EP2052065B1 - Procédé simplifié pour le raffinage des graisses des et huiles - Google Patents

Procédé simplifié pour le raffinage des graisses des et huiles Download PDF

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Publication number
EP2052065B1
EP2052065B1 EP07786306A EP07786306A EP2052065B1 EP 2052065 B1 EP2052065 B1 EP 2052065B1 EP 07786306 A EP07786306 A EP 07786306A EP 07786306 A EP07786306 A EP 07786306A EP 2052065 B1 EP2052065 B1 EP 2052065B1
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Prior art keywords
bleaching
crude oil
oil
acid
earth
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German (de)
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EP2052065A1 (fr
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Klaus Schurz
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Sued Chemie AG
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Sued Chemie AG
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    • 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
    • C11B3/10—Refining fats or fatty oils by adsorption

Definitions

  • the invention relates to a process for bleaching oils and fats.
  • bleaching earths are used to remove turbidity, discoloration or even to remove oxidation accelerators. Adsorptive cleaning significantly improves the taste, color and storage stability of oils and fats.
  • different classes of bleaching earths are used.
  • this group comprises acid-activated montmorillonites, wherein the acid activation is carried out in a complex process by dealuminating the crude clays with concentrated acids at high temperatures, usually at boiling heat. In this process, a bleaching earth product with a very high specific surface area and a large pore volume is obtained.
  • a disadvantage of these highly active bleaching earths is the fact that dealuminating with acid during production results in large quantities of acidic, high-salinity wastewater, which can only be treated or disposed of in complex processes.
  • the high costs for waste disposal and the complex production process justify the comparatively high prices of such highly active bleaching earths.
  • NABE Natural Active Bleaching Earth
  • These naturally occurring bleaching earths have been used for hundreds of years for the purification of fats and oils.
  • These nature-active systems also called Fuller's Earth or Fuller's Earth
  • They have only a low bleaching power, so they are usually not suitable for the cleaning of hard to bleach oils and fats.
  • much larger amounts of the adsorbent must be used in comparison to highly active bleaching earths in order to achieve the desired bleaching result.
  • higher losses of oil or fat must be accepted, since the bleaching earths can not be separated in pure form and certain amounts of oil or fat remain in the bleaching earth.
  • SMBE surface activated systems
  • SMBE surface modified bleaching earth
  • a naturally active raw clay with small amounts of acid is applied and thus achieved an "in situ activation”.
  • Attapulgite and hormone-containing raw clays have proven particularly suitable for this process. These have a very high specific surface area of natural raw materials of about 100 to 180 m 2 / g and a pore volume of about 0.2 to 0.35 ml / g.
  • salts formed in the acid activation or unreacted portions of the acid are not washed out, they remain on the product and are at least partially deposited in the pores.
  • these acid-activated bleaching earths generally do not achieve the same efficiency as achieved by highly active bleaching earths (HPBE) produced by dealuminating with acid.
  • HPBE highly active bleaching earths
  • the simple manufacturing process allows a comparatively low-cost production, with no acid effluents being a particular advantage.
  • a bleaching earth composition which comprises a neutral bleaching earth comprising attapulgite and smectite in a ratio in the range of 0.3: 1 to 1.5: 1, the proportion of attapulgite and smectite being at least 65% by weight of the bleaching earth , Further, the composition contains a polyvalent carboxylic acid having an even number of carboxyl groups arranged in pairs, the carboxyl groups each having an eclipsed configuration.
  • a bleaching earth composition comprising a mixture of a particulate clay and a particulate polyvalent carboxylic acid, the carboxylic acid having a pK a in the range of 1 to 7 and being substantially free of salts of organic acids.
  • the clay has a moisture content of not more than 8% by weight based on the clay.
  • the polyvalent carboxylic acid is contained in a proportion in the range of 1 to 8 wt .-%, based on the composition in this.
  • US 6,346,286 B1 a bleaching process in which the oil to be bleached is contacted with a particulate composition comprising particles of a clay mineral and particles of at least one organic acid, wherein the organic acid is substantially free of salts of the organic acid.
  • a particulate composition comprising particles of a clay mineral and particles of at least one organic acid, wherein the organic acid is substantially free of salts of the organic acid.
  • citric acid is mentioned as a suitable organic acid.
  • the refined oil After bleaching, the refined oil should meet certain color, taste and durability requirements. Thus, the oil must not be too dark and, depending on the type of oil, have a yellow to green color. Furthermore, the oil should be preserved over a longer period without taste deterioration, so do not taste rancid.
  • the oil is first degassed after drying and dried, for example, to remove dissolved oxygen. Subsequently, mucilages, in particular phospholipids, are removed.
  • the dried and degassed oil is treated with phosphoric acid and stirred at about 95 ° C and atmospheric pressure for about 15 to 20 minutes.
  • further water is added at the end of the degumming, for example in a proportion of 0.2% by weight.
  • the lecithin phase is separated, for example by centrifugation.
  • the subsequent bleaching of the degummed oil involves two stages, a wet bleaching and a vacuum equalization.
