EP1913122B1 - Method for obtaining natural oils from plant constituents - Google Patents

Method for obtaining natural oils from plant constituents Download PDF

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Publication number
EP1913122B1
EP1913122B1 EP06776628A EP06776628A EP1913122B1 EP 1913122 B1 EP1913122 B1 EP 1913122B1 EP 06776628 A EP06776628 A EP 06776628A EP 06776628 A EP06776628 A EP 06776628A EP 1913122 B1 EP1913122 B1 EP 1913122B1
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Prior art keywords
extraction
oils
residues
oil
carried out
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German (de)
French (fr)
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EP1913122A1 (en
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Johann Wiesmüller
Stephan Pilz
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Evonik Operations GmbH
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Evonik Degussa GmbH
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction

Definitions

  • the present invention is a process for the extraction of natural oils from plant constituents by extraction with the aid of compressed gases.
  • Natural oils are increasingly important starting materials for the production of protective and care products of the cosmetic industry. In the health sector, they are increasingly used, with z. B. the allergen treatment is to call.
  • the advantage of natural oils is especially that they are ingredients of renewable raw materials, which makes them appear extremely valuable from an ecological and economic point of view.
  • the use of natural ingredients significantly increases consumer acceptance, as the consumer community now has a high level of environmental awareness and selects products for body and health care very critically.
  • oils are generally understood to mean lipophilic substance mixtures of (semi-) liquid consistency.
  • Natural oils of plant origin are usually mixtures of phytohormones, isoflavonoids, phytosterols, terpenoids, lipophilic vitamins (tocopherols) and short-chain fatty acid esters. These oils are thus typical natural products.
  • a strict delimitation of vegetable oils due to the components involved in their construction can be made only limited and is usually not required.
  • Vegetable oils and especially apple oils are already used by the Cosmetics industry used in a variety of applications and in particular in skin and hair care products.
  • the raw material source for these exemplary apple oils are mainly pomace, ie more or less dried residues from the apple juice or pectin production.
  • the apple oils contained in this pomace usually come from the seeds of juice apples. After first the pomace sieved for nuclear production and from the remaining residue, the fruit waxes have been separated, the apple oil is usually obtained from the pressed apple seed with the aid of a solvent. This raw material is accessible without further transformation, d. H. it can be purified and recovered by purely physical methods such as adsorption, filtration and distillation. The residue from the core oil production can be used, as usually the total pomace as cattle feed.
  • US 4,331,695 describes a process for recovering oils by extracting a vegetable or animal material with a solvent under subcritical conditions and separating the oil from the extract by heating above the critical temperature.
  • the document discloses inter alia extraction of olive kernels with isobutane at a temperature of 120 ° C and a pressure of 37 atm.
  • DE 44 05 127 describes hair treatment compositions containing a vegetable oil such as almond oil or peach kernel oil.
  • WO 01/37792 describes cosmetic compositions containing rice starch, coconut powder, oil or butter and shea butter and which may additionally contain grape seed oil. The two documents do not describe how the vegetable oils were obtained.
  • the object of the present invention is to provide a new process for the extraction of natural oils from plant constituents by extraction with the aid of compressed C 2 -C 4 hydrocarbons, which meets the further increased requirements by the processing Industry and by the consumer.
  • the new process should be as commercially feasible as possible and provide natural oils from untypical starting materials in improved quality.
  • residues from fruit and fruit processing with regard to the starting material, in particular residues from the processing of fruit kernels and berries and particularly preferably from juice production being suitable.
  • residues of apples, pears, citrus fruits such as tangerine, orange or lemons, melons, squash, raspberries, blackberries, elderberries and / or currants may be used as starting materials, the residues being principally large in nuclei, e.g. Contents of ⁇ 50 wt .-% and in particular ⁇ 90 wt .-%, should have.
  • the water content of the extraction material is preferably ⁇ 15% by weight and in particular ⁇ 10% by weight.
  • suitable starting materials are also bark pieces, leaves, stems and lignified tissue of subterranean and above-ground parts of plants which all oil cells may have. These residues must only be pre-shredded and possibly washed.
  • the present invention takes into account ethane, propane and butane and mixtures thereof.
  • the compressed hydrocarbon (mixture) used in each case as extractant and entrainer such as dimethyl ether and alcohols are added, which then preferably in proportions of 0.5 to 50 wt .-% are used.
  • the present invention recommends pressures of ⁇ 50 MPa and temperatures of ⁇ 70 ° C, with a pressure range between 0.5 and 10 MPa and temperatures between 20 and 35 ° C are considered to be particularly preferred.
  • the process of the present invention should be carried out with an extractant throughput of 4 to 20 kg / kg of starting material, with a throughput of between 5 and 10 kg / kg of starting material being preferred.
  • the respective extracts are usually deposited by a pressure reduction to 5 to 10 bar at temperatures between 42 and 48 ° C.
  • the proposed method can also be carried out continuously;
  • the invention provides for the method to be carried out in batches, since in this way the process parameters can be adapted to the particular starting material, its composition and composition in an easily comprehensible manner.
  • the present invention also claims the use of a vegetable oil extracted by the proposed method in cosmetic preparations and in particular as a flavoring or for the care and treatment of the skin and its appendages, including above all hair and foot and fingernails to understand are.
  • skin in the context of the present invention, of course, initially the skin itself, but also mucous membranes and the skin appendages to understand if they include living cells.
  • hair follicles, hair roots, hair bulbs and the ventral epithelium of the nail bed, sebaceous glands and sweat glands are to be understood here.
  • the use according to the invention comprises the care as well as the therapeutic and non-therapeutic treatment, which includes above all the aromatherapy.
  • kernels which contain natural fruit and aroma oils are typically obtained as sieve residue.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Cosmetics (AREA)
  • Medicines Containing Plant Substances (AREA)

