JP7003313B1 - Powdered oil and fat composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a novel powder oil / fat composition, preferably a powder oil / fat composition having improved fluidity. SOLUTION: The powder fat and oil composition contains a fat and oil component containing one or more kinds of XXX type triglycerides having a fatty acid residue X having a carbon number x at the 1st to 3rd positions of glycerin, and the carbon number x is 16. It is an integer selected from about 20 and the powdered fat and oil composition contains β-type fat and oil, and the peak intensity ratio is 0.6 to 1 at the X-ray diffraction peak of the fat and oil component, and the powdered fat and oil composition. The degree of aggregation of the powdered fat or oil is 60% or less, the loosening bulk density of the powdered fat or oil composition is 0.05 to 0.6 g / cm3, and the relative value of the angle of repose is 90% or less. The composition is provided. [Selection diagram] Fig. 1

Description

The present invention relates to a powdered oil / fat composition and its use. More specifically, the present invention is a powder oil / fat composition containing an oil / fat component containing XXX-type triglyceride (containing β-type oil / fat and having a specific X-ray diffraction peak ratio at the X-ray diffraction peak). , A powdered fat composition characterized by having a specific degree of aggregation, a relative angle of repose, and a loose bulk density, a food containing the powdered fat composition, and the powdered fat composition. Containing powder fluidity improver and the like.

So far, as a powdered fat or oil composition, a powdered fat or oil composition containing a β-type fat or oil after melting the raw material of the fat or oil composition containing the XXX type liglyceride has been developed. (Patent Document 1). Such powdered oil / fat compositions have been used for the purpose of improving the powder fluidity of various powders, but there has been a demand for a material capable of further increasing the powder fluidity. Further, as a method for preparing a powdered oil / fat composition, a method of crushing an oil / fat having a high solid fat content at room temperature such as extremely hydrogenated oil and then aligning the particle size with a sieve (Patent Document 2), and a method of making the particle size uniform at room temperature such as extremely hydrogenated oil at room temperature. A method of melting fats and oils having a high solid fat content and directly spraying them (Patent Document 3) is known, but since the process is complicated, a method more suitable for industrialization has been sought. Further, there has been a demand for a material capable of further increasing the powder fluidity as compared with the powdered fats and oils produced by such a method.

International release WO2017 / 051910 Japanese Unexamined Patent Publication No. 52-71390 Japanese Unexamined Patent Publication No. 6-245700

One of the objects of the present invention is a powder oil / fat composition containing an oil / fat component containing XXX-type triglyceride, wherein the oil / fat component contains β-type oil / fat (at a specific X-ray diffraction peak ratio at an X-ray diffraction peak). It is possible to provide a powdered fat composition having a specific degree of aggregation, a relative angle of repose, and a loose bulk density.
One of the objects of the present invention may be to provide a food product and a powder fluidity improving agent, which comprises the above-mentioned powdered oil / fat composition.
One of the objects of the present invention may be to provide a powder having improved fluidity, for example, a powdered food having improved fluidity or a non-food powder having improved fluidity.

In order to achieve the above problems, the present inventors have made a powdered oil / fat composition containing an oil / fat component containing a specific XXX-type triglyceride (one or more), wherein the oil / fat component contains a β-type oil / fat. However, they have found that it is possible to provide a powdered oil / fat composition having novel properties such as improved fluidity when it has at least one property such as a specific degree of cohesion, a relative angle of repose, and a loose bulk density. It led to the invention. That is, the present invention may include the following aspects.

[1] A powdered oil / fat composition containing an oil / fat component containing one or more XXX-type triglycerides having a fatty acid residue X having the carbon number x at the 1st to 3rd positions of glycerin, wherein the carbon number x is 16 to 16. An integer selected from 20, wherein the powdered fat composition contains β-type fats and oils.
In the X-ray diffraction peak of the oil and fat component, the intensity ratio between the characteristic peak of β type near 4.6 Å and the characteristic peak of α type around 4.2 Å: [Peak intensity around 4.6 Å / ( Peak intensity around 4.6 Å + peak intensity around 4.2 Å)] is 0.6 to 1.
The degree of cohesion of the powdered oil / fat composition is 60% or less, the loosening bulk density of the powdered oil / fat composition is 0.05 to 0.6 g / cm ³ , and the relative value of the angle of repose determined by the formula (I) is A powdered oil / fat composition characterized by being 90% or less.
Relative value of repose = [angle of repose of the mixed powder of the powdered oil / fat composition and powdered starch] / [angle of repose of only the powdered starch not containing the powdered oil / fat composition] × 100 (I)
(In the formula (I), the "mixed powder" contains 1% by mass of the powdered oil / fat composition with respect to the total mass of the mixed powder.)
[2] The powdered fat or oil composition according to the above [1], wherein the powdered fat or oil composition contains 50% by mass or more of the XXX type triglyceride when the total mass of the powdered fat or oil composition is 100% by mass.
[3] The powdered fat or oil composition according to the above [1] or [2], wherein the powdered fat or oil composition is in the form of flakyse-containing particles in which a plurality of flakes are present on the surface.
[4] The powdered oil / fat composition according to the above [3], wherein the average particle size based on the volume average diameter of the particles is 0.5 to 200 μm.
[5]
The powdered oil / fat composition according to the above [3] or [4], wherein the average length of the long side of the flakes is 0.1 to 5 μm.
[6]
A food product comprising the powdered oil / fat composition according to any one of the above [1] to [5].
[7] A powder fluidity improving agent comprising the powder oil / fat composition according to any one of the above [1] to [5].

In addition, the present invention may include the following aspects.
[A]
A method for producing a powdered oil / fat composition containing an oil / fat component containing one or more XXX-type triglycerides having a fatty acid residue X having a carbon number x at the 1st to 3rd positions of glycerin, wherein the carbon number x is 16 to 16. It is an integer selected from 20, the fat and oil component contains β-type fat and oil, and the loosening bulk density of the powdered fat and oil composition is 0.05 to 0.6 g / cm ³ .
The following process,
(A) Step of preparing a solid oil / fat composition raw material containing XXX-type triglyceride,
(B) The solid oil / fat composition raw material obtained in step (a) is heated at a temperature below the melting point to change the oil / fat component in the solid oil / fat composition raw material into β-type oil / fat, and contains β-type oil / fat. The β-type oil-and-fat-containing composition raw material obtained in the steps of obtaining the composition raw material and (c) step (b) is pulverized by collision between the raw materials without mechanical pulverization to obtain a powdered oil-and-fat composition. Process,
A method for producing a powdered oil / fat composition, which comprises.
[B]
The method for producing a powdered fat or oil composition according to [A], wherein the powdered fat or oil composition contains 50% by mass or more of the XXX type triglyceride when the total mass of the powdered fat or oil composition is 100% by mass.
[C]
The method for producing a powdered fat or oil composition according to [A] or [B], wherein the temperature below the melting point of the step (b) is 1 to 30 ° C. lower than the melting point of the solid fat or oil composition raw material.
[D]
The method for producing a powdered oil / fat composition according to any one of [A] to [C], wherein the step (b) is performed in a state where the solid oil / fat composition raw material is allowed to stand.
[E]
The method for producing a powdered fat or oil composition according to any one of [A] to [C], wherein the step (b) is performed in a non-standing state of the solid fat and oil composition raw material.
[F]
The method for producing a powdered oil / fat composition according to [E], wherein the non-standing state is a state in which the solid oil / fat composition raw material is agitated.
[G]
The powdered oil / fat composition according to any one of claims [A] to [F], wherein the pulverization due to the collision between the raw materials in the step (c) is pulverization using an air flow type pulverizer without mechanical pulverization. Manufacturing method of things.
[H]
The method for producing a powdered fat or oil composition according to any one of claims [A] to [G], wherein the raw material for the solid fat and oil composition containing the XXX type triglyceride is rapeseed extremely hydrogenated oil.

INDUSTRIAL APPLICABILITY According to the present invention, a powdered oil / fat composition containing an oil / fat component containing XXX-type triglyceride, wherein the oil / fat component contains β-type oil / fat and has a specific degree of cohesion, a relative angle of repose, and a loose bulk density. An oil / fat composition can be provided.
INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide a food product and a powder fluidity improving agent, which are characterized by containing the powdered oil / fat composition.
INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide a powder having improved fluidity, for example, a powdered food having improved fluidity, a non-food powder having improved fluidity, or a powdered food.

It is an appearance photograph of the powder fats and oils composition (β type fats and oils) of Production Example 1. It is an appearance photograph of the powder fat composition (β type fat) of Production Example 4. It is an appearance photograph of the powder fat composition (α-type and β-type fats and oils) of the production comparative example 1. It is a micrograph of the powder fat composition (β type fat) of production comparative example 2. It is a micrograph of the powder fat composition (β type fat) of the production comparative example 5. It is a micrograph of the powder fat composition (β type fat) of the production comparative example 8. It is a micrograph of the powder fat composition (β type fat) of the production comparative example 9. It is an appearance photograph after the production example 1 was stored in the constant temperature bath of 40 degreeC for 5 days. It is an appearance photograph after the production comparative example 1 was stored in the constant temperature bath of 40 degreeC for 5 days. It is an appearance photograph after the production comparative example 4 was stored in the constant temperature bath of 40 degreeC for 5 days.

Here, the embodiments for carrying out the invention will be described in detail, but the preferred embodiments and more preferred embodiments exemplified below shall be used in combination with each other as appropriate regardless of expressions such as "favorable" and "more preferable". Can be done. Further, the description of the numerical range is an example, and a range in which the upper limit and the lower limit of each range and the numerical values of the examples are appropriately combined can also be preferably used. Further, terms such as "contains" or "contains" may be read as "essentially" or "consisting only".

<Powdered oil and fat composition>
One aspect of the present invention is a powdered oil / fat composition containing an oil / fat component containing one or more XXX-type triglycerides having a fatty acid residue X having carbon number x at the 1st to 3rd positions of glycerin. x is an integer selected from 16 to 20, and the powdered fat or oil composition contains β-type fat or oil.
In the X-ray diffraction peak of the fat component, the intensity ratio between the characteristic peak of β type near 4.6 Å and the characteristic peak of α type around 4.2 Å: [Peak intensity around 4.6 Å / ( Peak intensity near 4.6 Å + peak intensity near 4.2 Å)] (hereinafter, also referred to as peak intensity ratio) is 0.6 to 1.
The degree of cohesion of the powdered oil / fat composition is 60% or less, the loosening bulk density of the powdered oil / fat composition is 0.05 to 0.6 g / cm ³ , and the relative value of the angle of repose determined by the formula (I) is The present invention relates to a powdered oil / fat composition, which is characterized by being 90% or less.
Relative value of repose = [angle of repose of the mixed powder of the powdered oil / fat composition and powdered starch] / [angle of repose of only the powdered starch not containing the powdered oil / fat composition] × 100 (I)
Here, in the formula (I), the "mixed powder" contains 1% by mass of the powdered oil / fat composition with respect to the total mass of the mixed powder.
Hereinafter, the powdered oil / fat composition of the present invention will be described in detail.

