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WO1991013956A1 - Procede de production d'une huile vegetale - Google Patents

Procede de production d'une huile vegetale Download PDF

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Publication number
WO1991013956A1
WO1991013956A1 PCT/FI1991/000062 FI9100062W WO9113956A1 WO 1991013956 A1 WO1991013956 A1 WO 1991013956A1 FI 9100062 W FI9100062 W FI 9100062W WO 9113956 A1 WO9113956 A1 WO 9113956A1
Authority
WO
WIPO (PCT)
Prior art keywords
oil
slurry
seed
enzyme
product
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/FI1991/000062
Other languages
English (en)
Inventor
Stiven Laiho
Unto Tulisalo
Hannu Oksanen
Rune NYSTRÖM
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.)
Oljynpuristamo OY
Original Assignee
Oljynpuristamo OY
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 Oljynpuristamo OY filed Critical Oljynpuristamo OY
Publication of WO1991013956A1 publication Critical patent/WO1991013956A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
    • 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
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter

Definitions

  • the present invention relates to a process for the production of a vegetable-oil product from oilseed, in which process the seed is comminuted and slurried in water and the slurry is treated so that the oil is detached from the seed tissue, whereafter the oil is separated from the aqueous phase and is refined to produce the final product.
  • the inven ⁇ tion relates to a vegetable-oil product produced by the pro ⁇ cess.
  • the pressing and extraction process involves a problem in that the phospho- lipids, i.e. phosphatides, present in the seed end up in the extract, together with the oil.
  • the phosphatides must be removed from the oil in the first step of the refining so that they will not disturb the subsequent steps of the re- fining, in which the oil is purified of aldehydes and of free fatty acids, as well as of pigments.
  • phosphatides as part of oil refining has most commonly been carried out by using water or an acid. In each case, owing to their amphoteric character, the phosphatides hy- drolyze and become insoluble in oil. Thereupon they can be sep ⁇ arated from the oil by centrifugation, for example.
  • Other meth ⁇ ods for removing phosphatides include the use of membranes ac ⁇ cording to GB Patent 7 421 813 and the adsorption methods using bleaching clay or silica according to US Patents 635762 and 823217.
  • the object of the present invention is to provide a method sim ⁇ pler than previous ones for the preparation of a vegetable-oil product, eliminating the separate phosphatide removal step be ⁇ longing to the refining.
  • the process according to the inven ⁇ tion is characterized in that an enzyme is added to an aqueous slurry of the seed so that the oil is separated under its ac ⁇ tion to form a separate phase, whj-le the phosphatide present in the seed remains mainly in the aqueous phase, that the oil phase is separated and that the separated oil is transferred directly to physical refining, which consists of a treatment with an adsorbing agent and/or of deodorization.
  • the separation of the oil phase from the aqueous phase can be by mechanical means, for example, by centrifugation, the use of an organic solvent for the extraction of the oil is avoided in the invention, as is also the separation of the oil from the solvent, and an oil is obtained which is completely devoid of hazardous solvent residues.
  • an oil phase which has been separated according to the invention by an enzyme treatment and centrifugation has an even lower phosphatide content than has an oil which has been separated from seed by conventional prior-art methods and has been treated separately for the removal of phosphatides.
  • GB Appli cation 2 127 425 discloses a method in which an enzyme is used to promote the extraction of oil by means of hexane. Further ⁇ more, enzymes have been used in the separation of coconut oil (Mc Glone et al. J. Food Sci. 51, 1986, pp. 695-697) and avoca do oil (Buenrostro et al., Biotechnol. Lett. 8., 1986, pp. 505- 506).
  • the first step of the process for the preparation of a vegeta ⁇ ble-oil product according to the invention is the comminution of the seed, for example by flaking or by coarse milling. Thereafter the seed is preferably heated so that its inherent enzymes are destroyed. Thus it is ensured that the action of the subsequently added enzyme acting on phosphatides will not be disturbed and that the enzymatic reactions will occur in the desired manner, with control. After the heating, the comminution of the preliminarily comminuted seed is continued using a disc attrition mill, a pin mill or some other fine- milling equipment. The finely milled seed is slurried in water, and the slurry is cooked for 10-60 min, preferably 30- 40 min.
