Pressure vessel with magnetic disk for stirring
11464086 · 2022-10-04
Assignee
Inventors
Cpc classification
B01L7/02
PERFORMING OPERATIONS; TRANSPORTING
B01L9/06
PERFORMING OPERATIONS; TRANSPORTING
B01J3/03
PERFORMING OPERATIONS; TRANSPORTING
B01J3/04
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
The present invention relates to a pressure vessel (1) for receiving samples (P) to be heated, having a reaction chamber (2) as a pressure space for the initiation and/or facilitation of chemical and/or physical pressure reactions, the reaction chamber (2) being designed for receiving a liquid (5), a magnetic disk (8) mounted rotatably about an axis of rotation in the reaction chamber (2), and a magnet arrangement (10), provided outside the reaction chamber (2), for generating a rotating magnetic field for rotationally driving the magnetic disk (8) about its axis of rotation, the magnetic disk (8) having at least one passage bore (13), which extends transversely in relation to the axis of rotation and is provided in such a way that liquid (5) received in the reaction chamber (2) is driven through the passage opening (13) by rotation of the magnetic disk (8) in order to stir the liquid (5).
Claims
1. Pressure vessel (1) for receiving samples (P) to be heated, having a reaction chamber (2) as a pressure space for the initiation and/or facilitation of chemical and/or physical pressure reactions, the reaction chamber (2) being designed for receiving a liquid (5), a magnetic disk (8) mounted rotatably about an axis of rotation in the reaction chamber (2), and a magnet arrangement (10), provided outside the reaction chamber (2), for generating a rotating magnetic field for rotationally driving the magnetic disk (8) about its axis of rotation, the magnetic disk (8) having at least one passage bore (13), which extends transversely in relation to the axis of rotation and is provided in such a way that liquid (5) received in the reaction chamber (2) is driven through the passage opening (13) by rotation of the magnetic disk (8) in order to stir the liquid (5), and wherein the pressure vessel further comprising a plate (9), which is provided in the reaction chamber (2) and is permeable to the liquid (5), wherein the plate (9) defines with the reaction chamber (2) a space in which the magnetic disk (8) is mounted.
2. Pressure vessel (1) according to claim 1, wherein the at least one passage bore (13) passing through the magnetic disk (8) at least partly in an upward direction and away from the axis of rotation or toward the axis of rotation.
3. Pressure vessel (1) according to claim 1, wherein the at least one passage bore (13) passing through the magnetic disk (8) at least partly in a direction inclined tangentially to or counter to the turning direction about the axis of rotation.
4. Pressure vessel (1) according to claim 1, wherein the at least one passage bore (13) passing through the magnetic disk (8) at least partly in a direction inclined radially toward or away from the axis of rotation.
5. Pressure vessel (1) according to claim 1, wherein the magnetic disk (8) having at least two passage bores (13).
6. Pressure vessel (1) according to claim 1, wherein the plate (9) is permeable to the liquid (5) by way of holes (9b).
7. Pressure vessel (1) according to claim 6, wherein the plate (9) being produced from a ceramic material.
8. Pressure vessel (1) according to claim 6, wherein the reaction chamber (2) and/or the plate (9) having a region (2a, 9c) for mounting the magnetic disk (8).
9. Pressure vessel (1) according to claim 1 further comprising at least one sample container (6) for receiving the sample (P), the sample container (6) being held in the reaction chamber (2) in order to be warmed by the liquid (5) received in the reaction chamber (2) when the liquid (5) has been received in the reaction chamber (2).
10. Pressure vessel (1) according to claim 9, wherein the at least one sample container (6) having a stirring magnet (14) for stirring a sample (P) received in the sample container (6), and the stirring magnet (14) being provided with respect to the magnetic disk (8) in such a way that, for stirring the sample (P), the stirring magnet (14) is set in motion by the rotating magnetic field and/or by the rotating magnetic field obtained because of rotation of the magnetic disk (8).
11. Pressure vessel (1) according to claim 9, wherein the at least one sample container (6) being held in the reaction chamber (2) by way of a sample holder (7).
