EP2361298B1 - Procédé de réduction de la teneur en 3-mcpd dans des huiles végétales raffinées - Google Patents

Procédé de réduction de la teneur en 3-mcpd dans des huiles végétales raffinées Download PDF

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Publication number
EP2361298B1
EP2361298B1 EP09771302.8A EP09771302A EP2361298B1 EP 2361298 B1 EP2361298 B1 EP 2361298B1 EP 09771302 A EP09771302 A EP 09771302A EP 2361298 B1 EP2361298 B1 EP 2361298B1
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EP
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Prior art keywords
oil
bleaching
acid
bleaching earth
mcpd
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EP09771302.8A
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German (de)
English (en)
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EP2361298A1 (fr
Inventor
Klaus Schurz
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Sued Chemie IP GmbH and Co KG
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Sued Chemie IP GmbH and Co KG
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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
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • 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
    • C11B3/006—Refining fats or fatty oils by extraction
    • 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
    • C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • 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
    • 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
    • C11B3/12—Refining fats or fatty oils by distillation
    • C11B3/14—Refining fats or fatty oils by distillation with the use of indifferent gases or vapours, e.g. steam

Definitions

  • the invention relates to a method for reducing the 3-monochloropropane-1,2-diol content in refined vegetable oils, wherein a crude oil is first degummed, so that a degummed oil is obtained, the degummed oil is mixed with a bleaching earth and bleached, wherein bleached oil is separated, the bleaching earth is separated from the bleached oil, so that a filter oil is obtained, and the filter oil is deodorized.
  • 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 amounts 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 natural active raw clay with small amounts of acid is applied and thus achieved an "in situ activation".
  • attapulgite and hormite containing have for this process Rohtone proven.
  • 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 subgroup of the SMBE is the Dry Milled Bleaching Earth (DMBE) .
  • the raw clay is generally treated with an aqueous solution of the acid for the manufacture of the SMBE, whereas the DMBE uses a solid acid, usually citric acid, for the activation grind the solid acid together with the raw clay.
  • 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 WO 2006/052974 A1 refers to seed oil compositions containing linoleic acid.
  • a process is described for refining crude oil wherein the crude oil is degummed by the addition of water or, alternatively, phosphoric acid and / or citric acid.
  • the degummed oil is bleached by adding bleach, as well as bleaching earth, to the heated degummed oil.
  • US 4,939,115 A describes a process for removing phospholipids and impurities, such as metal ions Ca, Mg, Fe, and Cu, in oil.
  • phospholipids and impurities such as metal ions Ca, Mg, Fe, and Cu.
  • a degumming with 1% water at 70 ° C takes place.
  • the bleaching of the degummed oil is carried out with amorphous silica.
  • WO 2006/131136 A1 discloses a process for refining fats and oils wherein the crude oil is bleached by treating it with a bleaching earth product containing a raw clay. The crude oil is also fed to a degumming stage, which may include pre-degumming with water and acid degumming.
  • 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. In order to separate the mucilage easier, is the end of the even more water are added, for example in a proportion of 0.2 wt .-%. After brief stirring, the lecithin phase is separated, for example by centrifugation. Subsequent bleaching of the degummed oil involves two stages, wet bleaching and vacuum bleaching.
  • the degummed oil is added 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.
  • a vacuum is applied (for example 100 mbar) and the oil is stirred for a further 30 minutes at 95.degree.
  • 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.
  • 3-monochloropropane-1,2-diol (3-MCPD) can be found in the production of foodstuffs, for example in the production of soy sauce, in baking and toasting, but also in the refining of vegetable oils and fats.
  • 3-MCPD has been shown to be carcinogenic.
  • its mutagenicity could be detected in vitro , but not in vivo.
  • 3-MCPD affects fertility in mammals.
  • 3-MCPD can be present in the food centers both in free or in bound form, for example in the form of an ester.
  • 3-MCPD was found in different fats and oils.
  • the concentration in vegetable fats and oils can range from several hundred to several thousand ppm, calculated as free 3-MCPD.
  • the mechanism by which 3-MCPD is formed in fat and oil refining has not yet been fully elucidated.
  • model studies have shown that chloride ions as well as glycerine as well as mono-, di- and triglycerides are potential starting materials in the formation of 3-MCPD.
  • the present invention has for its object to provide a method for refining oils, wherein a crude oil is first degummed, so that a degummed oil is obtained, the degummed oil is mixed with a bleaching earth and bleached, whereby a bleached oil is obtained Bleaching earth is separated from the bleached oil, so that a filter oil is obtained, and the filter oil is deodorized, which leads to the lowest possible formation of 3-MCPD.
  • the degumming of the crude oil is carried out only with water without the addition of acids.
