EP3727626A1

EP3727626A1 - Device and method for the high-pressure treatment of bulk material by extraction and/or impregnation and use

Info

Publication number: EP3727626A1
Application number: EP18829404.5A
Authority: EP
Inventors: Volkmar Steinhagen; Ansgar HERBER
Original assignee: ThyssenKrupp AG; Uhde High Pressure Technologies GmbH
Current assignee: ThyssenKrupp AG; Uhde High Pressure Technologies GmbH
Priority date: 2017-12-22
Filing date: 2018-12-21
Publication date: 2020-10-28
Also published as: WO2020127957A3; DE102018222874A1; DE102018222882A1; CN111757772A; KR102369887B1; CN111757772B; WO2020127889A3; EP3897900A2; DE102018222883A1; DE102018222881A1; US11612831B2; US20200324223A1; WO2020127957A4; WO2020127889A2; WO2020127889A4; KR20210119971A; KR20210095715A; US20220062788A1; EP3897899A2; WO2019122387A1

Abstract

The invention relates to a device and a method for the high-pressure treatment of bulk material by extraction and/or impregnation, wherein the bulk material is arranged in the interior volume (Vi) of a pressure vessel device (10) and is treated at a high pressure level, in particular high pressure in the range of 40 to 1000 bar, while sealed off from the surroundings (U), wherein the high-pressure treatment is carried out in batches in a closed system in the pressure vessel device sealed off in a pressure-tight manner from the surroundings, in that the bulk material is fed to the interior volume (Vi) in batches with the pressure vessel device closed and is arranged on at least one treatment level and, after the high-pressure treatment has taken place, is discharged from the interior volume in batches with the high-pressure vessel closed. This also provides advantages in handling, in particular also with regard to material flow, and with regard to operational safety. The invention also relates to the use of a supporting tray module with at least one treatment level for high-pressure treatment in a closed system.

Description

Apparatus and method for high-pressure treatment of bulk material by extraction and / or impregnation and use

Description:

TECHNICAL AREA

The invention relates to an apparatus and a method for high-pressure treatment of bulk material by extraction and / or impregnation. Furthermore, the invention relates to the use of a support floor module with at least one treatment level for the high-pressure treatment in a closed system. In particular, the invention relates to an apparatus and a method respectively according to the preamble of the respective independent claim.

BACKGROUND

Bulk materials, in particular in the form of granules, must in many cases be freed of substances, in particular solvents. In particular, the bulk materials must generally be subjected to a pure extraction, independent of solvents. This can advantageously take place under high pressure, in particular at pressures above 100 bar, in particular in conjunction with the effect of heat at elevated temperature. An extraction, in particular extraction of solvent (s), is in many cases preferably using supercritical fluids (or extraction media), for example carbon dioxide (CO ₂ ), propane, butane, in particular since surface forces can be minimized and the extraction becomes particularly effective , also with regard to a drying effect. Both fluids and solids can be extracted.

Prominent examples of extraction methods are, for example, the decaffeination of tea leaves, coffee beans or hops extraction. Since the extraction is related to the production of various consumer products, the number of variants of extraction methods is comparatively high. This is also reflected in the structure and size of the systems. It is not uncommon, for example, to realize an extraction column with a height of more than 10 m, or several extractors (pressure vessels) together to form a plant boarded. In any case, a large variety can be observed in the existing system concepts, also with regard to size variations.

For impregnation methods, whether carried out separately or in combination with an extraction, comparable examples can be enumerated.

So far, the extractive solvent removal of bulk material or of granules in many cases by placing the bulk material in an extractor (pressure vessel), in particular on a plane in a layer with a predetermined maximum layer height, which layer with extraction medium (in particular C0 ₂ ) is applied and flows through becomes. For the arrangement of the bulk material usually serves a basket-like use, also known as a product receiving basket, for example, with a volume of about 250 liters and cylindrical mantle wall, with a gas-permeable, wire mesh-like, hole plate-like or sintered metal filter bottom, on which the use in Extractor is supported. A lid of the basket can also be gas-permeable, wire mesh-like, hole plate-like or made of sintered metal. The basket-like insert can be introduced in the region of a lid of the extractor, and after extraction, the largely freed of solvent bulk material can be removed by removing the basket-like insert for further use. The next batch can then be arranged by the same or another basket-type insert in the extractor. In other words, the high-pressure treatment process is carried out in batches, wherein the basket-like use is also intended to facilitate the handling of the respective batch, for example the removal.

In the previous way of extractive solvent removal, a relatively high personnel and time is required. The handling of the basket-like insert can not be automated in a simple manner. In the case of dangerous goods or harmful or flammable media or solvents, considerable work safety especially with regard to explosion protection, not least because usually people must be involved.

A disadvantage of previous devices and methods are therefore in particular the forming explosive gas mixtures and the health impairments for persons involved. Therefore, there is an interest in simplifying high-pressure treatment processes for bulk materials, in particular with minimized personnel expenditure, in particular for large quantities of bulk material, in particular for extraction and / or impregnation.

DESCRIPTION OF THE INVENTION

The object of the invention is to provide an apparatus and a method with the features described above, whereby the high-pressure treatment can be simplified or the apparatus or process-related expense associated with the high-pressure treatment can be reduced. In particular, the operational and / or work safety should be increased. Last but not least, there is also interest in a preferably (time) efficient process especially in the extraction, in particular solvent extraction, and / or in the impregnation in each case at high pressure.

This object is achieved by the devices and methods described below, wherein for the purpose of better understanding with the description of the device and the manner of arrangement of the bulk material is started.

This object is achieved by a pressure vessel device adapted for high-pressure treatment of bulk material by extraction and / or impregnation, with a lid and a high-pressure resistant wall, which surrounds a wall of the environment by means of a cover pressure-sealed or fusible inner volume, and with a to the Internal volume coupled inlet fitting and an outlet fitting respectively for the bulk material; wherein the pressure vessel device comprises a tray module having a plurality of actuatable ones Treatment levels has which support floor module or which treatment levels are arranged / arranged in such a way in the inner volume and partial load with bulk material are loaded with bulk material and closed at high pressure level high pressure treatment with closed pressure vessel device teilchargenweise dischargeable or aktuierbar that the high-pressure treatment in a closed, from The environment foreclosed system is executable. This also allows a process with reduced process engineering effort, especially with regard to manual activities, and facilitates not least the process automation.

The loading and extraction and / or impregnation (high-pressure treatment) in a closed system also has the advantage that explosion protection must meet less stringent requirements. Measures for operational safety can therefore remain relatively inexpensive. Also, a risk that a high-pressure seal is not done correctly, can be greatly minimized.

High pressure closures do not need to be opened.

Without inserted support module, the inner volume preferably corresponds to an empty cavity, in particular with a cylindrical geometry, optionally conical at the outlet.

For each treatment level, for example, 30 to 100 kg of bulk material or granules are picked up, in particular approx. 55kg.

The inner volume defined by the pressure containing device is, for example 100 liter to 10 m ³ or even up to 20m. ³ In the

Food handling, for example, volumes in the range of 3 to 5m ^{3 are} used, especially at a high pressure of about 300 to 600bar. The volume of the bulk material taken up in the internal volume is, for example, 50 L to 5 m ³ or even up to 10 m ³ , provided that the bulk material swells during extraction. Non-swelling bulk material can optionally also occupy a larger volume fraction of the internal volume, for example 0.7 to 0.8 times the internal volume.

The volumes mentioned here are to be understood as examples. The inventive arrangement or the inventive method can also be realized for smaller volumes, for example on a laboratory scale, for example with 5 to 25L, for example in extraction autoclaves.

