EP3897899A2

EP3897899A2 - Device and method for the continuous high-pressure treatment of bulk material and use thereof

Info

Publication number: EP3897899A2
Application number: EP19831718.2A
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: EP3727626A1; DE102018222883A1; US20220072447A1; KR102556664B1; CN111757772B; KR102369887B1; WO2020127889A4; WO2020127889A2; US20220062788A1; US11980832B2; DE102018222881A1; KR102592507B1; WO2020127957A4; WO2020127957A2; DE102018222874A1; US20200324223A1; KR20200097340A; CN111757772A; WO2020127957A3; WO2020127889A3

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 vessel device (20) and 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 (V3); 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 vessel 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). This enables, in particular, a process optimisation of high-pressure treatment processes, 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 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 for 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 known 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 production of various intermediate and end-user products, especially from the food industry the number of variants of extraction processes is also comparatively high. This is also reflected in the structure and 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, also referred to as a product receiving basket, is usually used to arrange the bulk material, for example with a volume of approx. 250 liters and with a cylindrical jacket wall, with a gas-permeable, wire mesh-like, perforated plate-like or sintered metal filter base on which the insert is in the extractor is supported. 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. Is the bulk goods dangerous goods or become If 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 in the introduction, which simplifies the high-pressure treatment of bulk material or that associated with the high-pressure treatment device or process engineering effort can be reduced, especially with the highest possible efficiency of the method (throughput per unit of time). In particular, operational and / or occupational safety should also be increased. 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 more 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 / being arranged in a stationary (static) manner during the high-pressure treatment, and wherein 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. 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 materials that can vary greatly in volume, in particular with Volume increases in the range of factor 10, for example especially during drying.

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 adjustable, especially independent of material flow and high pressure conditions in the second step sequence. The discontinuous procedure can also include pressurization and expansion 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 V2.

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 also be adjusted 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 optionally continuously unchanged without a time interruption and (at least theoretically) without a time Restriction and (at least theoretically) without restriction with regard to the amount (mass, volume) of the bulk material treated, in particular also with a continuous flow of material 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 / arbitrary point in 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 be either 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 volume are driven, especially in connection with the supply and / or discharge of material.

A fixed 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 fixedly arranged, i.e. without having to assume a function with regard to bulk material displacement by shifting the high-pressure treatment volume . In any case, it is not necessary to shift the high-pressure treatment volume relative to the other components of the arrangement. No material flow function has to be performed by means of the high-pressure treatment volume. In other words, the high-pressure treatment volume does not have to be moved according to the invention (neither absolutely nor relatively) in order to be able to ensure the continuity of the method. Rather, the bulk material can be supplied to the high-pressure treatment volume and discharged again without having to interrupt the high-pressure treatment. Actuating movements can be carried out optionally within the high-pressure treatment volume, in particular to define a specific type of material flow, but the high-pressure treatment volume can remain stationary. Last but not least, this facilitates the coupling 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 partial 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 also be described as a high-pressure treatment cavity enclosed in a high-pressure-tight manner by the pressure container device. 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 with material flow and high pressure medium in counterflow 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 goods 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 loading, type of extraction medium, 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 been built up, the first sequence of steps V1 can essentially only be provided to provide a respective batch of bulk goods for the pressure vessel 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. The respective container can be locked for this.

A comparatively long expansion line can be provided in the third step sequence V3, in particular immediately downstream of the second step sequence 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.

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.

According to one exemplary embodiment, all three step sequences V1, V2, V3 can be implemented by means of a pipe or a pipe coil, the corresponding section of the pipe in the third step sequence V3 being able to be designed as a relaxation line. An advantage here is a largely arbitrary scalability (in particular extension of the tube length), or a comparatively large variability with regard to additional assemblies. A backflow of the bulk material can advantageously be prevented in a simple manner. A high degree of filling can advantageously be made possible. In other words, the available volume can be used efficiently. io

The bulk material can remain stationary in the high-pressure treatment volume until further bulk material is entered via the first step sequence V1.

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 granules can be introduced into the high-pressure container at extraction pressure and can be removed again after a defined time without having to change the high-pressure treatment level. Here, e.g. extraction medium can also be continuously conveyed through the high-pressure container.

In contrast to this, in the case of a discontinuous (partially) batch-wise process management (batch operation), 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) batchwise process, 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. The process pressure prevails at all times in the second volume, so that high-pressure treatment can take place in the second volume. The treated bulk material (granulate) is then conveyed into a third volume in which the relaxation can take place. Exemplary embodiments according to the invention are described below.

