EP0967264A1 - Verfahren und Vorrichtung zur Extraktion von Öl aus Ölsaaten - Google Patents

Verfahren und Vorrichtung zur Extraktion von Öl aus Ölsaaten Download PDF

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Publication number
EP0967264A1
EP0967264A1 EP99390012A EP99390012A EP0967264A1 EP 0967264 A1 EP0967264 A1 EP 0967264A1 EP 99390012 A EP99390012 A EP 99390012A EP 99390012 A EP99390012 A EP 99390012A EP 0967264 A1 EP0967264 A1 EP 0967264A1
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EP
European Patent Office
Prior art keywords
oil
alcohol
seeds
phosphoric acid
twin
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Withdrawn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
EP99390012A
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English (en)
French (fr)
Inventor
Luc Rigal
Zéphirin Mouloungui
Corinne Lacaze-Dufaure
Antoine Gaset
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.)
Toulousaine De Recherche Et De Developpement "trd"
Original Assignee
Toulousaine De Recherche Et De Developpement "trd"
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 Toulousaine De Recherche Et De Developpement "trd" filed Critical Toulousaine De Recherche Et De Developpement "trd"
Publication of EP0967264A1 publication Critical patent/EP0967264A1/de
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B9/00—Presses specially adapted for particular purposes
    • B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
    • B30B9/12—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing
    • B30B9/16—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing operating with two or more screws or worms
    • 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
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • 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
    • C11B1/06—Production of fats or fatty oils from raw materials by pressing
    • 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
    • C11B1/102—Production of fats or fatty oils from raw materials by extracting in counter-current; utilisation of an equipment wherein the material is conveyed by a screw