<Fat and oil components>
The powdered oil / fat composition of the present invention contains an oil / fat component. The fat and oil component contains at least XXX type triglyceride, and optionally contains other triglycerides.
The above fats and oils include β-type fats and oils. Here, the β-type fat and oil is a fat and oil composed of only β-type crystals, which is one of the polymorphs of crystals of the fat and oil. Other polymorphic fats and oils include β'type fats and oils and α-type fats and oils, and β'type fats and oils are fats and oils composed only of β'type crystals, which is one of the polymorphic crystals of fats and oils. The α-type fats and oils are fats and oils composed of only α-type crystals, which is one of the polymorphs of crystals of fats and oils. Some fat crystals have the same composition but different sublattice structures (crystal structures), and are called crystal polymorphs. Typically, there are hexagonal type, orthorhombic vertical type and triclinic parallel type, which are called α type, β'type and β type, respectively. Further, the melting points of each polymorph become higher in the order of α, β', β, and the melting point of each polymorph differs depending on the type of fatty acid residue X having the number of carbon atoms x. The melting points (° C) of each polymorph in the case of tripalmitin, tristearin, and triarachidin are shown. Table 1 was prepared based on Nissim Garti et al., "Crystallization and Polymorphism of Fats and Fatty Acids", Marcel Dekker Inc., 1988, pp. 32-33. Then, in preparing Table 1, the melting point temperature (° C.) was rounded off to the first decimal place. Further, if the composition of the fat and oil and the melting point of each polymorph thereof are known, it is possible to detect at least whether or not the β-type fat and oil is present in the fat and oil.

A common method for identifying these polymorphs is X-ray diffraction, and the diffraction conditions are given by Bragg's equation below.
2dsinθ = nλ (n = 1, 2, 3 ...)
A diffraction peak appears at a position that satisfies this equation. Here, d is a lattice constant, θ is a diffraction (incident) angle, λ is an X-ray wavelength, and n is a natural number. From 2θ = 16 to 27 ° of the diffraction peak corresponding to the short surface spacing, information on the packing (secondary lattice) of the side surface in the crystal can be obtained, and the polymorph can be identified. Especially in the case of triacylglycerol, the characteristic peak of β type is at 2θ = 19, 23, 24 ° (near 4.6 Å) (near 3.9 Å), and α at around 21 ° (4.2 Å). A characteristic peak of the type appears. The X-ray diffraction measurement is performed using, for example, an X-ray diffractometer maintained at 20 ° C. (Rigaku Co., Ltd., a fully automated multipurpose X-ray diffractometer Smart Lab 9 kW). CuKα rays (1.54 Å) are most often used as the light source for X-rays.

Here, the fat and oil component contains β-type fat and oil and has a peak intensity ratio of 0.6 to 1, or contains β-type fat and oil as a main component (more than 50% by mass with respect to the powdered fat and oil composition or the fat and oil component). ).
A preferred embodiment of the fat and oil component is one in which the fat and oil component is substantially composed of β-type fat and oil, a more preferred embodiment is one in which the fat and oil component is composed of β-type fat and oil, and a particularly preferable embodiment is the above-mentioned fat and oil component. It consists only of β-type fats and oils. The case where all of the above fats and oils are β-type fats and oils is a case where α-type fats and oils and / or β'type fats and oils are not detected by the differential scanning calorimetry method.
As a further aspect of the present invention, it is preferable that all of the above fats and oils are β-type fats and oils, but other α-type fats and oils and β'type fats and oils may be contained.

Specifically, based on the above-mentioned findings regarding the X-ray diffraction measurement, the peak intensity of 2θ = 19 ° (4.6 Å), which is a characteristic peak of β type, and 2θ = 21 which is a characteristic peak of α type. Ratio of peak intensities of ° (4.2 Å): Peak intensities around 19 ° / (Peak intensities around 19 ° + Peak intensities around 21 °) [Peak intensities near 4.6 Å / (Peak intensities around 4.6 Å + By calculating the peak intensity around 4.2 Å)], it can be understood that "contains β-type fats and oils" as an index showing the abundance of β-type fats and oils as the above-mentioned fats and oils component. In the present invention, it is ideal that all of the above fats and oils are β-type fats and oils (that is, peak intensity ratio = 1).
That is, when this peak intensity ratio is 0, it is known that all are α-type fats and oils, and when the peak intensity ratio is 1, it is known that all are β-type fats and oils, and the peak intensity ratio is 1. If the number is close to, it can be seen that there are many β-type fats and oils.
In the present invention, it is preferable that the amount of β-type fats and oils in the fats and oils component is larger, so that the peak intensity ratio is preferably a value close to 1.
Therefore, the peak intensity ratio is preferably 0.6 to 1, more preferably 0.7 to 1, still more preferably 0.8 to 1, and even more preferably 0.9 to 1. , Particularly preferably 0.95 to 1.
The oil and fat component of the present invention is, for example, 50 to 100% by mass, 70 to 100% by mass, 80 to 100% by mass, 85 to 100% by mass, 92 to 100% by mass, and 95 to 100% by mass with respect to the powdered oil and fat composition. It may be about%.

<XXX type triglyceride>
The oil and fat component of the present invention contains one or more XXX-type triglycerides having a fatty acid residue X having the number of carbon atoms x at the 1st to 3rd positions of glycerin. The XXX-type triglyceride is a triglyceride having a fatty acid residue X having the number of carbon atoms x at the 1st to 3rd positions of glycerin, and each fatty acid residue X is the same as each other. Here, the number of carbon atoms x is an integer selected from 16 to 20, preferably an integer selected from 16 to 18, and more preferably 18.
The fatty acid residue X may be a saturated or unsaturated fatty acid residue. Specific examples of the fatty acid residue X include, but are not limited to, residues such as palmitic acid, stearic acid, and arachidic acid. The fatty acids are more preferably palmitic acid and stearic acid, and even more preferably stearic acid.
The content of the XXX-type triglyceride is, for example, 50% by mass or more, preferably 60% by mass or more, more preferably 70% by mass or more, when the total mass of the powdered fat composition or the fat component is 100% by mass. More preferably, the lower limit is 80% by mass or more, and for example, the upper limit is 100% by mass or less, preferably 99% by mass or less, and more preferably 95% by mass or less. One type or two or more types of XXX type triglyceride can be used, preferably one type or two types, and more preferably one type. When there are two or more types of XXX-type triglyceride, the total value is the content of XXX-type triglyceride.

<Other triglycerides>
The oil and fat component of the present invention may contain other triglycerides other than the above-mentioned XXX type triglyceride as long as the effects of the present invention are not impaired. The other triglyceride may be a plurality of types of triglycerides, and may be synthetic fats and oils or natural fats and oils. Examples of synthetic fats and oils include glyceryl tricaprylate and glyceryl tricaprate. Examples of natural fats and oils include cocoa butter, sunflower oil, rapeseed oil, soybean oil, cottonseed oil and the like. When the total triglyceride in the powdered fat composition or the fat component of the present invention is 100% by mass, the other triglycerides are, for example, 1% by mass or more when the total mass of the powdered fat composition or the fat component is 100% by mass. Or, there is no problem even if it is contained in an amount of about 5 to 50% by mass. The content of other triglycerides is, for example, 0 to 50% by mass, preferably 5 to 40% by mass, and more preferably 10 to 30% by mass when the total mass of the powdered fat composition or the fat component is 100% by mass. , More preferably 15 to 25% by mass.

<Other ingredients>
In addition to the above-mentioned oil and fat components such as triglyceride, the powdered oil and fat composition of the present invention may optionally contain other components (additives) such as emulsifiers, fragrances and colorants. Any of these other components can also be added to the powdered oil / fat composition of the present invention.
Here, examples of the emulsifier as the other component include monoglyceride, polyglycerin fatty acid ester, sucrose fatty acid ester, sorbitan fatty acid ester, lecithin and the like, and examples of the fragrance include limonene, vanillin and orange. , Vanilla, jasmine and the like, and examples of the coloring agent include natural coloring agents such as turmeric pigment, cutinashi pigment, benivana pigment, paprika pigment, red cabbage pigment, and synthetic coloring agent such as tar-based pigment. be able to.
The amount of these other components can be any amount as long as the effect of the present invention is not impaired. For example, when the total mass of the powdered oil / fat composition is 100% by mass, for example, 0 to 30% by mass. It is preferably 1 to 18% by mass, more preferably 2 to 15% by mass, and further preferably 3 to 8% by mass. 90% by mass or more of the other components are preferably powders having an average particle size of 1000 μm or less, and more preferably powders having an average particle size of 500 μm or less. Further, since fine particles of 20 μm or less are difficult to be perceived by human senses, a powder having an average particle size of, for example, 20 μm or less, preferably 0.1 to 20 μm, and more preferably 1 to 12 μm is used in the mouth. It is preferable because it eliminates the rough and rough feel of the powder when it is contained in. Unless otherwise specified, the average particle size referred to in the present specification is a value measured by a laser diffraction / scattering method (ISO13320 and JIS Z 8825-1 compliant). The laser diffraction / scattering method will be described in detail below.
However, it is preferable that the preferred powdered oil / fat composition of the present invention is substantially composed of only the above-mentioned oil / fat component, and the oil / fat component is preferably composed of substantially only triglyceride. Further, "substantially" means that the component other than the oil and fat component contained in the oil and fat composition or the component other than the triglyceride contained in the oil and fat component is 100% by mass of the powdered oil and fat composition or the oil and fat component. For example, it means 0 to 15% by mass, preferably 1 to 10% by mass, and more preferably 2 to 5% by mass.

<Characteristics of powdered oil and fat composition>
The powdered oil / fat composition of the present invention is a solid powder at 20 ° C. The powdered oil / fat composition of the present invention may have the following physical properties.
[Cohesion]
The "degree of agglomeration" is a numerical value of the ease of agglomeration of particles. The degree of cohesion can be determined, for example, by applying a constant vibration to the sieve for a predetermined time and measuring the amount of powder remaining. It can be determined that the smaller the degree of cohesion is, the higher the fluidity of the powder is, and the larger the degree of cohesion is, the lower the fluidity of the powder is.
As an example of measuring the degree of cohesion, a method of measuring using a powder tester PT-X (manufactured by Hosokawa Micron Co., Ltd.) can be mentioned. Specifically, three circular sieves with different mesh openings (7.5 cm in diameter: upper sieve: mesh opening 355 μm, middle sieve: mesh opening 250 μm, lower mesh: mesh opening 150 μm) are stacked and accurately preliminarily on the upper sieve. About 2 g of the weighed sample powder is provided, and the entire sieve is vibrated horizontally with an amplitude of 1 mm at a vibration time T (seconds) described later. Then, the mass of the sample powder remaining on each sieve is further weighed, and the degree of cohesion can be calculated from the following formula (II).
The degree of cohesion is measured three times for one sample, and the average value of the obtained values is taken as the degree of cohesion of the sample.

Cohesion degree (%) = (U / N + M / N × 3/5 + L / N × 1/5) × 100 (II)

(In the formula, U: mass of sample powder on upper sieve (g), M: mass of sample powder on middle sieve (g), L: mass of sample powder on lower sieve (g), N : Mass of initial sample powder (g))

The degree of cohesion of the powdered oil / fat composition of the present invention that can be calculated from the above formula (II) is, for example, 0% or more and 60% or less, 55% or less, or 51% or less, preferably 1 to 60%. It is more preferably 2 to 55%, and even more preferably 3 to 51%.

[Vibration time T]
The vibration time T (seconds) used in the measurement of the degree of cohesion is calculated by the following formula (III).
T (seconds) = 20 + {(1.6-W) /0.016} (III)
Here, W is the dynamic bulk density of the powder and is calculated from the following equation (IV).
W = (QP) C / 100 + P (IV)
(In the formula, P: loose bulk density, Q: solid bulk density, C: degree of compression) However, when W ≧ 1.6, T = 20.
Further, the solidified bulk density, the loosened bulk density, and the degree of compression can be obtained as follows.

