Device and method for preparing mixtures
Patent Information
- Application Number
- EP2023708729
- Authority / Receiving Office
- EP · EP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2022-02-25
- Filing Date
- 2023-02-27
- Publication Date
- 2025-01-01
AI Technical Summary
Existing methods fail to effectively mix ingredients that are not soluble in each other into a homogeneous mixture, particularly stable emulsions without emulsifiers, and require movable mixing elements which can be inefficient and abrasive.
A device with a container having projections on its walls and driven in a back-and-forth movement along two axes at different frequencies, creating a non-linear trajectory that intensively mixes ingredients without a stirrer, allowing for the production of stable emulsions and suspensions without emulsifiers.
This method enables rapid and efficient mixing of insoluble ingredients into finely distributed, stable emulsions and suspensions, improving the homogeneity and reducing wear on the mixing container, as demonstrated by enhanced battery performance and reduced lithium plating in lithium-ion batteries.
Smart Images

Figure 1.1
Abstract
Description
[0001] Device and method for producing mixtures
[0002] The invention relates to a device and a method, which is preferably carried out using the device, for producing a mixture which is preferably a powder mixture, optionally with a liquid portion in the form of a suspension, or an emulsion, e.g. of at least two ingredients which are preferably not soluble in one another.
[0003] The device and the method have the advantage of converting ingredients in a container into a mixture, which is preferably a pure powder mixture, a suspension or an emulsion, without a mixing element that is movable relative to the container being mounted or contained in the container, in particular no stirrer, so that the container is designed without a bearing for a movable mixing element.
[0004] The device is designed to carry out a mixing process which, within a short period of time, e.g. within a maximum of 10 hours, a maximum of 8 hours, a maximum of 6 hours, a maximum of 4 hours, a maximum of 2 hours, a maximum of 1 hour, preferably a maximum of 5 minutes, a maximum of 3 minutes, a maximum of 120 seconds, a maximum of 100 seconds, a maximum of 60 seconds or a maximum of 30 seconds, results in intensive mixing of the ingredients in the container, e.g. produces a powder mixture, a suspension or an emulsion consisting of finely divided and evenly distributed solid particles and / or liquid ingredients. In the case of liquid ingredients that are not soluble in one another, e.g. one lipophilic and one hydrophilic, an emulsion is produced which has such finely distributed fat or oil droplets in water or water droplets in a fat phase that it can be stable without an emulsifier or surfactant.
[0005] WO 2015 / 114118 A1 describes the production of meat products by subjecting raw meat pieces to a load in a container driven along two axes to a forced reciprocating motion at a frequency of at least 0.5 Hz. Due to the load, the raw meat pieces absorb, for example, aqueous or oily compounds or may stick together.
[0006] EP 3 620 067 A1 describes a mixing and kneading process for a polymer with another ingredient, at least one of which is liquid, by moving a container back and forth at at least 1 Hz along two axes at different frequencies.
[0007] The object of the invention is to provide a device and a method that can be carried out therewith, with which mutually insoluble ingredients can be effectively converted into a homogeneous mixture, in particular to produce a homogeneously distributed powder mixture, a homogeneously distributed suspension, or an emulsion. Preferably, the device and method should be suitable for producing a stable emulsion, which is a homogeneous mixture, from at least two liquids that are insoluble in each other, wherein the resulting emulsion does not contain an emulsifier.
[0008] The invention solves the problem with the features of the claims and in particular provides a device for use as a mixing apparatus and a method for producing a mixture with the device, wherein the device has a container with a cross section of at least 5 mm in diameter, wherein the cross section is spanned by a wall which preferably has projections arranged at intervals and projecting into the cross section with a height of at least 0.05 mm or at least 0.1 mm, e.g. from 0.05 to 0.5 or to 0.2 or to 0.1 mm, wherein the projections are preferably distributed over the entire wall and / or the distances between the projections e.g.from 5 to 50 mm, the wall alternatively having a smooth surface, the container being driven to reciprocate along a trajectory curve obtainable by superimposing the movement along at least two axes which are at an angle to each other and preferably in the plane of the cross-section of the container, at different frequencies.
[0009] The container preferably has a round cross-section, or a cross-section that has at least 3, at least 4, at least 5, at least 6, at least 7, or at least 8 corners, e.g., a maximum of 20 corners in each case. The diameter of the container can be, for example, between 0.5 and 100 cm, e.g., 10 or 20 cm up to 80 or 60 cm.
[0010] The cross-section of the container can be square, round, or oval. The cross-section results in a continuous relative movement of the ingredients filled into the container against the container wall during the reciprocating movement along curved paths, e.g., by reciprocating along two axes that are at an angle to each other and in the plane of the container's cross-section. It is assumed that the intensive and effective mixing of ingredients by the process is also due to the fact that the continuous movement completely encompasses the ingredients, e.g., without any of the ingredients being able to settle or separate.
[0011] The projections projecting into the cross-section of the container can, for example, have a height from the wall of 1 / 30 up to 1 / 1 or up to 1 / 2 or up to 1 / 5 or up to 1 / 10 of the diameter of the container, e.g. 1 / 20 up to 1 / 1 or up to 1 / 2 of the diameter of the container, in particular a height of 0.1 to 20 mm, e.g. at least 2 mm, at least 3 mm, 4 mm or at least 5 mm, e.g. up to 18 mm or up to 15 mm in each case. The projections can have side surfaces perpendicular to the container wall, e.g. be cylindrical or cuboid-shaped, and / or can have side surfaces that extend at an angle of >95°, preferably >100° or >110° or >120° from the container wall, e.g. with at least a triangular cross-section and one or two side surfaces perpendicular to the container wall, conical or truncated cone-shaped.The projections may have a second section spaced from the container wall, which has a larger cross-section than a first section connecting the container wall to the second section, e.g., a T-shaped profile. Preferably, the projections have side surfaces whose profile extends arcuately from the wall, with the side surfaces adjoining the wall in an arcuate manner.
