '761,' 106 and '797.
Another object of the present invention is to provide a continuous separation system.
The present invention is described in detail below, and is composed of certain novel features and combinations of parts shown in the attached drawings, and various modifications may be made without departing from the spirit of the invention or sacrificing any advantages. It will be appreciated that can be done in detail.

DETAILED DESCRIPTION OF THE INVENTION The system 10 of the present invention addresses the separation of metals such as titanium, alloys or ceramic products from the reaction products in the Armstrong process, which is only given as an example. The Armstrong method is applicable to a wide variety of exothermic reactions, but is mainly applicable to metals, mixtures, alloys and ceramics disclosed in the above-mentioned patents. The product of the Armstrong process is a slurry composed of excess reducing agent metal, product metal and alloy or ceramic, and salt formed from the reaction. The slurry must be separated so that the various parts can be recycled, and the resulting metal, alloy or ceramic is separated and passivated (passivation or film protection) as necessary.

  Referring now to the schematic diagram of the system and method of the present invention shown in FIG. 1, system 10 is described for illustrative purposes only with titanium tetrachloride source 12, which is of the type described above with respect to the Armstrong process. It is introduced into a reactor (or reactor) 15. It is transferred from a supply tank or reservoir (or reservoir) 17 that supplies sodium (or other reducing agent) 18 to a reactor 15 by a pump 19 where excess reducing agent and metal, alloy or ceramic and salt are used. The constructed slurry product 20 is produced at high temperatures, all of which are similar to those already described in the patents incorporated herein.

  The slurry product 20 is transferred to a container 25 (shown in the shape of a dome, but need not be in that shape), and the container 25 has an interior 26 into which the slurry product 20 is introduced. A filter 27 (preferably cylindrical but not essential) is disposed within the interior 26 to define an annulus 28 and the slurry product 20 is placed inside the cylindrical filter 27. An annular heat exchanger 29 is disposed around the vessel 25, all of which will be described later.

  The container 25 further includes a movable bottom closure (or closure) 30. The heat exchange plate 32 is connected to an isolated heating system 50 as described below. A collection container 35 is disposed below the container 25 and is sealed (or sealed) to the container 25 by the movable bottom closure 30. The collection container 35 has a bottom surface 36 that is inclined inward. The bottom surface 36 leads to a crusher 38 and a valve 39 at an outlet 40 of the collection container 35.

  Finally, the vapor conduit 42 interconnects the upper portion of the vessel 25 and in particular its interior 26 with the condenser vessel 45, which is connected to an isolated cooling system 60 as described below. Have The condenser 45 is connected to a condenser reservoir 49, and the condensate collected therein is sent to a sodium supply tank or reservoir 17.

  The isolated heating system 50 includes a head tank 52 for heating fluid, which is transferred to a heater 55 by a pump 53 as will be described below, and the heater 55 encloses the vessel 25 and the interior of the vessel 25. The heat exchange plate 32 is connected to both. The isolated cooling system 60 is also provided with a head tank 62, a pump 63, and a cooler 65. The cooler 65 cools the cooling fluid circulating in the isolated loop and sends it to the cooling plate 46, as will be described later. It works as follows.

  Below the valve 39 and the collection vessel 35 is a product conveyor 70 which has a baffle or cake spreader 71 extending downwardly into the conveyor 70. A conveyor 70 on which the metal, alloy or ceramic and salt produced from the recovery vessel 35 after excess reductant metal is removed is in communication with an oxygen source 76 and an inert gas source such as argon. In contact with countercurrent gas 77 (preferably oxygen and argon, but not essential) from the blower 75 that is present. In order to deactivate the produced metal, alloy or ceramic as required, an oxygen / argon mixture 77 is flowed countercurrently against the produced metal, alloy or ceramic to such an extent that it does not contaminate the produced material. A heat exchanger 79 is in communication with the blower 75 so as to cool the oxygen / argon mixture 77 when the product particles are brought into contact with oxygen.

  As shown in the flow sheet of FIG. 1, a plurality of flow meters 81 are distributed throughout the system as needed and as is well known in the engineering arts. A pressure transducer (PT) 86 and a pressure control valve (PCV) 89 are arranged as needed, all of which are within the engineering capabilities of the art. If necessary, a back filter valve 91 is provided to flush the filter 27. In addition, various standard shut-off bubbles 93 are arranged in the loop as needed as will be described later. The container 25 is evacuated using a vacuum pump 95 as described later. Considering that the accompanying drawings relate to a single reactor 15 and one separation vessel 25, the reference numeral 100 indicates that the same or similar systems can always be operated, in this case industrial production. A plurality of reactors 15 may be operated simultaneously like a plant, indicating that each reactor 15 may have more than one separation vessel 25, all due to engineering economy and normal scale-up problems. It can be decided.

  Product 20 exits reactor 15 through line 110 and enters vessel 25 from its top. Line 110 is shown as entering above filter 27, but preferably line 110 and filter 27 are such that slurry 20 is introduced below the top of filter 27, at the center of the filter, or both. Be placed. As described above in the patents incorporated herein, the slurry product 20 is composed of excess reducing agent metal, salt formed by the reaction, and the product of the reaction, the product of the reaction being In this particular example, titanium is present as solid particles. The slurry form product 20 from the reactor 15 is at elevated temperature depending on the amount of excess reducing agent metal present, its heat capacity, and other factors in the reactor 15 while operating in the Armstrong process. In the container 25, the filter 27 occupies part of the interior 26 of the container 25, which is optionally heated by an annular heat exchanger 29. The slurry product 20 is guided to the inside of the filter 27, where the slurry comes into contact with the heat exchange plate 32.

  In the heating system 50, the heat exchange fluid in the plate 32 passes through the line 112 with the heat exchange fluid from the annular heat exchanger 29 through the line 111. The line 112 connects the heat exchange medium supply source in the head tank 52 to the heat exchanger 55. As the heated heat exchange fluid exits heat exchanger 55 and flows through line 113 and returns to heat exchange plate 32 and / or annular heat exchanger 29, the fluid is pumped from heater 55 to heat exchange plate 32 by pump 53. Move through. Since the heating system 50 is closed loop, the heat exchange fluid may or may not be the same as the reducing agent metal used in the reactor 15. An example is NaK because it has a low melting point, but any other suitable heat exchange fluid may be used. A suitable valve 93 controls the flow of heat exchange fluid from the heater 55 to either or both of the heat exchanger 29 and the plate 32. Preferably, the plates 32 are relatively close to each other, on the order of a few inches, so as to supply more heat to the cake that forms as the excess reducing agent metal evaporates. Further, the closer plate 32 shortens the process of heat transfer and the process of passing through the cake with excess reducing agent metal vapor, thereby distilling away excess reducing agent metal from the vessel 25. The time required for this is shortened. The exact spacing of the plates 32 includes a number of factors including, but not limited to, the total surface area of the plate, the heat transfer coefficient of the plate, the amount of reducing agent metal to be evaporated, and the temperature difference between the inside and outside of the plate. Is not determined).