Definitions

  • the invention relates to a process for extracting oil from oil seeds, in particular whole sunflower seeds.
  • Oileed means both seeds oilseeds per se (i.e. rich in triglycerides), that proteo-oil seeds (i.e. rich in triglycerides and proteins), and that seeds not specially known to be oilseeds but containing triglycerides.
  • seeds is meant any type of organ of a plant in which lipids are stored (seeds, beans, germs, seeds, almonds.). The invention extends to a device specially designed for putting of the process.
  • the first oil expressed by pressing is a quality oil called "virgin oil”, but the extraction yields of this virgin oil are limited (ceiling around 70% for an oil of first pressure); these yields increase slightly with an increase in temperature but the quality and stability of the oil obtained then decreases due to the degradation reactions which develop at the heart thereof and amplify considerably from 100 ° / 110 ° C.
  • Conventional refining operations essentially include a degumming operation to remove from the oil the gums which constitute the most troublesome and polluting by-products (J. Denise, "Degumming or degumming", The Refining of fatty substances, Les Editions du Beffrois, 1984, pp 55-60).
  • This degumming is generally obtained by an acid treatment of the oils extracted (most often by means of citric acid, or aqueous phosphoric acid or a mixture of the two). This acid treatment combined with washing with water ensures the precipitation and elimination of the gums by reacting with the Ca ++ or Mg ++ cations of the phospholipids responsible for said gums.
  • twin-screw devices comprising two co-penetrating screws for extracting oil by pressing oil seeds: WO 97/43113 and FR 2,747,128, for example, twin-screw devices for pressing seeds.
  • the present invention proposes to overcome the aforementioned drawbacks of conventional oil extraction processes.
  • the objective essential of the invention is to carry out an extraction of oil from the seeds single-stage oilseeds, with oil extraction yields of quality, far superior to first pressure process yields conventional or yields currently obtained by means of twin-screw devices.
  • Another objective is to remove the need for subsequent refining operations which increase the cost of extraction processes known or, in any case, to reduce the cost of these operations.
  • Another objective is to obtain a solid co-product much easier to develop than that from the pressing process traditional.
  • Another objective is to indicate a process likely to be implemented at milder temperature conditions than the processes in order to considerably limit the degradation reactions of oil.
  • the extraction process targeted by the invention is of the type in which the seeds are introduced into a twin-screw device comprising two co-penetrating screws rotating in a tubular enclosure in order to subject to a thermomechanical treatment, the liquid phase is drawn off containing the oil, and the remaining solid phase is collected;
  • the process according to the present invention is characterized in that a two-screw device is injected alcohol and phosphoric acid or a salt of this acid in order to combine with thermomechanical treatment chemical action of destructuring of lipids seed membranes.
  • the reactive medium must be poorly hydrated (equal hydration or lower than the natural hydration of the seeds), and alcohol and phosphoric acid used are advantageously anhydrous or poorly hydrated.
  • the proportion by weight of alcohol relative to with seeds is chosen to be substantially between 50% and 200% and the weight proportion of phosphoric acid or salt relative to said seeds is substantially between 5% and 50%.
  • These proportions correspond to a optimal efficiency of transport of phosphoric acid by alcohol and at a optimal effectiveness of the action of phosphoric acid.
  • the alcohol also participates in the extraction by its known role of solvent; however, taking into account the recommended proportions, this role of solvent is secondary, and the essential role of alcohol is to transport phosphoric acid which, by its destructuring action, prepares the seed for mechanical expression of the oil.
  • the process of the invention leads to oils of quality (quality equal to or better than first pressing oils) with much higher yields (around 90%).
  • This obtaining of an oil quality which does not require any refining operation can be explained by the phosphoric acid intervention mechanism (in the absence of added water): in an essentially organic medium, the phospholipids which constitute the most undesirable polluting compound combine with phosphoric acid and lead to a hydrophilic phosphorus complex which remains in the solid phase hydrophilic; the oil extracted, hydrophobic, is naturally free of this pollutant without further operation.
  • the temperature of the enclosure of the twin-screw device so as to adjust the temperature of the seed / alcohol / phosphoric acid or salt mixture within a range substantially between 50 ° C and 100 ° C.
  • This moderate temperature range leads with the above-mentioned excellent yields, without risk of parasitic reactions ( producing above 100 ° C / 110 ° C). This avoids the appearance of other products contaminants (resulting in reduced extraction yield and a decrease in the quality of the oil) and degradations of the triglycerides more fragile (in particular unsaturated triglycerides).
  • the method of the invention is well suited for extracting oils from very rich whole sunflower seeds into unsaturated triglycerides.
  • the extracted oil contains a certain amount of alcohol. It is possible in some applications to use the oil / alcohol mixture directly obtained for example as a starting reagent for certain lipochemical reactions ; it is also possible to subject the liquid phase after racking to a alcohol separation operation, in particular by distillation. (This operation is inexpensive and is operated before refining in the processes to remove the solvent).
  • a short chain alcohol having a lower carbon number or equal to 12 which is easier to remove by distillation; it should be noted that the methanol and ethanol can be used when used at low temperature due to their low boiling point.
  • the process of the invention leads to solid co-products which are collected in the terminal area of the twin-screw device, characterized by a low triglyceride content (about 2 to 3 times lower than the contents of classical expression processes): these co-products are thus more easy to recover, since triglycerides generally represent discomfort for achieve this recovery and a factor in reducing their stability (rancidity over time).
