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EP3897899A2 - Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation - Google Patents

Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation

Info

Publication number
EP3897899A2
EP3897899A2 EP19831718.2A EP19831718A EP3897899A2 EP 3897899 A2 EP3897899 A2 EP 3897899A2 EP 19831718 A EP19831718 A EP 19831718A EP 3897899 A2 EP3897899 A2 EP 3897899A2
Authority
EP
European Patent Office
Prior art keywords
pressure treatment
pressure
bulk material
continuous
volume
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP19831718.2A
Other languages
German (de)
English (en)
Inventor
Volkmar Steinhagen
Ansgar HERBER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ThyssenKrupp AG
Uhde High Pressure Technologies GmbH
Original Assignee
ThyssenKrupp AG
Uhde High Pressure Technologies GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ThyssenKrupp AG, Uhde High Pressure Technologies GmbH filed Critical ThyssenKrupp AG
Publication of EP3897899A2 publication Critical patent/EP3897899A2/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0242—Moving bed of solid material in towers, e.g. comprising contacting elements
    • B01D11/0246—Moving bed of solid material in towers, e.g. comprising contacting elements comprising rotating means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0203—Solvent extraction of solids with a supercritical fluid
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F5/00—Coffee; Coffee substitutes; Preparations thereof
    • A23F5/24—Extraction of coffee; Coffee extracts; Making instant coffee
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0207—Control systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0219—Fixed bed of solid material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0226—Moving bed of solid material with the general transport direction of the solids parallel to the rotation axis of the conveyor, e.g. worm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0234—Moving bed of solid material using other slow rotating arms or elements, whereby the general transport direction of the solids is not parallel to the rotation axis, e.g. perpendicular
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0238—Moving bed of solid material on fixed or rotating flat surfaces, e.g. tables combined with rotating elements or on rotating flat surfaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0242—Moving bed of solid material in towers, e.g. comprising contacting elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0253—Fluidised bed of solid materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • B01D11/0284—Multistage extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/008—Processes carried out under supercritical conditions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
    • C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0253—Fluidised bed of solid materials
    • B01D11/0257—Fluidised bed of solid materials using mixing mechanisms, e.g. stirrers, jets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2300/00—Characterised by the use of unspecified polymers
    • C08J2300/14—Water soluble or water swellable polymers, e.g. aqueous gels
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2300/00—Characterised by the use of unspecified polymers
    • C08J2300/30—Polymeric waste or recycled polymer
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
    • C12C3/00—Treatment of hops
    • C12C3/04—Conserving; Storing; Packing
    • C12C3/08—Solvent extracts from hops
    • C12C3/10—Solvent extracts from hops using carbon dioxide

Definitions

  • 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.
  • the invention relates to the use of a pressure vessel device for the continuous high-pressure treatment of bulk material.
  • the invention relates to a device and a method in each case according to the preamble of the respective independent claim.
  • 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.
  • 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 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.
  • 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 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.
  • 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).
  • 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.
  • 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.
  • 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.
  • 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).
  • 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.
  • a temperature level in the high pressure treatment volume can also be set; in particular, a constant temperature can be maintained.
  • 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 .
  • No material flow function has to be performed by means of the high-pressure treatment volume.
  • 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.
  • 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.
  • the high-pressure medium can correspond to an extraction medium used.
  • 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.
  • 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.
  • a high-pressure pump can be provided, which can optionally also have several heads. Alternatively, several high-pressure pumps can be used in parallel.
  • 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.
  • 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.
  • 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).
  • solvent extraction may be desired / required.
  • 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.
  • 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.
  • 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.
  • 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).
  • 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.
  • extraction medium can also be continuously conveyed through the high-pressure container.
  • 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.
  • 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.
  • the pressure build-up, the high-pressure treatment and the relaxation can be spatially separated from one another.
  • 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.
  • granular starting material 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 can have the following components:
  • 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.
  • a / the conveying device conveys the bulk material in the high-pressure treatment volume, in particular upwards and further into a downpipe.
  • extraction medium in particular C0 2
  • Liquid solvent collects at the bottom of the high-pressure treatment volume and is discharged there through a nozzle or outlet.
  • 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:
  • 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.
  • 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.
  • the relaxation can be achieved via the pressure loss in a long relaxation line.
  • 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.
  • 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
  • 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.
  • 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.
  • 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.
  • 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.
  • PS polystyrene
  • the gas flow is preferably reduced (reduced throughput) and the bulk material can be collected at the (respective) treatment level.
  • 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.
  • 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.
  • 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.
  • the invention is also based on the concept of spatially separating or separating the individual step sequences.
  • 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.
  • 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 .
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • the continuous high-pressure treatment comprises an autonomous, gravitational force-driven continuous displacement of the bulk material without rotary or translational actuators.
  • this also provides a lean device-related structure, the material flow being able to take place at least in sections in an autonomous manner.
  • 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.
  • 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.
  • 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.
  • 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).
  • the material flow can also be decoupled from high-pressure treatment parameters in the second step sequence.
  • 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.
  • 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.
  • 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.
  • 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.
  • a motor fluid motor, electric motor
  • actuating the respective actuator optionally also within the pressure vessel device.
  • 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.
  • 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.
  • the material flow can also be optimized with regard to large volume changes / increases in the range of a factor of 10.
  • Fig. 1 in a schematic representation or in at least partially sectioned
  • FIGS. 7A, 7B, 7C, 7D each in a sectional side view individual
  • FIG. 1 shows a high-pressure treatment arrangement 100.
  • a pressurization device 10 10a, 10b, 10c, 10d, 10e, 10f are shown.
  • 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.
  • 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.
  • FIGS. 1 and 2 to 4 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.
  • the respective pressure vessel device 20 has components from the following group:
  • 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.
  • 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.
  • 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.
  • FIG. 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 °.
  • 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.
  • 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.
  • 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.
  • 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.
  • FIG. 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.
  • FIG. 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.
  • the batch can also be optimally stored / relocated with regard to pressure / compression and expansion possibilities.
  • 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.
  • 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.
  • 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).
  • the internals can also be provided as conveying elements which are loaded when high pressure is already present.
  • 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.
  • 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.
  • FIG. 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.
  • 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.
  • FIG. 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.
  • FIG. 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.
  • the material flow in the high-pressure treatment volume Vi can be regulated independently of the supply or discharge of partial batches.
  • 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.
  • the high-pressure treatment volume can be provided, for example, by a cylindrical or tubular pressure vessel device.
  • FIG. 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
  • 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.
  • FIGS. 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).
  • a plurality of 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).
  • the dwell time contact time
  • e.g. only two or four or even more compartments / stages may be provided.
  • the hatching density schematically illustrates the level of the high pressure level.
  • a first sequence of steps V1 (pressurization) comprises, in particular, three steps which can be delimited or regulated individually:
  • a second step sequence V2 (continuous high-pressure treatment) comprises in particular the following steps:
  • Moving S2.1 can optionally include one of the following steps:
  • a third step sequence V3 (relaxation) comprises in particular the following steps:
  • 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.
  • a pressure build-up element in particular a pump
  • 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.
  • 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.
  • 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.
  • FIG. 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.
  • FIG. 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.
  • pressure generating means in particular pump or piston