  As the slurry product 20 exits the reactor 15, the slurry product 20 is at a pressure less than about twice the operating pressure of the reactor 15, usually atmospheric pressure. The product slurry 20 enters the inside of the filter 27 under pressure, the liquid reducing agent metal is expressed by gravity through the filter 27 into the annular space 28 and fed to the reservoir 17 by the line 120. The driving force for separating the part is gravity and the pressure difference between the reactor 15 and the inlet pressure of the pump 19. If necessary, the annulus 28 may be operated under vacuum to assist in the removal of the liquid reducing agent metal, or the pressure in the vessel 25 may be increased while the reducing agent metal is drained. Good. After sufficiently extracting the liquid metal from the filter 27 by the above-described method, the PCV valve 89 is closed and the other valve 93 is closed to isolate the container 25, and then the valve 93 leading to the vacuum pump 95 is opened to open the container 25. A vacuum state is formed in the interior 26 of the chamber. A heated fluid (liquid or vapor, such as Na vapor) is directed to the heat exchanger plate 32 to boil the remaining reducing agent metal and produce a filter cake. The temperature of the container 25 is raised enough to evaporate the remaining liquid metal reducing agent 18 in the container 25, and this is withdrawn from the conduit 42 to the condenser 45. The conduit 42 needs to be relatively large in diameter to allow rapid drainage from the interior 26 of the container 25. Since the pressure drop between the container 25 and the condenser 45 during evaporation of the reducing agent metal 18 is small, the specific volume is large and mass transfer is small, thus requiring a large diameter conduit. Boiling of the reducing agent metal on the shell side is realized by heat exchange with the heating fluid on the tube side.

  The vessel 25 is further maintained to maintain the squeezed liquid in the annulus 28 at a temperature sufficient to easily flow and / or to assist in evaporating excess reducing agent metal from the interior 26 of the vessel. In some cases, the annular heat exchanger 29 is operated to supply heat. After removing the liquid metal reducing agent vapor from the interior 26 of the vessel 25, the filter cake is left from the slurry 20. The appropriate valve 93 is closed and the vacuum pump 95 is isolated from the system.

  A heat exchanging plate 46 is disposed in the condenser 45 for cooling the reducing agent metal vapor introduced therein. As described below, the cooling system 60 is operated in a closed loop and is maintained at a temperature that is sufficiently low that the reductant metal vapor introduced into the condenser 45 condenses and flows out of the condenser. The cooling system 60 includes the cooler 65 and the pump 62 as described above. The coolant exits cooler 65 and passes through line 114, which enters heat exchange plate 46, leaves line 115, and leads to line 116 that interconnects head tank 62 to cooler 65. As can be seen from the schematic of FIG. 1, the heating system 50 and the cooling system 60 may be maintained separately or mixed together, so that the heat exchange fluid used in the systems 50 and 60 is the same, May be different.

  Both vessel 25 and condenser 45 are operated for at least part of the time under a protective atmosphere of argon or other suitable inert gas from argon source 85 and the pressure is monitored by transducer 86. At this time, the inert gas (argon) supply source 85 is connected to the condenser 45 by a line 117, and the condenser 45 communicates with the container 25 by an oversized conduit 42. Further, as can be appreciated, each of the heating system 50 and the cooling system 60 is provided with their own pumps 53 and 63, respectively. As suggested in the schematic diagram of FIG. 1, heating and cooling fluids are preferred because of its low melting point NaK, but this is not essential, and as disclosed, the alternative is either liquid or vapor phase However, it may be the same as the possible reducing agent metal.

  What remains after sufficient removal of reducing agent metal 18 from slurry 20 via filter 27 and conduit 42 is a combination of titanium product in powder form and the salt produced during the exothermic reaction in reactor 15. The resulting dried cake has a smaller volume than the introduced slurry product 20, so that when the movable bottom closure 30 is opened, the dried cake falls from the filter 27 to the collection vessel 35, so that the inclined bottom wall 36 causes the salt and titanium combination to fall to crusher 38. If the cake does not easily fall off spontaneously, various standard vibration generating mechanisms or cake crushing mechanisms may be used to assist in transferring the cake to the collection vessel 35. The illustrated collection container 35 is maintained under an inert atmosphere at approximately atmospheric pressure, and after the cake has passed through the outlet 40 through the crusher 38, the cake travels downward through the valves 39 onto the conveyor 70. Downstream of the valve 39 is a cake spreader or baffle 71 that disperses the cake, which when in contact with a mixture 77 of inert gas (preferably argon) and oxygen flowing countercurrent to the product direction, The titanium powder is passivated and cooled. Although the conveyor 70 is positioned horizontally in FIG. 1, it is convenient to tilt and move the conveyor upward as a safety measure if excess reductant metal does not flow toward the water wash because the closure 30 does not function. It can be. In addition, it may be cost effective to have the product washer at the same level (or horizontal position) as the separator.

  Cooling and passivation is achieved in cooler 79 by a blower 75 that blows the cooled argon and oxygen mixture through conduit 121 to the product. In order to minimize the amount of oxygen used in the passivation process, the countercurrent flow of argon and oxygen to the product generally has the highest oxygen concentration because it is in contact with the already passivated and cooled titanium. You can see from the figure. Oxygen is led from the oxygen source 76 to the system through valve 93 and line 122, and this oxygen is typically maintained at a concentration of about 0.1 to about 3 weight percent. Thereafter, the passivated titanium and salt mixture is fed to a cleaning system (not shown). Various flow meters 81 are placed throughout the system as needed, as are the pressure control valve 89 and pressure transducer 86. A filter backwash valve 91 is arranged so that the filter 27 can be backwashed when the filter 27 is clogged or when other backwashing is required. Standard engineering equipment such as valves 93, vacuum pumps 95 and pressure transducers 86 are arranged as needed. Reference numeral 100 is used to indicate that a parallel system equivalent or similar to all or part of the illustrated system 10 can be operated simultaneously or sequentially.

  In the Armstrong process, the production of metal, alloy or ceramic is continuous as long as the reactants are fed into the reactor. The present invention provides a separation system, apparatus and method that can be quickly switched and separated by appropriate valve operation to be continuous as required, whether continuous or sequential batch processing. An object of the present invention is to provide a separation apparatus, system and method capable of operating the reactor 15 continuously or economically in an industrial plant. In order to operate the plant economically, it is important to shorten the distillation time in the vessel 25, and the exact size, number and configuration of the separation and production systems used are determined by the economy. Although described with respect to Ti powders, the present invention applies to the separation of any metals, their alloys or ceramics produced by the Armstrong process or other industrial processes.

  Although the heating mechanism shown is by fluid heat exchange, the heater may be electrical or other equivalent means, all of which are incorporated herein. The bottom closure 30 is shown as a hinge type and is commercially available. However, the closure 30 may be clamped when closed and may be hydraulically moved to the open state, but a sliding closure such as a gate valve may also be utilized and is incorporated herein. Although the reactor 20 is shown separated from the vessel 25, the present invention includes, but is not limited to, engineering changes within the knowledge of the art, such as incorporating the reactor 20 into the vessel 25. Although not shown in FIG. 1, it is contemplated that the slurry can be agitated when forming the cake on the filter and that the cake can be crushed to facilitate distillation and / or transport. Although the container 35 will be described in one embodiment, the container 35 can be easily designed as a pipe or the like. The crusher 38 may be installed in the container 25 or in the middle between the container 25 and the container 35. Further, the cake formed on the filter 27 may be crushed before, during or after removing the liquid metal therefrom. Similarly, for an inert environment, the present invention encompasses not only inert gases, but also vacuum (or reduced pressure) conditions. An important feature of the present invention is that the containers 25 and 35 are separated so that each environment of the containers 25 and 35 is maintained separately. In this way, oxygen does not contaminate any container.

