EP3897900A2

EP3897900A2 - Device and method for the continuous high-pressure treatment of bulk material and use thereof

Info

Publication number: EP3897900A2
Application number: EP19832108.5A
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: 2019-12-20
Publication date: 2021-10-27
Also published as: EP3897899A2; KR20200097340A; WO2020127957A2; KR102369887B1; DE102018222881A1; EP3727626A1; WO2019122387A1; KR102592507B1; DE102018222883A1; WO2020127957A3; US20220072447A1; WO2020127889A2; WO2020127889A4; KR20210119971A; US20220062788A1; WO2020127957A4; DE102018222882A1; US11612831B2; DE102018222874A1; KR102556664B1

Abstract

The invention relates to a method for the high-pressure treatment of bulk material (1) via extraction and/or impregnation, which bulk material is arranged in the high-pressure treatment volume (Vi) of a pressure container device (20) an treated at a high pressure level, in particular high pressure in the region of 40 to 1000 bar, wherein the method comprises at least the three following, respectively individually controllable step sequences: pressure application (V1), high-pressure treatment (V2), release; wherein the high-pressure treatment (V2) is carried out continuously in the high-pressure treatment volume (Vi), wherein the high-pressure treatment volume (Vi) or the entire pressure container device (20) is arranged stationarily during the high-pressure treatment (V2), and wherein the continuity of the high-pressure treatment (V2) is ensured solely by the one high-pressure treatment volume (Vi), and wherein the bulk material is conveyed through the high-pressure treatment volume by means of a rotational adjusting movement or according to at least one translational adjusting movement during the high-pressure treatment. This enables, in particular, a process optimisation of high-pressure treatment process, e.g. the extraction. The invention relates to a corresponding device for the high-pressure treatment of bulk material.

Description

Device and method for the continuous high pressure treatment of bulk material and use

Description:

The invention relates to a device and a method for the continuous high-pressure treatment of bulk material, in particular by extraction and / or impregnation. In particular, the invention relates to the use of a pressure vessel device with at least one actuator for adjusting the material flow in the continuous high-pressure treatment of bulk material. In particular, the invention relates to a device and a method in each case according to the preamble of the respective independent claim.

Bulk goods, especially in the form of granules, have to be freed from substances, especially solvents, in many cases. Depending on the application, the bulk goods are also subjected to pure extraction without the need for solvents. The extraction can advantageously be carried out under high pressure, in particular at pressures above 100 bar, in particular in connection with the action of heat at an elevated temperature generated in a controlled manner. It is known that extraction, in particular extraction of solvent (s), can in many cases preferably be carried out using supercritical fluids or extraction media (for example carbon dioxide CO ₂ , propane, butane), in particular since surface forces or surface tensions can be minimized and the extraction becomes particularly effective, also with regard to a drying effect. Both liquids (fluids in the liquid phase, in particular also viscous fluids) and solids can be subjected to extraction as starting materials. Both the high-pressure treated bulk material (also referred to as raffinate in this state) and extracts obtained by extraction can, depending on the application, be called the product of high-pressure treatment.

Prominent examples of extraction processes are the decaffeination of tea leaves, coffee beans or the extraction of hops. Since the extraction is related to the manufacture of various intermediate and end-user products, especially from the food industry, the number of variants is also different from Extraction process comparatively high. This is also reflected in the different variants with regard to construction and the size range of the systems. For example, it is not uncommon to realize an extraction column with a height of more than 10m, or to connect several extractors (pressure vessels) to one another. In any case, a large variety of variants can be observed in the existing system concepts, also with regard to size variations.

Comparable examples can be enumerated for impregnation processes, be they carried out separately or in combination with an extraction.

So far, extraction, in particular extractive solvent removal, has been carried out in the case of bulk material or granules in many cases by arranging the bulk material in an extractor (pressure vessel), in particular in a layer with a predetermined maximum layer height, which layer applies extraction medium (in particular C0 ₂ ) and is flowed through. A basket-like insert, which is also referred to as a product holding basket, is usually used to arrange the bulk material in the high-pressure treatment volume (i.e. in the receiving cavity for the granulate defined by the pressure container), for example with a volume of approx. 250 liters and with a cylindrical jacket wall a gas-permeable, wire mesh-like, perforated plate-like or sintered metal filter base, on which the insert basket is supported in the extractor. A filter cover of the basket can also be gas-permeable, wire mesh-like, perforated plate-like or made of sintered metal. The basket-like insert can be introduced into the area of a lid of the extractor, and after the extraction, the bulk material largely freed from solvent can be removed for further use by removing the basket-like insert. The next batch can then be arranged in the extractor using the same or a further basket-like insert. In other words, the high-pressure treatment process is carried out in batches, and the basket-like use is also intended to facilitate the handling of the respective batch.

With the previous method of extractive solvent removal, a comparatively high expenditure of personnel and time is required. The handling of the basket-like insert cannot be automated easily. If the bulk goods are dangerous goods or become harmful or flammable media or solvents are used, considerable effort must also be made with regard to safety, in particular occupational safety or explosion protection, not least because people with specialist knowledge for manual work usually have to be involved.

A disadvantage of previous devices and methods is not only the handling of the bulk material (material flow), but also the dusts or gases that form, in particular explosive gas mixtures, and health impairments for the people involved. There is therefore interest in simplifying high-pressure treatment processes for bulk goods, in particular for large quantities of bulk goods, in particular for extraction and / or impregnation.

JP 1293129 A describes a high-pressure process in which a storage container and a collecting container facilitate the batch-wise provision of bulk material in the high-pressure chamber, the bulk material sliding gravitationally in batches through a high-pressure treatment chamber as a function of the supply and discharge.

CN 1827201 A describes a high-pressure treatment process in which the high-pressure container is conveyed through a type of pressure lock.

DE 42 16 295 A1 describes a method for high-pressure treatment in which a container which is open on both sides is used, an advantageous throughput or an advantageous process control being able to be ensured by means of a translatory movement of a piston and by means of several chamber regions.

EP 1 725 706 B1 describes the transfer of pretreated solid as a suspension to a high pressure stage.

The object of the invention is to provide a device and a method with the features described at the outset, with which the high-pressure treatment of bulk material can be simplified or the device or process engineering outlay associated with the high-pressure treatment can be reduced, in particular with the highest possible efficiency of the method (Throughput per unit of time). Aspects of Occupational safety and health risks can be taken into account. Last but not least, there is also interest in a (time-) efficient high-pressure treatment process, especially for extraction, especially extraction of solvent (s), and / or for the impregnation of bulk goods of very different types, so that the process - despite any optimization measures with regard to efficient high-pressure treatment (Keyword: maximized throughput) - can guarantee the greatest possible variability.

This object is achieved by the devices and methods described below.

This object is achieved according to the invention by a method for high-pressure treatment of bulk material by extraction and / or impregnation, which bulk material is arranged in the high-pressure treatment volume of a pressure vessel device and is treated at a high-pressure level, in particular high pressure in the range from 40 to 1000 bar, with isolation from the environment, whereby the method comprises at least the three following step sequences which can be individually regulated (in particular with regard to material flow): pressurization V1, high pressure treatment V2, relaxation V3.

According to the invention, it is proposed that the high-pressure treatment or the high-pressure treatment in the second step sequence V2 is carried out in a continuous manner at the high-pressure level in a closed system in the high-pressure treatment volume, the high-pressure treatment volume or the entire pressure vessel device being / remaining stationary (static) during the high-pressure treatment, whereby the continuity of the high-pressure treatment or the high-pressure treatment sequence of steps is ensured solely by means of the one (single) high-pressure treatment volume Vi, and the bulk material is conveyed by the high-pressure treatment volume by means of a rotary actuating movement or as a function of at least one translatory actuating movement, in particular by continuous or discontinuous relocation of a single batch or a plurality of partial batches. This enables simplifications in the process management and can also ensure advantages with regard to a large turnover of bulk material (output quantity). There are also advantages, particularly with regard to the material flow of bulk goods that vary greatly in volume, in particular also with volume increases in the range of factor 10, for example especially during drying.

A / the rotary actuating movement is preferably carried out by rotating a rod or shaft or similar rotary drive means arranged in the high-pressure treatment volume (optionally guided through the wall of the pressure vessel device), and takes place about at least one longitudinal axis or actuating axis of the pressure vessel device arranged centrally or eccentrically in the inner volume . Optionally, several rotary positioning movements around several positioning axes can take place. Optionally, a material flow of one or more batches can be ensured through the entire high-pressure treatment volume by means of a respective adjusting movement. Optionally, a material flow of a plurality of partial batches can be ensured over a section along the material flow path through the high-pressure treatment volume by means of a respective adjusting movement. The rotary actuating movement can be a continuous and / or an at least temporarily actuated movement. The (respective) rotary actuating movement can be specified uniformly for the entire high-pressure treatment volume, and / or at least at times can be specified specifically for individual predefinable high-pressure treatment levels.

A / the translational actuating movement is preferably carried out by translating a rod or similar drive means arranged in the high-pressure treatment volume (optionally led through the wall of the pressure container device), in particular along at least one longitudinal axis or adjusting axis of the pressure container device arranged centrally or eccentrically in the inner volume. Several translational positioning movements can optionally be carried out. Optionally, a material flow of one or more batches can be ensured through the entire high-pressure treatment volume by means of a respective adjusting movement. Optionally, a material flow of a plurality of partial batches can be ensured over a section along the material flow path through the high-pressure treatment volume by means of a respective adjusting movement. The translational actuating movement can be a continuous and / or an at least temporarily timed actuating movement. The (respective) translatory adjusting movement can be uniform for the whole High-pressure treatment volumes are specified, and / or at least from time to time are specified specifically for individual predefinable high-pressure treatment levels.

The sequence of pressures V1 and relaxation V3 can be (partially) batch-wise for individual bulk (partial) batches as discontinuous processes individually at least with regard to bulk material flow and / or pressure level, i.e. they are separate from the continuous high-pressure treatment and are individual controllable, especially independent of material flow and high pressure conditions in the second step sequence V2. The discontinuous procedure (upstream and downstream of the high-pressure treatment) can also include pressurization and relaxation for individual partial batches of bulk material, the size of the respective partial batch being independent of a batch or partial batch treated in the second step sequence.

The high pressure range from 40 to 1000 bar can be further differentiated depending on the application. In particular, the advantageous high-pressure range can be restricted to 40 to 400 bar or 50 to 300 bar and / or to 650 to 1000 bar. At particularly high pressures, the solution properties of the extraction medium can in particular also be set or changed. Process-related advantages can also arise in the high pressure range from 100 to 250 bar, in particular 100 to 200 bar. Optionally, a pressure range below or above a critical point of an extraction medium used (for example C0 ₂ ) can be set.

Either a pure substance or a mixture of substances can be used as the extraction medium, especially with process parameters above the critical point of the substance or above a critical line of a two-substance mixture or above a critical area of a mixture of substances from more than two substances ( especially three-substance mixtures).

In the examples of extraction explained below, an extraction of substances (loading) other than solvents can also be referred to synonymously for extraction of solvents. A continuous high-pressure treatment is to be understood as a high-pressure treatment in which no process interruption due to pressure fluctuations and / or due to material flow is required for the high-pressure treatment of the bulk material, but in which the high-pressure treatment at the high-pressure level is optionally continuously unchanged without any time interruption and (at least theoretically ) can be carried out without time restriction and (at least theoretically) without restriction with regard to the amount (mass, volume) of the bulk material treated, in particular also with continuous material flow within the high-pressure treatment volume. In the case of continuous high-pressure treatment, the desired or required high pressure can be ensured at any desired time, in particular also independently of preparatory and post-processing steps. The high pressure level does not have to be lowered; in particular, the high pressure level does not have to be lowered in order to ensure the flow of bulk material. The material flow can either be by continuous shifting, in particular of at least one entire batch (no distinction with regard to individual partial batches along the material flow path within the high-pressure treatment volume), or by discontinuous shifting of a single batch or of partial batches, in particular in individual sections of the material flow path be ensured in the high-pressure treatment volume. Any pressure fluctuations are at most technical, for example due to the supply and / or discharge of material. Optionally, the continuous high-pressure treatment can also include setting / regulating a temperature level that is kept constant (as good as possible depending on the application). The continuous high-pressure treatment at a (single) predefined high-pressure level, which can be kept / regulated constantly within narrow tolerance limits, enables an exact predefinition of extraction conditions or process parameters for the high-pressure treatment. This can also improve the quality of the product obtained.

Optionally, in addition to the at least approximately constant high pressure level, a temperature level in the high pressure treatment volume can also be set; in particular, a constant temperature can be maintained. Optionally, a temperature cycle in the High-pressure treatment volumes are driven, especially in connection with the supply and / or discharge of material.

A stationary arrangement is to be understood as a static arrangement in which the high-pressure treatment volume or the corresponding high-pressure treatment cavity delimited by the pressure container device (or by its wall) can remain arranged in a stationary manner. In other words, the pressure vessel device or the entire arrangement does not have to take on any function with regard to bulk material shifting by shifting the high-pressure treatment volume. In any case, in the case of a stationary arrangement, no displacement of the high-pressure treatment volume relative to the other components of the arrangement is necessary. The material flow function does not have to be fulfilled by means of the high-pressure treatment volume. In other words: that

According to the invention, high-pressure treatment volume does not have to be moved (neither absolutely nor relatively) in order to ensure the continuity of the process (continuous material flow). Rather, the bulk material can be supplied to the high-pressure treatment volume and discharged again without having to interrupt the high-pressure treatment. One or more (continuous or discontinuous) actuating movements can optionally be carried out within the high-pressure treatment volume, in particular to define a specific type of material flow in the continuous high-pressure treatment, but the high-pressure treatment volume can remain stationary. This not least facilitates the coupling of the high-pressure treatment volume to the first and third sequence of steps, and last but not least, there are also advantages with regard to the pressure-tight design of the entire arrangement.

A single or single high-pressure treatment volume is to be understood as an embodiment in which the high-pressure treatment does not have to be carried out in successive individual volumes, but in which the respective batch is arranged only once in a single container, in a single cavity or in a single volume and is subjected to high pressure treatment. The high-pressure treatment volume can limit the entire material flow path of the bulk material provided for the high-pressure treatment. The high-pressure treatment volume can therefore also be as a high pressure treatment cavity enclosed by the pressure vessel device in a high pressure-tight manner can be described.

In many applications, significantly more time is required for an extraction phase than for an impregnation phase, especially for natural product extraction. The high-pressure treatment time, which is considerable for the design of the method, can be predefined primarily from the time required for the extraction. The start and end times (in the sense of a dwell time for the bulk material) of the respective phase of the high pressure treatment and their duration can be set individually depending on the bulk material and medium.