  • the solids content of the slurry may be within the range 20-70 %, preferably 40-50%.
  • the solids content of the slurry may be within the range 10- 60%, preferably 15-40 %.
  • the slurry can be wet milled by using, for example a colloid mill. After possible dilution and cooling, the slurry is ready for the ad ⁇ dition of the enzyme having action on phosphatides.
  • the enzyme used has typically some optimal pH value to which the slurry is adjusted by adding an acid or a base.
  • the enzyme is added in a dose which may be 0.1-5.0 % by weight, most commonly 0.5-3.0 % by weight of the solids of the slurry, depending on the type of the seed and the enzyme used.
  • the slurry is incubated at the operational optimum temperature of the enzyme for 0.5-6 hours, preferably 3-4 hours.
  • the optimum conditions for the enzyme action in the pro ⁇ cess according to the invention are not necessarily those re ⁇ ported by the enzyme manufacturer on the basis of his charac- terizational studies; they have to be determined separately by experimentation.
  • the enzymes used may vary according to the complexity of the cell walls of the seed; multi-activity enzymes have proven to be suitable, although carbohydralases have also yielded good results.
  • the desired division of the material into an oil phase, an aqueous phase and the remaining solids of the seed has taken place.
  • the enzyme it has, according to the invention, been accomplished that the phosphatide present in the seed has in the main hydrolyzed and passed into the aqueous phase.
  • the incubated slurry is heated to the temperature range 50-95 °C, preferably 70-95 °C, and is centrifuged in a decanting vessel in order to remove the solid seed material and any oil drops possibly adhering to it.
  • the remaining liquid phase is maintained at a temperature of 70-95 °C and is clarified in a clarifier centrifuge, in which solid material will still separate out from the liquid.
  • the so lids obtained from the decanter are reslurried in water at a temperature of 60-80 C C, and the seed hulls are separated using a vibratory screen.
  • the separated hulls are drained, pressed to dewater, and dried.
  • the solids separated in the clarifier centrifuge are slurried in the washing water which has passed through the vibratory screen.
  • the obtained slurry- is heated to the temperature range 60-80 °C and is divided in the-clarifier centrifuge into a solid phase and a liquid phase.
  • the liquid phases obtained form the clarifier in the said two steps are pooled together, maintained at a tempera ⁇ ture of 50-95 °C, preferably 70-90 °C, and divided in a puri- .
  • the so ⁇ lids obtained from the clarifier are homogenized and dried using, for example, a spray drier.
  • To the obtained oil phase there is added, at a temperature of 30-70 °C, preferably 40-60 °C, approx. 0.1-3 % filter aid mixed with 0.1-0.5% so ⁇ dium sulfate, whereafter mixing is carried out in a mixing tank.
  • the oil is filtered using a conventional filter, such as a plate filter, and, when so desired, it can be further dried in a vacuum dryer.
  • the phosphatide content in the oil obtained is so low that, after this, a mere physical refining treatment will suffice, without the chemical step normally carried out for the removal of phosphatides.
  • the physical refining of the oil may comprise, as the first step, an adsorption treatment in which, by using siliceous earth or other similar adsorption agent, mainly pigments and possibly remaining phosphatides are removed from the oil.
  • the duration of the treatment may be, for example, 50 min.
  • deodorization which may be carried out, for example, by blowing steam through the oil for approx. an hour at a temperature of approx. 250 °C.
  • the deodor ⁇ ization removes from the oil free fatty acids, aldehydes and other oxidation products, and the oil obtained is ready for use, for example, as a foodstuff.
  • Low-glucosinolate rapeseed (Westar) were flaked and steam cooked at 95 °C for 30 min in order to inactivate the yro- sinase enzyme inherently present in the seed.
  • the cooked, flaked seed was thereafter comminuted in a disc attrition mill fitted with serrated discs.
  • a slurry with a solids content of 40 % was prepared from the comminuted seed, and this slurry was cooked for 30 min.
  • the slurry was then diluted with cold water to a 20 % solids content, whereby the temperature of the slurry was also lowered.
  • the pH of the slurry was adjusted to 4.0 by using acetic acid.