As granules is to be understood any bulk material, be it artificial or made-up material or natural substances as well as food, such as polymer beads, or coffee beans, or hops. The granules need not necessarily be preformulated for the process, but may also be a natural product or foodstuff intended for high pressure treatment immediately after recovery (e.g., spice, herbs). The high-pressure treatment according to the invention can also be used e.g. be used for cleaning metal or plastic parts. The bulk material or granules can be present in a wide range of hardness, for example, it can also be comparatively soft. The bulk material can be swelling (volume increase) or shrinking or compacting (volume decrease), regardless of the degree of hardness. The granules have e.g. a grain size in the range of 3 to 6mm. The bulk material may be swelling at considerable volume change, for example by a factor of 2 to 10 (in particular based on the diameter or volume), for example from 5mm to 10mm particle diameter. Swelling bulk material can be metered in such a way that the respective treatment level still has a buffer volume even after swelling; For example, only about 50% of the loading capacity of the treatment level is loaded before the high-pressure treatment. An arrangement of the bulk material on several levels also allows a swelling behavior, which is not or hardly noticeable influenced by gravity influences.

It has been found that the method according to the invention is advantageous not only for extraction treatments, but also for Impregnation treatments. In this case, according to the invention, a combination of both treatment methods can also be carried out, in particular in the closed system optionally at least at approximately the same high pressure level.

The respective treatment level does not have to be strictly horizontal or exactly plan. The respective treatment level serves the arrangement of the bulk material, in particular with predefined layer thickness. If the supply and / or discharge should take place in the lateral direction, it may be advantageous to tilt the treatment level and / or to design it with a curvature.

As a closed pressure vessel device or as a closed system is to be understood an arrangement in which at least one lid of the pressure vessel device remains mounted. A removal of inlet baskets or the like receptacles out of the pressure vessel device is not required; the pressure vessel device can remain closed.

According to one embodiment, the pressure vessel device has an automatically actuatable inlet fitting for the batchwise feeding of the bulk material, in particular coupled to the lid. According to one embodiment, the pressure vessel device has an automatically actuatable outlet fitting for the batch discharge of the bulk material, in particular coupled to a bottom of the pressure vessel device. In this way, in each case the automation can be facilitated and optionally also an interface or system boundary to the high-pressure area can be formed. Automated actuation can be carried out in particular by means of a control device set up for this purpose.

According to one embodiment, the at least one treatment level is adapted to receive the bulk material in a particular horizontally oriented plane and further adapted for the passage of bulk material. This also provides flexibility in the manner of loading / unloading the Pressure vessel device, in particular in a controlled in several sub-batches process.

According to the invention, the support floor module has a plurality of actuatable treatment levels, which can be loaded / unloaded with bulk material in each case when the pressure container device is closed. As a result, a variation in the arrangement of bulk material can take place even in the closed system, in particular with regard to a maximum layer thickness.

According to one exemplary embodiment, at least one partial region of the respective treatment plane can be displaced from a corresponding high-pressure treatment position into at least one loading / unloading position, in particular by means of pivoting kinematics. This also has advantages in terms of material flow. In particular, the material flow can be organized by gravity.

The displacement of the respective treatment level can be done by means of a kinematics, which is preferably designed as a pivoting kinematics. When pivoting is to be understood as a rotation about an at least approximately horizontally aligned axis. Optionally, the kinematics may also include a rotation mechanism about an alternative orientation axis and / or at least one translational mechanism. The kinematics may include a folding mechanism with hinges and push rods. The (pivoting) kinematics can also include a translational displacement. The kinematics can be formed or supplemented by traction means, for example in the form of chains or cables, and optionally also by spring elements. The (pivoting) kinematics can also comprise rotary drives arranged in a respective pivot axis or axis of rotation. Rotary actuators can provide the advantage that no high-pressure-tight bushings in the wall are required. The rotary actuators can be arranged inside in the inner volume. According to one embodiment, the respective treatment level is defined by at least one gas-permeable plate. This embodiment is also characterized by simplicity and robustness.

According to one embodiment, the respective treatment level is defined by at least one pivotally actuable gas-permeable plate mounted in the inner volume, in particular by two plates pivotally mounted relative to each other about a pivot axis (x, y), in particular at least downwardly pivotable, preferably both downwardly and downwardly swiveling above. In this way, a robust kinematics can be provided, by means of which both the loading and the emptying can be carried out in a simple manner. In particular, the plates can be pivoted upwards for loading, in each case for releasing a treatment level arranged below them. The plates can be pivoted for unloading in particular downwards, in particular successively each to release only one treatment level. The downward pivoting can also provide an advantage in terms of protection of individual components of the kinematics, in particular of components that are arranged below the respective treatment level.

According to one exemplary embodiment, the respective treatment level is defined by two gas-permeable plates mounted pivotably about a pivot axis relative to each other on a transverse web, in particular with the crosspiece held on at least two holding units extending in the vertical direction, in particular by a first upward swivel angle of at least 60 ° or 75 °, preferably at least 85 ° or about 90 °, and by a second pivoting angle downwards of at least 45 ° or 60 °. This provides great variation in loading / unloading. In particular, the comparatively large tilt angle upwards can provide advantages when loading treatment levels arranged further down, and a comparatively small tilt angle downwards can also allow a directional material flow, for example radially outward, away from centrally arranged kinematics. Components. A swivel angle of about 90 ° upwards also promotes a homogeneous filling of the planes. Swinging beyond 90 ° is also possible.

According to one exemplary embodiment, the support floor module has a kinematics with a construction which is symmetrical in relation to at least one pivot axis in a respective treatment plane. This also results in advantages in terms of material flow. In particular, the respective treatment level can be loaded homogeneously even with a comparatively large container diameter. For example, a respective plane of symmetry is coupled to a respective inlet conduit.

According to one embodiment, the respective treatment level can be actuated between at least two positions, namely a first position for the passage of bulk material and in a second position for receiving (or arrangement) and treatment of bulk material, in particular by means of a drive unit integrated in the lid or fastened to the lid and at least one actuatable actuator. This results in a comparatively simple way of controlling / regulating operating states. Optionally, intermediate positions can also be provided.

The actuation can take place from the outside, that is from outside the internal volume. This provides degrees of freedom in the selection and configuration of the respective drive unit, in particular independently of the pressure level prevailing in the inner volume. Optionally, one or more drive units can also be arranged in the inner volume.

The respective actuator may be formed as a pull / push rod, or as a pure traction means (rope, chain), optionally coupled to a spring element (in particular with respect to a return movement). An actuation and / or bulk material supply via the cover can provide several advantages: no height positions or height levels must be defined in predetermined height positions; the high-pressure vessel can be made structurally simpler and / or pressure-resistant; Economies of scale; optional central drive unit for several actuators.

According to one embodiment, the pressure vessel device has at least one drive unit and a plurality of actuators in the form of push / pull rods arranged for bidirectional translational actuation of the respective treatment level, in particular with the actuators in a linear arrangement next to each other in a transverse plane (xz, yz). This makes it possible to realize a compact kinematics, without requiring much space in the interior volume, and without noticeable side effects in terms of material flow. Push / pull rods can provide robustness and operational reliability even with positioning movements in several directions.

According to one embodiment, the respective treatment level or a plate of the treatment level is coupled via at least one adjusting lever and two rotary joints to an actuatable, high-pressure tight guided by the lid into the inner volume actuator, in particular externally actuated. As a result, a robust, simply constructed (swivel) kinematics can be provided. In this case, the coupling may preferably be provided below the treatment level.

According to one embodiment, the pressure vessel device comprises a pneumatic, hydraulic, electrical, electromagnetic and / or magnetic drive unit, which is coupled to the at least one treatment level. As a result, the automation is simplified, the type of drive can be selected in particular depending on the bulk material to be treated.

According to one embodiment, the pressure vessel device comprises a drive unit which is coupled to the at least one treatment level and which can be arranged on the outside of the cover or arranged inside the internal volume. This allows Stellbewegungen be automated individually per treatment level. In an arrangement outside, the drive unit can be coupled via at least one actuator to the respective treatment level. A high-pressure seal provided in the cover, in particular in the form of a stuffing box with a packing, can thereby form a high-pressure-tight passage for the actuator. Rod and shaft seal technology can be used here.