A procedure for material flow and high pressure medium in counterflow to one another can also be advantageous. In the case of an extraction, the high-pressure medium can correspond to an extraction medium used. According to the invention, the manner in which bulk material and high-pressure medium are guided and forwarded can be adapted to the respective application in a very varied and very flexible manner (e.g. pressure level, type of bulk material, type of solvent). High-pressure medium, in particular extraction medium, and bulk material can optionally also be conveyed in the same direction.

In this case, in particular when extracting solvent (s), in particular also with aerogels as the starting material, an inclination of the pressure vessel device or the high-pressure treatment volume with respect to the horizontal can be advantageous, in particular with regard to the outflow or discharge of liquid solvent. An angle in the range of 10 to 30 ° with respect to the horizontal or optionally also with respect to the vertical has proven to be advantageous for this. The slope can be ascending or descending.

A high pressure is built up in the first step sequence V1. This can be done in particular according to two variants. On the one hand, a high-pressure pump can be provided, which can optionally also have several heads. Alternatively, several high-pressure pumps can be used in parallel. On the other hand, when the pressure has already built up, the first sequence of steps V1 can essentially only be provided for one to provide the respective bulk goods batch for the pressure container device or for the second sequence of steps V2.

Several relaxation units or relaxation containers can be provided for the third sequence of steps V3 (relaxation device). This can increase the flexibility or variability in terms of bulk material discharge. The relaxation is preferably carried out in a discontinuous manner, depending on the high pressure level, in particular in several stages. The respective container can be locked for this.

In the third sequence of steps V3, a comparatively long expansion line can optionally also be provided, in particular immediately downstream of the second sequence of steps V2. The expansion line enables a structurally very simple and robust arrangement and can minimize the process or system engineering effort for the expansion V3.

The invention relates to a method or a device with which the extraction can proceed continuously, in particular in such a way that a cycle of loading, pressure build-up, high-pressure treatment or extraction, relaxation and unloading, at least in relation to the high-pressure treatment, which has been operated in batch steps up to now in any case or extraction can be operated in a continuous manner, so that the type of high-pressure treatment can be decoupled from the preparatory and postprocessing steps. In addition to advantages in terms of variability and customizability and controllability of the high-pressure treatment process, this also enables a higher production capacity to be achieved than with a classic arrangement (with a comparable system size). Process engineering advantages can be realized in particular because the high-pressure treatment does not have to be carried out in a cycle selected in the first step sequence V1 (pressurization) and / or in the third step sequence V3 (relaxation).

According to the invention, the granulate (bulk material) can be introduced into the high-pressure container at extraction pressure and can be discharged again after a defined time. without having to change the high pressure treatment level. For example, extraction medium can also be continuously conveyed through the high-pressure container.

The variants described here for realizing the material flow are particularly advantageous even in the event of drastic volume changes. For example, a pressure vessel device with a translatory conveying device in the form of a push rod with pivotally mounted plates for defining series-connected cavities for partial batches in the high-pressure treatment volume in the respective cavity can be filled with bulk material up to half the maximum filling height, in relation to a volume of the unexpanded bulk material, so that for the high-pressure treatment, a doubling of the volume of the bulk material is tolerable when the high-pressure treatment volume is gradually passed through from cavity to cavity.

In contrast to this, in the case of a batchwise (batch) batch process that has usually been carried out hitherto, the starting material for the extraction can in many cases only be piled up to a certain height, in particular in order to avoid excessive compression. A pressure vessel is filled cyclically, high pressure is applied and the extraction medium flows through for high pressure treatment. The pressure vessel is then relaxed and emptied again. In the case of a discontinuous (partially) batch-wise process management, the pressurization and the high pressure treatment depend on the material flow. The material flow can only take place depending on the pressure conditions. In particular, the pressure must be relieved to a pressure well below the required high pressure level in order to be able to convey the bulk material further. The discontinuous, batch-wise process control (batch operation) is therefore comparatively complex, at least with regard to the required pressure fluctuations, because at least a relaxation or pressure reduction of the high-pressure level is required for each batch.

According to the invention, the pressure build-up, the high-pressure treatment and the relaxation can be spatially separated from one another. In particular, the bulk material can be brought to pressure in a first volume and conveyed to a second volume (high-pressure treatment volume). In the second volume the process pressure prevails at all times, so that in the second volume, the high pressure treatment can be carried out in a continuous manner. The treated bulk material (granulate) is conveyed from the second volume (continuously or in individual partial batches) to a third volume in which the relaxation can take place. Exemplary embodiments according to the invention are described in more detail below.

It has been shown 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). In the case of aerogels in particular, solvent extraction may be desired / required. In the case of aerogels (highly porous solids) in particular, a change in volume, in particular an increase in volume, can be particularly strong during high pressure treatment, for example in the range of a factor of 10, or in other words, for example in the range of 2-3 times the radius increase. The variants described here for realizing the material flow are particularly advantageous even in the event of drastic volume changes. For example, a pressure vessel device with a conveyor in the form of a screw conveyor, in particular in a horizontal orientation, can be filled with bulk goods up to half the maximum fill level in relation to a volume of the unexpanded bulk goods, so that a doubling of the volume of the bulk goods is tolerable for the high pressure treatment .

According to the invention, granular starting material (bulk material in the form of granules, airgel bodies, pellets, powder, beans and / or particles) can be freed from a load in an extractive manner, in particular from solvent (s). Supercritical drying can also take place, in particular by means of CO ₂ . The term “supercritical drying” is understood to mean drying in particular in the sense of extraction of solvents and / or water using an extraction medium (for example C0 ₂ ), the state of which lies above the critical point (or above the critical line or area).

One of the exemplary embodiments (in particular a first variant) can in particular have the following components:

Pressurization device with at least one pump set up to apply high pressure to the granulate in the first step sequence V1; Pressure vessel device, in particular in the form of a high-pressure extractor, in particular as a vertically oriented extractor, for the second sequence of steps V2;

Conveying device, in particular screw conveyor, in particular arranged along the longitudinal axis of the pressure vessel device;

Inlet / outlet member and optionally also inlet / outlet fitting, in particular each comprising a connecting piece (connection), the outlet member being part of an outlet fitting, in particular also comprising a downpipe;

Relaxation device with at least one relaxation tank

(Relaxation unit), for the third sequence of steps V3.

Exemplary mode of operation: Granules or bulk goods are fed under high pressure into the pressure vessel device, in particular directed to the lower end of a conveyor device or to the upper side of a translationally displaceable and / or pivotable level, and / or the granules (in particular a partial batch) is promoted from one partial volume to an adjacent partial volume. Optionally, a / the conveying device conveys the bulk material in the high-pressure treatment volume by moving the bulk material along the material flow path in the

High pressure treatment volume, especially upwards and further into a downpipe. At the same time, extraction medium, in particular C0 _{2, is introduced} through a nozzle (connection) into the high-pressure treatment volume, which flows through the bed in countercurrent, frees from solvent and leaves the high-pressure treatment volume again through a further nozzle. Liquid solvent collects at the bottom of the high-pressure treatment volume and is discharged there through a nozzle or outlet. After (continuous or discontinuous) discharge from the high-pressure treatment volume, the bulk material is passed into one of several expansion tanks. These are shut off with a valve, whereupon the relaxation can take place in the respective relaxation tank.

A further exemplary embodiment (in particular a second variant) can, in a modification or in addition to the variant described above, in particular have the following components:

horizontal or slightly inclined pressure vessel device with extractor (pressure vessel device set up for extraction); Conveying device, in particular screw conveyor, in particular with its longitudinal axis in the same orientation as the pressure vessel device, in particular in a horizontal or slightly inclined orientation; or

pivotable and / or translationally displaceable levels or plates, arranged individually or in pairs in a plurality of translational longitudinal positions.

The conveying device is in particular arranged within a tube made of perforated sheet metal or wire mesh (inside the bulkhead arranged inside the high-pressure treatment volume), which is permeable to fluids, but acts as a bulkhead for the bulk material.

Another exemplary mode of operation: The bulk material is brought to pressure as already described and introduced into the high-pressure treatment volume at the appropriate connection piece (inlet fitting). In a predefinable unit of time, the bulk material is conveyed through the high-pressure treatment volume by means of the conveying device, while at the same time C0 _{2 is passed} through the bed, for the extraction of the solvent from the bulk material. Liquid solvent can pass through a fluid-permeable wall (internal partitioning, for example with perforated sheet metal) and be collected and discharged at an exit point, in particular on an underside of the pressure vessel device. The bulk material can be discharged, for example, by falling or being discharged into an outlet connection at one end of the tube / extractor. The relaxation can be carried out as in the variant described above.

Alternatively, a piston engine with (in relation to a pump) reverse function can be used for the relaxation. This piston engine is preferably connected in such a way that mechanical energy is recovered, which is preferably used to build up pressure in the first step sequence V1. Both processes (compression and relaxation) are then preferably mechanically coupled. As a further embodiment, the relaxation can be achieved via the pressure loss in a long relaxation line. In other words, the continuity of the high pressure treatment can also be advantageous from an energy point of view, especially when using a relaxation motor. A relaxation motor is to be understood as a unit that is set up to supply the high pressure medium with energy via mechanical work To remove relaxation, in particular by means of pistons or turbines driven by the high pressure medium.

For example, relaxation in the third step sequence V3 can take place in particular according to at least two different variants: relaxation in or by means of a pressure-driven piston; Relaxation in a predefined relaxation volume (cavity with a predefined size / geometry). A pressure translation can also take place. A volume change can also take place directly in the (respective) outlet fitting, with a variable transfer cavity (in particular provided by a pressure-driven piston). Relaxation energy can be recovered by means of the piston.

Another exemplary mode of operation: in the first step sequence V1, the bulk material is pressurized by means of at least one pump and conveyed into the high-pressure treatment volume of the pressure vessel device. The high-pressure treatment volume is flowed through in countercurrent (in particular with C0 ₂ ) in order to carry out an extraction. The C0 ₂ (extraction medium) is introduced at one nozzle and leaves the high-pressure treatment volume at another nozzle. Liquid solvent is drained off at another nozzle. The nozzles are each equipped with retention devices for bulk material, eg with sieve plates. At the outlet end of the tube, a relaxation is prepared by the third sequence of steps V3, in particular by means of a piston engine. The bulk material can be shifted by means of rotary adjustment movements.

In this case, externally operable / unlockable check valves can also be provided, in particular in order to facilitate regulated conveying of the bulk material.

Advantageously, the pressure vessel device can be heavily utilized in the respective mode of operation, in particular in terms of space almost 100% with regard to the volume available for high pressure treatment, and in particular also in terms of time (no time intervals without high pressure treatment). Pressure build-up or relaxation phases are not necessary. Compared to a discontinuous process, only a fraction of the load changes are required, if at all. Ultimately, there are also economic advantages, in particular thanks to the high throughput of bulk material.

According to one embodiment, individual partial batches are supplied to the high-pressure treatment volume and / or discharged from the high-pressure treatment volume during the high-pressure treatment. Handling the material flow in partial batches can also provide advantages in terms of pressure build-up and relaxation.

According to one embodiment, in the case of continuous high-pressure treatment, a constant displacement speed of the bulk material or a clocking of a discontinuous partial batch-wise displacement, in particular between individual high-pressure treatment levels, and thereby the dwell time or the high-pressure treatment time for the bulk material in the high-pressure treatment volume is set by means of the rotary actuating movement. This also provides an advantageous distribution, mixing and / or flow around the bulk material or the respective batch. In addition, the volume available for the high-pressure treatment can be used well, in particular by adapting the bed volumetrically to the available high-pressure treatment volume with regard to volume increases.

According to one embodiment, the bulk material flow is regulated in continuous high-pressure treatment by the bulk material being shifted continuously or in individual discontinuous partial batches in the high-pressure treatment volume by the rotary actuating movement depending on the size and / or a timing of supplied (partial) batches. This adjustability can further improve the variability of the entire process.

In this case, a timing with alternating direction of an actuating movement can also be provided, for example for a back and forth movement. Optionally, the inlet and the outlet can be provided on the same side of the pressure vessel device. Optionally, the direction of material flow within the high-pressure treatment volume can be reversed, in particular by switching the direction of rotation of at least one rotary actuator. In an advantageous arrangement, the pressure vessel device is arranged inclined, in particular with an inclination of the longitudinal axis in the range of approximately 10 to 30 degrees with respect to the horizontal plane, the inclination being able to increase or decrease in the direction of material flow. Especially with an inclined arrangement, the

Material flow path laterally limited by a gas-permeable pipe or bulkhead or plate.

According to one embodiment, the continuous high-pressure treatment comprises fluidizing the bulk material, in particular in the sense of a fluidized bed (active generation or regulation of the transition from a fixed bed to a fluidized bed). The fluidized bed is in particular generated exclusively by means of an extraction medium. The bulk material is advantageously introduced into a fluidized bed in which only one high-pressure treatment level is provided for the fluidized bed (in particular in the form of a displaceable or pivotable flap level or as a rotatable or rotating plate level), 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 corresponding treatment level can be sealed off or closed before the bulk material is removed (bulk material is collected). The fluidized bed can also be formed on several treatment levels, in particular on several levels one above the other (fluidized bed in a broader sense). The fluidized bed enables advantageous mass transport properties to be achieved in combination with unlimited expansion of the treated bulk materials. For example, with polystyrene (PS) granules, a targeted surface treatment can also be carried out. For example, with polystyrene (PS) granules, a targeted surface treatment can also be carried out.

After high pressure treatment, the gas flow is preferably reduced (reduced throughput) and the bulk material can be collected at the (respective) treatment level. The high-pressure treatment volume can be provided as a single volume for the entire high-pressure process, that is to say for the entire high-pressure treatment stage V2. In other words, it is not necessary to provide a plurality of high pressure stages.

According to one embodiment, the high-pressure treatment step sequence V2 is carried out exclusively at the one (single) high-pressure level. Last but not least, this results in time advantages. Pressure fluctuations do not have to be built up or reduced. The process is becoming leaner and, last but not least, cheaper and more energy efficient. The fact that the (single) high pressure level can be maintained also makes the continuous process more precise, because without the need for pressure fluctuations, the effect of high pressure treatment on the bulk material can be adjusted as precisely as possible, in particular via the dwell time, in particular depending on a single predefined / predefinable pressure levels.

According to one embodiment, during the high-pressure treatment, individual partial batches of bulk material generated in the first step sequence are supplied to the high-pressure treatment volume, the partial batches forming a batch under continuous high-pressure treatment. As a result, the individual step sequences can also be decoupled from one another in terms of process technology. The first sequence of steps can e.g. be optimized with regard to the size of the partial batch and with regard to pressure stages, without the second sequence of steps having to be changed or adapted thereby. Apart from the supply of bulk material, the second step sequence can also remain decoupled from the first step sequence with regard to continuous or discontinuous material flow in the high-pressure treatment volume and can be individually regulated and optimized. The present invention accordingly also enables a considerable simplification when optimizing method parameters of the second sequence of steps.