[Loose bulk density]
The loose bulk density (g / cm ³ ) is the value obtained by dividing the mass of the powder by the bulk volume occupied by the powder, that is, the mass of the powder per unit bulk volume.
The loosening bulk density can be measured using a powder tester PT-X (manufactured by Hosokawa Micron Corporation). In the measurement by the powder tester PT-X, the injection method is adopted, and the measurement is performed by freely dropping the powder or granular material containing air into the container by the vibration of a sine and cosine wave.
Specifically, 200 to 300 cm ³ of the powder sample is placed on a circular sieve with a diameter of 7.5 cm and an opening of 1.7 mm, vibrated with an amplitude of 1.5 mm, and dropped from the sieve (free fall due to vibration of a sine wave). .. The powder sample that freely fell from a height of 27 cm was injected into a stainless steel 100 cm ³ cup (inner diameter of about 5 cm × height of about 5 cm) placed under the sieve until the powder sample overflowed from the cup. After that, stop the vibration of the sieve. Then, the excess powder sample on the cup is ground along the upper surface of the cup with a rectangular blade, and the mass (A (g)) of the powder sample in the cup is measured to loosen the bulk density by the following formula (V). ).
The loosening bulk density is measured three times for one sample, and the average value is taken as the value of the loosening bulk density of the sample.

Loose bulk density (g / cm ³ ) = A (g) / 100 (cm ³ ) (V)

The loosening bulk density of the powdered oil / fat composition of the present invention is, for example, 0.05 to 0.6 g / cm ³ , preferably 0.1 to 0.5 g / cm ³ when it is substantially composed of only the oil / fat component. It is more preferably 0.1 to 0.4 cm ³ , and even more preferably 0.1 to 0.3 g / cm ³ .

[Hardening bulk density]
The solidified bulk density (g / cm ³ ) is the bulk density obtained from the powder obtained by further tapping and solidifying the loose bulk density powder.
Specifically, a cylindrical shape having a hole of the same size as the cup at the upper part of the opening of a 100 cm ³ cup (inner diameter of about 5 cm x height of about 5 cm) made of stainless steel after loosening and measuring the bulk density as described above. A cap (hole diameter 5.04 cm x height 4 cm, both ends of the cylinder are open) is attached to extend the opening of the cup. A stainless steel 100 cm ³ cup with a tubular cap is placed under a circular sieve with a diameter of 7.5 cm and an opening of 1.7 mm. A powder sample of 200 to 300 cm ³ is placed on a sieve, vibrated with an amplitude of 1.5 mm, and dropped from the sieve (free fall due to vibration of a sine wave). A sample that has freely fallen from a height of 27 cm is injected into a stainless steel 100 cm ³ cup installed below in a sufficient amount, and the cup is tapped 180 times (stroke 18 mm, tapping speed 60 times / minute) to prepare the sample. Consolidate. When tapping is performed, the powder or granular material is compacted and its volume is reduced. If the powder level of the powder or granular material drops below the top of the cup due to a decrease in the volume of the powder or granular material during tapping, the sample is injected into the cup again in the same manner, and the powder surface of the powder or granular material is at the top of the cup. Try to be higher. After the tapping is completed, the cap is removed, the excess sample on the cup is ground along the surface of the cup with a blade, and the mass (B (g)) is measured to calculate the solidification bulk density from the following formula (VI).
The compaction bulk density is measured three times for one sample, and the average value is taken as the value of the compaction bulk density of the sample.

Hardening bulk density (g / cm ³ ) = B (g) / 100 (cm ³ ) (VI)

The solidified bulk density of the powdered oil / fat composition of the present invention is, for example, 0.1 to 2.0 g / cm ³ , preferably 0.1 to 1.0 g / cm ³ when it is substantially composed of only the oil / fat component. It is more preferably 0.15 to 0.7 cm ³ , and even more preferably 0.2 to 0.5 g / cm ³ .

[Compression]
The degree of compression C (%) is a value obtained by the following formula (VII) using the loosened bulk density P and the hardened bulk density Q.
C (%) = 100 × (QP) / Q (VII)

[Relative value of angle of repose]
The powdered fat composition of the present invention has a specific relative angle of repose. Here, the relative angle of repose means the ratio of the angle of repose of the mixture when the powdered oil / fat composition is mixed with the starch such as powdered potato to the angle of repose of the starch itself such as powdered potato. The value is called the relative value of the angle of repose. By confirming the relative angle of repose, the effect of improving the starch fluidity of the powdered oil / fat composition can be confirmed. The angle of repose relative value is specifically a value obtained by the following equation (I).

Relative value of repose (%) = [Angle of repose of a mixed powder of the powdered oil / fat composition and powdered starch] / [Angle of repose of only the powdered starch not containing the powdered oil / fat composition] × 100 (I)

Here, in the formula (I), the "mixed powder" contains 1% by mass of the powdered oil / fat composition with respect to the total mass of the mixed powder. As the "powdered starch", powdered potato starch, potato starch and the like can be used. The average particle size of the powdered starch is, for example, 1 to 100 μm, preferably 10 to 50 μm, and more preferably 20 to 40 μm. Here, the average particle size means the volume average diameter [MV] measured by the laser diffraction / scattering method (ISO13320 and JIS Z 8825-1 compliant), and is specifically as described below. The "angle of repose" is defined as the angle at which the free surface of the stationary powder deposit layer (the ridgeline of the mountain formed by the deposited powder) becomes horizontal after the powder is dropped on a horizontal plane. .. In general, a powder having good fluidity has a small angle of repose, and a powder having poor fluidity has a large angle of repose.
Therefore, when the relative value of the rest angle obtained by the above formula (I) becomes larger than 100%, the fluidity of the mixed powder of the powdered oil / fat composition and the powdered starch becomes worse than the fluidity of the powdered starch itself, that is, , The powdered oil / fat composition adversely affected the fluidity of the powdered starch, and conversely, if the relative rest angle value is smaller than 100%, the fluidity of the mixed powder of the powdered oil / fat composition and the powdered starch Is better than the fluidity of the powdered starch itself, that is, the powdered oil and fat composition has improved the fluidity of the powdered starch.

The relative value of the angle of repose of the powdered oil / fat composition of the present invention is, for example, 90% or less, preferably 88% or less, more preferably 86% or less, and even more preferably 84% or less. The angle of repose relative value of the powdered oil / fat composition of the present invention is, for example, 70% or more, preferably 75% or more, and more preferably 80% or more.
The angle of repose required for calculating the relative value of the angle of repose can be measured using, for example, a test device such as Powder Tester PT-X (manufactured by Hosokawa Micron Corporation).
Specifically, 297 g of powdered potato starch (product name: domestic potato starch (Hokkaido) (manufactured by Hinokuni Food Industry Co., Ltd.), average particle size of 34.8 μm measured by the laser diffraction scattering method described later) was used as the test target. Add 3 g of various powders to be added, stir and mix with a food processor (product name "Food Processor 1.9 L", manufactured by Conair Japan GK) for 20 seconds, and add 1% by mass of the powdered oil / fat composition to the total mass. The mixed powder to be contained) is prepared.
As a control, the powdered potato starch to which the powdered fat composition is not added is stirred and mixed with a food processor for 20 seconds in the same manner as described above to prepare a control sample.

The angle of repose of the obtained sample and the control sample can be measured using the above-mentioned powder tester.
Specifically, 200 to 300 cm ³ of the above sample or control sample is placed on a circular sieve with a diameter of 7.5 cm and an opening of 710 μm, vibrated with an amplitude of 1.5 mm, and dropped from the sieve (free fall due to vibration of a sine wave). ). After passing through a funnel with a diameter of 5 mm at the opening under the sieve, the above samples and the like are dropped from a height of 7.5 cm from the lower end of the funnel onto a circular table (diameter 8 cm), and powder is released from the end of the table. Accumulate to the extent that it overflows. After that, the angle formed by the free surface (the ridgeline of the mountain formed by the deposited powder) of the powder deposit layer formed by the stationary sample or the like is calculated by an image, and the value is used as the angle of repose.
The angle of repose is measured three times for one sample, and the average value is taken as the value of the angle of repose of the sample.

〔Specific surface area〕
The specific surface area (cm ² / g) of the powdered oil / fat composition can be measured by the N ₂ gas adsorption method (multi-point method).
The measurement by the N ₂ gas adsorption method (multi-point method) can be performed by using, for example, a specific surface area measurement analyzer manufactured by Micromeritics. Specifically, 1.2 to 1.5 g of a sample is collected in a cell, and about 24 at room temperature (about 25 ° C.) using a pretreatment device (manufactured by Micromeritics, device name “VacPrep 061”). After degassing under reduced pressure for a period of time, the specific surface area can be measured by the N ₂ gas adsorption method (multi-point method) using a specific surface area measurement analyzer (manufactured by Micromeritics, device name "3Flex"). .. The value of the specific surface area of the powdered oil / fat composition is, for example, 0.5 to 10 m ² / g, preferably 0.5 to 8 m ² / g, more preferably 1 to 8 m ² / g, still more preferably 1 to 7 m ² . / G is appropriate.

[Shape of powdered oil / fat composition]
The powdered oil / fat composition of the present invention has the form of flakes-containing particles in which a plurality of flakes are present on the surface. The shape of the flakes-containing particles has an indefinite shape in which irregularities are formed on the surface due to the existence and accumulation of a plurality of flakes on the surface. Although it is not clear what kind of structure the inside of the fragment-containing particles has because the cross section of the particles cannot be directly seen, the powdered oil / fat composition of Production Example 1 in FIG. 1 (average particle size 3.5 μm). And, judging from the appearance photograph of the powdered oil / fat composition (average particle size 10.5 μm) of Production Example 4 in FIG. 2, even the particles of Production Example 1 crushed to be smaller than Production Example 4 are grains. Similar to the particles of Production Example 4 having a large diameter, a plurality of flakes are present on the surface of the particles, and the appearance thereof is almost the same. Will be done.
In the examples, the micrographs of the particles and the relative values of the angle of repose will be compared, and the relative value of the angle of repose of the powdered oil / fat composition of the present invention is 90% or less, although the mechanism is not clear. It is presumed that this is due to the structure of such special particles.
The average particle size (effective diameter) of the particles is, for example, preferably 0.5 to 200 μm, more preferably 1 to 100 μm, still more preferably 1 to 50 μm, and particularly preferably 1 to 30 μm.
Here, the average particle size (effective diameter) refers to a volume average diameter [MV], and is a laser diffraction scattering method (ISO13320, manufactured by Shimadzu Corporation, device name: SALD-2300) using a particle size distribution measuring device. Based on JIS Z 8825-1), the volume-based particle size distribution was measured by dry measurement to obtain the volume average diameter [MV], and the obtained volume average diameter [MV] was used as the average particle size. The volume average diameter [MV] can be obtained from the following formula using the respective values of the particle size of the particles, the volume of the particles, and the sum of the volumes of the particles.

Volume average diameter [MV] = sum of (particle size x volume of the particle) / sum of the volume of the particle

The effective diameter means the particle size of the spherical shape when the measured diffraction pattern of the crystal to be measured matches the theoretical diffraction pattern obtained by assuming that the crystal is spherical. In this way, in the case of the laser diffraction / scattering method, the effective diameter is calculated by matching the theoretical diffraction pattern obtained assuming a spherical shape with the measured diffraction pattern, so that even if the measurement target is a plate shape. Even if it has a spherical shape, it can be measured by the same principle.