  • the oil is then bleached at a temperature in the range of 80 to 100 ° C, preferably at a temperature of about 95 ° C.
  • degumming has a significant influence on the concentration of 3-MCPD which is formed during the refining of oils and fats, while the bleaching has a significantly lower influence or the concentration of bleaching earth increases the concentration of 3-MCPD.
  • MCPD in the refined oil or fat after degumming is lowered.
  • 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 then mixed with water and stirred at a relatively low temperature.
  • 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 less than 15% by weight, more preferably less than 10% by weight. According to one embodiment, the added amount of water at least 0.2 wt .-%, according to another embodiment at least 0.5 wt .-% and according to yet another embodiment at least 1% by weight. The percentages are based on the crude oil used.
  • the degumming is carried out without the addition of acids.
  • the degumming is performed at a relatively low temperature of less than 70 ° C, preferably less than 60 ° C, preferably in the range of 35 to 55 ° C, more preferably in the range of 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 separated from the degummed oil, for example, by centrifuging, decanting or by filtration. If the amount of water is less than 0.5% by weight, removal of the water phase may be omitted. However, it is preferred that even with smaller amounts of water, the water phase is separated from the degummed oil.
  • the degummed oil is heated to a temperature in the range of 80 to 100 ° C, preferably 90 to 98 ° C, preferably about 95 ° C. Excessive bleaching temperatures have been found to increase the level of 3-MCPD in the refined oil. Overheating of the oil should therefore be avoided.
  • the bleached earth is then added to the heated degummed oil. It has been found that when too low amounts of bleaching earth, the concentration of 3-MCPD or 3-MCPD precursors, which have formed during degumming, can not be reduced sufficiently.
  • the bleaching earth is therefore added to the heated degummed oil in an amount of more than 1.5% by weight, preferably in an amount in the range of from 2.0 to 3.0% by weight, based on the crude oil.
  • bleaching earth has only a low adsorption power for 3-MCPD or its precursors. It was found that 3-MCPD or whose precursors are contained in the oil only in amounts in the ppm range. However, an increase in bleaching amount used for bleaching above 1.5% by weight results in a marked reduction in the amount of 3-MCPD in the refined oil.
  • the oil After adding the bleaching earth to the heated oil, the oil is then bleached in a conventional manner.
  • the bleaching can be done by applying directly after addition of the bleaching earth vacuum, so without having previously given water to the crude oil.
  • the bleaching then takes place as a pure vacuum bleaching.
  • the vacuum bleaching is carried out at elevated temperature, more preferably at temperatures of 80 to 110 ° C.
  • the bleaching is carried out in at least two stages, initially wet bleaching followed by vacuum equalization.
  • 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 stirred at 80 to 100 ° C, more preferably 90 to 95 ° C.
  • 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 earth is separated from the bleached oil.
  • conventional methods can be used.
  • the bleaching earth can be allowed to sediment and the supernatant clear oil can be decanted off.
  • the bleached oil is filtered, for example through a paper filter, so that a filter oil is obtained.
  • oil obtained from the bleached oil is referred to as a filter oil, regardless of the method used to separate the bleaching earth.
  • the filter oil is finally deodorized.
  • usual methods are used under the usual conditions.
  • superheated steam is passed through the oil, whereby a Vollraffinat is obtained.
  • the superheated steam preferably has an outlet temperature in the range of 200 to 290 ° C.
  • the deodorization is preferably carried out for a period of 30 minutes to 2 hours.
  • the deodorization can be carried out in one stage, wherein the outlet temperature of the superheated steam is kept substantially constant. But it is also possible to carry out the deodorization in several stages, wherein the temperature of the superheated steam is changed during deodorization.
  • superheated steam is first introduced, which has a temperature in the range of 250 to 290 ° C. This first step is preferably carried out for a period of 20 to 45 minutes.
  • the exit temperature of the steam is lowered, preferably in a range of 200 to 240 ° C.
  • the superheated steam is then preferably passed through the oil for a further 30 to 120 minutes.
  • deodorization releases 3-MCPD, which the inventors believe to be previously bound in precursors, for example, glycerides or compounds derived therefrom.
  • surface-rich bleaching earths are preferably used.
  • the bleaching earth has a specific surface area of more than 175 m 2 / g, according to another embodiment a specific surface area of more than 220 m 2 / g, and according to another embodiment a specific surface area of more than 300 m 2 / g According to one embodiment, the bleaching earth has a specific surface area of less than 400 m 2 / g.
  • the bleaching earths used in the process according to the invention have a specific pore volume of more than 0.2 ml / g, more preferably more than 0.3 ml / g, particularly preferably a specific pore volume of more than 0.4 ml / g on.
  • the bleaching earth has a pore volume of more than 0.45 ml / g and according to another embodiment, a pore volume of less than 0.95 ml / g.
  • a bleaching earth is selected which has a pore volume in the range of 0.4 to 1.0 ml / g.
