SIMULTANEOUS DISTILLATION AND ALLOYING

20230083353 · 2023-03-16

Assignee

Inventors

Cpc classification

International classification

Abstract

A device for producing a target material from starting material comprises a chamber, at least one trough, at least a first heating element being configured to heat the chamber such that starting material is vaporized, and at least one collecting vessel being configured to receive a condensate that will constitute the target material. The device optionally comprises at least a first source of negative pressure or at least a first supply device being in connection with the chamber being configured to evacuate the chamber or to supply an inert gas to the chamber. The device further comprises at least one condensation device, wherein said condensation device is configured to condensate the vaporized starting material, whereby the condensate is formed, and/or at least a first gate device being in connection with the chamber such, that the starting material is introducible into the chamber via said first gate device.

Claims

1. A device for producing a target material, from starting material comprising: a chamber; at least one trough being provided in the chamber, wherein the trough is configured to receive the starting material; at least a first heating element, wherein the first heating element is configured to heat the chamber such that a starting material being received in the trough is vaporized; and at least one collecting vessel, wherein the collecting vessel is configured to receive a condensate that will constitute the target material, wherein the device further comprises at least one condensation device, wherein said condensation device is configured to condensate the vaporized starting material, whereby the condensate is formed.

2. A device for producing a target material, from starting material comprising: a chamber; at least one trough being provided in the chamber, wherein the trough is configured to receive the starting material; at least a first heating element, wherein the first heating element is configured to heat the chamber such that starting material being received in the trough is vaporized; at least one collecting vessel, wherein the collecting vessel is configured to receive a condensate that is formed upon a condensation of the starting material and which condensate will constitute the target material; at least a first source of negative pressure that is in connection with the chamber and that is configured to evacuate the chamber or at least a first supply device that is in connection with the chamber and that is configured to supply an inert gas to the chamber, and optionally at least one condensation device, wherein said condensation device is configured to condensate the vaporized starting material, whereby the condensate is formed; wherein the device further comprises at least a first gate device being in connection with the chamber such, that the starting material is introducible into the chamber via said first gate device.

3. The device according to claim 2, wherein the device is configured such, that the starting material is introducible into the chamber via said first gate device while the chamber remains evacuated or under an inert gas atmosphere.

4. The device according to claim 2, further comprising heated antechamber that is in connection with the chamber via the first gate device, wherein the antechamber is configured to receive and pre-melt the starting material and to transfer the pre-melted starting material into the trough via the first gate device. and wherein the device further comprises at least a second source of negative pressure that is in connection with the antechamber in order to evacuate the antechamber.

5. The device according to claim 2, further comprising at least a second gate device being in connection with the at least one collecting vessel, and wherein the condensate is removable from the at least one collecting vessel via said second gate device.

6. The device according to claim 5, further comprising a retrieval chamber that is in connection with the collecting vessel via the second gate device and with the first source of negative pressure or with the first supply device, and wherein the retrieval chamber is configured to extract the condensate from the collecting vessel.

7. The device according to claim 1, wherein the collecting vessel and the condensation device are formed separately from one another.

8. The device according to claim 1, wherein the condensation device projects from an upper wall of the chamber at least partially into an interior of the chamber, and/or wherein the condensation device is an integral or a separable part of the chamber.

9. The device according to claim 1, wherein the condensation device corresponds to a heat exchanger.

10. The device according to claim 1, further comprising at least one cover element, wherein the cover element is at least partially arranged above the collecting vessel with respect to a vertical direction and is configured to guide vaporized starting material that has condensed at an upper wall of the chamber back into the trough.

11. The device according to claim 10, wherein the cover element extends from a main body of the condensation device laterally outwards, or wherein the cover element extends from the upper wall of the chamber at least partially into the chamber; and/or wherein the cover element is arranged at an angle with respect to a vertical direction, and wherein the angle is about 90° or less.

12. The device according to claim 1, wherein at least part of an outer wall of the condensation device and/or of an inner wall of the chamber and/or an inner wall of the collecting vessel is coated with a coating, and wherein the coating is inert.

