EP3227418B1 - Procédé continu de fractionnement à sec d'huiles glycéridiques - Google Patents

Procédé continu de fractionnement à sec d'huiles glycéridiques Download PDF

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EP3227418B1
EP3227418B1 EP15766668.6A EP15766668A EP3227418B1 EP 3227418 B1 EP3227418 B1 EP 3227418B1 EP 15766668 A EP15766668 A EP 15766668A EP 3227418 B1 EP3227418 B1 EP 3227418B1
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Prior art keywords
glyceride oil
oil
temperature
glyceride
sop
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German (de)
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EP3227418A1 (fr
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Noor Hidayu OTHMAN
Ahmadilfitri MD NOOR
Mohd Suria Affandi Yusoff
Syed Said SYED SAGGAF
Ahmad Jaril ASIS
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Sime Darby Plantation Intellectual Property Sdn Bhd
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Sime Darby Plantation Intellectual Property Sdn Bhd
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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
    • C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points

Definitions

  • the present invention provides a continuous process for the dry fractionation of glyceride oils. More particularly, the present invention concerns a continuous process of dry fractionating a glyceride oil, said process comprising:
  • the present disclosure further relates to a system for continuous dry fractionation of glyceride oils, which is useful for understanding the invention without being part of it, comprising: a feeding vessel; a plate heat exchanger; a homogenizer; a sequence of at least 2 crystallizers; and a solid-liquid separator having an inlet that is connected with the outlet of the last crystallizer.
  • Fractionation processes are central to the modern edible oil and fat processing industry, especially to the palm oil processing industry. Starting from a glyceride oil with given melting characteristics, these processes permit to recover separate oil fractions with different melting profiles and different viscosities. Since a specific melting profile is required depending on the application of the oil (e.g. more liquid at room temperature for spreads, more solid at room temperature for margarines), fractionation opens up a larger variety of possibilities for applying the initial glyceride oil, thereby adding value to its use.
  • Fractionation involves creating circumstances that induce a partial (fractional) crystallization of the oil.
  • a solid fraction is formed (stearin) which can then be separated from the remaining liquid phase (olein).
  • the higher melting triglycerides contained in the oil will crystallize into the solid fraction and the lower melting triglycerides will remain in liquid form.
  • the stearin fraction of the oil typically has a high solids content, while the olein fraction of the oil typically has a low solids content.
  • the quality of the olein fraction depends only on the crystallization step; meanwhile the quality of the stearin fraction depends on both crystallization and the separation step.
  • the key challenge in fractionation is to use crystallization and separation process conditions that allow for a high quality and yield of the olein and stearin fractions.
  • Dry fractionation In dry fractionation, melted oil is cooled in a controlled way in order to crystallize it through a batch crystallization process. The liquid fraction is then physically separated from the solid fraction by means of vacuum filter or a membrane filter press (M. Kellens, 1994). In this process, no additives are used in the crystallization process and no supplementary post-treatment of the finished products is required. Dry fractionation thus is a purely natural and physical oil modification process that creates no undesirable byproducts. It is the simplest, environmental friendliest and cheapest fractionation process, which can satisfy today's increasing environmental and health concerns by fully or partially replacing the chemical modification processes (R.E. Timms, 2005).
  • Controlled crystallization of the melt is considered as the backbone of any dry-fractionation process as this determines the grades of the olein and stearin fractions obtained.
  • olein and stearin with various degrees of unsaturation i.e. different iodine values (IV) may be obtained.
  • Controlled cooling during dry fractionation is achieved by pre-selecting a cooling mode based on the heat exchange fluid temperature, the oil temperature and the temperature difference between them (delta T). Because heat is released when a hump occurs, the temperature is affected and the switching of pre-selected cooling mode during the crystallization process is delayed. This causes the crystallization period to be longer than normal, causing the oil slurry to become more viscous or even sometimes jellified. These properties negatively affect the filtration performance because the soft stearin cake tends to stick to the membrane plate when the membrane filter press is depressurized.
