Apparatus and method for producing a mixture
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-02-27
- Publication Date
- 2026-03-18
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Abstract
Description
[Technical field]
[0001] The present invention relates to an apparatus for producing a mixture, e.g. a powder mixture or an emulsion, preferably with a liquid proportion, optionally in the form of a suspension (slurry), consisting of at least two ingredients, which are preferably insoluble in each other, and to a method, preferably carried out using said apparatus. [Background technology]
[0002] The device and method have the advantage of converting the raw material in a vessel into a mixture, preferably a pure powder mixture, suspension or emulsion, without any mixing elements, in particular a stirrer, being provided or included in the vessel that are movable relative to the vessel, so that the vessel is formed without bearings for the movable mixing elements.
[0003] The apparatus is configured for carrying out a mixing method, which results in intensive mixing of the ingredients in the vessel within a short period of time, for example within 10 hours, 8 hours, 6 hours, 4 hours, 2 hours, 1 hour, preferably within 5 minutes, 3 minutes, 120 seconds, 100 seconds, 60 seconds or 30 seconds, for example producing a powder mixture, suspension or emulsion of finely distributed (dispersed) and evenly distributed (dispersed) particles and / or liquid ingredients. In the case of liquid ingredients that are not soluble in each other, for example lipophilic and hydrophilic, emulsions are produced in which finely distributed fat or oil droplets have water or water droplets in the fat phase, so that they are stable without emulsifiers or surfactants.
[0004] The patent application WO 2005 / 023363 describes the production of meat products by subjecting raw meat pieces to a load in a vessel driven along two axes for a forced guided reciprocating motion at a frequency of at least 0.5 Hz. The raw meat pieces may, due to the load, absorb, for example, aqueous or oily compounds or adhere to each other.
[0005] Patent document 2 describes a mixing and kneading method for polymers with other ingredients, at least one of which is liquid, by reciprocating a container along two axes at different frequencies of at least 1 Hz. [Prior art documents] [Patent documents]
[0006] [Patent Document 1] International Publication No. 2015 / 114118 [Patent Document 2] European Patent Application Publication No. 3620067 Summary of the Invention [Problem to be solved by the invention]
[0007] The object of the present invention is to provide an apparatus and a method which can be carried out by means of the apparatus, which can effectively convert mutually insoluble raw materials into a homogeneous mixture and, in particular, on this basis produce homogeneously distributed powder mixtures, homogeneously distributed suspensions or emulsions. Preferably, the apparatus and the method should be suitable for producing homogeneous mixtures, stable emulsions, from at least two liquids which are insoluble in each other, the resulting emulsions being free of emulsifiers. [Means for solving the problem]
[0008] The present invention solves the above problem by the features of the claims and in particular provides an apparatus for use as a mixing device and a method for the production of a mixture by means of the apparatus, the apparatus comprising a container having a cross section of at least 5 mm diameter, the cross section being described by a wall, the wall preferably comprising spaced apart protrusions protruding into the cross section with a height of at least 0.05 mm or at least 0.1 mm, for example 0.05-0.5 mm or 0.2 mm or 0.1 mm, the protrusions being preferably distributed over the entire wall and / or the spacing between the protrusions may be, for example, 5-50 mm, alternatively the wall may have a smooth surface, the container being propelled into a reciprocating motion along a curved path, the reciprocating motion being obtained at different frequencies by superposition of motions along at least two axes at an angle to each other and preferably lying in the plane of the cross section of the container.
[0009] The vessel preferably has a circular cross section or a cross section having at least 3, at least 4, at least 5, at least 6, at least 7, at least 8, such as up to 20 corners respectively. The diameter of the vessel may for example be from 0.5 to 100 cm, for example from 10 or 20 to 80 cm or 60 cm respectively.
[0010] The cross section of the vessel may be angular, circular or oval. The cross section is subjected to a relative movement of the ingredients filled in the vessel against the vessel wall in a continuous motion, for example by a reciprocating motion along two axes that are in the plane of the vessel cross section at an angle to each other. It is speculated that the intensive and effective mixing of the ingredients by the method may be due to the continuous motion completely capturing the ingredients, for example without partial settling or separation of the ingredients.
[0011] The protrusion protruding into the cross section of the container has, for example, a height from the wall of 1 / 30 to 1 / 1 or 1 / 2 or 1 / 5 or 1 / 10 of the diameter of the container, for example 1 / 20 to 1 / 1 or 1 / 2 of the diameter of the container, in particular a height of 0.1 to 20 mm, for example at least 2 mm, at least 3 mm, at least 4 mm or at least 5 mm, for example up to 18 mm or up to 15 mm, respectively. The protrusion can have sides perpendicular to the container wall, for example cylindrical or cubic, and / or can have sides extending from the container wall at an angle of more than 95°, preferably more than 100° or 110° or 120°, for example conical or frustoconical, with at least a triangular cross section and one or two sides perpendicular to the container wall. The protrusion may comprise a second portion spaced from the container wall, the second portion having a larger cross section than a first portion joining the container wall with the second portion, e.g. T-shaped. Preferably, the protrusion has a side surface, the profile of which extends from the wall in an arcuate manner, and the side surface joins the wall in an arcuate manner.
[0012] The protrusions may be separate from one another or may be connected to one another as webs with recesses, for example in the form of openings or blind holes, arranged therebetween.