  • the degummed oil is mixed with 0.1 to 0.5% by weight of water and, after the oil has been heated to 95 ° C., 0.3 to 2% by weight of bleaching earth is added. The mixture is then stirred at normal pressure for about 20 minutes. Subsequently, a vacuum is applied (for example 100 mbar) and the oil is stirred for a further 30 minutes at 95.degree. After bleaching, the spent bleaching earth is separated off, for example by filtering the mixture through a suction filter covered with a paper filter.
  • the oil After bleaching, the oil is still deodorized.
  • superheated steam which has an outlet temperature of about 240 ° C, passed through the oil to remove free fatty acids and unpleasant flavors and odors.
  • the deodorization is carried out in vacuo at a pressure in the range of less than 5 mbar, preferably 1 to 3 mbar.
  • the oil After refining, the oil must meet certain requirements in terms of, for example, color, taste and shelf life. For example, the oil should not appear brown but, depending on the variety, have a yellow to green color. A benchmark for this is the Lovibond color number red, which should be as low as possible. To increase the shelf life, the oil should have a very low iron or phosphorus content. Furthermore, the oil should be as resistant to oxidation as possible in order to prevent the development of a rancid odor and taste.
  • the present invention therefore an object of the invention to provide a method for bleaching oils and fats, which can be carried out with given quality requirements, with less time compared to the prior art and under more economically favorable conditions.
  • the bleaching earth is added in comparison with the prior art low temperatures in the range of 35 to 50 ° C.
  • the process according to the invention thus has the advantage that the oil for the addition of the bleaching earth does not have to be heated to high temperatures and the amount of bleaching earth can be reduced.
  • a crude oil is initially provided in the usual way. This can be obtained, for example, in an oil mill by pressing.
  • the crude oil can also be degassed and dried in the usual way.
  • the crude oil is heated to a temperature in the range of 35 to 55 ° C, preferably 40 to 50 ° C.
  • the temperature is chosen so that the oil is in liquid form. If the oil is not already in liquid form, the temperature is preferably selected only slightly above the melting point, preferably 5 to 20 ° C, in particular 10 to 15 ° C above the melting point of the oil.
  • the bleaching earth is then added to the heated oil and the oil is bleached in a conventional manner.
  • the amount of bleaching earth is chosen depending on the desired color lightening.
  • the amount of bleaching earth is selected in the range of 0.5 to 2.5 wt .-%, particularly preferably in the range of 1 to 2 wt .-%, based on the crude oil.
  • the bleaching earth mixed with the bleaching earth can be heated to 95 ° C. in a conventional manner.
  • the bleaching can be done by directly after the addition of the bleaching earth vacuum is applied, without having previously given water to the crude oil.
  • the bleaching then takes place as a pure vacuum bleaching.
  • the vacuum bleaching is preferably carried out at elevated temperature, particularly preferably at temperatures of 80 to 110 ° C.
  • the bleaching is preferably carried out at least in sections, likewise at low temperature.
  • the temperature is preferably in the range of 35 to 55 ° C, especially preferably chosen 40 to 50 ° C.
  • the bleaching is carried out at least in two stages, initially wet bleaching followed by vacuum equalization. That wet bleaching is preferably carried out at low temperature, ie in the range of 35 to 55 ° C, particularly preferably 40 to 50 ° C, while the vacuum is preferably at higher temperatures, preferably in the range of 80 to 95 ° C.
  • the crude oil is first mixed with water.
  • the amount of water is preferably selected in the range of 0.05 to 1.5 wt .-%, particularly preferably 0.1 to 1 wt .-%.
  • the mixture is then preferably stirred at 35 to 55 ° C, particularly preferably 40 to 50 ° C.
  • the low temperature during wet bleaching allows a further increase in color lightening or a further reduction in the amount of bleaching earth.
  • the vacuum is equal to the above conditions, ie preferably at temperatures of 80 to 95 ° C and a pressure in the range of about 100 mbar.
  • the bleaching process according to the invention is particularly suitable for low-phosphorus oils, which preferably have a phosphorus content of less than 100 ppm. Possibly.
  • conventional degumming may be performed to achieve the preferred low phosphorus content.
  • the process according to the invention is suitable for the bleaching of palm oil.
  • the degumming is preferably carried out in such a way that the crude oil is mixed with water before bleaching.
  • the amount of water added for degumming is preferably at least 0.05% by weight and is more preferably in the range of 0.06 to 1.5% by weight, more preferably in the range of 0.15 to 0.5% by weight. % and very particularly preferably selected at about 0.2 wt .-%, based on the crude oil used.
  • the crude oil is added for degumming with citric acid.
  • the citric acid is preferably added as an aqueous solution, the concentration of the solution preferably being chosen such that the preferred amounts of water given above are added to the crude oil.
  • the amount of added citric acid, calculated as monohydrate and based on the crude oil, is preferably in the range of 0.02 to 0.8 wt .-%, particularly preferably 0.04 to 0.5 wt .-%, particularly preferably 0, Selected from 06 to 0.1 wt .-%.
  • the degumming is also carried out at a relatively low temperature in the range of 35 to 55 ° C, preferably 40 to 50 ° C.
  • the treatment time of the oil for degumming is preferably selected in the range of 10 to 30 minutes, more preferably 15 to 25 minutes.
  • the lecithin phase is preferably separated from the degummed oil, for example by centrifugation.
  • an improvement of the color lightening can be achieved per se for all bleaching earths, ie both for HPBE, as well as for SMBE and HUB.