  • an enzyme mixture con ⁇ sisting of the enzymes Novo SP-249 and Pectinex 3XL was added to the slurry at 2 % of the dry weight of the slurry, and the slurry was incubated at 45 °C for 24 hours. After the incuba ⁇ tion the slurry was heated to 80 °C and was centrifuged in a laboratory centrifuge so that three separate phases were ob ⁇ tained, i.e. the solid sediment, the aqueous phase, and the oil phase. The aqueous phase was centrifuged in a bucket cen ⁇ trifuge, whereby a solid sediment not containing hull material and an aqueous phase containing practically no oil were ob ⁇ tained.
  • the solid sediments obtained in the centrifugation operations were resuspended in water at 70 °C and were cen ⁇ trifuged once more into three separate phases.
  • the two oil phases obtained in the centrifugation operations were pooled together, and a mixture containing filter clay 1 % by weight of the oil amount and sodium sulfate 0.2 % by weight of the oil amount were added to them.
  • the oil was mixed at 50 C C, whereafter it was filtered.
  • the obtained crude oil was finally dried under vacuum.
  • Table 1 The measurement results characterizing the quality of the oil are given in the following table.
  • the reference process in the table is a solvent extraction in which the oil was produced in a laboratory, by using ⁇ oxhlet apparatus, from the same heat treated and flaked seed as in the enzyme process, by using hexane as the solvent.
  • Rapeseed was treated for the adding of the enzyme as in Example 1. After the cooking and dilution, the pH was ad ⁇ justed as in Example 1 and the temperature was maintained at 50 °C. Enzyme Pectinex 3XL (Novo) was added to the slurry, and the slurry was incubated for 4 hours. After the incubation the oil was separated as described in Example 1. The measurement results characterizing the quality of the oil are presented in the following table.
  • Example 3 Process of Example 2 (Pectinex 3XL) 10.2 116.0 0.55 19.5 1.8
  • Example 3
  • Low-glucosinolate rapeseed (Tobin), which differed from the seed used in Example 1, was treated for the adding of enzyme as described in Example 1.
  • the slurry was wet milled in a Siego mill. The milled slurry was diluted to a solids content of 20 %, the pH was adjusted to 4.5 and the tem ⁇ perature to 50 °C. Enzymes .Olease (Biocon) and Pectinex 3XL (Novo) at 2 % by weight of the solids of the slurry were added to the slurry. The slurry was incubated for 4 hours, and the oil was separated as described in Example 1. The measurement results characterizing the quality of the oil obtained are pre ⁇ sented in the following table:
  • Rapeseed (Tobin), which was the same as that used in Example 3, was treated for the adding of enzyme as described in Ex ⁇ ample 1. After the cooking and dilution, the pH was adjusted to 5 and the temperature to 50 °C. Olease (Biocon) at 2 % by weight of the solids of the slurry was added to the slurry, and the slurry was incubated for 4 hours. After the incubatio the oil was separated as described in Example 1. The measure- ment results characterizing the quality of the oil obtained are presented in the following table:
  • Rapeseed (Westar) was treated for the adding of enzyme as de ⁇ scribed in Example 1. After the cooking and dilution, the pH of the slurry was adjusted to 4.5 and the temperature to 50 °C. The enzyme mixture according to Example 1 at 2 % by weight of the solids of the slurry was added to the slurry, and the slurry was incubated for 4 hours. The oil was separ ⁇ ated as described in Example 1, and its quality charac ⁇ teristics were determined. The measurement results obtained are presented in the following table.
  • the oil was subjected to a physical refining, at the beginning of which the oil was treated with 100-400 ppm ci ⁇ tric acid at 60 °C for 20 min.
  • Adsorption clay was added to the oil, and the oil was maintained at 100 °C under a pressure of 310 Pa generated by using an inert gas.
  • the oil phase was deodorized under a pressure of 0.4 kPa at 245 °C by blowing steam through it for one hour.
  • Fi ⁇ nally the oil was cooled, clarified by filtering it with clay, and analyzed by measuring the parameters characterizing the quality of the oil. The measurement results are presented in the following table.
  • the examples show that the phosphorus content of the crude, un refined oil was in all cases at maximum 3 ppm.
  • the upper limits of phos ⁇ phorus for degum ed and superdegummed oils are 200 ppm and 50 ppm (Canadian General Standard Board).
  • the phosphorus content of the crude rapeseed oil obtained according to the invention is thus only a fraction of the said values, and also consider ⁇ ably lower than the upper limit, 15 ppm, set for refined rape ⁇ seed oil (Canadian General Standard Board) . It can be seen from the results of Example 5 that in the physical refining .step of the process according to the invention the phosphorus content of the oil further considerably decreases.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • Fats And Perfumes (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