Description

Gegenstand der vorliegenden Erfindung ist ein Verfahren zur Gewinnung von natürlichen Ölen aus pflanzlichen Bestandteilen durch Extraktion mit Hilfe verdichteter Gase.The present invention is a process for the extraction of natural oils from plant constituents by extraction with the aid of compressed gases.

Natürliche Öle stellen zunehmend wichtige Ausgangsmaterialien für die Herstellung von Schutz- und Pflegeprodukten der kosmetischen Industrie dar. Auch im Gesundheitsbereich finden sie vermehrt Anwendung, wobei z. B. die Allergenbehandlung zu nennen ist. Der Vorteil natürlicher Öle ist insbesondere darin zu sehen, dass es sich dabei um Inhaltsstoffe nachwachsender Rohstoffe handelt, was sie unter ökologischen und ökonomischen Gesichtspunkten als äußerst wertvoll erscheinen lässt. Zudem steigt durch die Anwendung natürlicher Inhaltsstoffe die Verbraucherakzeptanz deutlich an, da die Verbraucherschaft zwischenzeitlich ein ausgeprägtes ökologisches Bewusstsein besitzt und Produkte für die Körper- und Gesundheitspflege äußerst kritisch auswählt.Natural oils are increasingly important starting materials for the production of protective and care products of the cosmetic industry. In the health sector, they are increasingly used, with z. B. the allergen treatment is to call. The advantage of natural oils is especially that they are ingredients of renewable raw materials, which makes them appear extremely valuable from an ecological and economic point of view. In addition, the use of natural ingredients significantly increases consumer acceptance, as the consumer community now has a high level of environmental awareness and selects products for body and health care very critically.

Speziell im Bereich der natürlichen Öle werden unterschiedliche Begriffe verwendet, wobei man unter Ölen nach allgemeinem Verständnis lipophile Substanzgemische von (halb-)flüssiger Konsistenz versteht. Bei natürlichen Ölen pflanzlicher Herkunft handelt es sich in der Regel um Gemische aus Phytohormonen, Isoflavonoiden, Phytosterolen, Terpenoiden, lipophilen Vitaminen (Tocopherole) und kurzkettigen Fettsäureestern. Diese Öle stellen somit typische Naturprodukte dar. Eine strenge Abgrenzung der pflanzlichen Öle aufgrund der an ihrem Aufbau beteiligten Komponenten kann nur beschränkt vorgenommen werden und ist auch meist nicht erforderlich.Especially in the field of natural oils, different terms are used, which oils are generally understood to mean lipophilic substance mixtures of (semi-) liquid consistency. Natural oils of plant origin are usually mixtures of phytohormones, isoflavonoids, phytosterols, terpenoids, lipophilic vitamins (tocopherols) and short-chain fatty acid esters. These oils are thus typical natural products. A strict delimitation of vegetable oils due to the components involved in their construction can be made only limited and is usually not required.