According to one variant, partial batches can also be supplied at the desired high pressure level. Optionally, the pressure level in an inlet fitting can also be lower than the high pressure level, in particular also with a gravity-driven supply of bulk material. The first step sequence is preferred on the output side provided pressure at least as high as the high pressure level. This can also favor the material flow.

According to one embodiment, individual partial batches are discharged from the high-pressure treatment volume during the high-pressure treatment. This also allows the material flow in the high-pressure treatment volume to be optimized. Particularly in the case of sensitive bulk goods which, for example, must not be mechanically compressed to a great extent, working in partial batches can be advantageous, in particular on individual high-pressure treatment levels.

In the following, advantageous configurations with regard to a control-technical coordination of all three step sequences V1, V2 and V3 are explained.

According to one exemplary embodiment, in the first step sequence of pressurization, the (partial) batch material flow quantity that can be set in batches, in particular the size of the respective (partial) batch and / or a timing of the (partial) batch, is calculated as a function of the Sequence of steps envisaged for the bulk material throughput (absolute material flow) or the high pressure level. By adjusting the process parameters in the first step sequence by adapting (partial) batch sizes or timing to the requirements or process parameters of the second step sequence, the setting of process parameters in the second step sequence can remain as flexible as possible. According to the invention, therefore, there are large optimization potentials and a large variety of variants for the second sequence of steps, which widens the range of applications for high-pressure treatment.

According to one exemplary embodiment, the relaxation of the batch-wise bulk material flow quantity, in particular the size of the respective (partial) batch and / or a timing of the (partial) batches, as a function of the bulk material flow or the high-pressure level in the high-pressure treatment -Step sequence regulated. This also makes it possible to optimize the second sequence of steps with regard to the material flow and to optimize it as focused as possible with regard to the high pressure treatment as such. According to one exemplary embodiment, a respective bulk batch of bulk goods provided by the first sequence of pressures is smaller in volume or in mass than the batch under continuous high-pressure treatment, that is to say smaller than the amount of bulk material treated or relocated during high-pressure treatment, in particular by a factor of 3 up to 1000 smaller. This also results in great procedural flexibility. The factor can, for example, also be 10 or 100, depending on the application and the type of bulk material.

According to one exemplary embodiment, in continuous high-pressure treatment, the dwell time or the high-pressure treatment time for the bulk material in the high-pressure treatment volume is set by regulating, in particular, a constant displacement speed of the bulk material (preferably continuous movement, continuous material flow) or by regulating a cycle of a discontinuous displacement of high-pressure-treated partial batches between individual high-pressure treatment levels. As a result, the desired effects of the high pressure treatment can be set or optimized in a comparatively exact manner despite the continuity of the method.

According to one exemplary embodiment, the bulk material flow is regulated in continuous high-pressure treatment, in that the bulk material is displaced continuously or in individual discontinuous partial batches in the high-pressure treatment volume depending on the size and / or a timing of supplied partial batches. This provides flexibility and a wide range of variants, also with regard to the material flow during high-pressure treatment, so that a wide range of applications can be developed for various bulk materials.

The invention is also based on the concept of spatially separating or separating the individual step sequences. By decoupling the material flow in the first and third sequence of steps from the material flow in the second sequence of steps, spatial decoupling can optionally take place. This not only has spatial advantages, but also provides great degrees of freedom when designing the process, especially when choosing the most advantageous system components for high-pressure treatment. In the following, advantageous configurations with regard to the high pressure treatment V2 step sequence are explained.

According to one exemplary embodiment, the bulk material for the high-pressure treatment V2 is arranged on at least one predefined first high-pressure treatment level and, starting from this first high-pressure treatment level, continuously or between further high-pressure treatment levels (that is to say from high-pressure treatment level to high-pressure treatment level) in the high-pressure treatment volume during high-pressure treatment V2 by means of the rotary or translational actuating movement and / or shifted in response to the rotational or translational actuating movement. As a result, sensitive bulk goods in particular can be treated efficiently. An arrangement on individual levels can also provide advantages with regard to a flow of high pressure medium that is as homogeneous as possible.

According to one exemplary embodiment, the continuous high-pressure treatment comprises continuous displacement of the bulk material in a predefined direction of material flow in the high-pressure treatment volume, in particular in a horizontal, vertical or in an inclined upward direction. As a result, the direction of material flow and the direction of flow of high-pressure medium can also be coordinated.

According to one embodiment, a dwell time of the bulk material in the high-pressure treatment volume is set by continuously displacing the bulk material (bulk material constantly in motion) or by discontinuous displacement between individual high-pressure treatment levels during high-pressure treatment, in particular by setting a rotational speed of rotary actuators and / or by clocking rotary or translatory actuators or optionally also gravitational force driven or optionally additionally by adjusting the speed or by clocking translatory actuators optionally additionally provided. As a result, the effects of high-pressure treatment can be influenced in an exact manner, in particular locally independently and in terms of process technology independently of the first and third sequence of steps. According to one embodiment, the continuous high-pressure treatment comprises a continuous displacement of the bulk material in two different predefined material flow directions in the high-pressure treatment volume Vi, in particular in two opposite material flow directions, namely a material flow direction predetermined by the rotary or translational actuating movement and in a second gravitational force-driven material flow direction. This also makes it possible to implement advantageous configurations for moving the bulk material in the high-pressure treatment volume. In addition, the entry and the discharge of the material can optionally take place at the same end of the pressure vessel device, for example on the floor.

According to one exemplary embodiment, the continuous high-pressure treatment comprises continuously displacing the bulk material against gravity (or gravitational force) by supplying potential energy into the bulk material by means of the rotary or translational actuating movement. In this way, the discharge of bulk material from the high-pressure treatment volume can be optimized in particular.

In the following, advantageous configurations with regard to the manner in which bulk material is displaced are explained in the high pressure treatment V2 step sequence.

According to one exemplary embodiment, the continuous high-pressure treatment comprises a continuous displacement of the bulk material or a discontinuous displacement between individual high-pressure treatment levels, in each case by means of a rotation or translation, in particular by a rotation or translation, of at least one rotary or translational actuating element about an axis of rotation oriented in the material flow direction. According to one exemplary embodiment, the continuous high-pressure treatment comprises shifting the bulk material in batches by means of rotation or translation, in particular by means of temporally timed rotation or translation of at least one rotary or translatory actuator. As a result, the bulk goods can be relocated in a technically simple and exact manner. The rotary actuating movement can advantageously be coupled into the high-pressure treatment volume. The continuous high-pressure treatment can optionally also comprise a continuous displacement of the bulk material or a discontinuous displacement between individual high-pressure treatment levels, each by translating at least one optionally additionally provided translatory actuating element, in addition to at least one rotary actuating movement. In this way, the material flow can also be decoupled from gravity.

According to one exemplary embodiment, the continuous high-pressure treatment comprises, at least in sections, an autonomous, gravitational force-driven continuous displacement of the bulk material. In particular, this also provides a lean construction in terms of device technology, the material flow being able to take place at least in sections in an autonomous manner, for example in connection with a downpipe.

According to one exemplary embodiment, the continuous high-pressure treatment comprises fluidizing the bulk material, in particular in at least one fluidized bed, in particular in an area on the outlet side of the pressure vessel device. In this way, in particular, an effective mass transfer can be ensured, that is, an efficient high-pressure treatment. The at least one fluidized bed is in particular generated exclusively by means of an extraction medium.

If the high-pressure treatment volume is defined by a single coherent compartment or has only one high-pressure treatment level, the fluidized bed can be generated in the entire compartment (fluidized bed in the classic, narrower sense). If the high-pressure treatment volume is defined by a plurality of compartments and / or has a plurality of high-pressure treatment levels, the fluidized bed can also be adjusted by means of turbulent flow behavior and associated turbulent fluidization in the respective compartment or on the respective high-pressure treatment level (fluidized bed in the broader sense in the manner of a plurality of turbulent vortex areas).

According to one exemplary embodiment, the continuous high-pressure treatment comprises a continuous displacement of the bulk material by means of a continuous rotary actuating movement or by means of several discontinuous translatory actuating movements, in particular with the rotary actuator designed as a screw conveyor or coupled to a screw conveyor, or in particular with the translatory actuator designed as a push rod with at least one gas-permeable plate pivotally mounted thereon. This also provides a device technology structure for a wide range of applications. The positioning axis of the rotary actuator can define the axis of rotation of a screw conveyor.

According to one embodiment, the continuous high-pressure treatment comprises a discontinuous gravitational force-driven displacement of the bulk material by several discontinuous rotary actuating movements, in particular with the rotary actuator in the form of a shaft with at least one gas-permeable plate with at least one passage segment connected to it in a rotationally fixed manner. This also enables a targeted influence on the arrangement of the bulk material or the respective partial batches within the high-pressure treatment volume. The rotary actuating movement can also be specified via the respective high-pressure treatment level (opposite kinematics; vice versa).

According to one exemplary embodiment, the continuous high-pressure treatment comprises discontinuous displacement of the bulk material in individually displaced / relocatable partial batches, in each case between predefined high-pressure treatment levels, in particular between high-pressure treatment levels, each defined by at least one gas-permeable plate or gas-permeable bulkhead that is arranged horizontally or inclined relative to the horizontal (in particular, can be actuated by rotation). In this way, in particular the material flow and the mass transport can also be optimized, in particular also in the case of bulk material or granulate, which may only be compressed a little or be subjected to little mechanical or abrasive stress.

Any type of element that is permeable or blocking for fluids can be understood as a plate, which enables an at least partial separation in the high-pressure treatment volume and is set up (at least in sections) to define one of the high-pressure treatment levels. The plate can be arranged in a stationary or displaceable manner. The plate can in particular also be set up to arrange a partial batch of the bulk material. Optionally, the plate can be in inclined orientation and / or can be arranged pivotably, alternatively also rotatably or additionally also translationally displaceable, or vice versa.

In the following, advantageous configurations of the step sequence pressurization V1 are explained.

According to one exemplary embodiment, the first step sequence of pressurization is carried out in a discontinuous manner and comprises at least one step from the following group: partial batch pressure generation, in particular by means of a pump, and / or partial batch feed of bulk material to the high pressure treatment step sequence by means of an inlet fitting receiving the respective partial batch. The inlet valve can e.g. include a punch, a seat-cone fitting (fitting in the narrower sense), a ball valve and / or a flap. The principle of using a stamp is disclosed, for example, in published patent application DE 42 16 295 A1.

According to one exemplary embodiment, the step sequence of pressurization comprises partial batch feeding of bulk material, the partial batch feeding being carried out by means of an inlet fitting with at least one inlet member, in particular a valve and / or lock (pressure lock, cellular wheel lock). As a result, the material flow can also be decoupled from high-pressure treatment parameters in the second step sequence.

The partial batch supply of bulk material for pressurization and / or a partial batch discharge of bulk material after high pressure treatment has been carried out can also be carried out at multiply graduated pressure levels, in particular at a pressure level between ambient pressure and high pressure level, in particular at at least 2 or 3 bar, in particular at more than 6 or above 10bar. Depending on the application, the ambient pressure can also be increased in relation to atmospheric pressure, in particular in the range from 3 to 10 bar.

Bulk material discharged from the high pressure treatment volume can also be conveyed based on a pressure difference (suction conveyance). There is no oppression required. A suppression can optionally be generated in the third sequence of steps to convey the bulk material downstream of the high-pressure treatment step.

The devices in the pressure application step sequence and in the relaxation step sequence are set up to ensure a pressure difference of at least 40 bar individually or in total (in particular from ambient pressure or atmospheric pressure to the high pressure level).

Advantageous embodiments of the relaxation sequence V3 are explained below.

According to one exemplary embodiment, the third expansion sequence is carried out in a discontinuous manner and comprises at least one step from the following group: partial batch expansion, in particular by means of a piston engine, and / or partial batch discharge of bulk material from the high pressure treatment sequence by means of an outlet fitting accommodating the respective partial batch. The outlet fitting can e.g. comprise a punch, a ball valve, a seat-cone fitting (fitting in the narrower sense) and / or a flap.

According to one exemplary embodiment, the relaxation sequence comprises a partial batch discharge of bulk material, the partial batch discharge being carried out by means of an outlet fitting with at least one outlet element, in particular a valve and / or lock (pressure lock, cellular wheel lock). In this way, the material flow can also be decoupled from high-pressure treatment parameters in the second sequence of steps.

According to one exemplary embodiment, the quantity of bulk material is recorded, in particular in a gravimetric manner, in particular in relation to individual partial batches of bulk material, when supplying and / or discharging bulk material in at least one of the step sequences of pressurization and expansion. This not only enables the material flow to be monitored, but also facilitates control, particularly with regard to partial batches (in particular times, volumes). According to one exemplary embodiment, when supplying and / or discharging bulk material in batches, in at least one of the pressurization and expansion step sequences, inlet and / or outlet fittings are activated, in particular as a function of gravimetric measured values of partial batches of bulk material recorded in real time. This favors further optimization measures, especially with regard to material flow.

Advantageous configurations of the high pressure treatment V2 step sequence are explained below.

According to one exemplary embodiment, the continuous high-pressure treatment comprises at least one continuous extraction, in particular extraction of solvents. This also enables process parameters specially optimized for the extraction process. This also provides procedural synergies, especially with regard to the extraction or reuse of solvents.

According to one exemplary embodiment, the continuous high-pressure treatment comprises at least one continuous impregnation, in particular the impregnation of polymers. This also enables process parameters specially optimized for the impregnation process. This also enables process engineering synergy effects to be realized. The impregnation can also be carried out in combination with at least one extraction.

According to one embodiment, the continuous high-pressure treatment comprises both a continuous extraction and a continuous impregnation, in particular the extraction of monomers and the impregnation with additives. This also widens the range of applications of the invention.

According to one exemplary embodiment, the high-pressure treatment comprises at least one continuous extraction of solvent (s) and is carried out above the critical temperature and above the critical pressure of the extraction medium (that is to say supercritically). In particular, this also provides high process efficiency, in particular since this enables surface forces to be minimized and the extraction to be particularly effective, also with regard to a drying effect. A particularly high continuous throughput can thus also be achieved. As starting materials, both Liquids (fluids in the liquid phase, in particular also viscous fluids) and solids are subjected to extraction. The following can be mentioned as examples of high-pressure treated bulk goods:

Granules (in particular polymer granules), airgel bodies, pellets, powders, beans, particles and / or other free-flowing accumulations of a large number of bodies.

According to one embodiment, the continuous high-pressure treatment comprises high-pressure medium flowing through the bulk material, in particular in countercurrent to a continuous or discontinuous displacement (or

Direction of displacement / direction of material flow) of the bulk material. This also enables advantages in terms of mass transfer and homogeneity of the high pressure treatment to be realized.

