WO2014121311A1 - Procédé d'enrichissement de substances de valeur à partir d'une matière première liquide - Google Patents

Procédé d'enrichissement de substances de valeur à partir d'une matière première liquide Download PDF

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Publication number
WO2014121311A1
WO2014121311A1 PCT/AT2014/000006 AT2014000006W WO2014121311A1 WO 2014121311 A1 WO2014121311 A1 WO 2014121311A1 AT 2014000006 W AT2014000006 W AT 2014000006W WO 2014121311 A1 WO2014121311 A1 WO 2014121311A1
Authority
WO
WIPO (PCT)
Prior art keywords
extractant
extractor
vorkonzentratabscheider
preconcentrate
storage container
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.)
Ceased
Application number
PCT/AT2014/000006
Other languages
German (de)
English (en)
Inventor
Eduard Lack
Helmut Seidlitz
Martin Sova
Franz Lang
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.)
Natex Prozesstechnologie GmbH
Original Assignee
Natex Prozesstechnologie 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 Natex Prozesstechnologie GmbH filed Critical Natex Prozesstechnologie GmbH
Priority to MX2015010196A priority Critical patent/MX2015010196A/es
Priority to EP14705694.9A priority patent/EP2953699A1/fr
Publication of WO2014121311A1 publication Critical patent/WO2014121311A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0446—Juxtaposition of mixers-settlers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0488—Flow sheets
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
    • C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
    • C09F1/02—Purification