[0012] The projections can be separated from one another or connected to one another, e.g. as webs between which recesses, e.g. in the form of openings or blind holes, are arranged.
[0013] In general, the projections can be designed as webs that are formed between recesses that extend into the container wall. Such webs can be produced, for example, by recesses made in the container wall, or by a sheet metal attached to the container wall that has openings or blind holes, e.g. in the form of bores or elongated holes. The openings can extend parallel or perpendicular to the cross-section of the interior, or at an angle of >0° to <90° to the cross-section of the interior. Optionally, additionally or alternatively, the openings can extend along the radials or at an angle of 10 to 45° to radials that emanate from the longitudinal axis of the cross-section spanned by the inner wall. Optionally, the openings have a constant cross-section or a cross-section that widens with increasing distance from the longitudinal axis.Optionally, the openings have a chamfer, preferably arcuate, to avoid sharp edges adjacent to the cross-section, or the openings are cylindrical or extend conically widening away from the longitudinal axis without a chamfer to form a sharp edge.
[0014] In one embodiment, the side surfaces of the projections merge continuously into the recesses formed therebetween.
[0015] In an alternative embodiment, the projections are arranged at a distance from the container wall so that the side surfaces of the projections do not merge into the container wall or are not connected to the container wall. In this embodiment, the projections can be formed, for example, by a metal sheet mounted at a distance from the container wall and having perforations, e.g. through-going round bores or through-going slots. Such a metal sheet can, for example, be mounted at a distance of 1 to 30 mm from the container wall, preferably parallel to the container wall, e.g. connected to the container wall by supports. It has been shown that projections which extend over the container wall into the cross-section of the container accelerate the mixing of ingredients during the back and forth movement of the container, e.g. in comparison with a cylindrical container with a flat wall.
[0016] According to the invention, the ingredients are mixed by moving the container in a back and forth movement along a trajectory curve with a frequency of at least 1 Hz along two axes, each with a different frequency, over a path along each axis of preferably at least 2.5 mm, at least 1 cm, at least 2 cm or at least 3 cm or at least 10 cm, e.g. up to 50 cm, up to 30 cm, up to 20 or, for shorter paths, up to 10 cm.
[0017] The back and forth movement of the container can, for example, extend over a distance of at least 1.5 mm, more preferably at least 3 mm, more preferably at least 1 cm, more preferably at least 2 cm or at least 5 cm, at least 10 cm or at least 15 cm, e.g. up to 50 cm, up to 30 cm or up to 20 cm. More preferably, the back and forth movement of the container is harmonious along a trajectory curve. The back and forth movement of the container is non-linear and can be sinusoidal, loop-shaped or arc-shaped, preferably along a trajectory curve that preferably lies in the plane or is two-dimensional. In general, a non-linear axis of movement, preferably a back and forth movement along a trajectory curve, which can be a Lissajous figure or hypocycloid, promotes uniform and intensive mixing, even with components of the composition that have a similar or the same specific gravity.Each axis of motion can be linear, so that the non-linear movement of the container is generated by the superposition of the movements along two axes. Optionally, the back-and-forth movement can also extend into a third dimension, perpendicular to the plane spanned by the first and second axes.
[0018] The container is driven to reciprocate along at least one trajectory curve, which can be generated by superimposing the reciprocation along at least two axes that are at an angle to each other, wherein preferably two of the axes lie in the plane of the cross-section of the container, wherein the reciprocation along each axis occurs at different frequencies and / or with a phase offset.The trajectory curve can be generated by superimposing the reciprocating motion along two or three axes at different frequencies and / or with a phase shift, and comprises a sequence of trajectory segments, of which at least one, preferably each, comprises or consists of exactly one complete reciprocating motion along the axis along which the reciprocating motion occurs at the lower frequency, wherein the superimposed reciprocating motions at the higher frequency or the same frequency, each optionally with a phase shift, are included along the other axis or axes. The lower frequency of the complete reciprocating motion forms the frequency of the sequence of trajectory segments.For each track segment, a frequency ratio of the reciprocating movement along two axes of a maximum of 1:20 or a maximum of 1:15 or a maximum of 1:10, a maximum of 1:4 or a maximum of 1:3 is preferred, more preferably between 1:1 and 1:2, even more preferably greater than 1:1 and 1:2 or up to 1:1.5, e.g. with a frequency ratio of 1:1.001 and 1:2 or up to 1:1.5.
[0019] In the case of a trajectory that can be generated by superimposing the back and forth movement along two axes at different frequencies and / or with a phase shift, the axes preferably lie in the plane of the cross-section of the container. In the case of a trajectory that is formed by superimposing the back and forth movement along three axes, two of the axes preferably lie in the cross-sectional plane of the container and the third axis is at an angle to this cross-sectional plane. The lowest frequency of the complete back and forth movement along one of the three axes forms the frequency of the sequence of trajectory segments. In general, the linear movement axes are preferably at right angles to one another. In general, the trajectory does not include any rotation of the container around its own axis.