L'invention se rapporte à un procédé de préparation d'une huile végétale à partir d'une graine telle que le colza ainsi qu'au produit obtenu au moyen du procédé, au cours duquel la graine est pulvérisée, éventuellement traitée à chaud et mélangée à de l'eau pour former une pulpe. D'après l'invention, on ajoute un enzyme à cette pulpe dont la fonction est de retenir dans la phase aqueuse les phosphatides présents dans la graine, tandis que l'huile se sépare pour former une phase distincte, séparée mécaniquement, par exemple par centrifugation. L'huile végétale brute ainsi obtenue, qui ne contient pas des résidus de solvants organiques et est pratiquement exempte de phosphatides, est raffinée physiquement pour obtenir un produit final, le raffinage comprenant un traitement avec un agent d'adsorption et/ou désodorisation.
PCT/FI1991/000062 1990-03-06 1991-03-04 Procede de production d'une huile vegetale Ceased WO1991013956A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI901135A FI901135L (fi) 1990-03-06 1990-03-06 Foerfarande foer framstaellning av vaextoljeprodukt.
FI901135 1990-03-06

Publications (1)

Publication Number Publication Date
WO1991013956A1 true WO1991013956A1 (fr) 1991-09-19

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ID=8530012

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FI1991/000062 Ceased WO1991013956A1 (fr) 1990-03-06 1991-03-04 Procede de production d'une huile vegetale

Country Status (3)

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CA (1) CA2015695A1 (fr)
FI (1) FI901135L (fr)
WO (1) WO1991013956A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2046135A1 (es) * 1992-07-03 1994-01-16 Univ Santiago Compostela Tratamiento enzimatico de semillas oleaginosas para mejorar la extraccion de aceite y simultaneamente aumentar la calidad nutricional de la harina.
WO1994013743A1 (fr) * 1992-12-17 1994-06-23 Novo Nordisk A/S Procede d'isolation d'oleoresines vegetales pouvant etre obtenues par extraction par hexane
DE102006062045A1 (de) 2006-12-29 2008-07-03 Ab Enzymes Gmbh Verbessertes Verfahren zur Gewinnung von Öl aus Pflanzensamen
CN101735884B (zh) * 2009-12-07 2011-12-21 金湖县广原油脂有限公司 煎炸无泡沫国标四级菜籽油的生产方法
WO2011158203A1 (fr) 2010-06-17 2011-12-22 Danisco A/S Procédé
WO2013104659A2 (fr) 2012-01-13 2013-07-18 Dupont Nutrition Biosciences Aps Procédé
CN107057830A (zh) * 2017-03-20 2017-08-18 江南大学 一种近红外预处理辅助水酶法提取菜籽油的方法
CN113249165A (zh) * 2021-05-31 2021-08-13 中国热带农业科学院农产品加工研究所 一种腰果仁油的提取方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1767027A1 (de) * 1968-03-22 1971-09-02 Drevici Kux Ursula Dr Verfahren zur Gewinnung von Fett aus den Samen der Fruechte der Pflanzengattung Theobroma
FR2078467A5 (en) * 1970-02-18 1971-11-05 Thaelmann Schwermaschbau Veb Fats and proteins recovery from vegetablesoi
FR2196648A5 (en) * 1972-07-28 1974-03-15 Cpc International Inc Vegetable oil recovery - by treating finely divided raw material as aq slurry with cellulose
GB1402769A (en) * 1972-08-08 1975-08-13 Cpc International Inc Process for obtaining oil from oil-containing grain germs
EP0113165A1 (fr) * 1982-09-28 1984-07-11 Imperial Biotechnology Limited Extraction d'huiles et de protéines végétales à partir de graines
WO1989009255A1 (fr) * 1988-03-30 1989-10-05 Bucher-Guyer Ag Maschinenfabrik Procede et installation d'extraction d'huiles et de graisses de produits naturels
US4904483A (en) * 1988-02-16 1990-02-27 Novo Industri A/S Method for production of an upgraded coconut product