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 have the following components:

Pump set up to apply high pressure to the granulate in the first step sequence V1;

Pressurization device with at least one 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 element and optionally also inlet / outlet valve, in particular in each case comprising a connecting piece (connection); the outlet member can be 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 material is fed under high pressure into the pressure vessel device, in particular directed to the lower end of a conveyor. Optionally, a / the conveying device conveys the bulk material in the high-pressure treatment volume, in particular 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 being discharged from the high-pressure treatment volume, the bulk material is directed into one of several expansion tanks. These are shut off with a valve, after which the relaxation can take place.

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

horizontal or slightly inclined pressure vessel device with extractor;

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.

The conveying device is in particular arranged within a tube made of perforated sheet metal or wire mesh, which is permeable to fluids, but acts as a partition for the bulk material. Another exemplary mode of operation: The bulk material is brought to pressure as already described and introduced into the extractor at the corresponding nozzle. In a predefinable unit of time, the bulk material is conveyed through the extractor by means of the conveying device, while at the same time C0 _{2 is passed} through the extractor, for the extraction of the solvent from the bulk material. Liquid solvent can pass through a fluid-permeable wall and be collected and discharged at an exit point (outlet), in particular in the bottom of the extractor. The bulk material falls into an outlet nozzle at one end of the extractor. The relaxation can be carried out as in the variant described above.

Alternatively, a piston engine with the reverse function of the pump can be used for the expansion. This 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 which is set up to extract energy from the high-pressure medium via mechanical work during relaxation, in particular by means of pistons or turbines driven by the high-pressure medium.

For example, in the third sequence of steps V3, relaxation can take place 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 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. A further exemplary embodiment (in particular a third variant) can have the following components as a modification or in addition to the two variants described above: pressure vessel device in the form of a pipe or pipe coil;

The second sequence of steps V2 can in particular be implemented in series with the first and third sequence of steps V1, V3, the first and / or third sequence of steps V1, V3 also being able to be at least partially integrated into the tube.

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 is introduced at one nozzle and leaves the pipe 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 pipe can be / are subdivided into different areas with externally operable / unlockable check valves, in particular in order to be able to ensure regulated conveyance of the bulk material through the pipe.

Advantageously, the pressure container device can be heavily used in the respective mode of operation, in particular in terms of space to almost 100% with respect to the available high-pressure treatment volume, and in particular also to 100% in terms of time. Pressure build-up or relaxation phases are not necessary. Compared to a discontinuous process, only a fraction of the load changes are required. Ultimately, there are also economic advantages, in particular thanks to the high throughput of bulk material. 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 for the fluidized bed (in particular in the form of a displaceable or pivotable flap level or as a rotatable or rotating plate level) is provided, in particular at a lower end of the pressure vessel device. The fluidized bed can be sealed off on both sides by one of several high-pressure treatment levels. The 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 bulk materials being treated. 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. By maintaining the one (only) high pressure level, the continuous process is also more exact, because without the requirement of Pressure fluctuations can be adjusted in the most exact way possible, in particular via the dwell time, the effect of the high-pressure treatment on the bulk material, in particular as a function of a single predefined / predefinable pressure level.

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 pressure provided on the output side by the first sequence of steps is preferably 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 embodiment, in the first step sequence of pressurization, the (partial) batch-wise adjustable bulk material flow quantity, in particular the size of the respective (partial) batch and / or a timing of the (partial) batch, is shown 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, in the third sequence of steps, the batch-wise bulk material flow quantity, in particular the size of the respective (partial) batch and / or a timing of the (partial) batches, is shown as a function of the bulk material material flow or the high pressure level in the high pressure treatment - Sequence of steps 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 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 embodiment, the bulk material flow is regulated in continuous high-pressure treatment, in that the bulk material is shifted 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 (ie from High-pressure treatment level to high-pressure treatment level) in the high-pressure treatment volume during high-pressure treatment V2. 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 exemplary 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 or by clocking translatory actuators or gravitational gears . 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 exemplary embodiment, the continuous high-pressure treatment comprises 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. 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 discharge of the material can optionally take place at the same end of the pressure vessel device, e.g. on the ground.

According to one exemplary embodiment, the continuous high-pressure treatment comprises a continuous displacement of the bulk material against gravity (or Gravitational force) by supplying potential energy into the bulk material. 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 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 a rotation, in particular by a rotation of at least one rotary actuator 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 goods in batches by means of a rotation, in particular by means of at least one rotary actuating element, which is timed in time. 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.

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 translation of at least one translatory actuator. In this way, the material flow can also be decoupled from gravity.

According to one exemplary embodiment, the continuous high-pressure treatment comprises an autonomous, gravitational force-driven continuous displacement of the bulk material without rotary or translational actuators. In particular, this also provides a lean device-related structure, the material flow being able to take place at least in sections in an autonomous manner.

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 output-side area 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 a turbulent flow behavior and an associated turbulent whirling up 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 vortices).

