Composite pigment and its manufacturing method

The composite pigment, produced via mechanochemical treatment, addresses skin pigmentation issues by enhancing bonding between substrate and pigment, reducing color bleeding and ensuring high coverage, thus minimizing skin pigmentation.

JP7800776B2Active Publication Date: 2026-01-16DIC CORP
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Patent Information

Application Number
JP2025523004
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2023-12-19
Filing Date
2024-11-28
Publication Date
2026-01-16
Estimated Expiration
2044-11-28

AI Technical Summary

Technical Problem

Existing composite pigments used in cosmetics often cause pigmentation on the skin due to bleeding of color components.

Method used

A composite pigment with a substrate coated by an organic pigment, produced through mechanochemical treatment, exhibits low bleeding and high coverage, characterized by specific absorbance and particle size distribution, ensuring strong bonding between the substrate and pigment.

Benefits of technology

The composite pigment effectively reduces skin pigmentation by minimizing color component bleeding, providing excellent pigmentation resistance and maintaining high coverage.

✦ Generated by Eureka AI based on patent content.

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Abstract

The composite pigment comprises a base material and a pigment covering a surface of the base material. The pigment contains an organic pigment, and, when 0.05 g of the composite pigment is dispersed in 20 mL of ethyl acetate and the precipitate is separated from the supernatant by allowing the resulting dispersion to stand for 24 hours, the absorbance of the supernatant at the maximum absorption wavelength is not more than 0.15.
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Description

[Technical Field]

[0001] The present disclosure relates to composite pigments and methods for making the same. [Background technology]

[0002] In the fields of cosmetics, inks, and paints, there has traditionally been a demand for materials that have good color development, luster, and brightness when applied. In particular, makeup cosmetics such as lipstick, eye shadow, blush, and nail polish are required to have uniform color development in order to enhance the finish obtained when applied to the skin. Against this background, composite pigments obtained by combining a base material (e.g., a luster material such as mica) with a pigment (e.g., an organic pigment) are used in the fields of cosmetics, inks, paints, etc.

[0003] For example, Patent Document 1 describes a flaky pigment having an average particle size of 5 to 60 μm, which is characterized by the formation of composite particles based on an ordered mixture by subjecting a mixture of a flaky substrate material consisting of flaky substrate particles with an aspect ratio of 10 to 120 and a pigment and / or dye consisting of particles with an average particle size of 5 μm or less to a high-speed stirring process without using a liquid medium.

[0004] In recent years, dry particle compositing apparatuses have come to be used as apparatuses for compositing a base material and a pigment.

[0005] For example, Patent Document 2 discloses a processing device that includes a rotating shaft having multiple stirring members attached to its outer periphery and a casing having an inner periphery positioned at a small gap from the stirring members, and that stirs and processes material inside the casing using the stirring members that move as the rotating shaft rotates, wherein, when viewed from a direction perpendicular to the axial direction of the rotating shaft, the end position of each of the multiple stirring members in a direction parallel to the axial direction of the rotating shaft is located more inside the end position of adjacent stirring members than the other stirring members; and a processing device that includes a rotating shaft having multiple stirring members attached to its outer periphery and a casing having an inner periphery positioned at a small gap from the stirring members, and that stirs and processes material inside the casing using the stirring members that move as the rotating shaft rotates, wherein the diameter of the inner periphery of the casing is less than twice the diameter of the outer periphery of the rotating shaft.

[0006] The device described in Patent Document 2 has, for example, the structure shown in Figures 1 to 3. With regard to the device having the structure shown in Figures 1 to 3, Patent Document 2 contains the following description.