  In one embodiment, a reactor 15 that produces 2 million pounds of titanium powder or alloy powder per year generally requires two containers, each 14 feet high and 7 feet in diameter, with appropriate valves. Thereby, the reactor 15 can be operated continuously, and when one container 25 is filled, the slurry product from the reactor can be automatically switched to the second container 25. The filling time of each container 25 is the same as or somewhat longer than the time of liquid removal, distillation and discharge of the container 25.

  Changing the production rate of the reactor 15 only requires engineering calculations on the size and number of vessels 25 and associated equipment and separation systems. The invention as disclosed allows for the continuous production and separation of metal or ceramic powders, using containers 25 available in two or up to three for each reactor 15 according to the disclosed embodiments. Continuous separation is possible. In multiple reactors 15, the number of vessels 25 and associated equipment is probably 2-3 times the number of reactors.

  2 to 4, a system 10A for continuously treating a liquid metal slurry containing particulates is disclosed. In this description, powder and granules are used interchangeably. More specifically, the system 10A includes a reactor 11 (eg, but not limited to a reactor of the type shown in the Armstrong process), which includes a nozzle 12 that flows through liquid metal and a housing 14 that surrounds the nozzle. Have The gas inlet 15 functions to introduce gas from the source 16 into the liquid metal, thereby causing an exothermic reaction as described in the Armstrong patent. The product of the exothermic reaction is a slurry of a liquid reducing agent metal (such as sodium), in which particles of the generated element or alloy (such as titanium or its alloy) are dispersed, and a reaction product from a gas (In the case of sodium and titanium tetrachloride, it may be a combination of sodium chloride or chloride salts). Slurry is introduced from the reactor housing 14 through the outlet 18 and into the receiving vessel 20. The receiving container 20 has a dome portion 21 and a cylindrical portion 22 near the top thereof, and the cylindrical portion 22 terminates at a truncated cone portion 23, the truncated cone portion 23 has a discharge port 25 at the bottom thereof, and an annular flange 26. Terminate at The motor 30 can be attached to the top of the container 20 in a state where it is connected to an output shaft 31 having a stirrer 32 at the bottom of the cylindrical portion 22 or the truncated cone portion 23 as shown in the figure for the purpose described later.

  In particular, as shown in FIG. 3, an indexing filter (or filtration) system 35 is in communication with the container 20, and more particularly includes a housing 36, the housing 36 having a top 37, an opposing top. It has a cylindrical side wall 38 with an aperture 39 and an opposing lower aperture 41. The housing 36 also includes an outlet 43 for purposes described below, the outlet 43 having a conduit 44 extending therefrom.

  The indexing drive 45 includes a motor 46, and the motor 46 has an output shaft 47. The shaft 47 is coupled to a clutch mechanism 48 connected to a mandrel 49, and the end of the mandrel 49 is supported by a bearing 51. An axial aperture 49A is provided on the cylindrical wall 38 to accommodate the mandrel 49.

  An indexing disk 55 is rotatably mounted on a mandrel 49, which has a plurality of longitudinally spaced chambers 56 therein, with six chambers shown for illustrative purposes.

  A collar 60, preferably a metal wedge wire, but not essential, is located in the outlet conduit 65 and is maintained in sealing (or sealing) contact with the disk 55 via a spring and pin arrangement 62 (Or an annular member) 61. The chambers 56 on the disk 55 are also in contact with the collar and spring and pin arrangements that communicate with the inlet conduit 63 to provide a seal arrangement for each chamber as each chamber 56 rotates about the mandrel 49. ing. As shown in FIG. 3, there is a T-shaped conduit 66 with a flange and seal 67 connecting the outlet 25 of the container 20 to the indexing disk 55, and a seal flange 26A (FIG. 2) is provided to provide a conventional seal (FIG. (Not shown) provides a suitable connection between the container 20 and the indexing filter system 35.

  A consolidation ram assembly 70 is attached to the housing 36 of the index filter system 35 and includes a piston rod 71 to which a piston 72 is attached. The piston rod 71 is surrounded by a bellows seal 73 and is connected at one end to a suitable drive or motor assembly 74 to move longitudinally away from and away from the chamber 56 as described below.

  A discharge ram assembly 80, similar to the consolidation ram assembly 70, is attached to the housing 36 that includes a similar piston rod 82, bellows seal 83, and drive motor 84. In FIG. 3, the discharge ram assembly 80 is shown rotated for clarity, but as will be well understood by a skilled technician, the chamber 56 is positioned within the disk 55 during indexing. It may be placed anywhere around the housing 36 to be used. In addition, the system 10A of the present invention may include more than one consolidation ram assembly and more than one discharge ram assembly, each version being a design choice and knowledge of the art. Is within the range. The discharge ram assembly 80 further includes a collar 86 and springs and retaining pins 87, similar to the compaction ram assembly 70, for purposes described below, the discharge ram assembly 80, the indexing disk 55, and the outer containment tube or conduit 91. To ensure a seal with the outlet conduit 90 surrounded by

  A cake crusher 93, which may be in the form of a stationary grid or a flexible member, is placed at the end of the distillation system 95 for purposes described below.

  A distillation system 95 is connected to the outlet conduit 90 of the index filter system 35 and comprises a longitudinally extending conveyor 96 in heat exchange relation with the heat exchanger 97 in a container 98 having a heat exchanger 97. . The distillation system 95 is in communication with the condenser assembly 100 by one or more tubes 101 extending from the container 98 to the condenser container 103, although the condenser container 103 is shown as an elongated container for purposes of illustration. It will be appreciated that it may be of any predetermined size or shape. The condenser container 103 is also connected to the outlet 43 of the housing 36 by a conduit 44. The conduit 102 communicates between the condenser assembly 100 and the liquid metal source 105, which is in the form of a container to which a distillation vacuum pump 106 and an outlet pipe 107 are connected. Pump 108 pumps liquid metal from source vessel 105 through conduit 109 to liquid metal storage tank 115. The tank 115 is also filled with liquid metal from the head tank 110 that communicates with the outlet conduit 65 from the index filter system 35 (the head tank 110 is in communication with the storage tank 115 by a conduit 113). As will be described later, if it is necessary to supply heat to or remove heat from the liquid metal exiting the index filter system 35, the heat exchanger 112 is in heat exchange with the outlet conduit 65. Good.

  A vessel 120 is disposed in communication with the distillation system 95 and comprises a valve 121, the vessel 120 is in communication with a pump 122, and the pump 122 is in communication with a vessel 125 with a valve 126 at the bottom or a lock hopper. . The container or lock hopper 125 communicates with the passivation system 130 via a valve 126 that includes a containment container 131 and a conveyor 132 that communicates with a gas inlet conduit 133 and a gas outlet conduit 134 that communicates with a pump 135. . Passivation system 130 has an outlet 136, all of which are described below.

