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
  • C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
  • C11B7/0008—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
  • A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
  • A23D9/02—Other edible oils or fats, e.g. shortenings or cooking oils characterised by the production or working-up
  • A23D9/04—Working-up
• • 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
  • C11B7/0008—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents
  • C11B7/0016—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents in hydrocarbons or halogenated hydrocarbons
• • 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
  • C11B7/0008—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents
  • C11B7/0025—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents in solvents containing oxygen in their molecule

Definitions

• the present invention relates to a novel fractionation process for producing a palm oil product from a palm oil starting material.
• Hard PMF is generally produced via fractionation of palm oil. Fractionation is primarily a separation process in which fat is solidified and subsequently separated from the liquid phase. There are three common types of fractionations, namely dry fractionation, solvent fractionation, and detergent fractionation. Solvent fractionation involves the addition of solvent to oil to promote crystallization and followed by separation via filtration into a liquid fraction, also called an olein fraction, and a solid fraction, also called a stearin fraction. Higher separation efficiency can be achieved as compared to when solvents are not used. Crystallization during solvent fractionation is commonly carried out via scraped surface heat exchanger process or in a batch crystallizer cooled by vacuum-evaporation of solvent.
• the present disclosure provides a process for producing a palm oil product that comprises the steps of (a) solidifying a palm oil starting material in the presence of a solvent and obtaining a mixture comprising solvent and solids of the palm oil starting material; (b) partially re-melting the mixture obtained in step (a); (c) solidifying the mixture obtained in step (b); and (d) separating the mixture obtained in step (c) into a solid fraction and a liquid fraction, wherein after the solidification step a) the slurry of solids of the partially solidified mixture from step a) is at a temperature range of the mixture obtained in step a) is from 7 to 12°C; after partially re-melting, the mixture obtained in step (b) is at a the temperature range of the mixture obtained in step b) is from 10 to 16°C; after solidification, the mixture obtained in step c) is at a temperature range of the mixture obtained in step c) is from 5 to 10°C.
• the palm oil starting material is palm oil or palm oil fraction.
• ppm parts per million
• percentage percentage
• ratios are on a by weight basis. Percentage on a by weight basis is also referred to as wt.% below.
• the acts can be carried out in any order without departing from the principles of the disclosure, except when a temporal or operational sequence is explicitly recited. Furthermore, specified acts can be carried out concurrently unless explicit claim language recites that they be carried out separately. For example, a claimed act of doing X and a claimed act of doing Y can be conducted simultaneously within a single operation, and the resulting process will fall within the literal scope of the claimed process.
• the present disclosure relates to a process for producing a palm oil product, comprising the steps of:
• step (b) partially re-melting the mixture obtained in step (a);
• step (d) separating the mixture obtained in step (c) into a solid fraction and a liquid fraction wherein after the solidification step a) the slurry of solids of the partially solidified mixture from step a) is at a temperature range of the mixture obtained in step a) is from 7 to 12°C; after partially re-melting, the mixture obtained in step (b) is at a the temperature range of the mixture obtained in step b) is from 10 to 16°C; after solidification, the mixture obtained in step c) is at a temperature range of the mixture obtained in step c) is from 5 to 10°C.
• Step (a) Solidifying palm oil starting material in the presence of a solvent and obtaining a mixture comprising solvent and solids of palm oil starting material
• a palm oil starting material is first mixed with a solvent.
• the mixture of solvent and the palm oil starting material is cooled to solidify and partially crystallize the palm oil starting material.
• a mixture comprising solvent and solids of partially crystallized palm oil starting material (partially crystallized solid-solvent mixture) is thus obtained.
• Palm oil starting material refers to palm oil or any oil and/or fat that has been obtained from palm oil by means of fractionation, interesterification, and/or hydrogenation.
• the palm oil starting material may have an iodine value (IV) of from 35 to 65, or more preferably, an IV of from 50 to 60.
• the palm oil starting material is palm oil, a palm oil fraction, interestenfied palm oil. interesterified palm oil fraction, hydrogenated palm oil, hydrogenated palm oil fraction or a combination of two or more thereof, wherein each time the term “fraction” is referring to palm olein, palm stearin or soft palm mid fraction.
• the palm oil starting material is selected from the group consisting of palm oil, palm olein, interesterified palm oil, interesterified palm olein, interesterified palm oil stearin, and combinations of two or more thereof. Most preferably, the palm oil starting material is palm oil, palm olein or combinations thereof. In a preferred aspect of the invention, the palm oil starting material is palm olein.
