EP3946668A2 - Procédé et dispositif de contrôle de la production d'un extrait par extraction solide-liquide - Google Patents

Procédé et dispositif de contrôle de la production d'un extrait par extraction solide-liquide

Info

Publication number
EP3946668A2
EP3946668A2 EP20710422.5A EP20710422A EP3946668A2 EP 3946668 A2 EP3946668 A2 EP 3946668A2 EP 20710422 A EP20710422 A EP 20710422A EP 3946668 A2 EP3946668 A2 EP 3946668A2
Authority
EP
European Patent Office
Prior art keywords
mass
raffinate
mixture
extract
residual moisture
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
EP20710422.5A
Other languages
German (de)
English (en)
Inventor
Colman O'GORMAN
Ulrich ROLLE
Maria Carmen LEAL CARCIA
Ludger Tacke
Franz-Joseph HELMS
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.)
GEA TDS GmbH
Original Assignee
GEA TDS 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 GEA TDS GmbH filed Critical GEA TDS GmbH
Publication of EP3946668A2 publication Critical patent/EP3946668A2/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
    • B01D11/0207—Control systems
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00—Tea; Tea substitutes; Preparations thereof
    • A23F3/16—Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/18—Extraction of water soluble tea constituents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00—Tea; Tea substitutes; Preparations thereof
    • A23F3/16—Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/22—Drying or concentrating tea extract
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00—Tea; Tea substitutes; Preparations thereof
    • A23F3/40—Tea flavour; Tea oil; Flavouring of tea or tea extract
    • A23F3/42—Isolation or recuperation of tea flavour or tea oil
    • A23F3/423—Isolation or recuperation of tea flavour or tea oil by solvent extraction; Tea flavour from tea oil
    • 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
    • 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
    • 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
    • B01D—SEPARATION
    • B01D37/00—Processes of filtration
    • B01D37/04—Controlling the filtration
    • B01D37/043—Controlling the filtration by flow measuring