According to one exemplary embodiment, the continuous high-pressure treatment comprises discontinuous displacement of the bulk material in individually relocated / 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, which is arranged horizontally or inclined relative to the horizontal. 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 arranged in an inclined orientation and / or optionally pivotable and / or translationally or rotatably displaceable.

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. 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 material flow can also be pressure-driven at least in sections, that is, on the basis of a differential pressure (pressure promotion, in particular based on the high pressure already provided in the first step sequence V1). Suction conveyance can also be provided. In the case of suction conveying, the conveying element is at the end of the conveying path to be bridged; this arrangement is useful, for example, in the third sequence of steps. The high-pressure treated product / raffinate / bulk material can also be conveyed from a pressureless container by suction, downstream of the relaxation that has already taken place. In the third sequence of steps V3, a vacuum (negative pressure) can optionally also be drawn in order to increase the pressure difference for the delivery.

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 seat and cone fitting, a ball valve and / or a flap.

According to one exemplary embodiment, the expansion sequence comprises a partial batch discharge of bulk material, the partial batch discharge using an outlet fitting with at least one outlet member, in particular a valve and / or lock (pressure lock, cellular wheel lock) is carried out. 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, the inlet and / or outlet fittings are activated in at least one of the step sequences of pressurization and expansion, in particular as a function of gravimetric measured values of bulk material partial batches recorded in real time. This favors further optimization measures, especially with regard to material flow.

The following are advantageous refinements of the sequence of steps

High pressure treatment V2 explained.

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. Both liquids (fluids in the liquid phase, in particular also viscous fluids) and solids can be subjected to extraction as starting materials. The following can be mentioned as examples of high-pressure-treated bulk goods: granules (in particular polymer granules), airgel bodies, pellets, powder, beans, particles and / or other free-flowing accumulations of a large number of bodies.

According to one exemplary embodiment, the continuous high-pressure treatment comprises flowing high-pressure medium through the bulk material, in particular in countercurrent to a continuous or discontinuous displacement (or displacement direction / material flow direction) 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 desired 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 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.

The above-mentioned object is also achieved according to the invention by a control device set up to carry out a previously described method, the control device set up being coupled to at least one sensor unit 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 the 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. This results in the aforementioned advantages.

The control device or the sensor unit can be coupled to an actuator of the pressure vessel device. 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 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 stationary 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. 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. In this way, the material flow can also be set or regulated in a flexible manner. In the high-pressure treatment volume, at least one predefined first high-pressure treatment level or optionally also more

High-pressure treatment levels can be provided, each set up for arrangement of 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 individually controllable, 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 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 Step sequence high pressure treatment. 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 embodiment, the pressure vessel device defines an at least approximately vertically oriented material flow direction. 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 horizontal, in particular at an angle of 10 to 30 °. In this way, advantages in terms of mass transport and / or in terms of mixing the bed can also be realized.

According to one embodiment, the pressure vessel device defines an at least approximately horizontally oriented material flow direction. This enables e.g. also the use of non-return valves as barriers, especially 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. In the case of an inclined arrangement of several plates, the plates can be arranged in a cascade-like manner offset from one another. 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, the pressure vessel device has at least one actuator designed for actuating at least one high-pressure treatment level of the pressure vessel device, in particular an actuator that can be displaced in rotation or a actuator that can be displaced in translation, in particular at least one actuator that is coupled in from the environment into the high-pressure treatment volume in a pressure-tight manner. In this way, partial batches in the high-pressure treatment volume can also be individually shifted.

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.

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 shifted in partial batches between individual high-pressure treatment levels at predefinable / predefined times, in particular using the pressure vessel device in a previously described method, in particular using the pressure vessel device in a previously described

High-pressure treatment arrangement, in particular under high pressure at pressures above 40 to 1000bar. 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 particular using the pressure container 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 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 aerogels, by extraction and / or by impregnation, the continuous high-pressure treatment V2 being carried out as a sequence of steps between pressurization V1 and relaxation V3, the Bulk material is treated in a fixedly arranged high-pressure treatment volume Vi in a continuous manner at the high-pressure level, in particular using the pressure vessel device in a previously described method, in particular using the pressure vessel 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. 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

Fig. 1 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;

2A, 2B, 2C, 2D, 2E, 2F, 2G, 2H, 2J, 2K, 2L each in section

Side view of individual exemplary embodiments for devices set up for the second sequence of steps, in each case according to one exemplary embodiment;

3A, 3B each show a further variant of a sectional side view

Embodiment for a device set up for the second sequence of steps;

4A, 4B, 4C, 4D each in a sectional side view another

Variant of an embodiment for a device set up for the second sequence of steps;

5 shows a schematic illustration of individual steps of a method according to one embodiment;

6A, 6B, 6C, 6D, 6E, 6F each in a sectional side view individual

Embodiments for devices set up for the first

Step sequence, in each case according to an embodiment; and FIGS. 7A, 7B, 7C, 7D each in a sectional side view individual

Embodiments for devices set up for the third

Step sequence, in each case 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 exemplary embodiments are first described together for the sake of clarity, in order to then explain a particular feature of specific exemplary embodiments in the further course by reference to individual figures. 1 shows a high-pressure treatment arrangement 100. For a first sequence of steps V1, individual variants of a pressurization device 10, 10a, 10b, 10c, 10d, 10e, 10f are shown. 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 12.1, 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.