• the palm oil starting material used for the process of the present invention is a refined, bleached and/or deodorized oil.
• the palm oil starting material is an RBD oil, i.e. a refined, bleached and deodorized oil.
• solidifying as used in the present invention are encompassing crystallization as well as any process whereby acylglycerides are completely or partially transitioning from liquid into solid form. Said solid acylglycerides can be in crystalline and/or amorphous form. Furthermore, the term “partial solidification” or “partially solidified” relates to a process or mixtures respectively, wherein acylglycerides are present in solid form as well as and in liquid form.
• the palm olein used for the process has an IV of from 55 to 58, preferably of 56 (hereafter called “palm olein IV56”’).
• the palm olein may have a solid fat content (SFC). measured according to standard method of IUPAC 2.150a, as shown in Table 1 and a triglyceride composition comprising the triglycendes as shown in Table 2.
• Solvent may be mixed with the palm oil starting material in a ratio of palm oil starting material/solvent in a range of from 1/4 to 1/0.5, from 1/3 to 1/0.75, such as 1/1 or 1/2 (for example a palm oil starting material/solvent of 1/4 being a mixture of 1 part palm oil starting material and 4 parts solvent).
• solvent include, but are not limited to, acetone, hexane, heptane, isopropyl alcohol, methanol, or a combination of two or more thereof.
• the solvent is acetone.
• the solidification of the mixture of solvent and palm oil starting material can be done by cooling.
• cooling can be done in a batch crystallizer that is cooled by vacuum-evaporation of solvent at a pressure in a range of from 125 to 600 mbar.
• the pressure can be reduced in three stages: in the first stage, the pressure is reduced to between 400 and 600 mbar; in the second stage, the pressure is reduced to between 100 and 300 mbar; and in the final stage, the pressure is reduced to between 120 and 150 mbar.
• cooling can be done in a double jacketed cooling vessel with scraped surface (also known as scraped surface heat exchanger) or without scraped surface.
• scraped surface also known as scraped surface heat exchanger
• solid fat may be present in an amount from 12 to 70 wt.%, from 20 to 60 wt.%, or from 30 to 50 wt.% based on the total weight of the palm oil starting material (i.e.. not including the weight of the solvent).
• the partially solidified mixture from step a) also contains liquid oil, i.e oil from the palm oil starting material that was not solidified in step a) of the process.
• the amount of solid fat present in the partially solidified mixture from step a) is from 15 to 60 wt.%, preferably from 20 to 50 wt.%. more preferably from 30 to 40 wt.% based on the total weight of palm oil IV56 (i.e.. not including the weight of the solvent), most preferably from 35 to 40 wt%.
• the slurry of solids of the partially solidified mixture from step a) is at a temperature of from 7 to 12°C, from 8 to 11°C. or from 8.5 to 10.5°C.
• Step (b) Partially re-melting the mixture obtained in step (a)
• step (a) The partially solidified mixture obtained in step (a) is heated in step (b) to partially re-melt the solids.
• Partially re-melting can be expressed as the reduction of solids present in the mixture at the end of step (b) as compared to the amount of solids present in the mixture at the end of step (a).
• the solids content of the mixture at the end of step (b) may be reduced by a range of from 40 to 80%, from 50 to 75%, or preferably from 55 to 70% as compared to the amount of solids present in the mixture at the end of step (a) due to remelting in step b).
• solid fat may be present in an amount from 12 to 70 wt.%, from 20 to 60 wt.%, or from 30 to 50 wt.% based on the total weight of the palm oil starting material. Therefore, in the mixture obtained at the end of step (b), the actual content of solids present is from 2.4 to 42 wt.% (corresponding to!2-70% times 20-60%, which is the remaining portion of solids left after reduction of the solids with 40 to 80%), from 5 to 30 wt.%, or 9 to 22.5 wt.% based on the total weight of the palm oil starting material (z.e., not including the weight of the solvent).
• the amount of solids present in the mixture obtained at the end of step (b) is from 3 to 36 wt.% (corresponding to 15 -60% times 20-60%, which is the remaining portion of solids left after reduction of the solids with 40 to 80%), from 5 to 25 wt.%, or from 9 to 18 wt.% based on the total weight of palm oil IV56 (/.e., not including the weight of the solvent).
• Re-melting in step b) may be done by heating up of the mixture obtained in step a).