  • NABE naturally active bleaching earths
  • SMBE surface-modified bleaching earths
  • HPBE highly active bleaching earths
  • the surface activation of the bleaching earths is preferably carried out with sulfuric acid.
  • surface-rich bleaching earths are particularly preferably used.
  • the preferred natural bleaching earths have a specific pore volume of more than 0.5 ml / g, more preferably a specific pore volume in the range of 0.5 to 1.0 ml / g, particularly preferably 0.7 to 1.0 ml / g on. More preferably, at least 40%, more preferably at least 50%, and most preferably at least 60% of the pore volume is provided by pores having a pore diameter of at least 14 nm and providing at most 25% of the pore volume of pores having a diameter of less than 7 , 5 nm exhibit.
  • the specific surface area (BET surface area) and the specific pore volume are determined by means of nitrogen porosimetry according to DIN 66131 and evaluation according to the BJH method.
  • the total pore volume refers to pores with a diameter of 2 to 130 nm.
  • the ion exchange capacity of the preferred natural bleaching earths is preferably more than 40 meq / 100 g, preferably more than 50 meq / 100 g, and more preferably is in the range of 55 to 75 meq / 100 g.
  • a slurry of 10% by weight of the naturally active bleaching earth in water preferably has a pH in the range of 5.5 to 8.5, preferably 5.9 to 8.2. The pH is determined with a pH electrode.
  • the naturally active bleaching earths can be activated by treatment with acid.
  • the raw clays are brought into contact with an inorganic or organic acid.
  • any method known to those skilled in the art for acid activation of clays can be used, for example by spraying or impregnating with acid.
  • the excess acid and the salts formed during activation are not washed out.
  • no washing step is carried out, but the treated raw clay dried and then ground to the desired particle size.
  • a typical bleaching earth fineness is usually set.
  • the dry sieve residue on a screen with a mesh size of 25 microns is in the range of 50 to 65 wt .-%.
  • the activation of the crude clay can be carried out, for example, in an aqueous phase.
  • the acid is brought into contact with the crude clay as an aqueous solution. It can proceed in such a way that first the raw clay, which preferably in Form of a powder is provided, is slurried in water. Subsequently, the acid is added in concentrated form.
  • the raw clay can also be slurried directly in an aqueous solution of the acid, or the aqueous solution of the acid can be applied to the raw clay.
  • the aqueous acid solution can be sprayed, for example, onto a preferably crushed or powdery raw clay, the amount of water being preferably chosen to be as low as possible and, for example, using a concentrated acid or acid solution.
  • the amount of acid may preferably be between 1 and 10% by weight, more preferably between 2 and 6% by weight of a strong acid, especially a mineral acid such as sulfuric acid, based on the anhydrous crude clay (atro). If necessary, excess water can be evaporated and the activated raw clay then ground to the desired fineness. As already explained above, no washing step is required even in this embodiment of the method according to the invention.
  • After application of the aqueous solution of the acid is only, if necessary, dried until reaching the desired moisture content. Most of the water content of the resulting bleaching earth product is adjusted to a proportion of less than 20 wt .-%, preferably less than 10 wt .-%.
  • the acid itself can be chosen arbitrarily. Both mineral acids and organic acids or mixtures of the above acids can be used. Usual mineral acids may be used, such as hydrochloric acid, phosphoric acid or sulfuric acid, with sulfuric acid being preferred. Concentrated or diluted acids or acid solutions can be used. As organic acids, solutions of, for example, citric acid or oxalic acid can be used. Preferred is citric acid.
  • the grain size or the mean grain size of the bleaching earth should preferably be chosen so that a complete and simple separation of the used bleaching earth from the refined product is made possible.
  • the mean grain size of the powdered raw clay is selected in a range of 10 to 63 ⁇ m.
  • the fineness is chosen so that on a sieve with a mesh size of 63 microns about 20 to 40 wt .-% of the mixture remain (sieve residue) and on a sieve with a mesh size of 25 microns about 50 to 65 wt .-% of Stay behind. This can be referred to as typical bleaching earth fineness.
  • FIG. 1 schematically the individual steps are shown, which are passed through in a physical refining of palm oil according to the prior art.
  • the crude palm oil is first degassed at 95 ° C and a reduced pressure of 100 mbar for 15 minutes and dried. 0.06% by weight of phosphoric acid is then added to the dried palm oil for degumming and the mixture is stirred at atmospheric pressure and 95 ° C. for 15 minutes. Then, in a second degumming step, 0.2 wt% water is added to the mixture and the mixture is stirred for an additional 10 minutes at atmospheric pressure and 95 ° C.
  • FIG. 2 shows the sequence of the method according to the invention using the example of a refining of palm oil.
  • the crude palm oil which need not be dried and degassed, is added with 0.28% by weight of a 25% citric acid solution and stirred for degumming for 10 minutes at 45 ° C and atmospheric pressure.
  • the bleaching earth is added at 45 ° C and the mixture for wet bleaching at atmospheric pressure and stirred at 45 ° C for 20 minutes.
  • the mixture is heated to 95 ° C and then applied for 30 minutes, a reduced pressure of 100 mbar.
  • the used bleaching earth is separated by filtering the hot mixture through a paper filter.
  • the filtered oil is then deodorized as described above.
  • the specific surface was carried out on a fully automatic nitrogen porosimeter from Micromeritics, type ASAP 2010, in accordance with DIN 66131.