According to one embodiment, the continuous high-pressure treatment is carried out at constant high pressure or in the event of unavoidable pressure fluctuations due to technical reasons (more or less noticeable depending on the application), in particular at a high pressure in the range from 500 to 1000 bar. Such pressure fluctuations, for example due to control valves, pulsations, lock processes or temperature fluctuations, are in the range from 3 to 5 bar or in the maximum single-digit percentage range of the high pressure level. This continuously constant pressure level also enables high procedural efficiency. Optionally, an active pressure control in the direction of the target high pressure level can take place from a pressure variation of 1 bar or 2 bar, in particular if the technically induced unavoidable pressure fluctuations are comparatively strong. In the area of these technical variations, the high pressure level can be considered / defined according to the present definition as constant.

According to one exemplary embodiment, the pressure container device comprises a pneumatic, hydraulic, electrical, electromagnetic and / or magnetic drive unit, which is coupled to at least one rotationally actuatable treatment level, in particular by means of an actuator. This simplifies automation, and the type of drive can be selected in particular as a function of the bulk material to be treated. In the embodiments of a translational actuation described below, the advantages described above in connection with a rotary actuation result in particular.

According to one embodiment, the at least one translational actuator is designed as a pull and / or push rod (unidirectionally or bidirectionally actuating), which extends in the radial direction. This also provides advantages in terms of customizable control of a single one of a large number of high-pressure treatment levels.

According to one embodiment, the translatory actuator has a promoting effect on the bulk material for material flow at least approximately in the direction of gravity. Last but not least, this also has advantages in terms of gravity-driven discharge of bulk material.

According to one exemplary embodiment, in the case of continuous high-pressure treatment, the translational actuating movement sets a displacement speed or a clocking of a discontinuous partial batch-wise displacement, in particular between individual high-pressure treatment levels or between individual partial volumes, the residence time or the high-pressure treatment time for the bulk material in the high-pressure treatment volume thereby being set.

According to one embodiment, the bulk material is conveyed in batches through the high-pressure treatment volume in batches during the high-pressure treatment, in that the translational actuator is moved back and forth between a first stroke position and a second stroke position and thereby actuates at least one swivel kinematics for the passage or blocking of material flow.

According to one embodiment, the bulk material is conveyed in batches through the high-pressure treatment volume in batches during the high-pressure treatment, in that the translational actuator is moved back and forth between at least two translationally displaceable levels between a first stroke position and a second stroke position. According to one embodiment, the bulk material is conveyed in batches through the high-pressure treatment volume in batches during the high-pressure treatment, in that the translational actuator is moved back and forth between a first stroke position and a second stroke position, the respective stroke position being defined in each case by a fixedly arranged high-pressure treatment level.

According to one embodiment, the bulk material is conveyed in batches through the high-pressure treatment volume in batches during the high-pressure treatment, in that the translational actuator is moved back and forth between a first stroke position and a second stroke position, the first stroke movement from the first to the second stroke position being a blocking stroke movement with a displaced pivoting kinematics and a passing pivoting kinematics, and wherein the second lifting movement from the second to the first stroke position is a permitting lifting motion with a displacing pivoting kinematics arranged and a blocking pivoting kinematics arranged.

According to one embodiment, the bulk material for the high-pressure treatment is arranged on at least one predefined first high-pressure treatment level and, based on this first high-pressure treatment level, is shifted between further high-pressure treatment levels in the high-pressure treatment volume during the high-pressure treatment by means of the respective translational actuating movement.

According to one embodiment, a discontinuous partial batch transfer between individual high-pressure treatment levels during high-pressure treatment by means of the respective translational actuating movement sets a dwell time of the bulk material in the high-pressure treatment volume, in particular by clocking the respective translatory actuating element, in particular by clocking a plurality of translatory actuating elements, in each case as a function of time.

According to one exemplary embodiment, the continuous high-pressure treatment comprises a discontinuous batch-wise gravitational force-driven displacement of the bulk material, in particular at least approximately in the direction of gravity. According to one exemplary embodiment, the continuous high-pressure treatment comprises discontinuous partial batch displacement of the bulk material by a plurality of individual translatory positioning movements, in particular back and forth movements, in particular with at least one translatory positioning element in the form of a push rod with at least one pivot kinematics mounted axially fixed thereon.

According to one embodiment, the continuous high-pressure treatment comprises a discontinuous partial batch-wise gravitational force-driven displacement of the bulk material by several discontinuous translatory positioning movements, in particular with at least one translatory positioning element in the form of a push / pull rod with at least one unidirectionally locking pivoting kinematics comprising at least one gas-permeable plate.

According to the invention, the aforementioned object is also achieved by a

Control device set up to carry out a previously described method, wherein the control device is coupled to at least one sensor unit set up for detecting a flow of bulk material or a mass or a mass difference or a volume, which sensor unit in the material flow path in

High-pressure treatment volume can be arranged, the control device optionally also comprising at least one sensor unit configured to detect a path and / or a force and / or a pressure, the control device being configured to evaluate and regulate a rotary actuating movement or a translatory actuating movement in each case for specifying the bulk material -Material flow through a / the high pressure treatment volume. This results in the aforementioned advantages.

The control device or the sensor unit can be connected to an actuator

Pressure vessel device can be coupled. The respective sensor unit can in particular also be coupled to an inlet or outlet fitting or integrated therein.

According to the invention, the aforementioned object is also achieved by a

High-pressure treatment arrangement set up for high-pressure treatment of bulk goods by extraction and / or impregnation at a high-pressure level, in particular high pressure in the range from 40 to 1000 bar, comprising: a pressurizing device with pressure generating means, in particular at least one pump, for pressurizing V1 as a first step sequence;

a pressure vessel device coupled to the pressurization device in a high-pressure-tight connection with a high-pressure-resistant wall enclosing a high-pressure treatment volume, for the high-pressure treatment V2 as a second step sequence; a relaxation device coupled to the pressure vessel device in a high-pressure-tight connection for a relaxation V3 as a third sequence of steps;

wherein the pressure vessel device for the high pressure treatment can be arranged / arranged in a fixed manner and is set up for continuous high pressure treatment solely by means of the one (single) fixedly arranged high pressure treatment volume at the high pressure level, and wherein the pressure vessel device is a rotary actuator (an actuator which can be adjusted by rotation) or an actuator which can be displaced in translation has and is set up for a rotary adjustment movement or for at least one translatory adjustment movement in each case for the displacement of the bulk material during the high pressure treatment by the high pressure treatment volume, in particular from an inlet fitting to an outlet fitting or to a unit coupled to the outlet fitting. This results in the aforementioned advantages. At least the high pressure level is preferably present after the first sequence of steps V1. An extractant circuit can e.g. set up by means of a high-pressure pump to provide a pressure level at least at the high-pressure level, in particular also independently of the material flow in the high-pressure treatment volume.

According to one exemplary embodiment, the high-pressure treatment arrangement is set up for supplying individual batches of bulk material to the high-pressure treatment volume during the high-pressure treatment and furthermore set up for continuous or discontinuous displacement of the bulk material as a single batch or in partial batches in the high-pressure treatment volume during the high-pressure treatment. Last but not least, this also provides high variability, depending on the application.

According to one exemplary embodiment, the high-pressure treatment arrangement is set up to discharge individual partial batches from the high-pressure treatment volume during the high-pressure treatment. This also allows the material flow to be adjusted in a flexible manner or be regulated. In the high-pressure treatment volume, at least one predefined first high-pressure treatment level or optionally also further high-pressure treatment levels can be provided, each configured to arrange the bulk material (or a batch or several partial batches) in predefined longitudinal or vertical positions. The discharge can optionally take place at a central outlet, but optionally also at several decentralized outlets, in particular also specifically for each high-pressure treatment level.

In other words, the pressure vessel device is set up in particular for continuous high-pressure treatment at the high-pressure level, in that the high-pressure treatment arrangement has an inlet fitting coupled to the high-pressure treatment volume in a high-pressure-tight connection and an outlet fitting in each case for the bulk material, which can be controlled discontinuously and in each case to provide individual bulk material batches can be regulated individually, at least with regard to the bulk material flow, that the high-pressure treatment can be carried out in a continuous manner at the high-pressure level in the high-pressure treatment volume Vi.

According to one embodiment, the rotary actuator is designed as a screw conveyor, in particular with its longitudinal axis in alignment with the longitudinal axis of the high-pressure treatment volume or parallel to it. Last but not least, this provides a very robust structure.

According to one embodiment, the rotary actuator is designed as a screw conveyor, which extends around a down pipe for discharging the bulk material. Last but not least, this also has advantages in terms of gravity-driven discharge of bulk material.

According to one embodiment, the rotary actuator is designed as a screw conveyor, which is arranged in a fluid-permeable, in particular gas-permeable and bulk material partitioning tube (internal partitioning). Last but not least, this favors the separation of extracted media from the bed.

According to one embodiment, the rotary actuator is designed as an eccentric screw arranged in the high-pressure treatment volume, optional also several actuators can be provided. Last but not least, this also allows for variations in the dwell time. In particular, comparatively sensitive, sensitive bulk goods in smaller partial batches can simultaneously be simultaneously treated with high pressure.

According to one embodiment, the rotary actuator is set up to actuate at least one plate with at least one passage segment, to arrange or to pass bulk material in each case in a high-pressure treatment plane defined by the plate. This also favors a partial batch transfer of the bulk goods.

According to one exemplary embodiment, the pressure vessel device has at least one high-pressure treatment level, which is arranged such that it is stationary in the high-pressure treatment volume Vi or can be adjusted or displaced and can be loaded with bulk material when the pressure vessel device is closed and which can be unloaded when the high pressure treatment takes place or after the high pressure treatment has taken place with the pressure vessel device closed, that the high pressure treatment can be carried out in a continuous manner. For this purpose, the respective high-pressure treatment level can be oriented inclined, for example. The respective high-pressure treatment plane can optionally be oriented at least approximately orthogonally to the direction of gravity and be movable and / or adjustable in the cross-sectional profile. This allows the material flow to be regulated.

According to one embodiment, the inlet fitting for the partial batch feed of the bulk material to the second step sequence V2 (high pressure treatment) can be actuated automatically, a transfer cavity being able to be provided in particular by means of a piston or a (cellular wheel) lock. The same applies to the outlet fitting and to the partial batch discharge of the bulk material from the high-pressure treatment step sequence. This also simplifies control of the material flow, in each case in particular also based on measurement data from gravimetric and / or volumetric sensors, and / or based on a timing. According to one exemplary embodiment, the pressure container device defines an at least approximately vertically oriented material flow direction through the high-pressure treatment volume, in particular through the rotary actuating movement. This also offers advantages through the use of gravity; the discharge of the bulk material can also be simplified.

According to one embodiment, the pressure vessel device defines a material flow direction that is inclined with respect to the vertical or the horizontal, in particular at an angle of 10 to 30 °, in particular by the rotary actuating movement. In this way, advantages in terms of mass transport and / or in terms of mixing the bed can also be realized. The material flow direction can be specified by means of the actuating movement.

According to one exemplary embodiment, the pressure container device defines an at least approximately horizontally oriented material flow direction, in particular by means of the rotary actuating movement. This also provides advantages in terms of draining extracted media, particularly in terms of collecting and discharging liquid solvent. In the case of a horizontal arrangement, the material flow can also be set and controlled largely independently of gravitational forces, so that comparatively high variability with regard to the selection of the bulk material (mass, density, surface quality) can also be ensured. Here, e.g. the use of non-return valves may also be advantageous, in particular as barriers between individual compartments of the high-pressure treatment volume.

According to one exemplary embodiment, at least one of the high-pressure treatment planes is defined by at least one gas-permeable plate arranged horizontally (or orthogonally to the direction of gravity) or inclined with respect to the horizontal, or by a correspondingly arranged gas-permeable bulkhead. The inclined arrangement also enables autonomous gravity-driven bulk material transfer in the high-pressure treatment volume. In the case of an inclined arrangement of the plate, the plate preferably extends only over approximately 3/4 of the diameter of the pressure vessel device. With an inclined arrangement of several plates, the plates can be cascaded be arranged to each other. This configuration is also advantageous with regard to volume changes in the bulk material.

A horizontal arrangement can also be understood to mean an arrangement at least approximately orthogonal to the longitudinal extent of the pressure vessel device.

According to one exemplary embodiment, a plurality of high-pressure treatment levels are defined in the high-pressure treatment volume by gas-permeable plates, each of which is arranged in pairs, one of which is in a rotationally fixed connection with the rotary actuator. This also enables a simple, robust construction in which the material flow between individual levels can be predefined in a simple manner.

According to one exemplary embodiment, a plurality of high-pressure treatment levels are defined in the high-pressure treatment volume by gas-permeable plates arranged in pairs, each of which is axially fixed to the respective translational actuating element via a pivoting kinematics, in particular with pivoting kinematics which block on one side.

According to one exemplary embodiment, a plurality of high-pressure treatment levels are defined in the high-pressure treatment volume each by at least one gas-permeable plate with bevels and with at least one passage segment, in particular in an aligned arrangement centrally in the high-pressure treatment volume. Last but not least, this also facilitates an arrangement that is gentle on the granules and has advantageous bed thicknesses.

According to one embodiment, the rotary or translationally displaceable actuator is set up for individually actuating one high-pressure treatment level of the pressure vessel device and / or for simultaneous synchronous actuation of all high-pressure treatment levels of the pressure vessel device. This also provides a high degree of variability. The actuator can, for example, be connected in a rotationally fixed manner to a plate in a respective high-pressure treatment level. Optionally, a locking mechanism can also be provided. According to one exemplary embodiment, the pressure vessel device has at least one rotationally displaceable actuator designed to actuate at least one high-pressure treatment level of the pressure vessel device, and in particular optionally additionally also a translationally displaceable actuator, in particular at least one actuator that is coupled from the environment into the high-pressure treatment volume in a pressure-tight manner. As a result, partial batches in particular

High-pressure treatment volumes can be shifted individually.

The respective actuator can be guided into the pressure vessel device on at least one bushing, e.g. by means of a stuffing box or a magnetic coupling. Optionally, a motor (fluid motor, electric motor) can also be provided for actuating the respective actuator, optionally also within the

Pressure vessel device.

According to one embodiment, the inlet fitting comprises at least one inlet member, in particular a valve and / or a (cellular wheel) lock. The inlet fitting can optionally also have several or different inlet members, in particular with a variable-size transfer cavity.

According to one exemplary embodiment, the translational actuator can be moved back and forth between a first stroke position and a second stroke position, the first and second stroke positions each being defined by a high-pressure treatment level.

According to one exemplary embodiment, the translational actuator is kinematically coupled to a pivoting kinematics that can be arranged in a blocking and permeable manner. Last but not least, this favors the relocation of partial batches using robust, simple kinematics.