  • 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 bleaching earths is preferably more than 15 meq / 100 g, preferably more than 25 meq / 100 g and in one embodiment more than 40 meq / 100 g.
  • bleaching earths can be used in the process according to the invention.
  • both natural bleaching earths NABEs
  • acid-activated bleaching earths SBE
  • SBE surface-activated bleaching earths
  • HPBE highly active bleaching earths
  • the mode of activation of the bleaching earth used in the process according to the invention has an influence on the amount of 3-MCPD contained in the refined oil. It was surprisingly found that acid-activated bleaching earths lead to lower concentrations of 3-MCPD in the refined oil. This is particularly surprising since the addition of acid during degumming leads to an increase in the concentration of 3-MCPD in the refined oil, ie the formation of 3-MCPD or of precursors of this compound is presumably acid-catalyzed.
  • the acid activated bleaching earth as a 10% slurry in water, preferably has a pH of less than 5, and more preferably less than 4. In one embodiment, the pH of the slurry is greater than 2. In one embodiment, the slurry has a pH of less than 8.5, and in another embodiment has a pH of less than four. The pH is determined with a pH electrode.
  • SMBE surface-activated bleaching earths
  • These surface-activated bleaching earths are obtained by acid-plating a natural raw clay leaving excess acid on the clay. So no washing step is carried out after the activation.
  • the raw clay Before activation, the raw clay can be prepared in the usual way and, for example, dried or ground.
  • the surface activation of the raw clay can be carried out by covering the raw clay with a, preferably aqueous, solution of the acid used for the activation.
  • the assignment can be done, for example, by moving the raw clay and the solution of the acid is sprayed onto the raw clay. But there are also other methods possible to apply the solution of the acid to the raw clay, such as soaking.
  • 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.
  • the crude clay which is preferably provided in the form of a powder, in water.
  • 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 abandonment of 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 activation can be carried out with both inorganic and organic acids.
  • Suitable inorganic acids are, for example, sulfuric acid, phosphoric acid or else hydrochloric acid.
  • a suitable organic acid is, for example, citric acid.
  • the excess acid and the salts formed during activation are not washed out. Rather, after the task of acid, as usual in the acid activation, preferably no washing step is carried out, but the treated raw clay dried and then ground to the desired particle size.
  • a suitable acid is, for example, citric acid.
  • the grain size is set in the desired range.
  • the amount of acid used for activation is preferably selected to be greater than the ion exchange capacity of the raw clay, preferably in the range of 100 to 140% of the ion exchange capacity of the raw clay.
  • a highly active bleaching earth is preferably used as the acid-activated bleaching earth.
  • These highly active bleaching earths are obtained by extracting a crude clay at elevated temperature, preferably at about boiling heat, with a strong acid. Essentially, aluminum ions from the crystal structure removed. After extraction, the bleaching earth is separated from the aqueous phase, for example by filtration, and then washed with water. This method is known per se to the person skilled in the art. The highly activated bleaching earth is also ground to the desired grain size.
  • the grain size or the mean grain size of the bleaching earth should preferably be selected so that a complete and simple separation of the used bleaching earth from the refined product is 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.
  • the inventive method is suitable in itself for the refining of any oils and fats.
  • the method according to the invention is particularly suitable for the refining of vegetable oils.
  • 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.
  • the process according to the invention is suitable for the bleaching of palm oil.
  • 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, which are obtained from the evaluation of the adsorption isotherm according to BJH.
  • the total pore volume according to the BJH method refers to pores with a diameter of 2 to 130 nm.
  • 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.
  • a sample of crude palm oil is first heated to the temperature indicated in Table 1 for degumming and then dried and degassed for 15 minutes at 100 mbar. After degassing, the palm oil was added to the amount of 50% phosphoric acid or water indicated in Table 1 and stirred for 15 minutes at ambient pressure.
  • the aqueous phase was separated off (index "f” in Table 1), for the bleaching the oil was adjusted to the temperature indicated in Table 1 and then the amount of bleaching earth indicated in Table 1 was added.
  • the oil was first bleached for 20 minutes at atmospheric pressure and then for 30 minutes at a reduced pressure of 100 mbar.
  • the oil was filtered hot through a paper filter.
  • the filtered oil was still deodorized by first passing superheated steam having an exit temperature of 270 ° C for 30 minutes and then passing through the oil for 60 minutes superheated steam having an exit temperature of 240 ° C.
  • the concentration of 3-MCPD was determined. The results are summarized in Table 1.
  • the bleaching earths used in the examples have the properties listed in Table 2: Table 2: Properties of bleaching earths BE Cl pH SPO MPV 2 - 130 nm IUF (%) (m 2 / g) (ml / g) (meq / 100g) HPBE 1 0.02 3.1 257 0.35 21 Supr. 112 FF 0.01 2.3 183 0.75 nb HPBE2 0.05 3.2 293 0.44 29 Supr. 114 FF 0.03 3.5 347 0.48 Supr.

