WO2019013358A1 - 油脂の製造方法 - Google Patents

油脂の製造方法 Download PDF

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WO2019013358A1
WO2019013358A1 PCT/JP2018/026668 JP2018026668W WO2019013358A1 WO 2019013358 A1 WO2019013358 A1 WO 2019013358A1 JP 2018026668 W JP2018026668 W JP 2018026668W WO 2019013358 A1 WO2019013358 A1 WO 2019013358A1
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oil
fat
temperature
cooling
type
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PCT/JP2018/026668
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English (en)
French (fr)
Japanese (ja)
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誠也 竹口
秀隆 上原
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日清オイリオグループ株式会社
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Priority to MYPI2020000211A priority Critical patent/MY200954A/en
Publication of WO2019013358A1 publication Critical patent/WO2019013358A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • 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

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  • the present invention relates to a method of producing fats and oils.
  • JP-A 2009-249614 describes a method of separating fat and oil which can efficiently separate liquid part and solid part by changing temperature of fat and oil variously. It is done.
  • Patent Document 1 The method described in Patent Document 1 involves steps of repeatedly raising and lowering the temperature of the fat to precipitate crystals of the fat, and there is room for improvement in terms of work efficiency and complexity. Therefore, there is a need for a method of producing fats and oils that can perform separation processing more simply and with reduced working time.
  • the present inventors have found that the above-mentioned problems can be solved by adopting a configuration including the presence of a pre-seed of ⁇ -type crystal in fats and oils of a predetermined temperature, and the present invention has been accomplished. That is, the present invention (A) a step of melting the raw material fat and oil, (B) cooling the fat and oil to a temperature t (° C.) where (A-12) ⁇ t ⁇ A, where A (° C.) is the melting temperature of the fat and oil; (C) providing a pre-seed of ⁇ -type crystal in the oil-and-fat at the temperature, and (d) forming a seed of ⁇ -type crystal from the pre-seed. .
  • the present invention (A) a step of melting the raw material fat and oil, (B) cooling the fat and oil to a temperature t (° C.) where (A-12) ⁇ t ⁇ A, where A (° C.) is the melting temperature of the fat and oil; (C) providing a pre-seed of ⁇ -type crystal in the fat at the temperature, and (d) forming a seed of ⁇ -type crystal from the pre-seed.
  • the efficiency of formation of stable ⁇ -type crystals can be improved, and accordingly, the working time of fractionation in the production of fats and oils can be shortened and the cost can be reduced.
  • the present invention (A) a step of melting the raw material fat and oil, (B) cooling the fat or oil to a temperature t (° C.) where (A-12) ⁇ t ⁇ A, where A (° C.) is equal to or less than the melting temperature of the fat or oil; (C) providing a pre-seed of ⁇ -type crystal in the oil-and-fat at the temperature, and (d) forming a seed of ⁇ -type crystal from the pre-seed. It is a thing. Each step will be specifically described below.
  • the step (a) of the present invention is a step of melting the raw material fat and oil.
  • the raw material fats and oils which can be used for this invention are not specifically limited, For example, palm oils and fats (fractionated oil derived from palm oil and palm oil), such as palm oil, palm stearin, palm olein, palm middle melting point fraction (PMF), are used. Among the above, palm oil and palm stearin are preferable.
  • the above-mentioned fats and oils may be processed fats and oils subjected to treatments such as purification, transesterification, hydrogenation and fractionation.
  • the iodine value of the raw material fat and oil varies depending on the type of the raw material fat and oil, but in the case of palm oil, for example, it is preferably 50 to 55, and more preferably 51 to 54.
  • palm stearin When palm stearin is used, its iodine value is preferably 20 to 48, more preferably 30 to 42.
  • the raw material fats and oils used in the present invention are preferably triglycerides, and preferably the fatty acid content of 16 to 18 carbon atoms is 30% by mass or more, 40% by mass or more, 50% by mass or more, 60% by mass It is preferable that the content is 70% by mass or more, 80% by mass or more, or 90% by mass or more.
  • Examples of the above-mentioned fatty acids include palmitic acid, stearic acid, oleic acid and linoleic acid.
  • the main triglyceride is preferably a triglyceride of SSS type (tri-saturated type) or SUS type (2-unsaturated, 1,3-di-saturated type).