13. The device according to claim 1, further comprising a funnel element which is arranged above an inlet opening of the collecting vessel, wherein the funnel element is configured to guide the condensate into the inlet opening of the collecting vessel, and/or further comprising at least one sealing element which is arranged around an upper region of the collecting vessel, wherein the sealing element is configured to provide a sealing between the upper region of the collecting vessel and the chamber.

14. The device according to claim 1, further comprising a fourth heating element, wherein said fourth heating element is arranged in a lower region of the chamber and in vicinity to an upper region of the collecting vessel, and wherein said fourth heating element is configured to heat the upper region of the collecting vessel to a vessel temperature being above a melting point of the starting material and to heat a lower region of the collecting vessel to a vessel temperature being slightly above a melting point of the target material and/or a liquidus temperature of the target material.

15. The device according to claim 1, wherein the condensation device is made of a material that differs from a material the collecting vessel is made from, and/or wherein the chamber is made of a material that differs from the material the collecting vessel is made from, and/or wherein the chamber is made of a material comprising at least one of heat-resistant steel, stainless steel, and chromium steel, and/or wherein the condensation device is made of a material comprising at least one of heat-resistant steel, stainless steel, chromium steel, graphite, boron nitride, one or more metals, and one or more oxides, and/or wherein the collecting vessel is made of a material comprising at least one of graphite, boron nitride, one or more metals, and one or more oxides.

16. A method of producing a target material, from starting material comprising the steps of: introducing the starting material in at least one trough being provided in a chamber; heating the chamber with at least a first heating element such, that the starting material being received in the trough is vaporized; receiving a condensate that will constitute the target material in at least one collecting vessel; wherein the method further comprises the step of condensating the vaporized starting material with at least one condensation device, whereby the condensate is formed.

17. A method of producing a target material, from starting material comprising the steps of: evacuating a chamber with at least a first source of negative pressure that is in connection with the chamber or supplying an inert gas into the chamber via at least a first supply device that is in connection with the chamber; introducing the starting material in at least one trough being provided in a chamber (2); heating the chamber with at least a first heating element such that the starting material being received in the trough is vaporized; receiving a condensate that will constitute the target material in at least one collection vessel; and optionally condensating the vaporized starting material with at least one condensation device, whereby the condensate is formed. characterized in that the method further comprises the step of introducing the starting material into the chamber via at least a first gate device being in connection with the chamber while the chamber remains evacuated or under an inert gas atmosphere

18. The method according to claim 16, wherein the condensation device is cooled to a condensation device temperature that is slightly higher than a melting point of the target material and/or a liquidus temperature of the target material.

19. The method according to claim 16, wherein the condensate being received in the collection vessel is removed from the collection vessel while the chamber remains heated.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0055] Preferred embodiments of the invention are described in the following with reference to the drawings, which are for the purpose of illustrating the present preferred embodiments of the invention and not for the purpose of limiting the same. In the drawings,

[0056] FIG. 1 shows a sectional view through a device comprising a condensation element and a coating;

[0057] FIG. 2 shows a sectional view through a device comprising a condensation element, a coating and a cover element according to another embodiment;

[0058] FIG. 3 shows a sectional view through a device comprising a condensation element and a cover element according to another embodiment;

[0059] FIG. 4 shows a sectional view through a device comprising a condensation element and a funnel element according to another embodiment;

[0060] FIG. 5 shows a sectional view through a device comprising a condensation element, a coating, a funnel element, and a collecting vessel according to another embodiment;

[0061] FIG. 6 shows a sectional view through a device comprising a condensation element, a coating, a collecting vessel, and a first source of negative pressure or supply device and a second source of negative pressure or supply device according to another embodiment;

[0062] FIG. 7 shows a sectional view through a device comprising a condensation element, a coating, a collecting vessel, and a first source of negative pressure or supply device and a second source of negative pressure or supply device according to another embodiment.