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  • Microbiology (AREA)
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Claims (10)

  1. Procédé de réduction de la teneur en 3-monochloropropane-1,2-diol dans des huiles végétales raffinées, dans lequel une huile brute est tout d'abord débourbée, de manière à obtenir une huile débourbée, l'huile débourbée est mélangé avec une terre décolorante et blanchie, une huile blanchie étant obtenue, la terre décolorante est séparée de l'huile blanchie, de manière à obtenir une huile filtrée, et l'huile filtrée est désodorisée, caractérisé en ce que
    - de l'eau est ajoutée à l'huile brute pour le débourbage, et le débourbage est réalisé sans ajout d'acide à une température inférieure à 70 °C,
    - l'huile débourbée est portée à une température dans la plage allant de 80 à 110 °C, et la terre décolorante est ajoutée à l'huile débourbée chauffée en une quantité de plus de 1,5 % en poids,
    - le blanchiment est réalisé à une température dans la plage allant de 80 à 100 °C.
  2. Procédé selon la revendication 1, caractérisé en ce que de l'eau est ajoutée à l'huile brute pour le débourbage en une quantité de moins de 15 % en poids.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'huile débourbée est séparée d'une phase aqueuse.
  4. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la terre décolorante présente une surface spécifique de plus de 175 m2/g.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la terre décolorante présente un volume de pores de plus de 0,2 ml/g.
  6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la capacité d'échange d'ions de la terre décolorante est de plus de 15 meq/100 g.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la terre décolorante est une terre décolorante activée acide.
  8. Procédé selon la revendication 7, caractérisé en ce que la terre décolorante activée acide est une HPBE.
  9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'huile est une huile végétale.
  10. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'huile est l'huile de palme.
EP09771302.8A 2008-12-02 2009-12-01 Procédé de réduction de la teneur en 3-mcpd dans des huiles végétales raffinées Not-in-force EP2361298B1 (fr)

