EP0473985A2 - Procédé de démucilagination - Google Patents

Procédé de démucilagination Download PDF

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Publication number
EP0473985A2
EP0473985A2 EP91113617A EP91113617A EP0473985A2 EP 0473985 A2 EP0473985 A2 EP 0473985A2 EP 91113617 A EP91113617 A EP 91113617A EP 91113617 A EP91113617 A EP 91113617A EP 0473985 A2 EP0473985 A2 EP 0473985A2
Authority
EP
European Patent Office
Prior art keywords
oil
water
acid
content
added
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.)
Granted
Application number
EP91113617A
Other languages
German (de)
English (en)
Other versions
EP0473985B1 (fr
EP0473985A3 (en
Inventor
Herbert Dipl.-Ing. Rohdenburg
Károly Dipl.-Ing. Csernitzky
Béla Dr. Dipl.-Chem. Chikány
József Dr. Dipl.-Chem. Perédi
Attila Dipl.-Chem. Boródi
Anna Dipl.-Chem. Fábicsné Ruzics
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.)
Krupp Elastomertechnik GmbH
Original Assignee
Krupp Maschinentechnik GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Krupp Maschinentechnik GmbH filed Critical Krupp Maschinentechnik GmbH
Publication of EP0473985A2 publication Critical patent/EP0473985A2/fr
Publication of EP0473985A3 publication Critical patent/EP0473985A3/de
Application granted granted Critical
Publication of EP0473985B1 publication Critical patent/EP0473985B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/04—Refining fats or fatty oils by chemical reaction with acids