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Abstract

L'invention concerne un procédé de traitement haute pression de produits en vrac (1) par extraction et/ou imprégnation, lesdits produits en vrac étant disposés dans un volume de traitement haute pression (Vi) d'un dispositif sous la forme d'un récipient sous pression (20) et traités à un niveau de pression élevée, notamment à une haute pression située dans une plage de 40 à 1000 bars, ledit procédé comprenant au moins les trois étapes suivantes, pouvant être réglées respectivement de manière individuelle : application d'une pression (V1), traitement haute pression (V2), détente (V3) ; le traitement haute pression (V2) étant effectué en continu dans le volume de traitement haute pression (Vi), ce dernier ou la totalité du dispositif sous la forme d'un récipient sous pression (20) étant fixé(e) à demeure pendant le traitement haute pression (V2), et la continuité du traitement haute pression (V2) étant assurée uniquement au moyen du volume de traitement haute pression (Vi). Cela permet en particulier une optimisation, sur le plan de la technique de processus, d'opérations de traitement haute pression, telles que l'extraction par exemple. L'invention concerne en outre un dispositif correspondant pour le traitement haute pression de produits en vrac.
EP19831718.2A 2017-12-22 2019-12-20 Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation Pending EP3897899A2 (fr)

Applications Claiming Priority (3)

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DE102017223712 2017-12-22
DE102018222881.7A DE102018222881A1 (de) 2017-12-22 2018-12-21 Vorrichtung und Verfahren zum kontinuierlichen Hochdruckbehandeln von Schüttgut sowie Verwendung
PCT/EP2019/086552 WO2020127889A2 (fr) 2017-12-22 2019-12-20 Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation

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EP3897899A2 true EP3897899A2 (fr) 2021-10-27

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EP18829404.5A Pending EP3727626A1 (fr) 2017-12-22 2018-12-21 Dispositif et procédé de traitement à haute pression de matière en vrac par extraction et/ou imprégnation, et utilisation
EP19832108.5A Pending EP3897900A2 (fr) 2017-12-22 2019-12-20 Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation
EP19831718.2A Pending EP3897899A2 (fr) 2017-12-22 2019-12-20 Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation

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EP19832108.5A Pending EP3897900A2 (fr) 2017-12-22 2019-12-20 Dispositif et procédé pour le traitement haute pression en continu de produits en vrac et utilisation

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US (2) US11612831B2 (fr)
EP (3) EP3727626A1 (fr)
KR (3) KR102369887B1 (fr)
CN (1) CN111757772B (fr)
DE (4) DE102018222882A1 (fr)
WO (3) WO2019122387A1 (fr)

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KR102369887B1 (ko) 2022-03-07
US20220072447A1 (en) 2022-03-10
KR20200097340A (ko) 2020-08-18
WO2020127889A4 (fr) 2020-11-05
DE102018222883A1 (de) 2019-06-27
WO2020127889A3 (fr) 2020-09-03
US20220062788A1 (en) 2022-03-03
DE102018222881A1 (de) 2019-06-27
WO2020127957A4 (fr) 2021-03-18
US11612831B2 (en) 2023-03-28
WO2020127889A2 (fr) 2020-06-25
DE102018222874A1 (de) 2019-06-27
WO2020127957A2 (fr) 2020-06-25
EP3727626A1 (fr) 2020-10-28
KR102592507B1 (ko) 2023-10-24
DE102018222882A1 (de) 2019-06-27
US20200324223A1 (en) 2020-10-15
KR20210095715A (ko) 2021-08-02
WO2019122387A1 (fr) 2019-06-27
CN111757772A (zh) 2020-10-09
CN111757772B (zh) 2022-10-21
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