Pflanzliche Öle und insbesondere Apfelöle werden bereits von der Kosmetikindustrie in vielfältigen Anwendungsbereichen und insbesondere in Haut- und Haarpflegeprodukten eingesetzt.Vegetable oils and especially apple oils are already used by the Cosmetics industry used in a variety of applications and in particular in skin and hair care products.

Als Rohstoffquelle für diese beispielhaften Apfelöle dienen in der Hauptsache Trester, also mehr oder weniger getrocknete Rückstände aus der Apfelsaft- bzw. Pektinfabrikation. Die in diesem Trester enthaltenen Apfelöle entstammen meist den Kernen von Saftäpfeln. Nachdem zunächst der Trester zur Kerngewinnung abgesiebt und aus dem verbliebenem Rückstand die Fruchtwachse abgetrennt worden sind, wird in der Regel aus den gepressten Apfelkernen mit Hilfe eines Lösemittels das Apfelöl gewonnen. Dieses Rohmaterial ist ohne weiterreichende Stoffumwandlung zugänglich, d. h. es kann durch rein physikalisch wirkende Methoden wie bspw. Adsorption, Filtration und Destillation gereinigt und gewonnen werden. Der Rückstand aus der Kernölgewinnung kann, wie üblicherweise der Gesamttrester als Viehfutter eingesetzt werden.The raw material source for these exemplary apple oils are mainly pomace, ie more or less dried residues from the apple juice or pectin production. The apple oils contained in this pomace usually come from the seeds of juice apples. After first the pomace sieved for nuclear production and from the remaining residue, the fruit waxes have been separated, the apple oil is usually obtained from the pressed apple seed with the aid of a solvent. This raw material is accessible without further transformation, d. H. it can be purified and recovered by purely physical methods such as adsorption, filtration and distillation. The residue from the core oil production can be used, as usually the total pomace as cattle feed.

Die bereits angesprochene Isolierung der Kernöle erfolgt also bislang hauptsächlich mit Hilfe organischer Lösemitteln, die für die Lebensmittelbehandlung zugelassen sind. Da die Kosmetikindustrie zunehmend unabhängig vom jeweiligen Anwendungsgebiet reinere Produkte mit definiertem Komponentenspektrum fordert, ist die Extraktion v. a. auch unter wirtschaftlichen Gesichtspunkten mit organischen Lösemitteln jedoch nicht mehr ausreichend.So far, the above-mentioned isolation of the core oils takes place mainly with the help of organic solvents that are approved for food treatment. Since the cosmetics industry increasingly demands purer products with a defined component spectrum independent of the respective field of application, the extraction of v. a. However, from an economic point of view with organic solvents, not enough.

Wie bereits angedeutet, stellen natürliche Öle keine einheitliche Substanzklasse dar, sondern ein Gemisch verschiedener Stoffklassen. Aufgrund der überwiegend lipophilen Zusammensetzung der bislang für die Kernölgewinnung eingesetzten Presskerne und der bekannten unbedenklichen Eigenschaften von Kohlendioxid wäre der Einsatz von überkritischem CO2 das Verfahren der Wahl. Allerdings haben die nachteiligen Verfahrensbedingungen wie hohe Drücke und ein hoher CO2-Durchsatz sowie eine geringe Selektivität zu enttäuschenden Ergebnissen geführt.As already indicated, natural oils are not a single substance class but a mixture of different classes of substances. Due to the predominantly lipophilic composition of the press cores hitherto used for the production of nuclear oil and the known harmless properties of carbon dioxide, the use of supercritical CO 2 would be the method of choice. However, the adverse process conditions such as high pressures and high CO 2 throughput and low selectivity have led to disappointing results.