[0020] Generally, the device is configured to drive the container along a trajectory formed by the superimposition of the reciprocating motion of at least two superimposed linear axes arranged at an angle to one another, wherein the reciprocating motion along the linear axes occurs at different frequencies and / or with a phase offset. The linear axes, along which the superimposed reciprocating motions occur at different frequencies and / or with a phase offset, form the trajectory along which the reciprocating motion of the container occurs, for which the device is configured.
[0021] By moving the container along the trajectory curve, the device is designed to accelerate the mixer relative to the container, so that solids and / or liquids contained in the container are sheared against the container wall by the acceleration and by the movement along or against the container wall and are thereby intensively mixed.
[0022] Because the trajectory can be adjusted or predetermined by the different frequencies and / or the phase shift of the superimposed movements along the linear axes, the device is designed for the reciprocating movement of the container along the trajectory and for the relative movement of the solids and / or liquids and the mixture with respect to the container.
[0023] Generally, the container is preferably not rotationally driven and more preferably not or not fully rotatable, e.g., guided to rotate about its central axis by a maximum of 30°, or by a maximum of 20°, or 10°. Generally, the container is preferably driven exclusively for a reciprocating movement along a curved path.
[0024] The trajectory, which can be adjusted or predetermined by the different frequencies and / or phase shift of the overlapping movements along at least two linear axes, accelerates solids and / or liquids and their mixture relative to the container. The reciprocating movement of the container drives the solids and / or liquids and their mixture toward the inner wall of the container.
[0025] The trajectory allows the angle of incidence and reflection of the solids and / or liquids and the mixture thereof against the container wall to be determined. Furthermore, the device is optionally configured to move the container along the trajectory with an adjustable or predetermined acceleration and speed. Because the device is configured for an adjustable or predetermined trajectory and / or an adjustable or predetermined acceleration and / or an adjustable or predetermined speed along the trajectory of the reciprocating movement of the container, solids and / or liquids and the mixture thereof are driven relative to the container with an adjustable or predetermined acceleration and / or speed, allowing a predetermined or continuous adaptation of the method to the solids and / or liquids and to the mixture thereof.In general, a trajectory can be formed by at least two superimposed individual oscillations. Preferably, a trajectory resembles the trajectory generated by superimposing reciprocating movements along at least two linear axes of motion, each at different frequencies and / or by a phase shift. A reciprocating movement along a trajectory that resembles a reciprocating movement along superimposed linear axes of motion exhibits different frequencies and / or a phase shift. Therefore, in general, a trajectory is optionally not a circular path.
[0026] The difference in frequencies can be, for example, at least 0.01 Hz and / or 0.01% to 900%. The phase shift of the reciprocating movements along the linear axes can be, for example, from 0.01° to 180°, preferably 1 to 179° of 360°, which corresponds to a complete reciprocating movement. 0.01 to 180° of a complete reciprocating movement of 360° is equal to 0.0028% to 50% of a complete reciprocating movement, and 1 to 179° of 360° is equal to 0.28% to 49.7% of a complete reciprocating movement.
[0027] The linear motion axes are perpendicular to each other or at another angle, e.g., 5° to 85°, in particular in the plane of the container's cross-section and / or perpendicular to a central axis of the container. Optionally, the trajectory contains at least one straight section, the end of which is, e.g., a vertex of the trajectory, at which the solids and / or liquids and their mixtures are accelerated from or against the container wall.
[0028] To set different frequencies and / or a phase shift of the superimposed reciprocating movements along at least two linear axes of motion, these reciprocating movements can be coupled to one another by a gear or a guide rail and driven by a motor. A motor-driven gear that adjusts the reciprocating movement along the trajectory curve can have a fixed gear ratio between the superimposed movements along each axis, or an adjustable gear ratio, e.g., a continuously or stepwise shiftable gear. Optionally, the gear can be subject to slip, e.g., a belt drive or a friction gear.
[0029] The output speed of the gear that drives the reciprocating movement of the container is preferably at least 1 Hz, more preferably at least 2.5 Hz, more preferably at least 5 Hz, more preferably at least 7 Hz. e.g. up to 50 Hz, up to 40 Hz, up to 30 Hz, up to 20 Hz or up to 10 Hz. The output speed of the gear is equal to the frequency of the reciprocating movement.
[0030] Alternatively, the reciprocating motion along each of the linear motion axes can be driven by a separate motor, with the lower output speed being the frequency of the reciprocating motion and constituting the frequency of the sequence of path segments. In either embodiment, the speed of each drive motor can be controlled, fixed, or variable over the duration of the process.
[0031] The device allows the trajectory to accelerate the solids and / or liquids and the mixture in a defined direction toward a specific location on the inner wall of the container. The geometry of the container and its inner wall, in conjunction with the trajectory, can support the mixing process, allowing the trajectory to be adjusted cross-sectionally depending on the shape and size of the container.
[0032] Optionally, the device is configured to change the trajectory of the reciprocating movement and / or the acceleration and / or speed of the reciprocating movement during the method, e.g., in a first phase, to set the reciprocating movement along a first trajectory and with a first acceleration and speed, and to set the reciprocating movement in a subsequent second phase along a changed trajectory and / or changed acceleration and / or speed.
[0033] Another option is for the reciprocating movement to be a linear reciprocating movement in a first phase and a reciprocating movement along merging trajectories in a second phase. The trajectory can be determined, for example, by a gear that drives the movement of the container.