Definitions

  • the invention relates to a process for the enrichment of valuable substances, in particular phytochemicals, such as e.g. Polyphenoie, dyes, antioxidants and the like, from a liquid raw material, e.g. Lipids, fermentation broths or solvent extracts, as well as an apparatus for carrying out this method.
  • phytochemicals such as e.g. Polyphenoie, dyes, antioxidants and the like
  • Paprikaole- oresin also called paprika extract
  • paprika extract an extract from the red pepper pulp. It contains, among other things, capsanthin and capsorum, which are responsible for the red color of the pepper fruit.
  • the paprika extract is used in oil- and water-soluble commercial preparations for coloring meat and fish preserves, sweets (marzipan), mayonnaises, sausages and cosmetics. Also as a feed additive for egg yolk and skin pigmentation of poultry fattening, the two dyes are used.
  • the present invention therefore aims to provide a method and a device which (s) the enrichment of a variety of recyclables from liquid starting materials with low apparati low cost and high efficiency.
  • the method according to the invention of the type mentioned initially consists essentially in that the liquid raw material is mixed in a mixing device with a compressed extractant, in particular CO 2 , from a storage container, whereupon the mixture is fed to a preconcentrate separator and the substances which are predominantly more readily soluble in the extractant are separated from the undissolved constituents which include undissolved valuable substances, the laden extractant being withdrawn from the preconcentrate separator and the undissolved constituents remaining as preconcentrate, the laden extractant being passed through a separator system in which the dissolved substances are separated from the loaded extractant and the purified extractant is returned to the storage container.
  • the extractant is thus used for the extraction of more soluble substances, such as short-chain lipids, so that the less soluble or insoluble substances, such as the long-chain lipid components remain together with the under the prevailing conditions sparingly soluble recyclables.
  • the economy of the process according to the invention is ensured in particular by the recycling of the extractant.
  • the extractant is left in the compressed state during the entire circulation, so that a complete relaxation and subsequent recompression and the associated effort can be avoided.
  • the enrichment according to the invention can only take place in one stage, so that the abovementioned preconcentrate represents the end product of the process.
  • the enrichment takes place in two stages, the valuable substances with the sparingly soluble constituents of the raw material being concentrated in a first enrichment stage to form a preconcentrate and the preconcentrate being concentrated in a second enrichment stage to form a final concentrate.
  • the second enrichment stage is carried out here with changed compared to the first enrichment stage pressure and / or temperature conditions.
  • the two-stage enrichment can be either continuous or discontinuous.
  • the preconcentrate is either continuously withdrawn from the preconcentrate separator and fed to an extractor connected downstream of the preconcentrate separator, in which it is then further concentrated by renewed supply of extractant from the storage container.
  • the Vorkonzentratabscheider can be designed in this case in the form of a cyclone.
  • the process is further developed such that the preconcentrate in the preconcentrator is enriched further from the storage container to the desired concentration after completion of the feedstock feed with compressed extractant.
  • the process according to the invention is preferably further developed in such a way that the compressed extractant is present in a liquid or supercritical state in the preconcentrator and optionally in the downstream extractor, by way of example as carbon dioxide.
  • the advantage of the supercritical C0 2 over liquid carbon dioxide lies in the fact that the supercritical phase has both a lower viscosity and a lower surface tension than its liquid counterpart. Due to the low viscosity, a high diffusion or through the intensive mixing of the raw material with the supercritical fluid, a rapid mass transfer is achieved. This property thus ensures extraction of substances soluble in the respective extractant from the liquid raw material.
  • the process according to the invention is preferably developed such that the pressure in the preconcentrator is chosen such that the more easily soluble substances dissolve more strongly in the extractant than the sparingly soluble valuable substance to be enriched.
  • the pressure in Vorkonzentratabscheider or optionally in the downstream extractor is thus adjusted so that the more soluble substances (eg short-chain lipids) solve, while the poorly soluble fraction (eg long-chain lipids, carotenoids, phytochemicals) in undissolved form in Vorkonzentratabscheider or optionally remains in the downstream extractor.
  • the pressure should be selected such that the valuable material hardly or not solved.
  • the pressure in Vorkonzentratabscheider or optionally in the downstream extractor is hereby preferably selected between 150 and 450 bar. Particularly preferably, the pressure is between 250 to 400 bar.
  • the method according to the invention is further developed such that the temperature in the preconcentrate separator is selected such that a sufficient difference in density for the separation is achieved.
  • the temperature in Vorkonzentratabscheider between 20 and 100 ° C. This achieves a sufficiently low density of the extractant and of the substances dissolved therein, which causes the thus loaded extractant to rise in the preconcentrate separator and can subsequently be withdrawn.
  • the process according to the invention can be developed in particular to the effect that the separation of the dissolved substances from the loaded extractant is favored by a change in the solubility, in particular a pressure and / or a temperature change.
  • the separation of the dissolved substances from the loaded extractant in the process according to the invention can also be effected by adsorption or a membrane process.
  • tomato oil, hazelnut oil, algae oil, crustacean oil, paprika oleoresin, rice peel oil, coffee oil, fatty acid distillate, fermentation broths or roasted aromatic oil as liquid raw material for subsequent enrichment of the valuable substances contained therein and accordingly lycopene, hazelnut aroma, carotenoids, dyes .
  • the process according to the invention is advantageously developed in such a way that the final concentrate is discharged via a final concentrate separator in which the extractant remaining in the final concentrate is separated off. This step ensures further separation of the extractant remaining in the stock concentrate, with the result that the end product of the claimed process is in a much purer form than without this last step and that a higher level of extractant can be recycled to the storage container.
  • the apparatus for carrying out the method described above comprises a compressed extractant storage container, a liquid raw material storage container, a mixing device connected to the compressed extractant storage container and the liquid raw material storage container, a separator connected to the mixing apparatus which has a discharge port for discharging a loaded extractant and a discharge port for discharging a preconcentrate, the discharge ports for discharging the loaded extractant being connected to a separator system connected to the compressed extractant storage container through a return line ,
  • the inventive construction can be developed such that the mixing device is designed as a static mixer, mixing chamber or nozzle.
  • the formation according to the invention may further preferably be such that the downstream extractor is designed as a thin-layer extractor or as a column extractor.
  • a thin-layer extractor is to be understood as meaning a device as can be taken, for example, from WO 2004/018070 A1.
  • Such a thin-layer extractor has a pressure-resistant reactor with at least one feed opening for the pre-extract and the compressed extraction medium and corresponding discharge openings, wherein the feed opening for the pre-extract to be treated opens on the inner jacket of the reactor, at which a film-like layer of the pre-extract forms ,
  • a rotor is arranged, the radial arms of which interact with the preconcentrate film on the inner jacket of the reactor.
  • the rotor forms the tools for mechanical processing of the thin film, which in the simplest case of wipers, rollers, doctor blades or the like can be formed.
  • the thickness of the film is determined by the preset distance of the rotating tool to the inner jacket of the reactor.
  • the tools, such as rollers may have a helical profiling, but may also be conical, concave or convex, the profiling, during unrolling along the preconcentrate film, simultaneously promoting downward movement of the film in the direction of the discharge opening.
  • Countercurrent to the pre ⁇ concentrate the extraction agent is then introduced ⁇ to the reactor, with the corresponding feed opening off the bottom part is formed.
  • the extractant rises inside the reactor and comes into intensive contact with the preconcentrate film, whereby the surface of the film exposed to the extractant is constantly renewed by the kneading process effected by the rotating tools.
  • the loaded extractant may subsequently be withdrawn via an outlet opening provided in the lid.