[0007] This device is equipped with a rotating shaft 2 with multiple stirring members 3 attached to its outer periphery, located in the center of a cylindrical casing 1 enclosed in a jacket 4. The casing 1 has an inner periphery that is separated from the stirring members 3 by a small gap (clearance), and the stirring members 3 move as the rotating shaft 2 rotates, stirring the material inside the casing 1. The rotating shaft 2 is supported on one side by a bearing 7 and is connected to a drive unit 8 consisting of a motor or the like. The raw material inlet 5 is located on the side or top of the end of the casing 1, and the product outlet The inlet 6 is provided at the bottom of the casing 1, at the end opposite the powder inlet 5. In other words, the rotating shaft 2 is supported only at one axial end (left side in FIG. 1), and the casing 1 is formed in a bottomed cylindrical shape that is open only at one axial end (left side in FIG. 1) of the rotating shaft 2 and closed at the other axial end (right side in FIG. 1), and is configured to be movable along the axial direction of the rotating shaft 2 between an operating position (position in FIG. 1) that covers the processing space 9 between the rotating shaft 2 and the casing 1, and a non-operating position (not shown) that does not cover the processing space 9." (Paragraphs

[0039] and

[0040] )

[0008] "The outer periphery of the rotating shaft 2 is provided with plate-shaped stirring members 3a and 3b at an angle inclined relative to the axial direction, and the rotating shaft 2 is provided with diffusion members 10 on both end surfaces 2a." (Paragraph

[0043] )

[0009] "As shown in Figure 2, when the rotating shaft 2 of this device is viewed from a position perpendicular to the axial direction, the end position of agitating member 3b(2), for example, in a direction parallel to the axial direction of rotating shaft 2, is located inside the other adjacent agitating members 3a(1) and 3a(3) relative to the end positions of those other agitating members. In other words, if extension lines L1 and L3 are drawn vertically from the end of agitating member 3b(2), it will overlap with part of the adjacent agitating members 3a(1) and 3a(3). The same positional relationship applies to the other agitating members 3a(1), 3a(3), 3b(4), 3a(5), and 3b(6). When agitating members 3a and 3b are positioned in this way, the powder penetrates deep into the adjacent agitating members 3a and 3b from the ends of agitating members 3a and 3b, and as a result, the force of the agitating members can be strongly transmitted to the powder." (Paragraph

[0044] )

[0010] "As shown in Figure 3, in this device, the diameter D1 of the inner periphery of the casing 1 is less than twice the diameter D2 of the outer periphery of the rotating shaft 2. In other words, the relationship is D1 ≦ D2 × 2. Figure 3 shows an example in which D1 is 1.8 times D2. By making D2 relatively large compared to D1, the space (processing space) 9 in which force acts on the powder is limited, and as a result, even if the peripheral speed of the agitating members 3a, 3b is the same, the force of the agitating members 3a, 3b can be strongly transmitted to the powder. If D1 exceeds twice the value of D2, the space 9 in which force acts on the material to be processed becomes too large, and the force applied to the powder becomes weaker." (Paragraph

[0045] )

[0011] "At least some of the plurality of stirring members 3a, 3b are formed as feeding stirring members 3a that feed the material to be processed in one axial direction of the rotary shaft 2 as the rotary shaft 2 rotates, and another portion of the plurality of stirring members 3a, 3b are formed as returning stirring members 3b that return the material to be processed in the other axial direction of the rotary shaft 2 as the rotary shaft 2 rotates." (Paragraph

[0046] )

[0012] "As shown in FIG. 2, the plate surface of the feed stirring member 3a is inclined so as to feed the powder in the feed direction, i.e., in one direction along the axial direction of the rotating shaft 2 as the rotating shaft 2 rotates. When the raw material inlet 5 and the product outlet 6 are provided at both ends of the casing 1 (as in FIG. 1), the direction from the raw material inlet 5 to the powder outlet 6 (to the right in FIG. 2) is referred to as the feed direction. On the other hand, the plate surface of the return stirring member 3b is inclined so as to return the powder in the return direction, i.e., in the direction opposite to the feed direction along the axial direction of the rotating shaft 2 as the rotating shaft 2 rotates. When the raw material inlet 5 and the product outlet 6 are provided at both ends of the casing 1 (as in FIG. 1), the direction from the product outlet 6 toward the raw material inlet 5 (to the left in FIG. 2) is referred to as the return direction. The inclination angle of the stirring members 3a and 3b is preferably set within the range of ±5 to ±85 degrees with respect to the axial direction of the rotating shaft 2." (Paragraph