  • palm fats and oils, or raw material fats and oils containing SUS type triglycerides are particularly preferable.
  • SSS type triglyceride examples include tripalmitin, tristearin and the like.
  • 2-oleo-1,3-dipalmitin and the like can be mentioned.
  • the temperature at which the raw material fat is melted while optionally stirring the raw material fat is 40 ° C. or more, preferably 50 ° C. or more, more preferably 60 to 100 ° C., for example, 0.5 to 3 hours.
  • the raw material fat is melted by heating for 1 to 2 hours.
  • a publicly known heating method can be used as a heating method, for example, a constant temperature bath with a predetermined temperature, an oil bath, steam heating, heat exchange and the like can be used.
  • the step (b) of the present invention is a step of cooling the melted fat and oil to a temperature t (° C.) where (A-12) ⁇ t ⁇ A, where A (° C.) is the melting temperature of the fat and oil.
  • the target temperature or temperature range to be cooled is determined based on the melting temperature of the raw material fat. That is, it may be cooled to a temperature t (° C.) where the melting temperature of the raw material fat and oil is A (° C.) and (A-12) ⁇ t ⁇ A or a temperature range satisfying the above relationship.
  • the above temperature t (° C.) does not have to be constant, and may be appropriately varied within the temperature range satisfying the relationship of the above equation.
  • the melting temperature of the raw material fat can be determined, for example, by DSC measurement.
  • the melting temperature in DSC measurement is 42.8 ° C., so the oil temperature is cooled to be in the range of 30.8 to 42.8 ° C.
  • the melting temperature in DSC measurement is 58.1 ° C., so the oil temperature is cooled to be in the range of 46.1 to 58.1 ° C.
  • the cooling temperature t (° C.) in the step (b) is more preferably (A-10) ⁇ t ⁇ (A-2), where A (° C.) is the melting temperature of the raw material fat and oil.
  • the melting temperature of the fat or oil is, for example, in the DSC measurement, the fat or oil completely heated by heating to 70 ° C. to 80 ° C. and cooled to -60 to -70 ° C. at a cooling rate of -3 to -5 ° C./min. Thereafter, the temperature is raised by heating at a temperature rising rate of +3 to + 5 ° C./min to eliminate heat absorption. More specifically, as can be seen in FIG. 1, it can be determined as the temperature at the intersection of the baseline where the endotherm is completely eliminated by heating and the rising line that returns from the last endotherm to the baseline.
  • the temperature of the whole fat does not fall below the lower limit value of the above temperature range at any time in the middle. Moreover, it is preferable not to raise the temperature of the whole fats and oils until it starts the following process (c) after operation to cool to the temperature range prescribed
  • the melting point of the ⁇ -type crystal is the highest
  • the melting point of the ⁇ ′-type crystal is the second highest
  • the melting point of the ⁇ -type crystal is the lowest.
  • Cooling of fats and oils can be performed with stirring and / or standing.
  • the cooling can be performed by natural cooling using an external temperature or any cooling device, but a thermostatic bath or an oil bath may be used in order to perform cooling efficiently and under controlled conditions.
  • a refrigerant such as cold water may be circulated to the outside or inside of the container for cooling.
  • the speed at which the temperature is reduced can be arbitrarily determined by those skilled in the art based on the amount of oil to be cooled, the method of cooling, etc.
  • the step (c) of the present invention is a step of causing a pre-seed of ⁇ -type crystal which is an unstable fat crystal to be present in the fat or oil at the temperature cooled in the step (b).
  • the pre-seed of the ⁇ -type crystal is present in the oil and fat while the temperature of the oil and fat is in the temperature range defined in the step (b).
  • the temperature of the whole fat may be kept constant during the operation for causing the pre-seed of the ⁇ -type crystal to be present in the step (c), and the fat is selected under the condition that it is within the above temperature range.
  • An operation may be performed to cause a pre-seed of ⁇ -type crystal to exist while cooling.
  • the temperature of the fat is not increased.
  • cooling oil and fat, oil and fat are preferably cooled at the same temperature reduction rate as step (b).