  • the pore volume was determined using the BJH method ( EP Barrett, LG Joyner, PP Haienda, J. Am. Chem. Soc. 73 (1951) 373 ). Pore volumes of certain pore size ranges are determined by summing up incremental pore volumes resulting from the evaluation of the pore size ranges Adsorption isotherms are obtained according to BJH.
  • the total pore volume according to the BJH method refers to pores with a diameter of 2 to 130 nm.
  • This analysis is based on the total digestion of the raw clay or the corresponding product. After dissolution of the solids, the individual components are treated with conventional specific analytical methods, e.g. ICP, analyzed and quantified.
  • conventional specific analytical methods e.g. ICP
  • the crude clay to be investigated was dried at 105 ° C. over a period of two hours. Thereafter, the dried material was reacted with an excess of aqueous 2N NH 4 Cl solution for one hour under reflux. After a service life of 16 hours at room temperature was filtered, whereupon the filter cake was washed, dried and ground and the NH 4 content in crude clay by nitrogen determination (CHN analyzer from. Leco) was determined according to the manufacturer. The proportion and type of exchanged metal ions was determined in the filtrate by ICP spectroscopy.
  • the X-ray images are taken on a Phillips high-resolution powder diffractometer (X'-Pert-MPD (PW 3040)) equipped with a Cu anode.
  • the NABE EX 1221 (I) characterized in Example 1 was mixed with water and then activated with 3% by weight of H 2 SO 4 .
  • 100 g of powder dried to 9.3% H 2 O were intimately mixed with 208 g of water and 2.83 g of H 2 SO 4 (96% strength) in a beaker.
  • the resulting mixture was dried at 110 ° C. to a water content of 9.4% and then ground to a typical bleaching earth fineness (dry sieve residue to 63 ⁇ m sieve: 20 to 40% by weight, dry sieve residue to 25 ⁇ m sieve: 50 to 65% by weight. -%).
  • Such bleaching earth is offered by Süd-Chemie AG under the name "EX 1221 (II)".
  • a 50% H 3 PO 4 solution and a 25% citric acid solution were used.
  • the rancimat test was carried out in each case (Rancimat 743, Metrohm).
  • a constant stream of air was passed through the heated sample and collected in a measuring vessel filled with distilled water.
  • the oxidation results in short-chain organic acids, especially formic acid, which dissolve in the distilled water of the measuring vessel.
  • the conductivity of the distilled water was measured as a function of time. The conductivity initially remains constant and then increases. A tangent was created on the rising branch of the curve and the induction time was read on the x-axis.
  • the values obtained in the measurements are in the FIGS. 1 to 14 played.
  • FIG. 4 the Lovibond color numbers are shown in red and yellow, which are obtained using a SMBE (EX 1221 (II)) after bleaching and deodorizing.
  • the Lovibond color number yellow follows the trend of the Lovibond color number red.
  • a lovibond yellow color of 46 is obtained in the prior art process (Process 3A). Without degumming and only a vacuum equalization at 95 ° C (procedure 3A.2), a Lovibond color number yellow of 39 is already reached. If the bleaching temperature is lowered to 45 ° C. (procedure 3B.2), a Lovibond color number yellow of 35 is obtained.
  • the Lovibond color numbers are reproduced in red, which were respectively measured after bleaching and after deodorization, wherein the refining was carried out with different bleaching earths.
  • the bleaching earth "Optimum 215 FF" from Süd-Chemie AG corresponds to a highly active bleaching earth, which is obtained by extracting natural clays with hot mineral acid.
  • a Lovibond color number red of 9.3 is obtained after bleaching and a Lovibond color number red of 2.2 after deodorization.
  • a vacuum blanching at a temperature of 45 ° C process 3B.2
  • the Lovibond color number decreases red after bleaching to 8.3 and after deodorizing to 2.1.
  • citric acid is also added during degumming (process guide 3C)
  • a Lovibond color number red of 8.6 is obtained after bleaching. After deodorizing, however, the Lovibond color number drops red to 1.9.
  • a Lovibond color number yellow of 31 is obtained after bleaching and deodorizing according to process procedure 3A. This decreases to 26 when only a vacuum blanching is performed at 45 ° C (procedure 3B.2). If citric acid is added during degumming (procedure 3C), the Lovibond color number can be reduced to 23 yellow.
  • Example 1 If one uses the natural bleaching earth "EX 1221 (I)" characterized in Example 1, the result is an induction period of 8.7 h in a process procedure according to the prior art (Process 3A). If only a vacuum equalization is carried out at 45 ° C. (method 3B.2), the induction period drops to 8.1 h. However, when citric acid is added during degumming (procedure 3C), an induction period of 11.6 is achieved which is close to the value achieved for an HPBE in the prior art process.
  • FIG. 11 the Lovibond color numbers are shown in red, which are measured after bleaching or deodorization, using different amounts of bleaching earths.
  • bleaching earth is obtained at a starting amount of 2.0% by weight a Lovibond color number of 8.6 after bleaching and 1.9 after deodorization. These values increase to 12.2 and 2.2, respectively, when the bleaching mass is lowered to 1.4%.
  • Lovibond color number yellow shown in red in comparison to the Lovibond color number gives the same trend.
  • a Lovibond color number yellow of 31 is achieved at an input quantity of 2.0% HPBE "Optimum 215 FF". Decreasing the amount used to 1.4%, the Lovibond color number increases yellow to 46.
  • Lovibond color number of 27 is obtained in the process of the invention 3C at a starting amount of 2.0%, which is at a reduction of the amount used to 1.7%, 1.4%, or 1.1% only moderately increases from 28 over 30 to 31.
  • Fig. 13 shows that in all process variants, a reduction of the iron or phosphorus content can be achieved below the detection limit.
  • FIG. 14 illustrated induction periods show the same trend.
  • the amount used can be reduced without dramatic losses in durability must be taken into account.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Claims (7)