Aus dem europäischen Patent EP 591 981 B1 ist bereits ein Verfahren zur Extraktion von Fetten und Ölen aus Naturstoffen bekannt, das mit Hilfe von flüssigem Propan als Lösemittel durchgeführt wird und bei dem auf fett- oder ölhaltige Naturstoffe u. a. auf pflanzlicher Basis als Ausgangsmaterial zurückgegriffen wird. Als Beispiele für pflanzliche Öle sind Olivenöl, Palmöl, Rapsöl, Flachsöl und Öl von Sonnenblume, Weizen- und Reiskeimen sowie Baumwollsaaten, Soja- und Palmkernen genannt. Die diesbezüglich durchgeführte Extraktion mit flüssigem Propan wird in einem sehr engen und definierten Druck- und Temperaturbereich durchgeführt, der bei 10 bis 30 bar und 10 bis 55 °C liegt, da bei Drücken > 30 bar, insbesondere bei der Extraktion von Ölsaaten, die Extraktionseigenschaften des flüssigen Propans zunehmend unselektiv werden. Bei dem in diesem Patent beschriebenen Verfahren werden somit pflanzliche Naturstoffe extrahiert, bei denen es sich um typische Quellen für pflanzliche Öle, wie Oliven, Palmkerne, Raps, Flachs, Sonnenblumenkerne und Weizen- bzw. Reiskeime handelt.From the European patent EP 591 981 B1 Already known is a process for the extraction of fats and oils from natural substances, which is carried out with the aid of liquid propane as a solvent and in which fat or oil-containing natural substances, inter alia, based on plant-based starting material is used. Examples of vegetable oils are olive oil, palm oil, rapeseed oil, flax oil and sunflower oil, wheat and rice germs, as well as cottonseed, soya and palm kernels. The extraction with liquid propane carried out in this respect is carried out in a very narrow and defined pressure and temperature range, which is 10 to 30 bar and 10 to 55 ° C, because at pressures> 30 bar, especially in the extraction of oilseeds, the extraction properties of liquid propane become increasingly unselective. The process described in this patent thus extracts plant natural products which are typical sources of vegetable oils such as olives, palm kernels, rape, flax, sunflower seeds and wheat or rice germs.

In diesem europäischen Patent EP 591 981 B1 wird auch auf weitere Dokumente aus dem Stand der Technik verwiesen, die die Verwendung von verdichtetem Propan für die Extraktion von Ölen vorbeschreiben. Gemäß DE-OS 28 43 920 werden rohe pflanzliche Fette und Öle mit überkritischen Gasen wie Propan und CO2 raffiniert. Gemäß US-PS 2,254,245 erfolgt eine Fettextraktion bei sehr niedrigen Temperaturen < 0 °C, während gemäß US-Patent 1,802,533 ein maximaler Extraktionsdruck von 7 bar empfohlen wird. Außerdem wird darauf verwiesen, dass kritische Zustandsparameter oftmals bei der Abscheidung der extrahierten Lipide gewählt werden, da auf diese Weise eine Phasentrennung in eine ölreiche und eine ölarme Propanphase ausgenutzt werden kann, um so das Öl abzutrennen oder zu fraktionieren ( US 2,660,590 oder US 2,548,434 ).In this European patent EP 591 981 B1 Reference is also made to other prior art documents which describe the use of compressed propane for the extraction of oils. According to DE-OS 28 43 920 Raw vegetable fats and oils are refined with supercritical gases such as propane and CO 2 . According to U.S. Patent 2,254,245 fat extraction takes place at very low temperatures <0 ° C, while according to U.S. Patent 1,802,533 a maximum extraction pressure of 7 bar is recommended. In addition, it is pointed out that critical state parameters are often chosen in the deposition of the extracted lipids, since in this way a phase separation into an oil-rich and a low-oil propane phase can be exploited, so as to separate off or fractionate the oil ( US 2,660,590 or US 2,548,434 ).

Alle zitierten Verfahren greifen auf Ausgangsmaterialien zurück, bei denen es sich um typische Quellen für natürliche Öle handelt, wobei immer wieder darauf hingewiesen wird, dass die jeweiligen Verfahrensparameter bei der Anwendung von verdichteten Kohlenwasserstoffen, wie bspw. Propan, so zu wählen sind, dass eine maximale Selektivität hinsichtlich der zu extrahierenden Öle erreicht wird. Die Gewinnung von pflanzlichen Ölen aus unspezifischen pflanzlichen Ausgangsmaterialien ist bislang noch nicht vorbeschrieben.All of the cited methods make use of starting materials which are typical sources of natural oils, again and again It should be noted that the particular process parameters in the application of compressed hydrocarbons, such as propane, are to be chosen so that a maximum selectivity is achieved with respect to the oils to be extracted. The production of vegetable oils from unspecific plant raw materials has not been previously described.