[0034] By adjusting the trajectory and acceleration of the reciprocating movement of the container, the device allows a predetermined or dynamically variable and directed acceleration of the ingredients as process material relative to the container. In one embodiment, in which the container can be driven in a controlled manner to a linear reciprocating movement in a first phase, the device is designed to move solids and / or liquids and the mixture thereof perpendicularly against the container wall with a controllable acceleration that is significantly greater than the acceleration due to gravity and therefore essentially independent of the acceleration due to gravity, e.g., with a maximum acceleration of at least 15 m / s. 2 , preferably 25 m / s 2 , preferably at least 50 m / s 2 or at least 100 m / s 2 or at least 200 m / s 2 or at least 350 m / s 2 e.g. up to 500 m / s 2 .
[0035] In general, the device can be designed to accelerate the container with a maximum acceleration of at least 20 m / s 2 or at least 100 m / s 2 , e.g. at least 200 m / s 2 , preferably up to 1000 m / s 2 or up to 300 m / s 2 to accelerate along the path segments, e.g. at a vertex of the path segments.
[0036] The container is preferably designed for a back and forth movement with a maximum acceleration of at least 0.5 m / s 2 or at least 1 m / s 2 or at least 2 m / s 2 at least 3.5 m / s 2 , preferably at least 60 m / s 2 , preferably at least 100 m / s 2 , at least 150 m / s 2 , at least 160 m / s 2 , at least 200 m / s 2 , e.g. up to 300 m / s each 2 or 450 m / s 2 , up to 260 m / s 2 or up to 250 m / s 2driven along each of two axes. Generally, the container is preferably driven along one of the axes, preferably along each axis, in combination with the acceleration to an average speed of at least 0.5 m / s, preferably at least 2 m / s, more preferably at least 3.5 m / s, e.g., up to 10 m / s or up to 20 m / s or up to 6 m / s, e.g., 3 to 4 m / s. The path of movement along at least one axis, preferably along each axis, is, e.g., 0.1 cm to 24 cm.
[0037] The container can, for example, be driven to move back and forth over a distance of at least 1 mm or at least 2.5 mm, at least 1 cm, more preferably at least 2 cm or at least 5 cm, at least 10 cm or at least 15 cm, e.g. up to 100 cm, up to 50 cm, up to 30 cm or up to 20 cm, along each axis. More preferably, the moving back and forth movement of the container is harmonic. The moving back and forth movement of the container can be linear in a first phase; in general, the trajectory is non-linear and can, for example, be sinusoidal, loop-shaped or arc-shaped, preferably along a so-called Lissajous figure or hypocycloid, which preferably lies in the plane or is two-dimensional, optionally three-dimensional.Preferably, the reciprocating movement is linear in a first phase and, in a second phase, is formed into a trajectory curve along at least two merging, non-linear path segments, each containing at least one vertex. This is because, in general, a non-linear path curve, e.g., a movement along a trajectory curve whose path segments each have at least one vertex, promotes the impact of solids and / or liquids and their mixing, e.g., perpendicular to the container wall, as well as a movement along the container wall.
[0038] The reciprocating movement preferably comprises the reciprocating movement along a trajectory curve comprising at least two, preferably at least three, more preferably at least four different trajectory segments, each of which has at least one vertex and preferably merges into one another in a temporal sequence, preferably in a program-controlled manner. Each of the movement axes along which the movements overlap to form a trajectory curve can be linear or arcuate, so that the non-linear movement of the container along a sequence of trajectory segments is generated from the superposition of the movements along two movement axes. The vertices and intermediate sections of a trajectory segment are determined by the frequency difference and / or the phase position of the superimposed reciprocating movements along at least two axes.In general, the device can be configured to change the frequency difference and / or the phase position during the reciprocating movement.
[0039] Generally, the container wall is preferably the circumferentially closed wall of the container, which extends around a central axis and between opposing end cross-sections or lids attached thereto. The container has an optionally circular cross-section that extends around a central axis and is spanned by the container wall. Generally, the end cross-sectional openings of the container are each covered by a lid, of which at least one optionally has a through-opening.
[0040] In general, it is preferred that at least one path segment has a vertex at which the direction of the path segment changes by at least 90°, more preferably by at least 120°, even more preferably by at least 180°, e.g., within a maximum of 24.5%, a maximum of 24%, a maximum of 23%, a maximum of 22%, a maximum of 21%, a maximum of 20%, a maximum of 15%, or a maximum of 10%, more preferably a maximum of 5%, a maximum of 3%, a maximum of 2%, or a maximum of 1% of the length of a path segment. This is because a vertex of the path segment leads to a strong relative acceleration of the solids and / or liquids and their mixing against the container.
[0041] A preferred method for producing a mixture, in which the container optionally has a wall with a smooth inner surface that spans the cross-section, is a method for producing a suspension of at least two powders in a liquid, preferably with a first step in which at least two powders are dry-mixed to produce a dry powder mixture, a second step in which a solvent, aqueous solvent, organic solvent or a mixture thereof is mixed into the powder mixture to produce a suspension in the solvent, and an optional third step in which at least one adhesive is mixed into the suspension in the solvent. In each step, the mixing by reciprocating motion can have a duration of a maximum of 50 s, preferably a maximum of 40 s or a maximum of 30 s, e.g. with the frequencies and accelerations of the reciprocating motion according to the invention.Optionally, all components of the mixture, in particular the powder, a solvent and adhesive, can be mixed in exactly one step, or the dry powder mixture can be prepared in a first step and, in a second step, adhesive can be mixed into the dry powder mixture as a mixture with or as a solution in solvent. At least one powder is preferably selected, and two powders are more preferably selected, from a powdered metal (oxidation state zero), a metal oxide, e.g. an alkali metal mixed oxide, e.g. LiCoO?, a conductive carbon compound, e.g. graphite, carbon black, fullerene, carbon nanotubes, graphene, and optionally a water-soluble alkali salt, e.g. a lithium salt. The solvent can be water, an organic solvent or a mixture of at least two of these; the adhesive can be, for example, CMC (carboxymethylcellulose) or SBR (styrene-butadiene rubber).Preferably, the powders are the components of an anode active material or a cathode active material or an electrolyte of a battery, in particular a lithium-ion battery, or an electrolyte for an electrical capacitor.