According to one exemplary embodiment, the pressure vessel device has at least one pivoting kinematics which can be arranged in a blocking and permeable manner and are arranged in a fixed manner in the high-pressure treatment volume. According to one embodiment, the pressure vessel device has at least a first and at least a second pivoting kinematics, which are respectively blocking and transmitting in the same pivoting direction.

According to one exemplary embodiment, the pressure vessel device has at least one displaceable pivoting kinematics which are coupled to the translational actuating element, and therefore at least one second pivoting kinematics which are arranged in a stationary manner in the high-pressure treatment volume. This favors a batch-wise conveying of partial batches through the high-pressure treatment volume in predefined length sections. The local arrangement of the bed can thus be predefined in a comparatively exact manner. This can e.g. can also be advantageous with regard to impregnation or series connection of several high-pressure treatment steps.

According to one embodiment, the first and second pivot kinematics of the pressure container device are designed to pivot autonomously without a pivot drive, that is to say pivoting solely in response to translational movement or in response to a force exerted by bulk material.

According to one embodiment, a respective high-pressure treatment level is defined by at least one gas-permeable plate.

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 set up for bidirectional translational actuation of the respective high-pressure treatment level, in particular with the actuators in a linear arrangement next to one another in a transverse plane.

According to one exemplary embodiment, the respective high-pressure treatment level or a plate of the high-pressure treatment level is coupled via at least one adjusting lever and two swivel joints to an actuatable actuator that is guided into the high-pressure treatment volume in a high-pressure-tight manner. This kinematics in particular also enables a bidirectionally controllable swiveling movement. According to one exemplary embodiment, the pressure container device comprises a pneumatic, hydraulic, electrical, electromagnetic and / or magnetic drive unit which is coupled to the at least one level or high-pressure treatment level. With regard to the type of drive, the optimization can take place in the respective application.

According to one embodiment, the translational actuator is designed as a push rod, in particular with its longitudinal axis in alignment with the longitudinal axis of the high-pressure treatment volume or parallel to it. This also favors a simple construction.

According to one embodiment, the translational actuator is designed as a push rod with a plurality of pivot kinematics connected axially fixed thereto. This can simplify the entire kinematics, in particular thanks to a central actuating movement.

Depending on the application, the configurations described above with regard to translation can be used alternatively or in addition to the rotary configurations.

The above-mentioned object is also achieved according to the invention by using a pressure vessel device for the continuous high-pressure treatment of bulk material by extraction and / or impregnation in a closed system which is sealed off from the environment U in a high-pressure-tight manner, the high-pressure treatment V2 being carried out as a sequence of steps between pressurization V1 and relaxation V3 and is regulated individually, the bulk material being continuously displaced in a fixedly arranged high-pressure treatment volume in the pressure vessel device or being displaced in partial batches, in particular between individual high-pressure treatment levels, at predefinable / predefined times by the bulk material being used by means of at least one rotary actuating movement or depending on at least one translatory actuating movement is promoted (shifted) through the high-pressure treatment volume, in particular using the pressure vessel device in a previously described method, in particular using the pressure container device in a previously described high-pressure treatment arrangement, in particular under high pressure at pressures above 40 to 1000 bar. This results in numerous advantages mentioned above.

The aforementioned object is also achieved according to the invention by using a pressure vessel device for the continuous high-pressure treatment of bulk material in the form of polymers, by extraction and optionally also by impregnation, for supercritical drying to provide the polymers as super-insulators, the high-pressure treatment V2 being a sequence of steps between one Pressurization V1 and a relaxation V3 is carried out, the bulk material being treated in a fixedly arranged high-pressure treatment volume in a continuous manner at the high-pressure level, in that the bulk material is conveyed through the high-pressure treatment volume by means of at least one rotary actuating movement or as a function of at least one translatory actuating movement Use of the pressure container device in a previously described method, in particular use of the pressure container device in a previously described high pressure Jerk treatment arrangement, especially under high pressure at pressures above 40 to 1000 bar. This results in numerous advantages mentioned above.

The above-mentioned object is also achieved according to the invention by using a pressure vessel device for the continuous high-pressure treatment of bulk material in the form of aerogels, by extraction and / or by impregnation in a closed system which is sealed off from the environment in a high-pressure-tight manner, the continuous high-pressure treatment V2 being a sequence of steps between pressurization V1 and a relaxation V3 is carried out, the bulk material being treated in a fixedly arranged high-pressure treatment volume Vi in a continuous manner at the high-pressure level, the bulk material being continuously displaced in the pressure vessel device or in partial batches, in particular between individual high-pressure treatment levels, at predefined / predefined times is by the bulk material by means of at least one rotary actuating movement or by means of at least one translatory actuating movement by the high pressure treatment volume is conveyed through, in particular using the pressure vessel device in a previously described method, in particular Use of the pressure container device in a high-pressure treatment arrangement described above, in particular under high pressure at pressures above 40 to 1000 bar. This results in numerous advantages mentioned above. In particular, the material flow can also be optimized with regard to large volume changes / increases in the range of a factor of 10.

Further features and advantages of the invention result from the description of at least one exemplary embodiment with reference to drawings, and from the drawings themselves

1A, 1B each in a schematic representation or in an at least partially sectioned side view, an overview of individual variants of a first, second and third sequence of steps and the devices provided for this, in each case according to one exemplary embodiment;

Fig. 2 in a sectional side view in a schematic representation

High-pressure treatment arrangement according to an embodiment;

3A, 3B, 3C each in a sectional side view in a schematic

Representation of individual embodiments of a

High pressure treatment assembly;

4A, 4B, 4C each in a sectional side view in a schematic

Representation of individual exemplary embodiments of a pressure vessel device of a high-pressure treatment arrangement according to one exemplary embodiment; 5A, 5B, 5C in a sectional side view and in perspective detail views in a schematic representation a further exemplary embodiment of a pressure vessel device of a high-pressure treatment arrangement according to an exemplary embodiment;

6 shows a schematic illustration of individual steps of a method according to a

Embodiment;

Fig. 7A in a schematic representation or in at least partially sectioned

Side view an overview of individual variants of a first, second and third sequence of steps and the devices provided for this in each case according to an embodiment; 7B, 7C, 7D, 7E, 7F, 7G, 7H, 7J, 7K, 7L, 7M, 7N, 70 each in a sectional side view in detail views of individual exemplary embodiments of a pressure vessel device of a high-pressure treatment arrangement;

8A, 8B, 8C, 8D, 8E, 8F each in a sectional side view in successive operating states or process stages

Embodiment of a pressure vessel device

High-pressure treatment arrangement according to an embodiment;

9A, 9B, 9C, 9D, 9E each in a sectional side view in successive operating states or process stages

Embodiment of a pressure vessel device

High-pressure treatment arrangement according to an embodiment;

10 in a sectional side view in successive operating states or process stages an embodiment of a pressure vessel device of a high-pressure treatment arrangement according to an embodiment.

Reference symbols which are not explicitly described with reference to a single figure are referred to the other figures. In the following, the individual exemplary embodiments are first described together for the sake of better clarity, at least with regard to individual partial aspects, in order to then explain a particular feature of specific exemplary embodiments in the further course by reference to individual figures.

1A, 1B show individual variants of a high-pressure treatment arrangement 100 according to the invention. Individual variants of a pressurization device 10, 10a, 10b, 10c, 10d, 10e, 10f are shown for a first step sequence V1. In particular, a pump or a piston can be used as the pressure generating means 11. An inlet fitting 12 can have one or more inlet members, in particular a valve and / or a (cellular wheel) lock. A rotary valve in particular also has the advantage that gas transfer is made more difficult. Furthermore, individual variants of a pressure vessel device 20, 20a, 20b, 20c, 20d, 20e, 20f, 20g (reference to rotary actuating movement) of the high-pressure treatment arrangement 100 are shown for a second sequence of steps V2.

Furthermore, individual variants of a relaxation device 30, 30a, 30b, 30c, 30d of the high-pressure treatment arrangement 100 are shown for a third sequence of steps V3. A plurality of expansion units 31 can be provided, which can be coupled to a respective second sequence of steps V2 via a central or a plurality of decentralized inlet fittings 32. A piston or piston engine 33 can be connected via at least one expansion unit 31 to an outlet fitting 35 for the final discharge of the bulk material.

A control device 101 indicated by way of example for variant 20b is connected to or comprises a logic unit 103. The controller 101 can e.g. also be coupled to sensor units and / or to actuators. The control device can also include the logic unit and be set up to regulate the method steps described here in detail.

The arrangement in columns for the individual devices 10, 20, 30 of the respective step sequence V1, V2, V3 illustrates that the respective variants can be combined with one another. The individual variants for the second step sequence V2 are shown in detail in FIGS. 2 to 5C.

The pressure vessel device 20a shown in FIG. 1A illustrates the use of a rotary actuator in a horizontal orientation; this variant is also described in detail in FIGS.

The pressure vessel device 20b shown in FIG. 1A illustrates the use of a rotary actuator in a vertical orientation; this variant is also described in detail in FIG. 2.

The pressure vessel device 20c shown in FIG. 1A illustrates the use of a rotary actuator in a vertical orientation, the actuator being coupled to a plurality of levels or plates; this variant is also described in detail in FIGS. The pressure vessel device 20d shown in FIG. 1A is distinguished (in contrast to the pressure vessel device according to variant 20c) by an annular gap for supplying or removing extraction medium or extracted solvent; Another annular gap can be provided on the central tube (double tube; tube-in-tube) inside the high-pressure treatment volume, at least one outlet being provided for each high-pressure treatment level, in particular in such a way that the extraction medium in the respective high-pressure treatment level radially (inwards or outwards) outside) can flow through. For the configuration of the pressure vessel device 20d, the keyword “cross flow” can be mentioned: the inner tube and the outer double wall are designed to be fluid-permeable, so that the fluids used flow through the respective bed in the radial direction. The individual high-pressure treatment levels are preferably not made fluid-permeable, but rather fluid-impermeable.

The pressure vessel device 20e shown in FIG. 1B illustrates the use of a rotary actuator in a vertical orientation, the actuator being coupled to a multiplicity of levels or plates, each level being arranged radially spaced from the inner wall of the pressure vessel arrangement by an internal partition. so that an annular gap lying radially outside of the batch is created. The rotation kinematics can be permanently installed together with the levels or can be retrofitted individually for each level.

The pressure container device 20f shown in FIG. 1B shows the use of a rotary conveying device which is supported on the cover of the pressure container device. This variant makes it possible, for example, to adapt the conveying device to the type of bulk material being treated.

The pressure vessel device 20g shown in FIG. 1B illustrates the use of a rotary actuator in an inclination with respect to the horizontal and vertical; Variants of this exemplary embodiment are also described in detail in FIGS. 3.

The continuity of the high-pressure treatment in the variants 20a, 20b, 20e, 20f, 20g according to FIG. 1A, 1B, 2, 3A, 3B, 3C, 4A, 4B, 4C, 5A, 5B, 5C, in particular thanks to the high-pressure level High-pressure treatment volume Vi are ensured in particular in combination with a single, in particular homogeneous, rotary actuating movement (optionally constant rotational speed) for moving the batch against gravity and for gravity-driven discharge from the high-pressure container, or for moving the batches in at least approximately a horizontal direction. If the container is arranged horizontally, the batch can also be optimally stored / relocated with regard to pressure / compression and expansion options. Thanks to the screw conveyor, the fill can also form as a single continuous batch even when material is fed in batches. Optionally, the batch can also be moved in a direction inclined with respect to the horizontal plane. With such an arrangement of the container or the axis of the conveying element, the batch can also be handled in an optimized manner with regard to the removal of solvent (s).

The continuity of the high-pressure treatment can be ensured in the variants 20c, 20d according to FIG. 1A, in particular thanks to the high-pressure treatment volume Vi maintained at the high-pressure level, in particular in combination with rotary actuating movements for gravitationally driven partial batch-wise displacement of partial batches in each case one level down, in each case in response to one individual rotary actuation movement or in response to actuation movements activated individually for each level.

For a better overview, the pressure container device 20 that can be implemented in the second step sequence V2 is described in advance by a general description. The respective pressure vessel device 20 has, in particular, components from the following group: internal partitioning 21, inlet fitting 22, high-pressure-resistant wall 23, heating device, in particular heating jacket 24, outlet fitting 25, inflow / outflow fitting 26, inflow / outflow fitting 27, rotary actuator 28.

2 shows a variant of the high-pressure treatment arrangement 100, in which a rotary actuator 28 (in particular rod / shaft) is coupled in a rotationally fixed manner to a conveyor device 28.1 in the form of a conveyor screw, and the conveyor screw is coupled to a down pipe 25.2 of an outlet fitting 25. This variant also has the advantage that the bulk material can be shifted against gravity in a comparatively well-controlled manner, in particular in the case of comparatively long dwell times, and can also unfold before being discharged, that is to say not in the form of a sealed, packed bed. Last but not least, this also favors an operationally reliable material flow with a minimized risk of material jam or disadvantageously strong mechanical pressure on the bed. The entire conveyor can be inserted into the high-pressure treatment volume and, for example, screwed to the lid of the high-pressure container and / or supported at least laterally on the inner wall 23. Sieve-like inserts can be provided on the inside of the inflow and outflow fittings 26, 27, in particular for retaining bulk material. Optionally, the fitting 26 can also be arranged in the lid of the pressure vessel device.

A material flow of an individual batch through the entire high-pressure treatment volume can be ensured by means of the actuating movement, which is preferably continuous in this exemplary embodiment and which takes place about a single longitudinal axis or actuating axis L. The batch is composed of individual partial batches fed into the high-pressure treatment volume, but is treated and relocated as a single batch within the high-pressure treatment volume.

In the high-pressure treatment volume Vi, which is sealed off from the surroundings U, high-pressure treatment of tea leaves, coffee beans or hops takes place, for example. Extraction medium can circulate via the inflow / outflow fittings 26, 27.

3A, 3B, 3C show in detail a variant of the high-pressure treatment arrangement 100 with an inclined arrangement of the pressure vessel device 20. The inclined arrangement can provide advantages in certain bulk materials with regard to material flow and also with regard to the density of the filling (porosity); In addition, the loading of the bed with extraction medium and the discharge / discharge of extract or solvent can be favored. The inclined arrangement provides advantages, particularly when extracting solvent, with regard to collecting the solvent in order to be able to discharge the solvent in the liquid state at a central outlet.

FIG. 3A also shows an internal bulkhead, in particular a cylindrical bulkhead (fluid-permeable inner wall) 21, which surrounds the rotary actuator 28 and bulkhead the bulk material from an annular cavity. In the ring-shaped cavity Fluids can advantageously be supplied or removed between the partition 21 and the wall 23.

As in the exemplary embodiment described in FIG. 2, the adjusting movement takes place continuously and / or clocked about a single adjusting axis L for the entire high-pressure treatment volume Vi along the entire material flow path.

