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WO2002004580A1 - Procede d'extraction - Google Patents

Procede d'extraction Download PDF

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Publication number
WO2002004580A1
WO2002004580A1 PCT/EP2001/008301 EP0108301W WO0204580A1 WO 2002004580 A1 WO2002004580 A1 WO 2002004580A1 EP 0108301 W EP0108301 W EP 0108301W WO 0204580 A1 WO0204580 A1 WO 0204580A1
Authority
WO
WIPO (PCT)
Prior art keywords
solvent
extraction
oils
chamber
process according
Prior art date
Application number
PCT/EP2001/008301
Other languages
English (en)
Inventor
John Henry Davis
Original Assignee
Country Roads Seating Inc.
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 Country Roads Seating Inc. filed Critical Country Roads Seating Inc.
Priority to AU2001272549A priority Critical patent/AU2001272549A1/en
Publication of WO2002004580A1 publication Critical patent/WO2002004580A1/fr

Links

Classifications

    • 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
    • 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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting

Definitions

  • This invention relates to an extraction process, and in particular to the solvent-based extraction of essential oils from natural products.
  • the present invention is based on the discovery that solvent extraction is especially effective if conducted using pulses of solvent, and that the resultant extracts are of particularly high quality.
  • solvent extraction is especially effective if conducted using pulses of solvent, and that the resultant extracts are of particularly high quality.
  • a pulse or 'slug' of solvent into a relatively warm extraction chamber, more effective extraction is achieved than if there is no difference in temperature.
  • an explanation for this effect may be that the leading edge of the plug goes into the gas phase, giving supercritical extraction, followed by cold solvent extraction. Description of the Invention
  • the solvent that is used in the invention may be any organic compound that is a solvent for the desired extract. It will usually be a gas under ambient conditions. Whereas C0 2 sublimes at -78.5°C (760 mm Hg pressure), a gas used in the present invention may liquefy at a temperature above -60°C and/or below 0°C.
  • suitable extractants for use in the invention are hydrocarbon gases such as butane, propane and analogous gases with similar physical properties, or halocarbon variants such as the Freons.
  • hydrocarbon gases such as butane, propane and analogous gases with similar physical properties
  • halocarbon variants such as the Freons.
  • Hydrocarbons and halocarbons are readily available, and their use does not require that the extraction apparatus should withstand such high pressures as for scC0 2 .
  • the apparatus can therefore be constructed cheaply and simply. Further, the reduced costs and reduced complexity of the novel method give it a much wider variety of uses in the preparation of flavourings, nutraceutical extracts, cosmetic extracts etc.
  • This invention can be used to extract extractant-soluble material from a wide variety of samples. These include plants such as flowers, vegetables, fruit and seeds, and foodstuffs.
  • the sample may be fresh or dried.
  • plants from different species are combined in the extraction chamber together to be extracted as one, the oils may undergo a reaction in the chamber, and combined to produce new molecules of a completely new oil.
  • the new oils may exhibit different crystal formations than either of the original oils, and cannot be separated into the original oils.
  • the drawings are an exploded view of an extraction chamber comprising a well casing-type tube 1 having an O-ring 2 at its upper end, above which may be placed a cover 3A or 3B having an compressed air inlet 4 (for the PSCE variant described below), a gas (extractant) nozzle/venturi inlet 5 and a pressure gauge 6; at its lower end, there are an oil collection chamber 7 having an outlet drain 8 and, separating the chamber from the tube, an O-ring 9 and a filter base plate 10.
  • the collection chamber should have a valve on it for collecting the gas from the extracts.
  • the chamber should be valved from the extraction pipe as well. If a clear hose can be used between the two, the colour of the liquid gas can be seen. This is utilised, to determine if extraction is complete.
  • the ends of the pipe may be removed for insertion and removal of spent materials.
  • the sample from which the oil fractions are to be removed is placed in the extraction chamber, which is typically in the form of an upright cylinder, and which is typically made of metal, preferably stainless steel.
  • the extraction chamber may be of almost any dimension, from as small as a few cm 3 in cases where extractions are to be made from rare, precious or test samples, to chambers large enough to contain 1 tonne or more of sample material, for full-scale commercial/industrial applications. Plants have already been built at both these scales, and found to operate equally efficiently in a wide range of ambient temperatures. Further, suitable apparatus may be made portable, e.g. for use in the field to check for the best time for oil harvest from oil plants, seeds, roots, leaves etc.
  • the sample in as tightly as possible, and this can be done by tamping, or by using an air or hydraulic ram or similar technique. It is generally easier to pack the sample material in from the top, pushing it down to the base where it may be retained by a (removable) filter base-plate. This is typically a stainless steel disc with perforations too small to allow the material through, but large enough to permit passage of the oil fraction.
  • the carrier/solvent gas e.g. butane, in gaseous or in liquid pressurised form, is pumped or gravity fed into the extraction chamber through the gas inlet, e.g. at a pressure of 0 to 100 bar, preferably 0 to 5 bar. It enters the extraction chamber through a venturi nozzle which is designed to allow a degree of liquid- to-gas transformation, so that significant adiabatic cooling takes place.
  • the cold gas flows down through the column, freezing the sample, and the remaining liquid carrier/solvent more or less simultaneously dissolves out all lipid and lipid- soluble elements ('the oils').
  • the liquid gas carrier/solvent with its load of dissolved oils flows down to the base of the extraction chamber, where controlled warming is applied, typically with a water circuit.
