EP2127480A1 - Extraction à chaud - Google Patents

Extraction à chaud

Info

Publication number
EP2127480A1
EP2127480A1 EP08715866A EP08715866A EP2127480A1 EP 2127480 A1 EP2127480 A1 EP 2127480A1 EP 08715866 A EP08715866 A EP 08715866A EP 08715866 A EP08715866 A EP 08715866A EP 2127480 A1 EP2127480 A1 EP 2127480A1
Authority
EP
European Patent Office
Prior art keywords
container
microwave
extraction system
condensation
chamber
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.)
Withdrawn
Application number
EP08715866A
Other languages
German (de)
English (en)
Inventor
Werner Lautenschlaeger
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.)
Mikrowellen Systeme MWS GmbH
Original Assignee
Mikrowellen Systeme MWS 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 Mikrowellen Systeme MWS GmbH filed Critical Mikrowellen Systeme MWS GmbH
Publication of EP2127480A1 publication Critical patent/EP2127480A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/80—Apparatus for specific applications
    • H05B6/802—Apparatus for specific applications for heating fluids
    • H05B6/804—Water heaters, water boilers
    • 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
    • B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
    • 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
    • B01D11/0292—Treatment of the solvent
    • B01D11/0296—Condensation of solvent vapours

Definitions

  • the invention relates to a microwave-assisted extraction system for the production of filtered extracts by means of separation of heating and extraction zone by a two-part container system.
  • Microwave heating is a surface heating method that results in a more uniform and faster heating of a solvent than is the case with conventional thermal surface heating methods.
  • the spreading vapor of the solvent permeates a substance to be extracted, hereinafter also referred to as sample, and subsequently condenses. An extract of the sample remains.
  • Hot extraction is used both in the manufacture of kitchen products, such as the production of coffee extracts for espresso, and in the extraction of samples for analytical testing.
  • DE 696 24 006 T2 also shows a thermal hot extraction process for a coffee machine consisting of a two-piece, stacked container system, the lower container a boiler and the upper container is a collection container. Between the two containers another, funnel-shaped container for receiving the material to be extracted is arranged.
  • the funnel-shaped container is spatially connected on the one hand to the interior of the booster and on the other hand with a conduit through which the extract can flow into the collecting container.
  • the line has an overpressure valve on its outlet side to produce a certain overpressure with respect to the atmospheric pressure in the boiler.
  • the pressure relief valve opens as soon as a predetermined pressure is reached. For heating, the water in the boiler is heated in a conventional manner; for example on a stove.
  • the extraction system for microwave-assisted extraction comprises a first container for receiving a solvent. Furthermore, the extraction system has a chamber in fluid communication with the first container for receiving a substance to be extracted. Furthermore, the extraction system has a condensation vessel in fluid communication with the chamber for collecting the extract.
  • the first container is included microwave transparent. The inside of the condensation tank is shielded against microwaves. The first container, the condensation container and the chamber form a unit for placing in a microwave space for microwave-assisted extraction.
  • the two-part container system it is possible to provide a microwave-assisted extraction system in which direct solvent heating by means of microwaves is enabled in a first container while the extract is in the condensation container in fluid communication with the first container is shielded from microwaves.
  • the shielding of the interior of the condensation container from microwaves ensures that burning and decomposition of the extract is prevented by heating by means of microwaves. It is thus possible to put the extraction system as a whole into a microwave space for extraction.
  • the container system can be made compact and thus equally used both for domestic use and for technical applications.
  • a channel for fluid communication is arranged between the chamber and the condensation tank. It is therefore possible to direct the solvent with the extract targeted to the condensation tank.
  • the channel is formed integrally with the condensation tank according to a third aspect of the invention.
  • the channel is microwave-shielding. In this way, penetration of microwaves into the interior of the condensation container via the channel wall is prevented.
  • the interior of the condensation container is in fluid communication with the environment of the extraction system by means of a pressure relief. It is thus possible to accelerate the condensation of the extract into the condensation tank.