[0042] It has been shown that the process for producing an electrolyte for a lithium-ion battery has the advantage of producing better granularity, e.g., a grain size of maximum 20 μm, when each of the three steps lasts 30 s, compared to an Eirich intensive mixer with a mixing duration of 30 min each, which results in a granularity with a grain size of maximum 35 μm. Furthermore, it has been shown that lithium-ion batteries whose electrolyte mixture was produced using the process according to the invention in the mixing device, with each mixing step lasting 30 s, had a 10 to 30% higher battery capacity and also a lower tendency towards lithium plating on the anode and / or a lower tendency towards the formation of Li dendrites than batteries produced with a mixture of the same components, but with mixing in the Eirich intensive mixer, with each mixing step lasting 30 min.It is believed that the mixing process according to the invention leads to a more homogeneous distribution of the powder components and to less destruction of the adhesive.
[0043] The control of the drive of the container is optionally controlled depending on the signal from a sensor, preferably an acoustic sensor, which records vibrations, in particular noises of the container during the back and forth movement, in particular during the first and / or during the second phase. The acoustic sensor can, for example, be attached to the outer surface of the container or fixed at a distance from the container in a position past which the back and forth movement of the container passes. Preferably, the acoustic sensor is fixed at a short distance, e.g. 0.5 to 5 cm, from the apex of the back and forth movement, e.g. fixed to a frame relative to which the container is moved along the trajectory. The acoustic sensor can be a vibration sensor, e.g. a microphone.In this embodiment, the control of the reciprocating movement can be configured to allow the reciprocating movement to proceed at a changed speed and / or with a changed phase offset, and / or to control it from a linear movement to a curved path, in particular from a first phase to a second phase of the reciprocating movement, upon a change in the signal emitted by the acoustic sensor by a predetermined deviation within a predetermined time of the reciprocating movement, and / or upon reaching a predetermined signal emitted by the acoustic sensor. The sensor can also be an optical sensor attached to the container, e.g., a turbidity sensor.
[0044] Optionally, a device for generating electrical voltage is attached to the container, in particular a device with a magnet and a coil arranged so as to be movable relative to the magnet, which are configured to generate electrical voltage when moved relative to one another. This device is preferably connected by means of an electrical line to a transmitter attached to the container in order to supply the transmitter with electrical voltage. The transmitter is preferably connected by means of a data line to at least one of the sensors in order to receive sensor signals. The transmitter is configured, for example, to transmit received sensor signals. Furthermore, the sensor can be connected to the device for generating electrical voltage by means of an electrical line.In this embodiment, the device is configured so that a sensor and a transmitter attached to the container can be energized by the device for generating electrical voltage as soon as the container is moved along the trajectory curve. Accordingly, the device can be designed without an electrical cable extending between a frame, relative to which the container is moved, and the container.
[0045] Preferably, the container has a lower lid that can be opened or moved away from the interior volume to allow the mass to be removed, dropped out, or flowed out after the reciprocating movement. Further preferably, the container has an upper lid that can be moved away from the interior volume to allow the interior volume to be opened to allow the components of the initial composition to be added. In this way, the container can be used for a batch process after opening the upper lid, with subsequent closing of the interior volume by means of the upper lid, and after the reciprocating movement, opening a lower lid to allow the mass to drop out.Such openable upper and lower lids can be formed by only one lid if the container is moved from a first position in which one lid is arranged above the internal volume to a second position in which this lid is arranged below the internal volume, and the opposite cross-sectional opening of the container is closed by a fixed lid.
[0046] Optionally, the container is temperature-controlled, in particular cooled. The container can be cooled by arranging it in a cooled housing or by having a double jacket through which a coolant can flow.
[0047] In general, the container can have a triangular or square, optionally polygonal, cross-section, which can be closed at one end by a first lid and a second lid arranged at the opposite end. The container can be arranged such that one of the lids is located above the other lid; preferably, the container is arranged with its cross-section parallel to the horizontal. Preferably, the container has an oval or round cross-section, the end openings of which are covered by lids, which can be curved or flat. The container preferably comprises a cylindrical interior volume.In general, preferably in the case of a container having at least a triangular or polygonal cross-section, the movement can take place along a sequence of path segments, each having at least one vertex, preferably each path segment having a number of vertices equal to the number of corners of the container's cross-section. Alternatively or additionally, the number of vertices of each path segment can be equal to the number of corners of the container's cross-section. The vertices can, for example, encompass an angle that is at least twice as large, preferably at least three times as large, as the angle encompassed by one of the adjacent path curves.
[0048] Each lid may extend in the plane of the cross-section of the container or taper in a dome-shaped, preferably conical, manner from the terminal cross-section of the container.