  • IN 2028/DEL/2011 describes a continuous flow method of crystallizing saturated fat from oil comprising first subjecting the oil to fast cooling followed by slow cooling of the oil. After slow cooling, the oil is again subjected to fast cooling. The fast cooling of the oil is carried out to a temperature above the melting point of the oil at which nuclei formation of the saturated fat is initiated. This is followed by the slow cooling of the oil to a temperature below the melting point of the oil to facilitate crystal formation and natural hardening of crystals. The method comprises of further fast cooling the oil to a temperature that facilitates crystal maturation of the saturated fat.
  • WO 98/51753 discloses a method of fractionating a mass of triglycerides, said method comprising the steps of: (a) heating the mixed mass of triglycerides to form a melt; (b) cooling the melt to a temperature below the temperature sufficient for crystal growth and above the critical temperature of the melt to form a supercooled solution; (c) inputting energy to said supercooled solution sufficient to form crystal nuclei; and (d) growing said crystal nuclei into crystals in a static solution.
  • the inventors have developed an improved process for the continuous fractionation of glyceride oils comprising at least 80 wt% of palm oil that enables the manufacture of a high quality olein fraction in high yield and in a relatively short period of time.
  • the continuous dry fractionation process of the present invention comprises the following successive steps:
  • the present process is particularly suited for dry fractionation of palm oil.
  • the process can suitably be used to produce palm oleins having an iodine value (IV) in the range of 56 to 64.
  • the liquid glyceride oil is kept a temperature within 1°C of the prenucleation temperature T p for at least 0.5 hour, said T p being 0.5-10°C below the solidification onset point (SOP) of the glyceride oil, the SOP of the glyceride oil being the minimum temperature at which the glyceride oil has a N-value of 0%.
  • SOP solidification onset point
  • the SOP is significantly higher than the slip melting point of the same glyceride oil. This is because at the slip melting point these glyceride oils contain some crystalline fat. For instance, palm oil typically has a slip melting point of 37°C.
  • palm oil has a solid fat content at it is slip melting point of around 5%.
  • Temperature (°C) Solid fat content (%) 10 52-56 15 35-42 20 23.6-30.7 25 16-18.5 30 7.5-9.5 35 3.7-6.6 40 0.5-4 45 0-0.7 50 0 1 determined by pulsed NMR
  • the present disclosure also provides a system for continuous dry fractionation of glyceride oils, which is useful for understanding the invention without being part of it, comprising:
  • one aspect of the invention relates to a continuous process of dry fractionating a glyceride oil comprising at least 80 wt% of palm oil, said process comprising:
  • glycolide refers to esters of glycerol, one or more fatty acids and optionally another acid, e.g. phosphoric acid.
  • oil refers to a lipid material that may be liquid or solid at ambient temperature (20°C).
  • fat refers to an oil that is solid or semi-solid at 20°C.
  • solidification onset point or "SOP” is the minimum temperature at which the glyceride oil has a N-value of 0%. For palm oil the SOP typically is around 45°C.
  • N t The N-value at a temperature of t°C (N t ) refers to the solid fat content of the oil at that temperature of t °C as measured by means of ISO 8292 - Animal and vegetable fats and oils - Determination of solid fat content - Pulsed nuclear magnetic resonance method.
  • liquid glyceride oil employed in the process according to the present invention has no crystal memory.
  • the glyceride oil used is first heated until all its crystal memory is destroyed in order to provide the liquid glyceride oil.
  • the glyceride oil is first heated to a temperature above the SOP, more preferably to a temperature that is at least 5°C higher than the SOP, even more preferably to a temperature that is at least 10°C higher than the SOP.
  • the glyceride oil is heated to a temperature of at least 60°C, more preferably of at least 65°C.
  • the process according to the present invention is preferably used to fractionate a glyceride oil with a SOP of at least 25°C. More preferably, the glyceride oil has a SOP in the range of 30-55°C.
  • the glyceride oil comprises at least 80 wt.%, more preferably at least 90 wt.% and most preferably at least 95 wt.% of palm oil.
  • Said palm oil is preferably a refined bleached deodorized palm oil (RBDPO).
  • RBDPO bleached deodorized palm oil
  • the liquid glyceride oil is precooled in order to shorten the cooling time required in the further process steps.