  • ⁇ -type crystals are produced by lowering the temperature of fats and oils to below the melting point of ⁇ -type crystals. Therefore, in the step (c), for example, by locally cooling the temperature of the fat or oil to the melting point of the ⁇ -type crystal or less, pre-seed of the ⁇ -type crystal can be present in the fat or oil. Or it is also possible to carry out by adding the pre-seed of the separately prepared ⁇ -type crystal to the fats and oils after the step (b). That is, in the step (c), it is not necessary to cool the whole melted fat and oil to the melting point or less of the ⁇ -type crystal in order to form a pre-seed of the ⁇ -type crystal. It is possible to reduce.
  • the ⁇ -type crystal which is a pre-seed for forming a seed of ⁇ -type crystal which is a stable type, is cooled to below the melting point of the ⁇ -type crystal.
  • ⁇ -type crystal which is a pre-seed for forming a seed of ⁇ -type crystal which is a stable type
  • “To locally cool the temperature of the oil or lower to the melting point of the ⁇ -type crystal” means maintaining the temperature of the whole oil except for the locally cooled portion within the temperature range defined in step (b). It means that only a part of the fat and oil is cooled to the melting point or lower of the ⁇ -type crystal.
  • the temperature of the whole fat or oil mentioned above is a temperature achieved by the effect of a cooling device such as an outside air temperature or a thermostatic bath or an oil bath used for controlling the fat and oil temperature in step (b).
  • a cooling device such as an outside air temperature or a thermostatic bath or an oil bath used for controlling the fat and oil temperature in step (b).
  • the temperature of the local cooling is preferably 10 ° C. or more lower than the temperature of the oil of the other portion, more preferably 20 ° C.
  • the temperature may be, for example, 30 to 80 ° C. lower.
  • the time for cooling may be determined by those skilled in the art, but can be, for example, 1 second to 10 minutes, preferably 15 seconds to 5 minutes, more preferably 30 seconds to 2 minutes.
  • the local cooling of the oil can be carried out by contacting any solid, liquid or gas cooling body at a temperature below the melting point of the ⁇ -form crystal with a part of the oil.
  • the two approaches to such an extent that the heat conduction to lower the temperature of part of the fat or oil to the melting point or lower of the ⁇ -type crystal is possible.
  • the contact between the fat and oil and the cooling body may be carried out, for example, by flowing cold water in a pipe provided in the fat and oil, or introducing a cooled particulate matter, linear substance, liquid drop, etc. into the fat and oil. And so on. In one embodiment, this step is performed by pouring dry ice into fats and oils.
  • the temperature of the cooling body may be equal to or lower than the melting point of the ⁇ -type crystal in order to cause the pre-seed of the ⁇ -type crystal to exist in the fat and oil. Simply, it may be lower than the crystallization start temperature of fats and oils.
  • the crystallization start temperature of the fat or oil can be determined, for example, by DSC measurement. For example, in DSC measurement, the fat completely heated by heating to 70 ° C. to 80 ° C. can be melted at -3 to -5 ° C./minute It is the heat generation start temperature when cooled at the cooling rate. More specifically, as seen in FIG. 1, it is determined as the temperature at the intersection of the baseline until the onset of heat generation and the rising line of heat generation.
  • the crystallization onset temperature in DSC measurement is 21.2 ° C.
  • the crystallization start temperature is 33.1 ° C.
  • the temperature of the cooling body is preferably 10 ° C. or more lower than the crystallization start temperature.
  • the oil produces ⁇ -type crystals is confirmed by solidifying (crystallization) a small amount of melted oil at the temperature of the cooling body and measuring the X-ray diffraction of the solidified oil. It can. That is, for fat crystals, X-ray diffraction is measured in the range of 2 ⁇ of 17 to 26 degrees with respect to short face intervals, and a strong diffraction peak (peak A) corresponding to an interplanar spacing of 4.1 to 4.3 ⁇ is detected If the peak (peak B) is not detected at 3.8 to 3.9 ⁇ or if it is a minute diffraction peak, it can be judged as an ⁇ -type crystal.
  • the X-ray diffraction intensity of peak B (peak B / peak A) relative to the X-ray diffraction intensity of peak A is preferably 0.1 or less, more preferably 0.05 or less, and still more preferably 0 to 0. It is 02.
  • the step (c) can also be carried out by adding separately prepared pre-seed of ⁇ -type crystal to the fats and oils after the step (b).