12. Pressure vessel (1) according to claim 1, wherein the magnet arrangement having one or more electromagnets (10).
13. Pressure vessel (1) according to claim 12, wherein the electromagnet (10) being provided below, obliquely below or laterally in relation to the magnetic disk (8).
14. Pressure vessel (1) according to claim 12, wherein the electromagnet (10) being provided in a bore (lb) provided in the pressure vessel wall and extending in the direction of the magnetic disk (8).
15. Pressure vessel (1) according to claim 1, wherein the magnet arrangement having at least one permanent magnet provided rotatably, in particular rotatably about the magnetic disk (8), so that the rotating magnetic field for rotationally driving the magnetic disk (8) is generated by the turning of the permanent magnet.
16. Pressure vessel (1) according to claim 15, wherein the magnet arrangement having a permanent magnet receptacle, in which the at least one permanent magnet is received for turning or rotating the at least one permanent magnet.
17. Pressure vessel (1) according to claim 15, wherein the magnet arrangement having a drive for driving the at least one permanent magnet or the permanent magnet receptacle, so that the permanent magnet or magnets rotate(s) in such a way as to generate the rotating magnetic field.
18. Pressure vessel (1) according to claim 1, wherein the magnetic disk (8) having at least two magnetic elements (8c) for the magnetization of the magnetic disk (8).
19. Pressure vessel (1) according to claim 18, wherein one of the at least one passage bore (13) being provided between two magnetic elements (8c), seen in plan view of the magnetic disk (8).
20. Pressure vessel (1) according to claim 18, wherein the at least two magnetic elements (8c) being in each case a magnetic column.
21. Pressure vessel (1) according to claim 1, further comprising a microwave generator, which is provided in such a way that microwaves generated by the microwave generator are coupled into the reaction chamber (2) at least by way of the magnetic field generated by the magnet arrangement (10).
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1)
(2)
(3)
(4)
(5)
(6)
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
(7)
(8) The pressure vessel 1 may be a (high-pressure) autoclave. The pressure vessel 1 preferably consists of a high-pressure-resistant material, such as for example metal, preferably steel, particularly preferably a corrosion-resistant high-grade steel alloy. The pressure vessel 1 is in this case preferably formed in such a way that it can be used at pressures up to at least 200 bar, preferably up to at least 500 bar, and at temperatures of up to and even above 300° C.
(9) The pressure vessel 1 has furthermore a reaction chamber or a pressure space 2 for the initiation and/or facilitation of the chemical and/or physical pressure reactions on the samples P. It can be seen that the pressure vessel 1 surrounds the reaction chamber 2, to be precise preferably on all sides. The sample or samples P is/are arranged in the reaction chamber 2 for the sample processing and can be removed from it, preferably through an opening.
(10) The pressure vessel 1 preferably has a (pot-shaped) lower part 3 and a cover part 4, which can be closed together and in the closed state surround the reaction chamber 2 on all sides. Here, the cover 4 closes the opening provided in the pressure vessel 1, that is to say the lower part 3 of the pressure vessel 1, for introducing and removing the sample P. By means of the cover 4, the pressure vessel 1 and/or the reaction chamber 2 can consequently be opened and closed.
(11) As can be seen in particular from
(12) The sample P may be provided in a sample container 6, such as for example a test tube. The sample P is preferably provided in the pressure vessel in such a way that the liquid 5 reaches at least up to part of the height of the sample P. It may however also be provided that the liquid 5 reaches beyond the height of the sample P. Preferably, the pressure vessel 1 or the reaction chamber 2 is designed to receive two or more samples P. In a corresponding way, a number of sample containers 6 may also be provided, that is to say at least one sample container 6 for receiving one sample P each.