  • the process of the invention is preferably carried out in a twin-screw device comprising a zone, known as a shear zone, provided with shear mixers, followed by a so-called crushing zone with crushers, alcohol and phosphoric acid or its salt being injected upstream of the shear zone.
  • a racking area with a filter includes one or more axial compression modules (openwork threads located in downstream of the filter) to ensure the exit of the oil through the filter.
  • the action shear mechanics delivers cellular lipid membranes to the action of phosphoric acid, and the mechanical crushing action then ensures extraction of the oil released from the membrane barriers.
  • the invention extends to a specially twin-screw device designed for implementing the above method.
  • This device includes a tubular enclosure, means of thermal regulation of said enclosure, twin-screw modules with two co-penetrating screws, one seed inlet at one end upstream, a solids outlet at a downstream end, means for liquid withdrawal fitted with a filter and located upstream of the material outlet solid; according to the invention, this device is characterized in that it comprises, of a part, means of injection of alcohol and phosphoric acid or salt, located in downstream of the seed inlet, on the other hand, and shear mixers and crushing mixers located between these injection means and the means of liquid filling.
  • the device was made from modules marketed by the company "CLEXTRAL” (registered trademark) under the reference general "BC21".
  • Each module includes a double tubular enclosure wall 1 and 2 which allows thermal regulation of the core of the enclosure where are housed the active organs.
  • Some modules are of the type comprising two screws identical co-penetrating, direct or reverse pitch, others of the type comprising shear mixers composed of two-lobed discs, others of the type comprising crushing mixers composed of discs monolobes.
  • the various modules are rotated in synchronism by an electric motor 3 making it possible to obtain a speed of rotation of its shaft output speeds of up to 600 rpm In the examples, the speed of rotation chosen is 125 rpm.
  • the seed used are oleic sunflower seeds ("Olbaril” variety) with 52% oil compared to the dry matter and 5.7% moisture.
  • the alcohol used is 2-ethyl hexanol and phosphoric acid with 99% purity is dissolved beforehand in alcohol before injection of the mixture. In each example, we first perform a expression of the oil without injection of alcohol and / or phosphoric acid. The results of extraction yield and purity of the extracted oil are compared.
  • the temperature is regulated to the set point of 80 ° C.
  • the recovered filtrate is centrifuged at 3500 rpm for 1 hour in order to separate the solid particles passed through the filter, which make up the bottom of the oil.
  • the mass of supernatant oil is weighed.
  • the oil extraction yield is calculated after determination of the triglycerides and the phospholipid content of the oil is determined. Operating conditions Extraction yields (in% relative to the oil in the seed) Phospholipid content (mg of phosphorus per kg of oil) Without injection of alcohol or phosphoric acid 69 235 With injection of alcohol and phosphoric acid 88 29
  • This example illustrates the performance of the process in terms low temperature extraction yield and purity of the extracted oil.
  • the temperature is regulated to the set point of 90 ° C.
  • the recovered filtrate is centrifuged at 3500 rpm for 1 hour in order to separate the solid particles passed through the filter, which make up the bottom of the oil.
  • the mass of supernatant oil is weighed.
  • the oil extraction yield is calculated after determination of the triglycerides and the phospholipid content of the oil is determined. Operating conditions Extraction yields (in% relative to the oil in the seed) Phospholipid content (mg of phosphorus per kg of oil) Without injection of alcohol or phosphoric acid 80 220 With injection of alcohol and phosphoric acid 89 98
  • This example illustrates the performance of the process in terms extraction efficiency and oil quality when increasing temperature.
  • the temperature is regulated to the set point of 85 ° C.
  • the recovered filtrate is centrifuged at 3500 rpm for 1 hour in order to separate the solid particles passed through the filter, which make up the bottom of the oil.
  • the mass of supernatant oil is weighed.
  • the oil extraction yield is calculated after determination of the triglycerides and the phospholipid content of the oil is determined. Operating conditions Extraction yields (in% relative to the oil in the seed) Phospholipid content (mg of phosphorus per kg of oil) Without injection of alcohol or phosphoric acid 73 235 With injection of alcohol and phosphoric acid 86 262
  • the injection of phosphoric acid and alcohol results in a high extraction yield.
  • the quantity of phosphoric acid injected being low in this example, the purity of the oil obtained remains equivalent to that of the oil obtained by direct pressure from oleic sunflower seeds without injection of alcohol or phosphoric acid.
  • the temperature is regulated to the set point of 100 ° C.
  • the recovered filtrate is centrifuged at 3500 rpm for 1 hour in order to separate the solid particles passed through the filter, which make up the bottom of the oil.
  • the mass of supernatant oil is weighed.
  • the oil extraction yield is calculated after determination of the triglycerides and the phospholipid content of the oil is determined. Operating conditions Extraction yields (in% relative to the oil in the seed) Phospholipid content (mg of phosphorus per kg of oil) Without injection of alcohol or phosphoric acid 72 / With injection of alcohol and phosphoric acid 90.5 452
  • This example illustrates the performance of the process in terms extraction yield.
  • the high extraction temperature results in a content in phosphorus in the oil a little high.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Fats And Perfumes (AREA)
EP99390012A 1998-06-25 1999-06-21 Verfahren und Vorrichtung zur Extraktion von Öl aus Ölsaaten Withdrawn EP0967264A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9808063A FR2780410B1 (fr) 1998-06-25 1998-06-25 Procede et dispositif pour l'extraction d'huile de graines oleagineuses
FR9808063 1998-06-25