Priority Applications (1)

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PL09771302T PL2361298T3 (pl) 2008-12-02 2009-12-01 Sposób zmniejszania zawartości 3-MCPD w rafinowanych olejach roślinnych

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008060059A DE102008060059A1 (de) 2008-12-02 2008-12-02 Verfahren zur Reduzierung des 3-MCPD-Gehalts in raffinierten Pflanzenölen
PCT/EP2009/008557 WO2010063450A1 (fr) 2008-12-02 2009-12-01 Procédé de réduction de la teneur en 3-mcpd dans des huiles végétales raffinées

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EP2361298A1 EP2361298A1 (fr) 2011-08-31
EP2361298B1 true EP2361298B1 (fr) 2017-05-17

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EP (1) EP2361298B1 (fr)
DE (1) DE102008060059A1 (fr)
DK (1) DK2361298T3 (fr)
ES (1) ES2637347T3 (fr)
HU (1) HUE035623T2 (fr)
PL (1) PL2361298T3 (fr)
PT (1) PT2361298T (fr)
WO (1) WO2010063450A1 (fr)

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WO2014012548A1 (fr) 2012-07-18 2014-01-23 Aarhuskarlshamn Ab Réduction de composés de mcpd dans l'huile végétale raffinée pour aliments
WO2014081279A1 (fr) 2012-11-21 2014-05-30 Universiti Putra Malaysia Procédé de raffinage d'huile de palme perfectionné
CN103525548B (zh) * 2013-11-06 2014-10-01 江南大学 一种用于降低植物油中氯源及3-氯-1,2-丙二醇酯前体物质含量的脱胶方法
LT3154374T (lt) 2014-05-16 2018-12-10 Sime Darby Malaysia Berhad Neapdoroto palmių vaisių aliejaus produkto rafinavimo būdas
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EP3098292A1 (fr) 2015-05-27 2016-11-30 Evonik Degussa GmbH Procédé de raffinage d'huile glycéridique comprenant un traitement de sel d'ammonium quaternaire basique
EP3098293A1 (fr) 2015-05-27 2016-11-30 Evonik Degussa GmbH Procédé d'élimination de métaux à partir d'une huile de glycérides contenant un métal comprenant le traitement d'un sel d'ammonium quaternaire basique
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WO2018156013A1 (fr) 2017-02-21 2018-08-30 Sime Darby Plantation Berhad Procédé de production d'huile de fruit de palmier raffinée
EP3321348B1 (fr) 2017-08-23 2019-12-18 Bunge Loders Croklaan B.V. Procédé de raffinage d'huile végétale avec suppression des impuretés indésirables
EP3483237A1 (fr) 2017-11-10 2019-05-15 Evonik Degussa GmbH Procédé d'extraction d'acides gras d'une huile glycéridique
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PL238351B1 (pl) 2018-08-27 2021-08-09 Komagra Spolka Z Ograniczona Odpowiedzialnoscia Sposób wytwarzania rafinowanego oleju jadalnego o niskiej zawartości niepożądanych 3-MPCD, 2-MPCD oraz glicydów
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Publication number Publication date
PT2361298T (pt) 2017-08-25
PL2361298T3 (pl) 2017-10-31
EP2361298A1 (fr) 2011-08-31
WO2010063450A1 (fr) 2010-06-10
DK2361298T3 (en) 2017-07-24
DE102008060059A1 (de) 2010-06-10
HUE035623T2 (en) 2018-05-28
ES2637347T3 (es) 2017-10-11

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