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1767027A1 (de) * 1968-03-22 1971-09-02 Drevici Kux Ursula Dr Verfahren zur Gewinnung von Fett aus den Samen der Fruechte der Pflanzengattung Theobroma
FR2078467A5 (en) * 1970-02-18 1971-11-05 Thaelmann Schwermaschbau Veb Fats and proteins recovery from vegetablesoi
FR2196648A5 (en) * 1972-07-28 1974-03-15 Cpc International Inc Vegetable oil recovery - by treating finely divided raw material as aq slurry with cellulose
GB1402769A (en) * 1972-08-08 1975-08-13 Cpc International Inc Process for obtaining oil from oil-containing grain germs
EP0113165A1 (fr) * 1982-09-28 1984-07-11 Imperial Biotechnology Limited Extraction d'huiles et de protéines végétales à partir de graines
US4904483A (en) * 1988-02-16 1990-02-27 Novo Industri A/S Method for production of an upgraded coconut product
WO1989009255A1 (fr) * 1988-03-30 1989-10-05 Bucher-Guyer Ag Maschinenfabrik Procede et installation d'extraction d'huiles et de graisses de produits naturels

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2046135A1 (es) * 1992-07-03 1994-01-16 Univ Santiago Compostela Tratamiento enzimatico de semillas oleaginosas para mejorar la extraccion de aceite y simultaneamente aumentar la calidad nutricional de la harina.
WO1994013743A1 (fr) * 1992-12-17 1994-06-23 Novo Nordisk A/S Procede d'isolation d'oleoresines vegetales pouvant etre obtenues par extraction par hexane
DE102006062045A1 (de) 2006-12-29 2008-07-03 Ab Enzymes Gmbh Verbessertes Verfahren zur Gewinnung von Öl aus Pflanzensamen
US8822201B2 (en) 2006-12-29 2014-09-02 Ab Enzymes Gmbh Method for recovering oil from plant seeds
CN101735884B (zh) * 2009-12-07 2011-12-21 金湖县广原油脂有限公司 煎炸无泡沫国标四级菜籽油的生产方法
WO2011158203A1 (fr) 2010-06-17 2011-12-22 Danisco A/S Procédé
WO2013104659A2 (fr) 2012-01-13 2013-07-18 Dupont Nutrition Biosciences Aps Procédé
WO2013104659A3 (fr) * 2012-01-13 2013-09-06 Dupont Nutrition Biosciences Aps Procédé
CN107057830A (zh) * 2017-03-20 2017-08-18 江南大学 一种近红外预处理辅助水酶法提取菜籽油的方法
CN113249165A (zh) * 2021-05-31 2021-08-13 中国热带农业科学院农产品加工研究所 一种腰果仁油的提取方法
CN113249165B (zh) * 2021-05-31 2023-01-03 中国热带农业科学院农产品加工研究所 一种腰果仁油的提取方法

Also Published As

Publication number Publication date
FI901135A7 (fi) 1991-09-07
FI901135L (fi) 1991-09-07
FI901135A0 (fi) 1990-03-06
CA2015695A1 (fr) 1991-09-06

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