  • the wave of cooling which passes down through the extraction chamber may be important, as it can cause freezing of aqueous components in the sample material and thereby prevent them from flowing out together with the oils. This prevents the formation of oil-water mixtures or emulsions which may be unstable, and which may contain substances which could lead to degradation of the oils.
  • the freezing, and the consequent retention of the aqueous phase also make it possible to extract from fresh source material, with consequent improvements in the profile of the extract.
  • the cooling may also be critical in capturing volatiles and thermo-labile components in the sample material; such components include ketones, esters and aldehydes which might otherwise be lost and/or destroyed in steam distillation or when other solvents are used with higher boiling points, are captured in the oils.
  • the oils may be allowed to stand for a short time at room temperature, to allow any remaining traces of dissolved carrier/solvent to evaporate, before being decanted into more permanent storage. If the residue is particularly viscous, a partial vacuum may be used, to accelerate removal of the carrier.
  • the warming circuit is attached to the collection chamber. In this variant, the solvent/carrier liquid and its load of dissolved oils pass out of the extraction chamber into the collection chamber. Warming and/or a partial vacuum is then applied, causing the gas to evaporate, leaving the oils in the collection chamber.
  • Timing and pressure inside the extraction chamber should be controlled. Progress of the moving front of cooling and extraction as it passes down the extraction chamber should ideally be monitored; this can be done most simply (but quite effectively) by observation, and the inflow of liquid gas into the extraction chamber may be stopped when the frost which appears on the external surface of the extraction chamber reaches the bottom.
  • wavefronts of solvent are either supercritical fluid or liquid, or some combination of the two.
  • the pulsed variants described are termed pulsed liquid extraction (PLE), pulsed mixed extraction (PME), and pulsed supercritical fluid extraction (PSFE).
  • PLE, PME and PSFE have the twin advantages of using less solvent, which is important in non-enclosed systems (see section below re recycling of solvent); and achieving a high efficiency of extraction per unit of time.
  • Pressures and temperatures may need to be controlled and altered, depending on the characteristics of the sample which is being extracted, and on the solvent/carrier being used.
  • the depth, volume and frequency of the solvent slug are also important, and can be chosen by the operator. The optimal selection of these operating parameters may vary, but may be determined by one skilled in the art, and when properly employed, extraction is effectively total. Samples which have been subjected to a second pass in the extraction chamber typically yield little if any oils.
  • the extractant gas is allowed to vent off once the extraction is complete.
  • the controlled warming is allowed to progress until all the extractant has gasified, and vented out of the extraction and collection chambers, which can most easily be done via the original gas inlet.
  • the solvent is drawn off as a gas, it is absolutely pure, and contains no oils from the processed sample. It can then be recompressed for subsequent re-use.
  • the entire process acts not only as an oil-extracting system but also as a heat exchanger.
  • the heating and cooling sides of the gas/liquid compression/expansion cycle are used to modify the temperature of the environment where the process is taking place.
  • the process of the invention may be conducted in what is effectively a closed circuit, somewhat similar to a refrigeration circuit or heat exchanger.
  • the cooled liquid/gas mix freezes the organic matter, so that unwanted aqueous materials remain in situ.
  • the lipid-soluble elements in the sample are dissolved into the remaining liquid carrier/solvent, and flow to the bottom of the expansion chamber.
  • the solvent/solute mix is drawn off into a second collection chamber. In either case, controlled and slight warming is applied directly or indirectly to the solvent/solute mix.
  • the novel process has an additional advantage.
  • the oils Once the oils have been removed (from, for example, nuts), the remainder may be a low-calorie, fat-free nut, having good taste.
  • it can also be used as a decontamination procedure.
  • oils can be removed from contaminated materials, i.e. fouled oil filters, or sand or soil contaminated with oil spill or seepage. When these materials are processed, there is a very complete de-oiling. Indeed, oil-contaminated soil may become fertile once more; and the oils thus removed are generally sufficiently clean to be used for their original purposes.
  • the following experiments A and B were conducted in order to illustrate the merits of using pulsed extraction.
  • Timing of complete extraction may vary, depending on density of packed material in extraction column, but is typically between 5 and 20 minutes. In extreme cases, the extraction time may extend to a few hours. Running temperatures are typically between -5°C and +5 °C. The general principle of increased extraction efficiency holds through almost all of the above parametric range.
  • each pulse may reach saturation before it can dissolve out sufficient solute, and extraction efficiency declines.
  • the general principle that pulsing is better than a single pass
  • the volume of solvent used in a single pulse exceeds some threshold value so that it becomes effectively complete extraction.
  • the advantages of pulsed extraction disappear.
  • the single pass method requires higher volumes of solvent and longer processing times, and is less therefore less cost-effective.
  • the following rule of thumb may apply: Using a defined volume of solvent (e.g., 1000 ml), the most complete extraction of a material (e.g., 100 g) can be made by dividing the solvent into several smaller portions (e.g., 5 x200 ml each)and sequentially extracting, rather than using the entire volume to make one extract of the material. In practice, this means that the carrying capacity of the solvent will be more completely saturated with the first portion of extract and less so in the subsequent extracts. Without wishing to be bound by theory, this phenomenon may be related to the fact that a migration equilibrium of the active agent is established between the solvent and the ballast. The ballast is the source material from which the extraction is being made.