  • the device according to the invention is developed in an advantageous manner to the effect that the discharge of the preconcentrator for discharging the preconcentrate with a downstream extractor is in communication and that in the Vorkonzentratabscheider connecting the downstream extractor line another mixing device is arranged with the storage container connected is.
  • This further mixing device allows an additional separation of dissolved in the extractant substances and thus favors the recovery of a final product with very high purity.
  • the device can be designed such that additional extractors are arranged after the previously mentioned extractor for further concentration, the feed in each case being effected via a mixing device in which fresh extractant and correspondingly pre-concentrated mixed material from the respective previous extractor are intensively mixed ,
  • the device is developed to the effect that the separation system comprises at least two separators, which are connected to each other with the interposition of at least one throttle valve. This ensures that different pressures prevail in the different separators of the system, which are different from the pressure in the preconcentration ratabscheider are chosen lower, which causes the substances dissolved in the extractant can be separated again from the extractant and that the purified extractant can be recycled to the storage container.
  • the device is preferably designed in such a way that a discharge opening of the preconcentrator or the downstream extractor for discharging the preliminary or final concentrate is connected to a final concentrate separator whose discharge opening for recovering the remaining extractant via a line and a downstream compressor with the Storage tank is connected.
  • the second enrichment step is carried out after completion of the first enrichment step, so that it is a total of a discontinuous procedure.
  • 3542 g of paprika oleoresin (30070CU) were injected at a mass flow rate of 9.2 g / min radially into supercritical CO2 (350 bar, 50 ° C) in a mixing device formed by a tube.
  • the mass flow of the C0 2 was 33kg / h.
  • the mixture of laden C0 2 and the undissolved portion of the oleoresin in C0 2 was conducted to a preconcentrator in which the loaded CO 2 was separated from the portion of the oleoresin which was not dissolved in CO 2 .
  • the loaded CO2 was further expanded into a separator system.
  • the undissolved portion of the oleoresin was accumulated in the preconcentrate separator.
  • 1037 g of the preconcentrate obtained in step 1 were introduced into an extractor.
  • the extractor used here can be the preconcentrate separator used in step 1 or a separate aggregate.
  • the preconcentrate was extracted with supercritical CO 2 at 33 kg / h at 350 bar and 50 ° C. After about 135 minutes and 75kg C0 2 2 485g Oleoresinex- were the loaded C0 tract (dye ert 10082CU) withdrawn from the extractor. The remaining residue (552 g) in the extractor reached a colorant value of 105348CU.
  • FIG. 1 shows a device for the batch process according to the present invention
  • FIG. 2 shows a device for the continuous process according to the present invention.
  • a storage container for the compressed extraction medium is denoted by 1 and a storage container for the liquid raw material by 2.
  • the storage containers 1 and 2 are connected via the lines 3 and 4 with the mixing device 5.
  • the extractant is compressed by the use of the motor-driven pump 7 and thereby brought to the desired pressure level.
  • a pre-pressure pump 6 or a pre-cooler in line 3 is installed.
  • the heat exchanger 8 brings the compressed extractant to the desired temperature. temperature.
  • the heat exchanger 9, which is located in line 4 provides for adjusting the temperature of the liquid raw materials.
  • the flow of the compressed extractant and the liquid raw materials can be controlled by means of speed regulators on the pumps 7 and 12.
  • the ratio of liquid raw material to volume flow of the extractant influences the extraction performance and can be set individually by the speed controls of the pumps 7 and 12.
  • the guided through the shut-off valve 10 liquid raw material is fed by means of the downstream pump 12 in the mixing device 5, while the compressed extractant reaches the mixing device 5 via line 3.
  • the mixing device 5 which is preferably designed as a static mixer, the two components are mixed intensively. This results in a disperse mixture of extractant and liquid raw material.
  • This mixture is withdrawn from the mixing device 5 and spent in the Vorkonzentratabscheider 13.
  • pre-concentrate separator 13 for example, there is a pressure of 350 bar at a temperature of, for example, 50.degree.
  • the more readily soluble components such as the short-chain lipids are present in dissolved form in the extractant, while the fraction of poorly soluble components such as the long-chain lipids and the valuable substances are undissolved in the preconcentrate separator 13.
  • the density difference of the two fractions leads to the formation of two phases - in the extractant, the more readily soluble components such as short-chain lipids as the first phase and undissolved sparingly soluble components such as long-chain lipids and recyclables as the second phase.
  • the first of the above-described loaded phases subsequently rises due to their clotting ⁇ cal density upwards and is withdrawn there via the discharge opening 14.
  • the selected pressure and temperature level ensures makes a sufficient density difference between the two phases.
  • the Austragsöff sion 14 is connected via the line 15 with a separator system, which consists of two preconcentrator downstream of the precipitators 16 and 17.
  • the line 15 further has a throttle valve 18 which controls the extractant flow as needed.
  • the respective pressure level in the downstream separators 16 and 17 is gradually reduced, the separator 16 having an internal pressure of for example 90-120 bar and the separator 17 having an internal pressure of, for example, only 40-60 bar.
  • the two separators 16 and 17 are connected to one another via the line 19, wherein the pressure of the loaded extractant in separator 16 is regulated by a further throttle valve 20 and an increase of the temperature and / or an evaporation of the extractant is achieved via the heat exchanger 21 ,
  • the control valves 24 and 25 By means of the control valves 24 and 25, the sparingly soluble components such as triglycerides and recyclables separated by the extractant can be withdrawn via the lines 22 and 23, the now unloaded extractant being fed again to the storage container 1 via line 35 and with the interposition of a condenser 27.
  • the storage tank 1 reached extractant thus has at this time already back at the right temperature and the right pressure to become again the procedure applied ⁇ leads.
  • the unresolved fraction of valuable substances (the preconcentrate) remaining after discharge of the feed of liquid raw material into the preconcentrate separator 13 is removed via the discharge opening 26.
  • the concentrate thus obtained is thus introduced into the line 28 and reaches the final concentrate separator 29, from which the final concentrate is subsequently transported via the discharge opening 30 in line 31, wherein the withdrawal can be controlled via a control valve 32.
  • the pressure in Endkonzentratabscheider 29 is adjusted by means of a control valve 50.
  • the continuous process includes a further line 36, in which the extraction agent is compressed by the use of the motor-driven pump 38 and brought to the desired pressure level.
  • a pre-pressure pump 37 or a pre-cooler in line 36 is installed.
  • the heat exchanger 39 ensures that the compressed extractant to bring to the desired temperature.
  • the continuous process includes an extractor 40 and downstream of the preconcentrator 13 another arranged between Vorkonzentratabscheider 13 and the downstream extractor 40 mixing device 41.
  • the withdrawn from the Vorkonzentratabscheider 13 via line 28 amount can be controlled by a level measurement in Vorkonzentratabschei- 13 and / or a corresponding pump 51.
  • the discharge opening 26 together with line 28 and the line 36 open into the mixing device 41, where a renewed intensive mixing of the withdrawn from the Vorkonzentratabscheider 13 preconcentrate and the extraction agent from line 36 takes place.
  • the mixture thus obtained is fed in the sequence in the downstream extractor 40.
  • a predominantly increased pressure - in nachge ⁇ switched extractor 40 is either the same pressure as in the upstream Vorkonzentratabscheider 13 prevails.
  • the less soluble components thus dissolve in the extractant while the fraction of recyclables and higher polar components remain undissolved in the downstream extractor 40.
  • the density difference of the two fractions leads, as already described above, to the formation of two phases.
  • the first phase loaded with the additional components to be removed increases and is withdrawn via the further discharge opening 49 from the downstream extractor 40.
  • the remaining in the downstream extractor 40 unresolved fraction of recyclables and higher polar components is withdrawn via the discharge port 42 and spent in the line 43, this can be regulated again via a throttle valve 44 and then reaches the Endkonzentratabscheider 45, which with eg 10 bar internal pressure has a substantially lower pressure than the extractor 40.
  • the final concentrate is withdrawn via line 46 from the Endkonzentratabscheider 45, wherein this is again regulated via a throttle valve 47, while any remaining amount of extractant is returned via the discharge opening 48 in the storage container 1.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