Preferably, a respective adjusting lever is arranged below the respective treatment level. In particular, the respective adjusting lever is coupled with a first rotary joint to the adjusting member and coupled with a second rotary joint to an underside of a plate of the treatment level. In this way, a pivoting movement between at least two pivoting positions of the plate can be induced by a translational adjusting movement of the actuator, in particular both upwards and downwards (absolute pivot angle about a pivot axis, for example in the range of 135 ° to 175 ° or even up to 180 ° °). Thanks to the arrangement below the respective treatment level and jamming or wedging of bulk material can be effectively avoided on the levers. The container can be loaded from above and unloaded downwards, wherein the respective plate / treatment level covers the actuators respectively and protects against contact with bulk material.

Preferably, in a respective treatment level two semicircular plate elements are each coupled together to an actuator, in particular each with a double-sided pivotally mounted lever.

According to one embodiment, the pressure vessel device in each case has at least one inlet and / or outflow fitting, in particular a nozzle for high-pressure or extraction medium, in particular in radial or lateral alignment. In this way, a simple structural design can be achieved, in particular with respect to an axially flowed through (fixed bed) bed. Input and output Outflow fittings can be provided as a radial connection at the top and bottom of the container, for axial flow of the internal volume, upwards and / or downwards.

The respective nozzle can be passed through the container wall, optionally through the lid. The sockets can also be arranged opposite each other in a comparable height position, in each case with respect to a treatment level.

According to one exemplary embodiment, the pressure vessel device has a heating device which heats the internal volume, in particular in the form of a fully enveloping heating jacket, which extends in the vertical direction over the treatment plane (s). This allows a temperature control of the internal volume.

Solvents can also be exported via the outlet fitting from the pressure vessel. Optionally, a further outlet or nozzle is provided specifically for solvents, in particular at a deposition or convection point of the pressure vessel. Several inlet / outlet fittings for fluids may be advantageous in terms of even more homogeneous flow through the bed.

For the insertion and removal of the bulk material, it may be advantageous to provide further nozzles, in particular per level. This allows e.g. Also material flow, if it should come in the direction of gravity to a jam or a blockade. According to the invention, however, it is already sufficient to provide only a single inlet fitting and a single outlet fitting for the bulk material, which also provides advantages in terms of design effort. The inlet and outlet fittings may preferably be arranged one above the other in the direction of gravity, with at least the outlet fitting in a preferably centric arrangement.

According to one exemplary embodiment, the support floor module is integrated in the cover or at least held, arranged and / or supported in the interior volume by means of the cover. As a result, a simple structural design can be realized. In other words, the high-pressure-resistant cover is designed to absorb tensile forces exerted by the charge and the module. An assembly of the module hanging in the inner volume Vi not least facilitates the assembly, or simplifies scaling, and may also favor the flow of material, in particular since no bottom-supporting abutments hinder the flow of material. In this context, the arrangement of drives externally outside of the internal volume is advantageous, especially on the lid.

According to one embodiment, the lid of the pressure vessel device forms a lid of the tray module. According to one embodiment, the inlet fitting for bulk material is integrated in the cover, in particular in an arrangement with a vertical conveying direction. As a result, the expenditure on equipment can be further minimized in each case.

According to one embodiment, the inner volume is cylindrical or at least rotationally symmetrical. This form may already be particularly preferred due to the application for high pressure. However, this also results in advantages in terms of material flow and flow profile. The wall can be correspondingly cylindrical, except for a preferably conical bottom section. Preferably, the wall along the treatment planes is cylindrical with at least approximately the same diameter, and also terminates upwardly toward the lid with the same constant diameter. This also has advantages in terms of material flow.

According to one embodiment, at least three treatment levels are provided, preferably at least four or five treatment levels. As a result, the high-pressure treatment can be carried out more effectively and / or more efficiently. In particular, fluidic disadvantages of fixed beds with a comparatively long flow path can be avoided. According to one embodiment, the pressure vessel device is configured to carry out a previously described method. This results in the aforementioned advantages.

According to one exemplary embodiment, the respective treatment level can be displaced by at least one actuator that can be actuated in a rotational manner, for example by a shaft with plates rotatably coupled thereto. This also extends the variability and allows combinations in the design of the type of kinematics for the material flow. In particular, partial aspects with regard to material flow can be optimized.

According to one embodiment, the respective treatment level is displaceable by at least one translatorically actuable actuator, be it pivotable or displaceable in the translational direction. This also makes it possible, for example, to vary the position of treatment levels.

According to one embodiment, the support floor module comprises both at least one actuator which can be actuated in a translatory manner and at least one actuator that can be actuated in a rotational manner. This allows a functional integration into a combined support floor module with at least two different kinematics.

The aforementioned object is also achieved according to the invention by a high-pressure treatment system, in particular a solvent extraction system having a pressure vessel device with a previously described support base module, in particular further comprising a control device and at least one sensor unit. This results in the aforementioned advantages.

The aforementioned object is also achieved by a method for high-pressure treatment of bulk material by extraction and / or impregnation, which is arranged in the internal volume of a pressure vessel device and at a high pressure level, in particular high pressure in the range of 40 to 1000 bar, under high pressure solvent extraction is carried out under pressure from the environment in bulk, in a closed system in the pressure-tight from the environment sealed pressure vessel device by the bulk material is supplied to the internal volume with the pressure vessel device closed and placed on at least one treatment level and after the high-pressure level (or high pressure) of high-pressure treatment with the pressure vessel device closed is discharged in batches from the internal volume. This results in the aforementioned advantages. In particular, the expense can be saved, which is required when opening a pressure vessel and removing an insert basket. According to the invention, the supply and removal of bulk material can take place in a closed system, optionally to / from a plurality of treatment levels, optionally also at elevated pressure.

According to one embodiment, the batchwise feeding of the bulk material takes place by means of an automatically actuatable inlet fitting, in particular in partial batches, in particular via a lid of the pressure vessel device. As a result, an automation of the overall process can be facilitated.

According to one embodiment, the batchwise discharging of the bulk material takes place by means of an automatically actuatable outlet fitting, in particular in partial batches, in particular via a bottom valve with inwardly opening closing element. This can also facilitate a controlled removal of the bulk material. The bottom valve can couple the internal cavity or the internal volume, in particular a conical region, with the environment. The bottom valve can be mounted or flanged directly on a wall of the conical region, wherein between the conical region and the valve preferably a sliding, continuous transition (continuous inner surface) is formed. This facilitates the discharge of bulk material.

According to the invention, the high-pressure treatment is carried out on a plurality of treatment levels arranged in the inner volume, in particular on at least three treatment levels. This allows, for example, the arrangement in preferred layer thicknesses. Also aerodynamic disadvantages of long fixed beds can be avoided.

According to one embodiment, the batchwise feeding of the bulk material comprises feeding partial charges respectively to one of a plurality of treatment levels, in particular successively first to a lowermost treatment level and then to a treatment level further above, in particular gravitationally driven in the direction of gravity. In this way, an arrangement of partial batches in the internal volume can be carried out with the system closed, wherein the partial batches can be characterized, for example, in terms of the layer thickness or the local distribution of the granules.

According to one embodiment, the batchwise discharging of the bulk material comprises discharging partial charges each from one of a plurality of treatment levels, in particular successively first from a lowermost treatment level and then respectively from a treatment level arranged above above, in particular gravitationally driven in the direction of gravity. This facilitates the flow of material and can not least prevent the damming of bulk material. For example, the volume of a partial charge is at most as large as the volume of a conical section of the pressure vessel device.

According to one embodiment, during the batchwise delivery and / or the batchwise discharge, at least one of the treatment levels arranged in the inner volume is actuated or displaced, in particular pivoted, in particular by automated actuation, in particular by at least one drive unit arranged outside the inner volume for passing the bulk material arranged thereon. As a result, the supply and removal of partial batches can also take place in a comparatively precisely controllable manner, in particular also gravity-driven, optionally exclusively gravity-driven from above below in partial batches. The arrangement outside of the internal volume is not mandatory, but can provide advantages in terms of material flow.