(13) The pressure vessel 1 may furthermore have a sample holder 7, with which the sample container 6 can be held in the reaction chamber 2. The sample holder 7 preferably carries the at least one sample container 6 in such a way that the sample container 6 is in the liquid 5. The sample holder 7 is in particular designed to place the at least one sample P or the at least one sample container 6 into the reaction chamber 2, and remove it again from the latter, for example by way of a handle 7a. The sample holder 7 may furthermore have a sample container receiving region 7b, which is preferably designed so as to correspond to the sample container 6. The sample container receiving region 7b may have a number of regions, in order for a sample container 6 to be received by a respective region. The sample container receiving region 7b has the effect here in particular that the sample containers 6 are provided in a specific pattern, that is to say for example are arranged in the form of a circle around the handle 7a. As can be seen in
(14) The pressure vessel 1 has furthermore a magnetic disk 8, which is mounted in the reaction 1o chamber 2 so as to be rotatable about an axis of rotation. The magnetic disk 8 has a form typical of a disk, that is to say in particular a flat and/or (circularly) round form. The magnetic disk 8 is provided in the reaction chamber 2 in such a way that—when the liquid 5 is present in the reaction chamber 2—the magnetic disk 8 is provided in the liquid 5. In particular, the magnetic disk 8 may be provided in a lower region of the reaction chamber 2, preferably on the base of the reaction chamber 2. The magnetic disk 8 preferably extends substantially over the entire base surface of the reaction chamber 2, and consequently leaves only a small gap between the magnetic disk 8 and the reaction chamber 2. The reaction chamber 2, preferably the base of the reaction chamber 2, may have a bearing region 2a, by way of which the magnetic disk 8 can be mounted in the reaction chamber 2, in particular in such a way that the magnetic disk is (only) movable or rotatable about its axis of rotation. The bearing region 2a is preferably designed so as to correspond to a bearing region 8a formed on the magnetic disk 8. That is to say that the magnetic disk 8 may be rotatably mounted in the reaction chamber 2 by way of the bearing regions 2a, 8a of the reaction chamber 2 and of the magnetic disk 8, respectively. For example, the bearing region 2a may be provided as a clearance or bore, while the bearing region 8a of the magnetic disk 8 is formed in a corresponding way, for example as a projection, and engages in this clearance.
(15) The pressure vessel 1 may furthermore have a plate (disk) or a pedestal 9, which is provided in the reaction chamber 2 and is permeable to the liquid 5. It can be seen that the plate 9 defines with the reaction chamber 2, in particular with the base of the reaction chamber 2, a space in which the magnetic disk 8 is mounted. For this, the plate 9 may for example be placed in the reaction chamber 2 and/or be connected to the side walls of the reaction chamber 2, for example in that the plate 9 rests on a projection or on a step 9e of the reaction chamber 2 (compare
(16) The plate 9 provided in the liquid 5 is permeable to the liquid 5, for example by way of holes or passage openings 9b. The holes 9b are preferably arranged uniformly distributed over the surface of the plate 9. It is preferred if the plate 9 is produced from a ceramic material, such as for example silicon carbide. Since these materials are highly microwave-absorbent, the plate 9 provided in the liquid 5 can consequently be heated by means of microwave radiation, so that the liquid 5 is heated both directly by way of microwave absorption and indirectly by way of heat dissipation from the plate 9.
(17) In particular in
(18) The plate 9 may furthermore have a bearing region 9d for the mounting or holding of the sample holder 7. It may be provided that the bearing region 9d of the plate 9 is designed so as to correspond to a bearing region 7c of the sample holder 7. For example, the bearing region 9d is provided as an opening or clearance, the bearing region 7c being formed in a corresponding way, for example as a projection, and engaging in the aforementioned opening or clearance. In particular, it may be provided that one of the holes 9b of the plate 9, preferably the one of the holes 9b for mounting the magnetic disk 8, forms the bearing region 9d, in that the bearing region 7c formed as a projection engages in the respective hole 9b. In other words, one of the holes 9b may form the bearing region both for the sample holder 7 and for the magnetic disk 8. The bearing region 9d or 7c has the effect here in particular that the sample holder is arranged in the reaction chamber 2 in a defined position and preferably immovably.
