EP0473985B1 - Entschleimungsverfahren - Google Patents
Entschleimungsverfahren Download PDFInfo
- Publication number
- EP0473985B1 EP0473985B1 EP91113617A EP91113617A EP0473985B1 EP 0473985 B1 EP0473985 B1 EP 0473985B1 EP 91113617 A EP91113617 A EP 91113617A EP 91113617 A EP91113617 A EP 91113617A EP 0473985 B1 EP0473985 B1 EP 0473985B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- oil
- acid
- water
- solution
- content
- 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.)
- Expired - Lifetime
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
- 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) lack the polar parts of the non-hydratable mucilages, and they mainly consist 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, after the acid treatment, a lye-like substance - a base - is added to the mixture, 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 oils containing wax and oils which contain triglycerides with a higher melting point, their excretion is also promoted.
- 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 waxes, 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, immediately separating it 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 each. The treated oil was held 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 nm) 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.
- Soy 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)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
HU529290 | 1990-08-23 | ||
HU905292A HU208037B (en) | 1990-08-23 | 1990-08-23 | Process for diminishing nonhydratable slime- and vax-content of plant-oils |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0473985A2 EP0473985A2 (de) | 1992-03-11 |
EP0473985A3 EP0473985A3 (en) | 1992-06-03 |
EP0473985B1 true EP0473985B1 (de) | 1994-12-07 |
Family
ID=10970002
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP91113617A Expired - Lifetime EP0473985B1 (de) | 1990-08-23 | 1991-08-14 | Entschleimungsverfahren |
Country Status (9)
Country | Link |
---|---|
US (1) | US5239096A (xx) |
EP (1) | EP0473985B1 (xx) |
CA (1) | CA2049720C (xx) |
DE (1) | DE59103777D1 (xx) |
DK (1) | DK0473985T3 (xx) |
ES (1) | ES2064834T3 (xx) |
HU (1) | HU208037B (xx) |
PL (1) | PL291494A1 (xx) |
YU (1) | YU47451B (xx) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Families Citing this family (43)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0583648A3 (en) | 1992-08-19 | 1995-02-01 | Vandemoortele Int Nv | Continuous refining process with reduced waste flows. |
ATE160166T1 (de) * | 1993-03-17 | 1997-11-15 | Unilever Nv | Entfernung von phospholipiden aus glyceridoelen |
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 |
US6376689B1 (en) | 1999-09-02 | 2002-04-23 | Cargill, Incorporated | Removal of gum and chlorophyll-type compounds from vegetable oils |
US7544820B2 (en) * | 2001-02-01 | 2009-06-09 | Carolina Soy Products Llc | Vegetable oil process |
US6511690B1 (en) * | 2001-02-01 | 2003-01-28 | Carolina Soy Products, Inc. | Soybean 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 |
AR069443A1 (es) * | 2007-11-27 | 2010-01-20 | Grace Gmbh & Co Kg | Purificacion de materiales grasos tal como aceite |
US8575409B2 (en) | 2007-12-20 | 2013-11-05 | Syntroleum Corporation | Method for the removal of phosphorus |
MY158569A (en) * | 2007-12-21 | 2016-10-14 | Grace Gmbh & Co Kg | Treatment of biofuels |
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 |
US8231804B2 (en) | 2008-12-10 | 2012-07-31 | Syntroleum Corporation | Even carbon number paraffin composition and method of manufacturing same |
UA111708C2 (uk) | 2009-10-16 | 2016-06-10 | Бандж Ойлз, Інк. | Спосіб рафінування олії |
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 | |