  • a heat exchanger is used to precool the liquid glyceride oil. It is preferred that this heat exchanger is a plate heat exchanger.
  • the precooling of the liquid glyceride oil in the present process comprises passing the liquid glyceride oil through a plate heat exchanger unit. Fast cooling is achieved by enhancing an effective and efficient heat transfer coefficient between the liquid glyceride oil and cooling medium (e.g. chilled water) supplied to the heat exchanger unit.
  • cooling medium e.g. chilled water
  • the temperature of the liquid glyceride oil is reduced in the heat exchanger with at least 8°C, more preferably with at least 10°C and most preferably with 12-30°C.
  • the temperature of the glyceride oil is typically reduced to a temperature that is not lower than 8°C below the SOP, more preferably to a temperature that is not lower than 5°C below the SOP and most preferably to a temperature that is not lower than 2°C below the SOP and not higher than 3°C above the SOP.
  • the temperature of the precooled glyceride oil is 40-55 °C, more preferably 42-52 °C and most preferably 45-50 °C.
  • the cooling rate used to precool the liquid glyceride oil is preferably of at least 2°C/min, more preferably 3-10 °C/min.
  • precursors of fat crystals e.g. small uniform nuclei of trisaturated triglycerides
  • T p the prenucleation temperature
  • the SMP is the temperature at which a column of the solid fat begins to rise in a tube due to buoyancy and because the outside surface of the solid fat is molten.
  • the SMP may be measured by means of ISO 6321:2002 - Animal and vegetable fats and oils - Determination of melting point in open capillary tubes (slip point).
  • T p is 0.7-8°C below the SOP, more preferably at least 0.8-7°C below the SOP and most preferably 1-5°C below the SOP.
  • T p lies in the range of 38°C to 48°C, more preferably in the range of 39°C to 45°C and most preferably in the range of 40°C to 43°C.
  • prenucleation of the precooled glyceride oil takes place during the homogenization step.
  • the homogenization step comprises passing the precooled glyceride oil through a homogenizer.
  • the temperature of the precooled glyceride oil may suitable be further reduced in the homogenizer, especially if the precooled glyceride oil has a temperature that exceeds the SOP.
  • the temperature of the cooled glyceride oil is reduced with 0.5-10°C, more preferably with 1-8°C and most preferably with 2-6°C.
  • the homogenization step is carried out using a homogenizer that comprises a multiple pitch blade impeller.
  • this multiple pitch blade impeller is mounted on vertical shaft to provide a better agitation during the homogenization process.
  • the temperature of the glyceride oil is controlled and kept within 1°C, preferably within 0.5°C of T p for at least 0.5 hour, preferably for at least 1 hour.
  • said oil is passed through one or more crystallizers in the crystallization step (d).
  • the glyceride oil is passed upwards through the one or more crystallizers.
  • the one or more crystallizers used in the present process comprise a stirrer or agitator with or without a surface scraper. More preferably, the one or more crystallizers used in the present process comprise a multiple flat blade impeller. Typically, said multiple flat blade impeller is mounted on a vertical shaft.
  • the one or more crystallizers employed in the present process are tubular crystallizers that are cooled by a cooling medium that moves through the crystallizer in counterflow with the stream of the glyceride oil.
  • the cooling medium is applied both externally and internally to the one or more crystallizers.
  • crystallization is induced in a controlled fashion comprising reducing the temperature of the prenucleated glyceride oil to a crystallization temperature T c at which fat crystals form.
  • T c crystallization temperature
  • the temperature of the prenucleated glyceride oil is reduced with at least 10°C, more preferably with at least 15 °C and most preferably with at least 20 °C.
  • T c is in the range of 12-30°C, more preferably in the range of 15-28°C.
  • the temperature of the glyceride oil in the crystallizers is controlled and kept at a temperature within 1°C of T c , preferably within 0.5°C of T c for at least 0.5 our, more preferably of at least 0.8 hour, and most preferably for at least 1 hour.
  • Crystallization is a highly delicate process.