[0013] Typically, the protrusions can be formed as webs formed between recesses extending into the container wall. Such webs can be formed, for example, by recesses provided in the container wall or by lamellas provided in the container wall with openings or blind holes, for example as holes or slots, respectively. The openings can extend parallel or perpendicular to the cross section of the interior space or at an angle greater than 0° and less than 90° to the cross section of the interior space. Optionally, in addition or alternatively, the openings can extend along a radius extending from the longitudinal axis of the cross section described by the inner wall or at an angle of 10 to 45° to said radius. Optionally, the openings have a constant cross section or a cross section that increases with distance from the longitudinal axis. Optionally, the openings are provided with a chamfer, preferably arcuate, to avoid sharp edges adjacent to the cross section, or the openings are cylindrical or extend conically to widen from the longitudinal axis without a chamfer to form sharp edges.
[0014] In one embodiment, the sides of the protrusions transition continuously into the recesses formed therebetween.
[0015] In an alternative embodiment, the protrusion is spaced apart from the container wall so that the sides of the protrusion do not merge into or are not connected to the container wall. In this embodiment, the protrusion can be formed, for example, by a thin plate with an opening, for example a through circular hole or a non-through slot, which is provided at a distance from the container wall. Such a thin plate can be provided, for example, at a distance of 1 to 30 mm from the container wall, preferably parallel to the container wall, and can be connected to the container wall, for example by a support.
[0016] It has been found that protrusions extending across the vessel wall into the cross section of the vessel accelerate mixing of the ingredients during reciprocating motion of the vessel, as compared to, for example, a cylindrical vessel having flat walls.
[0017] According to the invention, mixing of the ingredients is preferably performed by movement of the container in a reciprocating motion along a path curve at a frequency of at least 1 Hz along two axes at different frequencies respectively over a distance along each axis of at least 2.5 mm, at least 1 cm, at least 2 cm or at least 3 cm or at least 10 cm, for example up to 50 cm, up to 30 cm, up to 20 cm or for shorter distances up to 10 cm.
[0018] The reciprocating movement of the container may extend over a distance of, for example, at least 1.5 mm, preferably at least 3 mm, preferably at least 1 cm, preferably at least 2 cm, or at least 5 cm, at least 10 cm, or at least 15 cm, for example up to 50 cm, up to 30 cm, or up to 20 cm. More preferably, the reciprocating movement of the container is harmonic along a path curve. The reciprocating movement of the container may be nonlinear and sinusoidal, loop-like or arcuate, preferably extending along a path curve that is preferably in a plane or two-dimensional, since in general, reciprocating movement along a nonlinear axis of movement, preferably a path curve that may be a Lissajous figure or a hypocycloid, promotes uniform and intensive mixing even in the components of a compound having similar or identical specific weights. Since each axis of movement itself may extend linearly, it is possible to produce a nonlinear movement of the container consisting of a superposition of movements along the two axes of movement. Optionally, the reciprocating movement may additionally extend into a third dimension perpendicular to the plane described by the first and second axes.
[0019] The container is brought into a reciprocating motion along at least one path curve, which can be generated by the superposition of reciprocating motions along at least two axes positioned at an angle to one another, preferably two of the axes being in the plane of the cross section of the container, and the reciprocating motions being performed along each axis at different frequencies and / or with a phase shift. The path curve can be generated by the superposition of reciprocating motions along two or three axes at different frequencies and / or with a phase shift, and comprises a series of path segments, at least one of which, preferably all of which, comprises or consists of exactly one complete reciprocating motion along an axis along which a reciprocating motion at a lower frequency is performed, and superimposed reciprocating motions at higher or the same frequency, each optionally with a phase shift, along one or more other axes, where the lower frequency of the complete reciprocating motion forms the frequency of the series of path segments. For each path segment, the frequency ratio of the reciprocating motion along the two axes is preferably at most 1:20 or at most 1:15 or at most 1:10, at most 1:4 or at most 1:3, more preferably 1:1 to 1:2, even more preferably greater than 1:1 to 1:2 or 1:1.5, for example having a frequency ratio of 1:1,001 to 1:2 or 1:1.5.
[0020] In the path curves which can be generated by the superposition of reciprocating motions along two axes at different frequencies and / or with phase shift, the axes are preferably in the plane of the cross section of the container. In the path curves formed by the superposition of reciprocating motions along three axes, preferably two axes are in the cross section of the container and the third axis is at an angle to said cross section. Here, the lowest frequency of a complete reciprocating motion along one of the three axes forms the frequency of the set of path segments. In general, the linear axes of motion are preferably at right angles to each other. In general, the path curve does not include a rotation of the container about its own axis.
[0021] Typically, the apparatus is configured to propel the container along a curved path formed by the superposition of reciprocating motions of at least two linear axes superimposed and angled relative to one another, the reciprocating motions along the linear axes being at different frequencies and / or out of phase, the linear axes along which the superimposed reciprocating motions extend at different frequencies and / or out of phase forming the curved path along which the container is reciprocated and for which the apparatus is configured.
[0022] By movement of the container along the path curve, the apparatus is configured to accelerate mixing relative to the container, such that solids and / or liquids contained in the container are sheared by acceleration against the container walls and by movement along or against the container walls, thereby resulting in intensive mixing.
[0023] Since the path curve can be set (adjustable) or predefined with different frequencies and / or phase shifts of the superimposed movements along the linear axis, the device is configured for reciprocating movement of the container along the path curve and for relative movement of solids and / or liquids and mixing relative to the container.