DESCRIPTION OF PREFERRED EMBODIMENTS

[0063] FIGS. 1 to 7 depict several embodiments of a device 1 for producing a target material, preferably one or more metals and/or one or more alloys, from starting material. Although not always depicted the devices 1 according to all embodiments in each case comprise a chamber 2, within which a trough 3 is provided. In these examples the chamber 2 corresponds to a chamber 2 which is constituted by four chamber walls and whose cross-section is essentially squared. Namely an upper wall 7, a lower wall 31, and two side walls 32, 32′. The trough 3 corresponds to a recess being provided in the lower wall 31 of the chamber 2, which recess 3 extends entirely around a circumference of the chamber 2. The trough 3 is configured to receive the starting material. The device 1 further comprises a first heating element 4, which essentially entirely surrounds the chamber 2 and which is configured to heat the chamber 2 such that starting material being received in the trough 3 is vaporized. The lower wall 31 of the chamber 2 comprises a chamber opening 33 that is passed through a collecting vessel 5. The collecting vessel 5 is configured to receive a condensate that will constitute the target material. In the following, these and further features of the devices 1 according to the invention shall be explained in greater detail. It is important to note that features that are depicted here only in some figures can likewise be present in the devices depicted in the other figures. The same applies to features that are absent in certain figures. Such features could likewise be absent in the devices of the other figures. That is to say, the depicted embodiments shall be seen as explanatory examples of the individual features.

[0064] In the devices 1 depicted in FIGS. 1 to 7 a condensation device 6 is present in an upper region 2a of the chamber 2. The condensation device 6 extends from an outside of the device 1 through the heating element 4 as well as through the upper wall 7 of the chamber 2 at least partially into the interior 8 of the chamber 2. The condensation device 6 is configured to condensate the vaporized starting material, whereby the condensate is formed. Moreover, in the present examples the condensation device 6 is an integral part of the chamber 2. The collecting vessel 5 is arranged in a lower region 2b of the chamber 2 and located below the condensation device 6 with respect to a vertical direction V. In this case, condensate that drops or flows from the condensation device 6 vertically downward falls through an inlet opening 21 of the collecting vessel 5 and into the collecting vessel 5.

[0065] As follows from FIGS. 1, 2 and 6, a cross-section DC of the condensation device 6 can be smaller than a cross-section DV of the collecting vessel 5. However, it is likewise conceivable that a cross-section DC of the condensation device 6 is essentially equal to a cross-section DV of the collecting vessel 5 or larger than a cross-section DV of the collecting vessel 5, see FIG. 3 and FIGS. 5 and 7, respectively. In the latter case a funnel element 20 is arranged above the inlet opening 21 of the collecting vessel 5 so as to guide the condensate into the inlet opening 21 of the collecting vessel 5. The device 1 depicted in FIG. 4 furthermore comprises a sealing element 22 which is arranged around an upper region 5a of the collecting vessel 5. The sealing element 22 is configured to seal the upper region 5a of the collecting vessel 5 against the chamber 2, in particular against the chamber opening 33.