  • the quality and yield of the produced crystals is very sensitive to the temperature gradient applied, to the temperature used and to the length of the time period that that temperature is applied. It was found that the benefits of the invention are particularly achieved when the separatable fat crystals are formed in the prenucleated glyceride oil in at least two different temperature and time controlled stages: by first further nucleating the small uniform fat nuclei to facilitate crystal formation and subsequently using the fat crystal nuclei thus produced to crystallize into separatable fat crystals.
  • the first nucleation stage involves a faster cooling of the oil than the second crystallization stage.
  • the crystallizing of the prenucleated glyceride oil comprises:
  • the process of the present invention offers the advantage that it employs relatively short crystallization times.
  • the total residence time of the glyceride oil in the one or more primary crystallizers is in the range 0.5-2.5 hours, most preferably in the range of 0.8-2 hours.
  • ⁇ T 1 is in the range of 9-18°C, more preferably in the range of 10-15°C.
  • the nucleation temperature T n preferably is in the range of 27-38°C, more preferably in the range of 28-36°C and most preferably in the range of 29-35°C
  • the temperature reduction ⁇ T 1 is typically achieved in a period t 1 of 0.7-2.5 hours, most preferably of 1-2 hours.
  • mild agitation is applied in the one or more primary crystallizers in order to enhance crystal formation.
  • the mild agitation is performed at a speed of less than 25 rpm, more preferably less than 20 rpm.
  • the nucleated glyceride oil from the one or more primary crystallizers is transferred to the one or more secondary crystallizers by a gravity flow condition.
  • the total residence time of the glyceride oil in the one or more secondary crystallizers is at least 0.5 hours, more preferably at least 1 hour.
  • the residence time in the one or more secondary crystallizers depends on level of unsaturation of the olein fraction that is produced by the process. The higher the level of unsaturation, the longer the total residence time that is required to produce the olein.
  • the present process may be used, for instance, to produce a highly unsatured palm olein with an iodine value of 60 or more.
  • two or more secondary crystallizers to gradually reduce the temperature of the glyceride oil to e.g. less than 20 °C before removing the fat crystals (stearin) and recovering the olein fraction.
  • ⁇ T 2 is in the range of 4-22°C, more preferably in the range of 4.5-20°C and most preferably 5-18°C.
  • the glyceride oil is palm oil having an iodine value of 50-55, a SMP of 33-39°C and a SOP of 42-52°C, T c is in the range of 18-26°C and the palm olein obtained has an iodine value of 56-58.
  • the glyceride oil is palm oil having an iodine value of 50-55, a SMP of 33-39°C and a SOP of 42-52°C, T c is in the range of 18-22°C and the palm olein obtained has an iodine value of 58-60
  • the glyceride oil is palm oil having an iodine value of 50-55, a SMP of 33-39°C and a SOP of 42-52°C, T c is in the range of 15-21°C and the palm olein obtained has an iodine value of 60-62.
  • the glyceride oil is palm oil having an iodine value of 50-55, a SMP of 33-39°C and a SOP of 42-52°C, T c is in the range of 10-18°C and the palm olein obtained has an iodine value of at least 62.
  • the glyceride oil is a palm oil having an iodine value of 50-55, a SMP of 33-39°C and a SOP of 42-52°C, and in said process the fat crystals that are removed from the glyceride oil represent 10-20 wt.% of said glyceride oil, and these fat crystals have an iodine value of 25-40 and a SMP of 45-56°C.
  • mild agitation is applied in the one or more secondary crystallizers in order to maintain crystal formation and provide enough heat transfer during the crystallization process.
  • the mild agitation is performed at a speed of less than 15 rpm.
  • the crystallized glyceride oil from the one or more secondary crystallizers is subjected to a separation technique in order to remove the separable fat crystals (stearin) from the crystallized glyceride oil and recovering an olein fraction of the glyceride oil.
  • the separable fat crystals are removed from the crystallized glyceride oil by means of centrifugation and/or filtration. Centrifugation may refer to, for instance, a nozzle centrifuge, centrifugal filter or centrifugal decanter.
  • the separable fat crystals are removed from the crystallized glyceride oil by means of filtration, even more preferably by membrane filtration or hydraulic filtration and most preferably by membrane filtration.