US 4,331,695 beschreibt ein Verfahren zur Gewinnung von Ölen durch Extraktion eines pflanzlichen oder tierischen Materials mit einem Lösungsmittel unter unterkritischen Bedingungen und Abscheiden des Öls aus dem Extrakt durch Erhitzen über die kritische Temperatur. Das Dokument offenbart unter anderem eine Extraktion von Olivenkernen mit Isobutan bei einer Temperatur von 120 °C und einem Druck von 37 atm. US 4,331,695 describes a process for recovering oils by extracting a vegetable or animal material with a solvent under subcritical conditions and separating the oil from the extract by heating above the critical temperature. The document discloses inter alia extraction of olive kernels with isobutane at a temperature of 120 ° C and a pressure of 37 atm.

DE 44 05 127 beschreibt Haarbehandlungsmittel, die ein Pflanzenöl, wie z.B. Mandelöl oder Pfirsichkernöl enthalten. WO 01/37792 beschreibt kosmetische Zusammensetzungen, die Reisstärke, Kokosnusspulver, -öl oder -butter und Sheabutter enthalten und die zusätzlich Traubenkernöl enthalten können. Die beiden Dokumente beschreiben nicht, wie die Pflanzenöle gewonnen wurden. DE 44 05 127 describes hair treatment compositions containing a vegetable oil such as almond oil or peach kernel oil. WO 01/37792 describes cosmetic compositions containing rice starch, coconut powder, oil or butter and shea butter and which may additionally contain grape seed oil. The two documents do not describe how the vegetable oils were obtained.

Aufgrund dieses Nachteils des Standes der Technik hat sich für die vorliegende Erfindung die Aufgabe gestellt, ein neues Verfahren zur Gewinnung von natürlichen Ölen aus pflanzlichen Bestandteilen durch Extraktion mit Hilfe verdichteter C2-C4-Kohlenwasserstoffe bereitzustellen, welches den weiter gesteigerten Anforderungen durch die verarbeitende Industrie und durch den Verbraucher gerecht wird. Das neue Verfahren soll auf möglichst einfache Weise kommerziell durchführbar sein und natürliche Öle aus untypischen Ausgangsmaterialien in verbesserter Qualität zur Verfügung stellen.Because of this disadvantage of the prior art, the object of the present invention is to provide a new process for the extraction of natural oils from plant constituents by extraction with the aid of compressed C 2 -C 4 hydrocarbons, which meets the further increased requirements by the processing Industry and by the consumer. The new process should be as commercially feasible as possible and provide natural oils from untypical starting materials in improved quality.

Gelöst wurde diese Aufgabe mit einem Verfahren, das bzgl. des Ausgangsmaterials auf Rückstände aus der Frucht- und Obstverarbeitung zurückgreift, wobei insbesondere Rückstände aus der Verarbeitung von Fruchtkernen und Beeren und besonders bevorzugt aus der Saftherstellung geeignet sind. Insbesondere Rückstände von Äpfeln, Birnen, Zitrusfrüchten, wie Mandarine, Orange oder Zitronen, Melonen, Kürbissen, Himbeeren, Brombeeren, Holundern und/oder Johannisbeeren kommen als Ausgangsmaterialien in Frage, wobei die Rückstände vor allem große Gehalte an Kernen, z.B. Gehalte von ≥ 50 Gew.-% und insbesondere ≥ 90 Gew.-%, aufweisen sollten. Der Wassergehalt des Extraktionsgutes beträgt vorzugsweise < 15 Gew.-% und insbesondere < 10 Gew.%.This problem has been solved by a process which makes use of residues from fruit and fruit processing with regard to the starting material, in particular residues from the processing of fruit kernels and berries and particularly preferably from juice production being suitable. In particular, residues of apples, pears, citrus fruits such as tangerine, orange or lemons, melons, squash, raspberries, blackberries, elderberries and / or currants may be used as starting materials, the residues being principally large in nuclei, e.g. Contents of ≥ 50 wt .-% and in particular ≥ 90 wt .-%, should have. The water content of the extraction material is preferably <15% by weight and in particular <10% by weight.

Geeignete Ausgangsmaterialien stellen aber auch Rindenstücke, Blätter, Stengel und verholztes Gewebe unter- und oberirdischer Pflanzenteile dar, die alle Ölzellen aufweisen können. Diese Rückstände müssen lediglich vorzerkleinert und evtl. gewaschen werden.However, suitable starting materials are also bark pieces, leaves, stems and lignified tissue of subterranean and above-ground parts of plants which all oil cells may have. These residues must only be pre-shredded and possibly washed.