[0024] Typically the container is not rotationally driven, more preferably it is not rotatable or it is rotatably guided around its central axis by, for example, at most 30° or at most 20° or 10°, but is not fully rotatable. Typically and preferably the container is only propelled in a reciprocating motion along a path curve.
[0025] A settable or predefined path curve with different frequencies and / or phase shifts of the superimposed movements along at least two linear axes accelerates the solids and / or liquids and their mixture relative to the vessel. The reciprocating movement of the vessel propels the solids and / or liquids and their mixture into motion relative to the vessel wall.
[0026] The angles of entry and exit of the solids and / or liquids and mixtures thereof can be determined relative to the vessel wall by the path curve. Optionally, furthermore, the device is configured to move the vessel along the path curve with settable acceleration and velocity or with predefined acceleration and velocity. The device is configured for a settable or predefined path curve and / or settable or predefined acceleration and / or settable or predefined velocity along the path curve of the reciprocating motion of the vessel, so that the solids and / or liquids and mixtures thereof are propelled relative to the vessel with settable or predefined acceleration and / or settable or predefined velocity, allowing a predefined or continuous adaptation of the method to the solids and / or liquids and mixtures. In general, the path curve can be formed with at least two superimposed individual vibrations, preferably the path curve resembles a path curve that can be generated by superposition of reciprocating motions along at least two linear axes of motion at different frequencies and / or with phase shift. Reciprocating motions along path curves similar to reciprocating motions along superimposed mutually orthogonal linear axes of motion have different frequencies and / or phase shifts relative to each other, so that in general, optionally the path curves do not have circular orbits.
[0027] The frequency difference may be, for example, 0.01 Hz and / or 0.01-900%. The phase shift of the reciprocating motion along the linear axis may be, for example, 0.01-180°, preferably 1-179° out of 360° corresponding to a complete reciprocating motion. In this case, 0.01-180° of a complete reciprocating motion of 360° is equivalent to 0.0028-50% of a complete reciprocating motion, and 1-179° of a complete reciprocating motion of 360° is equivalent to 0.28-49.7% of a complete reciprocating motion.
[0028] In this case, the linear axes of movement are perpendicular to each other or at another angle, for example between 5 and 85°, in particular in the plane of the cross section of the container and / or perpendicular to the central axis of the container. Optionally, the path curve comprises at least one straight line portion, the end of which is for example a vertex of the path curve, at which the solids and / or liquids and mixtures thereof are accelerated by or against the container wall.
[0029] To set (adjust) different frequencies and / or phase shifts of the superimposed reciprocating movements along at least two linear axes of movement, said reciprocating movements can be related to one another by a transmission or a link guide and driven by a motor. In this case, the motor-driven transmission, which sets the reciprocating movements along the path curve, can have a fixed (constant) or adjustable gear ratio between the superimposed movements along each axis and can be, for example, a continuously or steplessly switchable gear. Optionally, the gear can be subject to slip, for example a belt drive, or can be a friction gear.
[0030] The driven speed of the gearing driving the reciprocating motion of the container is preferably at least 1 Hz, preferably at least 2.5 Hz, preferably at least 5 Hz, preferably at least 7 Hz, for example up to 50 Hz, up to 40 Hz, up to 30 Hz, up to 20 Hz or up to 10 Hz, where the driven speed of the gearing is the same as the frequency of the reciprocating motion.
[0031] Alternatively, the reciprocating motion along each linear axis of motion can be driven by a separate motor, with the lower driven rotational frequency being the frequency of the reciprocating motion and forming the frequency of the series of path segments for the purposes of the present invention. In all embodiments, the rotational frequency of each drive motor can be controlled and can be fixed (constant) set or can be variable over the duration of the method.
[0032] The device then allows a path curve to accelerate the solids and / or liquids and mixtures thereof in a predefined direction towards a target location on the vessel wall, where the geometry of the vessel and its inner wall can be supported in relation to the path curve of the mixing process, so that the path curve can be set depending on the shape and size of the vessel cross section.
[0033] Optionally, the apparatus is configured to modify the path curve of the reciprocating motion and / or the acceleration and / or speed of the reciprocating motion during the method, e.g. by setting (adjusting) in a first step a reciprocating motion along a first path curve and with a first acceleration and speed, and subsequently by setting (adjusting) in a second step a reciprocating motion along a modified path curve and / or with a modified acceleration and / or speed.
[0034] Further optionally, in a first stage the reciprocating motion is a linear reciprocating motion and in a second stage the reciprocating motion is a reciprocating motion along a path curve that transitions into one another, where the path curve can be defined, for example, by a gearing that drives the movement of the container.
[0035] The device allows for predefined or dynamically changeable and oriented acceleration of the process product relative to the vessel by setting (adjusting) the path curve and acceleration of the reciprocating motion of the vessel. In one embodiment where the vessel may be controlled to be propelled in a linear reciprocating motion in a first stage, the device is configured to move solids and / or liquids and mixtures thereof perpendicular to the vessel wall with a controllable acceleration that is much greater than and thus essentially independent of the acceleration of gravity, e.g., 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. 500m / s 2It has a maximum acceleration of up to
[0036] Typically, the device will have a speed of at least 20 m / s 2 Or at least 100 m / s 2 , e.g. at least 200 m / s 2 , preferably 1000 m / s 2 Up to 300m / s 2 The acceleration vector may be configured to accelerate the container along the path segment with an acceleration maximum value up to 100 Hz, for example at an apex of the path segment.