One or more pressure vessel devices according to variants 20, 20a, 20b, 20c, 20d, 20e, 20f, 20g, 20h, 20j, 20k, 20l can be used for the second sequence of steps.

Furthermore, individual variants of a relaxation device 30, 30a, 30b, 30c, 30d are shown for a third step sequence V3. A plurality of expansion units 31, 31a, 31b can be provided, which are coupled to a / the 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 to an outlet fitting 35 for the final discharge of the bulk material.

A control device 101 indicated by way of example for the variant 20c is connected to a logic unit 103 or comprises this. 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 sequence of steps V2 are shown in FIGS. 1 and 2 to 4. 2A, 2B, 2C, 2D, 2E, 2F, 2G, 2H, 2J, 2K, 2L show in detail the use and arrangement of individual treatment levels 5 in the fixed volume Vi, with optional rotary or translational actuators 28, 28a, 28b can be used.

For a better overview, the respective pressure vessel device is described in advance by a general description. The respective pressure vessel device 20 has components from the following group:

cylindrical inner wall 21, inlet fitting 22, inlet member 22.1, high pressure-resistant wall 23, heating device, in particular heating jacket 24, outlet fitting 25, outlet member / outlet connection 25.1, inlet / outlet fitting 26, inlet / outlet fitting 27, actuator 28, rotary actuator 28a, translatory actuator 28b .

FIG. 2A shows an exemplary embodiment (pressure vessel device 20a) with planes 5 arranged at an angle of inclination with respect to the horizontal and with respect to the vertical, which are each defined by a plate. The bulk material can flow gravitationally from one level to the next. The levels are arranged opposite one another with opposite inclinations and are alternately supported on opposite container inner surfaces. The free ends of the plates in the respective planes 5 are arranged to overlap in the radial direction, so that a simple meandering or serpentine material flow path can be forced onto the bulk material by means of simple measures.

2A 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 the bulk goods is loaded / loaded. The media flows M2, M3 can be single or two-phase.

The material flow can be explained using the example of FIG. 2A: 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 below

High pressure treatment. The bulk material flow is e.g. through several partial batches 4.1 carried out. 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 autonomous, gravitational force-driven material flow over the individual levels 5 or from level to level. The material flow is (ideally) continuous. The entire fill is (ideally) a coherent fill (a single batch; no partial batches), which is shifted across the levels to the outlet at the bottom of the container.

2B shows an exemplary embodiment (pressure vessel device 20b) with a multiplicity of treatment levels 5, in / on which a delimiting plate is arranged in each case over a circumferential angle of in particular approximately 300 °, with a passage over a circumferential angle of in particular approximately 60 °. When rotating, the passage can be positioned in a relative position, thereby releasing a gravitational material flow (downwards). 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 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 the rotary actuating movement.

According to a first variant (FIG. 2B), a wheel can be rotated with free spaces between separating plates. The respective plate, which contains the circular segment cutout (passage) over 60 ° and is otherwise fluid-permeable, but retains the bulk material, is / remains stationary in this variant. According to a further embodiment variant, the plates with the passages are rotatably mounted and the wheels or separating plates are provided as fixed internals.

The rotary actuating movement can optionally be specified centrally via a shaft or via the respective high-pressure treatment level.

In other exemplary embodiments, the plate 29 shown in FIG. 2B can also be designed as a continuous bulkhead, or the plate can be arranged optionally in an inclined orientation and / or optionally pivotably and / or translationally displaceable. 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 arranged in particular on a treatment level 5.

2C shows an exemplary embodiment (pressure container device 20c) in which the bulk material flow takes place from bottom to top against gravity. A screw conveyor conveys the bulk material during rotation up to an essentially vertically oriented downpipe, through which the bulk material can be conveyed downwards by gravity and discharged from the container. 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 single, in particular homogeneous, rotary actuating movement (optionally constant rotational speed) for shifting the batches against gravity and for gravitationally discharging them from the high-pressure container.

2D shows an exemplary embodiment (pressure container device 20d) with a screw conveyor with its longitudinal axis / axis of rotation in a horizontal orientation. The screw conveyor is provided with respect to the radial direction in the entire high-pressure treatment volume Vi and is geometrically designed to correspond to the inner surface of the wall 23. 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 single, in particular homogeneous, rotary one Adjustment movement (optional constant speed of rotation) for moving the batches in at least approximately horizontal direction. With this arrangement of the container, the batch can also be optimally stored / relocated with regard to pressure / compression and expansion possibilities. Even when material is fed in batches, the bed can be formed as a single coherent batch thanks to the screw conveyor (as in the variant according to FIGS. 2C, 2E).