  • the pre-seed can be prepared by cooling separately melted fats and oils to the melting point or lower of the ⁇ -type crystal.
  • the above pre-seed is preferably prepared from the same kind of fat as the fat to which it is added (hereinafter also referred to as "main fat"), but in the next step (d) it is finally seeded with ⁇ -type crystals
  • main fat the composition and concentration of the oil for preparing the pre-seed may be different from that of the main oil and fat.
  • the above operation is carried out, for example, by cooling the oil to 0 to 10 ° C., preferably 3 to 8 ° C., to form a slurry containing ⁇ -type crystals, and adding it to the body oil.
  • the amount of the pre-seed of the ⁇ -type crystal to be added can be determined as appropriate by those skilled in the art, but a small amount is usually sufficient compared to the amount of the main oil, for example 0.001 to 5% by mass relative to the main oil
  • the amount is 0.01 to 1% by mass, more preferably 0.05 to 0.2% by mass.
  • the step (d) of the present invention is a step of forming a seed of ⁇ -type crystal from pre-seed of the ⁇ -type crystal in fat and oil.
  • a pre-seed of ⁇ -type crystal is present in the oil and fat at a temperature t (° C.) where (A-12) ⁇ t ⁇ A where A (° C.) is the melting temperature of the oil.
  • the said temperature is higher than the crystallization start temperature of fats and oils. Therefore, the temperature of the oil and fat present around the pre-seed of the ⁇ -type crystal formed or added in the step (c) is equal to or higher than the melting point of the ⁇ -type crystal.
  • the ⁇ -type crystals temporarily present in the oil and fat are melted at the material temperature without forced heating, and melt-mediated transfer to the stable ⁇ -type crystals.
  • This step is carried out at a temperature t (° C.) such that (A-12) ⁇ t ⁇ A, where A (° C.) is the melting temperature of the oil, as in steps (b) and (c).
  • the melting temperature of A is set to A (.degree. C.) at a temperature t (.degree. C.) such that (A-10) .ltoreq.t.ltoreq. (A-2).
  • ⁇ -type crystals as seeds for ⁇ -type crystals by melt-mediated transfer, it is possible to save time and effort for separately preparing seeds for ⁇ -type crystals, and a finer state than adding seeds of prepared ⁇ -type crystals. Can be dispersed in fats and oils.
  • the oil can be further cooled to promote the crystal formation of triglyceride which is likely to form the ⁇ -type crystal contained in the raw material oil-and-fat.
  • a person skilled in the art can appropriately set the temperature for that purpose, but the target temperature or temperature range can be set so as to be, for example, equal to or higher than the crystallization start temperature of fats and oils based on the material temperature.
  • the temperature of the purified palm oil is 20 to 30 ° C., preferably 22 to 28 ° C., more preferably 23 to 27 ° C.
  • step (b) may be maintained at 34 to 50 ° C, preferably 38 to 48 ° C. More preferably, it may be cooled to a temperature of 40 to 46.degree.
  • the target temperature or temperature range is preferably cooled at the same rate of temperature decrease as step (b). Further, the temperature may be lowered intermittently, for example, by interrupting the drop of the product temperature if necessary, in the process of steps (b) to (d).
  • the temperature can be kept constant during the operation. However, in the present invention, it is preferable not to raise the temperature of the fat or oil, for example, by heating the fat or oil through the steps (b) to (d).
  • the temperature of the fat After the temperature of the fat has reached the target temperature or temperature range, it may be allowed to stand at that temperature or temperature range, or may be stirred if necessary.
  • the time for maintaining the temperature can be appropriately set by those skilled in the art, and can be, for example, 10 to 180 minutes, preferably 20 to 120 minutes, and more preferably 40 to 90 minutes.
  • the resultant product obtained by the above step (d) is in the state of a slurry in which a solid portion and a liquid portion containing ⁇ -type crystals of fat and oil are mixed.
  • a known method for producing a fractionated fat and oil may be appropriately performed.
  • the solid portion containing the formed seed may be appropriately separated from the liquid portion using a conventional method.
  • the solid-liquid separation in the above step is performed by, for example, press filtration or vacuum filtration.
  • compression filtration is carried out, for example, at 3 to 30 kgf at a temperature (preferably 20 to 27 ° C.) lower than room temperature using a compression filter used for fractional filtration of palm oil etc. / cm 2, preferably 5 ⁇ 20kgf / cm 2, more preferably be carried out under pressing pressures of about 8 ⁇ 12kgf / cm 2.