  The operation of the system 10A is as follows. The gas source 16 is brought to the temperature of the boiler (which is to be contained in the container 16) and transferred via a conduit or gas inlet pipe 15 to a nozzle 12 through which a reducing metal such as sodium flows. Sodium is supplied from the head tank 110 or the supply source container 105. It will be appreciated that these containers may be single or divided into several, which is the scope of knowledge in the art when designing the actual combination of parts (or parts) in the system. Is within. The liquid metal pump 105 supplies a continuous flow (or stream) of liquid metal to the nozzle 12 and regulates the amounts of liquid metal and gas to maintain the reactor 11 at a predetermined, typically low, about 400 ° C. temperature. Various temperatures can be selected as the operating temperature, but currently about 400 ° C. is preferred. Similar to the examples shown in the Armstrong et al. Patent incorporated herein by reference, the reaction product in the reactor 11 contains excess sodium, sodium chloride particles and titanium particles. Of slurry. This slurry flows through outlet conduit 18 to receiving vessel 20. The material temperature at this time is still close to the outlet temperature from the reactor 11 (eg, can be about 400 ° C.). When the stirrer 32 is operated by the motor 30 in the container 20, the slurry is stirred in the container. The slurry exits the container 20 through its outlet 25 and enters the index filter system 35.

  By gravity, the slurry entering the indexing filter system 35 enters the T-shaped connector 66, then enters the inlet conduit 63, flows through the filter 60 to the outlet conduit 65. As liquid sodium flows through filter 60 (which can be, for example, a 125 micron wedge wire filter), the solid (or solids) concentration increases as liquid sodium is withdrawn. Actuation of the compaction ram assembly 70 advances the piston 72 into the chamber 56, compressing the material in the conduit 66, thereby squeezing the liquid metal out of the filter 60 and eventually squeezing most of the liquid metal To form a cake which remains what can be classified as wet cake particulate salt and particulate titanium. This cake has sufficient integrity to keep its shape, but at the same time still contains some (or a small amount) of liquid metal. As shown, the liquid metal exiting the index filter system 35 through the outlet conduit 65 is then recycled to the head tank 110 and transferred back to the nozzle 12 of the reactor 11 by the pump 108. After compression by the compaction ram 70, the motor 74 pulls back the piston 72 and rotates the index disk 55 by the index drive mechanism 45 to advance the next chamber 56 to a predetermined position for a new operation. As can be seen, the inlet conduit 66 is connected to the container 20 by gravity, so more slurry enters the system as soon as the compaction ram 70 is pulled back. Since the disk 55 is rotated immediately after the ram is pulled back, after consolidation, the slurry material does not enter the chamber 56 until the next chamber is in line with the consolidation ram 70, and the next chamber is in line with the consolidation ram 70. The chamber 56 is filled with slurry and then compacted or compressed.

  When the discharge ram assembly 80 is aligned or aligned with another chamber 56 of the indexing disc 55 and the chamber 56 having the consolidated or compressed material therein is aligned with the discharge ram 80, the piston 82 moves the cake in chamber 56 to distillation system 95.

  As shown in FIG. 3, a plurality of seals 61 and 86 containing liquid metal are provided in a suitable conduit and in its restricted path. However, the seal is not necessarily perfect in practice, and the sealing mechanism in the conduit is intended to provide a seal against liquid metal, but it is inevitable that some leakage will occur, as described below. It is collected in housing 36 for further recycling and exits outlet 43 and conduit 44 to flow to condenser assembly 100. Although one compaction ram assembly 70 and one discharge ram assembly 80 are shown, the inclusion of more than one compaction and / or discharge ram assembly 70, 80 is well within the knowledge of the art.

  Particles from the cake are heated by a heat exchanger 97 in a distillation system 95. The heat exchanger 97 may be by conduction, convection, induction heating, or any other suitable industrial method of heating the powder or particles that are conveyed by the conveyor 96 through the cake crusher 93 to the container 120. Cake crusher 93 is shown schematically, which may be a fixed series of wires or various other mechanical mechanisms that crush the compacted particulate material into a loose brittle material. Liquid metal evaporated in distillation system 95 is collected and sent to condenser assembly 100 and container 103 through conduit 101. The container 103 is maintained at a temperature low enough to condense the liquid metal vapor into a liquid, which is transferred to a reservoir such as in the head tank 110 or the like. As described above, the liquid metal in tanks 105 and 110 is eventually recirculated to reactor 11 and more specifically to nozzle 12 by pump 108. A valve 121 exists between the container 120 and the container or lock hopper 125. In addition, the pump 122 communicates with the container or lock hopper 125 to ensure that steam does not flow back into the system 10, and the system can be used when the lock hopper 125 needs to be isolated by actuation of valves 121 and 126. Can be empty. The particulate material from the lock hopper 125 is transferred to the passivator 130 while supplying the passivating gas or liquid from the gas or water inlet or conduit 133, and more specifically to the conveyor 132 moving within the containment vessel 131. Transfer. As shown, the particles move in a countercurrent direction relative to the passivating material, but this need not be the case. Preferably the passivating fluid is a gas containing a low proportion (eg 0.2% by volume) oxygen and an inert gas such as argon. The passivated material is then transferred from the outlet 136 to the cleaning and drying system 140. If desired, the passivating fluid is drained by pump 135 and conduit 134 and recycled.

  Referring to FIG. 5, another aspect of the present invention is shown, wherein like numerals apply to like members. The main difference in the embodiment of FIG. 5 is that the indexing disc 55 and therefore the indexing filter system 35 are arranged horizontally rather than vertically, so that when the slurry is withdrawn from the bottom of the container 20, the liquid reducing metal is removed. Consolidation is performed after the filter 60 is extracted and the indexing disk 55 is rotated. After further rotation, the discharge ram assembly 80 is activated to transfer the cake to the distillation system 95. Except for the placement of the indexing disk 55 (which requires indexing during slurry recovery and consolidation), the operation of the two systems is the same.

  Assuming that a single armstrong reactor can produce products such as titanium or titanium alloys (eg, titanium, 6% aluminum and 4% vanadium) at 2,000,000 pounds per year, chamber 56 is 10 inches in diameter. And can be 6 inches long. Based on the calculation that the slurry and / or gel produced by the Armstrong process is about 22-23 solids weight percent, each disk 55 preferably has six such chambers. Based on the chamber, the indexing disc 55 will be indexed approximately every 11 seconds. Different chamber volumes or number of chambers require different indexing times, which is within the knowledge of the art. In this embodiment, to ensure that the cake removed by compaction ram assembly 80 has a solids composition of about 1.5 inches thick and between about 64-65 wt%, the material in chamber 56 is 1 / Compress to 4.

  Referring now to FIG. 6, a schematic diagram of various methods and resulting products (or products) according to the present invention is disclosed. The “reduction” frame is an Armstrong method in which an exothermic reaction takes place under control using the configuration taught above and in the Armstrong et al. Patent incorporated herein. Separation involves passivation as described herein above. The passivated material is then sent to a cleaning and drying system 140 where the salt product (in this example sodium chloride) is removed from the product particles (in this example titanium or titanium alloy powder). Referring to FIG. 6, this schematic can melt the powder to form an ingot or other solid product by various methods such as casting, or utilize, for example, pressure It can be sent to a powder metallurgy process including, but not limited to, cold isostatic pressing, hot isostatic pressing, etc. to densify the metal powder to a predetermined shape and density. The product can also be produced by cold spraying the metal powder as a gas jet, or lasering the metal powder, or spheridizing the metal powder with a plasma. As is well known in the art, the metal powder can be in the form of a foam (or foam) and then pressed and sintered to form a stable metal foam. The powder can be pressed against a mandrel and then rolled to form a thin tube. Furthermore, a powder product can be formed by drawing or extruding metal powder. If it is necessary to change the morphology (or morphology) of the product, for example packing fraction (or filling rate), average size or size distribution, the wear mechanism can be used to change the morphology of the powder containing the packing fraction, or The overall size distribution of the powder can be reduced.