[0047] )

[0013] "The agitating members 3a and 3b are grouped together and spaced apart in the circumferential direction of the rotating shaft 2. The agitating members 3a and 3b in each group are distinguished by the (1), (2), (3), etc., added after 3a and 3b. In Figure 2, the agitating members 3a and 3b in the same group are inclined relative to the rotating shaft 2 so as to guide the powder in the same direction, i.e., either the forward direction or the return direction. However, this is not limited to this. Furthermore, in Figure 2, the agitating members 3a and 3b are grouped together and are spaced 180 degrees apart from each other on the rotating shaft 2. However, the agitating members 3a and 3b may be grouped together and consist of multiple members, such as three members spaced 120 degrees apart or four members spaced 90 degrees apart." (Paragraph

[0048] )

[0014] "One of the agitating members 3a, 3b adjacent in the circumferential direction of the rotating shaft 2 is formed on the feed agitating member 3a, and the other 3b is formed on the return agitating member 3b. Specifically, as shown in FIG. 3, one of the agitating members 3a(5), 3b(6) adjacent in the circumferential direction of the rotating shaft 2, 3a(5), is formed on the feed agitating member 3a, and the other 3b(6) is formed on the return agitating member 3b. It is desirable that each pair of agitating members 3a, 3b be offset by a certain angle from the other pair of agitating members 3a, 3b adjacent in the axial direction of the rotating shaft 2 when viewed from the axial direction. In FIG. 3, the agitating members are offset by an angle of 90 degrees, but this angle is not limiting." (Paragraph

[0049] )

[0015] "In Figure 2, there are six sets of feed stirring members 3a and return stirring members 3b, three of each arranged alternately in the axial direction of the rotating shaft 2. In this case, the powder is subjected to a force of "feed → return → feed → return → feed → return" alternately. Compared to when the powder is subjected to a force in only one direction, the path the powder travels within the casing is more complex and longer. As a result, the powder is subjected to an even stronger force from the stirring members 3a and 3b." (Paragraph

[0050] )

[0016] "In FIG. 2 (omitted)..., the inclination angles of the feed stirring members 3a (omitted)... and the return stirring members 3b (omitted)... are the same, but this is not limited to this. The inclination angles of the stirring members 3a, 3b may all be different, or only some of them may have different inclination angles." (Paragraph

[0051] )

[0017] "The agitating members 3a and 3b are formed in a plate shape. By making the agitating members 3a and 3b in a plate shape, the entire rotating shaft 2 can be made lighter than block-shaped agitating members, making it possible to design a rotating shaft 2 that rotates at a higher speed, and as a result, the force of the agitating members 3a and 3b can be transmitted to the powder more strongly. Note that "plate-shaped" means that at least the portions of the agitating members 3a and 3b close to the inner periphery of the casing 1 are plate-shaped, and the rotating shaft 2 and the agitating members 3a and 3b may be joined by rod-shaped arms or the like." (Paragraph

[0052] )

[0018] It is desirable to keep the gap (clearance) between the inner periphery of the casing 1 and the agitating members 3 constant and small. Keeping the clearance constant is to apply a uniform force to the powder, and keeping it small is to apply a stronger force by reducing the escape route for the powder. If simple rectangular plate-like members that are seen from the direction intersecting the axial direction are provided on the rotating shaft 2 as the agitating members 3a and 3b, the clearance between the center of the plate-like member and the inner periphery of the casing 1 will be wider than at both ends of the plate-like member, so it is desirable to consider the shape of the agitating members 3a and 3b on the inner periphery side of the casing 1 so as to keep the clearance constant. However, it is not necessary for the clearance between the inner periphery of the casing 1 and one set of agitating members 3 and the clearance between that inner periphery and another set of agitating members 3 to be the same. For example, in Figure 2, the clearance of the agitator 3a(1) at the feed base end near the raw material inlet 5 may be set wider than the clearance of the agitator 3a(5) at the feed end near the product outlet 6. Furthermore, the width of the clearance is preferably set to 0.05 to 7.5% of the diameter D1 of the inner periphery of the casing, more preferably 0.75 to 3%. If it exceeds 7.5%, the powder has a large escape route and it is not possible to apply a strong force. With a clearance of 0.05% or less, there is a risk that the agitators 3a and 3b may come into contact with the casing 1 due to vibrations that occur during operation. Specifically, it is desirable to set the gap between the inner periphery of the casing 1 and the agitators 3a and 3b in the range of 0.3 mm to 50 mm. (Paragraphs