According to one embodiment, the batchwise feeding and the batchwise discharging take place unidirectionally in a single direction through the internal volume, in particular in the axial direction of gravity downward. This simplifies the flow of material, especially in high-pressure vessels. Not least, the structural design of the entire device can remain relatively simple. Optionally, the unidirectional flow of material can also take place at least partially in the radial direction, in particular in connection with a corresponding configuration of the treatment levels and optionally additional fittings.

According to one embodiment, the feeding and / or discharging takes place pneumatically or by pneumatic assistance. This also enables a robust and suitable for various bulk materials type of automation and control.

According to one embodiment, the feeding and / or discharging is carried out at a pressure level between ambient pressure and high pressure level, in particular at least 2 or 3 bar, in particular at more than 6 or more than 10 bar. This can also save process time and printing work.

According to one embodiment, the high pressure treatment is carried out sequentially for a plurality of closed system batches in the sealed-off pressure vessel device, in particular for a period of one to two hours per batch. This also makes it possible to further increase the degree of automation.

According to one embodiment, the amount of bulk material is detected during feeding and / or discharging, in particular in a gravimetric manner, in particular with respect to individual bulk bulk batches. As a result, for example, the height of a layer be recorded or regulated at a respective treatment level.

According to one embodiment, in batch-wise feeding and / or discharging, an activation of inlet and / or outlet fittings takes place, in particular as a function of gravimetric measured values of bulk material partial batches recorded in real time. As a result, on the one hand, a control or monitoring of the process can take place, on the other hand optionally also a dosing.

Dosing may be of particular interest in terms of maximum loading of a particular treatment level. Between individual

Treatment levels can be formed partial internal volumes in which, for example, the operating state of a fluidized bed can be adjusted, for example, when flowing from bottom to top. The respective partial interior volume corresponds to an individual treatment compartment. In other words, it can be a fluidization of the bulk material between adjacent treatment levels or plates. In particular, it is possible to react to any fluidic inhomogeneities by individually adjusting the loading of a respective treatment level, in particular with regard to the same effectiveness of the treatment from all levels.

According to one embodiment, the high-pressure treatment is carried out under thermal energy action at an elevated temperature level, in particular in the range from 30 to 100 ° C. This results in further process variables during high-pressure treatment. The heat energy effect can be effected by means of at least one heating device coupled to the pressure vessel device. In addition, e.g. also the flow (volume flow) of high-pressure medium can be adjusted.

According to one embodiment, the bulk material during high-pressure treatment is supplied with heat energy by means of high-pressure medium and / or by means of at least one heating device in such a way that an increased temperature level is maintained is, in particular in the range of 30 to 100 ° C, for example 40 to 70 ° C for natural substances or 60 to 70 ° for plastics. By setting and regulating an exact temperature level, the bulk material can be treated in a tolerance range which is desired in each case.

As a high-pressure medium, for example, C0 _{2 is} used. C0 ₂ has the advantage of a comparatively low critical temperature, so that in particular natural substances can be high pressure treated by means of C0 ₂ at comparatively moderate temperatures.

According to one embodiment, the high-pressure treatment comprises at least one extraction, in particular solvent extraction. The solvent can be discharged in particular by means of the high-pressure medium. The direction of flow of high-pressure medium can be set largely freely depending on the selected process (axial, radial).

According to one embodiment, the high-pressure treatment comprises at least one impregnation, in particular the impregnation of polymers, for example as described in the publications EP 0 222 207 A2 and EP 0 683 804 B1. This results in advantages that have already been described above with regard to extraction. The impregnation medium can be entered in particular by means of the high-pressure medium. With regard to the type of impregnation media that can be used, reference may also be made by way of example to these publications.

According to one embodiment, the high-pressure treatment comprises both an extraction and an impregnation, in particular the extraction of monomers and the impregnation with additives, in particular of polymers. This provides a wide range of applications and, last but not least, enables an efficient process combination. The extraction can be carried out before impregnation. According to one embodiment, the high-pressure treatment comprises at least one solvent extraction and is carried out above the critical temperature and above the critical pressure of the solvent. As a result, surface forces can be minimized, and extraction or drying can be carried out in a particularly effective manner.

According to one embodiment, bulk material is high pressure treated as an aerogels by extraction and / or by impregnation. It has been found that the arrangement according to the invention or the procedure according to the invention is particularly advantageous also for bulk goods in the form of aerogels (or airgel bodies). Especially with aerogels, extraction of solvents may be desired / required. Particularly in the case of aerogels (highly porous solids), a change in volume, in particular an increase in volume, can be particularly pronounced in the case of high-pressure treatment, for example in the range of a factor of 10, or in other words, for example in the region of 2-3 times the radius increase.

According to one embodiment, the high-pressure treatment comprises fluidizing the bulk material, in particular in a fluidized bed (actively generating or regulating the transition from a fixed bed to a fluidized bed), in particular in an outlet-side region of the pressure vessel device. In particular, the fluidized bed is produced exclusively by means of an extraction medium. Advantageously, the bulk material is introduced into a fluidized bed in which only one high-pressure treatment level for the fluidized bed (in particular as a displaceable or pivotable flap plane) is provided, in particular at a lower end of the pressure vessel device. The fluidized bed can be sealed off on both sides by one of several high-pressure treatment levels. The appropriate treatment level can be sealed off or closed before removal of the bulk material (bulk material is collected). The fluidized bed can also be formed on several treatment levels, in particular on several levels above each other. The fluidized bed makes it possible to realize advantageous mass transfer properties in combination with unrestricted expansion possibility of the treated bulk materials. For example, polystyrene (PS) granules can also be a targeted surface treatment.

The aforementioned object is also achieved by a control device configured to carry out a method described above, wherein the control device is coupled to at least one sensor unit configured to detect a flow of bulk material or a mass or a mass difference or a volume or a volume difference, optionally also equipped with at least one sensor unit for detecting a path and / or a force, in particular coupled to a respective actuator of the pressure vessel device. This results in the aforementioned advantages.

The above object is also achieved by using a support base module with a plurality of treatment levels for high-pressure treatment of bulk material by extraction and / or impregnation in a closed, pressure sealed off from the environment system, wherein the support base module is disposed in the inner volume of a pressure vessel device, in particular by a cover of the support floor module forms the cover of the pressure vessel device, wherein the (respective) treatment levels for high pressure treatment and / or passage of the bulk material arranged thereon displaceably stored and positioned in the inner volume, in particular use of the support floor module in a previously described method, in particular using the support floor module in a previously described pressure vessel device, in particular under high pressure at pressures above 40 to 1000bar. This results in the aforementioned advantages.

DESCRIPTION OF THE FIGURES Other features and advantages of the invention will become apparent from the description of at least one embodiment with reference to drawings, as well as from the

Drawings themselves. It shows

Fig. 1, 4 each in a sectional side view in a schematic

Representation of a closed pressure vessel device or a high-pressure treatment system according to an embodiment;

Fig. 2, 3 each in a sectional side view in a schematic

Representation of an open pressure vessel device (without support floor module) or the support base module according to a

Embodiment;

Fig. 5 in a plan view of an underside a treatment level of a

Tragbodenmoduls a pressure vessel device according to a

Embodiment;

Fig. 6 in a sectional side view in a schematic representation of a

Pressure vessel device according to an embodiment;

7 to 15 each show a schematic representation in different views of further embodiments;

16 shows a schematic representation of method steps of a method for

High-pressure treatment according to an embodiment;

17A, 17B, 17C and FIG. 18:

in a sectional side view and in perspective detail views in a schematic representation in each case a further embodiment of a pressure vessel device;

19 is a sectional side view in a schematic representation of a concept for the use of translational actuators in a pressure vessel device according to embodiments; and

20A, 20B and FIGS. 21A, 21B and FIGS. 22A, 22B:

in a sectional side view and in exploded view in each case in a schematic representation of another embodiment of a pressure vessel device with a combined support floor module for both translational and rotational positioning movements. For reference numbers that are not explicitly described with respect to a single figure, reference is made to the other figures.