Definitions

  • the invention relates to a method and a device for controlling the production of an extract by solid-liquid extraction, preferably by solid-liquid hot extraction and in particular for large-scale industrial applications, by means of at least one extraction container in which a secondary solvent with a predetermined first mass and a primary mixture, consisting of a solid, primary solvent and a transition component, are brought into contact with one another with a predetermined second mass for obtaining the extract for a predetermined residence time. After the retention time, the extract obtained and a complementary portion of raffinate are separated from one another.
  • the proposed invention is intended in particular to produce a tea concentrate which, in terms of process engineering and technology, is based on the aforementioned solid-liquid hot extraction and in which the tea raw material, for example tea leaves, flowers, stalks, grains, seeds, roots or other plant components, and hot water or boiling water be brought into contact with each other, controlled.
  • tea raw material for example tea leaves, flowers, stalks, grains, seeds, roots or other plant components, and hot water or boiling water be brought into contact with each other, controlled.
  • DE 699 29 220 T2 or PCT / US99 / 23178 describes a method for extracting a consumable material from a solid raw material, for example coffee or tea.
  • the solid raw material is formed in an enclosed volume of a container, for example in the form of a bed.
  • a volume of aqueous solvent is added to the enclosed volume and the amount of solid raw material.
  • the extraction is carried out under the application of pressure, the solvent being water, which has a temperature which exceeds room temperature and is preferably between about 88 and about 100 degrees Celsius.
  • the water flows through the solid raw material and the resulting aqueous extract is removed from the container.
  • CN 109 569 018 A discloses a circulation line for the solvent with the primary mixture, which is routed through an extraction container and which branches off from a discharge line and opens into the head space of the extraction container.
  • a feed line opens into the head space of the extraction vessel from above, independently of the circulation line.
  • the invention is based on a method for controlling the production of an extract [tea concentrate] by solid-liquid extraction by means of at least one extraction container.
  • a secondary solvent hot water or boiling water
  • a primary mixture consisting of a solid, primary solvent [carrier] and a transition component [clay and other desired and undesirable accompanying substances]
  • a predetermined second mass for obtaining the extract for a predetermined residence time [brewing time] brought into contact with one another.
  • the basic idea of the invention consists on the one hand essentially in the fact that the primary mixture [tea leaves] is not subject to spatial restrictions in order to solve the problem with a view to improving the exchange of substances during extraction.
  • the primary mixture is not extracted in a spatially limited volume (for example in the sense of perforated boundary walls, permeable bags, sacks, sieve containers).
  • This allows the primary mixture [tea leaves] to be kept in suspension in the secondary solvent, which does not hinder its swelling behavior, facilitates the penetration of secondary solvents and thus intensifies the exchange of substances compared to extraction in the so-called fixed bed.
  • the primary mixture is not introduced in its entirety as a predetermined second mass, but more or less in the smallest partial quantities or minimal individual portions and continuously over a predetermined metering time into the secondary solvent provided in the extraction container in the scope of the first mass .
  • the metering time is to be provided much shorter than the dwell time in order to ensure the narrowest possible dwell time spectrum for all partial quantities of the primary mixture.
  • the basic idea of the invention consists in that, in order to solve the problem with a view to the controlled dehumidification of the raffinate with residual moisture [extracted tea leaves with residual moisture] to obtain further valuable extract [tea concentrate], the two mixture components present after the extraction, namely a mixture of extract and raffinate, are further treated at least in such a way that the complementary portion in the form of a raffinate with residual moisture [extracted tea leaves with residual moisture] is that from extract existing residual moisture is at least partially withdrawn by dehumidification and added to the extract that has already been separated out.
  • One embodiment of the method provides that mechanical energy in the broadest sense is supplied to the raffinate with residual moisture.
  • This can be, for example, vibrations or shaking or pressure surges by means of a pulsed and possibly intermittent compressed gas to which the raffinate to be treated is exposed.
  • a balance or determination of the degree of dehumidification is carried out by comparing the mass flows of the substrate before and after the dehumidification step, the respective mass flows being determined.
  • the degree of dehumidification is controlled by a feedback control intervention on the determined first mass flow of a mixture discharged from the extraction container after the extraction [tea concentrate + extracted tea leaves] and / or on the supply of mechanical energy.
  • control intervention and the necessary control-related determinations can be clocked in finite time periods or in infinitesimal time periods.
  • the control intervention can be based on the determined data which are obtained on the treated substrate simultaneously before and after the dehumidifying step or on the same flowing substrate before and after the dehumidifying step.
  • the extraction container is filled quickly.
  • the smooth and gentle supply of the second mass is expediently carried out by adding a a suitable amount of water for the second mass, whereby a sludge is prepared, so to speak, which allows easy and gentle conveying, preferably by means of a rotating displacement pump that is gentle on the product.
  • the predetermined second mass is not introduced into the secondary solvent in its entirety, but in partial amounts and continuously.
  • the second mass is supplied, as is also proposed, either after step (i) or already in the course of step (i).
  • This distribution state and the resulting improved swelling behavior of the primary mixture also includes an intensification of the mass transfer in a mixture produced in this way during the dwell time by relative movement between the secondary solvent and the primary mixture.
  • the relative movement is either a movement of the primary mixture [tea leaves] in the secondary solvent [hot water or boiling water] or a flow around the primary mixture through the secondary solvent or a superposition of both forms of movement.
  • the relative movement is preferably generated by mechanical and / or fluid-mechanical stirring effects. It has been proven that the primary mixture kept in suspension swells more than in the fixed bed, which results in a more efficient extraction compared to the fixed bed.