(19) The pressure vessel 1 has furthermore at least one magnet arrangement, which is provided outside the reaction chamber 2 and in the exemplary embodiments shown in the figures has by way of example at least one electromagnet 10. Preferably, the pressure vessel 1 has, as represented, a number of electromagnets 10, which are preferably arranged uniformly distributed around the aforementioned axis of rotation or around the circumference of the reaction chamber 2. By means of the at least one electromagnet 10, a magnetic field that is rotating (in a circle) is formed for rotationally driving the magnetic disk 8 about its axis of rotation. For this, the at least one electromagnet 10 is preferably designed so as to correspond to a stator of a synchronous or stepping motor. To generate the rotating magnetic field, the pressure vessel 1 may have a control unit, which is not represented any more specifically and is functionally connected to the at least one electromagnet 10. The control unit preferably controls the electromagnets 10 in a way as known in the case of synchronous motors or stepping motors, that is to say for example in a sinusoidal manner. The control unit may in particular be designed to control an alternating current fed into the electromagnets 10, that is to say in particular to set the frequency of the alternating current. By way of setting the frequency of the alternating current, the rotational speed of the magnetic field, and consequently the rotational speed of the magnetic disk, can consequently be changed/varied.
(20) The electromagnet 10 is preferably a magnetic coil or field coil and/or is formed as a field coil ring. The electromagnet 10 may however also be any other element for generating a magnetic field or a rotating magnetic field. Preferably, the electromagnet 10 is produced from a ferromagnetic material. Preferably, the electromagnet 10 is connected fixedly or reconnectably to the outer wall of the pressure vessel 1. As can be seen in
(21) As can be seen in particular in
(22) The invention is not however thereby restricted to such an arrangement of the electromagnet 10. A further configuration for arranging the electromagnet 10 or of the number of electromagnets 10 outside the reaction chamber 2 is shown in
(23) In
(24) The clamp 12 preferably has two clamp halves 12a, 12b, which are movable in relation to one another in order to be brought into connection with the pressure vessel 1 or the outer wall of the pressure vessel 1. That is to say that the clamp halves 12a, 12b are preferably connected to one another in an articulated manner at one of their ends and can be (re-)connected or fastened to one another at the other of their ends or by way of their free ends. The free ends of the clamp halves 12a, 12b may for example be connected to one another with a fastening means 12c. The clamp 12 can therefore reach around the pressure vessel 1 or its outer wall, the clamp 12, in particular its inwardly directed surface, coming into at least force-fitting contact with the outer wall of the pressure vessel 1 as a result of tightening of the fastening means 12c, in order in this way to hold the at least one electromagnet 10 with respect to the magnetic disk 8. The fastening means 12c may be for example a screw, which can be led through the free end of the one clamp half 12b and is screwed in the other clamp half 12a, in order in this way to move the clamp halves 12a, 12b toward one another, so that they are pressed against the outer wall of the pressure vessel 1.
(25) It is preferred if the clamp 12 is provided on the pressure vessel 1 in such a way that the electromagnet 10 received therein is level with the magnetic disk 8. The clamp 12 has the effect in particular that the at least one electromagnet 10 can be provided variably in its height with respect to the magnetic disk 8. By means of the clamp 12, the electromagnet 10 can in particular 30o be provided with respect to the magnetic disk 8 without structural modifications of the pressure vessel 1, in particular without structural modifications of the pressure vessel wall.
(26) Since the magnetic disk 8 is located in the rotating magnetic field brought about by the electromagnet 10, a rotational speed of the magnetic disk 8 that corresponds to the rotational speed of the magnetic field brought about by the electromagnet 10 will be established. With regard to the magnetization, the magnetic disk 8 is preferably designed so as to correspond to a rotor of a synchronous or stepping motor. For the magnetization of the magnetic disk 8, the magnetic disk 8 may have a permanent magnet and/or a separately excited magnet—that is to say a magnet that is operated by a supply of current. It is preferred if at least two, preferably three, particularly preferably four, magnetic elements 8c are provided for the magnetization of the magnetic disk 8. As can be seen in
(27) It may in particular be provided that the respective magnetic element 8c is designed as a magnetic column. The magnetic column preferably has a cylindrical form. Preferably, the magnetic disk 8 has a clearance or blind-hole bore corresponding to the magnetic column. In this way it can be provided that the magnetic column can be inserted or can be fitted into the magnetic disk 8 or into the clearance designed so as to correspond to the magnetic column, in order in this way to bring about for example easy changing of the magnetic elements 8c. The respective clearance may be provided horizontally (parallel), transversely or perpendicularly in relation to the axis of rotation of the magnetic disk 8. In this way, magnetic elements with a high magnetic density can be used. If the electromagnets 10 are provided below the magnetic disk 8, that is to say for example in the lower housing part 3 or in the pressure vessel base 3a, it is of advantage if the clearance is provided parallel to the axis of rotation. In this way, a high field strength of the magnetic elements 8c in the downward direction is brought about, so that the magnetic disk 8 can be driven more effectively. As an alternative or in addition, the magnetic elements 8c may also be embedded/encapsulated in the magnetic disk 8, in particular welded in, fused in and/or enclosed.