DETAILED DESCRIPTION OF THE FIGURES

Fig. 1 shows a pressure vessel device 10 with integrated, built-in support base module 20 (shown in the assembled state) for receiving and arranging bulk material 1 or granules, wherein in an area bounded by a high-pressure wall 12 of the pressure vessel device internal volume Vi (or in the corresponding cavity ) is formed a bed or batch 2 in the form of several partial batches 2.1, 2.2, 2.n, which are each arranged on an individual treatment level 27. By way of example, five treatment levels are shown. The respective treatment level 27 defines a height position z27 for the arrangement of bulk material 1.

A high-pressure-resistant sealingly mountable cover 11 of the pressure vessel device 10 is provided by a cover 21 of the support base module 20, or vice versa. By mounting the support floor module, the container 10 can be closed high-pressure-tight ("integral construction"). A high pressure resistant attachment can be done by means of fastening means 11.5, in particular circumferentially provided screw, and a centering 11.7. A cylindrical portion 12.1 of the wall 12 has corresponding fastening means.

The lid 11, 21 is identified here by two reference numerals to emphasize that the lid 21 can be provided as a supporting, supporting component of the support base module and at the same time can form the lid 11 of the pressure vessel device 10. This type of construction is to be described here with the term "integral construction". On the lid 11, 21 fastening means 11.1 are provided for at least one inlet fitting 13, in particular fixable by means of screw. Further, in the lid 11, 21 a plurality of passages 11.2 formed for bulk material 1, in particular two passages in a symmetrical arrangement with respect to a central longitudinal axis M of the pressure vessel device 10 and the support base module 20th

On the lid 1 1, 21 is optionally further provided at least one passage 1 1.3 for at least one actuator (25), wherein in the implementation of 1 1.3 a high pressure resistant seal is provided 11.4. Via the feedthrough 11.3, a drive unit (22) can be coupled to the respective actuator. Alternatively, the drive unit may be arranged in the internal volume Vi.

Bulk material 1 is introduced via one or more inlet lines 13.2 by means of inlet members 13.1, in particular valves and / or locks, in the inner volume Vi and arranged for a high-pressure treatment as partial charges 2.1, 2.2, 2.n in a respective treatment level 27 in different height positions. For this purpose, the support base module 20 has a kinematics described in more detail in connection with FIGS. 3, 5.

The high-pressure treatment comprises, in particular, extraction and / or impregnation. The high-pressure treatment can be carried out under the action of heat. A laid around the wall 12 heater 14 in the manner of a heating jacket can feed the corresponding desired heat energy, for example, in addition to thermal energy, which is entered via high-pressure medium M2.

Similar to the material flow in partial batches into the internal volume, a discharge into partial batches can take place. Below a conical portion 12.2 of the wall 12, an outlet fitting 15, in particular container bottom unit is provided, with at least one outlet member 15.1, in particular bottom valve and / or lock. The outlet fitting 15 may be integrated into the conical section 12.2 and / or be attached to it in a high-pressure-tight manner, in particular by means of screw connections. The Discharge member 15.1 has an inwardly opening closing element 15.2, in particular in the manner of a cone, which can be actuated by means of an actuator 15.3 (FIG. 4). The granules 1 can be discharged via an outlet 15.4 from the internal volume.

For the supply and discharge of high-pressure medium M2 inlet / Ausströmarmaturen 16, 17 are provided, in particular in the manner of neck.

The pressure vessel device 10 and the support base module 20 together form a high-pressure treatment system 30 in the mounted state. The respective treatment plane 27 can be formed, in particular, by one or more perforated plates and / or braids.

The indicated coordinate system identifies a width direction x, a transverse or depth direction y, and the vertical or gravitational direction or height direction z.

In the arrangement shown in Fig. 1, the flow of material (flowing bulk material) can be unidirectional in the direction of gravity, so consistently gravity-driven from top to bottom, without diversion or deviation.

Fig. 2 shows the pressure vessel device 10 in an open state, without support base module 20, without charge. The internal volume Vi is not isolated from the environment U. In this state, the support base module 20 can be arranged in the inner volume Vi, in particular by mounting the lid 11, 21 on the wall 12. Especially for very bulky containers, this type of assembly can provide great benefits.

In Figs. 3, 5, the support floor module 20 is shown in detail. Outside the cover 21, a drive unit 22 is provided, in particular with a pneumatic cylinder, which is coupled to a kinematics 23. The kinematics 23 comprises in particular five Actuators 25, in particular each designed as a push / pull rod, and a plurality of levers 25.1, which are mounted on both sides in swivel joints 25.2, 25.3. Thus, the kinematics is set up to actuate each treatment level individually. Optionally, the kinematics can be set up to actuate all treatment levels simultaneously or coupled to one another.

In Fig. 3, 5, a first and second part 27a, 27b of the respective treatment level 27 are visible, designed as gas-permeable plates in pivotable storage. A cross bar 24 supplies each treatment level 27 each have a pivot axis for the kinematics 23. The plates 27a, 27b may be formed in particular as a semicircular perforated plates. The entire structure may be formed symmetrically with respect to the transverse webs 24. The actuators 25 are preferably arranged exactly in the plane of symmetry (yz).

In FIGS. 1, 6, a first swivel angle a upwards against the direction of gravity and a second swivel angle ß down in the direction of gravity are shown. For the feeding of bulk material into the empty inner volume, all treatment levels, apart from the lowest treatment level, are pivoted in an upward vertical orientation (angle a to 90 °). The first partial batch can fall to the lowest treatment level, in particular until a desired loading (mass) is reached. Thereafter, the second treatment level from the bottom is pivoted to the horizontal orientation, and the process of supplying a partial batch is repeated. In this way, you can easily load three, five or even more treatment levels. Once the top treatment level has been loaded, the high-pressure treatment can take place. The unloading / discharging of bulk material then takes place preferably also in partial batches, although all treatment levels could be shifted more or less simultaneously downwards. First, the lowest treatment level is shifted down, and the partial batch then slides into the conical area 12.2. The closing element 15.2 can be opened inwards (or is already open), and the partial batch can be discharged. Then the next higher treatment level is moved down. Depending on the nature of the process, the closing element 15.2 can either remain in the open position, or be closed in the meantime. In the meantime closed, sealing closure element 15.2, the material discharge can be controlled.

For the purpose of mechanical stability and support, at least one geometrically coupling intermediate element 26 (only in FIG. 5), in particular a centering ring, as well as a plurality of holding units 29, in particular holding bar (s), may be provided. The intermediate element 26 can promote the material flow, for example with regard to an arrangement of granules in the wall region. Optionally, a support unit 28, in particular in the form of a (centering) ring for the purpose of radial support, may be provided in the lower region of the module 20. An axial support is not necessarily required, in particular since the entire module 20 can be arranged hanging in the internal volume Vi, supported on the lid 11 and at the upper end of the wall 12th

4 further shows a control device 31, a logic unit 33 and a plurality of sensor units 35 arranged at different measuring points in the system 30, in particular for temperature, pressure, force, displacement, mass and / or flow. The feeding, high-pressure treatment and discharge can take place by means of the control device 31 in an at least partially automated manner, preferably fully automated.

The position of individual sensor units can be freely selected. In particular, a plurality of pressure sensors may be provided, which are arranged such that a pressure loss over the partial batches can be detected. A self-adjusting differential pressure can be a process variable during impregnation and / or extraction, via which the process can be easily controlled, regulated and / or monitored. Of course, the pressure loss also depends on the type of granules, and must be monitored individually. The resulting differential pressure can also be related be detected on inlet and outlet fittings. Optionally, a safety system in the manner of a bypass may be provided to avoid excessive differential pressures.

Preferably, a plurality of mass sensors are provided, in particular in each treatment level at least one mass sensor. This facilitates the collection of partial batches and the regulation of the supply and discharge of bulk material.

In FIG. 4, three media streams are further indicated: the first media stream M1 characterizes the bulk material flow, the second media stream M2 characterizes high-pressure medium or extraction medium, optionally comprising impregnation medium, and the third medium stream M3 denotes solvent which is separate or together with the high-pressure medium M2 can be discharged.