FIG. 2E shows a variant (pressure vessel device 20e) of the exemplary embodiment according to FIG. 2D, the longitudinal axis being arranged at an angle of approximately 25 to 35 ° with respect to the horizontal plane, and the radial diameter of the screw conveyor being smaller than the diameter of the High pressure treatment volume. A cylindrical insert 21 forms an annular gap with the inner lateral surface of the wall 23, through which in particular solvent can be removed. The cylindrical fluid-permeable inner wall 21 surrounds the rotary actuator 28a and seals off the bulk material from an annular cavity. Fluids can advantageously be supplied or removed in the annular cavity between the inner wall 21 and the wall 23. 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 single, in particular homogeneous, rotary actuating movement (optionally constant rotational speed) for displacing the batches in a direction inclined with respect to the horizontal plane. With this arrangement of the container or the axis of the screw conveyor, the batch can also be handled in an optimized manner with regard to the removal of solvent (s).

2F, 2G each show an exemplary embodiment (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. According to one variant, 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 check valves are permeable to fluid (especially with blocking elements in Design as perforated sheet / wire mesh). Optionally, the internals can also be provided as conveying elements which are loaded when high pressure is already present.

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. FIG. 2F describes a structure with a single cavity for the high-pressure treatment volume (no division, no partitioning). 2G 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 shown in FIG. 2H (pressure vessel device 20h), 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. 2F, 2G, 2H can be ensured in each case 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.

2J shows an exemplary embodiment (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; 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. 2J can be described as a concept of a reciprocating piston pump or a lever pump. The flaps are each permeable to fluid (in particular with blocking elements in the form of a perforated plate / wire mesh). Joints or bearings for the fixed plates 29 can in particular be attached to the container wall; there can also be counter bearings or stops for the moving flaps 29a be attached. Fixed webs can also be provided in the center, in particular in order to provide a plate in an articulated manner thereon. Both the plates 29 and the flaps 29a open in the conveying direction (to the right in FIG. 2J). 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 ( 2J to the right) is a lifting movement to convey the material (actively initiated / activated material flow through unidirectional translational actuating movement), and the filling in partial batches on the individual levels or in the individual compartments defined in the plates in the high-pressure treatment volume Vi is gradual is shifted. The kinematics (28, 28b, 29, 29a) used for the one-sided locking mechanism can be described as translational swivel kinematics.

2K shows a top view of an exemplary embodiment (pressure container 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. 2K). 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 evaluated 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 two compartments of the High-pressure treatment volume Vi from each other, which are each connected via a line section. The flaps 29 are moved in the lateral direction according to the arrangement in FIG. 2K (upwards or downwards according to FIG. 2K). The arrangement according to FIG. 2K can also be constructed in several stages in a row. 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.

2L shows an exemplary embodiment (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 arrangement of 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. 2A to 2L 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. 3A, 3B show two exemplary embodiments based on FIG. 2F, in which the material flow on the inlet and outlet sides of the high-pressure treatment volume Vi is brought about by means of a translatory piston mechanism. According to FIG. 3A, the high-pressure treatment volume can be provided, for example, by a cylindrical or tubular pressure vessel device. 3B shows an exemplary embodiment with the pressure vessel in the form of a line with two valves 29, each of which can be flowed through to the right. The first (on the left) check valve 29 comprises a check function, and the second (on the right) valve 29 is designed without a check function. The material flow is brought about by means of two pistons or piston motors 33, the pistons acting bidirectionally, on the one hand reducing pressure (pressure drop), on the other hand pushing / increasing pressure (pressure build-up). The second valve is connected to the piston engine 33 via a control loop (dashed line). The continuity of the high pressure treatment can be ensured in particular in the manner described in connection with FIGS. 2F, 2G, 2H.

4A, 4B, 4C, 4D show exemplary embodiments which are related to the exemplary embodiment of FIG. 2F. A first check valve 29 arranged on the inlet side opens to the right in the material flow direction and blocks to the left, and a second check valve 29 arranged on the outlet side opens to the left against the material flow direction and blocks to the right. The high-pressure container 20, which is of tubular design in geometry, has an outlet on the base, in particular for solvents. The continuity of the high pressure treatment can be ensured in particular in the manner described in connection with FIGS. 2F, 2G, 2H.

4A to 4C show the same embodiment. 4A shows an operating state in which bulk material is discharged from the high-pressure treatment volume (first check valve 29 on the left in the closed position; second check valve 29 on the right in the open position).