L'invention concerne un procédé d'enrichissement de substances de valeur, en particulier de produits phytochimiques tels que, par exemple, des polyphénols, des colorants, des antioxydants et similaires, à partir d'une matière première liquide telle que, par exemple, des lipides, des bouillons de fermentation ou des produits extraits par solvants. Dans un dispositif mélangeur (5), la matière première est mélangée avec un agent d'extraction comprimé, en particulier du CO2, provenant d'un réservoir (1). Le mélange est ensuite amené dans un séparateur de préconcentré (13) où les composants plus facilement solubles dans l'agent d'extraction sont séparés des constituants non dissous. L'agent d'extraction chargé est soutiré du séparateur de préconcentré (13), les constituants non dissous demeurant en tant que préconcentré. L'agent d'extraction chargé passe dans un système séparateur dans lequel les substances dissoutes sont séparées de l'agent d'extraction chargé et l'agent d'extraction épuré est renvoyé dans le réservoir (1).
PCT/AT2014/000006 2013-02-07 2014-01-14 Procédé d'enrichissement de substances de valeur à partir d'une matière première liquide Ceased WO2014121311A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
MX2015010196A MX2015010196A (es) 2013-02-07 2014-01-14 Procedimiento de enriquecimiento de sustancias valiosas a partir de una materia prima liquida.
EP14705694.9A EP2953699A1 (fr) 2013-02-07 2014-01-14 Procédé d'enrichissement de substances de valeur à partir d'une matière première liquide