Here, as the dimensions (long side, short side, thickness) of the particle surface of the powdered oil / fat composition of the present invention, an average value obtained by measuring the size from an electron micrograph can be adopted. .. The average length of the long sides of the flakes is, for example, preferably 0.01 to 5 μm, more preferably 0.05 to 4 μm, still more preferably 0.1 to 3 μm, still more preferably 0.2 to 2. It is 5 μm. The average length of the short sides of the flakes is shorter than the long sides, eg, preferably 0.01-4 μm, more preferably 0.05-3 μm, even more preferably 0.1-2 μm, even more preferably 0. .2 to 1 μm. The average length of the thickness of the flakes is shorter than the long and short sides, for example, preferably 0.005 to 0.5 μm, more preferably 0.01 to 0.3 μm, still more preferably 0.02 to 0.02. It is 0.2 μm, and even more preferably 0.03 to 0.15 μm.

<Manufacturing method of powdered oil / fat composition>
The powdered oil / fat composition of the present invention does not melt, for example, a solid oil / fat composition raw material containing one or more XXX-type triglycerides having a fatty acid residue X having the number of carbon atoms x at the 1st to 3rd positions of glycerin. By heating the oil / fat component in the raw material to a specific temperature according to the type of XXX-type triglyceride at a temperature below the melting point, β-type oil / fat (preferably, the peak intensity ratio of the X-ray diffraction peak is 0.6 to After the change to 1), the raw materials are made to collide with each other and pulverized to obtain a powdery fat or oil composition (powdered fat or oil composition). Specifically, the following method for producing a powdered oil / fat composition can be exemplified.

A method for producing a powdered oil / fat composition containing an oil / fat component containing one or more XXX-type triglycerides having a fatty acid residue X having a carbon number x at the 1st to 3rd positions of glycerin, wherein the carbon number x is 16 to 16. It is an integer selected from 20, the fat and oil component contains β-type fat and oil, and the loosening bulk density of the powdered fat and oil composition is 0.05 to 0.6 g / cm ³ .
Preferably, in the X-ray diffraction peak of the oil and fat component, the intensity ratio between the characteristic peak of β type near 4.6 Å and the characteristic peak of α type around 4.2 Å: [peak near 4.6 Å]. Intensity / (peak intensity around 4.6 Å + peak intensity around 4.2 Å)] is 0.6 to 1, and preferably, the degree of cohesion of the powdered oil / fat composition is 60% or less.
The following process,
(A) Step of preparing a solid oil / fat composition raw material containing XXX-type triglyceride,
(B) The solid fat / oil composition raw material obtained in step (a) is heated at a temperature below the melting point so as not to be preferably melted, and the fat / oil component in the solid fat / oil composition raw material is made into β-type fat / oil. (Preferably, the peak intensity ratio of the X-ray diffraction peak is changed to 0.6 to 1) to obtain a β-type oil / fat-containing composition raw material, and (c) contains the β-type oil / fat obtained in step (b). A step of crushing a composition raw material by collision between the raw materials without mechanical crushing to obtain a powdered oil / fat composition.
A method for producing a powdered oil / fat composition, which comprises.
Hereinafter, the steps (a) to (c) will be described.

(A) Raw Material Preparation Step The raw material for a solid oil / fat composition containing XXX-type triglyceride prepared in the step (a) is one or more XXX having a fatty acid residue X having the number of carbon atoms x at the 1st to 3rd positions of glycerin. It is manufactured based on a method for producing fats and oils such as ordinary XXX-type triglycerides containing type triglycerides, or can be easily obtained from the market. The solid oil / fat composition raw material may have any shape such as powder, flakes, and blocks. Here, the XXX-type triglyceride specified by the number of carbon atoms x and the fatty acid residue X may be the same as that of the desired powdered oil / fat composition or oil / fat component finally obtained except for the polymorphism. .. That is, the details of each term such as the XXX type triglyceride, the oil / fat component, the powdered oil / fat composition, etc. can be defined as already described above except that it does not matter whether the crystalline polymorph is β type or not. .. The raw material may contain α-type fats and oils, β'-type fats and oils, or β-type fats and oils.
The solid oil / fat composition raw material may contain one or more of the XXX-type triglycerides as described above, preferably one or two, and more preferably one.
Specifically, for example, the XXX-type triglyceride can be produced by direct synthesis using a fatty acid or a fatty acid derivative and glycerin. As a method for directly synthesizing the XXX type triglyceride, (i) a method for directly esterifying the fatty acid X having the carbon number x and glycerin (direct ester synthesis), and (ii) the carboxyl group of the fatty acid X having the carbon number x is alkoxyl. A method for reacting a fatty acid alkyl bonded to a group (for example, fatty acid methyl and fatty acid ethyl) with glycerin under basic or acidic catalytic conditions (ester exchange synthesis using fatty acid alkyl), (iii) carbon number x. Examples thereof include a method (acid halide synthesis) in which a fatty acid halide (for example, fatty acid chloride and fatty acid bromide) in which the hydroxyl group of the carboxyl group of fatty acid X is replaced with a halogen is reacted with glycerin under a basic catalyst.
The XXX-type triglyceride can be produced by any of the above-mentioned methods (i) to (iii), but from the viewpoint of ease of production, (i) direct ester synthesis or (ii) transesterification synthesis using fatty acid alkyl is possible. Preferably, (i) direct ester synthesis is more preferred.

In order to produce XXX-type triglyceride by (i) direct ester synthesis, it is preferable to use 3 to 5 mol of fatty acid X or fatty acid Y with respect to 1 mol of glycerin, and 3 to 4 mol is used. Is more preferable.
The reaction temperature of the XXX-type triglyceride (i) in the direct ester synthesis may be any temperature as long as the water produced by the esterification reaction can be removed from the system, for example, 120 ° C to 300 ° C, preferably 150 ° C to 270 ° C. More preferably, 180 ° C to 250 ° C is even more preferable. By carrying out the reaction at 180 to 250 ° C., XXX-type triglyceride can be produced particularly efficiently.

In (i) direct ester synthesis of XXX-type triglyceride, a catalyst that promotes the esterification reaction may be used. Examples of the catalyst include acid catalysts and alkoxides of alkaline earth metals. The amount of the catalyst used is preferably about 0.001 to 1% by mass with respect to the total mass of the reaction raw materials.
In (i) direct ester synthesis of XXX-type triglyceride, catalysts and unreacted raw materials are removed by performing known purification treatments such as washing with water, alkaline deoxidation and / or vacuum deoxidization, and adsorption treatment after the reaction. can do. Further, by subjecting the decolorization / deodorization treatment, the obtained reaction product can be further purified.

The amount of XXX-type triglyceride contained in the solid oil / fat composition raw material is preferably 100 to 50% by mass, for example, when the total mass of all triglycerides contained in the raw material or the oil / fat component is 100% by mass. Is 95 to 55% by mass, more preferably 90 to 60% by mass. Even more preferably, it is 85 to 65% by mass.

<Other triglycerides>
As other triglycerides used as raw materials for solid oil and fat compositions containing XXX-type triglycerides, in addition to the above-mentioned XXX-type triglycerides, various triglycerides may be included as long as the effects of the present invention are not impaired. As other triglycerides, for example, one of the fatty acid residues X of the XXX-type triglyceride is replaced with the fatty acid residue Y, and two of the fatty acid residues X of the XXX-type triglyceride are replaced with the fatty acid residue Y. XY2 type triglyceride and the like can be mentioned.
The amount of the other triglycerides is, for example, 0 to 50% by mass, preferably 5 to 45% by mass, more preferably 10 to 40% by mass, and even more preferably 10% by mass, when the total mass of all triglycerides is 100% by mass. It is 15 to 35% by mass.

Further, as the raw material for the solid oil / fat composition of the present invention, instead of directly synthesizing the above-mentioned XXX-type triglyceride, a naturally-derived triglyceride composition obtained by hydrogenation, transesterification or fractionation may be used. .. Examples of the naturally derived triglyceride composition include rapeseed oil, soybean oil, sunflower oil, hyoleic sunflower oil, safflower oil, palm stea and mixtures thereof. In particular, hydrogenated oils, partially hydrogenated oils, and extremely hydrogenated oils of these naturally derived triglyceride compositions are preferred. Further preferred are hard palm stea, high oleic sunflower oil extremely hydrogenated oil, rapeseed extremely hydrogenated oil, soybean extremely hydrogenated oil, and even more preferably rapeseed extremely hydrogenated oil.

Further, examples of the raw material for the solid fat and oil composition of the present invention include commercially available triglyceride compositions and synthetic fats and oils. For example, examples of the triglyceride composition include hard palm stearin (manufactured by Nisshin Oillio Group Co., Ltd.), rapeseed extremely hydrogenated oil (manufactured by Yokoseki Oil & Fat Industry Co., Ltd.), and soybean extremely hydrogenated oil (manufactured by Yokoseki Oil & Fat Industry Co., Ltd.). can. Examples of synthetic fats and oils include tripalmitin (manufactured by Tokyo Chemical Industry Co., Ltd.), tristearin (manufactured by Sigma-Aldrich), tristearin (manufactured by Tokyo Chemical Industry Co., Ltd.), and triarakidin (manufactured by Tokyo Chemical Industry Co., Ltd.). can.

<Other ingredients>
In addition to the triglyceride, the solid oil / fat composition raw material may optionally contain other components such as a partial glyceride, a fatty acid, an antioxidant, an emulsifier, and a solvent such as water. The amount of these other components can be any amount as long as the effect of the present invention is not impaired, but for example, when the total mass of the raw material for the oil and fat composition is 100% by mass, it is preferably 0 to 5% by mass. Is 0 to 2% by mass, more preferably 0 to 1% by mass.

When a plurality of components are contained in the solid oil / fat composition raw material, they may be arbitrarily mixed. Any known mixing method may be used as long as a homogeneous reaction substrate can be obtained, and the mixing is carried out by, for example, a paddle mixer, a horse mackerel homomixer, a disper mixer, a V-type mixer, a W-type mixer, a ribbon mixer or the like. be able to.

(B) Step of changing to β-type fat and oil Before the step (c), the fat and oil component in the solid fat and oil composition raw material prepared in the above step (a) is subjected to β-type fat and oil (preferably X-ray diffraction peak). The crystal polymorph is changed so that the peak intensity ratio of is 0.6 to 1).
In the process of changing to β-type fats and oils, the fat component changed to one containing β-type fats and oils. It can be judged from the intensity of the β-type characteristic peak / (intensity of the α-type characteristic peak + the intensity of the β-type characteristic peak)] (peak intensity ratio).
Specifically, based on the above-mentioned findings regarding the X-ray diffraction measurement, the peak intensity of 2θ = 19 ° (4.6 Å), which is a characteristic peak of β type, and 2θ = 21 which is a characteristic peak of α type. Ratio of peak intensities of ° (4.2 Å): Peak intensities around 19 ° / (Peak intensities around 19 ° + Peak intensities around 21 °) [Peak intensities near 4.6 Å / (Peak intensities around 4.6 Å + By calculating the peak intensity around 4.2 Å)], it can be understood that "contains β-type fats and oils" as an index showing the abundance of β-type fats and oils as the above-mentioned fats and oils component.
That is, when this peak intensity ratio is 0, it is known that all are α-type fats and oils, and when the peak intensity ratio is 1, it is known that all are β-type fats and oils, and the peak intensity ratio is 1. If the number is close to, it can be seen that there are many β-type fats and oils. In the present invention, it is ideal that all of the above fats and oils are β-type fats and oils (that is, peak intensity ratio = 1).
Therefore, in the step of changing to β-type fat and oil, the peak intensity ratio of the fat and oil component is preferably 0.6 to 1, more preferably 0.7 to 1, still more preferably 0.8 to 1, and even more preferably 0. The treatment is carried out so as to be 9.9 to 1, particularly preferably 0.95 to 1.