  • step d2 of the present process comprises passing the nucleated glyceride oil through a sequence of at least two secondary crystallizers, including a first secondary crystallizer and a second secondary crystallizer, wherein the temperature of the nucleated glyceride oil is reduced with 4-8°C in the first secondary crystallizer and the residence time in the first crystallizer is at least 0.5 hour, and wherein the temperature of the glyceride oil is reduced with 3-6°C in the second secondary crystallizer and the residence time within the second crystallizer is at least 0.5 hour.
  • the temperature of the nucleated glyceride oil is reduced with 4-8°C, more preferably with 3-6°C in the first secondary crystallizer.
  • the temperature of the nucleated glyceride oil is reduced in the first secondary crystallizer to 28°C or below and more preferably to 27°C or below.
  • the residence time in the first secondary crystallizer is at least 0.5 hour, more typically at least 1 hour.
  • the temperature of the glyceride oil is reduced with 3-6°C, more preferably with 3-4°C in the second secondary crystallizer, even more preferably to 24°C or below and most preferably to 22°C or below.
  • the residence time in second secondary crystallizer is at least 0.5 hour, more typically at least 1 hour.
  • the temperature of the glyceride oil is reduced with 0.5-2°C, more preferably with 0.5-1 °C in each of the further secondary crystallizers.
  • the residence time in each of the further secondary crystallizers is at least 0.5 hour, more typically at least 1 hour.
  • prenucleation in the homogenization stage and crystallization in the crystallization stage are suitably carried out under agitation.
  • the level of agitation employed in the crystallization stage is substantially lower than in the homogenization stage. This is because the glyceride oil typically contains larger crystals in the crystallization stage that should not be damaged.
  • the homogenization of the precooled glyceride oil comprises passing the precooled glyceride oil through a homogenizer comprising one or more rotating blades and the amount of mechanical power that is applied to the glyceride oil within the homogenizer exceeds 1x10 -3 W/kg
  • the crystallizing of the prenucleated glyceride oil comprises passing the prenucleated glyceride oil through one or more tubular crystallizers comprising one or more rotating blades, wherein the amount of mechanical power that is applied to the glyceride oil within the crystallizer does not exceed 0.1 W/kg, and wherein the amount of mechanical power that.is applied in the homogenizer is at least 2 times as high, more preferably at least 3 times as high and most preferably at least 4 times as high as the amount of mechanical power that is applied during the cooling of the prenucleated glyceride oil in each of the one or more tubular crystallizers.
  • the present disclosure also relates to a system for continuous dry fractionation of glyceride oils, which is useful for understanding the invention without being part of it, comprising:
  • the homogenizer comprises a multiple pitch blade impeller.
  • the at least two crystallizers comprise a multiple flat blade impeller.
  • FIG. 1 is a block flow diagram of a continuous process for the dry fractionation of glyceride oils in accordance to the present invention.
  • the diagram comprises 6 sections:
  • FIG.2 is a process flow diagram showing the process units for precooling, homogenization and continuous crystallization of glyceride oil in the continuous dry fractionation process in accordance to the present invention.
  • the oil feeding section comprises a feed tank (A') containing a recycle pipeline to provide a continuous agitation during the heating process and for a better heat transfer circulation.
  • the precooling section comprises a plate heat exchanger unit (B') with chilled water that serves as a fast cooling medium to absorb heat from the hot feed oil line.
  • the steam line tracing is also included in case that encrustation of the oil would occur in the oil line.
  • the chilled water supplied is controlled at a temperature of at least 15°C or lower to efficiently cool the hot feed oil before being transferred into homogenizer unit.
  • the homogenization section comprises a homogenizer unit (C') that is equipped with a multiple pitch blade impeller mounted on a vertical shaft. This agitator serves to continuously agitate the feed oil during the homogenization process as well as to maintain the desired oil temperature before subjecting said oil to the crystallization process.
  • C' homogenizer unit
  • This agitator serves to continuously agitate the feed oil during the homogenization process as well as to maintain the desired oil temperature before subjecting said oil to the crystallization process.