6 shows a further exemplary embodiment of a pressure vessel device 100 and of a supporting floor module 200, wherein the features described above can also be partially or completely implemented in this exemplary embodiment. The drive unit 22 can optionally be arranged on the outside of the wall 12 or on the cover 11, and / or be arranged in the internal volume Vi, in particular in the design of at least one rotary drive on a pivot axis of the support floor module. For impregnation, a buffer tank 37 may be provided in combination with a metering 39.

In the following figures, individual aspects of advantageous variants or exemplary embodiments are explained. The respective variants or exemplary embodiments can be combined with one another, unless this is explicitly negated.

Figures 7A, 7B, 7C, 7D show three embodiments in which the tray module 300 defines a plurality of treatment planes, each formed by an integral plate. The kinematics for moving the plates is in particular by a respective push rod (FIG. 7B shows an eccentric arrangement of the push rod (lever linkage), with only one centrically arranged inlet fitting) and / or by a rotary drive (FIG. 7C). The drive variants can be provided by the combinations already described above. These embodiments provide advantages in particular with regard to robustness and simple construction. The plates swing down on one side. The feeding of the respective (partial) batch can be done centrally via the lid. The discharge can be done centrally via a bottom outlet fitting. The central bottom-side discharge delivers, for example, process-technical advantages, in particular in the case of gravity-driven discharge, in particular with regard to complete discharge without residues.

8A, 8B, 8C, 8D show three embodiments in which the support base module 400 is characterized by an eccentric arrangement of the actuators. For each treatment level a plate is provided which is mounted eccentrically and is pivotable up and down. Edge areas of a respective treatment level can be used for support structures.

9A, 9B, 9C show two exemplary embodiments, in which the support floor module 500, in particular in an embodiment according to FIGS. 7, 8, in a pressure vessel device 10; 100; 110 is arranged, with individual

Treatment levels of the support floor module can be actuated laterally. In the wall of the pressure vessel device passages are provided for lateral adjusting means 25a, each specific to each treatment level. The actuatable lateral adjusting means 25a allow a kinematics at least comprising a pivoting mechanism, in particular in the form of push rods. The adjusting means 25a can be coupled directly to the respective plate or indirectly by means of a kinematic coupling to the respective treatment level. FIGS. 9A, 9B show the principle of lateral actuation in the case of centric or eccentric mounting of plates, one or more plates being provided on each side of the treatment to be tilted downwards or upwards and downwards on both sides. Additionally or alternatively For the cover-side inlet for bulk material, an inlet fitting and / or outlet fitting can also be provided laterally at the level of the respective treatment level.

10A, 10B show two embodiments in which the support base module 600 has a centrally arranged lever linkage, by means of which the individual plates are pivotable by translation. Depending treatment level, two plates may be provided, in particular in a symmetrical arrangement. The pivoting takes place without an adjusting lever (FIG. 10A) or by means of a kinematics comprising in each case one adjusting lever per plate half (FIG. 10B).

11A, 11B show an embodiment in which the pressure vessel device 110 has solid trays per treatment plane, optionally in horizontal orientation (FIG. 11A) or in oblique orientation (FIG. 11B). It is only provided laterally arranged at the height of the respective treatment level inlet and outlet fittings. Optionally, a bulk material extraction is provided. In this pressure vessel device 110, the process according to the invention can be carried out in a closed system, in each case for a partial charge. The treatment levels can be individually loaded independently of each other. This embodiment provides e.g. also advantages in the simultaneous high pressure treatment of different bulk materials on different levels.

FIG. 12 shows an exemplary embodiment in which the support floor module 700 has pivoting kinematics and is arranged in a pressure vessel device 110 with lateral inlet fittings. The discharge of bulk material can be done centrally on the bottom outlet fitting. In this embodiment, the kinematics can be optimized for pivoting and discharging down.

FIGS. 13A, 13B show an exemplary embodiment in which the support floor module 800 has a kinematics with a rotating mechanism with an axis of rotation oriented at least approximately vertically. For each treatment level there are two superimposed Plates twisted against each other. FIG. 13B shows the respective treatment level in an open state, four passages being shown by way of example.

14A, 14B, 14C show an embodiment in which the support floor module 900 has a kinematics with translatory mechanism with at least approximately horizontally aligned displacement axis. Depending treatment level two superimposed plates are translationally displaced relative to each other. Fig. 14C shows the respective treatment level in an opened state. The translation kinematics can be realized for example by means of lateral adjusting means, or based on a further of the mechanisms described here. Optionally, an additional rotary drive can be provided, which is coupled to a central rotary shaft and in each case actuates at least one of the plates per treatment level.

FIGS. 15A, 15B, 15C, 15D, 15E, 15F show three exemplary embodiments, in which the support base module 990 each has an inwardly outwardly opening kinematics with flap construction, wherein drainage slopes are optionally also provided in the respective treatment plane and / or edge regions for support structures are provided. For each treatment level, at least two plates arranged symmetrically with respect to the center longitudinal axis and the transverse web are provided, each being pivotable downwards and upwards. The respective plate is mounted eccentrically about a pivot axis, and opening takes place from the center (pivoting down or up). The kinematics may in particular also include coupling joints and / or traction means and / or at least one spring mechanism with return movement.

16 shows individual method steps of a method for high-pressure treatment. A first step S1 comprises feeding bulk material, wherein an actuation S1.1 of at least one treatment level takes place. Preferably, the treatment levels are actuated starting from a lowest treatment level. The respective treatment level is brought into a receiving / treatment position, in particular pivoted in the horizontal plane. This is followed by feeding S1.2 of a (partial) batch. Thereafter, the overlying treatment level can be actuated.

In a second step S2, a pressure build-up takes place up to the desired high-pressure level, optionally starting from ambient pressure or from an elevated intermediate pressure level on the other hand.

In a third step S3, an extraction takes place, and / or in a fourth step S4, an impregnation takes place, which sequence is variable. In this case, in each case a pressure and temperature control can take place, illustrated in Fig. 4 by way of example by the sensor unit 35. One or more such sensor units may also be provided in the further steps for a control, in particular based on temperature, pressure, force, Displacement, mass and / or flow measurements.

In a fifth step S5, a pressure reduction takes place, optionally to ambient pressure or to a contrast elevated intermediate pressure level.

In a sixth step S6, a discharge of bulk material takes place, whereby an actuation S6.1 of at least one treatment level takes place. Preferably, the treatment levels are actuated starting from a lowest treatment level. The respective treatment plane is brought into a passage position, in particular pivoted at least approximately in the vertical plane, or at an angle of e.g. 10-20 ° to it. This is followed by a discharge S6.2 of a (partial) batch. Thereafter, the overlying treatment level can be actuated. The discharge of a particular partial batch can allow good control of the material flow.

In a seventh step S7, thereupon, in preparation for a subsequent high-pressure treatment, a high-pressure-tight sealing of the inner volume takes place at the Outlet fitting of the pressure vessel, in particular by means of an inwardly opening valve.

The present invention is also characterized in particular by the possibility of automated control and regulation of previously characterized by manual activities processes. Not only the work safety is increased, but also an automation of material flow or high-pressure treatment is possible in a simple way, so that a very efficient process can be realized for a variety of applications, in particular largely independent of the hazard class of extracted solvents or of the selected Impregnation medium, in particular also largely independent of the type of granules to be treated.

Figures 17A, 17B, 17C show in detail a variant in which a rotary actuator 25 (in particular rod) is coupled to a plurality of treatment planes 27, respectively plates, each treatment plane being defined by a pair of plates 27, of which the a stationary and static is arranged and the other is rotatably displaceable and rotatably connected to the actuator 25 is connected. A respective partial charge 2.1, 2.2, 2.n can be shifted between the individual treatment levels, in particular gravity-driven in reaction to a relative rotation of the two plates of a respective treatment level relative to one another.