  • the extraction system further comprises a lid for closing the condensation container. The extraction of the extract from the system and cleaning the container is facilitated.
  • the lid has a valve which closes the channel with the lid closed with a predeterminable contact pressure.
  • the seventh aspect of the invention when the solvent is heated by microwaves, there is an increasing pressure within the first container all the way to the channel.
  • the increased pressure in turn leads to a boiling point increase of the solvent used, which leads to an increase in the temperature of the solvent vapor.
  • This in turn has an effect on increasing the efficiency of the extraction since the extraction effect corresponding to the solvent vapor can be predetermined by the temperature.
  • the extraction may be at temperatures above the boiling point of the solvent done at atmospheric pressure. This leads to an increase in the diffusion coefficient, an increase in the solubility of the solvent and a reduction in its viscosity.
  • the latter has the particular advantage that the solvent passes more quickly into the pores of the sample. If the solvent vapor with the extract penetrates into the condensation vessel, concentration of the extract occurs simultaneously with the expansion proceeding due to the pressure drop, depending on the pressure setting.
  • the lid is screwed onto the condensation container according to an eighth aspect of the invention.
  • the condensation container can be securely closed and a pressure within the first container to the channel can be adjusted freely.
  • the condensation container has a hinge on which the lid is pivotally mounted.
  • the condensation container further comprises a latching device, in which the lid is locked in the closed state.
  • the lid can be quickly and safely closed and opened again.
  • the pressure relief is formed in the lid.
  • the chamber is provided with at least one filter.
  • the at least one filter is releasably inserted in the chamber according to a twelfth aspect of the invention. In this way it is possible to load the chamber quickly and conveniently with the sample and the filter hole plates or emptied.
  • the at least one filter is covered with at least one fine filter disk. This allows fine filtration of the extract.
  • a seal is arranged between the first container and the condensation container.
  • the seal ensures that a tight connection exists between the first container and the condensation container.
  • the condensation tank is provided with a spout. The pouring of the extract from the condensation tank is facilitated in this way.
  • the condensation tank is made of a microwave-shielding special stainless steel alloy.
  • the interior of the condensation vessel is shielded from microwaves by a metallic Faraday cage.
  • the chamber consists of a microwave-transparent or microwave-absorbing or microwave-reflecting Material.
  • the substance to be extracted can thereby optionally be shielded by microwave radiation or self-irradiated.
  • the first container 1 shows a microwave-assisted extraction system according to the invention, comprising a two-part container system with a first container 1 and a condensation container 2.
  • the first container 1 is preferably in fluid communication with a chamber 3, which in turn is in fluid communication with the condensation container 2.
  • the first container 1 is largely transparent to the microwave.
  • it is preferably made of a microwave-transparent material, so that the interior of the first container 1 represents a microwave-exposed space.
  • the first container 1 serves to receive a solvent L for the microwave-assisted extraction.
  • the solvent L for example, water, alcohol or other known solvents can be used. Due to the microwave transparency, direct heating of the solvent L by microwave MW is ensured.
  • the condensation tank 2 serves as a collection container for the extract E.
  • the container 2 is further shielded against microwave MW. It is irrelevant how the interior of the condensation vessel 2 is shielded from microwave MW.
  • the condensation container 2 is manufactured from a microwave-reflecting stainless steel alloy. Thus, the microwave MW are shielded by a metallic Faraday cage; the container 2 is therefore not microwave transparent. In this way, the condensation container 2 and thus, above all, the interior of the container 2 remains largely cold during microwave irradiation. Consequently, burning and / or decomposition of the extract in the container 2 is prevented by direct microwave irradiation.
  • the edge of the chamber 3 is preferably on the edge of the first container 1.
  • the chamber 3 protrudes completely into the first container 1.
  • the chamber 3 can be both microwave-transparent and microwave-absorbing or -reflective. This depends on whether a substance to be extracted is to be screened by microwave radiation MW or self-irradiated. The latter is advantageous if the sample P itself absorbs or contains water in order to shorten the extraction time.