  • the mixture is discharged while avoiding forced delivery solely by gravity as a result of an inflow height of the outlet connection of the extraction container opposite a target location for the mixture.
  • a second variant of the procedure looks in this regard propose to additionally support the discharge of the mixture by applying a gas pressure of a gaseous propellant to a free surface of the mixture. This also ensures that the product is conveyed gently.
  • step (iv) Separating the mixture discharged after step (iii) into a raffinate with residual moisture [extracted tea leaves with residual moisture] and an extract freed from raffinate with residual moisture [tea concentrate freed from extracted tea leaves with residual moisture].
  • the mixture is preferably separated by sieving off the raffinate with residual moisture, whereby, as is also provided, the dehumidification provided after step (v) is also achieved if mechanical energy in the broadest sense is supplied to the substrate to be treated during sieving.
  • the dehumidification increases the yield of the extract of the process according to the invention and thus its economic efficiency.
  • the tolerable proportion of extract is determined depending on the primary mixture used [tea leaves or tea raw material]. This determination helps to control the degree of solution or yield of noble and desired ingredients from the raffinate with residual moisture and it helps to avoid or at least reduce the solution or yield of base and undesirable ingredients.
  • the dehumidification is achieved in a surprisingly simple manner that the to be treated substrate mechanical energy in the broadest sense, for example vibrations or shaking or pressure surges with pneumatic means are supplied.
  • the mass flow determination in a predetermined, preferably finite or also infinitesimal period of time is expediently carried out with a mass flow meter, so that corresponding masses or mass differences can also be calculated from the mass flows determined.
  • a balance or a comparison of the mass flows or the mass differences in the period before and after dehumidification indirectly provides the degree of dehumidification of the raffinate with residual moisture [extracted tea leaves with residual moisture].
  • a homogeneous distribution of the primary mixture in the secondary solvent is a prerequisite for determining the mass of the primary solvent from the first mass flow.
  • the transition component [tein and other desired and undesired accompanying substances before extraction] which is contained in the primary mixture [tea leaves], can be neglected in the comparison to a good approximation.
  • the addition of water is simply taken into account in the above balance.
  • step (ix) controlling the degree of dehumidification carried out after step (v; vi) by feedback control intervention on the first mass flow and the supply of mechanical energy. If deviations from the defined, tolerable portion of extract are found, then these deviations are compensated according to the invention by changing the first mass flow, which is continuously determined, and / or by supplying mechanical energy.
  • step (vi) correlates with further control parameters which are determined with the following method steps (the necessary calculation equations are specifically specified below in the context of an exemplary embodiment):
  • step (xiii) Determination of a tolerable first differential mass of the raffinate with residual moisture [tolerable first differential mass of the extracted tea leaves with residual moisture] in accordance with the first difference determined in step (xi) reference mass and the second differential mass determined according to step (xii) based on the tolerable portion, which is defined as the quotient on the one hand from the difference between the tolerable first and second differential mass and on the other hand from the difference between the first and second differential mass.
  • the first mass flow knows which mass of tea leaves (based on the state before extraction and before being fed into the hot water or boiling water) is or must be contained in the first mass flow in the period of time .
  • the proposed balancing of the first and the second mass flow in the time span determines the actual value of a mass of tea leaves with residual moisture or the first differential mass that occurs during dehumidification.
  • the current proportion of tea concentrate in the extracted tea leaves with residual moisture is determined from this information. According to the invention, this proportion is to be reduced to the stipulated, tolerable or to a desirable proportion of tea concentrate in terms of control technology.
  • step (v) The dehumidification carried out after step (v) is carried out according to a proposal at the same time as or after the separation carried out according to step (iv).
  • the extract [tea concentrate] obtained as a whole is then subjected to filtering to separate out undesirable fine and extremely fine particles. It has proven to be useful if the filtering is preceded by a primary clarification by separation in a centrifugal field, as a result of which the service life of a filter device for performing the filtering is significantly increased.
  • the mixture discharged after step (iii) is discharged solely under the action of gravity.
  • the discharge of the mixture be additionally supported by applying a gas pressure of a gaseous propellant to a free surface of the mixture.
  • a first method with a view to the mode of operation of the extraction container provides that the part of the method defined by steps (i and ii) in one first extraction vessel is carried out, which is designed as a discontinuously operating homogeneous reaction vessel.
  • the second mass is fed entirely to the first mass.
  • the second mass is not split up into partial masses and that these partial masses are not added to corresponding partial masses of the first mass that are desolated in other places, and the second mass over a more or less long dosing time and a single area of the mass there located total th first mass is supplied.
  • more than one first extraction container is operated in parallel and at the same time or in parallel and with a time delay.
  • the further treatment of the mixture obtained in each case takes place at the same time or at different times in the single process line already described in accordance with steps (iii to v).
  • a second method with regard to the mode of operation of the extraction container provides that the part of the method defined by steps (i and ii) is carried out in a second extraction container, which is designed as a discontinuous homogeneous reaction container.
  • the second mass is divided into a finite number of second partial masses and in this case into at least two second partial masses.
  • the second partial masses are separated from one another and respectively corresponding first partial masses of the first mass to ensure a desired mass ratio of the second mass to the first mass.
  • the second method reduces the filling time with tea leaves according to the number of second partial masses while ensuring the desired product-gentle treatment and high quality with a view to adhering to a specified dwell time (brewing time).
  • a third method provides that the part of the method defined by steps (i and ii) is carried out in and with a third extraction container, the prior to step (i)