The rotational adjustment movement can be at least approximately a continuous movement, or optionally, the rotational adjustment movement can also be discontinuous between at least two adjustment positions (in particular open position and closed position).

In particular, Fig. 17A shows in detail the use and arrangement of individual treatment levels in the fixed volume Vi, wherein at least one rotary actuator 25 is provided. The material flow can also be explained using the example of FIG. 17A: bulk material 1 is supplied as a single partial charge 2.1. In the high-pressure treatment volume, several bulk material partial charges 2.1, 2.2, 2.n result in the entire bulk material charge under high-pressure treatment. The bulk material flow continues, for example, through several discharged partial batches. In this case, at least one sensor unit 35 may be provided, in particular for temperature, pressure, force, displacement, mass and / or flow.

FIGS. 17B, 17C illustrate how the respective treatment level can be set in a quenching state or in a transmitting state. Fig. 17B illustrates a passing state in which a respective passage segment 27.1 of the upper plate rotatably connected to the actuator is arranged in a rotational position in alignment with a respective passage segment 27.1 of the lower stationary plate. In this case, moreover, a respective inclined, in particular conical (in particular saddle-roof-shaped) segment 27.3 of the upper plate is arranged in alignment with a respective planar segment 27.2 of the lower plate. The respective paired plate assembly 27 can be through. The sloped surfaces can perform a function as drain slopes for the bulk material and also reduce the risk of unwanted local bulk material deposits.

Fig. 17C illustrates a partitioning condition in which a respective inclined, in particular conical, segment 27.3 of the upper plate is arranged in alignment with a respective passage segment 27.1 of the lower plate in response to a rotational adjustment movement Dg (rotation angle change). The respective paired plate assembly 27 locks.

The individual plates 27 are in particular designed in each case as a circular disc with the already described recesses (passage openings). Optionally, the levels z27 can be separated individually or simultaneously together the rotatory Actuating be actuated. The passage openings 27.1 can be arranged in alignment or offset.

The plate pair 27 shown in Fig. 17B may also be configured as a pair of two planar plates each having at least one passage 27.1 in other embodiments.

The respective adjusting movement in the exemplary embodiment shown in FIGS. 17A, 17B, 17C can ensure a material flow of a plurality of partial batches 2.1, 2.n over a section along the material flow path through the high-pressure treatment volume Vi. The rotary adjusting movement can be a continuous and / or an at least temporarily clocked adjusting movement. The (respective) rotary actuating movement can be specified uniformly for the entire high-pressure treatment volume for all high-pressure treatment levels, and / or at least temporarily specified in each case specifically for individual predefinable high-pressure treatment levels z27.

In FIG. 18, by way of example, a relative orientation of passage segments 27.1 relative to adjacent passage segments 27.1 in the respective subsequent treatment level is explained. The passage segments 27.1 are each offset in rotation angle to each other.

FIG. 19 schematically shows a variant with actuators which can be actuated in a translatory manner. Rotary kinematics can optionally also be integrated into the internal volume Vi.

20A, 20B there is shown a pressure vessel device 10 with a combined tray module formed of a first section 200 with a pivoting kinematics 23 and a second section 800 with a rotary kinematics, the pivoting kinematics 23 upstream in series from the rotary kinematics is arranged. This embodiment can in particular high volume increase of the bulk material during the high-pressure treatment be advantageous, especially if a subsequent extraction is carried out at a substantially constant volume. The pivoting kinematics with comparatively small heights between the levels allows a gentle treatment of the bulk material, and the subsequent rotational kinematics particularly favors efficient use of the available internal volume.

FIGS. 21A, 21B show a pressure vessel device 10 with a combined support floor module or a combination of at least two support floor modules, which is formed from a first section 200 with a pivoting kinematics 23 and from a second section 800 with a rotary kinematics the pivoting kinematics 23 is arranged upstream in series by the rotary kinematics. Downstream of the respective module 200, 800 may be provided a unit (in particular funnels with bulk material conductive function) for guiding the material flow, in particular with a funnel-shaped geometry. These units (preferably rigid internals) can direct the flow of material to the subsequent module or to the outlet, in particular for the purpose of spiraling the flow of the outlet.

Figures 22A, 22B show a pressure vessel apparatus 10 having a combined tray module formed of a first section 800 having a rotary kinematics and a second section 200 having a pivoting kinematics 23, the pivoting kinematics 23 being arranged downstream of the rotary kinematics is. In this arrangement, by means of the pivoting kinematics 23, the discharge / discharge of bulk material can be facilitated, in particular with regard to the size of partial batches. LIST OF REFERENCE NUMBERS

1 bulk material or granulate (bulk)

2 batch

2.1, 2.2, 2. n partial lot

10; 100; 110 pressure vessel device

11 lid

11.1 Fastening means or flange for inlet fitting

11.2 Passage for bulk material

11.3 Feedthrough for actuator

11.4 Seal on the actuator

11.5 Fasteners

11.7 Centering

12 high pressure resistant wall

12.1 cylindrical section

12.2 conical section

13 inlet fitting, in particular two-channel

13.1 inlet member, in particular valve and / or lock

13.2 Inlet line

14 heating device, in particular heating jacket

15 outlet fitting, in particular container bottom unit

15.1 outlet member, in particular bottom valve and / or lock

15.2 inwardly opening closing element, in particular cone

15.3 actuator

15.4 Outlet outlet

16 inlet / outlet fitting, in particular neck

17 inlet / outlet fitting, in particular neck

20; 200; 300; 400; 500; 600; 700; 800; 900; 990 support module 21 cover 22 drive unit, in particular with pneumatic cylinder

23 Kinematics, in particular Schwenkkinematik

24 crossbar

25 actuator, in particular push / pull rod

25a lateral adjusting means

25.1 Lever

25.2 Swivel

25.3 further swivel joint

26 intermediate element (geometrically coupling)

27 treatment level, in particular with perforated plate or braid

27a, 27b first and second part of the treatment level, in particular in pivotable storage

27.1 passage segment

27.2 flat segment

27.3 inclined, in particular conical or saddle roof-shaped segment

28 Support unit, in particular (centering) ring

29 holding unit, in particular holding bar (s)

30 high pressure treatment system

31 control device

33 logic unit

35 sensor unit, in particular for temperature, pressure, force, displacement, mass and / or flow

37 storage tank, reservoir

39 dosage

M1 first medium flow: bulk material

M2 second medium flow: high-pressure medium or extraction medium, optionally comprising impregnation medium

M3 third media stream: solvent M center longitudinal axis

U environment

Vi inner volume or cavity enclosed by the pressure vessel S1 first step, in particular feeding of bulk material

51.1 Activation of at least one treatment level

51.2 Feeding a batch

52 second step, in particular pressure build-up

53 third step, in particular extracting

S4 fourth step, especially impregnation

55 fifth step, especially pressure reduction

56 sixth step, in particular discharge of bulk material

56.1 Activation of at least one treatment level

56.2 Carrying out a partial batch

S7 seventh step, in particular high-pressure-tight partitioning of the internal volume at the outlet fitting z27 treatment level or height position of the treatment plane x width direction or pivot axis

y transverse or depth direction, swivel axis

z Vertical or gravity direction or height direction a first pivot angle, in particular upwards against the direction of gravity

ß second pivot angle, in particular downward in the direction of gravity g rotation angle of a rotary adjusting movement

Claims

claims

1. A method for high pressure treatment of bulk material (1) by extraction and / or impregnation, which in the internal volume (Vi) of a pressure vessel device (10; 100) is arranged and at a high pressure level, in particular high pressure in the range of 40 to 1000bar, with foreclosure of the Environment (U) is treated,

characterized in that the high-pressure treatment is carried out batchwise in a closed system in the pressure vessel device by the bulk material to the inner volume (Vi) supplied batchwise with closed pressure vessel device and arranged on at least one treatment level and is discharged batchwise from the inner volume after high pressure treatment with closed pressure vessel device, wherein the high-pressure treatment is performed on a plurality of treatment levels (27) arranged in the inner volume (Vi).