  • the chamber 3 preferably has a cup part 3a, the bottom of which protrudes into a tube 3b, which is connected to the cup part 3a via a conical section 3c. It is also conceivable any other embodiment that allows fluid communication between the first container 1 and the chamber 3.
  • At least one, preferably two filter hole plates 4, 5 are arranged in the cup part 3a.
  • the first filter 4 is arranged at the base of the cup portion 3 a of the chamber 3 and the second filter 5 at a predetermined distance above the filter 4.
  • the filters 4, 5 are preferably insertable into the chamber 3. But they can also be formed in one piece with the cup part 3a.
  • the Filter hole plates 4, 5 allow for a safe positioning of the substance to be extracted spaced from the solvent L and the condensed extract E.
  • a passage of the generated by means of microwave MW solvent vapor is made possible by means of holes in the filter hole plates 4; ie the fluid communication between the first container 1 and the chamber 3.
  • the filter hole plate 6 has the same tasks as the filter hole plates 4, 5; So a spacing of the substance to be extracted P from
  • the cup portion 3a and the filters 4, 5, 6 define a portion of the chamber 3, which represents the extraction area B.
  • the substance P to be extracted is in the extraction region B of the chamber 3.
  • the filter hole plates 4, 5, 6 can be additionally covered with at least one fine filter disc.
  • the filters 4, 5, 6 provide for the construction of a slight overpressure in the first container 1.
  • Both the first and second and the third filter hole plate 4, 5, 6 are preferably arranged detachably in the chamber 3.
  • the chamber 3, ie the extraction area B quickly and easily with the Sample P and the filter perforated plates 4, 5, 6 and optionally the fine filter discs loaded or emptied.
  • at least one of the filter hole plates 4, 5, 6 can also be formed integrally with the chamber.
  • the first container 1 is preferably frictionally connected to a lower side 2a of the condensation container 2.
  • the two containers are detachably connected by means of a non-positive screw connection. But it is also possible any other type of connection.
  • a seal 7 can additionally be arranged on the underside 2a of the chamber 3, which produces a tight connection between the first container 1 and the condensation container 2. This prevents escape of the solvent vapor and thus a pressure drop during the extraction.
  • the bottom 2a of the condensation container 2 is substantially closed.
  • the lower surface 2a extends conically inwardly from the outer wall portions 2b of the container 2 and upwardly at a shallow angle away from the first container 1.
  • the underside has the function of directing the solvent vapor with the extract E into the interior of the container 2 or to an inlet opening 8a of a channel 8.
  • the channel 8 extends between the chamber 3 and the interior of the condensation tank 2. In this way, fluid communication between the chamber 3 and the condensation tank 2 is made possible.
  • the channel 8 is preferably microwave-shielding.
  • the channel 8 is formed integrally with the condensation tank 2.
  • the channel 8 is preferably arranged coaxially with the outer walls of the container 2.
  • the channel 8 preferably extends in a cylindrical manner and parallel to the wall regions 2 b from the spatial center of the lower side 2 a of the condensation container 2 to its opening 2 a facing the side 2 a.
  • the channel 8 has an inlet opening 8a, which is preferably arranged on the side 2a of the container 2, and an outlet opening 8b, which is preferably open towards the opening of the container 2. In this way, in the assembled state of the container system, fluid communication arises from the first container 1 via the chamber 3 to the second container 2, so that the steam can flow through the entire container system.
  • the opening of the second container 2 is preferably closed with a lid 9.
  • the type of lid attachment is not relevant.
  • the cover 9, according to one embodiment, preferably by means of a screw on the second container 2 up or unscrewed.
  • the cover 9 is pivotally mounted on the second container 2 by means of a hinge.
  • a locking device on the second container 2 is provided, in which the pivotally mounted cover 9 is engaged and thus the second container 2 closes securely.
  • a pressure relief valve 10 is further mounted in the lid 9.
  • the valve 10 closes the outlet opening 8b of the channel 8. Dazu the valve 10 is pressed by means of a spring 11 arranged in the cover 9 with a certain contact pressure on the opening 8b of the channel 8. In this way, any pressure equal to or higher than the atmospheric pressure in the first tank 1 and the extraction area B for extraction, respectively, can be set.
  • the lid 9 further comprises a pressure relief 9a.