4B shows an operating state in which the high-pressure treatment volume is sealed off on both sides (first and second check valve in the closed position). Position). An extraction of solvent (s) takes place, for example, in the high-pressure treatment volume Vi which is sealed off from the environment U.

4C shows an operating state in which bulk material is introduced into the high-pressure treatment volume (first check valve 29 on the left in the open position as soon as there is pressure equalization or as soon as there is slight overpressure; second check valve 29 on the right in the closed position).

In the exemplary embodiment shown in FIG. 4D, a plurality of compartments (here: three compartments) are provided in the high-pressure treatment volume Vi, which are each arranged in a row with respect to one another and are sealed off from one another by means of check valves 29 that open on one side; these check valves can be coupled to one another, in particular by means of a piston rod, so that all check valves 29 on the outlet side can be actuated together by means of a translational adjusting movement. The majority of compartments favor the most precise possible control or regulation of the manner in which the bed flows and the dwell time (contact time). Optionally, e.g. only two or four or even more compartments / stages may be provided.

4A, 4B, 4C, 4D, the hatching density schematically illustrates the level of the high pressure level.

5 illustrates individual steps of a method according to the invention, in particular in an exemplary method sequence. A first sequence of steps V1 (pressurization) comprises, in particular, three steps which can be delimited or regulated individually:

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

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

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

6A, 6B, 6C, 6D, 6E, 6F show individual variants for steps of the first step sequence V1. 6A shows a piston 33, optionally in the form of a pressure build-up element (in particular a pump) and / or as a delivery element. Other pump designs can be used.

6B shows a plurality of pistons 33, which are coupled together to a line leading to the second sequence of steps V2.

6C shows a screw conveyor with a rotary actuator for providing a continuous material flow for the second step sequence V2.

6D shows a plurality of screw conveyors, each with a rotary actuator, which are coupled together to a line leading to the second sequence of steps V2.

6E shows a structure with a single pressurizing unit 11a.

6F illustrates a variant by means of which advantages with regard to the simplified implementation of continuity of the method can be ensured. Thanks to single or multiple redundancy of the pressurizing units 11a, 11b, the pressure can be built up in parallel with a time offset.

Comparable to the first step sequence V1, this concept can also be used for the third step sequences V3, that is to say for the arrangement and connection of relaxation units 31a, 31b. The relaxation can also take place in parallel with a time offset. First the bulk goods are discharged from the High-pressure volume in individual of the expansion units 31, and after expansion, the partial flows are brought together again to form a single material flow. The supply to the individual relaxation units 31 can be regulated individually.

7A, 7B, 7C, 7D show individual variants for the third sequence of steps V3. FIG. 7A shows a variant of the exemplary embodiment according to FIG. 6F. The bulk material is discharged from the high-pressure volume into the redundant expansion units 31, 31a, 31b, in particular alternately or one after the other, and after expansion each partial flow is continued individually. The relaxation units 31 can not only be arranged parallel to one another, but also at least partially in series. Thanks to redundancy, at least one relaxation unit 31 can be made available at any point in the process.

7B shows an exemplary embodiment with a piston / piston motor 33 and a relaxation unit 31 coupled to it, the piston motor 33 being used as an organ for regulating a volumetric material flow by driving the piston by means of excess pressure. The piston engine is in particular set up to adjust the material throughput. The piston engine also enables energy to be recovered from mechanical work.

7C, 7D each illustrate a further exemplary embodiment, in which the assumption can be made that the bulk material can be conveyed solely on the basis of a pressure gradient forming along a comparatively long (relaxation) line 34, with relaxation simultaneously over the corresponding run length is provided. The material flow path created over a predefinable run length is set up to perform the function of a throttle. It has been shown that a single continuous long line (pipe) 34 can optionally be used for the pressure reduction, the pressure difference arising in the pipe over a predefinable unit of length being used as the driving force for the material flow, in particular exclusively, that is to say independently from any other funding agencies. At least one control element can optionally be provided along the material flow path.

A variant with temperature control is shown in FIG. 7D, in particular in order to be able to compensate for a cooling that occurs during relaxation by supplying thermal energy (heating) along line 34. The line 34 can be arranged in sections or completely in a heat bath or in a heat supply unit which is sealed off from the surroundings. The process illustrated in FIGS. 7C, 7D as a continuous relaxation and transport process can also be understood synonymously as a large number of minimally small relaxation steps.