  1. Procédé pour blanchir des huiles ou des matières grasses, dans lequel
    - une huile brute, issue d'une source végétale ou animale est préparée
    - l'huile brute est débourbée à une température comprise dans une plage entre 35 à 55 °C en ajoutant à l'huile brute pour le débourbage de l'acide citrique
    - l'huile brute est chauffée à une température comprise dans une plage de 35 à 55°C
    - une smectite est ajoutée à l'huile brute chauffée
    - l'huile brute chauffée est blanchie, le blanchiment comprenant un blanchiment humide et un blanchiment dans le vide et le blanchiment humide est réalisé à une température comprise dans une plage entre 35 et 55°C ; et
    - la smectite est séparée de l'huile blanchie.
  2. Procédé selon l'une des revendications précédentes, dans lequel l'huile brute a une teneur en phosphore de moins de 100 ppm.
  3. Procédé selon l'une des revendications précédentes, dans lequel l'huile brute est de l'huile de palme.
  4. Procédé selon l'une des revendications précédentes, dans lequel une quantité d'eau d'au moins de 0.05% en poids par rapport à l'huile brute est ajoutée.
  5. Procédé selon l'une des revendications précédentes, dans lequel l'acide citrique dans une quantité de 0.02 à 0.8 % en poids, calculé comme monohydrate et par rapport à l'huile brute, est ajouté.
  6. Procédé selon l'une des revendications précédentes, dans lequel la smectite est une smectite avec une activité naturelle.
  7. Procédé selon l'une des revendications 1 à 5, dans lequel la sméctite est une sméctite dont la surface a été activée par un acide.
EP07786306A 2006-07-28 2007-07-24 Procédé simplifié pour le raffinage des graisses des et huiles Not-in-force EP2052065B1 (fr)