  • the pressure relief 9a is arranged at a closed cover 9 above the opening of the second container 2 and laterally spaced from the outlet opening 8b.
  • a pressure equalization of the pressure in the condensation tank 2 takes place with the ambient pressure of the extraction system, whereby the Condensation of the extract E in the sump 2 is still accelerated.
  • the extract condenses into the container 2.
  • the shielding of the interior of the vessel 2 against microwave MW further ensures that the extract is burned and decomposed by microwave heating MW is prevented.
  • the container system it is possible to place the container system as a coherent unit including the condensation container 2 in the microwave space during the extraction, without having a negative effect on the extract. It is thus possible to make the extraction system compact. It is also possible to use it in any commercial home-made microwave, which makes it equally possible to use microwave-assisted extraction both for domestic use and for technical applications.
  • the second container 2 preferably has a spout. This spout is preferably formed integrally with the condensation tank 2.
  • the filters 4, 5, 6 is a substance to be extracted or sample P in the chamber 3, more precisely in the Extraction area B placed.
  • a solvent such as, for example, water or alcohol, filled.
  • the chamber 3 is inserted with the sample P in the first container 1.
  • the chamber 3 can also be loaded with the sample P and optionally with the filters 4, 5, 6 and the fine filter discs only when it is inserted in the first container 1.
  • the lid 9 is screwed onto the second container 2 or snapped into the latching device of the second container 2, so that the valve 10 against the biasing force of the spring 11, the outlet opening 8b of the line 8 closes.
  • the biasing force of the spring 11 is freely adjustable.
  • the condensation tank 2 is connected to the first container 1.
  • the condensation container is preferably screwed onto the first container 1.
  • By means of the seal 7 is formed between the first container 1 and the condensation container 2, a tight connection.
  • the fully assembled container system now represents a unit that is placed in a microwave space as a whole.
  • microwave power MW the unit is irradiated in the microwave space.
  • the first container 1 is largely transparent to the microwave, direct solvent heating is made possible.
  • the condensation tank 2 and the interior of the container 2 remains cold.
  • the expansion of the solvent L and the propagating solvent vapor push the very hot solvent L through the tube 3b in the extraction area B of the chamber 3, in which the substance P to be extracted is located.
  • the substance P to be extracted is completely wetted by the solvent L.
  • the pressure in the first container 1 rises continuously as a result of the continuous heating of the solvent L by means of microwaves MW up to the outlet opening 8b. This results in a boiling point increase of the solvent L used, which has an effect on increasing the efficiency of the extraction.
  • the valve 10 is pressed against the spring biasing force and the extract E escapes into the condensation tank 2. Due to the microwave shielding property of the condensation tank 2, this is cold and the extract E condenses into the tank 2.
  • a part of the solvent L due to the pressure drop is simultaneously lost by the expansion of the extract. In this way one learns depending on the pressure specification, a concentration of the extract.
  • the pressure relief 9a the pressure in the collecting container 2 is kept constant in accordance with the ambient pressure of the extraction system.
  • the extraction process is ended.
  • the irradiation by means of microwave MW is set and the extraction system can be taken as a whole from the microwave space.
  • the entire system is unscrewed after use again and poured the extract E for consumption or for the analytical determination.
  • the casting is simplified by the integrally formed with the condensation container spout. It is also conceivable that the extract E is poured in still screwed together state of the extraction system. Furthermore, it is conceivable that the extraction system is again placed in the microwave space for extraction after pouring when solvent is still present in the first container 1. After completion of the extraction process and disassembly of the extraction system, the system is cleaned and, as described above, can be reused for microwave assisted extraction.
  • the invention is not limited to the abovementioned limitations. All conceivable embodiments of the container system are covered by this application.
  • the first container is arranged at the bottom while the condensation container is located at the top.
  • the position of the two containers can also be exchanged, for example, so that the first container 1 is arranged at the top and the condensation container 2 at the bottom, or the containers are arranged next to one another.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