Definitions

  • the invention relates to a method for reducing the content of mucilages which can no longer be hydrated with water and at the same time the wax content of vegetable oils.
  • phosphorus-containing compounds namely phosphorus glycerides and phosphosphyngolipids - collective names of mucilaginous substances or phosphatides - emerge together with oil from the cells of the raw materials and get into the oil.
  • the amount of it entering the crude oil fluctuates between 3.0 and 0.5%, based on the oil weight.
  • This precipitating substance causes turbidity and precipitation. It interferes with the further process steps of oil refining and its removal is therefore necessary.
  • hydratable mucilages are removed by treatment with water or steam, swelling or hydration with subsequent separation, usually by centrifugation.
  • This process step is called aqueous degumming.
  • the amount of these so-called non-hydratable mucilages - after the corresponding aqueous degumming - is approx. 0.15 to 0.20%, i.e. 5 to 30% of the mucilages originally present, and their removal requires special methods.
  • the phosphatides In contrast to the hydratable mucilages, the phosphatides, their Molecules containing a strongly polar portion (choline, ethanolamine, serine, inositol) are missing from the non-hydratable mucilages, these polar parts, and they consist mainly of the Ca and Mg salts of phosphatidic acid and lysophosphatidic acid. However, it can also be assumed that other cations (Fe, Cu, Al etc.) also participate in the salt formation.
  • German Offenlegungsschrift 26 09 705 One such is the process described in German Offenlegungsschrift 26 09 705, according to which the oil is treated with acid or acid anhydride and subsequently with water.
  • the treatment can be carried out more successfully from both of the above points of view, if a lye-like substance - a base - is added to the mixture after the acid treatment, so that from the Acid excess fat-soluble salts are formed.
  • the action of the base also enables the phosphatidic acid or lysophosphatidic acid freed from its cations (calcium, magnesium, iron, etc.) to dissociate, thereby promoting their hydration and excretion from the oil.
  • the gentle treatment is also from the point of view of economy, the second essential aspect (cost of chemicals and energy) advantageous.
  • the calcium, magnesium and iron content of the oils hydrated with water is lower than the value mentioned above, so that only a very small amount of acid of approx. 0.04 to 0.08% on oil is required to achieve the corresponding effect calculated, is sufficient.
  • a dilute (1 to 2%) lye solution is also added to the oil in a gentle manner, the oil being cooled to 20 to 40 ° C. before the addition.
  • phosphatidic acid and lysophosphatidic acid dissociate. They are hydrated and can be removed from the oil by separation.
  • the low temperature ensures that this phase of the treatment is also gentle.
  • the Oxidation characteristics of the oil do not change unfavorably.
  • Another advantage of the low temperature is that in the case of wax-containing oils and oils which contain triglycerides with a higher melting point, their excretion is also promoted.
  • the elimination and possible crystallization of the higher melting triglycerides and waxes is substantially prevented by the phosphatide compounds present in the oil. Therefore, after the non-hydratable phosphatides have been excreted by swelling, the aforementioned triglycerides and waxes are surprisingly eliminated from the oil in a short time.
  • the amount of lye is measured so that it is sufficient to neutralize the acid previously added to the oil.
  • the process can be carried out depending on the character of the oil to be degummed in such a way that the diluted lye contains a small part of the oil always present neutralizes free fatty acids, so a small amount of soap is created.
  • the gentle conditions including the low temperature, so that the oxidative characteristics of the oil do not increase during the treatment.
  • This fact also promotes the crystallization of the wax materials, since it is known that the oxidized fatty acids have crystallization-inhibiting properties.
  • the phases are separated by heating the mixture of oil and lye solution in a flash, separating it immediately and washing it with a little condensed water.
  • the separated mucilages and waxes are also neutral in terms of their pH and can be easily added to the extraction meal or other feed.
  • the amount of mucilages that can no longer be hydrated with water is significantly reduced, but due to the gentle treatment the oxidation characteristics of the oil do not significantly deteriorate, and at the same time the amount of triglycerides with a higher melting point and decreases the wax content of oils so that subsequent dewaxing is not necessary or this process step can be carried out more easily. If the goal is to significantly reduce the wax content in the oil, a very small amount of soap can be made in the oil by using a very small amount of excess liquor to take advantage of the micellar adsorptive effect.
  • Sunflower oil degummed with water was used as the basic material, which has the following characteristic properties: Acid number 1.5 Peroxide number 8.0 Anisidine number 0.9 Phosphorus content 75 ppm Iron content 1.00 ppm Copper content 0.04 ppm UV absorption (232 nm) 3.1 Wax content 0.06%
  • the oil described above was continuously heated to 50 ° C. and the 10% citric acid solution was continuously added in a tank provided with a stirrer. Based on solid citric acid, 700 g of citric acid was added to the oil to 1000 kg. The treated oil was kept in a stirring tank for 15 minutes while stirring slowly, then cooled to 30 ° C.
  • the mixture was then stirred in a tank with a quantity of 4% NaOH solution, which corresponds stoichiometrically to the acid number increase caused by the citric acid, for two hours, then heated to 80 ° C. in a flash and separated with a separator.
  • the oil phase obtained on separation was washed on another separator with 10% soft water.
  • the washed oil was dried or placed for further refining or in an apparatus suitable for the production of edible oil.
  • the characteristic properties of the ultrafine degummed oil thus obtained are as follows: Acid number 1.5 Peroxide number 8.0 Anisidine number 1.0 Phosphorus content 2.5 ppm Iron content 0.1 ppm Copper content 0.01 ppm UV absorption (232 nm) 3.2 Wax content 0.04%
  • the phosphorus content of the vegetable oil can be reduced to a value below 1 ppm and its color complies with the regulations.
  • Sunflower oil degummed with water was used with the following characteristic properties: Acid number 1.2 Peroxide number 7.5 Anisidine number 0.7 Phosphorus content 80 ppm Iron content 0.9 ppm Copper content 0.05 ppm UV absorption (232 ⁇ m) 3.5 Wax content 0.05%
  • the oil phase obtained during the separation was washed on a new separator with 10% soft water.
  • the washed oil was dried or sent for further refining.
  • the main properties of the degummed oil obtained are as follows: Acid number 1.0 Peroxide number 6.0 Anisidine number 1.0 Phosphorus content 4.5 ppm Iron content 0.08 ppm Copper content 0.01 ppm UV absorption (at 232nm) 3.5 Wax content 0.03%
  • the fabric was washed twice on two successive separators with 10% water.
  • the washed oil was dried or sent for further refining.
  • Rapeseed oil degummed with water was used with the following properties: Acid number 1.5 Peroxide number 8.5 Anisidine number 0.5 Phosphorus content 90 ppm Iron content 0.7 ppm Copper content 0.05 ppm UV absorption (at 232nm) 2.1
  • the material was heated to 80 ° C in a flash and placed on a separator. After separation, the fabric was washed twice with 10% soft water.
  • Soybean oil degummed with water was used with the following properties: Acid number 1.7 Peroxide number 7.1 Anisidine number 0.7 Phosphorus content 100 ppm Iron content 2.0 ppm Copper content 0.05 ppm UV absorption (at 232nm) 3.2
  • the above oil was heated to 60 ° C in continuous treatment and 10% citric acid solution was added in a stirrer tank. Based on solid citric acid, 800 g were added to 1000 kg of oil.
  • the fabric was kept in a stirring tank with slow stirring for 15 minutes, then cooled to 30 ° C and then stirred with 4% NaOH solution. An amount was added to the oil from the NaOH solution, which stoichiometrically neutralizes the citric acid. In the tank, the fabric was slowly stirred for two hours, then instantly heated to 80 ° C and separated on a separator.
  • the oil phase obtained in the separation was washed in another separator with 10% soft water. The washed oil was dried or conveyed for further refining.
  • Sunflower oil degummed with water was used as a starting material with the following characteristic properties: Acid number 1.2 Peroxide number 6.0 Anisidine number 0.9 Phosphorus content 52 ppm Iron content 1.0 ppm Copper content 0.03 ppm UV absorption (at 232nm) 3.0 Wax content 0.06%
  • the oil was heated to 50 ° C in continuous treatment and 15% citric acid solution was added in a stirrer tank. Based on 1000 kg, 300 g of citric acid were added to the oil. The treated fabric became slow for 15 minutes stirred, then cooled to 20 ° C. The substance was then stirred with an amount of 4% NaOH solution corresponding to the 100% stoichiometric increase in acid number caused by the citric acid for a further two hours, heated to 80 ° C. in a flash and separated in a separator.
  • the washed oil was dried or sent for further refining.
  • Characteristic properties of the end product are: Acid number 1.2 Peroxide number 6.0 Anisidine number 0.9 Phosphorus content 3.0 ppm Iron content 0.1 ppm Copper content 0.01 ppm UV absorption (at 232nm) 3.0 Wax content 0.02%