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ATA101/2013A AT513907B1 (de) 2013-02-07 2013-02-07 Verfahren zur Anreicherung von Wertstoffen aus einem flüssigen Rohstoff
ATA101/2013 2013-02-07

Publications (1)

Publication Number Publication Date
WO2014121311A1 true WO2014121311A1 (fr) 2014-08-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/AT2014/000006 Ceased WO2014121311A1 (fr) 2013-02-07 2014-01-14 Procédé d'enrichissement de substances de valeur à partir d'une matière première liquide

Country Status (4)

Country Link
EP (1) EP2953699A1 (fr)
AT (1) AT513907B1 (fr)
MX (1) MX2015010196A (fr)
WO (1) WO2014121311A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104927665A (zh) * 2015-05-20 2015-09-23 山东天博食品配料有限公司 一种利用超临界二氧化碳萃取发酵辣椒制备辣椒油树脂的方法
JP2019141829A (ja) * 2018-02-23 2019-08-29 国立研究開発法人産業技術総合研究所 マイクロ混合器を用いた高圧二酸化炭素による液液抽出方法及び装置

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Publication number Priority date Publication date Assignee Title
CN111921228B (zh) * 2020-07-29 2022-05-17 邹林宏 一种超声强化超临界流体萃取方法

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US4770780A (en) * 1984-04-25 1988-09-13 Cf Systems Corporation Liquid CO2 /cosolvent extraction
EP1258275A2 (fr) * 1996-12-06 2002-11-20 Advanced Phytonics Limited Dispositif de traitement de matériaux
US6589422B2 (en) * 2000-12-18 2003-07-08 Ineos Fluor Holdings Limited Apparatus and method for extracting biomass
WO2004018070A1 (fr) 2002-08-26 2004-03-04 Natex Prozesstechnologie Gesmbh Procede et dispositif d'extraction de substances contenues dans des liquides ou dispersions de matieres solides

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GB769454A (en) * 1953-08-24 1957-03-06 Herbert Peter August Groll Fractionation of oils or other soluble mixtures of organic substances by selective extraction
US4770780A (en) * 1984-04-25 1988-09-13 Cf Systems Corporation Liquid CO2 /cosolvent extraction
EP1258275A2 (fr) * 1996-12-06 2002-11-20 Advanced Phytonics Limited Dispositif de traitement de matériaux
US6589422B2 (en) * 2000-12-18 2003-07-08 Ineos Fluor Holdings Limited Apparatus and method for extracting biomass
WO2004018070A1 (fr) 2002-08-26 2004-03-04 Natex Prozesstechnologie Gesmbh Procede et dispositif d'extraction de substances contenues dans des liquides ou dispersions de matieres solides

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104927665A (zh) * 2015-05-20 2015-09-23 山东天博食品配料有限公司 一种利用超临界二氧化碳萃取发酵辣椒制备辣椒油树脂的方法
JP2019141829A (ja) * 2018-02-23 2019-08-29 国立研究開発法人産業技術総合研究所 マイクロ混合器を用いた高圧二酸化炭素による液液抽出方法及び装置
JP7051088B2 (ja) 2018-02-23 2022-04-11 国立研究開発法人産業技術総合研究所 マイクロ混合器を用いた高圧二酸化炭素による液液抽出方法及び装置

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Publication number Publication date
AT513907A1 (de) 2014-08-15
AT513907B1 (de) 2015-01-15
EP2953699A1 (fr) 2015-12-16
MX2015010196A (es) 2016-04-28

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