In der Praxis hat sich herausgestellt, dass mit diesem neuen Verfahren gemäß Erfindung nicht nur die Aufgabenstellung erfüllt werden konnte, sondern, dass damit überraschenderweise natürliche Öle und insbesondere Kernöle in z. T. deutlich gesteigerten Ausbeuten aus pflanzlichen Rückständen gewonnen werden können. Diese Ausbeuten gehen zwar nicht regelmäßig über die Ausbeuten hinaus, wie sie mit Hilfe von organischen Lösemitteln gemäß Stand der Technik erhältlich sind; die erfindungsgemäß erhältlichen Öle weisen aber ein qualitativ hoch stehendes Inhaltsspektrum auf. Die mit dem erfindungsgemäßen Verfahren erhältlichen Öle sind insgesamt von einer Qualität, die sie neuen Anwendungsgebieten zugänglich machen.In practice, it has been found that with this new method according to the invention not only the task could be met, but that surprisingly natural oils and in particular core oils in z. T. significantly increased yields can be obtained from vegetable residues. Although these yields do not regularly exceed the yields obtainable with prior art organic solvents; However, the oils obtainable according to the invention have a high-quality content spectrum. The oils obtainable by the process according to the invention are overall of a quality which makes them accessible to new fields of application.

Als Extraktionsmittel berücksichtigt die vorliegende Erfindung Ethan, Propan und Butan sowie Mischungen daraus. Dabei können im Bedarfsfall, dem jeweils als Extraktionsmittel eingesetzten verdichteten Kohlenwasserstoff (-Gemisch) auch Schleppmittel wie Dimethylether und Alkohole zugesetzt werden, wobei diese dann vorzugsweise in Anteilen von 0,5 bis 50 Gew.-% zur Anwendung gelangen.As extracting agent, the present invention takes into account ethane, propane and butane and mixtures thereof. In this case, if necessary, the compressed hydrocarbon (mixture) used in each case as extractant and entrainer such as dimethyl ether and alcohols are added, which then preferably in proportions of 0.5 to 50 wt .-% are used.

Hinsichtlich der Extraktionsparameter empfiehlt die vorliegende Erfindung Drücke von < 50 MPa und Temperaturen von ≤ 70 °C, wobei ein Druckbereich zwischen 0,5 und 10 MPa und Temperaturen zwischen 20 und 35 °C als besonders bevorzugt angesehen werden.With regard to the extraction parameters, the present invention recommends pressures of <50 MPa and temperatures of ≤ 70 ° C, with a pressure range between 0.5 and 10 MPa and temperatures between 20 and 35 ° C are considered to be particularly preferred.

In Abhängigkeit vom jeweiligen Ausgangsmaterial (bspw. dessen Feuchtigkeitsgehalt) sollte das Verfahren gemäß vorliegender Erfindung mit einem Extraktionsmitteldurchsatz von 4 bis 20 kg/kg Ausgangsmaterial durchgeführt werden, wobei ein Durchsatz als bevorzugt angesehen wird, der zwischen 5 und 10 kg/kg Ausgangsmaterial liegt.Depending on the particular starting material (eg its moisture content), the process of the present invention should be carried out with an extractant throughput of 4 to 20 kg / kg of starting material, with a throughput of between 5 and 10 kg / kg of starting material being preferred.

Die jeweiligen Extrakte werden üblicherweise durch eine Druckabsenkung auf 5 bis 10 bar bei Temperaturen zwischen 42 und 48 °C abgeschieden.The respective extracts are usually deposited by a pressure reduction to 5 to 10 bar at temperatures between 42 and 48 ° C.

Zwar kann das vorgeschlagene Verfahren auch kontinuierlich durchgeführt werden; aus praktischen Gründen sieht die Erfindung allerdings vor, das Verfahren batchweise durchzuführen, da so in leicht nachvollziehbarer Weise die Verfahrensparameter auf das jeweilige Ausgangsmaterial, dessen Beschaffenheit und Zusammensetzung abgestimmt werden können.Although the proposed method can also be carried out continuously; For practical reasons, however, the invention provides for the method to be carried out in batches, since in this way the process parameters can be adapted to the particular starting material, its composition and composition in an easily comprehensible manner.