2. The method according to the preceding method claim, wherein the batchwise feeding of the bulk material (1) comprises feeding partial batches (2.1, 2.2, 2.n) each to one of a plurality of treatment levels (27), in particular successively first to a lowest treatment level and then each on a further above treatment level arranged, in particular gravity-driven in the direction of gravity (z); and / or wherein the batchwise discharging of the bulk material is a discharge of partial charges (2.1, 2.2,

2.n) in each case from one of a plurality of treatment levels (27), in particular successively first from a lowermost treatment level and then each from a further above treatment level arranged, in particular gravity-driven in the direction of gravity (z); and / or wherein the high-pressure treatment is carried out on at least three treatment levels (27) arranged in the internal volume (Vi), in particular on at least three treatment levels.

3. The method according to any one of the preceding method claims, wherein in the batchwise feeding and / or the batch discharge at least one of the internal volume (Vi) arranged treatment levels (27) for passing the bulk material (1, 2.1, 2.2, 2.n) is displaced, in particular is pivoted, in particular by automated actuation; and / or wherein batch feeding and batch discharging unidirectionally in a single direction through the internal volume (Vi) through, in particular in the axial direction of gravity down.

4. The method according to any one of the preceding method claims, wherein the feeding and / or discharging is carried out at a pressure level between ambient pressure and high pressure level, in particular at least 2 or 3bar, in particular at about 6bar or about 10bar; and / or wherein the high pressure treatment is carried out batchwise for a plurality of closed system batches in the sealed pressure vessel device (10; 100).

5. The method according to any preceding method claims, wherein the supply of bulk material is detected during feeding and / or discharging, in particular gravimetrically, in particular with respect to individual bulk partial charges (2.1, 2.2, 2.n); and / or wherein in batchwise feeding and / or discharging, an activation of inlet and / or outlet fittings (13, 15) takes place, in particular as a function of gravimetric measured values of bulk bulk batches recorded in real time.

6. The method according to any one of the preceding method claims, wherein the high pressure treatment comprises at least one extraction, in particular solvent extraction; and / or wherein the high-pressure treatment comprises at least one impregnation, in particular the impregnation of polymers; or wherein the high-pressure treatment comprises both an extraction and an impregnation, in particular the extraction of monomers and the impregnation with additives; and / or wherein the high-pressure treatment comprises at least one solvent extraction and is carried out above the critical temperature and above the critical pressure of the solvent.

7. The method according to any one of the preceding method claims, wherein bulk material is high pressure treated in an embodiment as aerogels by extraction and / or by impregnation.

8. The method according to any one of the preceding method claims, wherein the high-pressure treatment comprises fluidizing the bulk material, in particular in a fluidized bed, in particular in an output-side region of the pressure vessel device.

9. Control device (31) configured for carrying out a method according to one of the preceding method claims, wherein the control device is coupled to at least one sensor unit (35) for detecting a flow of bulk material (1) or a mass or a mass difference or a volume or a volume difference is optionally also configured with at least one sensor unit for detecting a path and / or a force.

Use of a support floor module (20; 200; 300; 400; 500; 600; 700; 800; 900; 990) having a plurality of treatment levels for high-pressure treatment of bulk material (1) by extraction and / or impregnation in a closed, of the Environment (U) pressure-sealed system, wherein the support bottom module in the internal volume (Vi) of a pressure vessel device (10; 100) is arranged, wherein the treatment levels (27) for high-pressure treatment and / or for passing the bulk material (1, 2.1, 2.2, 2. n) be stored and positioned displaceably adjustable in the inner volume.

1 1. pressure vessel device (10; 100; 1 10) arranged for high-pressure treatment of bulk material (1) by extraction and / or impregnation, with a lid (1 1) and a high pressure resistant wall (12), which wall encloses an internal volume (Vi) , as well as with an inlet fitting (13) coupled to the internal volume and an outlet fitting (15) in each case for the bulk material;

characterized in that the pressure vessel device comprises a support floor module (20; 200; 300; 400; 500; 600; 700; 800; 900; 990) having a plurality of actuatable treatment levels (27), which treatment levels can be arranged in the internal volume (Vi) and can be loaded with bulk material in a batchwise manner with the pressure vessel device closed, and after the high-pressure treatment which has taken place on the high-pressure level in the case of a closed pressure vessel device can be partially discharged batchwise, that the High pressure treatment in a closed, isolated from the environment (U) system is executable.

12. Pressure vessel device according to the preceding claim, wherein the pressure vessel device has an automatically actuatable inlet fitting (13) for the batchwise feeding of the bulk material, in particular to the lid (1 1, 21) coupled; and / or wherein the pressure vessel device has an automatically actuatable outlet fitting (15) for the batch discharge of the bulk material, in particular coupled to a bottom of the pressure vessel device.

13. Pressure vessel device according to one of the preceding claims, wherein the at least one treatment level (27) is adapted for the passage of bulk material (1); and / or wherein at least a portion of the respective drying level from a corresponding high-pressure treatment position in at least one loading / unloading position is displaced, in particular by means of pivoting kinematics; and / or wherein the support floor module has a pivoting kinematics (23) with in a respective treatment plane with respect to at least one pivot axis (x, y) symmetrical structure.

14. Pressure vessel device according to one of the preceding claims, wherein at least one of the treatment levels (27) by at least one gas-permeable plate (27, 27 a, 27 b) is defined; and / or wherein the respective treatment level is defined by at least one pivotally actuatable gas-permeable plate (27a, 27b), in particular by two relative to each other about a pivot axis (x, y) pivotally mounted plates, in particular at least downwardly pivotable; and / or wherein the respective treatment level (27) is defined by two gas-permeable plates (27a, 27b) mounted relative to each other on a transverse web (24) downwardly and upwardly pivotable about a pivot axis (x, y), in particular with the transverse web held on at least two vertically extending holding units (29), in particular by a first pivot angle (a) upwards of at least 60 ° or 75 °, preferably at least 85 ° or 90 °, and by a second pivot angle (ß) downwards of at least 45 ° or 60 °.

15. Pressure vessel device according to one of the preceding claims, wherein the respective treatment level (27) is actuated between at least two positions, namely a first position for the passage of bulk material (1) and in a second position for receiving and high-pressure treatment of bulk material, in particular by means of a the cover (1 1, 21) integrated or fastened to the cover drive unit (22) and at least one actuatable actuator (25); and / or wherein the pressure vessel device has at least one drive unit (22) and a plurality of actuators (25) in the form of push / pull rods arranged for bi-directional translational actuation of the respective treatment level (27a, 27b), in particular with the actuators in a linear arrangement next to each other in a transverse plane (xz, yz); and / or wherein the respective treatment level (27) or a plate (27a, 27b) of the treatment level via at least one adjusting lever (25.1) and two hinges (25.2, 25.3) to a aktuierbares, high pressure tight through the lid (11, 21) into the inner volume guided actuator (25) is coupled; and / or wherein the pressure vessel device comprises a pneumatic, hydraulic, electrical, electromagnetic and / or magnetic drive unit (22) which is coupled to the at least one treatment level (27).

16. Pressure vessel device according to one of the preceding claims, wherein the support floor module (20; 200) in the lid (1 1) is integrated or at least by means of the lid (1 1) in the internal volume (Vi) held, arranged and / or supported; and / or wherein one / the inlet fitting (13) for bulk material is integrated in the lid (11), in particular in an arrangement with a vertical conveying direction.

17. Pressure vessel device according to one of the preceding claims, wherein at least three treatment levels (27) are provided, in particular at least five treatment levels.

18. Pressure vessel device according to one of the preceding claims, wherein the respective treatment level is displaceable by at least one rotatably actuatable actuator.

19. Pressure vessel device according to one of the preceding claims, wherein the respective treatment level is displaceable by at least one translatorically actuable actuator.

20. Pressure vessel device according to one of the preceding claims, wherein the

Tragbodenmodul both at least one translational actuatable actuator and at least one rotatably actuatable actuator comprises.