[0037] The vessel preferably has a velocity of at least 0.5 m / s 2 or at least 1 m / s2 or at least 2 m / s 2 , at least 3.5m / s 2 , preferably at least 60 m / s 2 , preferably at least 100 m / s 2 , at least 150 m / s 2 , at least 160m / s 2 , at least 200m / s 2 , e.g. 300m / s 2 or 450 m / s 2 Up to 260m / s 2 Up to 250m / s 2 The container is propelled into a reciprocating motion along each of the two axes with an acceleration maximum of up to 0.5 m / s, preferably at least 2 m / s, preferably at least 3.5 m / s, for example up to 10 m / s or up to 20 m / s or up to 6 m / s, for example 3-4 m / s, respectively along one of the axes, preferably along each of the axes, where the distance of the movement along at least one axis, preferably along each axis, is for example 0.1-24 cm.
[0038] The container can be propelled into a reciprocating motion extending along each axis over a distance of, for example, at least 1 mm or at least 2.5 mm, at least 1 cm, preferably at least 2 cm, or at least 5 cm, at least 10 cm or at least 15 cm, for example up to 100 cm, 50 cm or up to 20 cm, respectively. More preferably, the reciprocating motion of the container is harmonic. The reciprocating motion of the container is non-linear in a first stage, and in general the path curve is non-linear and may be, for example, sinusoidal, loop-like or arcuate, preferably extending along a so-called Lissajous figure or hypocycloid, preferably lying in a plane or in two dimensions, optionally in three dimensions. Preferably, the reciprocating motion is linear in a first stage and along at least two mutually transitioning non-linear path segments in a second stage, said path segments each forming at least one vertex for the path curve. This is because, in general, movement along a non-linear path curve, e.g., a path curve in which each path segment has at least one vertex, promotes collision of solids and / or liquids and mixtures thereof, e.g., perpendicular to a container wall and movement along the container wall.
[0039] Preferably, the reciprocating motion comprises a reciprocating motion along a path curve comprising at least two, preferably at least three, more preferably at least four different path segments each having at least one apex and preferably transitioning into one another in a time sequence, preferably program-controlled. Each axis of motion along which motion is superimposed onto the path curve may itself extend linearly or arcuately, thus making it possible to produce a non-linear motion of the container along a series of path segments consisting of a superposition of motions along two axes of motion. The apexes of the path segments and the portions therebetween are determined by the frequency difference and / or phase position of the superimposed reciprocating motions along at least two axes. In general, the device may be configured to vary the frequency difference and / or phase position during the reciprocating motion.
[0040] Typically, the container wall is a generally closed wall of the container extending about the central axis and between the opposing cross sections or covers at the respective ends. The container optionally has a circular cross section extending about the central axis and described by the container wall. Typically, the cross section openings at the respective ends of the container are preferably covered by covers, and optionally at least one of the covers is provided with a through opening.
[0041] Generally, it is preferred that at least one path segment has a vertex where the direction of the path segment changes by at least 90°, preferably at least 120°, more preferably at least 180°, for example by no more than 24.5%, no more than 24%, no more than 23%, no more than 22%, no more than 20%, no more than 15% or no more than 10%, more preferably no more than 5%, no more than 3%, no more than 2% or no more than 1% of the length of the path segment, since the vertex of the path segment results in a large relative acceleration of solids and / or liquids and mixtures thereof with respect to the container.
[0042] A preferred method for producing a mixture, the container having an optionally cross-sectional smooth inner surface, is a method for producing a suspension of at least two powders in a liquid, preferably comprising 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, an aqueous solvent, an organic solvent or a mixture thereof is mixed into the powder mixture to produce a suspension in a solvent, and an optional third step in which at least one adhesive is mixed into the suspension in the solvent, whereby in each step the mixture can have a duration of up to 50 seconds, preferably up to 40 seconds or up to 30 seconds, for example by reciprocating motion at the frequency and acceleration according to the invention of the reciprocating motion. Optionally, all components of the mixture, in particular the powders, the solvent and the adhesive, can be mixed in just one step, or first a dry powder mixture is produced in a first step, and in a second step the adhesive is mixed into the dry powder mixture with or as a solution in the solvent. In this case, at least one powder, preferably two powders, are selected from powdered metals (zero oxidation stage), metal oxides, such as alkali metal mixed oxides, for example LiCoO2, conductive carbon compounds, such as graphite, carbon black, fullerenes, carbon nanotubes, graphene, and optionally water-soluble alkali salts, such as lithium salts. The solvent may be water, an organic solvent or a mixture of at least two of them, and the adhesive may be, for example, CMC (carboxymethylcellulose) or SBR (styrene butadiene rubber). Preferably, the powder is a component of an anode active material or a cathode active material or an electrolyte for a battery, in particular a lithium-ion battery, or an electrolyte for an electrical capacitor.
[0043] It has been found that the method for producing electrolytes for lithium ion batteries has the advantage that a better particle size is produced, for example up to 20 pm, when each of the three steps lasts 30 seconds, instead of compared with an Eirich Intensive Mixer with a mixing duration of 30 minutes each resulting in a particle size of up to 35 pm. Furthermore, it has been found that lithium ion batteries in which the electrolyte mixture is produced with the method according to the invention in a mixing device with each step for 30 seconds of mixing have a 10-30% higher battery capacity and a lesser tendency to lithium plating at the anode and / or a lesser tendency to the formation of lithium dendrites than batteries with the same mixture of components but produced with the mixture in an Eirich Intensive Mixer with each step for 30 minutes of mixing. It is presumed that the mixing method according to the invention results in an even distribution (dispersion) of the powder components and less crushing of the adhesive.