[0066] The condensation device 6 corresponds to a heat exchanger and is preferably configured such, that a temperature gradient is established at the condensation device 6, see also explanations provided further below. The devices 1 according to FIGS. 1 to 5 in each case comprise a condensation device 6 in the form of a heat exchanger with comprises one or more supply tubes 9 extending from an outside of the device 1 into an interior 11 of the condensation device 6 and one ore more discharge tubes 10 extending from the interior 11 of the condensation device 6 to the outside of the device 1. A cooling medium, preferably air at room temperature, is supplied from the outside into the interior 11 of the condensation device 6 via the supply tube 9. Because the temperature within the chamber 2 is high during the distillation process, said cooling medium is heated up in the lower region 6b of the condensation device 6, wherein the heated cooling medium will afterwards be discharged from the condensation device 6 towards the outside via the discharge tube 10. As already mentioned it is preferred that a temperature gradient is established at the condensation device 6. Although not depicted in the figures it is preferred that the device 1 further comprise at least one temperature sensing element, preferably a thermocouple, which is in thermal contact with the condensation device 6 so as to measure the condensation device temperature. For instance, the temperature sensing element can be integrated into the condensation device 6. The condensation device temperature preferably follows a temperature gradient, wherein an upper region 6a of the condensation device 6 has a higher temperature than a lower region 6b of the condensation device 6. That is, whereas the lower region 6b of the condensation device 6 is preferably slightly above the melting point of the target material and/or the liquidus temperature of the target material, the upper region 6a of the condensation device 6 preferably essentially corresponds to a chamber temperature. To this end the condensation device 6 in the said FIGS. 1 to 5 comprises a supply tube 9 and a discharge tube 10 of different length. Here, a length LS of the supply tube 9 is longer than a length LD of the discharge tube 10 with respect to a vertical direction V. Other configurations are of course likewise possible. For example, and as can be seen in FIG. 3, a wall thickness wa of the condensation device 6 in an upper region 6a of the condensation device 6 can be made thinner than a wall thickness wb of the condensation device 6 in a lower region 6b of the condensation device 6. In this case, a temperature gradient is established by the difference in wall thicknesses. The chamber 2, in particular the trough 3, however is preferably heated to a chamber temperature being above the melting points of the starting material. In this way it is possible to evaporate the starting materials being received in the trough 3 of the chamber 2.

[0067] A contamination of the starting material and/or of the target material by dissolved particles generated by unwanted condensed drops at the inner wall 18 of the chamber 2, from the outer wall 12 of the condensation device 6, i.e. the condensation surfaces, and from the inner wall 23 of the collecting vessel 5 can be prevented by means of an appropriate coating 19. The coating 19 is essentially chemically and/or physically inert to the starting material and/or to the condensate and is depicted in FIGS. 1, 2, 5 and 6. In fact, the coating 19 depicted in FIG. 1 corresponds to a coating 19 that is applied to the inner wall 18 of the chamber 2 in the upper region 2a of the chamber 2 as well as on the entire outer wall or surface 12 of the condensation device 6. This is in contrast to the device 1 depicted in FIG. 5, wherein a coating 19 is only applied on the entire outer wall or surface 12 of the condensation device 6. In addition to such a coating or instead of such a coating the device 1 can comprise a cover element 13a, 13b which likewise serves the purpose of providing a protection against a contamination of the target material contained in the collecting vessel 5. The devices 1 depicted in FIGS. 2 and 3 comprise such a cover element 13a, 13b. The cover elements 13a, 13b depicted in FIGS. 2 and 3 are in each case arranged in an upper region 2a of the chamber 2 as well as at least partially above the collecting vessel 5 with respect to the vertical direction V. Particularly, the device 1 according to FIG. 2 comprises a first cover element 13a extending from a main body 14 of the condensation device 6 laterally outwards and a second cover element 13b extending from the upper wall 7 of the chamber 2 at least partially into the chamber 2. Both cover elements 13a, 13b are arranged at an angle αa, αb with respect to the vertical direction V, wherein the angle αa associated with the first cover element 13a is inclined downwardly by about 45° with respect to the vertical direction V. Likewise, the angle αb associated with the second cover element 13b is inclined downwardly by about 45° with respect to the vertical direction V. Furthermore, a surface 34 of the first cover element 13a is coated with a coating 19. This is in contrast to the cover element 13a depicted in FIG. 3, which cover element 13a is free from any coating and is arranged at an angle αa of about 90° with respect to the vertical direction V. The cover elements 13a, 13b depicted in FIG. 2 extend with respect to a horizontal direction H running perpendicularly to the vertical direction V to an extent such, that the cover element 13a is at least partially located above the collecting vessel 5 and the cover element 13b is at least partially located above the trough 3 with respect to the vertical direction V. The cover element 13a of FIG. 3, however, is arranged partly above the collecting vessel 5, but does not extend until the trough 3. The device 1 depicted in FIG. 6 comprises a collecting vessel 5 whose inner wall 23 is coated with the coating 19.