  • the first mass laid down which is preferably fed in via the upper region of the third extraction container, is removed in the dwell time in the form of a piston flow oriented vertically in the direction of gravity.
  • the first mass is forcibly discharged and a mass flow of the second mass is continuously added to a mass flow of the first mass that is forcibly generated in the process so that a desired mass ratio of the second mass to the first mass is ensured in the obtained mixture of primary mixture and secondary solvent.
  • the mixture of primary mixture and secondary solvent is fed from above to a free surface of a mixture located in the third extraction vessel.
  • the mixture of primary mixture and secondary solvent flows to the free surface to the extent that secondary solvent leaves the third extraction container via its outlet connection during the dwell time.
  • the metering of the second mass into the first mass ends when the mixture first fed to the third extraction container has flowed through the third extraction container as a mixture in the form of the piston flow from top to bottom after the dwell time has elapsed.
  • the process is then continued according to steps (iii to v).
  • the third process implements a quasi-continuous process with very precise setting and compliance with the desired dwell time or brewing time.
  • the formation of a piston flow is favored if the third extraction vessel has a slim geometry, i. E. when its liquid-loaded height is a multiple of its diameter or its dimensions transverse to its height.
  • a design in this regard leads to a flow pipe with a corresponding residence time behavior.
  • the third method can be carried out with a method according to any one of claims 2 to 10.
  • a device for performing the method according to the invention for controlling the production of an extract by solid-liquid extraction by means of an extraction container starts from an extraction container which has at least a first interior region.
  • This first inner area has in an upper area an inlet connection for the supply of a secondary solvent, a first inlet connection for the supply of a primary mixture and in a lower area an outlet connection for the complete discharge of a mixture consisting of an extract and a raffinate.
  • the drain connection opens into a drain line which, based on the direction of gravity, is spaced from the drain connection by an inflow height.
  • the drain line has, viewed in the direction of flow, a control valve for changing a mass flow flowing through the control valve, a first mass flow meter for determining a first mass flow for the mixture, a separating device for separating the mixture into the extract and a raffinate with residual moisture, a dehumidifying device for dehumidifying the Raffinate with residual moisture and a second mass flow meter to determine a second mass flow for an extract freed from raffinate with residual moisture. Furthermore, a control device is provided which is signal-technically connected to at least the control valve, the first and the second mass flow meter and the dehumidifying device.
  • the separating and dehumidifying devices are implemented in the form of a controllable vibrating or vibrating screen.
  • both procedural measures namely the separation and dehumidification, are carried out particularly effectively and efficiently in a single unit.
  • the sieve openings are dimensioned so that the raffinate [extracted tea leaves] is sufficiently separated from the extract [tea concentrate].
  • a filter device is arranged in connection with the second mass flow meter in the discharge line. Since the filter device should preferably carry out a final clarification of the extract, that is to say a separation of fine and finest particles, coarser particles that pass through the sieve openings have a negative impact on the service life of the filter device.
  • a centrifugal separator is connected upstream of the filter device, which ensures primary clarification of the extract.
  • the device according to the invention is alternatively equipped with three differently designed extraction vessels, a first extraction vessel being designed as a discontinuously operating homogeneous reaction vessel.
  • the first extraction container delimits a first inner area which has a single inlet connection and a single outlet connection.
  • the invention proposes a second extraction container, which is designed as a discontinuous homogeneous reaction container and which is above the first inner area and has at least one second inner region immediately adjacent to it.
  • Each further interior area is arranged above and directly adjacent to the preceding interior area.
  • a further first inlet connection for the primary mixture is assigned to each inner area above the first inner area.
  • Each further first inlet connection is assigned a further outlet connection below and at a distance from it in such a way that the mixture obtained in the respectively assigned interior area is discharged as unadulterated as possible from the primary mixture which is fed to the respectively adjacent interior area below via the respectively assigned first inlet connection .
  • the aforementioned inner areas extend over the height of the second extraction container. They are not separated from one another by any kind of built-in structure, but rather simply separated from one another in terms of flow technology in their area by the respective flow guide according to the invention, with a limited mixing movement being able to take place over the imaginary boundaries between the inner areas. It is also proposed that the first inlet connection and each further first inlet connection be connected to a rotating conveying device that is gentle on the product.
  • a quasi-continuous extraction process is implemented when the device according to the invention is equipped with a third extraction container, over which a circulation line branching off from a discharge line is passed.
  • This third extraction container has a feed line for the supply of a secondary solvent [hot water or boiling water] or a mixture of a primary mixture [tea leaves] and a secondary solvent.
  • the feed line enters the third extraction container via a third footwell, penetrates this into a third headspace and opens there via an outlet.
  • the third extraction container has a drain connection for the discharge of the secondary solvent or a mixture [tea concentrate + extracted tea leaves], consisting of an extract [tea concentrate] and a raffinate [extracted tea leaves], with the drain connection opening out from the third footwell and there merges into the drain line.
  • the drain line viewed in the direction of flow and spaced vertically by an inlet height from the drain connection in the direction of gravity, has a control valve, a first mass flow meter for determining a first mass flow for the mixture, a separating device for separating the mixture into the extract and a raffinate with residual moisture [extracted Teeblät ter with residual moisture], a dehumidifying device for dehumidifying the raffinate with residual moisture, and a second mass flow meter to determine a second mass flow for an extract freed from raffinate with residual moisture [tea concentrate freed from extracted tea leaves with residual moisture].
  • the circulation line branches off at a branching point, which joins the inlet line at a junction and which is flowed through from the branch to the junction.