Landscapes

  • 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)
  • Extraction Or Liquid Replacement (AREA)

Abstract

Procédé d'extraction par solvant, d'huiles essentielles à partir d'un produit naturel, dans une chambre d'extraction, consistant à introduire des pulsations de solvant froid. La chambre peut être chaude par rapport au solvant, butane, par exemple.
PCT/EP2001/008301 2000-07-07 2001-07-06 Procede d'extraction WO2002004580A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001272549A AU2001272549A1 (en) 2000-07-07 2001-07-06 Extraction process

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0016827A GB0016827D0 (en) 2000-07-07 2000-07-07 Extraction process
GB0016827.8 2000-07-07

Publications (1)

Publication Number Publication Date
WO2002004580A1 true WO2002004580A1 (fr) 2002-01-17

Family

ID=9895298

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2001/008301 WO2002004580A1 (fr) 2000-07-07 2001-07-06 Procede d'extraction

Country Status (3)

Country Link
AU (1) AU2001272549A1 (fr)
GB (1) GB0016827D0 (fr)
WO (1) WO2002004580A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI500759B (fr) * 2014-10-15 2015-09-21
US9296979B1 (en) 2014-12-12 2016-03-29 Metal Industries Research & Development Centre Flower essential oil extraction method
US9649575B2 (en) 2014-09-03 2017-05-16 Hopkins Holdings Llc Organic oil extraction device

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1802533A (en) * 1928-09-13 1931-04-28 Columbia Engineering & Man Cor Extraction of oils
US2254245A (en) * 1934-08-04 1941-09-02 Rosenthal Henry Method and product of cottonseed extraction
EP0812903A1 (fr) * 1994-04-05 1997-12-17 Agritech International, L.L.C. Extraction d'huile à partir de parties de plantes oléagineuses
US5980964A (en) * 1998-06-18 1999-11-09 Gilroy Foods, D/B/A/Conagra Corporation Extraction of oil from oil bearing products with a chilled liquefied normally gaseous solvent
US6225483B1 (en) * 1998-06-01 2001-05-01 Henry L Franke Cold solvent extraction process for extracting oil from oil-bearing materials

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1802533A (en) * 1928-09-13 1931-04-28 Columbia Engineering & Man Cor Extraction of oils
US2254245A (en) * 1934-08-04 1941-09-02 Rosenthal Henry Method and product of cottonseed extraction
EP0812903A1 (fr) * 1994-04-05 1997-12-17 Agritech International, L.L.C. Extraction d'huile à partir de parties de plantes oléagineuses
US6225483B1 (en) * 1998-06-01 2001-05-01 Henry L Franke Cold solvent extraction process for extracting oil from oil-bearing materials
US5980964A (en) * 1998-06-18 1999-11-09 Gilroy Foods, D/B/A/Conagra Corporation Extraction of oil from oil bearing products with a chilled liquefied normally gaseous solvent

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9649575B2 (en) 2014-09-03 2017-05-16 Hopkins Holdings Llc Organic oil extraction device
TWI500759B (fr) * 2014-10-15 2015-09-21
US9296979B1 (en) 2014-12-12 2016-03-29 Metal Industries Research & Development Centre Flower essential oil extraction method

Also Published As

Publication number Publication date
GB0016827D0 (en) 2000-08-30
AU2001272549A1 (en) 2002-01-21

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