[0044] The control of the propulsion of the container is optionally controlled depending on the signal of a sensor, preferably an acoustic sensor, which receives vibrations, in particular noises of the container during the reciprocating motion, in particular during the first and / or second phase. The acoustic sensor can be attached, for example, to the outer surface of the container or can be fixed at a distance from the container at a point where the reciprocating motion of the container passes by. Preferably, the acoustic sensor is fixed, for example, to a frame at a small distance, for example 0.5-5 cm, from the apex of the reciprocating motion, the container moving along a path curve relative to the frame. The acoustic sensor can be a vibration sensor, for example a microphone. In this embodiment, the control of the reciprocating motion can be configured to control the reciprocating motion with a changed speed and / or a changed phase shift and / or from a linear motion to a path curve, in particular from the first to the second phase of the reciprocating motion, when the signal emitted by the acoustic sensor changes by a predetermined deviation within a predetermined time of the reciprocating motion and / or when a predetermined signal emitted by the acoustic sensor is reached. The sensor may be an optical sensor, for example a turbidity sensor, attached to the vessel.
[0045] Optionally, a voltage generating device, in particular a device having a magnet and a coil arranged movably relative to the magnet, configured to generate a voltage in a relative movement relative to each other, is attached to the container. The device is connected to a transmitter attached to the container, preferably by means of an electric line, in order to apply a voltage to the transmitter. The transmitter is connected to at least one of the sensors, preferably by means of a data line, in order to receive a sensor signal. The transmitter is then configured, for example, to transmit the received sensor signal. Furthermore, the sensor can be connected to the voltage generating device by means of an electric line. In this embodiment, the device is configured such that the sensor and the transmitter attached to the container can be energized by the voltage generating device when the container moves along the path curve. Correspondingly, the device can be formed without an electric cable extending between the container and a frame relative to which the container moves.
[0046] Preferably, the container comprises a lower cover, which can be opened or moved away from the internal volume so that the internal volume can be opened for removal or withdrawal or flow-out of the mixture after the reciprocating motion. Furthermore, preferably, the container comprises an upper cover, which can be moved away from the internal volume so that the internal volume can be opened for filling with the components of the initial composition. In this way, the container can be affected in a batchwise manner after the opening of the upper cover, by subsequent closing of the internal volume with the upper cover and by opening the lower cover after the reciprocating motion to withdraw the mixture. The upper and lower covers, by which the container should be opened and closed in this way, can be formed by only one cover, if the container moves from a first place where one cover is arranged above the internal volume to a second place where the cover is arranged below the internal volume, and the cross-sectional opening on the opposite side of the container is closed with a fixed cover.
[0047] Optionally, the container is thermostated, in particular cooled. The container can be cooled by placing it in a cooled housing or by providing a double jacket through which a cooling medium can flow.
[0048] Generally, the container may have a triangular or square, alternatively polygonal, cross section, which may be closed at one end by a first cover and at the opposite end by a second cover. The container may be arranged such that one of the covers is arranged above the other, preferably the covers are arranged parallel to the horizontal line in its cross section. Preferably, the container has an oval or circular cross section, the end opening of which is covered by a cover which may be arched or flat. Preferably, the container encloses a cylindrical internal volume. Generally, movements along a series of path segments may be performed in a container, preferably with at least a triangular or polygonal cross section, the path segments having at least one vertex, preferably each path segment having the same number of vertices as the number of corners of the cross section of the container. Alternatively or additionally, the number of vertices of each segment may be the same as the number of corners of the cross section of the container. The vertex may for example include an angle at least twice, preferably at least three times, the angle included by one of the adjacent path curves.
[0049] Each cover may extend in the plane of the cross section of the container or may taper from the cross section of the distal end of the container in a dome-like, preferably conical, manner.
[0050] The movement along the two axes or the reciprocating movement can be driven by a drive motor, the different frequencies of the movement along the axes being achieved, for example, by means of link guides, eccentric drives and / or gearing. Alternatively, the reciprocating movement can be driven by two controlled drive motors. The drive motors can be linear drives, for example electric or hydraulic or pneumatic linearly acting drives or rotary motors.
[0051] The container has a symmetric or asymmetric cross section, for example at least triangular or quadrangular, more preferably pentagonal to octagonal, preferably oval or circular, for generating a rolling movement, and the reciprocating movement along the axis of movement is performed in a plane that extends at a small angle, for example at most 20°, to the cross section, for example approximately parallel to the cross section. Preferably, the plane extends parallel to the horizontal line. The reciprocating movement can then be set (adjusted) for the rolling movement by changing the phase position of the movement along the axis. Correspondingly, the frequency of the movement along each axis can be optionally changed over the duration of the reciprocating movement and / or the phase position of the movement along the axis can be changed. In general, the movement along a series of path segments can be performed in a container having at least a triangular or polygonal cross section, the path segment having at least one vertex, preferably each path segment having the same number of vertices as the number of corners of the cross section of the container. Alternatively or additionally, the number of vertices of each segment can be the same as the number of corners of the cross section of the container. A vertex may, for example, subtend an angle that is at least twice, and preferably at least three times, the angle subtended by one of the adjacent path curves.