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DE102006035064A DE102006035064A1 (de) 2006-07-28 2006-07-28 Vereinfachtes Verfahren zur Raffination von Fetten und Ölen
PCT/EP2007/006580 WO2008012072A1 (fr) 2006-07-28 2007-07-24 Procédé simplifié pour le raffinage des graisses des et huiles

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AT (1) ATE451443T1 (fr)
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WO (1) WO2008012072A1 (fr)

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DE102008060059A1 (de) 2008-12-02 2010-06-10 Süd-Chemie AG Verfahren zur Reduzierung des 3-MCPD-Gehalts in raffinierten Pflanzenölen
US20210388401A1 (en) * 2017-05-24 2021-12-16 Poet Research, Inc. Methods of refining a grain oil composition, and related systems, compositions and uses

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GB2144143B (en) * 1983-06-28 1986-11-05 Institiut Penyelidikan Minyak Refining of palm oils
US5151211A (en) * 1988-12-05 1992-09-29 Oil-Dri Corporation Of America Oil bleaching method and composition for same
US5004570A (en) * 1988-12-05 1991-04-02 Oil-Dri Corporation Of America Oil bleaching method and composition for same
US6346286B1 (en) * 1995-04-26 2002-02-12 Oil-Dri Corporation Of America Sorptive purification for edible oils
JP2815562B2 (ja) * 1995-11-13 1998-10-27 植田製油株式会社 高度不飽和脂肪酸含有油脂の精製方法

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EP2052065A1 (fr) 2009-04-29
DE502007002286D1 (de) 2010-01-21
DE102006035064A1 (de) 2008-01-31
WO2008012072A1 (fr) 2008-01-31
ATE451443T1 (de) 2009-12-15

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