  All these product manufacturing processes and the products formed thereby are intended to be included in the present invention when combined with the separation process of the present invention.

  The P trap is the pressure above the filter as the operation proceeds (assuming that the downstream pressure remains constant). Flow 2 is the flow rate of sodium (Na) and the V reactor indicates when product is formed. At t = 8420, sodium flow into the trap was started. The trap pressure was relatively constant until the reactor valve was opened and cake started to form, and remained the same as when Na was flowing through a clean filter (125 microns). The cake DP increased linearly until t = 8520 when the reaction speed started to drop because the nozzle was blocked by the subsonic operation of the nozzle. When the thickness of the cake after distillation was measured, it was 5 to 6 inches on average. The cake bottom was observed to be less dense than the cake top, and the measured cake density was 1.1 g / cc at the cake top and 0.73 g / cc at the cake bottom. Since the bottom is formed at a lower pressure, it is considered to be less dense. For example, DP is determined by the flow rate, and in this operation, the flow rate is 30 kg / min. Also, after finishing product production and continuing Na flow, the cake was observed to be more compacted (after t = 8505, the flow decreased while the pressure increased). Behold). Prior to stopping Na flow, DP was 22 psig at maximum, compared to 18 psig at the end of production of sufficient product (see FIGS. 1 and 2, see FIGS. 7 and 8).

  Heat was supplied to the cake area, the vapor was removed, and sent from the top of the trap to the external first condenser, and by distillation to a second condenser through a wedge wire filter. A total of 5.9 kg Na was removed from the cake during the distillation and after distillation the cake weighed 3.4 kg. It was found that 3.8 kg of 5.9 kg was condensed in the second condenser (see FIG. 9).

  In another Nutsche operation, the trap was designed to allow distillation through the filter to the bottom of the trap in order to maximize the trap diameter for moving the steam. This trap also had a standard 1 inch line leading to the first condenser (see FIG. 10). Heat was concentrated on the cake while keeping the bottom of the trap cool to support the Na condensate. After distillation, 1.6 kg of Na was transferred to the first condenser, 1.3 kg of Na was distilled to the bottom of the trap, leaving 3.1 kg of cake composed of titanium and NaCl.

  However, crushing the filter cake has been found to significantly reduce the distillation time and rate of liquid metals such as sodium. Using a crushing bar or any other mechanical means (such as a moving finger or mixer), the first part of the vacuum distillation is from 40,000 to 50,000 seconds (11 to 14 hours) to 20,000 to 30,000. Decrease significantly in seconds (about 6-8 hours). The second part of the distillation (the part where the temperature and pressure drop, called the tail) was not affected by the crushing of the filter cake.

  By using an inert sweep gas such as argon heated preferably between about 500 ° C. and about 800 ° C. during the second distillation or tail, the time required for distillation of the reducing agent metal (sodium) is reduced. It was also found that the time can be shortened from about 40,000 to 50,000 seconds to about 10,000 seconds (about 3 hours). This is a significant advance over conventional methods. Reduce distillation time from about (22 or 28) hours to about (9-11) hours by using either one of the above methods or a combination of filter cake crushing in combination with a sweep with an inert gas. be able to. This is extremely important in plant design by simplifying the design and reducing collection tanks, valves, piping and other related equipment.

  After vacuum (or reduced pressure) distillation is clearly complete, it becomes practically difficult to remove any trapped remaining reducing agent metal (sodium). Although it seems obvious that the filter cake is put into water and the remaining salt (NaCl) is washed away from the titanium powder, the reducing metal (sodium) trapped in the filter cake is a problem, which is A significant explosion occurs when combined with. In fact, a mixture of sodium liquid and water will cause an explosion with an energy greater than an equivalent amount of TNT.

With respect to producing Ti by subsurface reduction of TiCl ₄ with Na, the filter cake is made small (eg, less than about 5 centimeters in diameter, preferably about 2 to about 5 centimeters in diameter, during or after sodium distillation. By crushing, all trapped Na can be treated without significant damage to the equipment or injury to the person if proper consideration is given to the equipment design and appropriate safety measures are in place. It has been found that particles or lumps can be made apparently small enough. After distillation, the filter cake is brittle and easily crushed. Produces various elemental metals and alloys described in the above-mentioned patents (especially sodium or other alkali metals are used as reducing agents) to the extent that large quantities of pulverized filter cake can be washed without fear of explosion The distillation time required for is greatly reduced.

  Alternatively, the entire distillation may be heated at positive pressure (eg, but not limited to psig), heated or hot inert gas (eg, but not limited to about 500 ° C. to about 800 ° C.). It was found that by evaporating and then cooling, the evaporated liquid metal (eg, but not limited to Na) can be condensed. The cooled liquid metal is then returned for further use.

  In summary, the present invention relates to a mechanism and method for reducing the distillation time of a filter cake obtained by the method described in the aforementioned patent. The filter cake can be crushed by a vibrating or moving mechanism in the filter cake area or by a stationary mechanical bar or member or other suitable mechanism in the filter cake area. In order to significantly reduce the distillation time of the liquid metal in the filter cake, a vacuum or non-vacuum inert sweep gas can be used alone or in combination with the above-described method of crushing the filter cake during distillation.

  Referring to FIG. 11 of the drawings, a transfer mechanism 10E is shown, comprising a double wall conduit including an outer conduit wall 11 with a liquid outlet 12, and an end wall 13, which wall 11 is preferably cylindrical. But not essential. The interior of the cylindrical wall 11 is an inner tube or conduit 15 having a solid portion 16 and a portion 17 provided with an aperture and may be any suitable size mesh. The inner tube or conduit 15 may be cylindrical as shown in FIG. 1 or conical as described below, with the inner conduit 15 having a discharge end 18 that opens to the vacuum chamber 25. And has an inlet end 19 that opens to a container or vessel 20 that communicates with a reactor as described in the Armstrong patent incorporated herein by reference.

  A feed screw 30 is disposed in the inner conduit 15 and has a rotatable shank 31 with a conical thread 32 disposed as is well known in the art. The threads 32 can have a constant or variable pitch. The pitch is a distance between adjacent threads, and the variable pitch is preferably a stepped (or gradually changing) pitch in which the pitch decreases from the container 20 toward the container or the container 25 for the purpose described later.

  In a preferred but not limited aspect of the present invention, the transfer mechanism 10E is used with a material produced by the Armstrong process. More specifically, for purposes of illustration only, the slurry described herein is a combination of liquid sodium, sodium chloride particles, and titanium and / or titanium alloy particles. As described in the Armstrong patent, this can produce a variety of metal and non-metal products, and the invention is not limited to any particular product produced by the Armstrong process. And, of course, are not intended to be limited to the preferred products described herein.