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

11a, 11b pressurizing unit

11 pressure generating means, in particular pump or piston

12 inlet fitting

12.1 Inlet element, in particular valve and / or lock

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

21 cylindrical inner wall

22 inlet fitting

22.1 Inlet element, in particular inlet socket

23 high pressure resistant wall

24 heating device, in particular heating jacket

25 outlet fitting

25.1 outlet element, in particular outlet nozzle

26 inflow / outflow fitting, in particular nozzle

27 Inlet / outlet fitting, in particular nozzle

28 actuator

28a rotary actuator

28b translational actuator

29 plate, bulkhead, flap, organ, each at least partially partitioning, optionally in an inclined orientation, pivotable and / or relocatable

29a moving flap

29b pistons

30, 30a, 30b, 30c, 30d relaxation device 31, 31a, 31b relaxation unit

32 inlet fitting

33 pistons or piston engine or piston pump

34 relaxation line

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

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

51.3 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

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

53.2 Pressure reduction in the relaxation volume S3.3 Discharge of bulk material from the expansion volume

U environment

Vi high pressure treatment volume or cavity sealed for high pressure tightness for high pressure treatment

V1 first step sequence

V2 second sequence of steps

V3 third sequence of steps

Claims

1. A method for 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 (20) and is treated at a high-pressure level, in particular high pressure in the range from 40 to 1000 bar, the method includes at least the following three individually adjustable sequences:

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

characterized in that the high-pressure treatment (V2) is carried out in a continuous manner in the high-pressure treatment volume (Vi), the high-pressure treatment volume (Vi) or the entire pressure vessel device (20) being arranged in a stationary manner during the high-pressure treatment (V2), and the continuity of the high-pressure treatment (V2 ) is ensured solely by means of the one high-pressure treatment volume (Vi).

2. The method according to the preceding method claim, wherein individual bulk batches (2.1, 3.1) generated in the first step sequence (V1) are fed to the high-pressure treatment volume (Vi) during the high-pressure treatment (V2), the partial batches being one / the batch (3) under continuous high pressure treatment; and / or wherein individual partial batches (3.1, 4.1) are discharged from the high-pressure treatment volume (Vi) during the high-pressure treatment.

3. The method according to any one of the preceding method claims, wherein a respective bulk material batch (2.1, 3.1) provided by the pressurization (V1) is smaller in volume or mass than one / the batch (3) under continuous high-pressure treatment, in particular by the Factor 3 to 1000 smaller.

4. The method according to any one of the preceding method claims, wherein in the continuous high pressure treatment by regulating a constant speed of displacement of the bulk material (1) or by regulating a cycle a relocation of high-pressure-treated partial batches (3.1) between individual high-pressure treatment levels (5) the dwell time or the high-pressure treatment time for the bulk material (1) in the high-pressure treatment volume (Vi) is set; and / or in the case of continuous high-pressure treatment, the bulk material flow is regulated by the bulk material (1) depending on the size and / or a timing of supplied partial batches (3.1) continuously or in individual discontinuous partial batches (3.2, 3.n) in the high-pressure treatment volume (Vi) is relocated; and / or by a continuous displacement of the bulk material (1) or by a discontinuous displacement between individual high-pressure treatment levels (5) during high-pressure treatment, a residence time of the bulk material (1) in the high-pressure treatment volume by setting a rotational speed of rotary actuators (28a) or by clocking translatory ones Actuators (28b) or gravitational force is set.

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 (1) or a discontinuous displacement between individual high-pressure treatment levels (5) in each case by a rotation, in particular by a rotation of at least one rotary actuator (28a) by one axis of rotation aligned in the direction of material flow; or wherein the continuous high-pressure treatment comprises shifting the bulk material (1) in batches in each case by means of a rotation, in particular by means of at least one rotational actuating element (28a) rotated in time; or wherein the continuous high-pressure treatment comprises a continuous displacement of the bulk material (1) or a discontinuous displacement between individual high-pressure treatment levels (5) in each case by translation of at least one translatory actuator (28b); or wherein the continuous high-pressure treatment comprises an autonomously gravitationally driven continuous displacement of the bulk material (1, 3) without rotational or translational actuators; and / or wherein the continuous high-pressure treatment comprises fluidizing the bulk material (1, 3), in particular in a fluidized bed, in particular in an outlet-side area of the pressure vessel device (20).

6. The method according to any one of the preceding method claims, wherein the first step sequence of pressurization (V1) is carried out discontinuously and comprises at least one step from the following group: partial batch pressure generation by means of a pump (11), and / or partial batch supply of bulk material (2.1 ) for high pressure treatment (V2) by means of an inlet fitting (12) accommodating the respective partial batch (2.1) comprising a plunger, a seat-cone fitting, a ball valve and / or a flap; and / or wherein the third step sequence relaxation (V3) is carried out in a discontinuous manner and comprises at least one step from the following group: relaxation in batches by means of a piston engine (33), and / or discharge of bulk goods (3.n) in batches from the second Sequence of steps high pressure treatment (V2) by means of an outlet fitting (25) receiving the respective partial batch comprising a plunger, a seat-cone fitting, a ball valve and / or a flap.