The energy efficiency can in particular also be optimized by means of an arrangement according to FIG. 3B. The two piston units 33 shown can in particular be aligned with one another with the longitudinal axes in a coaxial arrangement, so that energy recovery and energy use for the other piston unit can be realized when one piston unit is operating.

4A, 4B, 4C show in detail individual variants of the high-pressure treatment arrangement 100 with an at least approximately horizontal arrangement of the pressure container device 20, with a plurality of rotary actuators 28 optionally being provided, in particular in at least approximately parallel alignment with one another, in particular each coupled to a conveyor 28.1 in one embodiment as a screw conveyor. A variant with three actuators 28 is shown in FIG. 4C.

The three variants shown in FIG. 4A differ in that the high-pressure treatment volume Vi can optionally be limited by a partition 21. In other words, the cavity defined and limited by the device as the high-pressure treatment volume Vi is delimited by the bulkhead 21 (which can be permeable in particular to fluids, for example due to perforation or perforation or a wire mesh), and the bulkhead is externally delimited by the high-pressure-resistant wall 23, so that an annular cavity V21 lying further outside of the high-pressure treatment volume is defined, which is kept free of bulk material. The partition 21 is not necessarily resistant to high pressure; in particular, the bulkhead is gas-permeable and a bulkhead that only acts on the bulk material.

In the exemplary embodiment according to FIG. 4A, the rotary actuating movement is preferably designed as an actuating movement that displaces the entire batch, in particular as one continuous adjustment movement, which is specified uniformly for the entire high-pressure treatment volume.

In the exemplary embodiment according to FIGS. 4B, 4C, three rotary actuating movements are provided around an individual actuating axis L, each of which displaces one batch (independently of the other batches) along the entire material flow path in the high-pressure treatment volume, so that despite a plurality of high-pressure-treated batches is not spoken of partial batches. A plurality of batches 3 are arranged in the high-pressure treatment volume Vi, which are shifted individually by means of individual adjusting movements along the respective material flow path (here corresponding to the respective adjusting axis L). In this high-pressure treatment arrangement, the high-pressure treatment volume is divided into several partial volumes by fluid-permeable inner walls 21, in which the high-pressure treatment can be carried out simultaneously. The respective rotary actuating movement can be a continuous and / or at least temporarily actuated movement. The respective rotary actuating movement is specified uniformly along the entire material flow path. In particular, this exemplary embodiment also provides advantages with regard to the most homogeneous possible flow or charging of the bed with solvent.

5A, 5B, 5C show in detail a variant of the high-pressure treatment arrangement 100, in which a rotary actuator 28 (in particular rod / shaft) is coupled to a plurality of treatment levels 5, each treatment level 5 being formed by a pair of plates 29; 29a, 29b is defined, of which one is arranged in a stationary and static manner and the other is rotatably displaceable and is connected in a rotationally fixed manner to the actuator 28. A respective partial batch 3.1, 3.2, 3.n can be shifted between the individual treatment levels 5, in particular driven by gravity in response to a relative rotation of the two plates 29a, 29b of a respective treatment level 5 relative to one another.

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

5A shows in detail the use and arrangement of individual treatment levels 5 in the fixed volume Vi, at least one rotary actuator 28 being provided. 5A shows three different media streams: first media stream M1: bulk material; second media stream M2: high pressure medium or extraction medium, optionally comprising impregnation medium; third media stream M3: extract (in particular discharged solvent stream). The first media flow M1 can also include a supply of solvent present in / on the bulk material, which, however, does not correspond to an explicitly provided material flow or material flow path, but is dependent on the substances or components with which the bulk material is loaded / loaded. The media flows M2, M3 can be single or two-phase.

The material flow can also be explained using the example of FIG. 5A: bulk material 1 is fed in as a single partial batch 2.1. In the high-pressure treatment volume, several bulk batches 3.1, 3.2, 3.n result in bulk batch 3 under high-pressure treatment. The bulk material flow is e.g. through several partial batches 4.1 carried out. At least one sensor unit 105 can be provided, in particular for temperature, pressure, force, displacement, mass and / or flow. The respective sensor unit 105 is in particular also arranged on at least one treatment level 5.

5B, 5C illustrate how the respective treatment level 5 can be set in a partitioning state or in a transmitting state.

5B illustrates a permeable state in which a respective passage segment 29.1 of the upper plate 29a, which is non-rotatably connected to the actuator, is arranged in a rotational position in alignment with a respective passage segment 29.1 of the lower stationary plate 29b. In addition, a respective inclined, in particular conical (or full roof-shaped) segment 29.3 of the upper plate 29a is arranged in alignment with a respective flat segment 29.2 of the lower plate 29b. The respective paired plate arrangement 29a, 29b lets through. The inclined surfaces can perform a function as run-off slopes for the bulk material and also reduce the risk of unwanted local bulk material deposits.

5C illustrates a partitioning state in which a respective inclined, in particular conical segment 29.3 of the upper plate 29a is arranged in alignment with a respective passage segment 29.1 of the lower plate 29b in response to a rotary actuating movement Da (change in the angle of rotation). The respective paired plate arrangement 29a, 29b blocks.

The individual plates 29 are each designed in particular as a circular disk with the recesses (passage openings) already described.

The levels can be actuated individually separately or simultaneously with the rotary actuation movement. The passage openings 29.1 can be arranged in alignment or offset.

In other exemplary embodiments, the plate pair 29 shown in FIG. 5B can also be designed as a pair of two flat plates, each with at least one passage 29.1 for bulk material. The plates are each designed to be fluid permeable.

The respective adjusting movement in the exemplary embodiment shown in FIGS. 5A, 5B, 5C can ensure a material flow of a plurality of partial batches 3.1, 3.n over a section along the material flow path through the high-pressure treatment volume Vi. The rotary actuating movement can be a continuous and / or an at least temporarily actuated 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 in each case be specified specifically for individual predefinable high-pressure treatment levels 5.

An exemplary method sequence is described in FIG. 6.

A first step sequence V1 (pressurization) comprises in particular three different steps:

S1.1 Feeding bulk material as a (partial) batch into a pressurization volume 51.2 Pressure build-up in the pressurization volume, and maintaining the pressure

51.3 Conveying the bulk material into the high-pressure treatment volume

A second step sequence V2 (continuous high-pressure treatment) comprises in particular the following steps:

52.1 Relocating the bulk material in the high-pressure treatment volume

52.2 High pressure treatment by extraction

52.3 High pressure treatment by impregnation

52.4 Discharge of bulk material from the high pressure treatment volume

Moving S2.1 can optionally include one of the following steps:

S2.1a Partial batch conveying of the bulk material in high pressure volume

S2.1 b continuous conveying of the bulk material in high pressure volume

S2.1c Arranging partial batches of the bulk goods on one level

The displacement S2.1 comprises at least one rotary actuating movement, in particular by means of at least one actuator in the form of a rod or shaft (rotary drive means), in particular by means of plates coupled to it in a rotationally fixed manner. In particular, the shifting can be designed individually with regard to the following aspects: a single or multiple positioning axes; Actuating movement for material flow of one or more batches through the entire high-pressure treatment volume or actuating movement for material flow of a plurality of partial batches over a section along the material flow path through the high-pressure treatment volume; continuous and / or at least temporarily clocked actuating movement; uniform actuating movement for the entire high-pressure treatment volume and / or at least temporarily actuating movement that is specified in each case specifically for individual predefinable high-pressure treatment levels.

A third step sequence V3 (relaxation) comprises in particular the following steps:

53.1 Feeding bulk material as a (partial) batch into a relaxation volume

53.2 Pressure reduction in the relaxation volume

53.3 Discharge of bulk material from the expansion volume 7A shows individual variants of a high-pressure treatment arrangement 100 according to the invention. Individual variants of a pressurization device 10, 10a, 10b, 10c, 10d, 10e, 10f are shown for a first sequence of steps V1. In particular, a pump or a piston can be used as the pressure generating means 11. An inlet fitting 12 can have one or more inlet members, in particular a valve and / or a (cellular wheel) lock. A rotary valve in particular also has the advantage that gas transfer is made more difficult.

With reference to translational adjusting movements, the individual variants of the pressure vessel device are designated by the reference numerals 20a, 20b, 20c, 20d, 20e, 20f, 20g, 20h, 20j, 20k, 201, 20m, 20n. With regard to the rotary actuating movements described above, the reference numerals 20a, 20b, 20c, 20d, 20e, 20f, 20g have also been assigned, but denote configurations that can be implemented independently of this and serve only for numbering purposes.

A control device 101 indicated by way of example for variant 20b is connected to or comprises a logic unit 103. The controller 101 can e.g. also be coupled to one or more sensor units and / or to one or more actuators. The control device can also include the logic unit and be set up to regulate the method steps described here in detail.

The arrangement in columns for the individual devices 10, 20, 30 of the respective step sequence V1, V2, V3 illustrates that the respective variants are combined with one another can be. The individual variants for the second sequence of steps V2 are shown in detail in FIGS. 7B, 7C, 7D, 7E, 7F, 7G, 7H, 7J, 7K, 7L, 7M, 7N, 70.

For a better overview, the pressure container device 20 which can be implemented in the second step sequence V2 is described in advance by a general description, in particular with reference to FIG. 70. The respective pressure container device 20 has in particular components from the following group: inlet fitting 22, high pressure-resistant wall 23, heating device , in particular heating jacket 24, outlet fitting 25, inflow / outflow fitting 26, inflow / outflow fitting 27, translational actuator 28.

7B shows two exemplary embodiments in which individual treatment levels can be actuated laterally. Feed-throughs for lateral actuating means (in particular actuating element 28) are provided in the wall of the pressure container device 20b, each specifically for each treatment level. The actuatable lateral actuating means enable kinematics, at least comprehensively, a swivel mechanism, in particular actuated by means of push rods. The actuating means can be coupled directly to the respective plate or indirectly to the respective treatment level by means of a kinematic coupling. 7B shows the principle of lateral actuation in the case of centric or eccentric mounting of plates, with one or more plates which can be pivoted downwards on one side or upwards and downwards on both sides being provided for each treatment level. In addition or as an alternative to the inlet for bulk material on the cover side, an inlet fitting and / or outlet fitting can also be provided laterally at the level of the respective treatment level. The translational adjusting movement can take place, for example, in the radial direction in each plane (bidirectional; back and forth).

7C shows three exemplary embodiments of a pressure container device 20c, in each of which a kinematics with a flap construction that opens from the inside is provided, it being possible to optionally provide drainage slopes and / or edge areas for support structures in the respective treatment level. For each treatment level, at least two plates arranged symmetrically with respect to the central longitudinal axis and transverse web are provided, each pivotable downwards and upwards. The respective plate is mounted eccentrically around a swivel axis and is opened from the center (Swivel down or up). The kinematics can in particular also include coupling joints and / or traction means and / or at least one spring mechanism with a return movement. The translatory adjusting movement takes place in the axial direction.

7D shows two exemplary embodiments of a pressure container device 20d, in which a plurality of treatment levels are provided, each of which is formed by an integral plate. The kinematics for moving the plates is formed in particular by a respective pull / push rod 28 (actuator) (in particular an eccentric arrangement of the push rod (lever linkage), with only one centrally arranged inlet fitting). These exemplary embodiments provide advantages in particular with regard to robustness and simple construction. The plates swivel downwards on one side and optionally upwards. The respective (partial) batch can be fed centrally via the lid. The discharge can be carried out centrally via an outlet fitting on the bottom. The central discharge on the bottom provides e.g. Process-technical advantages, especially with gravity-driven discharge, especially with regard to complete discharge without residues. The translatory adjusting movement takes place in the axial direction.

7E shows an exemplary embodiment of a pressure container device 20e, in which a pivot kinematics is arranged in a pressure container device with lateral inlet fittings. Bulk material can be discharged centrally on the bottom outlet fitting. In this exemplary embodiment, the kinematics can be optimized for pivoting and discharging downwards. The translational actuating movement (actuator 28) takes place in the axial direction.

7F, 7G each show an exemplary embodiment of a pressure container device 20f, 20g with a comparatively narrow, elongated high-pressure treatment volume Vi, in particular provided by a tubular high-pressure container wall. The pistons guided into the high-pressure treatment volume on the end face serve to build up or reduce the pressure, and can also be provided in combination with one-way blocking internals in the manner of a check valve or in combination with unidirectionally blocking flaps. The optimal design of the flaps or shut-off devices can depend on the application or the type of bulk material; for example, semicircular, foldable plate halves can also be provided. Figure 7F describes an assembly with a single cavity for the high pressure treatment volume (no subdivision, no partitioning). 7G describes a multi-stage structure with a plurality of cavities delimited from one another within the high-pressure treatment volume, the cavities being sealed off from one another by the partitioning members 29.

In the exemplary embodiment of a pressure vessel device 20h shown in FIG. 7H, pressure build-up and relaxation units are outsourced, that is, they are not coupled to the high-pressure treatment volume or to the pressure vessel, but are provided upstream or downstream thereof.

The continuity of the high-pressure treatment according to FIGS. 7F, 7G, 7H can in each case be ensured in particular thanks to the high-pressure treatment volume Vi maintained at the high-pressure level, in particular in combination with the pressure-driven partial batch supply and discharge of partial batches of the fill.

7J shows an embodiment of a pressure container device 20j with plates 29 or flaps 29a in a paired arrangement. Both the plates 29 and the flaps 29a are blocking on one side (blocking for bulk goods; however, gas or fluid permeable); the plates 29 are arranged in a stationary manner, and the flaps 29a are rotating, that is to say coupled to the translational actuator 28a, in particular mounted thereon in a swivel joint. In principle, the exemplary embodiment shown in FIG. 7J can be described as a concept of a reciprocating piston pump or a lever pump. Joints or bearings for the fixed plates 29 can in particular be fastened to the container wall or to central webs which are fixedly connected to the container wall; counter-bearings or stops for the flaps 29a which move along can also be fastened there. Both the plates 29 and the flaps 29a open in the conveying direction (to the right in FIG. 7J). The continuity of the high-pressure treatment can be ensured in particular thanks to the high-pressure treatment volume Vi maintained at the high-pressure level, in particular in combination with successive repeated translational positioning movements back and forth between a translatory zero position and a translatory end position, the translational movement in one direction ( 7J to the right) is a lifting movement for conveying the material (actively initiated / activated material flow by means of unidirectional translatory actuating movement), and the bed in partial batches on the individual levels or in the individual compartments defined by the plates in the high-pressure treatment volume Vi is gradually shifted. The kinematics (28, 28b, 29, 29a) used for the one-sided locking mechanism can be described as translational swivel kinematics.