[0049] The movement along two axes, or the reciprocating movement, can be driven by a drive motor, with the different frequencies of the movements along the axes being achieved, for example, by means of a sliding guide, an eccentric drive, and / or a gear. Alternatively, the reciprocating movement can be driven by two controlled drive motors. A drive motor can be a linear drive, e.g., an electric, hydraulic, or pneumatic linear drive, or a rotary motor.
[0050] To generate a rolling movement, the container has, for example, at least a triangular or square, preferably a pentagonal to octagonal, symmetrical or asymmetrical cross-section, preferably an oval or round cross-section, and the back and forth movement along the axes of movement takes place in a plane which runs, for example, approximately parallel to or at a small angle, e.g. of max. 20°, to this cross-section. The plane preferably runs parallel to the horizontal. The back and forth movement can be set to a rolling movement by changing the phase position of the movement along the axes. Accordingly, the frequency of the movement along each axis can optionally be changed over the duration of the back and forth movement and / or the phase position of the movement along the axes can be changed.In general, preferably in the case of a container having at least a triangular or polygonal cross-section, the movement can take place along a sequence of path segments, each having at least one vertex, preferably each path segment having a number of vertices equal to the number of corners of the container's cross-section. Alternatively or additionally, the number of vertices of each path segment can be equal to the number of corners of the container's cross-section. The vertices can, for example, encompass an angle that is at least twice as large, preferably at least three times as large, as the angle encompassed by one of the adjacent path curves.
[0051] The device can have a supply line for the contents at a terminal cross-sectional area of the container, e.g., one of the lids. This is because the reciprocating movement can extend over short distances, e.g., 2 to 50 cm, or up to 20 cm, or up to 10 cm, so that an elastic line attached to the container can follow this movement if this line is fixed at a distance from the container.
[0052] Preferably, the projections each extend at the same distance from the container wall, e.g. the projections can have end faces spaced from the container wall and lying in a common plane.
[0053] The container may have the projections formed integrally with the container wall.
[0054] The container can be made of metal, e.g., stainless steel, titanium, or cerium, plastic, or ceramic. The device and method have the advantage that there is no movable element within the container, such as a stirrer, so that even with abrasive ingredients, e.g., metal powders or metal oxide powders, no wear from a stirrer can occur.
[0055] It has been shown that the container, in particular its inner wall, can be made of plastic or ceramic, e.g. in the production of mixtures with abrasive ingredients, e.g. with metal powders and / or metal oxide powders, optionally dry or with a liquid ingredient. This is because the movement of the container leads to little or no abrasion of its inner wall, or the abrasion is insignificant in terms of quantity and / or composition for the dry mixture or suspension produced. For example, in the production of suspensions containing metal powder or metal oxide powder, abrasion released into the suspension from a container made of plastic or ceramic may be insignificant for the subsequent use of the suspension.
[0056] The ingredients can be, for example, combinations of at least two powders, e.g., metal powder of oxidation state 0, metal oxide powder, plastic particles, glass frit, or combinations of at least two of these, each optionally with a liquid ingredient or exclusively dry powders, or consist of them. The optional liquid ingredient can be aqueous or organic, e.g., a solvent, a polymer, e.g., polyethylene glycol, a surfactant, inorganic, or a combination of at least two of these.
[0057] Preferably, the container is closable and vacuumable, e.g. by means of a closable connection attached to the container or its lid, to which a vacuum source can be connected and which is closed once the vacuum is achieved.
[0058] The invention will now be described in more detail by way of example with reference to the figures shown in
[0059] - Fig. 1A shows an embodiment of the container in perspective view and, rotated, in Fig. 1B in longitudinal section,
[0060] - Fig. 2A to 2K show embodiments of projections of the container wall.
[0061] In the figures, the same reference numbers denote functionally identical elements.
[0062] Fig. 1A shows a container 1 which, as is generally preferred, has a circular cross-section, with a first access opening 4 arranged along the longitudinal axis 2 on a first lid 3 and a second access opening 6 arranged on the opposite second lid 5 along the longitudinal axis 2. The first lid 3 and the second lid 5 each cover an end cross-section of the container 1. These lids 3, 5 run in a funnel shape from the container 1 to one of the access openings 4, 6. Alternatively, the container 1 can have only one access opening 4, 6 arranged in one of the lids 3, 5, so that the filling and emptying of the container 1 can take place through only one common access opening 4, 6. Further alternatively, the lids 3, 5 can be detachably attached to the container 1.
[0063] A sensor 30, attached to the container 1, is connected via an electrical line 31 to a voltage generating device 32, which is attached to the container 1 and has a magnet movable relative to a coil. A transmitter 33 is connected to the sensor 30 via a data line 34 and to the voltage generating device 32 via an electrical line 35.
[0064] The longitudinal section through the container 1 shown in Fig. 1B shows the projections 10 in an embodiment in which the projections 10 are formed as webs 11 between openings 12. In the embodiment shown here, the webs 11 are spaced apart from the container wall 7.
[0065] Alternatively or in addition to the projections 10 formed by the webs 11 spaced apart from the container wall 7, projections 10 can be attached directly to the container wall 7 and project into the container 1.
[0066] Figs. 2A-K each show embodiments of projections 10 which are attached to the container wall 7 and project beyond it.
[0067] The embodiments shown in Fig. 2A to 2D form interconnected projections 10 as webs 11 between openings 12. The webs 11 can rest directly on the container wall 7 or be arranged at a distance from the container wall 7, as shown, for example, in Fig. 2B.
[0068] Fig. 2A shows webs 11 between circular bores 12, which form openings 12, the opening of which directed towards the container 1 has a chamfer 13.