  • a control device is provided which is connected in terms of signaling at least to the control valve, the first and second mass flow meters and the dehumidifying device.
  • first, second or third extraction containers can be operated in parallel and at the same time or in chronological succession and the mixture obtained in each case can be discharged into the process line operated according to steps (iii to v).
  • an embodiment of the third extraction container provides that in a liq stechniksbeankschlagten At the edge of the outer area of the third head space, at least two third stirring devices are provided. These are preferably arranged evenly distributed over this outer area and, due to their respective installation position, are capable of generating a flow movement directed towards the center of the third extraction container with a downwardly oriented flow component.
  • a further embodiment of the third extraction container ensures that the piston flow is as undisturbed as possible in that the drain connection is arranged centrally and at the lower end of the third extraction container and that the feed line is passed concentrically through the drain connection.
  • the metering device is connected to a rotating displacement pump that is gentle on the product, whereby the primary mixture [tea leaves] is kept free from mechanical and / or fluid mechanical stresses as far as possible.
  • the first, second and third extraction container In order to accelerate the removal of the mixture [tea concentrate + extracted tea leaves] while maintaining the principle of gentle removal of the product, provision is made for the first, second and third extraction container to have a supply connection for the supply of a pressurized gas in the region of its upper end.
  • the invention can be implemented in the most varied of configurations of a method for controlling the production of an extract by solid-liquid extraction of the generic type and in each case by means of three differently designed ex traction containers. Furthermore, the invention is implemented in a wide variety of embodiments of a device for performing the above-mentioned respective method. The method and the device, each in conjunction with one of the three Ex traction containers and shown using the preferred application example for controlling the production of a tea extract, are described below with reference to the drawing. Show it
  • FIG. 1 shows a schematic representation of a first device with a first extraction container
  • FIG. 2 shows a schematic representation of a second device with a second extraction container
  • FIG. 3 shows a schematic representation of a third device with a third extraction container
  • FIG. 4 shows a flow diagram of the method which is carried out with each of the devices according to FIGS. 1 to 3.
  • a feed mixture (A °° B) is called “primary mixture” [tea leaves] and a solution created by the extraction is called “secondary mixture” or extract (C °° B) [tea concentrate ⁇ , where the notation (A °° B) or (C °° B) should indicate the phase "mixed” or “solution”.
  • a substance that changes from one phase to the other is a "transition component” [Tein and other desired or undesired accompanying substances], which is marked with B below.
  • a non-transferring component of the primary mixture is a “primary solvent” or a carrier A [carrier before extraction].
  • a first device 1 according to the invention for controlling the production of an extract by solid-liquid extraction, in particular a solid-liquid hot extraction, by means of a first extraction container 10 according to the invention is shown in FIG.
  • the first extraction container 10 has a single and first inner area Ib1, which in an upper area, a first head space 10.1, has a single inlet connection 11 with an inlet valve 11a for the supply of the secondary solvent C, which has a predetermined first mass M in the first inner area Ib1 is presented and forms a free surface N there. Furthermore, in the first head space 10.1 there is a first inlet connection 12 with a first inlet valve 12a for the supply of the primary mixture (A °° B) [tea leaves], which with a predetermined second mass m of the first mass M to form a corresponding mixture (A °° B) + C [mixture of tea leaves and hot water] is added.
  • a first footwell 10.2 of the first extraction container 10 has a single outlet connection 14 with an outlet valve 14a for the complete discharge of the mixture (C °° B) + A, consisting of the extract (C °° B) and the raffinate A. Furthermore, a feed connection 13 with a feed valve 13a for the feed of a compressed gas G with a gas pressure p is provided at the upper end of the first head space 10.1.
  • the first extraction container 10 has insulation D for thermal insulation from its surroundings and a first stirring device 10a, which ensures the most homogeneous, but in any case product-friendly, uniform distribution of the substrates in the discontinuously operating homogeneous reaction container.
  • the first inlet connection 12 is connected to a product-friendly, preferably rotating conveying device 22, which preferably has a conveying screw 22a, which is driven by a preferably controllable drive motor 22b (MA).
  • the primary mixture (A °° B) is stored in a storage container 22c, from which it flows to the screw conveyor 22a.
  • the drain connection 14 opens into a drain line 15 which, viewed in the direction of flow and spaced vertically from the drain connection 14 by an inflow height H in the direction of gravity, has a control valve 16.
  • the discharge line 15 also takes, again viewed in the direction of flow, a first mass flow meter 17 for determining a first mass flow m- L for the mixture, a separating device 18 with a suitable sieve 18a and a raffinate collecting container 18b for separating the mixture into the extract (C °° B) and a raffinate with residual moisture A + [extracted tea leaves with residual moisture], a dehumidifying device 19 for dehumidifying the raffinate with residual moisture A + and a second mass flow meter 20 for determining a second mass flow m 2 for one freed from raffinate with residual moisture A + Extract (C °° B) ** [tea concentrate freed from extracted tea leaves with residual moisture].
  • the separating and dehumidifying device 18, 19 can be implemented in two separate units or in a single unit, preferably in a vibrating or vibrating screen 18 + 19, whereby in the case of the integrated design the Sieve 18a is fed mechanical energy ME by means of a preferably controllable vibration or shaking drive 19a (MA).
  • MA controllable vibration or shaking drive 19a
  • the residence time of the raffinate with residual moisture A + can be influenced, which in turn allows its residual moisture content to be controlled. Greater inclination of the sieve shortens the dwell time and increases the residual moisture content; a lower inclination of the sieve influences these parameters in the opposite sense.
  • the sieve geometry also has an influence on the throughput of the mixture after extraction.
  • the width of the screen 18, 19 is determined by the required throughput. An expansion of the sieve width with increased throughput is necessary to ensure adequate distribution of the solid particles on the sieve surface.
  • An extension of the sieve 18, 19 increases the residence time of the solids on the sieve 18, 19 and means more extensive dehumidification of the raffinate with residual moisture A + due to a longer treatment.