(28) The magnetic disk 8 is not restricted to a specific material, but it is preferred if the magnetic disk 8 is produced from a ceramic material, such as for example silicon carbide. Since these materials are highly microwave-absorbent, the magnetic disk 8 provided in the liquid 5 can consequently be heated by means of microwave radiation, so that the liquid 5 is heated both directly by way of microwave absorption and indirectly by way of heat dissipation from the magnetic disk 8.
(29) As can be seen in particular in
(30) The passage bore 13 is provided in such a way that the liquid 5 received in the reaction chamber 2 is driven through the passage opening 13 by rotation of the magnetic disk 8 in order to stir the liquid 5. By means of the stirring effect, the liquid 5 is forced in an upward and outward direction, and consequently rises up on the inner wall of the reaction chamber 2. Consequently, seen in section, a substantially U-shaped liquid level is formed. The liquid 5 is therefore driven from one side of the magnetic disk 8, for example from its underside, to another side of the magnetic disk 8, for example to its upper side, in order in this way to allow the liquid 5 to circulate for the stirring. The liquid 5 circulates in the reaction chamber 2, in that it flows through the gap between the magnetic disk 8 and the plate 9, through the gap between the magnetic disk 8 and the base of the reaction chamber 2, through the gap between the magnetic disk 8 and the inner wall of the reaction chamber 2, and/or through the passage opening 8. The passage bore 8 therefore brings about a stirring or agitation of the liquid 5, whereby the liquid 5 is warmed more quickly and uniformly and the sample P is consequently heated more efficiently.
(31) To intensify the aforementioned stirring effect, it is preferred if the magnetic disk 8 has a number of, that is to say at least two, preferably three, particularly preferably four, passage bores 13, which—as can be seen in
(32) The passage bore 13 may also be designed in such a way that the liquid 5 is driven through the passage bore 13 and, depending on the turning direction of the magnetic disk 8 about its axis of rotation, the direction of flow of the liquid 5 through the passage bore 13 is changed. If therefore the magnetic disk 8 is turned in one direction (thus for example clockwise), the liquid 5 is driven through the passage bore 8 in a direction from below to above, while in the case of turning of the magnetic disk 8 in the other direction (thus for example counterclockwise) the liquid 5 is driven through the passage bore 13 in a direction from above to below. That is to say that the vector of the extent of the passage bore 13 through the magnetic disk 8 may have a component tangential to the direction of rotation of the magnetic disk, i.e. the passage bore 13 may be provided for example askew to the axis of rotation of the magnetic disk 8. As a result of the tangential component, the liquid can then be driven through the passage bore because of the torque of the magnetic disk 8, and, depending on the turning direction of the magnetic disk 8, the direction of flow of the liquid 5 through the passage bore 13 can be set.
(33) As can be seen in
(34) The stirring magnet 14 is provided with respect to the magnetic disk 8 in such a way that the stirring magnet 14 is set in motion by the rotating magnetic field of the electromagnet 10 and/or of the magnetic disk 8. For this, it is particularly of advantage if the stirring magnet 14 is provided in a (lower) part of the sample container 6 that is provided directly opposite the magnetic disk 8 and/or the plate 9, so that the magnetic field of the magnetic disk 8 acts well on the stirring magnet 14. The respective magnetic field of the magnetic disk 8 and/or of the electromagnet 10 therefore moves in relation to the sample container 6, whereby the stirring magnet 14 is set in motion or made to turn in a way that corresponds to the rotation of the respective magnetic field or the magnetic fields. By this movement, the sample P is consequently stirred by means of the stirring magnet 14, whereby in particular samples with high viscosity or many fractions of solid matter can be homogenized efficiently.