• heating up the mixture obtained in step a) is done by adding hot solvent, preferably at a temperature of from 30°C to 35°C.
• Solvent may be added to maintain a ratio of palm oil starting material/solvent in a range of from 1/4 to 1/0.5, from 1/3 to 1/0.75, such as 1/1 or 1/2.
• heating up of the mixture obtained in step a) may be done by means of a double jacketed heating from the vessel wherein the mixture is held and/or a heating coil.
• the mixture obtained in step (b) is at a temperature of from 10 to 16°C, from 1 1 to 15°C, or from 12 to 14°C.
• Temperature difference between the mixture obtained in step (b) and the mixture obtained in step (a) can be in a range of from 0.5 to 10°C, from 3 to 8°C. or from 4 to 6°C.
• the temperature difference can be in a range of from 0.5 to 7°C, from 1 to 6°C, or from 2 to 5°C.
• Step (c) Solidify ing the mixture obtained in step (b)
• the re-melted mixture obtained in step (b) is further solidified by cooling.
• solids are present in an amount of from 10 to 40 wt.%, or preferably from 15 to 28 wt.% based on the total weight of the palm oil starting material (i.e.. not including the weight of the solvent).
• the solidification in step c) can be done by cooling.
• cooling can be done in a batch crystallizer that is cooled by vacuum-evaporation of solvent at a pressure in a range of from 125 to 600 mbar.
• the pressure can be reduced in three stages: in the first stage, the pressure is reduced to between 400 and 600 mbar; in the second stage, the pressure is reduced to between 100 and 300 mbar; and in the final stage, the pressure is reduced to between 120 and 150 mbar.
• cooling in step c) can be done in a double jacketed cooling vessel with scraped surface (also known as scraped surface heat exchanger) or without scraped surface.
• scraped surface also known as scraped surface heat exchanger
• the mixture obtained in step c) is at a temperature of from 5 to 10°C, from 6 to 9°C, or from 6.5 to 8.5°C.
• Step (d) Separating the mixture obtained in step (c) into a solid fraction and a liquid fraction
• step (c) The mixture obtained in step (c) is separated into a solid fraction and a liquid fraction in step (d). Separation can be done in apparatus such as a vacuum belt filter or a membrane filter press.
• solvent can be recovered from the solid fraction and/or the liquid fraction; more preferably, the recovered solvent can be recycled into step (a).
• the solid fraction obtained in step (d) is a hard palm mid fraction (PMF) that has an IV of from 31 to 38, preferably from 32 to 37, more preferably from 33 to 36.
• the hard PMF can have:
• tripalmitoylglycerol PPP
• PPP tripalmitoylglycerol
• the process of the present disclosure may comprise one or more steps before, or after step (a) to step (d).
• steps (b) and (c) may be repeated once or more prior to step (d).
• This will contribute to an even better quality of the obtained hard PMF.
• It relates to a process a process for producing a palm oil product, which comprises: a) solidifying a palm oil starting material in the presence of a solvent, and obtaining a mixture comprising solvent and solids of the palm oil starting material; b) partially re-melting the mixture obtained in step a); c) solidifying the mixture obtained in step b); and d) partially re-melting the mixture obtained in step c); e) solidifying the mixture obtained in step d); and f) separating the mixture obtained in step e) into a solid fraction and a liquid fraction, wherein after the solidification step a) the slurry of solids of the partially solidified mixture from step a) is at a temperature range of the mixture obtained in step a) is from 7 to 12°C; after partially re-melting, the mixture obtained in step (b)
• Palm oil starting material may be treated prior to step (a) of the present inventive process. This pre-treatment may be by means of one or more refining steps such as degumming, bleaching, and/or deodorization.
• the palm oil starting material is preferably a degummed, bleached, and/or deodorized palm oil starting material.
• the process of the present disclosure for obtaining a hard palm mid fraction with IV in a range of from 31 to 38, preferably from 32 to 37, more preferably from 33 to 36, may result in a reduction of the amount of process steps required, and/or a reduction of the processing time.
• the process according to the present invention may allow for a promotion of formation of desired symmetrical crystals (POP) while the formation of undesired asymmetrical triglycerides, such as POO, is reduced, and that may contribute to the desirable quality of the resulting hard PMF.
• POP desired symmetrical crystals
• POO undesired asymmetrical triglycerides
• a desired hard PMF can be achieved with a single process step as compared to conventional processes that involve several fractionation steps.