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
EP91113617A 1990-08-23 1991-08-14 Procédé de démucilagination Expired - Lifetime EP0473985B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
HU905292A HU208037B (en) 1990-08-23 1990-08-23 Process for diminishing nonhydratable slime- and vax-content of plant-oils
HU529290 1990-08-23

Publications (3)

Publication Number Publication Date
EP0473985A2 true EP0473985A2 (fr) 1992-03-11
EP0473985A3 EP0473985A3 (en) 1992-06-03
EP0473985B1 EP0473985B1 (fr) 1994-12-07

Family

ID=10970002

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91113617A Expired - Lifetime EP0473985B1 (fr) 1990-08-23 1991-08-14 Procédé de démucilagination

Country Status (9)

Country Link
US (1) US5239096A (fr)
EP (1) EP0473985B1 (fr)
CA (1) CA2049720C (fr)
DE (1) DE59103777D1 (fr)
DK (1) DK0473985T3 (fr)
ES (1) ES2064834T3 (fr)
HU (1) HU208037B (fr)
PL (1) PL291494A1 (fr)
YU (1) YU47451B (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0583648A2 (fr) 1992-08-19 1994-02-23 N.V. Vandemoortele International Procédé de raffinage en continu avec des effluents réduits
WO1994021762A1 (fr) * 1993-03-17 1994-09-29 Unilever N.V. Procede d'elimination des phospholipides presents dans de l'huile glyceridique
US6376689B1 (en) 1999-09-02 2002-04-23 Cargill, Incorporated Removal of gum and chlorophyll-type compounds from vegetable oils
WO2017212076A1 (fr) 2016-06-10 2017-12-14 Drei Lilien Pvg Gmbh & Co. Kg Procédé d'extraction aqueuse pour obtenir des substances mucilagineuses et induire une séparation d'émulsion