  • the fat crystals of the solid portion of the fractionated fat produced through the steps (a) to (d) of the present invention contain ⁇ -type crystals. Thereby, it can be judged that melt-mediated transfer of the pre-seed of the ⁇ -type crystal to the ⁇ -type crystal is performed. It is judged from the diffraction peak obtained by the measurement of X-ray diffraction that fat crystals are ⁇ -type. That is, for fat crystals, when X-ray diffraction is measured in the range of 2 ⁇ of 17 to 26 degrees and the diffraction peaks corresponding to the surface spacing of 4.5 to 4.7 ⁇ are detected, ⁇ It can be judged that a type crystal is included.
  • the solid part of the fractionated fat and oil corresponds to the intensity G 'of the diffraction peak corresponding to the interplanar spacing of 4.1 to 4.3 ⁇ obtained by X-ray diffraction and the interplanar spacing of 4.5 to 4.7 ⁇
  • the intensity ratio (G '/ G) of the diffraction peak to the intensity G is preferably 0 to 0.3, more preferably 0 to 0.2, and further preferably 0 to 0.1. preferable.
  • Examples 1 to 5 and Comparative Examples 1 to 3 show the fractionation of purified palm oil (iodine number: 53.0).
  • the melting temperature in DSC measurement of the purified palm oil is 42.8 ° C., and the crystallization start temperature in DSC measurement is 21.2 ° C. (see FIG. 1).
  • the following Examples 6 to 8 and Comparative Examples 4 to 5 show the fractionation of purified palm stearin (iodine number: 35.0).
  • the melting temperature in DSC measurement of the purified palm stearin is 58.1 ° C.
  • the crystallization start temperature in DSC measurement is 33.1 ° C. (see FIG. 2).
  • DSC analysis method 3 to 10 mg of sample oil and fat is collected in a container made of aluminum, and sample oil and fat in a completely melted state at 70 ° C or higher is cooled at a cooling rate of -5 ° C / min. It measured and the temperature of the intersection of the baseline to the heat
  • Iodine value analysis method The iodine value was measured using AOCS test method (Official Method Cd 1-25). Specifically, 10 mL of cyclohexane is added to 0.5 to 3 g of a sample oil and dissolved, and then 25 mL of a whiss liquid is added and allowed to stand in the dark for 1 hour. Thereafter, the reaction is stopped by adding 20 mL of a 10 g / 100 mL potassium iodide solution and 100 mL of water, and then titration with 0.1 N sodium thiosulfate is performed to determine the amount of iodine added to the oil.
  • the iodine value conversion method is based on the following formula.
  • Iodine value (A ⁇ B) ⁇ F ⁇ 1.269 / C
  • C Amount of sample fat used (g)
  • Example 1 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil.
  • the melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.28 ° C./min.
  • the partially cooled piping was brought into contact with the oil and water at 5 ° C. was allowed to flow through the piping for 1 minute. Thereafter, the slurry was cooled to 25 ° C.
  • Example 2 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil.
  • the melted fats and oils were placed in a glass crystallization flask, and stirred and cooled in a thermostatic water bath so that the temperature decrease rate was 0.35 ° C./min on the basis of the product temperature.
  • the partially cooled piping was brought into contact with the oil and water at 5 ° C. was allowed to flow through the piping for 1 minute. Thereafter, the slurry was cooled to 25 ° C.
  • Example 3 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil.
  • the melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.42 ° C./minute on the basis of the product temperature.
  • the partially cooled piping was brought into contact with the oil and water at 5 ° C. was allowed to flow through the piping for 1 minute. Thereafter, the slurry was cooled to 25 ° C.
  • Example 4 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil.
  • the melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.28 ° C./min.
  • 0.1 g of dry ice was added. Thereafter, the slurry was cooled to 25 ° C. at a temperature decreasing rate of 0.22 ° C./min, stirred and cooled at the same temperature for 1 hour to obtain a slurry.
  • the obtained slurry was subjected to solid-liquid separation at 25 ° C. by press filtration (press pressure 10 kgf / cm 2 ) to obtain a solid part (solid fat and oil) and a liquid part (liquid fat and oil). It took 180 minutes from the start of cooling to the start of expression.