[0052] The device can be provided with an elastic line, for example a polymer hose, in the cross section of the end of the container, for example in the cover, a supply line for the ingredient, because the reciprocating movement can extend over a short distance, for example 2-50 cm, or up to 20 cm, or up to 10 cm, so that the elastic line fixed to the container can follow the movement when the line is fixed in position away from the container.
[0053] Preferably, the projections each extend the same distance from the container wall, for example the projections may have end faces spaced from the container wall that lie in a common plane.
[0054] The container may include a protrusion integrally formed with the container wall.
[0055] The vessel can be made of metal, such as stainless steel, titanium or cerium, or synthetic resin or ceramic. The apparatus and method have the advantage that there are no moving elements in the vessel relative to the vessel, such as the stirrer, so that abrasive raw materials, such as metal powders or metal oxide powders, do not cause wear of the stirrer.
[0056] It has been found that the container, and in particular its inner wall, can be made of synthetic resin or ceramic, for example when producing mixtures with abrasive raw materials, for example metal powders and / or metal oxide powders, optionally with dry or liquid raw materials, since the movement of the container leads to little or no wear of its inner wall, or the wear is not significant in amount and / or composition for the dry mixture or suspension produced. Thus, for example when producing suspensions containing metal powders or metal oxide powders, abrasion released from a container made of synthetic resin or ceramic into the suspension may not be significant for the subsequent use of the suspension.
[0057] The raw materials may be, for example, at least two powders, such as metal powders at oxidation stage 0, synthetic resin particles, glass frits, or a combination of at least two of these, each of which may optionally comprise or consist of only liquid raw materials or dry powders. The optional liquid raw materials may be aqueous or organic, for example solvents, polymers, such as polyethylene glycol, surfactants, inorganic, or a combination of at least two of these.
[0058] Preferably, the container is closable and evacuable, for example by a closable connection attached to the container or its cover, to which a vacuum source can be connected and which is closed after the vacuum is achieved.
[0059] The invention will now be explained more precisely by way of example with reference to the drawings, in which: [Brief description of the drawings]
[0060] [Figure 1A] FIG. 1 illustrates one embodiment of a container in perspective view. [Figure 1B] FIG. 1 shows one embodiment of a container in longitudinal section. [Figure 2A] 13A-13C show embodiments of protrusions on the container wall. [Figure 2B] 13A-13C show embodiments of protrusions on the container wall. [Figure 2C] 13A-13C show embodiments of protrusions on the container wall. [Figure 2D] 13A-13C show embodiments of protrusions on the container wall. [Figure 2E] 13A-13C show embodiments of protrusions on the container wall. [Figure 2F] 13A-13C show embodiments of protrusions on the container wall. [Figure 2G] 13A-13C show embodiments of protrusions on the container wall. [Figure 2H] 13A-13C show embodiments of protrusions on the container wall. [Figure 2I] 13A-13C show embodiments of protrusions on the container wall. [Figure 2J] 13A-13C show embodiments of protrusions on the container wall. [Figure 2K] 13A-13C show embodiments of protrusions on the container wall. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0061] In each figure, functionally identical elements are labeled with the same reference numerals.
[0062] 1A shows a container 1 with a generally preferably circular cross section, with a first access opening 4 in a first cover 3 along a longitudinal axis 2 and a second access opening 6 in an opposite second cover 5 along the longitudinal axis 2. The first cover 3 and the second cover 5 each cover an end cross section of the container 1. The covers 3, 5 extend from the container 1 in a funnel-like manner to the access openings 4, 6. Alternatively, the container 1 can have only one access opening 4, 6 in one of the covers 3, 5, so that the container 1 can be filled and emptied only via the common access opening 4, 6. Furthermore, alternatively, the covers 3, 5 can be removably provided on the container 1.
[0063] A sensor 30 mounted on the vessel 1 is connected by means of an electric line 31 to a device for generating a voltage 32, which comprises a magnet mounted on the vessel 1 and movable relative to a coil. A transmitter 33 is connected to the sensor 30 by means of a data line 34 and to the device for generating a voltage 32 by means of an electric line 35.
[0064] 1B shows the protrusions 10 in an embodiment in which they are formed as webs 11 between the through holes 12. The webs 11 are spaced apart from the container wall 7 in the embodiment shown here.
[0065] Instead of or in addition to the projections 10 formed by webs 11 spaced apart from the container wall 7, it is possible to provide projections 10 directly on the container wall 7 projecting into the container 1.
[0066] 2A to 2K each show an embodiment of a protrusion 10 that is provided on the container wall 7 and protrudes from the container wall.
[0067] The embodiment shown in Figures 2A-2D forms the interconnected protrusions 10 as webs 11 between the through holes 12. The webs 11 can then be located directly on the container wall 7 or can be spaced apart from the container wall 7 as shown in Figure 2B.
[0068] FIG. 2A shows webs 11 between the circular holes 12 which form the through holes 12, the opening 12 of which facing the container 1 is provided with a chamfer 13.
[0069] FIG. 2B shows cylindrical inter-hole webs 11 forming through holes 12, the opening of which facing towards the container 1 being provided with a 90° acute edge 14.
[0070] FIG. 2C shows webs 11 between the through holes 12 which have a triangular cross section, the openings of the through holes facing the container 1 being provided with an acute edge 14 of 90°.