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 |
EP2591081B1 (en) | 2010-07-08 | 2018-03-07 | Indian Oil Corporation Ltd. | Process for removal of metals from oils/fats |
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 |
PE20150179A1 (es) | 2012-06-14 | 2015-02-07 | Bunge Global Innovation Llc | Proceso para la produccion de aceites bajos en acidos grasos saturados |
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 |
BR112016029246B1 (pt) * | 2014-07-03 | 2021-08-31 | Archer-Daniels-Midland Company | Processo para hidratação de fosfolipídeos não hidratáveis em um óleo vegetal |
WO2016060656A1 (en) * | 2014-10-15 | 2016-04-21 | Arisdyne Systems, Inc. | Process for degumming oils |
CN109462988B (zh) | 2016-05-11 | 2022-01-28 | Reg合成燃料有限责任公司 | 生物可再生的煤油、喷气燃料、喷气燃料调合料和制造方法 |
AU2017277861A1 (en) | 2016-06-10 | 2019-02-21 | Drei Lilien Pvg Gmbh & Co. Kg | Aqueous extraction process for the recovery of mucilage and demulsification |
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 |
WO2019157334A1 (en) | 2018-02-09 | 2019-08-15 | Poet Research, Inc. | Methods of refining a grain oil composition to make one or more grain oil products, and related systems |
EP3799598B1 (en) | 2018-06-11 | 2022-10-05 | POET Research, Inc. | Methods of refining a grain oil composition feedstock and related systems compositions and uses |
WO2020245806A1 (en) * | 2019-06-07 | 2020-12-10 | Shirdi Sai Nutraceuticals Pvt Ltd | Enzyme assisted chemical refining of vegetable oils |
BR112023001291A2 (pt) | 2020-07-24 | 2023-04-04 | Reg Synthetic Fuels Llc | Processo de codimerização descarboxilativa e combustíveis sintéticos produzidos a partir do mesmo |
JP2023536097A (ja) * | 2020-07-31 | 2023-08-23 | アールイージー シンセティック フューエルス リミテッド ライアビリティ カンパニー | バイオ燃料原料の前処理方法 |
US11987832B2 (en) | 2020-08-06 | 2024-05-21 | Poet Research, Inc. | Endogenous lipase for metal reduction in distillers corn oil |
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 |
KR20240015669A (ko) | 2021-06-01 | 2024-02-05 | 레그 신써틱 퓨얼즈, 엘엘씨 | 바이오재생가능 경질 파라핀계 케로센 및 지속가능 항공 연료를 위한 방법 |
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 |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
EP0269277B1 (en) * | 1986-11-13 | 1991-07-24 | The Cambrian Engineering Group Limited | Process for degumming triglyceride oils |
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 |
DE69127127T2 (de) * | 1990-05-04 | 1998-01-08 | Unilever Nv | Verfahren zur Raffination eines Glyceridols |
-
1990
- 1990-08-23 HU HU905292A patent/HU208037B/hu unknown
-
1991
- 1991-08-14 EP EP91113617A patent/EP0473985B1/de not_active Expired - Lifetime
- 1991-08-14 DK DK91113617.4T patent/DK0473985T3/da active
- 1991-08-14 ES ES91113617T patent/ES2064834T3/es not_active Expired - Lifetime
- 1991-08-14 DE DE59103777T patent/DE59103777D1/de not_active Expired - Fee Related
- 1991-08-22 YU YU143291A patent/YU47451B/sh unknown
- 1991-08-22 PL PL29149491A patent/PL291494A1/xx unknown
- 1991-08-22 US US07/748,660 patent/US5239096A/en not_active Expired - Lifetime
- 1991-08-22 CA CA002049720A patent/CA2049720C/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
Also Published As
Publication number | Publication date |
---|---|
YU47451B (sh) | 1995-03-27 |
ES2064834T3 (es) | 1995-02-01 |
PL291494A1 (en) | 1992-08-24 |
YU143291A (sh) | 1994-01-20 |
EP0473985A2 (de) | 1992-03-11 |
CA2049720A1 (en) | 1992-02-24 |
EP0473985A3 (en) | 1992-06-03 |
HU208037B (en) | 1993-07-28 |
DK0473985T3 (da) | 1995-05-01 |
CA2049720C (en) | 2000-05-23 |
HU905292D0 (en) | 1991-02-28 |
US5239096A (en) | 1993-08-24 |
DE59103777D1 (de) | 1995-01-19 |
HUT59955A (en) | 1992-07-28 |
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