  • the results are shown in Table 1.
  • purification palm oil solidified on dry ice was (alpha) type.
  • Example 5 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil. The melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.28 ° C./min. At 39 ° C., the purified palm oil separately dissolved was allowed to stand for 10 minutes in a 5 ° C. refrigerator, and 0.4 g of ⁇ -type crystal slurry solidified by cooling was added. Thereafter, the slurry was cooled to 25 ° C.
  • Comparative Example 1 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil. The melted fats and oils were placed in a glass crystallization flask, and stirred and cooled in a thermostatic water bath to 25 ° C. so that the temperature decrease rate was 0.25 ° C./min on the basis of the product temperature. Thereafter, the mixture was stirred and cooled at 25 ° C. for 3 hours to obtain a slurry. The obtained slurry was subjected to solid-liquid separation at 25 ° C. by press filtration (press pressure 10 kgf / cm 2 ) to obtain a solid part (solid fat and oil) and a liquid part (liquid fat and oil). It took 300 minutes from the start of cooling to the start of expression. The results are shown in Table 1.
  • Comparative example 2 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil. The melted fats and oils were placed in a glass crystallization flask, and stirred and cooled to 39 ° C. in a thermostatic water bath so as to have a temperature decrease rate of 0.28 ° C./min on the basis of the product temperature. After stirring and cooling at 38 ° C. for 2 hours, the slurry was cooled to 25 ° C. at a temperature decreasing rate of 0.22 ° C./min and stirred for 3 hours at the same temperature to obtain a slurry.
  • Comparative example 3 400.0 g of purified palm oil (iodine number: 53.0) was heated at 60 ° C. for 1 hour using a 60 ° C. constant temperature water bath to completely melt the purified palm oil. The melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.20 ° C./min. At 43 ° C., the partially cooled piping was brought into contact with the oil and water at 5 ° C. was allowed to flow through the piping for 1 minute. Thereafter, the slurry was cooled to 25 ° C.
  • Example 6 400.0 g of purified palm stearin (iodine value: 35.0) was heated at 70 ° C. for 1 hour using a thermostat bath of 70 ° C. to completely melt the purified palm stearin.
  • the melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so that the temperature decrease rate was 0.22 ° C./min on the basis of the product temperature.
  • a partially cooled pipe was brought into contact with the oil and water at 5 ° C. was allowed to flow through the pipe for 1 minute. Thereafter, the mixture was stirred at 52 ° C. for 4 hours to obtain a slurry.
  • the obtained slurry was subjected to solid-liquid separation at 52 ° C. by press filtration (press pressure 10 kgf / cm 2 ) to obtain a solid part (solid fat) and a liquid part (liquid fat). It took 300 minutes from the start of cooling to the start of expression.
  • the results are shown in Table 1.
  • the fat-and-oil crystal polymorph of the purified palm stearin solidified at 5 ° C. was ⁇ -type.
  • Example 7 400.0 g of purified palm stearin (iodine value: 35.0) was heated at 70 ° C. for 1 hour using a thermostat bath of 70 ° C. to completely melt the purified palm stearin.
  • the melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.23 ° C./min.
  • the partially cooled piping was brought into contact with the oil and water at 5 ° C. was allowed to flow through the piping for 1 minute. Then, it stirred at 51 degreeC for 4 hours, and obtained the slurry.
  • the obtained slurry was subjected to solid-liquid separation at 51 ° C.
  • Example 8 400.0 g of purified palm stearin (iodine value: 35.0) was heated at 70 ° C. for 1 hour using a thermostat bath of 70 ° C. to completely melt the purified palm stearin.
  • the melted fats and oils were placed in a glass crystallization flask, and were stirred and cooled in a thermostatic water bath so as to have a temperature decrease rate of 0.27 ° C./min.
  • the partially cooled piping was brought into contact with the oil and water at 5 ° C. was allowed to flow through the piping for 1 minute. Thereafter, the mixture was stirred at 49 ° C. for 4 hours to obtain a slurry.
  • the obtained slurry was subjected to solid-liquid separation at 49 ° C. by press filtration (press pressure 10 kgf / cm 2 ) to obtain a solid part (solid fat) and a liquid part (liquid fat). It took 300 minutes from the start of cooling to the start of expression.