[0069] Fig. 2B shows webs 11 between cylindrical bores forming openings 12 whose openings directed towards the container 1 have sharp edges 14 of 90°.
[0070] Fig. 2C shows webs 11 between perforations 12 with a triangular cross-section, whose openings facing the container 1 have sharp edges 14 of 90°. Fig. 2D shows webs 11 between perforations 12 formed as elongated holes, whose openings facing the container 1 have sharp edges 14 of 90°.
[0071] Figs. 2E and 2F show projections 10 formed as webs 11 between recesses 15, which are embossed or drilled into the container wall, for example, as blind holes or blind holes. Fig. 2E shows circular blind holes as recesses 15, Fig. 2F shows triangular blind holes.
[0072] Figs. 2G to 2K show separate projections 10 that project beyond the wall 7 of the container 1. The projections 10 may have end faces 16 that lie in a common plane that is spaced from the wall 7 and may be substantially parallel to the wall 7. The end faces may, for example, be triangular (Fig. 2G) or round (Fig. 2H) or rectangular (Fig. 2J).
[0073] Fig. 21 shows projections 10 projecting over a container wall 7, the two opposite side surfaces 17a of which converge to an end surface 16, while the intermediate side surfaces 17b extend perpendicular to the container wall 7.
[0074] Fig. 2J shows projections 10 projecting over a container wall 7, the side walls 17b of which all run perpendicular to the container wall 7 and the end faces 16 of which are rectangular and spaced from the container wall 7 in a common plane.
[0075] Fig. 2K shows projections 10 projecting beyond a container wall 7, forming a T-profile with a first section 18a that spaced a second section 18b from the container wall 7. The second section 18b, parallel to the container wall 7, has a larger cross-section than the first section 18a. Generally, both sections can have a rectangular cross-section, with the second section extending symmetrically or optionally offset from the first section.
[0076] Example 1 : Preparation of water-based cream
[0077] As an example of an emulsion that optionally does not contain an emulsifier, a cream was prepared from 30% by weight of an oily substance, the remainder being water, totaling 1 kg, in a generally cylindrical container with an internal volume of 4 l and a diameter of approximately 20 cm. The container wall had projections extending into the container. The projections were formed by webs consisting of a 2 mm thick cylindrical sheet with 5 mm diameter holes. These projections, formed by webs, extended across the entire container wall, and the end cross-sections were reversibly closed by flat lids.
[0078] The container was moved along two mutually perpendicular axes, which were located in the cross-sectional plane of the container and perpendicular to its longitudinal axis, respectively. Along one axis, the movement was carried out over a distance of at least 10 cm at a reciprocating frequency of 7.1 Hz, and along the other axis, the movement was carried out over a distance of at least 10 cm at a reciprocating frequency of 5.95 Hz. After a movement duration of 20 to 300 s, preferably only 30 s, the resulting mass was assessed as homogeneous and, after spreading on a glass, as free of droplets visible to the eye. The mass retained this homogeneity when stored for at least 3 days at room temperature.
[0079] Example 2: Production of paste with metal powder
[0080] As an example of a suspension, at least two different metal powders, each with a grain size of 5 to 120 pm, were placed in a container as a liquid with a volume of 500 ml sufficient to produce a paste.
[0081] A PEEK container or a ceramic container was used, each moving a distance of 6 cm along two axes at a frequency of 7.1 Hz along one axis and 5.95 Hz along the other axis, both perpendicular to the longitudinal center axis of the container, at a 90° phase angle. The container was round with a diameter of 18 cm and a height of 16 cm.
[0082] The container had a bottom and its upper opening was closed with a lid and the interior of the container was vacuumed through a connection in the lid.
[0083] After a reciprocating motion lasting 5 minutes, a paste was produced in which the different metal powders were evenly distributed. No gas bubbles were detected during visual inspection. Alternatively, for an anode active material, 90 wt.% graphite and 5 wt.% nanomicroscopic carbon as conductive carbon black were mixed for 30 s in a mixing device according to the invention in a first step with a reciprocating motion at a frequency of 7 Hz, a path along a first axis of 5 cm and a second axis perpendicular to this axis of 5 cm along a Lissajous figure. Subsequently, in a second step, water was added as a solvent and mixed under the same conditions for 30 s. Subsequently, in a third step, 3 wt.% CMC and 2 wt.% SBR were added and mixed again under the same conditions for 30 s, where wt.% in each case is based on the total dry mass.
[0084] For a cathode active material, under the same conditions, 90 wt% LiCoCh, 5 wt% nanomicroscopic carbon were mixed in a first step, water as solvent in a second step, and 3 wt% CMC and 2 wt% SBR were added in a third step.
[0085] A lithium-ion battery produced with this anode active material and this cathode active material had a 10 to 30% higher electrical capacity and a significantly lower tendency to Li dendrite formation than a battery whose anode active material and cathode active material were produced from the same starting materials but by mixing for 30 minutes for each step in the Eirich intensive mixer (has a rotating mixing element arranged eccentrically in a rotating mixing container).