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US6844458B2 (en) 1998-11-20 2005-01-18 Ip Holdings, L.L.C. Vegetable oil refining
US6172248B1 (en) * 1998-11-20 2001-01-09 Ip Holdings, L.L.C. Methods for refining vegetable oils and byproducts thereof
US6511690B1 (en) 2001-02-01 2003-01-28 Carolina Soy Products, Inc. Soybean oil process
US7544820B2 (en) * 2001-02-01 2009-06-09 Carolina Soy Products Llc Vegetable oil process
US20040030166A1 (en) * 2002-03-18 2004-02-12 Dick Copeland Methods for treating deodorizer distillate
FR2878744B1 (fr) * 2004-12-06 2008-03-21 Alain Tournay Procede d'obtention d'une huile a partir de la graine de fenugrec pour des utilisations cosmetiques, nutritionnelles ou dermatologiques, composition de cette huile et utilisations
RU2007137272A (ru) * 2005-03-09 2009-04-20 Карджилл, Инкорпорейтед (Us) Разделение подсолнечного масла и воска
US7112688B1 (en) 2005-08-11 2006-09-26 Carolina Soy Products, Llc Soybean oil process
CN1935964B (zh) * 2006-09-30 2011-08-31 白长军 一种油脂脱胶的方法
US8507703B2 (en) * 2007-11-27 2013-08-13 Grace Gmbh & Co. Kg. Purification of fatty materials such as oils
US8575409B2 (en) 2007-12-20 2013-11-05 Syntroleum Corporation Method for the removal of phosphorus
EP2238220A2 (fr) * 2007-12-21 2010-10-13 Grace GmbH & Co. KG Traitement de biocombustibles
US8581013B2 (en) 2008-06-04 2013-11-12 Syntroleum Corporation Biorenewable naphtha composition and methods of making same
US20090300971A1 (en) 2008-06-04 2009-12-10 Ramin Abhari Biorenewable naphtha
DE102008048009A1 (de) 2008-09-19 2010-03-25 Rmenergy Umweltverfahrenstechnik Gmbh Vorrichtung zur dezentralen Aufbereitung nativer Öle und Fette zur Nutzung als Kraftstoff oder als Rohstoff für die Biodieselherstellung
US8231804B2 (en) 2008-12-10 2012-07-31 Syntroleum Corporation Even carbon number paraffin composition and method of manufacturing same
UA109884C2 (uk) 2009-10-16 2015-10-26 Поліпептид, що має активність ферменту фосфатидилінозитол-специфічної фосфоліпази с, нуклеїнова кислота, що його кодує, та спосіб його виробництва і застосування
UA111708C2 (uk) 2009-10-16 2016-06-10 Бандж Ойлз, Інк. Спосіб рафінування олії
DE102009049950A1 (de) * 2009-10-19 2011-04-21 Lurgi Gmbh Verfahren zur Aufarbeitung von leicht verseifbarem Rohöl pflanzlicher oder tierischer Herkunft, für die Weiterverarbeitung zu Biodiesel
US8394900B2 (en) 2010-03-18 2013-03-12 Syntroleum Corporation Profitable method for carbon capture and storage
WO2012004810A1 (fr) 2010-07-08 2012-01-12 Indian Oil Corporation Ltd. Procédé pour l'élimination de métaux d'huiles/matières grasses
DE102010048367A1 (de) * 2010-10-13 2012-04-19 Süd-Chemie AG Verfahren zur Entfernung von Phosphor-haltigen Verbindungen aus Triglycerid-haltigen Zusammensetzungen
GB2501519B (en) 2012-04-27 2020-01-15 N V Desmet Ballestra Eng Sa Physical refining of triglyceride oils and fats
ES2713402T3 (es) 2012-06-14 2019-05-21 Bunge Global Innovation Llc Procedimiento de producción de aceites de saturación baja
US9328303B2 (en) 2013-03-13 2016-05-03 Reg Synthetic Fuels, Llc Reducing pressure drop buildup in bio-oil hydroprocessing reactors
US8969259B2 (en) 2013-04-05 2015-03-03 Reg Synthetic Fuels, Llc Bio-based synthetic fluids
US9321983B2 (en) 2014-07-03 2016-04-26 Arisdyne Systems, Inc. Methods for degumming oils
CA2951013C (fr) * 2014-07-03 2021-04-13 Arisdyne Systems, Inc. Procedes de demucilagination d'huiles
WO2016060656A1 (fr) * 2014-10-15 2016-04-21 Arisdyne Systems, Inc. Procédé de démucilagination d'huiles
EP4700003A1 (fr) 2016-05-11 2026-02-25 REG Synthetic Fuels, LLC Kérosène biorenouvelable, carburéacteur, mélange de carburéacteur et procédé de fabrication
US12157822B2 (en) 2017-05-24 2024-12-03 Poet Research, Inc. Methods of producing vegetable oils with low minerals, metals, or other contaminants
EP3630880B1 (fr) 2017-05-24 2025-12-17 POET Research, Inc. Compositions d'huile contenant de l'ester d'alkyle amélioré, et procédés de production et d'utilisation desdites compositions
CN107779259B (zh) * 2017-11-29 2021-04-09 湖南粮食集团有限责任公司 一种浓香油脂的脱胶方法
US10711221B2 (en) 2018-02-09 2020-07-14 Poet Research, Inc. Method of refining a grain oil composition to make one or more grain oil products, and related systems
CA3103242C (fr) 2018-06-11 2023-08-29 Poet Research, Inc. Procedes de raffinage d'une matiere premiere de composition d'huile d'oleagineux, et systemes, compositions et utilisations associes
WO2020245806A1 (fr) * 2019-06-07 2020-12-10 Shirdi Sai Nutraceuticals Pvt Ltd Raffinage chimique d'huiles végétales assisté par des enzymes
EP4185665A1 (fr) 2020-07-24 2023-05-31 REG Synthetic Fuels, LLC Procédé de codimérisation par décarboxylation et carburants synthétiques produits à partir de celui-ci
CN115956112B (zh) * 2020-07-31 2025-01-24 Reg合成燃料有限责任公司 生物燃料原料的预处理方法
BR112023001818A2 (pt) 2020-08-06 2023-02-23 Poet Res Inc Lipase endógena para redução de metais em óleo de milho de destilaria
US12502625B1 (en) 2021-03-31 2025-12-23 Poet Research, Inc. Homogenous emulsion from a grain material fermentation
CN113322129A (zh) * 2021-05-31 2021-08-31 湖南万象生物科技有限公司 一种化妆品用无色无味无毒茶籽油及其制备方法
US20240218262A1 (en) 2021-06-01 2024-07-04 Reg Synthetic Fuels, Llc Process for biorenewable light paraffinic kerosene and sustainable aviation fuel
CN113444580A (zh) * 2021-07-08 2021-09-28 山东三星玉米产业科技有限公司 一种从助滤剂废弃物中同步提取中性油和食用蜡的生产工艺