L'invention concerne un système d'extraction destiné à l'extraction assistée par micro-ondes, comprenant : un premier conteneur (1) destiné à recevoir un solvant (L), une chambre (3) qui est en communication de fluide avec le premier conteneur (1), destinée à recevoir une substance à extraire (P), et un récipient de condensation (2) qui est en communication de fluide avec la chambre (3), destiné à la collecte de l'extrait (E), caractérisé en ce que le premier conteneur (1) est transparent aux micro-ondes, cependant que l'intérieur du récipient de condensation (2) est protégé contre les micro-ondes (MW), et en ce que le premier conteneur (1), le récipient de condensation (2) et la chambre (3) forment une unité destinée à être mise en place dans un espace micro-ondes pour l'extraction assistée par micro-ondes.
EP08715866A 2007-02-19 2008-02-19 Extraction à chaud Withdrawn EP2127480A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE202007002435U DE202007002435U1 (de) 2007-02-19 2007-02-19 Heißextraktion
PCT/EP2008/001291 WO2008101670A1 (fr) 2007-02-19 2008-02-19 Extraction à chaud

Publications (1)

Publication Number Publication Date
EP2127480A1 true EP2127480A1 (fr) 2009-12-02

Family

ID=38089952

Family Applications (1)

Application Number Title Priority Date Filing Date
EP08715866A Withdrawn EP2127480A1 (fr) 2007-02-19 2008-02-19 Extraction à chaud

Country Status (3)

Country Link
EP (1) EP2127480A1 (fr)
DE (1) DE202007002435U1 (fr)
WO (1) WO2008101670A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2953687B1 (fr) * 2009-12-15 2012-10-05 Labo Concept Nature Installation et procede pour le traitement d'un produit de type organisme vegetal ou animal
FR2975020B1 (fr) * 2011-05-13 2015-03-13 Univ D Avignon Et Des Pays De Vaucluse Obtention d'un extrait vegetal a l'aide de micro-ondes
CN103830954B (zh) * 2014-01-17 2016-04-20 中冶南方工程技术有限公司 一种易于维护的钢渣排水口滤板
CN105527149B (zh) * 2016-01-11 2018-08-03 云南中烟工业有限责任公司 一种多功能密闭微波萃取装置、其使用方法及用途
US10241014B2 (en) * 2017-07-10 2019-03-26 Cem Corporation Instrument for analytical sample preparation
US10330573B2 (en) 2017-07-10 2019-06-25 Cem Corporation Rapid sample preparation for analytical analysis using dispersive energized extraction
US10295447B2 (en) * 2017-07-10 2019-05-21 Cem Corporation Rapid energized dispersive solid phase extraction (SPE) for analytical analysis

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4143541C2 (de) * 1991-02-19 1999-03-04 Mls Gmbh Vorrichtung zum Extrahieren von Proben mittels eines Lösungsmittels bei erhöhter Temperatur
DE9321612U1 (de) * 1992-04-30 2000-12-14 MLS Mikrowellen-Labor-Systeme GmbH, 88299 Leutkirch Vorrichtung zur Verdampfungsbehandlung von vorzugsweise flüssigen Stoffen, insbesondere Reagenzstoffen, oder zum Aufbereiten oder Analysieren von Probenmaterial
IT1284992B1 (it) * 1996-10-18 1998-05-28 Alfonso Bialetti & C Spa Caffettiera a pressione per la preparazione di infuso di caffe'
DE10313870A1 (de) * 2003-03-21 2004-10-07 Anton Paar Gmbh Vorrichtung zur Behandlung von Proben in einem Mikrowellenfeld
DE10313873A1 (de) * 2003-03-21 2004-09-30 Anton Paar Gmbh Vorrichtung zur Lösungsmittelextraktion in einem Mikrowellenfeld
EP1629725B1 (fr) * 2004-07-20 2007-09-12 Milestone S.r.l. Extraction par microondes de composés naturels volatils

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2008101670A1 *

Also Published As

Publication number Publication date
WO2008101670A1 (fr) 2008-08-28
DE202007002435U1 (de) 2007-05-16

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