• the entire process can happen in just one reactor without one or multiple transfer(s) of the process materials as in conventional processes; thus, the risk of material loss during transfer can be minimized or even avoided.
• Process time of the present inventive process is about 2.5 hours, while dry fractionation in the conventional processes use 10 hours or more. Thus, process time may be saved for at least 75% with the present inventive process.
• the present disclosure also relates to the products that are directly obtained by the process of the invention.
• the present disclosure relates to a hard palm mid fraction (PMF) obtainable by the present process.
• PMF hard palm mid fraction
• the hard PMF obtained as the solid fraction after separation in step (d) has an iodine value of from 31 to 38, preferably from 32 to 37, more preferably from 33 to 36.
• the hard PMF obtained as the solid fraction after separation in step (d) has the following triglyceride contents:
• PPP tripalmitoylglycerol
• POP tripalmitoylglycerol
• POP 1.3-dipalmitoyl-2-oleoyl-glycerol
• the hard PMF obtained as the solid fraction after separation in step (d) has a solid fat content (SFC), measured according to IUPAC method 2.
• SFC solid fat content
• the liquid (olein) fraction that is obtained after removal of the solvent by the present process is also a useful product.
• the palm oil olein that is obtained by the process of the invention as the liquid fraction after separation in step (d), and after removal of solvent has an IV of from 60 to 70, preferably an IV of from 62 to 68, more preferably an IV of from 64 to 66.
• the hard PMF obtained by the process of the present disclosure can be used in various applications, including but not limited to. producing cocoa butter equivalents (CBE) or any other food application.
• CBE cocoa butter equivalents
• the hard PMF obtained by the present inventive process gives sharp melting and clean mouthfeel that are especially desirable in confectionary applications.
• the hard PMF is a POP-rich fat that makes it possible to blend with exotic fats such as shea butter, shea stearin, illipe butter, sal fat, mango kernel fat, kokum gurgi fat or combinations or two or more thereof.
• the resulting blend i.e; a cocoa butter equivalent, can achieve a 100% compatibility 7 with cocoa butter without changing the characteristics of the final products. Examples
• Step (a) Solidify ing palm oil starting material in the presence of a solvent and obtaining a mixture comprising solvent and solids of palm oil starting material:
• Palm olein having an iodine value (IV) of 56 (Palm olein IV56), with solid fat contents (SFC) and triglyceride composition as shown in Table 3, was used as the starting material and cooled to 20 to 25°C in a pre-cooler.
• the cooled palm olein IV56 and acetone were fed into a crystallizer in a ratio palm olein/acetone of 1/l
• the mixture of the palm olein IV56 and acetone was partially solidified by evaporative cooling at a reduced pressure of from 125 to 145 mbar.
• the mixture at the end of step a) had a temperature of 8.5-10.5°C.
• the mixture at the end of step a) had a content of 37 wt.% of solids.
• the amount of solids was determined by separating liquid and solid fraction by means of filtration and subsequently w eighing both fractions.
• Step (b) Partially re-melting the mixture obtained in step (a):
• step b) Warm acetone at a temperature of about 35°C was added to the crystallizer to heat up and re-melt the partially solidified mixture.
• the mixture at the end of step b) had a temperature of 12.5°C.
• the mixture at the end of step b) contained 13.9 wt.% of solids (i.e. not including the weight of the solvent), which is a reduction of 62 wt% of solids, still remaining 38 wt% of solids.
• Step (c) Solidifying the mixture obtained in step (b):
• step c) The mixture obtained in step c) was further solidified in the crystallizer by evaporative cooling at a reduced pressure of from 125 to 145 mbar.
• the mixture at the end of step c) had a temperature of 7.2°C.
• the mixture at the end of step c) contained about 15.5 to 16 wt.% of solids (i.e. not including the weight of the solvent).
• Step (d) Separating the mixture obtained in step (c) into a solid fraction and a liquid fraction:
• the solidified mixture was transferred to a belt filter to separate the mixture obtained in step c) into a solid fraction and a liquid fraction. After acetone was removed from the solid by distillation, hard PMF was obtained. The recovered acetone was recycled back to the cry stallizer.

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

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• 2024
  • 2024-02-23 EP EP24714108.8A patent/EP4669733A2/de active Pending
  • 2024-02-23 WO PCT/US2024/017003 patent/WO2024178287A2/en not_active Ceased

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