[0068] The devices 1 depicted in FIGS. 2 and 5 further comprise a second heating element 15, which is arranged in an upper region 2a of the chamber 2, here on top of the upper wall 7 of the chamber 2, and which is configured to heat the upper region 2a of the chamber 2 and the upper region 6a of the condensation device 6. The second heating element 15 allows to heat the upper region 2a of the chamber 2 and the upper region 6a of the condensation device 6, such that a lower region 6b of the condensation device 6 has a lower temperature than the upper region 6a of the condensation device 6. In this case a temperature gradient is established between the lower region 6b of the condensation device 6 and the upper region 6a of the condensation device 6. Such a second heating element 15 is also beneficial if a cover element 13a, 13b is present as it is shown in FIG. 2, where the second heating element 15 allows a heating of the cover element 13a, 13b to a temperature that essentially corresponds to the temperature of the vaporized starting material.

[0069] Further heating elements can be present. For example, and as is depicted in FIG. 6, a third heating element 16 can be arranged below the trough 3 with respect to the vertical direction V in order to additionally heat the trough 3. Moreover, and as follows from FIG. 2, a fourth heating element 17 being arranged in a lower region 2b of the chamber 2 and in vicinity to an upper region 5a of the collecting vessel 5 is conceivable, wherein said fourth heating element 17 is configured to heat the upper region 5a of the collecting vessel 5 to a vessel temperature being above a melting point of the starting material and to heat a lower region 5b of the collecting vessel 5 to a vessel temperature being slightly above a melting point of the target material and/or a liquidus temperature of the target material. This fourth heating element 17 allows an evaporation of any material that has solidified in gaps that exist between removable parts, such as a gap between the collecting vessel 5 and the chamber opening 33 for example. Any clamping caused by the solidified material can thereby be eliminated and a removal of the collecting vessel 5 from the chamber 2 is facilitated. Several configurations of the collecting vessel 5 are conceivable. Namely, and as already mentioned, a size such as the cross-section DV of the collecting vessel 5 is variable and can be chosen adapted to the use. Likewise, different lengths of the collecting vessel 5 are conceivable. Furthermore, and as depicted in FIG. 5, a collecting vessel 5 being composed of several parts is possible. For example, the collecting vessel 5 can comprise a first collecting vessel element 28a that is removable connectable to a second collecting vessel element 28b. The collecting vessel elements 28a, 28b depicted in FIG. 5 comprise different wall thicknesses, wherein a wall thickness of the second collecting vessel element 28b is greater than a wall thickness of the first collecting vessel element 28a. These different thicknesses result in an optimized temperature gradient along the collecting vessel 5.

[0070] The devices 1 depicted in FIGS. 1 to 7 are configured to be operated under vacuum or in the presence of an inert gas atmosphere, respectively. To this end either a first source of negative pressure 24a is provided that is in connection with the chamber 2 and which is configured to evacuate the chamber 2 or a first supply device 24b is provided that is likewise in connection with the chamber 2 and that is configured to supply an inert gas to the chamber 2. In the former case, the distillation being carried out by the device 1 is referred to as a vacuum distillation. As can be readily seen in the figures, the source of negative pressure 24a and the supply device 24b are in connection with the device 1 via appropriate connections 35, for example tubes or pipes. These and other elements associated with the application of a vacuum or an inert gas atmosphere will now be explained in greater detail with reference to FIGS. 6 and 7. It is once more noted that these features can likewise be present in the devices 1 depicted in FIGS. 1 to 5.