  • the method according to the invention can therefore, inter alia, by changing the feed quantity of the mixture on the sieve 18, 19, by the inclination of the Sieves 18, 19 and modified by changing the sieve geometry who the.
  • a control device 21 is provided which is signal-technically connected via signal transmission lines 21a to at least the control valve 16, the first and second mass flow meters 17, 20 and the dehumidifying device 19 (signal connections e to h).
  • the valves 11 to 14 are controlled in automatic mode by the control device 21 via the signal connections a to d.
  • a filter device 24 for separating fine and extremely fine particles from the extract is arranged in the discharge line 15, the extract being freed from the raffinate with residual moisture A + (C °° B) ** becomes the filtered extract (C °° B).
  • the filter device 24 optionally has a centrifugal separator 23 for separating coarser particles P, also seen in the direction of flow, which the sieve 18a of the separating device 18 when separating the raffinate with residual moisture A + have happened upstream, whereby the extract (C °° B) ** becomes a pre-clarified extract (C °° B) * , which extends the service life of the filter device 24.
  • first extraction containers 10 ′, 10 ′′ of the type described above can be connected to the drain line 15, between the drain valve 14a and the control valve 16, in order to increase the production output of the first device 1.
  • the first method like the second and third methods (FIGS. 2 and 3), is carried out by method steps (i) to (v) of claim 1 and, in an advantageous embodiment, by method steps (vi) to (xiii) of claims 3 to 5, which are graphically illustrated in their context of conditions and their meaning in a flow chart of FIG.
  • the second and third methods differ from the first method, the means of the first extraction container 10 is carried out by treating the substrate in the respectively assigned second or third extraction container 100, 1000 and the related procedural measures up to the removal of the mixture after step (iii) of the method.
  • the following description of the method is limited to the terms for the production of tea concentrate, as indicated in the list of reference symbols of the abbreviations used in concordance with the higher-level terms.
  • step (i) a first mass M [hot water C] is presented in the first extraction container 10 via the supply connection 11 (FIG. 4: specification C and Figure 1).
  • the extraction can be represented by the following scheme (1):
  • the concentration k is defined according to equation (4):
  • step (iii) after the dwell time t, the mixture (C °° B) + A [7ee- concentrate + extracted tea leaves] with the total mass M + m, consisting of the extract (C °° B) [tea concentra] and the raffinate A [tea leaves], discharged from the first extraction container 10 via the outlet connection 14 (FIG. 4: (M + m) ((OB) + A); FIG. 1).
  • step (iv) the mixture discharged after step (iii) is converted into a raffinate with residual moisture A + [extracted tea leaves with residual moisture] and one of Raffinate with extract freed from residual moisture A + (C °° B) ** [from extracted tea leaves with residual moisture A + freed tea concentrate separated by means of the separating device 18 (FIG. 4; FIG. 1).
  • step (v) a further treatment of the raffinate with residual moisture A + is provided at least in such a way that the residual moisture consisting of extract is at least partially removed from the raffinate with residual moisture A + by dehumidification and fed to the already separated extract (C °° B).
  • step (vi) the raffinate with residual moisture A + is dehumidified in the dehumidifying device 19, namely to a specified, tolerable proportion d extract (C °° B) ** in the raffinate with residual moisture A + by supplying mechanical energy (ME ) into the raffinate with residual moisture A + .
  • the extract (C °° B) ** obtained as a result is added to the extract (C °° B) ** obtained after step (iv) (FIG. 4: specification d and ME; FIG. 1).
  • step (vii) the following are determined: a first mass flow rr ⁇ of the mixture discharged after step (iii) via the mass flow meter 17 and via the second mass flow meter 20 a second mass flow m 2 of the raffinate obtained after steps (iv, v) extract freed with residual moisture A + (C °° B) * ⁇ in each case in a finite period of time At or an infinitesimal period of time dt (FIG. 4: default At, k; FIG. 1).
  • a second differential mass A (Aooß) of the primary mixture (A °° B) can be determined according to step (xii) of claim 5 with the default data At, k.
  • step (viii) the degree of dehumidification is determined by comparing the first mass flow rri 1 with the second mass flow m 2 (FIG. 4; FIG. 1). According to the balance equation (2)
  • a first differential mass Am (A + ) of the raffinate with residual moisture A + can be determined according to step (xi) of claim 5 with the default data At, 1 77i 2 .
  • step (ix) the degree of dehumidification carried out after step (v; vi) is determined by feedback control intervention on the first mass flow 771 ⁇ ! and / or the supply of mechanical energy ME is controlled. Specifically, this takes place in that from the first differential mass Am (A + ) and second differential mass Am (AooB) determined in accordance with steps (xi) and (xii) using the definition relationship (5) for the specified tolerable portion d extract (C °° B) in the raffinate with residual moisture A + , namely
  • a tolerable first differential mass Am (A + ) toi of the raffinate with residual moisture A + can be calculated. This is then used for control purposes in comparison with the first differential mass Am (A + ) of the raffinate with residual moisture A + if it is found that Am (A + )> Am (A + ) toi (FIG. 4, FIG. 1 ).
  • the tea concentrate (C °° B) ** freed from extracted tea leaves with residual moisture A + is expediently pre-clarified in the centrifugal separator 23 through the separation of particles P below the separation limit of the sieve 18a and then as pre-clarified tea concentrate (C °° B) * the filter device 24 is supplied, which it then leaves as a filtered tea concentrate (C °° B), for example to be further treated to a tea drink.
  • a second device 1 * according to the invention for controlling the production of an extract by solid-liquid extraction, in particular a solid-liquid hot extraction, by means of a second extraction container 100 according to the invention is shown in FIG. 2.
  • the second extraction container 100 is designed as a discontinuously operating homogeneous reaction container, which, however, in contrast to the first extraction container 10, is located above the first inner area Ib1 (with the first inlet connection 12, the first inlet valve 12a, the outlet connection 14, the Drain valve 14a) and has at least one second inner area Ib2 immediately adjacent to it.
  • each inner area Ib2, Ib3, ... provided above the first inner area Ib1 has a further first inlet connection 12.1, 12.2, ...
  • a second footwell 100.2 of the second extraction container 100 has the outlet connection 14 with the outlet valve 14a for the complete discharge of the mixture (C °° B) + A from the lowest, the first inner area Ib1. Furthermore, the supply connection 13 with the supply valve 13a for supplying the compressed gas G with the gas pressure p is provided at the upper end of a second head space 100.1.