Publications (1)

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EP0967264A1 true EP0967264A1 (de) 1999-12-29

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EP99390012A Withdrawn EP0967264A1 (de) 1998-06-25 1999-06-21 Verfahren und Vorrichtung zur Extraktion von Öl aus Ölsaaten

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EP (1) EP0967264A1 (de)
FR (1) FR2780410B1 (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1639905A1 (de) * 2004-09-23 2006-03-29 Filippo Pollino Vorrichtung zum Brechen von öligen Massen, insbesondere von pflanzlichem, öligen Fruchtfleisch sowie Verfahren hierfür
US20080269513A1 (en) * 2007-03-30 2008-10-30 Reliance Life Sciences Pvt Ltd. Integrated Process for the Preparation of Fatty Acid Methyl Ester (Biodiesel)
DE102007037783A1 (de) 2007-08-10 2009-02-19 Cognis Ip Management Gmbh Lipophile Zubereitungen
CN105500754A (zh) * 2016-01-12 2016-04-20 绵阳市广鑫粮油机械制造有限公司 自动温控一体化压榨机
CN114103224A (zh) * 2021-12-10 2022-03-01 武汉轻工大学 一种用于高含油燕麦加工的稳态挤压设备

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU806747A1 (ru) * 1979-05-30 1981-02-23 Харьковский Ордена Ленина Политех-Нический Институт Им. B.И.Ленина Способ извлечени масла из маслосодер-жАщЕгО МАТЕРиАлА
GB2096634A (en) * 1981-02-25 1982-10-20 Dravo Corp Process for extracting oleaginous seed materials
JPH04323297A (ja) * 1991-04-23 1992-11-12 Natl Food Res Inst 菜種油の製造方法
JPH07197074A (ja) * 1993-12-29 1995-08-01 Nisshin Oil Mills Ltd:The ２軸エクストルーダーによる植物油の製造法
FR2747128A1 (fr) * 1996-04-05 1997-10-10 Toulousaine De Rech Et De Dev Procede et dispositif pour la fabrication d'esters d'acides gras a partir de graines oleagineuses
WO1997043113A1 (fr) * 1996-05-14 1997-11-20 Clextral Procede et installation d'extraction en continu d'un liquide contenu dans une matiere premiere

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU806747A1 (ru) * 1979-05-30 1981-02-23 Харьковский Ордена Ленина Политех-Нический Институт Им. B.И.Ленина Способ извлечени масла из маслосодер-жАщЕгО МАТЕРиАлА
GB2096634A (en) * 1981-02-25 1982-10-20 Dravo Corp Process for extracting oleaginous seed materials
JPH04323297A (ja) * 1991-04-23 1992-11-12 Natl Food Res Inst 菜種油の製造方法
JPH07197074A (ja) * 1993-12-29 1995-08-01 Nisshin Oil Mills Ltd:The ２軸エクストルーダーによる植物油の製造法
FR2747128A1 (fr) * 1996-04-05 1997-10-10 Toulousaine De Rech Et De Dev Procede et dispositif pour la fabrication d'esters d'acides gras a partir de graines oleagineuses
WO1997043113A1 (fr) * 1996-05-14 1997-11-20 Clextral Procede et installation d'extraction en continu d'un liquide contenu dans une matiere premiere

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 8147, Derwent World Patents Index; Class D23, AN 81-86843D, XP002097912 *
PATENT ABSTRACTS OF JAPAN vol. 017, no. 162 (C - 1042) 30 March 1993 (1993-03-30) *
PATENT ABSTRACTS OF JAPAN vol. 095, no. 011 26 December 1995 (1995-12-26) *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1639905A1 (de) * 2004-09-23 2006-03-29 Filippo Pollino Vorrichtung zum Brechen von öligen Massen, insbesondere von pflanzlichem, öligen Fruchtfleisch sowie Verfahren hierfür
US20080269513A1 (en) * 2007-03-30 2008-10-30 Reliance Life Sciences Pvt Ltd. Integrated Process for the Preparation of Fatty Acid Methyl Ester (Biodiesel)
WO2008120223A3 (en) * 2007-03-30 2008-12-24 Reliance Life Sciences Pvt Ltd An integrated process for the preparation of fatty acid methyl ester (biodiesel)
US8481768B2 (en) * 2007-03-30 2013-07-09 Reliance Life Sciences Pvt. Ltd. Integrated process for the preparation of fatty acid methyl ester (biodiesel)
DE102007037783A1 (de) 2007-08-10 2009-02-19 Cognis Ip Management Gmbh Lipophile Zubereitungen
WO2009021641A2 (de) 2007-08-10 2009-02-19 Cognis Ip Management Gmbh Zubereitungen, enthaltend myristinsäure, palmitinsäure, squalan und/oder squalen und verfahren zu deren gewinnung aus mikroorganismen
CN105500754A (zh) * 2016-01-12 2016-04-20 绵阳市广鑫粮油机械制造有限公司 自动温控一体化压榨机
CN114103224A (zh) * 2021-12-10 2022-03-01 武汉轻工大学 一种用于高含油燕麦加工的稳态挤压设备

Also Published As

Publication number Publication date
FR2780410A1 (fr) 1999-12-31
FR2780410B1 (fr) 2000-09-15

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