Neben dem eigentlichen Verfahren selbst beansprucht die vorliegende Erfindung auch die Verwendung eines mit dem vorgeschlagenen Verfahren extrahierten pflanzlichen Öles in kosmetischen Zubereitungen und insbesondere als Aromastoff oder zur Pflege und Behandlung der Haut und deren Anhangsgebilden, worunter vor allen Dingen Haare und Fuß- sowie Fingernägel zu verstehen sind. Unter dem Begriff "Haut" sind im Rahmen der vorliegenden Erfindung natürlich zunächst die Haut selbst, aber auch Schleimhäute sowie die Hautanhangsgebilde zu verstehen, sofern diese lebende Zellen umfassen. Hier sind insbesondere Haarfollikel, Haarwurzel, Haarzwiebel sowie das ventrale Epithel des Nagelbetts, Talgdrüsen und Schweißdrüsen zu verstehen. Die erfindungsgemäße Verwendung umfasst die Pflege sowie die therapeutische und nicht-therapeutische Behandlung, was vor allem die Aromatherapie einschließt.In addition to the actual method itself, the present invention also claims the use of a vegetable oil extracted by the proposed method in cosmetic preparations and in particular as a flavoring or for the care and treatment of the skin and its appendages, including above all hair and foot and fingernails to understand are. The term "skin" in the context of the present invention, of course, initially the skin itself, but also mucous membranes and the skin appendages to understand if they include living cells. In particular, hair follicles, hair roots, hair bulbs and the ventral epithelium of the nail bed, sebaceous glands and sweat glands are to be understood here. The use according to the invention comprises the care as well as the therapeutic and non-therapeutic treatment, which includes above all the aromatherapy.

Mit dem neuen Verfahren zur Extraktion von natürlichen Ölen aus pflanzlichen Bestandteilen mit Hilfe von C2-C4-Kohlenwasserstoffen können natürliche Öle in verbesserter Qualität und gesteigerten Ausbeuten unter äußerst wirtschaftlichen Bedingungen aus Ausgangsmaterialien erhalten werden, die üblicherweise typische Abfallstoffe darstellen und nun als sekundäre Rohstoffe ihre Anwendung finden.With the new process for extracting natural oils from plant constituents using C 2 -C 4 hydrocarbons, natural oils of improved quality and yields can be obtained under extremely economical conditions from raw materials that are typically typical waste materials and now secondary raw materials find their application.

Das nachfolgende Beispiel belegt die Vorteile des beanspruchten Verfahrens.The following example demonstrates the advantages of the claimed method.

Beispielexample

Bei der Herstellung von Himbeersaft fallen typischerweise als Siebrückstand Kerne an, in denen sich natürliche Frucht- und Aromaöle befinden.In the production of raspberry juice, kernels which contain natural fruit and aroma oils are typically obtained as sieve residue.

Diese Kerne wurden vom restlichen Fruchtfleisch befreit, getrocknet und abschließend vermahlen. Die zerkleinerten Kerne werden dann in einem Autoklaven bei 30 bar und 35 °C mit flüssigem Propan extrahiert, wobei der Extraktionsmitteldurchsatz durchschnittlich 6,8 kg/kg Ausgangsmaterial betrug. Der so erhaltene Extrakt wurde nach erfolgter Druckabsenkung bei 8 bar und 46 °C abgeschieden.These kernels were freed from the remaining pulp, dried and finally ground. The crushed cores are then extracted in an autoclave at 30 bar and 35 ° C with liquid propane, the average extractor throughput being 6.8 kg / kg starting material. The resulting extract was deposited after pressure reduction at 8 bar and 46 ° C.

Auf diese Weise erhielt man einen gelb-grünen und klaren Himbeerkern-Ölextrakt in einer Ausbeute von etwa 14 %.In this way, a yellow-green and clear raspberry seed oil extract was obtained in a yield of about 14%.

Claims (9)

  1. Method for obtaining natural oils from plant constituents by extraction by means of compressed C2-C4-hydrocarbons, characterized in that residues from the processing of fruit pips and berries are used as starting material and the extraction is carried out at pressures of < 50 MPa and temperatures of ≤ 70°C.
  2. Method according to Claim 1, characterized in that residues from the production of juice are used.
  3. Method according to Claim 1 or 2, characterized in that the residues originate from the processing of apples, pears, citrus fruits, such as mandarins, oranges or lemons, melons, pumpkins, raspberries, blackberries, elderberries and/or currants.
  4. Method according to any one of Claims 1 to 3, characterized in that ethane, propane and butane, and mixtures thereof are used as extraction agent.
  5. Method according to any one of Claims 1 to 4, characterized in that the pressure is adjusted to 0.5 to 10 MPa and the temperature is adjusted to 20 to 35°C.
  6. Method according to any one of Claims 1 to 5, characterized in that entrainers such as dimethyl ether and alcohols are added to the compressed hydrocarbon mixture, preferably in amounts of from 0.5 to 50% by weight.
  7. Method according to any one of Claims 1 to 6, characterized in that the extraction is carried out with an extraction agent throughput of from 4 to 20 kg/kg of starting material and preferably 5 to 10 kg/kg.
  8. Method according to any one of Claims 1 to 7, characterized in that it is carried out batchwise.
  9. Use of an oil obtained by the method according to Claims 1 to 8 in cosmetic preparations, in particular as aroma substance and for the care of the skin and appendages thereof.
EP06776628A 2005-08-06 2006-08-04 Method for obtaining natural oils from plant constituents Not-in-force EP1913122B1 (en)