  In any case, a container or container 20 which is preferably operated under an inert atmosphere or under vacuum has a slurry of the particles described above in it, the slurry enters part 19 of the inner conduit or tube 15 and feed screw 30 Is rotated by the rotation of the shank 31, the slurry moves along the feed screw from left to right as shown in FIG. Since the feed screw 30 in FIG. 11 has a stepped pitch (ie, the threads 32 are closer together so that the pitch decreases from left to right), the material is transferred from the container or container 20 to the container or container. As it moves into the container 25, it is concentrated. Furthermore, because the portion 17 of the conduit or tube 15 is apertured or porous, liquid sodium is withdrawn therefrom for further processing and exits through the outlet 12. Thus, as the slurry is transferred from the container or container 20 to the container or container 25, the liquid is withdrawn so that the slurry becomes more concentrated and the density decreases as the pitch between adjacent threads decreases. Rises.

  The phenomenon is expressed in another way as follows. The volume between adjacent threads and cylinder or tube wall 16 decreases as material is moved from container or container 20 to container or container 25 by feed screw 30. By the time the slurry is concentrated to reach part 16 (the part 16 without any gaps in the inner tube or conduit 15), a seal is established between the container 25 and the container 20 containing the slurry from the reactor. The formation of a seal by the transfer mechanism 10 is an important aspect of the present invention. Because, as described in the Armstrong patent, separating liquid metal and salt from the desired particles of ceramic or metal alloy can include distillation in a vacuum chamber or vessel 25, and the Armstrong reactor itself is argon This is because the container can be inactivated by the above. Thus, it is possible to operate continuously between two containers without having to shut down one of the containers during transfer or damaging the protective atmosphere in the container 20 or the vacuum in the container 25. Therefore, it is important to form a seal between two containers or containers.

  With reference to FIGS. 12 and 13, another embodiment of the present invention is shown. It also has the essential feature that the volume between adjacent screw threads and the container or housing in which the feed screw is located decreases from container 20A to container 25A. As can be seen from FIG. 12, the transfer mechanism 10F has a housing 15A having a conical shape, and the screw 30 therein may or may not be a stepped pitch screw. The screw threads of the embodiment shown in FIG. 12 need not be close to each other, i.e., as the material moves from left to right and from container 20A to container 25A, adjacent threads and housings. It is not necessary that the pitch is reduced in order to reduce the volume of material between the walls. However, for engineering reasons, it may be advantageous to use both conical inner housings 15A with or without stepped pitch screws 30A.

  Referring to FIG. 13, another aspect 10G of the present invention is shown, in which the shank 31B of the screw 30B has a conical shape, with the larger end of the cone (or conical member) being The pitch between the threads 32B adjacent to and adjacent to the container 25B is constant or decreases. In either case, the volume of the area between adjacent threads and the inner container 15B decreases as the material moves from container 20B to container 25B.

  Although the present invention has been described with reference to an inert container and a vacuum container, the present invention includes moving and concentrating material from one container to another without compromising the environment of either container. . These containers can be connected pipes or containers, and the environment can be a vacuum, an inert atmosphere or otherwise. The heart of the present invention is the transfer of solids (or solids) from one environment to another while forming a seal between them to isolate one and the other from each other. Concentrate the solid at

  Referring to FIG. 14, there is shown a schematic diagram of a separation combining the above applications, illustrating another separation process, system and method relating to, but not limited to, the armstrong method described above. As with the systems, devices and methods described above, there are sources of halide and reducing agent metals that are introduced into the reactor as described above, and by exothermic reaction, for example, metal powder, salt particles and excess Resulting in a slurry composed of a reducing agent metal. As taught in the Armstrong patent, the reactor is operated under an inert atmosphere and the resulting slurry is transferred to the first vessel. Since the separation process can include portions that are either positive pressure or negative pressure, or both, as described below, the first vessel is also operated under an inert atmosphere and / or vacuum, ie, the first vessel is not pressurized. It has been activated. In order to allow continuous production without shutting down the first vessel or adding liquid metal (seasoning), the first vessel is prevented from being contaminated with oxygen during the processing of the slurry. Is very important, otherwise it is necessary to remove oxygen contaminants.

  There are various means of treating the slurry to remove unwanted components such as salt particles and excess reducing agent metal. However, any of them may be made up of either metal powder or a combination of metal powder and salt particles, moving excess excess reducing agent metal as a liquid or vapor or both from the first container, and wet (or Including leaving the cake in either a damp state) or a dry (or dry) state. There is a second container to maintain the integrity (or integrity) of the first container, which is a tank or pipe or any container operated under an inert atmosphere and / or vacuum. Well, the treated slurry (whether wet or dry, metal powder or a combination of metal powder and salt particles) is transferred for further processing and is inert from the deactivated container or container. It has a lock or valve or seal or plug mechanism so that the product can be transferred to an unstructured environment. As can be seen from the drawings, particularly FIG. 1, as described herein above, an apparatus is shown for heating the slurry in a first vessel to remove excess liquid metal as both liquid and vapor. Transfer the dried cake to a second inerting vessel for replacement. Agitation in the first vessel by mechanical or other means speeds up the distillation process and at the same time breaks the filter cake once it is formed, which is a further advantage. However, the cake can be crushed without significant changes as shown in FIG. 14, and the excess liquid reducing agent metal can be removed with an inert hot sweep gas, which is sufficient. When hot, not only the excess liquid reducing agent metal but also salt particles are evaporated, leaving a metal powder that is transferred to a second container (which may be a pipe) and optionally passivated via a locking mechanism Package (or bag) in an inert environment for transport without delivery to the station or passivation. Thus, as will be appreciated, the slurry can be treated by heating to obtain the metal powder alone or in combination with salt particles using the first vessel.

  As shown in FIGS. 2-6, the first container in system 10A may include a sequential (or sequence) indexing separation system 35, in which the first container of FIG. This is in combination with a squeezed (or squeezed) cake, as described above, that is produced sequentially and sent to a second vessel or distillation system 95). The second container or container of FIG. 14 can be arranged horizontally as a distillation system 95 in the system 10A shown in FIGS. 2-6, with or without a conveyor inside, all related to the technology. It depends on engineering reasons within the knowledge. As shown in FIG. 14, the material in the second container (which is now dry and can be either metal powder alone or a combination of metal powder and salt) can be used for further processing if necessary. The method is moved from a deactivated state of the second container to another environment via a lock, as shown, or via a seal or valve or any equivalent mechanism, and the process involves passivation and subsequent It can include simply packaging into a flushed or inactivated shipping container. The locking mechanism may be the variable pitch screw of FIG. 11 or a modification thereof shown in FIGS. 12 and 13, or any other suitable locking mechanism, such as but not limited to a gate valve.