  • the crystallization section comprises six crystallizers unit denoted as D'1, D'2, D'3, D'4, D'5 and D'6. It is known in the art that crystallizer units are basically equipped with internal cooling coils and/or cooling fins and/or an external jacket depending on the scale of production or size of crystallizer used. In the preferred embodiments of present invention, all crystallizers unit are equipped with a multiple flat blade impeller mounted on a vertical shaft as an agitator, an internal cooling coil and an external cooling jacket to provide sufficient heat transfer coefficient during the crystallization process. The internal cooling fins may be used to provide a better heat transfer and cooling effect inside the crystallizer without departing from the present embodiment.
  • the filtration section may comprise a hydraulic filter press or a membrane filter press (F') to separate the high melting triglycerides (stearin fraction) from the low melting triglycerides (olein fraction).
  • F' membrane filter press
  • the bottom line of crystallizer unit D'n may become an inlet line to receive the glyceride oil from crystallizer unit D'(n-1) or an outlet line to transfer the crystallized glyceride oil to the filtration section F', where n is 3 or higher.
  • Iodine value (IV) indicates the degree of unsaturation of oil. It is measured according to MPOB test method p3.2:2004, a method described in Ainie et al., "Determination of Iodine Value (WJIS) for Palm Oil and Palm Oil Products", p3.2:2004 . This method is technically equivalent to an industrial method described in ISO3961:1996, "Animal and Vegetable Fat and Oils".
  • Cloud point is the temperature at which the oil begins to cloud, following crystallisation under controlled cooling conditions. It is related to the unsaturation of the oil, and decreases as unsaturation of the oil increases.
  • the standard cloud point for palm olein IV56 is 10°C (max), for palm olein IV58 it is 8°C (max), for palm olein IV60 it is 6°C (max) and for palm olein IV62 to IV64 it is 3°C to 4°C (max).
  • the slip melting point is a temperature at which a column of fat of specified length starts to rise in an open capillary tube. It is determined according to MPOB test method 25 p4.2:2004, a method described in Ainie et al., "Method of Test for Palm Oil and Palm Oil Products: Determination of Slip Melting Point", p4.2:2004 .
  • the standard slip melting point of refined palm oil is 33°C to 39°C
  • RBD palm stearin is 47°C to 54°C
  • RBD palm olein is 19 °C to 24°C.
  • RBD palm oil with iodine value (hereinafter referred as IV) of 52 was heated at temperature of 60°C to 70°C in a 70kg feed tank to destroy the crystals memory.
  • the melt was then precooled to a temperature of 45-50°C in a continuous fashion by passing it through a plate heat exchanger (cooler) into a 50L homogenizer unit where it was kept agitated and maintained at temperature of 40°C to 43°C.
  • the homogenized precooled oil was continuously transferred from the homogenizer to the bottom of a jacketed crystallizer 1 and filled up until it overflowed to the next crystallizer unit.
  • Crystallizer 1 was supplied with cooled water inside the cooling coil and external jacketed as a cooling medium. It was continuously agitated at 14rpm to provide a sufficient heat transfer coefficient to the wall of crystallizer and kept the slurry moving.
  • the oil inside the crystallizer 1 was cooled to obtain an end oil temperature between 30°C to 34 °C when it about to overflow and transferred to the bottom of crystallizer 2.
  • the stirrer speed in the crystallizer 2 was set slower than crystallizer 1 of about 12rpm to prevent crystal damage.
  • the oil temperature in the crystallizer 2 was further reduced to maintain crystal growth until it achieved an oil temperature of about 25°C to 27°C before overflow and transfer to the next crystallizer unit (crystallizer 3).
  • the conditions in of crystallizer 3 were set similar to achieve an end oil cooling temperature of about 24°C to 25°C.
  • the glyceride oil exiting from crystallizer 3 was subjected to a filtration process.
  • the slurry was withdrawn from the bottom of crystallizer 3 and pumped to a membrane filter press to obtain the olein and stearin fractions.
  • All the three crystallizer units had similar volume capacity of 25L each.
  • the oil flow rate from homogenizer unit to the series of crystallizer unit was maintained along the continuous crystallization process.