Various methods can be used for changing to β-type fats and oils, but as a typical method, the solid fat and oil composition raw material obtained in step (a) is not melted and is kept at a temperature below the melting point. It is a method of heating. The "melting point" referred to here is the melting point of the oil / fat composition raw material, and more preferably the melting point of the oil / fat component in the oil / fat composition raw material. It is important that the raw material of the fat and oil composition does not melt, that is, the fat and oil component is changed to β-type fat and oil without melting. The heating temperature is preferably kept constant throughout the heating step. Here, “constant” means that, for example, it is appropriate to control the temperature change to ± 3 ° C, preferably ± 1 ° C, and more preferably ± 0.5 ° C.
Further, the heating is preferably performed at a temperature at which the fat and oil components in the solid fat and oil composition raw material do not melt through the heating step.
The step of heating the solid oil / fat composition raw material to change it into β-type oil / fat can be performed by putting the solid oil / fat composition raw material in a constant temperature bath and leaving it to stand, for example, a machine such as a horizontal stirring tank. Can also be used to heat the raw material with stirring, i.e., in a non-static environment. The method of heating in a non-static state has an advantage that the production efficiency is improved because the time for changing to β-type fats and oils is shorter.
For example, the heating temperature is 1 to 30 from the melting point of a solid fat or oil composition raw material containing a fat or oil component containing one or more XXX-type triglycerides having a fatty acid residue X having the number of carbon atoms x at the 1st to 3rd positions of glycerin. It is appropriate that the temperature is lower than the melting point, preferably 2 to 27 ° C. lower than the melting point, more preferably 3 to 23 ° C. lower than the melting point, and even more preferably 3 to 19 ° C. lower than the melting point.
For example, in the case of XXX-type triglyceride having three stearic acid residues having 18 carbon atoms, the melting point of β-type fats and oils is 74 ° C. (Table 1), so that the heating temperature is 1 to 30 ° C. lower than the melting point (Table 1). That is, it is preferably 44 to 73 ° C.), more preferably 2 to 27 ° C. lower than the melting point (that is, 47 to 72 ° C.), and 3 to 23 ° C. lower than the melting point (that is, 51 to 71 ° C.). ), And even more preferably a temperature 3 to 19 ° C. lower than the melting point (that is, 55 to 71 ° C.).
Further, in the case of the XXX type triglyceride having 16 carbon atoms, the heating temperature is preferably 36 to 65 ° C, more preferably 39 to 64 ° C. When the number of carbon atoms x is 20, the heating temperature is preferably 48 to 77 ° C, more preferably 51 to 76 ° C.
Further, for example, in the case of a flake-shaped rapeseed extremely hardened oil having a melting point of 67 ° C., the heating temperature is 1 to 30 ° C. lower than the melting point (that is, 37 to 66 ° C.), preferably 2 to 27 ° C. lower than the melting point. (Ie, 40-65 ° C), more preferably 3-23 ° C lower than the melting point (ie 44-64 ° C), even more preferably 3-19 ° C lower than the melting point (ie 48-64 ° C). Is appropriate.
The heating time may be a time sufficient for changing to β-type fats and oils, but for example, 10 minutes or more, preferably 20 minutes to 120 hours, more preferably 30 minutes to 100 hours, still more preferably 30 to 72. Time is appropriate.

The step (b) can be carried out in a stationary state or a non-static state of the solid oil / fat composition raw material.
Examples of heating in a stationary state include a method in which a solid oil / fat composition raw material is placed in a constant temperature room, a constant temperature bath, or the like and heated. In order to shorten the heating time of heating in a stationary state, it is preferable to heat in a state where heat is transferred to the entire raw material, and in order to achieve such a state, it is preferable to lower the height of the deposition of the raw material during heating. As a method of heating by lowering the height of the deposit of the raw material, for example, the height of the deposit of the solid oil / fat composition raw material is low in a stainless steel container having a length of 10 to 100 cm, a width of 10 to 100 cm, and a height of 5 to 30 cm. There is a method of spreading and laying it so as to be, and heating it in a constant temperature room, a constant temperature bath, or the like. If it is not necessary to shorten the heating time, it is not necessary to reduce the height of the deposition of the raw material.
The heating time in the case of heating in a stationary state is not particularly limited as long as it is a time sufficient for the fat and oil component to change to β-type fat and oil, for example, preferably 20 minutes or more, more preferably 30 minutes to 120 hours. , More preferably 10 to 100 hours, even more preferably 15 to 72 hours. Solid fats and oils to be heat-treated If the height of the deposit of the raw material is lowered and the heat is quickly transferred to the whole raw material, it can be changed to β-type fat and oil in a short time, but the deposit of the raw material If the height is high and the heat transfer to the whole raw material is slow, heating for a longer time is required.

Examples of the heating in the non-standing state include a method of heating a solid oil / fat composition raw material while stirring using a horizontal stirring tank or the like.
The heating time in the case of heating in a stationary state is not particularly limited as long as it is a sufficient time for the fat and oil component to change to β-type fat and oil, but is, for example, 10 minutes or more, 15 minutes or more, or 20 minutes or more. The upper limit of the heating time is preferably 5 hours or less, more preferably 2 hours or less. It is preferable that the heating time is short from the viewpoint of improving work efficiency.

(C) Step of crushing raw materials by collision with each other to obtain a powdered oil / fat composition The β-type oil / fat-containing composition raw materials obtained in the above step (b) are crushed together with an air flow type crusher or the like without mechanical pulverization. It can be pulverized by colliding the raw materials with each other to obtain a powdered oil / fat composition.
The crushing by colliding the raw materials can be performed by using an air flow type crusher or the like that does not involve mechanical crushing. "Mechanical crushing" means crushing mechanically with a crushing device such as an impeller or a hammer installed in a cyclone mill or a hammer mill. "No mechanical crushing" is interpreted to mean that "crushing by colliding raw materials with each other" does not simultaneously perform mechanical crushing. In the present invention, as an initial step of pulverization, although it is permissible to pulverize the raw material obtained in step (b) with a crusher and mechanically pulverize, a final powdered oil / fat composition is obtained. It is appropriate that the immediately preceding crushing is performed only by colliding the raw materials with each other, and at that time, no mechanical crushing is performed. Here, the "air flow type crushing" is a method of crushing a crushing object by using an air flow such as compressed air and colliding with each other moving objects to be crushed by the air flow. Unlike the method of mechanically crushing the crushed object, the crushed objects collide with each other, so that the surface of the crushed particles is smoothed by a hammer surface or the like, and the surface characteristics are not changed, and the particles are finer. Particles can be obtained. Further, by using an airflow type crusher equipped with a classifier, particles having a desired particle size can be obtained. Examples of the "air flow type crusher" include a fluidized layer type jet mill and a counter type jet mill. As a more specific air flow type crusher, for example, a crusher "counter jet" manufactured by Hosokawa Micron Co., Ltd. Mill 200AFG "and the like.
For example, when the counter jet mill is used, the classification speed can be set to, for example, 1800 to 12000 rpm. As the classification rate is increased, the average particle size of the obtained powdered oil / fat composition tends to be smaller. Therefore, the average particle size of the obtained particles can be adjusted by changing the classification rate.
It is appropriate that the step (c) is a step immediately before obtaining the final powdered oil / fat composition. As long as the raw materials are finally crushed by colliding with each other and then the final powdered oil / fat composition is obtained without mechanical crushing, even if the raw materials are crushed by a crusher or the like before being crushed by the airflow type crusher. good. Further, the raw material of the fat or oil composition converted into β-type fat or oil by heating may be pulverized after the product temperature has been cooled to room temperature (25 ° C. ± 5 ° C.).

<Use of powdered oil and fat composition>
The powdered fat and oil composition of the present invention can be used in various fields using powdered fats and oils as a raw material. In particular, it can be used in the food field such as bread, confectionery, cake mix, noodles, flour, batter, tempura flour, fried flour, powdered starch, and powdered potato starch. Further, the powdered oil / fat composition of the present invention can be used as a powder fluidity improving agent for improving the fluidity of powdered foods and the like.

<Foods and non-foods containing oil and fat compositions>
The content of the powdered oil / fat composition in the food of the present invention varies depending on the type of the target food, but for example, when the total amount of the finally obtained food is 100% by mass, for example, 0.1 to 99% by mass. %, Preferably 0.1 to 90% by mass, more preferably 0.5 to 80% by mass, still more preferably 1 to 70% by mass. The food product of the present invention can be produced by a known method except that the powdered oil / fat composition of the present invention is used as a raw material. When a powdered food is used, the average particle size of the powdered food is, for example, 1 to 100 μm, preferably 10 to 50 μm, and more preferably 20 to 40 μm. In addition, non-food powders other than foods can be used in the same manner as the above foods.

<Powder fluidity improver>
The powdered oil / fat composition used in the present invention can be used as a powder fluidity improving agent for improving the fluidity of the powder. For example, by adding the powdered oil / fat composition used in the present invention as a part of the raw material of the powdered food such as starch, the fluidity of the conventional powdered food can be improved. The improvement in fluidity can be confirmed, for example, by the degree of cohesion and the relative value of the angle of repose. Preferred cohesion and angle of repose relative values are as described above.
The powder fluidity improving agent of the present invention may be any as long as it contains the above-mentioned powdered oil / fat composition as an active ingredient, and other than this, dextrin, starch and the like can be added as long as the effects of the present invention are not impaired. It may contain other components such as a shaping agent and an emulsifier.
The powder fluidity improver of the present invention contains the above-mentioned powder oil / fat composition. The powder fluidity improver of the present invention contains the above-mentioned powdered oil / fat composition in an amount of preferably 50 to 100% by mass, more preferably 80 to 100% by mass, still more preferably 90 to 100% by mass.
However, it is preferable that the preferable powder fluidity improving agent of the present invention is substantially composed of only the powdered oil / fat composition. Further, "substantially" means, for example, 0 to 10% by mass when the component other than the powder oil / fat composition contained in the powder fluidity improving agent is 100% by mass of the powder fluidity improving agent. It means that it is preferably 0 to 5% by mass, more preferably 0 to 3% by mass.
The amount of the powder fluidity improving agent of the present invention added to powdered foods (starch, etc.) is preferably 0.05 to 20% by mass, more preferably 0.08 to 10% by mass, and further. It is preferably 0.1 to 5% by mass.

Next, the present invention will be described in detail with reference to Production Examples and Comparative Production Examples.
[Analysis method]
Hereinafter, various analysis methods used will be described. Although a part of Production Example 1 is described as an example, the same analysis is performed for all Production Examples and Production Comparative Examples described here unless otherwise specified.
-Triglyceride composition Triglyceride composition was performed by gas chromatography analysis. The measurement conditions are shown below. Gas chromatography analysis conditions
DB1-ht (0.32 mm x 0.1 μm x 5 m) Agilent Technologies (123-1131)
Injection volume: 1.0 μL
Injection port: 370 ℃
Detector: 370 ℃
Split ratio: 50/1 35.1kPa Constant pressure column CT: 200 ℃ (0min hold) ～ (15 ℃ / min) ～ 370 ℃ (4min hold)
・ X-ray diffraction measurement Using an X-ray diffractometer (Rigaku Co., Ltd., fully automated multipurpose X-ray diffractometer Smart Lab 9 kW), using CuKα (λ = 1.542 Å) as the radiation source, using a Cu filter, output The measurement was performed under the conditions of 9.0 kW, an operation angle of 0.96 to 30.0 °, and a measurement speed of 20 ° / min. By this measurement, the presence of α-type fat, β'-type fat, and β-type fat in the fat component containing XXX-type triglyceride was confirmed. If it has only a peak near 4.6 Å and does not have a peak around 4.1 to 4.2 Å, it can be determined that all of the fat and oil components are β-type fats and oils.
Therefore, from the results of the above X-ray diffraction measurement, the peak intensity ratio = [intensity of β-type characteristic peak (2θ = 19 ° (4.6 Å)) / (intensity of α-type characteristic peak (2θ = 21)). ° (4.2 Å)) + β-type characteristic peak intensity (2θ = 19 ° (4.6 Å)))] was calculated, and the value was judged as an index indicating the abundance of β-type fats and oils.