Applications Claiming Priority (2)

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DE102005037209A DE102005037209A1 (en) 2005-08-06 2005-08-06 Process for the extraction of natural oils from plant constituents
PCT/EP2006/007757 WO2007017206A1 (en) 2005-08-06 2006-08-04 Method for obtaining natural oils from plant constituents

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EP1913122A1 EP1913122A1 (en) 2008-04-23
EP1913122B1 true EP1913122B1 (en) 2012-10-03

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DE (1) DE102005037209A1 (en)
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DE102007033907A1 (en) * 2007-07-20 2009-01-22 Uhde High Pressure Technologies Gmbh Natural Product Extraction
DE102008042923A1 (en) 2008-10-17 2010-04-22 Evonik Goldschmidt Gmbh Preparations for the controlled release of active substances
JP5584863B2 (en) * 2009-02-26 2014-09-10 地方独立行政法人青森県産業技術センター Apple Incense Incense
US9687754B2 (en) 2013-01-04 2017-06-27 Matthew Ellis Apparatus for extracting oil from oil-bearing plants
US10053648B2 (en) 2013-01-04 2018-08-21 Matthew Ellis Continuous-flow extraction system and method
EP3175897B1 (en) * 2015-12-04 2018-04-04 Evonik Degussa GmbH Improved method for the extraction of aromatic substances from fat-containing and/or aqueous liquid phases
CN110382675A (en) * 2017-02-03 2019-10-25 西姆莱斯股份公司 For reappearing the method and detection kit of a kind of smell

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AT331374B (en) * 1972-12-22 1976-08-25 Studiengesellschaft Kohle Mbh PROCESS FOR THE PRODUCTION OF FATS AND OILS FROM VEGETABLE AND ANIMAL PRODUCTS
EP0092076B1 (en) * 1982-04-16 1986-12-17 Societe Des Produits Nestle S.A. Lipid composition for oral, enteral or parenteral feeding
US5041245A (en) * 1989-03-10 1991-08-20 Bioseparations, Inc. Continuous extraction of oil-containing vegetable matter with pressurized normally gaseous solvent
US5281732A (en) * 1991-12-31 1994-01-25 University Research & Marketing Solvent extraction of oil from oil-bearing materials
US5405633A (en) * 1992-10-08 1995-04-11 Skw Trostberg Aktiengesellschaft Process for the extraction of fats and oils
DE4405127A1 (en) * 1994-02-18 1995-08-31 Henkel Kgaa Hair treatment products
NO955076D0 (en) * 1994-12-17 1995-12-14 Sueddeutsche Kalkstickstoff Process for selective extraction of fat and / or oils from solids
DE4447116A1 (en) * 1994-12-29 1996-07-04 Sueddeutsche Kalkstickstoff Process for the fractionation or refining of lipid natural products
FR2801505B1 (en) * 1999-11-26 2002-02-01 Arnaud Ruel DERMO-COSMETOLOGICAL COMPOSITION OF CARE COMPRISING AMONG OTHERS RICE STARCH, COCONUT OIL AND SHEA BUTTER

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US20090028971A1 (en) 2009-01-29
JP2009504816A (en) 2009-02-05
AU2006278798C1 (en) 2011-08-04
ZA200801251B (en) 2008-10-29
WO2007017206A1 (en) 2007-02-15
EP1913122A1 (en) 2008-04-23
KR20080038205A (en) 2008-05-02
NZ565407A (en) 2010-09-30
AU2006278798A1 (en) 2007-02-15
CA2618509A1 (en) 2007-02-15
DE102005037209A1 (en) 2007-02-08

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