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GB736885A (en) * 1952-03-05 1955-09-14 Laval Separator Co De Improvements in or relating to the refining of fatty oils and fats
GB1541017A (en) * 1975-03-10 1979-02-21 Unilever Ltd Degumming process for triglyceride oils
JPS5573793A (en) * 1978-11-30 1980-06-03 Showa Sangyo Co Purification of oil and fat
FI73725C (fi) * 1982-06-29 1987-11-09 Unilever Nv Foerfarande foer rengoering av triglyceridoljor.
GB8506907D0 (en) * 1985-03-18 1985-04-24 Safinco Coordination Centre Nv Removal of non-hydratable phoshatides from vegetable oils
DE3771670D1 (de) * 1986-11-13 1991-08-29 Cambrian Eng Group Ltd Verfahren zum entschleimen von triglyceridoelen.
BR8703598A (pt) * 1987-07-13 1989-01-24 Brasil Pesquisa Agropec Processo de degomagem de oleos brutos de soja com alto conteudo de fosfatidios nao-hidrataveis
EP0456300B1 (fr) * 1990-05-04 1997-08-06 Unilever N.V. Procédé pour raffiner de l'huile glycéridique

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0583648A2 (fr) 1992-08-19 1994-02-23 N.V. Vandemoortele International Procédé de raffinage en continu avec des effluents réduits
WO1994021762A1 (fr) * 1993-03-17 1994-09-29 Unilever N.V. Procede d'elimination des phospholipides presents dans de l'huile glyceridique
US6376689B1 (en) 1999-09-02 2002-04-23 Cargill, Incorporated Removal of gum and chlorophyll-type compounds from vegetable oils
WO2017212076A1 (fr) 2016-06-10 2017-12-14 Drei Lilien Pvg Gmbh & Co. Kg Procédé d'extraction aqueuse pour obtenir des substances mucilagineuses et induire une séparation d'émulsion

Also Published As

Publication number Publication date
PL291494A1 (en) 1992-08-24
CA2049720A1 (fr) 1992-02-24
CA2049720C (fr) 2000-05-23
EP0473985B1 (fr) 1994-12-07
US5239096A (en) 1993-08-24
ES2064834T3 (es) 1995-02-01
EP0473985A3 (en) 1992-06-03
HUT59955A (en) 1992-07-28
YU143291A (sh) 1994-01-20
HU905292D0 (en) 1991-02-28
DK0473985T3 (da) 1995-05-01
DE59103777D1 (de) 1995-01-19
YU47451B (sh) 1995-03-27
HU208037B (en) 1993-07-28

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