-Cohesion degree The cohesion degree was measured using a powder tester PT-X (manufactured by Hosokawa Micron Corporation).
Specifically, three circular sieves having a diameter of 7.5 cm, which are selected from the bulk density and have different openings, (upper stage sieve: mesh opening 355 μm, middle stage sieve: mesh opening 250 μm, lower stage sieve: mesh opening 150 μm) are stacked. About 2 g of the powdered oil / fat composition of Production Example 1 was applied to the upper sieve, and the entire sieve was vibrated horizontally with an amplitude of 1 mm with a vibration time of 106 seconds. Then, the mass of the powdered oil / fat composition of Production Example 1 remaining on each sieve was weighed, and the degree of cohesion was calculated from the following formula (II). The degree of cohesion was measured three times for one sample powder (powdered oil / fat composition of Production Example 1), and the average value obtained was taken as the degree of cohesion of the powdered oil / fat composition of Production Example 1.

Cohesion degree (%) = (U / N + M / N × 3/5 + L / N × 1/5) × 100 (II)
(In the formula, U: mass of sample powder on upper sieve (g), M: mass of sample powder on middle sieve (g), L: mass of sample powder on lower sieve (g), N : Mass of initial sample powder (g))

The vibration time (T (seconds)) was calculated by the method using the formula (III) and the formula (IV) described in [Mode for carrying out the invention].
T (seconds) = 20 + {(1.6-W) /0.016} (III)
(W is the dynamic bulk density of the powder and is calculated from the following equation (IV))
W = (QP) C / 100 + P (IV)
(In the formula, P: loose bulk density, Q: solid bulk density, C: degree of compression) However, when W ≧ 1.6, T = 20.

Loose bulk density The loose bulk density (g / cm ³ ) was determined as the value obtained by dividing the mass of the powder by the bulk volume occupied by the powder, that is, the mass of the powder per unit bulk volume.
The loose bulk density was measured using a powder tester PT-X (manufactured by Hosokawa Micron Corporation). The powder tester PT-X adopts the injection method, and the measurement is performed by freely dropping the powder or granular material containing air into the container by the vibration of a sine and cosine wave.
Specifically, 200 to 300 cm ³ of the powder sample was applied to a circular sieve having a diameter of 7.5 cm and an opening of 1.7 mm, vibrated with an amplitude of 1.5 mm, and dropped from the sieve (free fall due to vibration of a sine wave). ). The powder sample that has fallen freely from a height of 27 cm is injected into a stainless steel 100 cm ³ cup (inner diameter of about 5 cm x height of about 5 cm) placed under the sieve, and after the powder sample is injected until it overflows from the cup. , Stopped the vibration of the sieve. Then, the excess powder sample on the cup is ground along the upper surface of the cup with a rectangular blade, and the mass (A (g)) of the powder sample in the cup is measured to loosen the bulk density by the following formula (V). Calculated from. The loosening bulk density was measured three times for one sample, and the average value was taken as the value of the loosening bulk density of the sample.
Loose bulk density (g / cm ³ ) = A (g) / 100 (cm ³ ) (V)

・ Hardened bulk density After measuring the loosened bulk density, a cylindrical cap (hole diameter 5) with a hole of the same size as the cup at the top of the opening of a 100 cm ³ cup (inner diameter approx. 5 cm x height approx. 5 cm) made of stainless steel. .04 cm x 4 cm in height, both ends of the cylinder are open) were attached to extend the opening of the cup. A stainless steel 100 cm ³ cup with a tubular cap was placed under a circular sieve with a diameter of 7.5 cm and an opening of 1.7 mm. A powder sample of 200 to 300 cm ³ was placed on a sieve, vibrated with an amplitude of 1.5 mm, and dropped from the sieve (free fall due to vibration of a sine wave). A sample that has freely fallen from a height of 27 cm is injected into a stainless steel 100 cm ³ cup installed below in a sufficient amount, and the cup is tapped 180 times (stroke 18 mm, tapping speed 60 times / minute) to prepare the sample. Consolidated. By tapping, the powder or granular material was compacted and its volume was reduced. If the powder level of the powder or granular material drops below the top of the cup due to a decrease in the volume of the powder or granular material during tapping, the sample is injected into the cup again in the same manner, and the powder surface of the powder or granular material is at the top of the cup. Made it higher. After the tapping was completed, the cap was removed, the excess sample on the cup was ground along the surface of the cup with a blade, and the mass (B (g)) was measured to solidify and the bulk density was calculated from the following formula (VI).
The compaction bulk density was measured three times for one sample, and the average value was taken as the value of the compaction bulk density of the sample.

Hardening bulk density (g / cm ³ ) = B (g) / 100 (cm ³ ) (VI)

-Compression degree The compression degree C (%) was obtained from the following formula (VII) using the loosening bulk density P and the solidifying bulk density Q.
C (%) = 100 × (QP) / Q (VII)

-Relative rest angle powder 297 g of potato starch (product name: domestic potato starch (Hokkaido) (manufactured by Hinokuni Food Industry Co., Ltd.), average particle size of 34.8 μm measured by the laser diffraction scattering method described later), Production Example 1 Add 3 g of the powdered fat and oil composition (containing 1% by mass of the powdered fat and oil composition to the total mass) to prepare a mixed powder, and use the mixed powder as a food processor (product name "Food Processor 1.9 L"). A sample was prepared by stirring and mixing for 20 seconds with (manufactured by Conair Japan GK). Samples to which the powdered oil and fat compositions of Production Examples 2 to 4 and Comparative Examples 1 to 9 were added instead of the powdered oil and fat composition of Production Example 1 were also prepared by the same method.
As a control, the powdered potato starch itself to which the powdered fat composition was not added was similarly stirred and mixed with a food processor for 20 seconds to prepare a control sample.
The angle of repose of the obtained sample was measured using a powder tester PT-X (manufactured by Hosokawa Micron Corporation).
Specifically, 200 to 300 cm ³ of the powder sample was applied to a circular sieve having a diameter of 7.5 cm and an opening of 1.7 mm, vibrated with an amplitude of 1.5 mm, and dropped from the sieve (free fall due to vibration of a sine wave). ). After passing through a funnel with a diameter of 5 mm at the opening under the sieve, the powder sample is dropped from a height of 7.5 cm onto a circular table (diameter 8 cm) and deposited to the extent that the powder overflows from the end of the table. I let you. The angle formed by the free surface of the powder deposit layer to be formed was calculated from an image, and the value was taken as the angle of repose.
The angle of repose was measured three times for one sample, and the average value was taken as the angle of repose of the sample.
Next, using the measured angle of repose value, the relative value of the angle of repose was obtained from the following equation (I).

Relative value of repose (%) = [Angle of repose of a mixed powder of the powdered potato starch and the powdered potato starch] / [Angle of repose of the powdered potato starch alone not containing the powdered potato starch] × 100 (I)

(In the formula (I), the "mixed powder" contains 1% by mass of the powdered oil / fat composition with respect to the total mass of the mixed powder).

-Specific surface area The specific surface area (cm ² / g) of the powdered oil / fat composition was measured by the N ₂ gas adsorption method (multi-point method).
Specifically, 1.2 to 1.5 g of a sample is collected in a cell, and a pretreatment device (manufactured by Micromeritics Co., Ltd., device name "VacPrep 061") is used for 24 hours at room temperature (25 ° C.). After the degassing treatment under reduced pressure, the specific surface area was measured by the N ₂ gas adsorption method (multi-point method) using a specific surface area measurement analyzer (manufactured by Micromeritics, device name "3Flex").

-Average particle size The average particle size is volume-based by dry measurement based on the laser diffraction and scattering method (ISO13320, JIS Z 8825-1) with a particle size distribution measuring device (manufactured by Shimadzu Corporation, device name: SALD-2300). The particle size distribution was measured to obtain the volume average diameter [MV], and the obtained volume average diameter [MV] was used as the average particle size. The volume average diameter [MV] was calculated from the following formula using the respective values of the particle size of the particles, the volume of the particles, and the sum of the volumes of the particles.

Volume average diameter [MV] = sum of (particle size x volume of the particle) / sum of the volume of the particle

-Observation of appearance The appearance of the obtained powdered oil and fat compositions was visually observed.
Further, the shape of the particles of the powdered oil / fat composition was observed at a magnification of 10,000 times using an electron microscope (“JSM-7500F” manufactured by JEOL Ltd.).
The method of vapor deposition of the sample observed with an electron microscope is described below.
First, a conductive tape was put on the copper plate and the sample powder was placed on the copper plate, and then a blower treatment with nitrogen gas was performed for the purpose of removing the surplus sample. Then, as the thin-film deposition treatment, an osmium vapor deposition treatment (30 nm) was performed using an Osmium plasma coator (“OPC-80” manufactured by Nippon Plasma & Electronics Lab.).

The size of the flakes present on the surface of the particles of the powdered oil / fat composition The size of the flakes present on the surface of the particles of the powdered oil / fat composition obtained in Production Examples 1 to 4 and Comparative Example 1 is described above. It was measured using the electron micrograph.
The long side (μm), short side (μm), and thickness (μm) of the slices shown in the electron micrograph were measured. The measurement was performed on 10 flakes, and the average value was calculated.
-The details of the flake-shaped rapeseed extremely hydrogenated oil used as a raw material in the raw material production example and the production comparative example are as follows.
It has a fatty acid residue X (stearic acid residue) with 18 carbon atoms at the 1st to 3rd positions of glycerin when the total mass of α-type fats and oils and rapeseed extremely hydrogenated oil manufactured by Yokoseki Yushi Kogyo Co., Ltd. is 100% by mass. The content of XXX type triglyceride is 79.6% by mass, peak intensity ratio: 0.03, melting point 67 ° C.

Production Examples 1 to 4 (constant greenhouse, counter jet mill)
Put 20 kg of flake-shaped rapeseed extremely hydrogenated oil in a paper bag (length: 800 mm, width 450 mm :, thickness: 150 mm) and put it in a constant temperature room (width: 5100 mm x height: 2100 mm x depth: 4050 mm, manufactured by ESPEC CORPORATION, It was placed in an apparatus name "TBUU") and allowed to stand at 62 ° C. where melting did not occur for 64 hours to obtain flake-shaped oils and fats.
12.0 kg of the obtained flaky fat and oil was crushed by a crusher to obtain a crushed fat and oil. A powdered fat or oil composition (powdered fat or oil composition) is obtained by crushing 6.0 kg of the obtained crushed fat or oil by collision between raw materials using an air flow type crusher (manufactured by Hosokawa Micron Co., Ltd., device name "Counter Jet Mill 200AFG"). When the total mass is 100% by mass, the content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin is 79.6% by mass) 4.8 kg. Got In addition, Production Examples 1 to 4 are produced by the same method except that the classification speed at the time of crushing is different as shown in Table 2. It was confirmed by X-ray diffraction analysis that the crystalline polymorphs of the fats and oils in the obtained powdered fats and oils compositions of Production Examples 1 to 4 were β-type. Table 2 shows the crushing conditions of the airflow type crusher, the appearance of each sample, the analytical values, and the crystal polymorphs of the fats and oils in each powdered fat and oil composition confirmed by X-ray diffraction analysis.