[0086] Reference symbol:
[0087] 1 container 16 front face of projection
[0088] 2 Longitudinal axis 17a tapered side surface
[0089] 3 first cover 17b perpendicular to the container wall
[0090] 4 first access opening side panel
[0091] 5 second cover 18a first section of projection
[0092] 6 second access opening 18b second section of projection
[0093] 7 Container wall 30 Sensor
[0094] 10 projection 31 electrical cable
[0095] 11 Bridge 32 Device for generating electrical
[0096] 12 Recess as opening tension
[0097] 13 Phase 33 Transmitter
[0098] 14 sharp edge 34 data line
[0099] 15 Recess as blind hole 35 electrical cable
Claims
Claims: A method for producing a mixture comprising the steps of: a. providing a container which does not contain a mixing element movable relative to the container, having a cross-section spanned by a wall; b. filling the container with at least two ingredients; c. moving the container back and forth along a trajectory which comprises a sequence of trajectory segments which can be generated by superimposing the back-and-forth motion along at least two axes with different frequencies and / or with phase shifts, and which each comprise exactly one complete back-and-forth motion along the axis along which the back-and-forth motion with the lower frequency takes place, and which each have at least one vertex at which the direction changes by at least 90° within a maximum of 24.5% of the length of a trajectory segment.A method according to claim 1, characterized in that the wall spanning the cross-section has projections of 0.01 to 0.5 mm in height, arranged at intervals of 10 to 30 mm and projecting into the cross-section. A method according to any of the preceding claims, characterized in that the ingredients comprise a liquid ingredient and at least one metal powder and / or metal oxide powder, optionally graphite and / or conductive carbon black, or a combination of at least two of these, and that the container is made of plastic or ceramic.The method according to claim 3, characterized in that in a first step at least two powders are dry mixed to produce a dry powder mixture, in a second step at least one solvent is mixed into the powder mixture to produce a suspension in the solvent, and in a third step in which at least one adhesive is mixed into the suspension in the solvent, wherein in each step the mixing has a duration of at most 50s. A method according to any one of claims 1 to 2, characterized in that the ingredients are exclusively liquid ingredients. A method according to any one of the preceding claims, characterized in that the web segments have at least one vertex at which they change their direction by at least 120° within a maximum of 10% of the length of a web segment. A method according to any one of the preceding claims, characterized in that the container is vacuum-sealed after the ingredients have been added and before step c). A method according to any one of the preceding claims, characterized in that the frequencies and / or the phase shift are changed during the reciprocating motion. A method according to any one of claims 2 to 8, characterized in that the projections are formed by webs that enclose recesses between them.A method according to claim 9, characterized in that the webs have openings as recesses and that the webs are arranged at a distance from the wall. A method according to any one of claims 2 to 10, characterized in that the projections have a height of 1 / 20 to 1 / 10 of the mean diameter of the container. Use of a device in a method according to any one of the preceding claims with a container (1) which does not contain a mixing element movable relative to the container, having a cross-section spanned by a wall which is configured to drive the container (1) to a reciprocating motion along a trajectory, wherein the trajectory comprises a sequence of trajectory segments which can be generated by superimposing the reciprocating motion along at least two axes with different frequencies and / or with phase shifts and which each comprise exactly one complete reciprocating motion along the trajectory. The axis, along which the reciprocating motion occurs at the lower frequency, comprises at least one vertex at which the direction changes by at least 90° within a maximum of 24.5% of the length of a track segment. Use according to claim 12, characterized in that the wall spanning the cross-section has spaced-apart projections (10) projecting into the cross-section, with a height of 0.05 to 0.1 mm. Use according to any one of claims 12 to 13, characterized in that the difference in frequencies is at least 0.01 Hz and 0.01% to 900%, and the phase shift is 0.0028% to 50% of the length of a track segment. Use according to any one of claims 12 to 14, characterized in that the trajectory has at least one track segment comprising a straight section.Use according to one of claims 12 to 15, characterized in that reciprocating movements along the path curve are driven by a transmission which is a belt drive driven by exactly one motor or a friction wheel transmission driven by exactly one motor.Device for use in a method according to any one of claims 1 to 11, comprising a container (1) which does not contain a mixing element movable relative to the container, having a cross-section spanned by a container wall (7) with projections extending beyond the container wall (7) by at least 0.05 to 20 mm, wherein the device is configured to drive the container (1) to a back-and-forth movement along a trajectory, wherein the trajectory comprises a sequence of trajectory segments which can be generated by superimposing the back-and-forth movement along at least two axes with different frequencies and / or with phase shift, and which each comprise exactly one complete back-and-forth movement along the axis along which the back-and-forth movement with the lower frequency takes place, and each at least one The device according to claim 17, characterized in that the projections (10) are formed by webs (11) between which recesses are arranged as openings (12) or blind holes (15). The device according to any one of claims 17 to 18, characterized in that the projections (10) are separated from one another and extend beyond the container wall (7) to a common distance from the container wall (7). The device according to any one of claims 17 to 19, characterized in that the container wall (7) or the entire container (1) is made of plastic or ceramic. The device according to any one of claims 17 to 20, characterized in that the webs (11) are formed by a sheet metal plate spaced apart from the container wall (7), which has openings (12).A device according to any one of claims 17 to 21, characterized by a sensor (33) connected to a control unit configured to control the frequency of the reciprocating motion and / or the acceleration of the container (1) during the reciprocating motion depending on the signal from the sensor (33), and by a device (32) attached to the container (1) comprising a magnet and a coil movable relative to the magnet, which are configured to generate an electrical voltage when moving relative to each other and are connected by means of an electrical conductor (31) to a transmitter (33) attached to the container (1). A device according to claim 22, characterized in that the sensor (30) is an acoustic sensor attached to the container (1) or fixed at a distance from a turning point of the trajectory on a frame on which the container (1) is guided for reciprocating motion. Device according to one of claims 21 to 23, characterized in that the sensor (30) is attached to the container (1) and is connected to the transmitter (33) for transmitting sensor signals.