  • the second head space Via the single inlet connection 11 with the inlet valve 11 a, which is located in the upper region of the second extraction container 100, the second head space
  • the secondary solvent C with the predetermined first mass M is placed in the intended inner areas Ib1, Ib2, Ib3, ..., and it forms the free surface N there in the uppermost inner area.
  • the second extraction container 100 has insulation D for thermal insulation from its surroundings and a second stirring device 100a, which can be designed in such a way that it is as homogeneous as possible in each of the inner areas Ib1, Ib2 and Ib3 of the homogeneous reaction container working as discontinuously However, the case is product-friendly even distribution of the there the substrates located.
  • the first inlet connection 12 and all further first inlet connections 12.1, 12.2, ... are each connected to a product-friendly, preferably rotating conveyor device 22, which preferably each has a conveyor screw 22a, which is each driven by a preferably controllable drive motor 22b (MA).
  • the primary mixture (A °° B) is preferably stored in a single storage container 22c, from which it flows to the respective screw conveyor 22a.
  • the drain connection 14 opens into the drain line 15, which, viewed in the flow direction and spaced vertically from the drain connection 14 by an inlet height H in the direction of gravity, opens into the control valve 16 and continues from there into the second device 1 *.
  • This part of the second device 1 * is identical to the corresponding part of the first device 1.
  • the second process is carried out in the scope of steps (i and ii) in the second extraction vessel 100, which is designed as a discontinuously operating homogeneous reaction vessel.
  • a delivery device 22 can be assigned to each of these first inlet connections.
  • a single conveying device 22 can also supply the first inlet connections 12.1, 12.2,... With the primary mixture (A °° B) through a suitable controllable distribution device.
  • a third device 1 ** according to the invention for controlling the production of an extract by solid-liquid extraction, in particular a solid-liquid FIG. 3 shows hot extraction by means of a third extraction container 1000 according to the invention, through which a circulation line 25 branching off from a discharge line 15 is passed.
  • the third extraction vessel 1000 has an inlet line 33 in which, seen in the direction of flow, a third shut-off valve 32 is provided upstream of a junction 27, this part of the inlet line serving to supply the secondary solvent C with the first mass M [hot water].
  • the supply line 33 enters via the supply connection 11 with the supply valve 11a for supplying the secondary solvent C [hot water] or a mixture (A °° B) + C of primary mixture (A °° B) and secondary Solvent C [mixture of tea leaves and hot water] enters the third extraction container 1000 via a third footwell 1000.2, through which it penetrates into a third headspace 1000.1 and there discharges via an outlet 34 above a free surface N (maximum height of a liquid level) .
  • the outlet connection 14 is preferably arranged centrally and at the lower end of the third extraction container 1000 and the inlet line 33 is preferably passed concentrically through the outlet connection 14.
  • the discharge line 15 is vertically spaced from the discharge connection 14 with a discharge valve 14a in the direction of gravity by the inlet height H, it opens into the control valve 16 and continues from there into the third device 1 **.
  • This part of the third device 1 ** is identical to the corresponding part of the first or second device 1, 1 *.
  • a branch point 26 From the drain line 15, upstream of the control valve 16, branches off at a branch point 26 from the circulation line 25, which opens at the junction 27 into the inlet line 33 and which flows through from the branch point 26 to the connection point 27 out.
  • the circulation line 25 based on the branching point 26, there is initially a first shut-off valve 28, a pump 29 for conveying the secondary solvent C, then a metering device 30 for metering the primary mixture (A °° B) into the secondary solvent C and a second shut-off valve 31 are provided.
  • the metering device 30 is connected via a first inlet connection 12 with a first inlet valve 12a to the rotating displacement pump 22, which is gentle on the product.
  • An advantageous embodiment of the third extraction container 1000 provides that at least two third stirring devices 1000a are provided in a liquid-loaded outer area of the third head space 1000.1, which are preferably evenly distributed over this outer area and are enabled by their respective installation position, each one to the center of the third extraction container 1000 directed flow movement with a flow component oriented in the direction of gravity, which supports the formation of a piston flow K.
  • the third extraction container 1000 has an insulation D for thermal insulation from its surroundings. Furthermore, the supply connection 13 with the supply valve 13a for supplying the compressed gas G with the gas pressure p is provided at the upper end of the third head space 1000.1.
  • control device 21 In automatic mode, the control device 21, not shown, is also connected in terms of signaling to the first shut-off valve 28, the pump 29, the metering device 30 and the second and third shut-off valves 31, 32 (signal connections i, j,, I, 11 and I2).
  • the third method is carried out within the scope of steps (i and ii) in and with the third extraction container 1000, wherein the first mass M presented after step (i), which is preferably fed to the inlet line 33 via the outlet 34 opening out above the free surface N. is, in the dwell time t in the form of the piston flow K oriented in the direction of gravity, is forcibly discharged via the outlet connection 14.
  • the continuously obtained mixture is fed from above to the free surface N of a mixture located in the third extraction container 1000.
  • the metering of the second mass m into the first mass M ends when the mixture (A °° B) + C [mixture of tea leaves + hot water] which is first fed to the third extraction container 1000 after the dwell time t has expired as a mixture (C °° B ) + A [tea concentrate + extracted tea leaves] has flowed through the third extraction container 1000 in the form of the piston flow K from top to bottom.
  • this cycle time which corresponds to the mean residence time or the brewing time t, the exchange of substances takes place by extraction.
  • the third method is then continued according to steps (iii to v) and, in advantageous embodiments, according to steps (vi to xiii) or carried out according to one of claims 2 to 10.
  • the mixture of tea leaves and hot water (A °° B) + C fed to the outlet 34 thus sinks in the mean residence time t from the maximum filling level L down to the outlet 14 of the third extraction container 1000, whereby a quasi-continuous extraction process is implemented.
  • the generation of the piston flow K is supported by the third stirring devices 1000a described, in particular in start-up operation, but also in continuous and shut-down operation.
  • G gaseous propellant - compressed gas air; nitrogen, inert
  • a primary solvent carrier A primary solvent carrier