  Thus, as will be appreciated, by treating the slurry in an inert atmosphere or vacuum or combination thereof in the first vessel, depending on the selected separation conditions, the metal powder or combination of metal powder and salt Can produce wet or dry cake. Heater (either internal or external or both) and / or hot inert sweep to remove material (either excess reductant metal alone or a combination of reductant metal and salt) from the first vessel The gas may be used at a pressure that may be either positive or negative pressure, or a combination of positive and negative pressure with a heater or sweep gas or both. Depending on what is transferred from the first container, a hot inert sweep gas or other mechanism may be applied to the second container to isolate the metal powder from unwanted components. It is then transferred to a conveyor or another mechanism for further processing or handling. As described above, passivation with an inert gas with a small amount of oxygen after cooling may be applied, followed by water washing and drying prior to packaging. Alternatively, if both the reducing agent metal and the salt are removed in the first container and / or the second container, washing and / or passivation may not be required, resulting in more oxygen contamination and / or expense. make low.

  Having described what is considered a preferred embodiment of the invention, it will be understood that various changes in detail may be made without departing from the concept of the invention and without sacrificing any of the advantages. .

1 is a schematic diagram of a separation system of the present invention. 1 is a schematic diagram of a system for implementing the method of the present invention. FIG. 3 is an enlarged schematic view of the product filtration disk portion of the system shown in FIG. 2 shown in a longitudinal cross-sectional view. FIG. 4 is a horizontal sectional view of the container shown in FIG. 3. 3 is another embodiment of the system shown in FIG. FIG. 3 schematically illustrates various processes and products produced by or from powders separated from slurries according to the present invention. It is a graph of the pressure rise with respect to time at the time of driving | running with Nutsche of a flat plate filter. Various temperature data with respect to time and pressure are shown. Fig. 3 shows a schematic of a filter trap for the above example. Fig. 4 shows a schematic of another embodiment of the filter trap of Fig. 3; FIG. 2 is a schematic diagram showing an embodiment of two containers and a transfer mechanism between them. 2 is a schematic of another embodiment of the present invention. FIG. 6 is a schematic view of yet another embodiment of the present invention. FIG. 14 is a schematic diagram of a separation system incorporating the features of FIGS.

Claims (91)