[0071] Hence, the devices 1 according to FIGS. 6 and 7 in each case comprise a first source of negative pressure 24a or a first supply device 24b that is in connection with the chamber 2 as just mentioned. Moreover, these devices 1 comprise a first gate device 26 being in connection with the chamber 2 such, that the starting material is introducible into the chamber 2 via said first gate device 26. In the present examples, the device 1 is configured such, that the starting material is introducible into the chamber 2 via said first gate device 26 while the chamber 2 remains evacuated or under an inert gas atmosphere. This is enabled by the presence of an antechamber 25 that is in connection with the chamber 2 via the first gate device 26. In particular, the first gate device 26 is arranged within a pipe or tube 36 that connects the antechamber 25 with the interior of the chamber 2. Here, the antechamber 25 is surrounded by a sixth heating element 37 which is configured to heat the antechamber 25. Hence, by introducing starting material into the antechamber 25 it is possible to pre-heat said starting material within the antechamber 25 and to then transfer said pre-heated starting material into the trough 3 via the pipe or tube 36 if the first gate device 26 is in an opened position. As the chamber 2 is preferably evacuated or under an inert gas atmosphere it is preferred to maintain said state within the chamber 2. The device 1 therefore further comprises a second source of negative pressure 27a or a second supply device 27b that is in connection with the antechamber 25 in order to evacuate the antechamber 25 or to supply inert gas to the antechamber 25. If the first gate device 26 is in its closed position the chamber 2 is closed towards an outside. Here, it is closed towards the antechamber 25. The antechamber 25 together with the first gate device 26 can thus be seen as a sluice device that allows a continuous introduction of the starting material into the chamber 2 while the chamber 2 remains evacuated or under an inert gas atmosphere and with or without cooling of the chamber 2.

[0072] The device 1 further comprises two second gate devices 29a, 29b that are in connection with the collecting vessel 5, and wherein the condensate is removable from the collecting vessel 5 via said second gate devices 29a, 29b. Here, one second gate device 29a is configured as a lid that is arranged in a bottom region of the collecting vessel 5. Said second gate device 29a is in connection with a second gate device 29b being arranged vertically below via a tube or pipe 38. Said lower second gate device 29b in turn is in connection with a retrieval chamber 30. By opening the second gate devices 29a, 29b the condensate received within the collecting vessel 5 can be transferred, either in its liquid state or in a solidified form, from the collecting vessel 5 into the retrieval chamber 30. If the condensate is to be removed in its liquid state it is preferred to provide a casting mould 39 within the retrieval chamber 30 that collects the liquid condensate. Furthermore, if the condensate shall be removed in the liquid state a seventh heating element 40 can be arranged around the collecting vessel 5 so as to ensure that the condensate remains in its liquid state. The casting mould 39 and the retrieval chamber 30, however, are preferably kept at room temperature. The retrieval chamber 30 can be in connection with the first source of negative pressure 24a or with the first supply device 24b, respectively. In doing so a second sluice device being constituted by the tube or pipe 38 that connects the second gate devices 29a, 29b and the retrieval chamber 30 is provided. This arrangement allows a removal of the condensate from the collecting vessel 5 while the chamber 2 remains evacuated or under an inert gas atmosphere.

[0073] Hence, the devices 1 according to the invention enable an introduction of starting material into the chamber 2 and a removal of the target material from the collecting vessel 5 while the chamber remains evacuated or under an inert gas atmosphere. In other words, the devices 1 enable a continuous distillation that is associated with high conversions and very attractive from an economical point of view.

TABLE-US-00001 LIST OF REFERENCE SIGNS  1 device  2 chamber  2a upper region of chamber  2b lower region of chamber  3 trough  4 heating element  5 collecting vessel  5a upper region of collecting vessel  5b lower region of collecting vessel  6 condensation device  6a upper region of condensation device  6b lower region of condensation device  7 upper wall of chamber  8 interior  9 supply tube 10 discharge tube 11 interior 12 outer wall of condensation device 13a, 13b cover element 14 main body 15 heating element 16 heating element 17 heating element 18 inner wall of chamber 19 coating 20 funnel element 21 inlet opening 22 sealing element 23 inner wall of collecting vessel  24a source of negative pressure  24b supply device 25 antechamber 26 gate device  27a source of negative pressure  27b supply device  28a first collecting vessel element  28b second collecting vessel element  29a gate device  29b gate device 30 retrieval chamber 31 lower wall of chamber .sup. 32, 32′ side wall of chamber 33 chamber opening 34 surface 35 connection 36 tube 37 heating element 38 tube 39 mould 40 heating element H horizontal direction V vertical direction LS length of supply tube LD length of discharge tube Wa wall thickness in upper region Wb wall thickness in lower region αa angle αb angle DC cross-section DV cross-section