7K shows a top view of an exemplary embodiment of a pressure vessel device 20k, which enables material flow by means of local geometric variations of compartments or sections within the high-pressure treatment volume Vi. Two pistons 29b are attached to the translational actuator 28b and are thus displaced in the high-pressure treatment volume Vi (in the horizontal direction according to FIG. 7K). The pistons 29b act bidirectionally: in a first direction, the respective piston generates a negative pressure difference on the inlet side (negligible compared to the high pressure level or at least not to be assessed as a pressure cycle), so that bulk material is conveyed into the high pressure treatment volume Vi (flap or check valve 29 opens at the Inlet side to high-pressure treatment volume Vi), and in a second opposite actuation direction, the respective piston generates an overpressure on the inlet side, so that bulk material is discharged from high-pressure treatment volume Vi (flap or check valve 29 closes on the inlet side to high-pressure treatment volume Vi). On the outlet side of the high-pressure treatment volume Vi, the same movement of the piston 29a leads to an opposite effect. The piston also seals off two compartments of the high-pressure treatment volume Vi, which are each connected to one another via a line section. The flaps 29 are shifted in the lateral direction according to the arrangement in FIG. 7K (upwards or downwards according to FIG. 7K). The arrangement according to FIG. 7K can be built up in series in several stages. The continuity of the high-pressure treatment can be ensured in particular thanks to the high-pressure treatment volume Vi maintained at the high-pressure level, in particular in combination with successively repeated translational positioning movements back and forth between two translational end positions, the translational movement being a bidirectional stroke movement for conveying the material (bidirectional translational Actuated material flow), and the bulk is shifted in partial batches in the individual sections or compartments in the high-pressure treatment volume Vi. 7L shows an exemplary embodiment of a pressure container device 20I, in which the material flow can take place independently of flaps or valves along the entire high-pressure treatment volume Vi independently of gravitational forces, in particular by means of a conveyor device, in particular a conveyor belt, which is guided horizontally through the high-pressure treatment volume Vi and which has a high-pressure treatment level for arranging the Bulk goods defined. The continuity of the high-pressure treatment can be ensured in particular thanks to the high-pressure treatment volume Vi maintained at the high-pressure level, in particular in combination with a rotary actuating movement (rotary drive for conveyor belt), which is converted into a translatory material flow movement of the entire bed by means of the kinematics of the conveying device. In this variant, too, the material flow in the high-pressure treatment volume Vi can be regulated independently of the supply or discharge of partial batches.

In the exemplary embodiments described above, a temperature control can optionally be carried out to maintain / regulate a constant temperature level. The internals shown in FIGS. 7B to 7E and 7L to 70 within the high-pressure treatment volume can optionally be permanently installed and installed or configured as at least one insert, in particular for mounting on a cover of the pressure vessel device. The design variants shown in FIGS. 7F to 7K can optionally consist of several assemblies, for example connected with high-pressure-tight flange connections, which are assembled one behind the other.

7M shows two exemplary embodiments of a pressure container device 20m, in which the translational kinematics has a centrally arranged lever linkage, by means of which the individual plates (levels) can be pivoted by translation. For each treatment level, e.g. two plates can be provided, in particular in a symmetrical arrangement. The pivoting takes place either without a control lever or by means of a kinematics comprising one control lever per plate half. The plates are shown redundantly in the individual shift / pivot positions in FIG. 7M.

7N shows two exemplary embodiments of a pressure container device 20n, which are characterized by an eccentric arrangement of the respective actuator 28. Each Treatment level is provided a plate which is pivotally mounted eccentrically (eccentrically arranged pivot axis) and is pivotable up and down. Edge areas of each treatment level can be used for support structures. The translatory adjusting movement takes place here in the axial direction.

70 shows three different media flows: first media flow M1: bulk material; second media stream M2: high pressure medium or extraction medium, optionally comprising impregnation medium; third media stream M3: extract (in particular discharged solvent stream). The first media flow M1 can also include a supply of solvent present in / on the bulk material, which, however, does not correspond to an explicitly provided material flow or material flow path, but is dependent on the substances or components with which the bulk material is loaded / loaded. The media flows M2, M3 can be single or two-phase. The third media flow M3 can also be generally understood as an (extracted) loading of the bulk material.

70 also illustrates a first swivel angle α, in particular upwards against the direction of gravity, and a second swivel angle β, in particular downwards in the direction of gravity.

In the exemplary embodiments shown above, the respective treatment level can each be formed by a first and a second part (in particular by two halves), which are each arranged in a pivotable mounting in a stationary or translationally displaceable manner.

8A, 8B, 8C, 8D, 8E, 8F, a cyclic translatory actuating movement to ensure the material flow for continuous high pressure treatment is explained in more detail. 8A shows a process state in which a translational actuator 28 is arranged in a neutral zero position, in particular in the middle between a first stroke position and a second stroke position.

8B shows a process state in which the translational actuator 28 is arranged in the first stroke position, here corresponding to a maximally retracted position. An inlet fitting clears the way to the first partial volume, so that a material flow path can be formed from the first step sequence to the first partial volume of the second step sequence. A (first) partial batch is conveyed into a first partial volume of the high-pressure treatment volume Vi, for example by means of a pump or a piston.

8C shows a process state in which the translational actuator is actuated by being shifted from the first to the second stroke position, a respective stationary flap / plate being simultaneously opened / pivoted by the material flow. The partial batch is conveyed from the first partial volume into a second partial volume by means of the respective translationally displaceable flap / plate (translational displacement).

8D shows a process state in which the actuator has reached the second stroke position, here corresponding to an end position. The partial batch has been completely requested in the second partial volume, so that the first partial volume is empty. From this position the actuator can now be moved back.

FIG. 8E shows the rear translatory stroke movement of the actuator, the displaceable flaps / plates pivoting and the fixed flaps / plates locking. This movement corresponds to the stroke movement in the narrower sense, that is to say the part of the movement cycle in which the stroke is created in order to be able to ensure the material flow in the subsequent part of the movement cycle.

An arrangement corresponding to that of FIG. 8B is shown in FIG. 8F, wherein the first partial volume can be loaded with a further partial batch 2.1. The process sequence described in FIGS. 8A to 8E can be repeated accordingly for a respective partial batch. The arrangement shown in FIGS. 8A, 8B, 8C, 8D, 8E, 8F can also be oriented in a different orientation, in particular also in the opposite vertical direction. Swivel joints or swivel mechanisms can optionally be actuated, for example, by means of drives and / or spring forces, in particular independently of gravitational forces.

The continuity of the high-pressure treatment can be ensured in particular thanks to the high-pressure treatment volume Vi, which is kept at the high-pressure level, in particular in combination with cyclic translatory lifting / actuating movements.

A material flow of a plurality of partial batches can be ensured simultaneously by means of the high-pressure treatment volume by means of the translatory actuating movement, which in the exemplary embodiment in FIG. 8 is preferably designed as a cyclical to-and-fro movement and which takes place along a single longitudinal axis or actuating axis L. . The entire batch is composed of individual partial batches fed into the high-pressure treatment volume in the respective partial volumes.

FIGS. 9A, 9B, 9C, 9D, 9E describe an arrangement that is independent of gravitational forces (in particular horizontal alignment of the longitudinal axis of the pressure vessel device; in particular translational adjusting movement in the horizontal plane), the material flow being comparable to the exemplary embodiment in FIG 8 can be done. In FIGS. 9C, 9D, however, the focus is on the process of removing material from the last partial volume. Starting from FIG. 9B, the partial batch in FIG. 9C is already shown in an arrangement in the last partial volume, the translational actuator being already in the end position (second stroke position). 9D, the actuator is moved back. The stroke of the translatory actuating movement (change in position) can be described by Dc (analogously by Dz in the case of an arrangement according to FIG. 8A).

The arrangement according to FIG. 9A can be described as follows:

the actuator is in the first stroke position;

a plurality of (first) blocking inlet-side levels are in the first lift position;

a plurality of (second) stationary levels on the outlet side are arranged in a blocking manner; The term “on the inlet side” relates to a level which is arranged upstream of a respective partial volume. The term “on the outlet side” relates to a level which is arranged downstream of a respective partial volume.

The arrangement according to FIG. 9B can be described as follows:

the actuator is moved from the first stroke position to the second stroke position in translation in the material flow direction;

a plurality of blocking levels on the inlet side are shifted in the material flow direction, in particular together with the actuator;

a plurality of stationary outlet-side planes are arranged to pass through;

The blocking levels push the material (partial batch) in the material flow direction into the adjacent partial volume, the levels on the outlet side being pivoted in a first direction of rotation.

The arrangement according to FIG. 9C can be described as follows:

the actuator is arranged in the second stroke position;

a plurality of blocking inlet-side levels are arranged blocking;

a plurality of stationary outlet-side planes are arranged to pass through;

The arrangement according to FIG. 9D can be described as follows:

the actuator is shifted from the second stroke position back to the first stroke position translationally against the material flow direction (stroke movement for reloading a further batch);

a plurality of levels on the inlet side are shifted, in a passage arrangement, counter to the material flow direction, in particular together with or by means of the actuator (s);

a plurality of stationary outlet-side planes are arranged in a blocking manner;

The stationary planes are pivoted back in a second direction of rotation, back into a blocking arrangement, and the displaceable planes are displaced back and pivoted in this / the first direction of rotation during this backward movement. The arrangement according to FIG. 9E essentially corresponds to that according to FIG. 8A. Movable and stationary levels are arranged in pairs adjacent to one another, in particular in a blocking arrangement. The material flow between the individual partial volumes can be ensured by two successive, opposite stroke movements (back and forth), in particular regardless of the number of partial volumes arranged in series.

In the first stroke position, the displaceable levels are pivoted back in a second direction of rotation, back into a locking arrangement; either the fixed planes can then be pivoted into a passage arrangement, or at least a pivoting kinematics can be released so that the stationary planes can be freely pivoted and in particular are pivoted into the passage arrangement due to material being displaced, in response to the translational actuating movement.

9A to 9E describe two types of levels, namely fixed levels and displaceable levels. Both types of planes can be arranged either blocking or transmitting, in particular blocking exclusively against the target material flow direction. The blocking or transmitting position of the respective level can be set, for example, using a swivel kinematics. According to one embodiment, the respective level has a plurality of pivotable or tiltable plates. The swivel kinematics can optionally have a drive or can be swiveled without drive around at least one swivel joint.

Note: The further partial volumes between the first and last partial volumes are also loaded with material in the process stages according to FIGS. 9B to 9E, which, however, is not shown for the sake of clarity. FIG. 9B accordingly illustrates four successive translational positioning movements through the four partial volumes, starting from the first partial volume up to the last partial volume.

FIGS. 9 also show a partial batch cavity V21 of the high-pressure treatment volume Vi, the cavity V21 being sealed off in a unidirectional manner. The continuity of the high-pressure treatment can be ensured in the exemplary embodiment in FIGS. 9 in the same way as in the exemplary embodiment in FIGS.

The material flow can also be explained in a more general manner using the example of FIGS. 8, 9: bulk material 1 is fed in as a single partial batch 2.1. In the high-pressure treatment volume, several bulk batches 3.1, 3.2, 3.n result in bulk batch 3 under high-pressure treatment. The bulk material flow is e.g. through several partial batches 4.1 carried out. At least one sensor unit 105 can be provided, in particular for temperature, pressure, force, displacement, mass and / or flow. The respective sensor unit 105 is in particular also arranged on at least one treatment level 5.

8 and 9 illustrate the manner in which the respective treatment level 5 can be set in a partitioning state or in a transmitting state.

10, the concept of the cyclical translational actuating movement is shown again in general, the direction of the actuating movement lying in the horizontal plane only by way of example.

With reference to FIG. 6, the shifting S2.1 can alternatively comprise at least one translational actuating movement, in particular by means of at least one actuating element in the form of a push / pull rod, in particular by means of pivotally coupled plates.

Reference symbol list:

1 bulk or granulate (fill)

2.1 Partial batch fed

3 Bulk batch under high pressure treatment

3.1, 3.2, 3.n Partial bulk goods batch under high pressure treatment

4.1 Partial batch carried out

5 high pressure treatment level

10, 10a, 10b, 10c, 10d, 10e, 10f pressurization device

11 pressure generating means, in particular pump or piston

12 inlet fitting

20, 20a, 20b, 20c, 20d, 20e, 20f, 20g, 20h, 20j, 20k, 20l, 20m, 20n pressure vessel device

21 internal bulkheads, especially cylindrical bulkheads

22 inlet fitting

23 high pressure resistant wall

24 heating device, in particular heating jacket

25 outlet fitting

25.2 downpipe

26 Inlet / outlet fitting, especially with nozzle

27 Inlet / outlet fitting, especially with socket

28 rotary actuator, in particular rod, shaft or tube; or

28 translatory actuator, especially push / pull rod

28.1 Conveying device, in particular screw conveyor 29 Kinematics, in particular swivel kinematics; or

29; 29a, 29b (first and second) plate, bulkhead, in each case at least partially partitioning, optionally rotatable, in particular in the form of a circular disk; or

29; 29a, 29b (first and second) plate, bulkhead, in each case at least partially partitioning, optionally translationally relocatable, in particular in the form of a circular, foldable or pivotable disc

29.1 Passage segment 29.2 flat segment

29.3 inclined, in particular conical segment

30, 30a, 30b, 30c, 30d relaxation device

31 relaxation unit

32 inlet fitting

33 pistons or piston engine

35 outlet fitting

100 high pressure treatment assembly

101 control device

103 logic unit

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

L longitudinal axis or adjusting axis or adjusting shaft for transmitting a torque M1 first media stream: bulk material

M2 second media stream: high pressure medium or extraction medium, optionally comprising impregnation medium

M3 third media stream: solvent

V1 first step: pressurization

51.1 Feeding bulk material as a (partial) batch into a pressurization volume

51.2 Pressure build-up in the pressurization volume, and maintaining the pressure

51.3 Conveying the bulk material into the high-pressure treatment volume

V2 second step sequence: continuous high pressure treatment including extraction and / or impregnation

52.1 Relocating the bulk material in the high-pressure treatment volume

S2.1a Partial batch conveying of the bulk material in high pressure volume

S2.1 b continuous conveying of the bulk material in high pressure volume

S2.1c Arranging partial batches of the bulk goods on one level

52.2 High pressure treatment by extraction 52.3 High pressure treatment by impregnation

52.4 Discharge of bulk material from the high pressure treatment volume

V3 third step sequence: relaxation

S3.1 Feed bulk material as a (partial) batch into a relaxation volume

S3.2 Pressure reduction in the relaxation volume

S3.3 Discharge of bulk material from the expansion volume

U environment

Vi fixed, statically arranged high pressure treatment volume or high pressure sealed cavity for high pressure treatment

V21 cavity defined by partitioning, in particular cylindrical ring cavity; or

V21 partial batch cavity, in particular unidirectionally sealed off; x transverse axis, in particular width direction

y transverse axis, especially depth direction

z vertical axis, especially vertical

Since rotary actuating movement (change in angle of rotation)

Dc, Dz translational positioning movement (change in position)

a first swivel angle, in particular upwards against the direction of gravity ß second swivel angle, in particular downwards in the direction of gravity

Claims

Claims:

1. A method for the high-pressure treatment of bulk material (1) by extraction and / or impregnation, which bulk material is arranged in the high-pressure treatment volume (Vi) of a pressure vessel device (10) and at a high-pressure level, in particular high pressure in the range from 40 to 1000 bar, with isolation from the environment (U) is treated, the method comprising at least the following three individually controllable step sequences:

Pressurization (V1), high pressure treatment (V2), relaxation (V3);

characterized in that the high-pressure treatment in the second step (V2) of the high-pressure treatment step sequence is carried out in a continuous manner at the high-pressure level in the high-pressure treatment volume (Vi), the high-pressure treatment volume (Vi) or the entire pressure vessel device (10) being arranged stationary during the high-pressure treatment (V2) is / remains, the continuity of the high-pressure treatment sequence of steps (V2) being ensured solely by means of the one high-pressure treatment volume (Vi), and the bulk material by means of a rotary positioning movement (Da) or depending on at least one translatory positioning movement during the high-pressure treatment by the high-pressure treatment volume is promoted.