As a result of observing each particle of the powdered oil / fat composition of Production Examples 1 to 4 with an electron microscope based on the above appearance observation, the particles have irregularities on the surface due to the presence / accumulation of a plurality of flakes on the surface. It was an indefinite shape. For reference, the electron micrograph of Production Example 1 is shown in FIG. 1, and the electron micrograph of Production Example 4 is shown in FIG.

Production Example 5 (β conversion treatment only, homeothermic treatment)
A beta treatment of α-type fats and oils was investigated using a homeothermic environment.
Specifically, 6 kg of flake-shaped rapeseed extremely hydrogenated oil is spread in a stainless steel container (width: 530 mm x depth: 325 mm x height: 200 mm) and spread in a constant temperature room (width: 5100 mm x height: 2100 mm x depth:). 4050 mm, manufactured by Espec Co., Ltd., device name "TBUU") placed in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm), heat-treated at 40 ° C for 28 days, and heat-treated flake-shaped oils and fats. (When the total mass of the powdered oil / fat composition is 100% by mass, the content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin is 79.6. Weight%) 6 kg was obtained.
By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the heat-treated flake-shaped fats and oils were β-type. Table 3 shows the heating method, appearance, analytical values, and polymorphs of fats and oils confirmed by X-ray diffraction analysis.

Production Example 6 (β conversion treatment only, homeothermic treatment)
A beta treatment of α-type fats and oils was investigated using a homeothermic environment.
Specifically, 6 kg of flake-shaped rapeseed extremely hydrogenated oil is spread in a stainless steel container (width: 530 mm x depth: 325 mm x height: 200 mm) and spread in a constant temperature room (width: 5100 mm x height: 2100 mm x depth:). Flake-shaped oil and fat placed in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm) in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm) in 4050 mm, manufactured by Espec Co., Ltd., and heat-treated at 62 ° C for 15 hours. (When the total mass of the powdered oil / fat composition is 100% by mass, the content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin is 79.6. Weight%) 6 kg was obtained.
By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the heat-treated flake-shaped fats and oils were β-type. Table 3 shows the heating method, appearance, analytical values, and polymorphs of fats and oils confirmed by X-ray diffraction analysis.

Production Example 7 (β conversion treatment only, horizontal stirring tank)
Using a horizontal agitation tank, β-formation treatment of α-type fats and oils was examined.
Specifically, 4.0 kg of flake-shaped rapeseed extremely hydrogenated oil is heated at 63 ° C. and a stirring speed of 100 rpm for 30 minutes using a horizontal stirring tank (manufactured by Matsubo Co., Ltd., device name “Radige Mixer M20”). By the treatment, XXX having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin when the total mass of the powdered oil / fat composition is 100% by mass. The content of the type triglyceride was 79.6% by mass) 3.8 kg was obtained. By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the heat-treated flake-shaped fats and oils were β-type. Table 3 shows the heating method, appearance, analytical values, and polymorphs of fats and oils confirmed by X-ray diffraction analysis.

Production Example 8 (β conversion treatment only, horizontal stirring tank)
Using a horizontal agitation tank, β-formation treatment of α-type fats and oils was examined.
Specifically, 4.0 kg of flake-shaped rapeseed extremely hydrogenated oil is heated at 65 ° C. and a stirring speed of 50 rpm for 1 hour using a horizontal stirring tank (manufactured by Matsubo Co., Ltd., device name “Radige Mixer M20”). By the treatment, XXX having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin when the total mass of the powdered oil / fat composition is 100% by mass. The content of the type triglyceride was 79.6% by mass) 3.8 kg was obtained. By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the heat-treated flake-shaped fats and oils were β-type. Table 3 shows the heating method, appearance, analytical values, and polymorphs of fats and oils confirmed by X-ray diffraction analysis.

From the results in Table 3 above, it was found that by heat-treating the α-type fats and oils at a temperature of 40 ° C. to 65 ° C., the raw materials can be converted into β-type fats and oils without melting. Further, as can be seen from Production Examples 5 and 6, when comparing the heating times when the same heating device is used, there is a tendency that the higher the heating temperature, the shorter the time for changing to β-type fats and oils. It was seen. Further, it is better to heat the heated raw material in a non-static state in a stirred state as in Production Examples 7 and 8 than to heat the heated raw material in a stationary state as in Production Examples 5 and 6. It was found that the time to change to β-type fats and oils can be shortened.

Manufacturing Comparative Example 1 (without β-treatment, counter jet mill)
12.0 kg of flaky rapeseed extremely hydrogenated oil was crushed with a crusher to obtain 11.5 kg of crushed oil and fat. By crushing 6.0 kg of the obtained crushed fat and oil with an air flow type crusher (manufactured by Hosokawa Micron Co., Ltd., device name "Counter Jet Mill 200AFG"), the powdered fat and oil composition (total mass of the powdered fat and oil composition is 100 mass). The content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin was 79.6% by mass), and 4.8 kg was obtained. By X-ray diffraction analysis, it was confirmed that the polymorphs of the fats and oils in the obtained powdered fats and oils composition were α-type and β-type.
Although the heat treatment was not performed in Production Comparative Example 1, it is considered that a part of the α-type fat and oil was changed to the β-type fat and oil due to the heat generated during crushing by the airflow type crusher.
Table 4 shows the crushing conditions of the airflow type crusher, the appearance of the sample, the analytical values, and the crystal polymorphs of the fats and oils in the powdered fats and oils composition confirmed by the X-ray diffraction analysis.

As a result of observing the particles of the powdered oil / fat composition of Production Comparative Example 1 with an electron microscope based on the above-mentioned appearance observation, the particles had irregularities on the surface due to the presence / accumulation of a plurality of flakes on the surface. It had an irregular shape. For reference, the electron micrograph of Production Comparative Example 1 is shown in FIG.

Manufacturing Comparative Example 2 (constant greenhouse, cyclone mill (mechanical and airflow crusher))
Spread 6.0 kg of flake-shaped rapeseed extremely hydrogenated oil in a stainless steel container (width: 530 mm x depth: 325 mm x height: 200 mm) and spread it in a constant temperature room (width: 5100 mm x height: 2100 mm x depth: 4050 mm, ESPEC. Placed in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm) in a steel rack (width: 760 mm x depth: 1795 mm) manufactured by Co., Ltd., and cycled at 66 ° C for 4 hours and 63 ° C for 4 hours three times, and flakes. The shape of oil and fat was obtained.
6.0 kg of the obtained flake-shaped fat and oil was crushed by a crusher to obtain a crushed fat and oil.
Next, 4.0 kg of the obtained crushed fat and oil was crushed with a mechanical airflow type crusher (manufactured by Shizuoka Plant Co., Ltd., device name "Cyclone Mill 150BMS") to obtain 3.5 kg of powdered fat and oil composition. Obtained. Here, the cyclone mill is a crusher having three functions of mechanical crushing by an impeller, airflow type crushing by collision of particles in a high-speed airflow, and centrifugal classification. In order to further reduce the particle size of the powdered fat and oil composition, 1.3 kg of the obtained powdered fat and oil composition was once again subjected to a mechanical and air flow type crusher (manufactured by Shizuoka Plant Co., Ltd., device name "Cyclone Mill". After crushing with 150 BMS ”), fatty acid residue X (stearic acid residue) having 18 carbon atoms is added to the 1st to 3rd positions of glycerin in the powdered fat and oil composition (when the total mass of the powdered fat and oil composition is 100% by mass). The content of the XXX-type triglyceride contained was 79.6% by mass), and 1.0 kg was obtained. By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the fats and oils in the obtained powdered fats and oils composition were β-type. Table 5 shows the crushing conditions of the mechanical and airflow crushers, the appearance of the sample, the analytical values, and the crystal polymorphs of the fats and oils in the powdered fats and oils composition confirmed by the X-ray diffraction analysis.

As a result of observing the particles of the powdered oil / fat composition of Production Comparative Example 2 with an electron microscope based on the above-mentioned appearance observation, some irregularly shaped particles in which the flakes are not present on the surface are present, and the flakes are present on the surface. There were also irregularly shaped particles with irregularities formed on the surface due to the existence and accumulation of multiple particles.
On the other hand, in the pulverization by the cyclone mill, not only the irregularly shaped particles having irregularities formed on the surface due to the presence of a plurality of flakes on the surface but also the irregularly shaped particles in which the flakes were not on the surface of the particles were present ( FIG. 4). The reason for the existence of irregularly shaped particles in which flakes are not on the surface of the particles is that in crushing with a cyclone mill, not only airflow crushing due to collisions between particles in a high-speed airflow, but also mechanical crushing with an impeller is performed at the same time. It is probable that the flakes on the surface were crushed and disappeared.
From this, in order to produce an amorphous powder oil / fat composition in which irregularities are formed on the surface of most particles due to the presence / accumulation of a plurality of flakes on the surface, the final powder oil / fat composition is prepared. It was found that in the crushing step immediately before the acquisition, it is necessary to manufacture using a crusher that does not perform mechanical crushing, for example, an air flow type crusher.

Production Comparative Examples 3 to 7 (solidification after melting, counter jet mill)
2 kg of flake-shaped rapeseed extremely hydrogenated oil is spread and spread in a stainless steel container (width: 530 mm x depth: 325 mm x height: 100 mm), and a total of 6 stainless steel containers are placed in a constant temperature room (width: 5100 mm x height: 2100 mm x). Depth: 4050 mm, manufactured by Espec Co., Ltd., device name "TBUU"), placed in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm) and maintained at 80 ° C, which exceeds the melting point, for 10 hours. After completely melting, it is cooled at 60 ° C. for 15 hours to form a solid substance having voids with increased volume, and after crystallization is completed, it is cooled to a room temperature (25 ° C.) state to obtain a fat and oil solid substance. rice field.
12.0 kg of the obtained fat and oil solid was crushed by a crusher to obtain a fat and oil crushed product. Next, 10.0 kg of the obtained crushed fat and oil was crushed by an air flow type crusher (manufactured by Hosokawa Micron Co., Ltd., device name "Counter Jet Mill 200AFG") to obtain a powdered fat and oil composition (all of the powdered fat and oil composition). When the mass is 100% by mass, the content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin is 79.4% by mass) 7.8 kg. Obtained. By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the fats and oils in the obtained powdered fats and oils composition were β-type. Table 6 shows the crushing conditions of the airflow type crusher, the appearance of the sample, the analytical values, and the crystal polymorphs of the fats and oils in the powdered fats and oils composition confirmed by the X-ray diffraction analysis.

As a result of observing the particles of the powdered oil / fat composition of Production Comparative Examples 3 to 7 with an electron microscope based on the above-mentioned appearance observation, the particles have irregularities formed on the surface due to the presence / accumulation of a plurality of flakes on the surface. It was not an indefinite shape, but just a plate shape. For reference, the electron micrograph of Production Comparative Example 5 is shown in FIG.