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Automation & Control Theory (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Tea And Coffee (AREA)

Abstract

L'invention concerne un procédé de contrôle de la production d'un extrait par extraction solide-liquide, de préférence par extraction solide-liquide à chaud, en particulier pour des applications industrielles à grande échelle et notamment pour la production d'un concentré de thé, au moyen d'au moins un récipient d'extraction (10 ; 100 ; 1000) selon le terme générique de la revendication 1. La présente invention a pour but, d'une part, d'améliorer l'échange de substances lors de l'extraction par rapport aux solutions selon l'état de la technique et, d'autre part, de permettre une déshumidification contrôlée d'un raffinat comportant de l'humidité résiduelle pour obtenir un extrait supplémentaire de valeur par le procédé selon l'invention. Selon le procédé, cet objectif est atteint par les étapes suivantes : (i) fourniture de la première masse (M) dans le récipient d'extraction (10 ; 100 ; 1000) ; (ii) introduction de la deuxième masse (m) prédéterminée sans restriction spatiale dans la première masse (M) fournie, la distribuer et la mélanger à la première masse (M) ; (iii) décharge d'un mélange ((C∞B)+A) constitué de l'extrait ((C∞B)) et du raffinat (A) du récipient d'extraction (10 ; 100 ; 1000) ; iv) séparation du mélange évacué après l'étape iii) en un raffinat contenant de l'humidité résiduelle (A+) et un extrait ((C∞B)**) débarrassé du raffinat contenant de l'humidité résiduelle (A+) et v) traitement ultérieur du raffinat avec de l'humidité résiduelle (A+) au moins de telle sorte, que l'humidité résiduelle constituée par l'extrait est au moins partiellement éliminée du raffinat avec l'humidité résiduelle (A+) par déshumidification et ajoutée à l'extrait déjà séparé ((C∞B)).
EP20710422.5A 2019-03-28 2020-02-19 Procédé et dispositif de contrôle de la production d'un extrait par extraction solide-liquide Pending EP3946668A2 (fr)

Applications Claiming Priority (2)

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DE102019002218.1A DE102019002218A1 (de) 2019-03-28 2019-03-28 Verfahren und Vorrichtung zur Steuerung der Herstellung eines Extraktes durch Fest-Flüssig-Extraktion
PCT/EP2020/000045 WO2020192959A2 (fr) 2019-03-28 2020-02-19 Procédé et dispositif de contrôle de la production d'un extrait par extraction solide-liquide

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US (1) US20220184524A1 (fr)
EP (1) EP3946668A2 (fr)
KR (1) KR20210143859A (fr)
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WO (1) WO2020192959A2 (fr)

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CN114733229B (zh) * 2022-04-20 2023-06-27 吕梁学院 一种茶多酚溶解提取装置
JP7454324B2 (ja) 2022-05-02 2024-03-22 アサヒ飲料株式会社 抽出液製造システム

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Publication number Priority date Publication date Assignee Title
FR1498026A (fr) * 1966-10-28 1967-10-13 Hydrocarbon Research Inc Procédé d'hydrogénation d'huiles de pétrole
US3992983A (en) * 1973-12-05 1976-11-23 Societe D'assistance Technique Pour Produits Nestle S.A. Preparation of tea extracts
GB2059276B (en) * 1979-09-21 1983-05-11 Coal Industry Patents Ltd Controlling the filtration of solid and liquid mixtures
US5997929A (en) * 1997-11-03 1999-12-07 Nestec S.A. Extraction process
US6203837B1 (en) 1998-10-06 2001-03-20 Xcafe' Llc Coffee system
US7172738B2 (en) * 2002-05-29 2007-02-06 Russell Matthew F Methods and apparatus for processing mixtures of liquids and solids
EP2837290A1 (fr) 2013-08-15 2015-02-18 Radeberger Gruppe KG Procédé et dispositif de fabrication d'une boisson au thé
JP2016034419A (ja) * 2014-08-04 2016-03-17 ザ コカ・コーラ カンパニーＴｈｅ Ｃｏｃａ‐Ｃｏｌａ Ｃｏｍｐａｎｙ 抽出液製造システム及び抽出液の製造方法
JP6616952B2 (ja) 2015-03-25 2019-12-04 Ｆｄｋ株式会社 筒型電池の封口体及び筒型電池
CN109126191A (zh) * 2018-09-10 2019-01-04 江阴天江药业有限公司 一种中药自动化提取分离装置及提取分离方法及其应用
CN109569018A (zh) * 2018-12-04 2019-04-05 江阴天江药业有限公司 一种种子类药材的自动化提取分离方法

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WO2020192959A4 (fr) 2021-01-07
DE102019002218A1 (de) 2020-10-01
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WO2020192959A3 (fr) 2020-11-19
KR20210143859A (ko) 2021-11-29

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