7. 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 extraction of solvent; and / or wherein the continuous high-pressure treatment comprises at least one continuous impregnation, in particular the impregnation of polymers; and / or wherein the high pressure treatment comprises at least one continuous extraction of solvent and is carried out above the critical temperature and above the critical pressure of the extraction medium; and / or wherein 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.

8. The method according to any one of the preceding method claims, wherein the continuous high pressure treatment comprises flowing through the bulk material (3) with high pressure medium (M2), in particular in countercurrent to a displacement of the bulk material.

9. Control device (101) set up to carry out a method according to one of the preceding method claims, the

Control device is coupled to at least one sensor unit (105) set up for detecting a flow of bulk material (1) or a mass or a mass difference or a volume, the control device optionally also set up at least one sensor unit (105) set up for detecting a path and / or one Force and / or pressure includes.

10. High-pressure treatment arrangement (100) set up for high-pressure treatment of bulk material (1) by extraction and / or impregnation on one

High pressure level, in particular high pressure in the range from 40 to 1000 bar, comprising:

a pressurization device (10) with pressure generating means, in particular with at least one pump (11), set up for pressurization (V1) as a first step sequence;

a pressure vessel device (20) coupled to the pressurization device and having a high-pressure-resistant wall (23) enclosing a high-pressure treatment volume (Vi), set up for the high-pressure treatment (V2) as a second step sequence;

a relaxation device (30) coupled to the pressure vessel device, designed for relaxation (V3) as a third sequence of steps;

characterized in that the pressure vessel device (20) for the high pressure treatment (V2) can be arranged in a stationary manner and is set up for continuous high pressure treatment solely by means of the one fixedly arranged high pressure treatment volume (Vi) at the high pressure level.

11. High-pressure treatment arrangement according to the preceding device claim, wherein the high-pressure treatment arrangement (100) is set up for supplying individual bulk batches (2.1) to the high-pressure treatment volume (Vi) during the high-pressure treatment and for continuously or discontinuously displacing the bulk material (1) as a single batch (3). or in partial batches (3.1, 3.n) 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.n) from the high-pressure treatment volume (Vi) during the high-pressure treatment.

12. High-pressure treatment arrangement according to one of the preceding device claims, wherein the pressure container device (20) has at least one high-pressure treatment level (5), which is arranged in the high-pressure treatment volume (Vi) in such a way that it is stationary or adjustable or relocatable, and with closed pressure container device (20) with bulk material (3 3.1) is loadable and which can be discharged during the high pressure treatment or after the high pressure treatment has taken place with the pressure vessel device (20) closed, such that the high pressure treatment can be carried out in a continuous manner; and / or wherein the high-pressure treatment plane (5) is defined by at least one gas-permeable plate (29) or gas-permeable bulkhead arranged horizontally or inclined relative to the horizontal.

13. High-pressure treatment arrangement according to one of the preceding device claims, wherein the pressure vessel device (20) has at least one actuator (28) set up for actuating at least one high-pressure treatment level (5) in the pressure vessel device, in particular a rotationally displaceable actuator (28a) or a translationally displaceable actuator (28b ), in particular at least one actuator (28, 28a, 28b) that is coupled in from the environment (U) into the high-pressure treatment volume (Vi) so as to be pressure-tight.

14. Use of a pressure vessel device (20) for continuous

High-pressure treatment of bulk material (1) by extraction and / or impregnation in a closed system that is sealed off from the environment (U) so that it is pressure-tight, whereby the high-pressure treatment (V2) is carried out and individually regulated as a sequence between pressurization (V1) and relaxation (V3) the bulk material (1, 3) is continuously shifted in a fixedly arranged high-pressure treatment volume (Vi) in the pressure vessel device (20) or in partial batches (3.1) between individual high-pressure treatment levels at predefined times, in particular when using the pressure vessel device (20) a method according to one of the preceding method claims, in particular use of the pressure container device (20) in a high-pressure treatment arrangement (100) according to one of the preceding device claims, in particular at pressures above 40 to 1000 bar.

15. Use of a pressure vessel device (20) for 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 continuous high-pressure treatment (V2) as a sequence of steps between pressurization (V1) and relaxation ( V3) is carried out, the bulk material (1, 3) being treated in a stationary high-pressure treatment volume (Vi) in a continuous manner at the high-pressure level, 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, especially at pressures above 40 to 1000 bar.

16. Use of a pressure vessel device (20) for continuous

High pressure treatment of bulk material (1) in the form of aerogels, by Extraction and / or impregnation, the continuous high-pressure treatment (V2) being carried out as a sequence of steps between pressurization (V1) and relaxation (V3), the bulk material (1, 3) in a fixedly arranged high-pressure treatment volume (Vi) in a continuous manner is treated at the high pressure level, 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 at pressures above 40 to 1000 bar.