  A method for separating metal powder from a slurry of liquid metal and metal powder and salt, wherein the slurry is introduced into a first vessel operated in an inert and / or vacuum environment to separate the liquid metal from the metal powder and salt. Mainly leaving the substantially non-existent salt and metal powder of the liquid metal, transferring the non-existent salt and metal powder of the liquid metal to a second container operated in an inert environment, and thereafter Treating the salt and metal powder to produce a passivated metal powder substantially free of salt and liquid metal.   The method of claim 1, wherein the inert environment is an argon atmosphere.   2. The method of claim 1, wherein prior to passivation, the salt and metal powder are crushed to form a mass having a diameter of about 5 centimeters or less.   The method of claim 1, wherein liquid metal is separated from the salt and metal powder as both liquid and vapor in a first vessel.   5. The method of claim 4, wherein the liquid metal vapor from the first vessel is transferred to a condenser operated in an inert environment.   The method according to claim 4, wherein the liquid metal is an alkali or alkaline earth metal or a mixture thereof.   7. A process according to claim 6, wherein the salt is a halide.   The method according to claim 7, wherein the metal powder is titanium or a titanium alloy.   The method according to claim 8, wherein the titanium or titanium alloy is CP1 to CP4.   The method of claim 9, wherein the metal powder has a diameter in the range of about 0.1 to about 10 microns.   The method according to claim 1, wherein the passivation is performed on a conveyor.   The method of claim 11, wherein the metal powder is continuously cooled and passivated.   The method of claim 1, wherein the environment of the first and second containers is protected from oxygen contamination while producing a metal powder that is substantially free of salt and liquid metal.   A liquid metal formed using a liquid metal in excess of the required stoichiometric amount by introducing a vapor of a metal halide below the surface of the liquid metal to cause an exothermic reaction to form a salt and a metal powder; and A method of separating metal powder from a slurry of metal powder and salt, the slurry being introduced into a first vessel operated in an inert and / or vacuum environment, and liquid metal being filtered from the metal powder and salt and To evaporate to leave mainly substantially non-existent salts and metal powders of liquid metal, and to transfer liquid metal vapor to a condenser operated in an inert environment to produce additional metal powders. Converting liquid metal vapor to liquid for recycling, transferring substantially non-existent salt and metal powder of liquid metal to a second container operated in an inert environment, and thereafter The methods and the processing the metal powder comprises preparing a metal powder passivated substantially in the absence of salt and the liquid metal.   15. The method of claim 14, wherein the slurry is heated in the first container by contacting a heat exchanger that is inside the first container and through which the heat exchange fluid is pumped.   15. The method of claim 14, wherein liquid metal vapor from the first vessel is cooled by contacting a heat exchanger that is internal to the condenser and through which the heat exchange fluid is pumped.   15. The method of claim 14, wherein the first container is heated by both internal and external heat exchangers.   The method according to claim 14, wherein the slurry is introduced into the candle filter in the first container, and the liquid metal is allowed to flow out of the first container through the candle filter.   The method of claim 14, wherein the inert environment of the first and second containers is an argon atmosphere.   The method of claim 19, wherein the condenser is operated in an argon atmosphere.   15. The method of claim 14, wherein the environment of the first and second containers is protected from oxygen contamination while producing a metal powder that is substantially free of salt and liquid metal.   A liquid metal formed using a liquid metal in excess of the required stoichiometric amount by introducing a vapor of a metal halide below the surface of the liquid metal to cause an exothermic reaction to form a salt and a metal powder; and A system for separating metal powder from a slurry of metal powder and salt, wherein the liquid metal is filtered from the slurry, and the liquid metal is heated to evaporate the liquid metal from the salt and metal powder. A first inerting vessel in communication with the heater and filter to form a filter cake of the first, an inerting condenser in communication with the first vessel, receiving metal vapor and converting it to liquid metal, A second inerting container for communicating with the one container by a valve and receiving the filter cake therefrom, and a filter in or in communication with the second inerting container A crusher for crushing the cake, a cooling and passivation station for receiving the crushed filter cake, and a first and second by air during the transfer of the filter cake from the first container to the cooling and passivation station. A system comprising a valve mechanism intermediate between the first and second containers and between the second container and the cooling and passivation station to prevent contamination of the two containers.   23. The system of claim 22, wherein the heater in communication with the first passivation container is inside the first passivation container.   24. The system of claim 23, wherein a heater within the first passivation vessel is in communication with a source of heat exchange fluid that is optionally provided to the heater.   23. The system of claim 22, wherein the filter in communication with the first passivation container is inside the first passivation container.   The filter is a filter that forms an annular body with respect to the first passivation container into which the liquid metal flows, and is a conduit that communicates with the annular body to send the liquid metal from the first passivation container to the deactivated liquid metal reservoir. 26. The system of claim 25, further comprising:   23. The system of claim 22, wherein the first and second deactivation containers are deactivated with argon.   28. The system of claim 27, wherein the condenser is inerted with argon.   29. The system of claim 28, wherein the passivation condenser is in communication with an argon passivation reservoir for liquid metal formed from condensed metal vapor.   23. The system of claim 22, wherein the condenser is in communication with a source of heat exchange fluid that is optionally provided to the condenser.   23. The system of claim 22, wherein a valve intermediate the first and second passivation containers is adapted to hinge open to the second passivation container.   23. The system of claim 22, wherein the first and second containers are integrated.   A method of separating metal particles from a slurry of liquid metal and metal and salt particles, the slurry being filtered to form a cake of metal and salt particles with some liquid metal, cake And removing the liquid metal from the crushed cake, and then separating the metal and salt particles.   34. The method of claim 33, wherein the liquid metal is removed from the crushed cake by vacuum distillation.   34. The method of claim 33, wherein the liquid metal is removed from the crushed cake with a hot sweep gas.   36. The method of claim 35, wherein the hot sweep gas is an inert gas.   37. A method according to claim 36, wherein the inert gas is argon.   37. The method of claim 36, wherein the hot sweep gas is at positive pressure.   38. The method of claim 37, wherein the hot argon sweep gas is at positive pressure.   34. The method of claim 33, wherein the liquid metal is present in the filter cake at no more than about 10 times the weight of the metal particles.   34. The method of claim 33, wherein the liquid metal is an alkali metal or alkaline earth metal or a mixture thereof.   34. A method according to claim 33, wherein the liquid metal is Na or Mg.   34. The method of claim 33, wherein the metal particles are Ti.   34. The method of claim 33, wherein the metal particles are a Ti alloy.   34. The method of claim 33, wherein the salt particles are halides.   34. The method of claim 33, wherein the salt particles are chloride.   34. The method of claim 33, wherein the metal particles are Ti or Ti alloy and the salt is Na or Mg chloride.   48. The method of claim 47, wherein the liquid metal is Na and the salt particles are NaCl.   34. The method of claim 33, wherein the cake is broken into pieces having a diameter of about 5 centimeters or less.   34. The method of claim 33, wherein the cake is broken into pieces having a diameter of about 2 centimeters or less.   A method of separating metal particles from a slurry of liquid metal and metal and salt particles, the slurry being filtered to form a cake of metal and salt particles with some liquid metal, cake To remove liquid metal from the crushed cake, to separate metal and salt particles, and to prevent unacceptable explosions when in contact with water, before washing with water Sizing the method.   52. The method of claim 51, wherein the liquid metal is removed from the crushed cake by vacuum distillation or by a hot sweep gas.   53. The method of claim 52, wherein the hot sweep gas is argon.   53. The method of claim 52, wherein the hot sweep gas is at positive pressure.   54. The method of claim 53, wherein the hot argon sweep gas is at positive pressure.   53. The method of claim 52, wherein the liquid metal is Na or Mg and is present in the filter cake at no more than about 10 times the weight of the metal particles.   57. The method of claim 56, wherein the metal particles are Ti or a Ti alloy.   58. The method of claim 57, wherein the cake is broken into pieces having a diameter of about 5 centimeters or less.   59. The method of claim 58, wherein the cake is broken into pieces having a diameter of about 2 centimeters or less.   A transfer mechanism under vacuum between a first container and a second container for containing a liquid and solid slurry, a housing communicating with the first and second containers, and a substance from the first container to the second container And a screw having a plurality of helical threads along the longitudinal shank in the housing for transferring the volume between the adjacent screw threads and the housing. As the slurry enters the housing from the first container, the solids therein are concentrated as the slurry is fed toward the second container by the screw, while the concentrated solids are concentrated in the first container. A transfer mechanism wherein liquid is squeezed out of the slurry as the solids are concentrated until a plug is formed that seals the second container to one container.   61. The transfer mechanism according to claim 60, wherein the screw is a variable pitch screw.   61. The transfer mechanism according to claim 60, wherein the screw is a stepped pitch screw, the smallest pitch being closest to the second container.   61. A transfer mechanism according to claim 60, wherein the housing is substantially cylindrical.   61. The transfer mechanism of claim 60, wherein the housing is conical and has its smallest end closest to the second container.   61. The transfer mechanism of claim 60, further comprising a slurry of liquid metal and salt particles and ceramic or metal or alloy particles in the transfer mechanism.   66. The transfer mechanism according to claim 65, wherein the liquid metal is Na or Mg.   68. The transfer mechanism of claim 66, wherein the ceramic or metal or alloy particles are Ti or an alloy thereof.   61. The transfer mechanism of claim 60, wherein the housing is cylindrical and the screw is a stepped pitch screw, the smallest pitch being closest to the second container.   61. The transfer mechanism of claim 60, wherein the housing is conical, its smallest end closest to the second container, and the screw has a constant pitch thread.   61. The transfer mechanism of claim 60, wherein the shank has a diameter that increases toward the second container.   61. The transfer mechanism of claim 60, wherein at least a portion of the housing in fluid communication with the first container has a plurality of apertures.   61. The transfer mechanism of claim 60, wherein the plurality of apertures are meshes.   61. The transfer mechanism of claim 60, further comprising an outlet in the housing for separating liquid from the slurry through the aperture.   A transfer mechanism under vacuum between a first container and a second container containing a slurry of liquid alkali or alkaline earth metal or mixtures thereof, and a metal or alloy or ceramic and halide salt particles, A housing in communication with the first and second containers, and a screw having a plurality of helical threads along the longitudinal shank within the housing for transferring material from the first container to the second container; The volume between the adjacent screw thread and the housing decreases between the first and second containers, so that the slurry entering the housing from the first container is directed toward the second container by the screw. The plug in which the particles therein are concentrated as it is delivered, while the concentrated particles seal the second container against the first container Until formation, so that the liquid metal is squeezed out of the slurry as the particles are concentrated, the transport mechanism.   75. The transport mechanism of claim 74, wherein the screw is a stepped pitch screw, the smallest pitch being closest to the second container.   75. A transfer mechanism according to claim 74, wherein the housing is substantially cylindrical.   75. The transfer mechanism of claim 74, wherein the housing is conical and has its smallest end closest to the second container.   75. The transfer mechanism of claim 74, wherein the housing is cylindrical and the screw is a stepped pitch screw, the smallest pitch being closest to the second container.   75. The transfer mechanism of claim 74, wherein the housing is conical, its smallest end being closest to the second container, and the screw has a constant pitch thread.   80. The transfer mechanism of claim 79, wherein the shank has a diameter that increases toward the second container.   75. The transfer mechanism of claim 74, wherein at least a portion of the housing in fluid communication with the first container has a plurality of apertures.   82. The transfer mechanism according to claim 81, wherein the plurality of apertures are meshes.   75. The transfer mechanism of claim 74, further comprising an outlet at the housing for separating liquid from the slurry through the aperture.   84. The transfer mechanism of claim 83, further comprising a slurry of liquid Na, NaCl particles, and Ti particles or alloys thereof.   84. The method of claim 83, wherein the inner wall comprises a double-walled housing having an apertured portion and a gapless portion, an outer wall having an outlet, and a screw disposed within the inner wall. The transfer mechanism described.   A method of concentrating and transferring a slurry from one container to another while sealing the container, communicating between the containers, transferring the slurry from one container to the other while squeezing liquid from the slurry, Thereby increasing the solids concentration of the slurry until a plug is formed between the two containers, while transferring solids from the plug to the other container.   90. The method of claim 86, wherein the container is operated under an inert atmosphere.   90. The method of claim 86, wherein the container is operated under vacuum.   90. The method of claim 86, wherein the slurry comprises liquid metal and metal particles.   90. The method of claim 89, wherein the slurry comprises a liquid alkali or alkaline earth metal. 90. The method of claim 86, wherein the slurry comprises particles of liquid sodium metal and Ti or an alloy thereof.

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