  • continuous crystallization of palm oil had produced 2% to 4.5% yield higher than batch process with more than 40% reduction in total crystallization period.
  • the product consistency of palm oil dry fractionation by continuous crystallization of palm oil were not much different within the same processing condition.
  • the olein produced was varies with average of IV56.6 (condition 1), IV57.4 (condition 2) and IV 56.86 (condition 3), respectively.
  • the highest yield recorded was 84% according to processing condition 3 at end cooling oil temperature of 34°C (crystallizer 1), followed by 26°C (crystallizer 2) and 25 °C (buffer) before subjected to filtration process. Beside it can be observed that the quality of olein obtained that varies from IV56.42 to IV57.76 was very promising with CP of 8°C to 9.5°C and SMP below 24°C (max).

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Claims (11)

  1. Procédé continu de fractionnement à sec d'une huile de glycéride comprenant au moins 80 % en poids d'huile de palme, ledit procédé comprenant :
    (a) se procurer une huile de glycéride liquide ayant une température qui est d'au moins 5°C supérieure au point de début de solidification (SOP) de l'huile de glycéride, le SOP de l'huile de glycéride étant la température minimale à laquelle l'huile de glycéride a une valeur N de 0 % ;
    (b) pré-refroidir l'huile de glycéride liquide à une allure de refroidissement d'au moins 1°C/min en faisant passer l'huile de glycéride à travers un échangeur de chaleur pour réduire la température de l'huile de glycéride liquide d'au moins 5°C à une température qui n'est pas inférieure à 10°C au-dessous du SOP et qui n'est pas supérieure à 5°C au-dessus du SOP ;
    (c) homogénéiser l'huile de glycéride pré-refroidie pour produire une huile de glycéride de pré-nucléation en faisant passer l'huile de glycéride pré-refroidie à travers un homogénéiseur dans lequel la température de l'huile de glycéride est maintenue à une température dans les 1°C de la température de pré-nucléation Tp pendant au moins 0,5 heure, ladite Tp étant de 0,5-10°C au-dessous du SOP ;
    (d) faire cristalliser l'huile de glycéride de pré-nucléation pour produire une huile de glycéride cristallisée contenant des cristaux de graisse séparables en faisant passer l'huile de glycéride de pré-nucléation à travers un ou plusieurs cristalliseurs pour réduire la température de l'huile de glycéride de pré-nucléation d'au moins 10°C à une température de cristallisation Tc et en maintenant l'huile de glycéride à une température dans les 1°C de la Tc pendant au moins 1 heure ; et
    (e) retirer les cristaux de graisse séparables de l'huile de glycéride cristallisée et récupérer une fraction d'oléine de l'huile de glycéride.
  2. Procédé selon la revendication 1, dans lequel l'huile de glycéride a un SOP se situant dans la plage de 30-55°C.
  3. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'échangeur de chaleur qui est utilisé pour pré-refroidir l'huile de glycéride liquide est un échangeur de chaleur à plaques.
  4. Procédé selon l'une quelconque des revendications précédentes, dans lequel la Tp dépasse le point de fusion par glissement (SMP) de l'huile de glycéride.
  5. Procédé selon l'une quelconque des revendications précédentes, dans lequel la Tp se situe dans la plage de 40°C à 55°C, de préférence dans la plage de 40°C à 50°C.
  6. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'homogénéiseur comprend une hélice à lames à pas multiples.