[0071] FIG. 2D shows webs 11 between the through holes 12 which are formed as slots, the openings of which facing the container 1 are provided with an acute edge 14 of 90°.
[0072] Figures 2E and 2F show protrusions 10 formed as webs 11 between recesses 15, which are cut or drilled into the container wall, for example as blind or blind holes. Figure 2E shows circular blind holes as recesses 15, and Figure 2F shows triangular blind holes.
[0073] 2G-2K show separate projections 10 projecting from a wall 7 of the container 1. The projections 10 may have end faces 16, which lie in a common plane spaced apart from and essentially parallel to the wall 7. The end faces may be, for example, triangular (FIG. 2G) or circular (FIG. 2H) or rectangular (FIG. 2J).
[0074] FIG. 2I shows a protrusion 10 protruding from the container wall 7, with two opposite sides 17a of the protrusion extending to the end face 16, while the side 17b therebetween extends perpendicular to the container wall 7.
[0075] FIG. 2J shows a protrusion 10 protruding from the container wall 7, with all of the side walls 17b of the protrusion extending perpendicular to the container wall 7, and with the end faces 16 of the protrusion being rectangular and spaced apart from the container wall 7 in a common plane.
[0076] 2K shows a projection 10 protruding from the container wall 7 with a first portion 18a spacing a second portion 18b away from the container wall, said projection forming a T-shaped cross section, where the second portion 18b has a larger cross section parallel to the container wall 7 than the first portion 18a. In general, both portions may have a rectangular cross section, the second portion extending symmetrically with respect to the first portion or optionally offset with respect to the first portion.
[0077] Example 1: Preparation of a moisturizing cream As an example for an emulsion that does not optionally contain an emulsifier, a cream was produced with a total of 1 kg of oily substance at 30% by weight, the remainder water, in a container with an internal volume of 4 liters, a roughly cylindrical shape with a diameter of about 20 cm, and a wall with a protrusion protruding into the container. The protrusion was formed by a web made of a cylindrical lamella with a thickness of 2 mm, with a hole with a diameter of 5 mm in it. The protrusion formed by the web extended over the entire container wall, and the end cross section was reversibly closed by a flat cover.
[0078] The container is moved along two mutually perpendicular axes, either in the transverse plane of the container or perpendicular to the longitudinal axis, along one axis over a distance of at least 10 cm in a reciprocating motion with a frequency of 7.1 Hz, and along the other axis over a distance of at least 10 cm in a reciprocating motion with a frequency of 5.95 Hz. After a period of movement of 20 to 300 seconds, preferably only 30 seconds, the resulting mixture (compound) is evaluated as being homogeneous and having no visible droplets after exposure on glass. The mixture retains said homogeneity upon storage at room temperature for at least 3 days.
[0079] Example 2: Production of a paste with metal powder As an example for a suspension, at least two different metal powders, each having a particle size of 5 to 120 pm, were placed in a container with a volume of 500 ml of liquid sufficient to make a paste.
[0080] A container made of PEEK as a synthetic resin or a container made of ceramic was used, and the container was moved along two axes perpendicular to the longitudinal central axis of the container by a distance of 6 cm, at a frequency of 7.1 Hz along one axis and at a frequency of 5.95 Hz along the other axis, with a phase position of 90°. The container was circular with a diameter of 18 cm and a height of 16 cm.
[0081] The container had a bottom and its upper opening was closed with a cover, and a vacuum was applied inside the container by a connection in the cover.
[0082] After 5 minutes of continued reciprocating motion, a paste was produced in which the different metal powders were evenly distributed, and no air bubbles were found upon visual inspection.
[0083] Alternatively, for the anode active material, 90% by weight of graphite and 5% by weight of nanofine carbon as conductive carbon black are mixed in a mixer according to the present invention in a first step with a reciprocating motion at a frequency of 7 Hz along a first axis at a distance of 5 cm and along a Lissajous figure at a distance of 5 cm along a second axis perpendicular thereto for 30 seconds, after which in a second step water is added as a solvent and mixed under the same conditions for 30 seconds, followed by the addition in a third step of 3% by weight of CMC and 2% by weight of SBR and mixing again under the same conditions for 30 seconds, where the weight percentages are for the total dry mix, respectively.
[0084] For the cathode active material, under the same conditions, 90 wt% LiCoO2 and 5 wt% fine carbon were mixed in the first step, water as a solvent was mixed in the second step, and 3 wt% CMC and 2 wt% SBR were added in the third step.
[0085] Lithium ion cells (lithium ion batteries) fabricated with the anode active material and the cathode active material had 10-30% more electrical capacity and were inherently less prone to lithium dendrite formation than cells fabricated by mixing in an Eirich Intensive Mixer (having a rotating mixing element eccentrically positioned in a rotating mixing vessel) for 30 seconds for each step, where the anode active material and the cathode active material were made from the same raw materials. [Explanation of symbols]
[0086] 1 container 2 Longitudinal axis 3 First Cover 4 First Access Opening 5 Second Cover 6 Secondary Access Opening 7 Container wall 10 Protrusion 11. Web 12 Recesses as openings 13 Chamfer 14 Sharp edges 15 Recesses as blind holes 16 End face of protrusion 17a Tapered Sides 17b Side perpendicular to the container wall 18a First portion of protrusion 18b Second part of the protrusion 30 Sensors 31 Electric Line 32 Devices that generate voltage 33 Transmitter 34 Data Line 35 Electrical Line
Claims
1. a. A step of providing a container having a cross-section drawn by a wall portion, which does not include a mixing element that is relatively movable relative to the container, b. A step of filling the container with at least two raw materials, c. A method for producing a mixture by the step of moving the container back and forth along a path curve that includes a series of path segments, The method is characterized in that the path segment can be generated by superimposing reciprocating motions at different frequencies and / or phase differences along at least two axes, each of which includes exactly one complete reciprocating motion along the axis where the reciprocating motion is performed at a lower frequency, and each of which has at least one vertex where the direction changes by at least 90° within a maximum of 24.5% of the length of the path segment.