2. The method according to the preceding method claim, wherein in the continuous high-pressure treatment by means of the rotary adjusting movement, a steady displacement speed of the bulk material (1) or a clocking of a discontinuous partial batch transfer, in particular between individual high-pressure treatment levels (5), and thereby the dwell time or the high-pressure treatment time for the bulk material in the high pressure treatment volume (Vi).

3. The method according to any one of the preceding method claims, wherein the bulk material for the high pressure treatment (V2) is arranged on at least one predefined first high pressure treatment level (5) and starting from this first high pressure treatment level continuously or between further high pressure treatment levels in the high pressure treatment volume (Vi) during the High-pressure treatment (V2) is shifted by the rotary control movement and / or in response to the rotary control movement.

4. The method according to any one of the preceding method claims, wherein the continuous flow of high-pressure material is regulated by the bulk material (1) depending on the size and / or a timing of (partial batches continuously or in individual discontinuous partial batches in the high-pressure treatment volume ( Vi) is shifted by the rotary actuating movement; and / or by a continuous displacement of the bulk material (1) or by a discontinuous displacement of the bulk material between individual high-pressure treatment levels (5) during high-pressure treatment by the rotary actuating movement, a residence time of the bulk material is set in the high-pressure treatment volume, in particular by adjusting a speed of rotation of a / the rotary actuator (28) and / or by clocking the rotary actuator; and / or wherein the continuous high-pressure treatment is a continuous displacement of the bulk material in two comprises different predefined material flow directions in the high-pressure treatment volume (Vi), in particular in two opposite material flow directions, namely a material flow direction predefined by the rotary actuating movement and in a second gravitational force-driven material flow direction; and / or wherein the continuous high-pressure treatment comprises a continuous displacement of the bulk material against the force of gravity by supplying potential energy into the bulk material by means of the rotary actuating movement.

5. The method according to any one of the preceding method claims, wherein the continuous high-pressure treatment comprises a continuous displacement of the bulk material by a continuous rotary actuating movement, in particular with the rotary actuator in the form of a screw conveyor; or wherein the continuous high-pressure treatment comprises a discontinuous gravitational force-driven displacement of the bulk material by several discontinuous rotary actuating movements, in particular with the rotary actuator in the form of a shaft with at least one a non-rotatably connected gas-permeable plate with at least one passage segment.

6. The method according to any one of the preceding method claims, wherein the continuous high pressure treatment comprises at least one continuous extraction, in particular solvent extraction; and / or wherein the continuous high-pressure treatment comprises at least one continuous impregnation, in particular the impregnation of polymers; or wherein the continuous high pressure treatment comprises both extracting and impregnating, in particular extracting monomers and impregnating 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 the continuous high pressure treatment comprises flowing high pressure medium through the bulk material, in particular in countercurrent to a continuous displacement of the bulk material.

8. The method according to any one of the preceding method claims, wherein the continuous high-pressure treatment at constant high pressure or in the event of pressure fluctuations is carried out at most in the range from 3 to 5 bar, in particular at high pressure in the range from 500 to 1000 bar.

9. The method according to claim 1, wherein in the continuous high-pressure treatment by the translational actuating movement, a displacement speed or a clocking of a discontinuous partial batch-wise displacement is set, in particular between individual high-pressure treatment levels (5) or between individual partial volumes, the residence time or the high-pressure treatment time for the bulk material thereby High pressure treatment volume is set; and / or wherein the bulk material during the High-pressure treatment in batches is promoted in batches by the high-pressure treatment volume by moving the translational actuator back and forth between a first stroke position and a second stroke position and thereby actuating at least one swivel kinematics for permitting or blocking material flow; and / or wherein the bulk material is conveyed in batches in batches through the high-pressure treatment volume during the high-pressure treatment, in that the translational actuator moves at least two translationally displaceable levels between a first stroke position and a second stroke position; and / or wherein the bulk material is conveyed in batches in batches through the high-pressure treatment volume during the high-pressure treatment, by moving the translational actuator back and forth between a first stroke position and a second stroke position, the respective stroke position being defined in each case by a fixedly arranged high-pressure treatment level ; and / or wherein the bulk material is conveyed in batches in batches through the high-pressure treatment volume during the high-pressure treatment, by moving the translational actuator back and forth between a first stroke position and a second stroke position, the first stroke movement from the first to the second stroke position blocking Stroke movement with a locked swivel kinematics and passing stationary swivel kinematics, and wherein the second stroke movement from the second to the first stroke position is a transmissive stroke movement with a displaceably arranged swivel kinematics and blocking stationary swivel kinematics.

10. The method according to method claim 1 or according to the preceding method claim, wherein the bulk material for the high-pressure treatment (V2) is arranged on at least one predefined first high-pressure treatment level and starting from this first high-pressure treatment level between further high-pressure treatment levels in the high-pressure treatment volume (Vi) during the high-pressure treatment (V2) the respective translatory actuating movement is shifted.

11. The method according to method claim 1 or one of the two preceding method claims, wherein a discontinuous partial batch shifting between individual high-pressure treatment levels during high-pressure treatment by the respective translational actuating movement sets a dwell time of the bulk material in the high-pressure treatment volume, in particular by clocking the respective translatory actuating element, in particular by clocking a plurality of translatory actuators, each as a function of time; and / or wherein the continuous high-pressure treatment comprises a discontinuous partial batch-wise gravitational force-driven displacement of the bulk material, in particular at least approximately in the direction of gravity.

12. The method according to method claim 1 or one of the three preceding method claims, wherein the continuous high-pressure treatment comprises a discontinuous partial batch shifting of the bulk material by a plurality of individual translational positioning movements, in particular back and forth movements, in particular with at least one translatory actuator designed as a push rod with at least one swivel kinematics mounted axially fixed thereon; or wherein the continuous high-pressure treatment comprises a discontinuous, partially batch-wise gravitational force-driven displacement of the bulk material by several discontinuous translatory positioning movements, in particular with at least one translatory positioning element in the form of a push / pull rod with at least one unidirectionally locking pivoting kinematics comprising at least one gas-permeable plate.

13. Control device (31) set up to carry out a method according to one of the preceding method claims, wherein the control device is coupled to at least one sensor unit (35) set up for detecting a flow of bulk material (1) or a mass or a mass difference, the control device optionally also includes at least one sensor unit configured to detect a path and / or a force and / or a pressure, the control device being configured to evaluate and regulate a rotary actuating movement or a translatory actuating movement in each case for specifying the bulk material material flow through a / the high-pressure treatment volume (Vi).

14. High-pressure treatment arrangement (100) set up for high-pressure treatment of bulk material (1) by extraction and / or impregnation at a high-pressure level, in particular high pressure in the range from 40 to 1000 bar, comprising:

a pressurization device with pressure generating means, in particular at least one pump, for pressurization (V1) as a first step sequence;

a pressure vessel device (10) coupled to the pressurization device in a high-pressure-tight connection and having a high-pressure-resistant wall (12) surrounding a high-pressure treatment volume (Vi), for the high-pressure treatment (V2) as a second step sequence;

a relaxation device for relaxation (V3) coupled in a high-pressure-tight connection to the pressure vessel device as a third step sequence;

characterized in that the pressure vessel device is arranged in a stationary manner and is set up for continuous high pressure treatment solely at the high pressure level by means of the one fixedly arranged high pressure treatment volume (Vi), the pressure vessel device having a rotary actuator or translationally displaceable actuator (28) and being set up for a rotary actuating movement or for at least one translatory adjusting movement in each case for the displacement of the bulk material (1) during the high pressure treatment by the

High pressure treatment volume (Vi).

15. High-pressure treatment arrangement according to the preceding device claim, wherein the high-pressure treatment arrangement (100) is set up for supplying individual partial batches (2.1) to the high-pressure treatment volume during the high-pressure treatment and for displacing the partial batches (3.1) in the high-pressure treatment volume during the high-pressure treatment; and / or wherein the high-pressure treatment arrangement (100) is set up to discharge individual partial batches (3.1) from the

High pressure treatment volume during high pressure treatment.

16. High-pressure treatment arrangement according to one of the preceding device claims, wherein the rotary actuator (28) is designed as a screw conveyor, in particular with its longitudinal axis in alignment with the longitudinal axis of the high-pressure treatment volume or parallel thereto; and / or wherein the rotary actuator is designed as a screw conveyor which extends around a down pipe (25.2) for discharging the bulk material; or wherein the rotary actuator is designed as a screw conveyor, which is arranged in a gas-permeable and bulk bulkhead pipe (21); or wherein the rotary actuator is designed as an eccentric screw arranged in the high-pressure treatment volume (Vi); or wherein the rotary actuator is set up to actuate at least one plate (29) with at least one passage segment (29.1), to arrange or to pass bulk material in each case in a high-pressure treatment level (5) defined by the plate.

17. High-pressure treatment arrangement according to one of the preceding

Device claims, wherein in the high-pressure treatment volume (Vi) a plurality of high-pressure treatment levels (5) are defined by gas-permeable plates (29a, 29b) arranged in pairs, one of which is in a rotationally fixed connection with the rotary actuator (28), or each with pivoting kinematics (29) have an axially fixed connection with the respective translatory actuator, in particular with pivoting kinematics which lock on one side; and / or wherein in the high-pressure treatment volume a plurality of high-pressure treatment levels are each defined by at least one gas-permeable plate with bevels and with at least one passage segment, in particular in an aligned alignment in the center of the high-pressure treatment volume.

18. High-pressure treatment arrangement according to one of the preceding

Device claims, wherein the rotationally or translationally displaceable actuator (28) is set up to individually actuate one high-pressure treatment level (5) of the pressure vessel device (20) and / or to simultaneously and synchronously actuate all high-pressure treatment levels of the pressure vessel device.

19. High-pressure treatment arrangement according to device claim 14, wherein the translational actuator can be moved back and forth between a first stroke position and a second stroke position, the first and second stroke positions each being defined by a high-pressure treatment level (5); and / or wherein the translational actuator (28) is kinematically coupled to a blocking and permeable pivoting kinematics; and / or wherein the pressure vessel device has at least one pivoting kinematics (29) which can be arranged in a blocking and permeable manner and which is arranged in a stationary manner in the high pressure treatment volume; and / or wherein the pressure container device has at least a first and at least a second pivot kinematics, which are respectively blocking and transmitting in the same pivot direction; and / or wherein the pressure vessel device has at least one first displaceable pivoting kinematics (29) coupled to the translational actuator (28) and has at least one second pivoting kinematics arranged in a fixed position in the high pressure treatment volume; and / or wherein a / the first and second pivot kinematics of the pressure container device are designed to pivot autonomously without a pivot drive, that is to say pivoting solely in response to translational movement or in response to a force exerted by bulk material; and / or wherein a respective high-pressure treatment level is defined by at least one gas-permeable plate; and / or wherein the pressure vessel device has at least one drive unit and a plurality of actuators (28) in the form of push / pull rods configured for bidirectional translational actuation of the respective high-pressure treatment level (Vi), in particular with the actuators in a linear arrangement next to one another in a transverse plane.

20. Use of a pressure vessel device (20) for the continuous high-pressure treatment of bulk material (1) by extraction and / or impregnation in a closed system which is sealed off from the environment (U) in a high-pressure-tight manner, the high-pressure treatment (V2) being a sequence of steps between pressurization (V1) and relaxation (V3) is carried out and regulated individually, the bulk material in a fixedly arranged high-pressure treatment volume (Vi) in the The pressure container device is continuously shifted or shifted in partial batches (3.1), in particular between individual high-pressure treatment levels (5), at predefinable / predefined times by the bulk material (3) using at least one rotary adjustment movement or depending on at least one translatory adjustment movement through the high-pressure treatment volume ( Vi) is conveyed through, in particular use of the pressure container device in a method according to one of the preceding method claims, in particular use of the pressure container device in a high pressure treatment arrangement (100) according to one of the following device claims, in particular under high pressure at pressures above 40 to 1000 bar; or use of a pressure vessel device (20) for the continuous high-pressure treatment of bulk material (1) in the form of polymers, by extraction and optionally also by impregnation, for supercritical drying to provide the polymers as super-insulators, the high-pressure treatment (V2) being a sequence of steps between one Pressurization (V1) and relaxation (V3) is carried out, the bulk material (3) being treated in a stationary high-pressure treatment volume (Vi) in a continuous manner at the high-pressure level, by the bulk material using at least one rotary actuating movement or depending on at least one translatory actuating movement is promoted through the high-pressure treatment volume, in particular use of the pressure container device in a method according to one of the preceding method claims, in particular use of the pressure container device in a high-pressure treatment arrangement (1 00) according to one of the following device claims, in particular under high pressure at pressures above 40 to 1000 bar.

21. Use of a pressure vessel device (20) for the continuous high-pressure treatment of bulk material (1) in the form of aerogels, by extraction and / or by impregnation in a closed system which is sealed off from the surroundings (U) in a highly pressure-tight manner, the continuous high-pressure treatment (V2) being Sequence of steps between pressurization (V1) and relaxation (V3) is carried out, the bulk material (1, 3) being arranged in a stationary manner High-pressure treatment volume (Vi) is treated in a continuous manner at the high-pressure level, the bulk material being shifted continuously in the pressure vessel device or in partial batches (3.1), in particular between individual high-pressure treatment levels (5), being shifted at predefinable / predefined times by the bulk material (3 ) is conveyed through the high-pressure treatment volume (Vi) by means of at least one rotary adjusting movement or by means of at least one translatory adjusting movement, in particular using the pressure container device (20) in a method according to one of the preceding method claims, in particular using the pressure container device (20) in a high-pressure treatment arrangement (100 ) according to one of the preceding device claims, in particular under high pressure at pressures above 40 to 1000 bar.