  7. Procédé selon l'une quelconque des revendications précédentes, dans lequel la Tc se situe dans la plage de 12-30°C.
  8. Procédé selon l'une quelconque des revendications précédentes, dans lequel la cristallisation de l'huile de glycéride de pré-nucléation comprend :
    (d1) faire passer l'huile de glycéride de pré-nucléation à travers un ou plusieurs cristalliseurs primaires pour produire une huile de glycéride de nucléation contenant des noyaux de cristaux de graisse par réduction de la température de l'huile de glycéride de pré-nucléation d'au moins ΔT1°C à une température de nucléation Tn qui est de 8-20°C au-dessous du SOP de l'huile de glycéride, ladite réduction de température étant obtenue dans une période t1 de 0,5-3 heures ; et
    (d2) faire passer l'huile de glycéride de pré-nucléation à travers un ou plusieurs cristalliseurs secondaires pour produire l'huile de glycéride cristallisée par réduction de la température de l'huile de glycéride de nucléation d'au moins ΔT2°C et maintenir l'huile de glycéride à une température se situant dans les 1°C de Tc pendant une période t2 de 1-20 heures ;
    dans lequel les étapes de refroidissement (d1) et (d2) sont effectuées dans des conditions d'agitation douce ; et dans lequel ΔT1 et ΔT2 satisfont les exigences suivantes : 8 ≤ ΔT 1 ≤ 20 ;
    Figure imgb0010
     3 ≤ ΔT 2 ≤ 25 ;
    Figure imgb0011
     ΔT 2 / t 2 ≤ 0,7 ΔT 1 / t 1 .
    Figure imgb0012
  9. Procédé selon la revendication 8, dans lequel la température de nucléation Tn se situe dans la plage de 30°C à 36°C.
  10. Procédé selon l'une des revendications 8 ou 9, dans lequel ΔT1 se situe dans la plage de 9-15°C.
  11. Procédé selon l'une quelconque des revendications précédentes, dans lequel l'huile de glycéride est une huile de palme ayant un indice d'iode de 50-55, un SMP de 33-39°C et un SOP de 42-52°C, et dans lequel une oléine de palme est obtenue après retrait des cristaux de graisse, ladite oléine de palme représentant 80-90 % en poids de ladite huile de glycéride, ayant un indice d'iode d'au moins 56.
EP15766668.6A 2014-12-03 2015-07-16 Procédé continu de fractionnement à sec d'huiles glycéridiques Active EP3227418B1 (fr)

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MYPI2014703630A MY184018A (en) 2014-12-03 2014-12-03 Continuous process for dry fractionation of glyceride oils
PCT/MY2015/000059 WO2016089196A1 (fr) 2014-12-03 2015-07-16 Procédé continu de fractionnement à sec d'huiles glycéridiques

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CN108837551B (zh) * 2018-07-28 2024-04-02 湖南懋天世纪新材料有限公司 一种超细仲钨酸铵蒸发结晶装置及结晶方法
CN110257169A (zh) * 2019-06-12 2019-09-20 深圳精益油脂技术有限公司 一种制备低缩水甘油酯及低3-mcpd酯含量的棕榈油的方法
AU2021234620B2 (en) * 2020-03-10 2023-12-07 LIEW, Heng Wen Dry fractionation of edible oil

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GB1120456A (en) * 1964-12-14 1968-07-17 Ranchers Cotton Oil Method of separating components of oleaginous mixtures by fractional crystallization
DE2901328C2 (de) * 1979-01-15 1985-07-25 Walter Rau Lebensmittelwerke GmbH & Co. KG, 4517 Hilter Verfahren zum selektiven Gewinnen von Triglyceriden oder Gemischen von Triglyceriden höherer Fettsäuren in kristalliner Form aus Naturfetten
CA1301775C (fr) * 1986-06-04 1992-05-26 Karel Petrus Agnes Maria Van Putte Fractionnement de melanges de matieres grasses
DE4132892A1 (de) * 1991-10-04 1993-04-22 Krupp Maschinentechnik Stoffgemischfraktionierung
NZ500294A (en) * 1997-05-12 2001-07-27 Wisconsin Alumni Res Found Continuous crystallization system with controlled nucleation for milk fat fractionation
EP1281749B1 (fr) * 2001-07-31 2009-10-14 De Smet Engineering N.V. Procédé et installation de fractionnement à sec
EP1818088A1 (fr) * 2006-01-20 2007-08-15 De Smet Engineering N.V. Cristallisateurs pour des procédés de fractionnement d'huiles et de graisses
GB2496606B (en) * 2011-11-15 2014-01-22 Desmet Ballestra Engineering S A Nv Continuous fractionation of triglyceride oils

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ES2753402T3 (es) 2020-04-08
PT3227418T (pt) 2019-11-05
DK3227418T3 (da) 2019-11-11

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