(35) For warming or heating, in particular the liquid 5, the plate 9 and/or the samples P, the pressure vessel 1 may have any means for the direct or indirect dissipation of heat. It is preferred if the pressure vessel 1 has a microwave generator, which is not represented any more specifically and couples microwaves into the reaction chamber 2 by way of the microwave coupling-in region 11. The generated microwaves in this case enter the reaction chamber 2 preferably by way of the magnetic field of the magnetic disk 8 and/or of the electromagnet 10, so that the magnetic field can interact with the coupled-in microwaves, in order for example to bring about an advantageous diversion of the microwaves.
(36) Instead of the electromagnet 10 as described above, according to an exemplary embodiment that is not represented any more specifically, the magnet arrangement may also have a rotatably provided permanent magnet described as follows, so that the rotating magnetic field for rotationally driving the magnetic disk is generated by the turning or rotation of the permanent magnet. Unless otherwise described below, the statements made above with respect to the electromagnet 10 apply analogously to such a magnet arrangement.
(37) The magnet arrangement may have a permanent magnet receptacle, in which the at least one permanent magnet is received for turning the at least one permanent magnet. The permanent magnet receptacle preferably (partially) surrounds the reaction chamber, particularly preferably the pressure vessel. The permanent magnet receptacle may have a form corresponding to the reaction chamber and/or the pressure vessel, for example an annular cross section, or it is formed as a ring. The permanent magnet receptacle preferably receives a number of, in particular two, permanent magnets. For each permanent magnet, the permanent magnet receptacle may have a receptacle corresponding to the respective permanent magnet, in which the respective permanent magnet can be inserted or can be fitted. Alternatively, it may also be provided that the at least one permanent magnet is embedded in the permanent magnet receptacle.
(38) If the magnet arrangement or the permanent magnet receptacle has a number of permanent magnets, they are preferably arranged uniformly distributed over the circumference of the permanent magnet receptacle. The arrangement of the permanent magnets is preferably such that the polarity of the permanent magnets alternates, that is to say alternately positively and negatively charged permanent magnets are provided along the circumference. For example, the cross section of the permanent magnet receptacle may be divided into sectors (of a circle), the sectors alternately having at least one or a group of permanent magnets with a positive polarity (preferably 6 to 8 of them) and at least one or a group of permanent magnets with a negative polarity (preferably 6 to 8 of them). For a particularly high field strength of the magnetic field, it may be provided that two sectors of a circle are provided, preferably lying directly opposite one another, in each case with an inscribed angle in the range from 120° to 180°, preferably in the range from 160° to 180°, a first sector of the circle having at least one or more (for example the aforementioned 6 to 8) permanent magnets with a positive polarity, and a second sector of the circle having at least one or more (for example the aforementioned 6 to 8) permanent magnets with a negative polarity. It is preferred if the respective permanent magnets of each sector of the circle are arranged uniformly distributed over the respective sector (of the circle), so that a particularly high and uniform field strength of the magnetic field is achieved.
(39) The permanent magnet receptacle may consist of any material that is suitable for receiving the at least one permanent magnet. Preferred materials are polypropylene (PP), aluminum (Al) and/or plastics in general, since with these materials a particularly low weight can be achieved.
(40) The magnet arrangement may furthermore have a drive for driving the at least one permanent magnet or the permanent magnet receptacle, so that the permanent magnet or the permanent magnet receptacle turns/rotates, in order to generate the rotating magnetic field. It is preferred if the drive turns the permanent magnet receptacle, in order to turn/rotate the permanent magnet as described above. For this, it may be provided that a corresponding transmission means (gear wheel, gear mechanism etc.) is provided between the drive and the permanent magnet receptacle, in order to transmit the driving force of the drive to the permanent magnet receptacle, and consequently the permanent magnet.
(41) The invention is not thereby restricted to the features described above. In particular, all of the features described above may be combined with one another in any desired way.