2. The method according to claim 1, characterized in that the wall portion that draws the cross-section is provided with protrusions having a height of 0.01 to 0.5 mm that protrude into the cross-section, arranged at intervals of 10 to 30 mm.
3. The method according to 1 or 2, characterized in that the raw materials include a liquid raw material, at least one metal powder and / or metal oxide powder, and optionally graphite and / or conductive carbon black, or a combination of at least two of these, and the container is made of synthetic resin or ceramic.
4. The method according to claim 3, characterized in that, in the first step, at least two powders are dry-mixed to produce a dry powder mixture; in the second step, at least one solvent is mixed into the powder mixture to produce a suspension in the solvent; and in the third step, at least one adhesive is mixed into the suspension in the solvent, and in each of the above steps, the mixture is mixed for a maximum of 50 seconds.
5. The method according to 1 or 2, characterized in that the raw materials consist only of liquid raw materials.
6. The method according to 1 or 2, characterized in that the path segment has at least one vertex that changes its direction by at least 120° within a maximum of 10% of the length of the path segment.
7. The method according to 1 or 2, characterized in that the container is vacuumed after filling with the raw material and before step c).
8. The method according to 1 or 2, characterized in that the frequency and / or the phase shift changes during the reciprocating motion.
9. The method according to the 2nd method, characterized in that the protruding portion is formed by a web and there is a recess between the webs.
10. The method according to 9, characterized in that the web has an opening as a recess, and the web is spaced apart from the wall.
11. The method according to 2, 9, or 10, characterized in that the protruding portion has a height of 1 / 20 to 1 / 10 of the average diameter of the container.
12. Use of the apparatus according to claim 1 or 2, wherein the apparatus is configured to cause the container (1) to reciprocate along a path curve, the path curve comprising a series of path segments, the path segments being generated by superimposing reciprocating motions at different frequencies and / or phase differences along at least two axes, each comprising exactly one complete reciprocating motion along the axis at a lower frequency, and each having at least one vertex where the direction changes by at least 90° within a maximum of 24.5% of the length of the path segment.
13. The use according to claim 12, characterized in that the wall portion that draws the cross-section is provided with projections (10) having a height of 0.05 to 0.1 mm that are spaced apart and protrude into the cross-section.
14. The use according to claim 12, characterized in that the frequency difference is at least 0.01 Hz and 0.01 to 900%, and the phase shift is 0.0028 to 50% of the length of the path segment.
15. The use according to claim 12, characterized in that the path curve comprises at least one path segment including a straight portion.
16. The use according to claim 12, characterized in that the reciprocating motion along the aforementioned path curve is driven by a transmission device, and the transmission device is either a belt drive unit driven by exactly one motor, or a friction transmission device driven by exactly one motor.
17. Apparatus for use in the method of claim 1 or 2, wherein the container (1) has a cross section drawn by a wall portion (7) having a projection that protrudes at least 0.05 to 20 mm from the container wall portion (7), and does not include a mixing element that is movable relative to the container, wherein the apparatus is configured to reciprocate the container (1) along a path curve, the path curve comprising a series of path segments, the path segments being generated by superimposing reciprocating motions at different frequencies and / or phase differences along at least two axes, each comprising exactly one complete reciprocating motion along the axis where the reciprocating motion is performed at a lower frequency, and each having at least one vertex where the direction changes by at least 90° within a maximum of 24.5% of the length of the path segment.
18. The apparatus according to claim 17, characterized in that the protruding portion (10) is formed by a web (11), and a recess as an opening (12) or a blind hole (15) is disposed between the webs.
19. The apparatus according to claim 17, characterized in that the protruding portions are separated from each other, and the container wall portion (7) protrudes from the container wall portion (7) to a common distance.
20. The apparatus according to claim 17, characterized in that the container wall portion (7) or the entire container (1) is made of synthetic resin or ceramic.
21. The apparatus according to claim 17, characterized in that the web (11) is formed of a thin plate provided spaced apart from the container wall portion (7) and having the opening (12).
22. The apparatus according to claim 17, characterized in that a sensor (33) is 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 a signal from the sensor (33), and the container (1) is provided with a device having a magnet and a coil arranged to be movable relative to the magnet, wherein the magnet and the coil are configured to generate a voltage when they are in relative motion with respect to each other, and are connected to a transmitter (33) provided in the container (1) using an electrical line (31).
23. The apparatus according to claim 22, characterized in that the sensor (30) is an acoustic sensor, and the acoustic sensor is fixed to the container (1) or installed on a platform that guides the container (1) for reciprocating motion, at a distance from the turning point of the path curve.
24. The apparatus according to claim 21, characterized in that the sensor (30) is fixed to the container (1) and connected to the transmitter (33) for transmitting sensor signals.