Manufacturing Comparative Example 8 (constant greenhouse, cyclone mill (mechanical and airflow crusher))
2.0 kg of flake-shaped rapeseed extremely hydrogenated oil was spread and spread in a stainless steel container (width: 530 mm x depth: 325 mm x height: 100 mm), and a total of three stainless steel containers were placed in a constant temperature room (width: 5100 mm x height: 100 mm). 2100 mm x depth: 4050 mm, manufactured by Espec Co., Ltd., device name "TBUU"), placed in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm) and maintained at 80 ° C above the melting point for 10 hours. After completely melting, the mixture was cooled at 60 ° C. for 16 hours to form a solid substance having voids with increased volume, and after crystallization was completed, it was cooled to a room temperature (25 ° C.) state to form an oil / fat solid substance. Got
6.0 kg of the obtained fat and oil solid was crushed by a crusher to obtain a fat and oil crushed product.
Next, 5.8 kg of the obtained crushed fat and oil was crushed by a mechanical and airflow type crusher (manufactured by Shizuoka Plant Co., Ltd., device name "Cyclone Mill 150BMS") to obtain a powdered fat and oil composition (powdered fat and oil composition). When the total mass of the substance is 100% by mass, the content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin is 79.4% by mass) 5. Obtained 0.4 kg.
Here, the cyclone mill is a crusher having three functions of mechanical crushing by an impeller, airflow type crushing by collision of particles in a high-speed airflow, and centrifugal classification.
By X-ray diffraction analysis, it was confirmed that the crystal polymorphs of the fats and oils in the obtained powdered fats and oils composition were β-type.
Table 7 shows the crushing conditions of the mechanical and airflow type crushers, the appearance of the sample, the analytical values, and the crystal polymorphs of the fats and oils in the powdered fats and oils composition confirmed by the X-ray diffraction analysis.

As a result of observing the particles of the powdered oil / fat composition of Production Comparative Example 8 with an electron microscope based on the above appearance observation, the particles had irregularities formed on the surface due to the presence / accumulation of a plurality of flakes on the surface. It was not a shape, but just a plate shape. For reference, the electron micrograph of Production Comparative Example 8 is shown in FIG.

Production Comparative Example 9 (Crystal after melting, mechanical crusher)
2.0 kg of flake-shaped rapeseed extremely hydrogenated oil was spread and spread in a stainless steel container (width: 530 mm x depth: 325 mm x height: 100 mm), and a total of three stainless steel containers were placed in a constant temperature room (width: 5100 mm x height: 100 mm). 2100 mm x depth: 4050 mm, manufactured by Espec Co., Ltd., device name "TBUU"), placed in a steel rack (width: 760 mm x depth: 460 mm x height: 1795 mm) and maintained at 80 ° C above the melting point for 10 hours. After completely melting, the mixture was cooled at 60 ° C. for 16 hours to form a solid substance having voids with increased volume, and after crystallization was completed, it was cooled to a room temperature (25 ° C.) state to form an oil / fat solid substance. Got
6.0 kg of the obtained fat and oil solid was crushed by a crusher to obtain a fat and oil crushed product.
Next, 5.8 kg of the obtained crushed fat and oil is crushed by a fine crusher with a built-in impact type classifier (manufactured by Hosokawa Micron Co., Ltd., device name "ACM-10A"), which is a mechanical crusher, to obtain powdered fat and oil. The content of XXX-type triglyceride having a fatty acid residue X (stearic acid residue) having 18 carbon atoms at the 1st to 3rd positions of glycerin when the total mass of the powdered oil / fat composition is 100% by mass is 79. 0.4% by mass) 5.5 kg was obtained. By X-ray diffraction analysis, it was confirmed that the polymorphism of the fat and oil in the obtained powdered fat and oil composition was β-type. Table 8 shows the pulverization conditions of the fine pulverizer with a built-in impact classifier, the appearance of the sample, the analytical values, and the crystal polymorphs of the oil and fat in the powdered oil and fat composition confirmed by the X-ray diffraction analysis.

As a result of observing the particles of the powdered oil / fat composition of Production Comparative Example 9 with an electron microscope based on the above appearance observation, the particles had irregularities formed on the surface due to the presence / accumulation of a plurality of flakes on the surface. It was not a shape, but just a plate shape. For reference, the electron micrograph of Production Comparative Example 9 is shown in FIG.

[Storage stability test at 40 ° C and 20 ° C]
The α-type and β-type oil-containing powder oil and fat compositions obtained in Production Comparative Example 1 and the β-type oil and fat-containing powder oil and fat compositions obtained in Production Example 1 and Production Comparative Example 4 are stable in storage at 40 ° C. Sex test 1 was performed. Specifically, about 100 g of each sample was placed in a polyethylene plastic bag, stored in a constant temperature bath (light-shielded state) at 40 ° C. for 5 days, and the appearance after storage was observed (FIGS. 8 to 10). Further, the storage stability test 2 in which the storage condition was changed from "40 ° C. for 5 days" to "20 ° C. for 5 months" was also performed in the same manner. The results of storage stability tests 1 and 2 are shown in Table 9.

From Table 9, when each powdered fat or oil composition was stored at 40 ° C. for 5 days, the appearance of the powdered fat or oil composition of Production Example 1 and Production Comparative Example 4 which were β-type fats and oils did not change (FIGS. 8 and 8). 10) In the powdered fat and oil composition of Production Comparative Example 1 containing α-type and β-type fats and oils (FIG. 9), blocking (aggregation of powder) occurred and large lumps were formed.
Further, when each powdered fat or oil composition was stored at 20 ° C. for 5 months (long-term storage), the appearance of the powdered fats and oils compositions of Production Example 1 and Production Comparative Example 4, which were β-type fats and oils, did not change, but α. The powdered fat and oil composition of Production Comparative Example 1 containing the mold and β-type fats and oils had some blocking (powder aggregation).
From the above, the powdered fat and oil composition of Production Comparative Example 1 containing α-type and β-type fats and oils is a powder having poor storage stability in both cases of 40 ° C. for 5 days and 20 ° C. for 5 months. Because it was there, it was judged that it had no commercial value.

[Angle of repose relative value test]
Tables 10 to 12 show the relative values of the angle of repose of the powdered potato starch to which 1% by mass of the powdered fat composition of Production Examples 1 to 4 and Production Comparative Examples 1 to 9 was added.
In addition, Table 13 shows the relative values of the angle of repose of the powdered potato starch to which 1% by mass of the powdered fat composition of Production Example 1 and Production Comparative Example 4 stored at 20 ° C. for 5 months after production was added.

From Tables 10 to 12, the cohesiveness of the powdered oil and fat compositions of Production Examples 1 to 4 was 60% or less, and the cohesiveness of the powdered oil and fat compositions of Production Comparative Examples 3 to 9 was 66% or more. It was found that the powder oil and fat compositions of Production Examples 1 to 4 had higher powder fluidity than the powder oil and fat compositions of Comparative Examples 3 to 9.
Therefore, since the powdered oil / fat composition of the present invention is a powder having good handleability, it is easy to handle at the time of manufacturing the powdered oil / fat composition, and the powdered oil / fat composition is added to other components to make a powder mixture. It is considered that the work efficiency of the production of the powder mixture is improved in the case of producing.
Further, the relative angles of repose of the powdered potato starch to which the powdered fat and oil compositions of Production Examples 1 to 4 were added were all 90% or less, and the powdered potato starch to which the powdered fat and oil compositions of Production Comparative Examples 2 and 4 to 9 were added had a relative angle of repose. The relative angle of repose was greater than 90%. From this, it was found that the powdered oil / fat composition of the present invention can improve the fluidity of the powder by adding it to a powder such as starch.
Although the mechanism is not clear, considering the shape of the particles of FIGS. 1 to 7, this difference in the relative value of the rest angle is due to the powdered oil and fat compositions (FIGS. 1 and 2) and the production of Production Examples 1 and 4 of the present invention. The particles of Comparative Example 1 (FIG. 3) are in the form of shard-containing particles having a plurality of shards on the surface, while the powder oil / fat composition of Production Comparative Example 2 has a surface due to the presence of a plurality of shards on the surface. Not only the irregularly shaped particles having irregularities formed on the surface, but also the irregularly shaped particles having no flakes on the surface of the particles (FIG. 4), and the powdered oils and fats of Production Comparative Examples 5, 8 and 9. It is presumed that the composition has a plate-like shape and no flakes are present on the surface of the particles (FIGS. 5 to 7).
Further, as can be seen from Tables 10 and 13, the angle of repose relative value (86.9%, Table 13) of the powdered potato starch to which the powdered fat composition of Production Example 1 stored at 20 ° C. for 5 months (long-term storage) was added. ) Was almost the same as the relative value of the angle of repose before storage (86.3%, Table 10).
On the other hand, as can be seen from Table 11, the powdered fat and oil composition of Production Comparative Example 1 containing the α-type and β-type fats and oils before storage has a degree of aggregation of 60% or less, and is a powdered potato starch to which the powdered fat and oil composition is added. The relative value of the angle of repose was 90% or less (89.1%), but as can be seen from Table 13, the powdered oil / fat composition of Production Comparative Example 1 stored at 20 ° C. for 5 months (long-term storage) was added. The relative value of the angle of repose of the powdered potato starch was 97.6%, which was considerably larger than that before long-term storage. From this, it was judged that the powdered oil / fat composition of Production Comparative Example 1 had no commercial value because the relative value of the angle of repose changed significantly when stored for a long period of time and the quality was not stable.

Claims (6)

A powdered oil / fat composition containing an oil / fat component containing one or more XXX-type triglycerides having a fatty acid residue X having a carbon number x at the 1st to 3rd positions of glycerin, wherein the carbon number x is selected from 16 to 20. The powdered fat and oil composition contains β-type fat and oil, and the peak near 4.6 Å, which is characteristic of β-type, and 4.2 Å, which is characteristic of α-type, at the X-ray diffraction peak of the fat and oil component. The intensity ratio with the peak in the vicinity: [peak intensity in the vicinity of 4.6 Å / (peak intensity in the vicinity of 4.6 Å + peak intensity in the vicinity of 4.2 Å)] is 0.6 to 1, and the powdered oil / fat composition. The degree of aggregation is 60% or less, the loose bulk density of the powdered oil / fat composition is 0.05 to 0.6 g / cm ³ , and the relative rest angle value determined by the formula (I) is 90% or less. The powdered oil / fat composition is in the form of fragment-containing particles in which a plurality of flakes are present on the surface, and the powdered oil / fat composition is obtained by a production method including the following steps (a) to (c). A powdered oil / fat composition, which is characterized by being a fatty acid.
Relative value of repose = [angle of repose of the mixed powder of the powdered oil / fat composition and powdered starch] / [angle of repose of only the powdered starch not containing the powdered oil / fat composition] × 100 (I)
(In the formula (I), the "mixed powder" contains 1% by mass of the powdered oil / fat composition with respect to the total mass of the mixed powder.)
(A) Step of preparing a solid oil / fat composition raw material containing XXX-type triglyceride,
(B) The solid oil / fat composition raw material obtained in the step (a) is heated at a temperature below the melting point, and the oil / fat component in the solid oil / fat composition raw material is β-type without melting the oil / fat composition raw material. The process of converting to fats and oils to obtain a raw material for a β-type fat and oil-containing composition, and
(C) A step of pulverizing the β-type oil / fat-containing composition raw material obtained in step (b) by collision between the raw materials without mechanical pulverization to obtain a powdered oil / fat composition. The powdered fat or oil composition according to claim 1, wherein the powdered fat or oil composition contains 50% by mass or more of the XXX type triglyceride when the total mass of the powdered fat or oil composition is 100% by mass. The powdered oil / fat composition according to claim 2 , wherein the average particle size based on the volume average diameter of the particles is 0.5 to 200 μm. The powdered oil / fat composition according to claim 2 or 3 , wherein the average length of the long sides of the flakes is 0.1 to 5 μm. A food product comprising the powdered oil / fat composition according to any one of claims 1 to 4 . A powder fluidity improving agent comprising the powdered oil / fat composition according to any one of claims 1 to 4 .

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