  • the results are shown in Table 1.
  • the fat-and-oil crystal polymorph of the purified palm stearin solidified at 5 ° C. was ⁇ -type.
  • Comparative example 4 400.0 g of purified palm stearin (iodine value: 35.0) was heated at 70 ° C. for 1 hour using a thermostat bath of 70 ° C. to completely melt the purified palm stearin.
  • the melted fats and oils were placed in a glass crystallization flask, and stirred and cooled to 51 ° C. in a thermostatic water bath so as to have a temperature decrease rate of 0.23 ° C./min on the basis of the product temperature. Then, it stirred at the same 51 degreeC for 22 hours, and obtained the slurry.
  • the obtained slurry was subjected to solid-liquid separation at 51 ° C. by press filtration (press pressure 10 kgf / cm 2 ) to obtain a solid part (solid fat and oil) and a liquid part (liquid fat and oil). It took 1380 minutes from the start of cooling to the start of expression.
  • Table 1 The results are shown in Table 1.
  • Comparative example 5 400.0 g of purified palm stearin (iodine value: 35.0) was heated at 70 ° C. for 1 hour using a thermostat bath of 70 ° C. to completely melt the purified palm stearin. The melted fats and oils were placed in a glass crystallization flask, and stirred and cooled in a thermostatic water bath to 40 ° C. so as to have a temperature decrease rate of 0.42 ° C./min on the basis of the product temperature. Then, it stirred at the same 40 degreeC for 4.5 hours, and obtained the slurry. The obtained slurry was subjected to solid-liquid separation at 40 ° C. by press filtration (press pressure 10 kgf / cm 2 ) to obtain a solid part (solid fat) and a liquid part (liquid fat). It took 300 minutes from the start of cooling to the start of expression. The results are shown in Table 1.

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CN113025419A (zh) * 2021-03-12 2021-06-25 郑州轻工业大学 一种鸭油的分提方法

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JP2001242102A (ja) * 2000-02-28 2001-09-07 Snow Brand Milk Prod Co Ltd 油脂中で発現している結晶型の評価方法
JP2003306691A (ja) * 2002-02-13 2003-10-31 Asahi Denka Kogyo Kk カカオ脂の分別方法
WO2005006870A1 (ja) * 2003-07-23 2005-01-27 Meiji Seika Kaisha, Ltd. 含水油脂組成物およびその製造方法
JP2005060523A (ja) * 2003-08-12 2005-03-10 Asahi Denka Kogyo Kk 油脂のドライ分別方法
WO2009028295A1 (ja) * 2007-08-31 2009-03-05 Fuji Oil Company, Limited 油脂の乾式分別法
WO2009060809A1 (ja) * 2007-11-05 2009-05-14 Fuji Oil Company, Limited チョコレート添加剤およびその製造方法
JP2015133954A (ja) * 2013-12-19 2015-07-27 日清オイリオグループ株式会社 油脂

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Publication number Priority date Publication date Assignee Title
JP2001242102A (ja) * 2000-02-28 2001-09-07 Snow Brand Milk Prod Co Ltd 油脂中で発現している結晶型の評価方法
JP2003306691A (ja) * 2002-02-13 2003-10-31 Asahi Denka Kogyo Kk カカオ脂の分別方法
WO2005006870A1 (ja) * 2003-07-23 2005-01-27 Meiji Seika Kaisha, Ltd. 含水油脂組成物およびその製造方法
JP2005060523A (ja) * 2003-08-12 2005-03-10 Asahi Denka Kogyo Kk 油脂のドライ分別方法
WO2009028295A1 (ja) * 2007-08-31 2009-03-05 Fuji Oil Company, Limited 油脂の乾式分別法
WO2009060809A1 (ja) * 2007-11-05 2009-05-14 Fuji Oil Company, Limited チョコレート添加剤およびその製造方法
JP2015133954A (ja) * 2013-12-19 2015-07-27 日清オイリオグループ株式会社 油脂

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113025419A (zh) * 2021-03-12 2021-06-25 郑州轻工业大学 一种鸭油的分提方法
CN113025419B (zh) * 2021-03-12 2022-09-23 郑州轻工业大学 一种鸭油的分提方法

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