[0053] and

[0054] )

[0019] "To ensure that the material to be treated is subjected to an effective agitation action within the casing 1, it is desirable to set the input volume of the material to be treated within the casing 1, relative to the internal volume of the treatment space 9 within the casing 1, between a lower limit of 5% and an upper limit of 95%. Here, the internal volume of the treatment space 9 within the casing 1 refers to the volume of the space obtained by subtracting the volume occupied by the rotating shaft 2 from the internal volume of the casing 1 itself (the actual space within the casing 1 in which the material to be treated can move around)." (Paragraph

[0055] )

[0020] "The action of the agitators 3a, 3b is less likely to reach both ends of the rotating shaft 2. Therefore, by providing the feed agitator 3a at one end of the rotating shaft 2 and the return agitator 3b at the other end, the movement of powder toward both ends of the rotating shaft 2 is suppressed, and as a result, it is possible to prevent powder from being discharged without being subjected to the strong agitation action of the agitator 3. In other words, the agitator 3a(1) located at one axial end of the rotating shaft 2 (the left end of Figure 2 (omitted)) is formed as the feed agitator 3a that sends the material to be processed from that one axial end to the other end (the right end of Figure 2 (omitted)). The agitators 3b(5), 3b(6) located at the other axial end of the rotating shaft 2 (the right end of Figure 2 (omitted)) are formed as return agitators 3b that return the material to one end from the other axial end." (Paragraph

[0057] )

[0021] "Actually, the agitating members 3a and 3b... (omitted)... The tip portions of the agitating members 3a and 3b that face the inner periphery of the casing 1 are formed in an acute-angled cross section when viewed from the axial direction of the rotating shaft 2, and the center line L of the acute tip portion is inclined from a perpendicular direction to the inner periphery of the casing 1.... (omitted)... The angle of the acute tip portion is not limited to 60 degrees, but can be set to any angle from close to 90 degrees to less than 60 degrees. However, considering wear of the tip portion, an angle that is too small is not preferable. The inclination angle of the center line L can also be set to an appropriate value." (Paragraph

[0058] )

[0022] "Diffusion members 10 are provided on both end face portions 2a of the rotating shaft 2. As the diffusion members 10 move with the rotation of the rotating shaft 2, centrifugal force is generated by the diffusion members 10 against powder that attempts to enter the both end face portions 2a, which are difficult to reach with the action of the agitating members 3, and the movement of powder to the both end face portions 2a is suppressed. As a result, it is possible to prevent the occurrence of powder that is discharged without being subjected to the strong agitation action of the agitating members 3. As shown in FIG. 3, the diffusion members 10 extend in opposite directions from the center of the rotating shaft 2 at each end face portion 2a. The diffusion member 10 is made up of two plate-like members. As shown by the solid and dashed lines, the agitating members 10 on both end face portions 2a are arranged at 90 degrees offset from each other when viewed in the axial direction of the rotating shaft 2. However, this is not limiting, and other shapes, angles, and numbers of members may be used as long as they are able to generate centrifugal force, and the diffusion member may be provided so as to cross the center of the rotating shaft 2 when viewed in the axial direction of the rotating shaft 2. Furthermore, the diffusion member 10 may be provided on only one end face portion 2a of the rotating shaft 2, but it is preferable to provide it on both end face portions 2a. (Paragraph

[0060] ) [Prior art documents] [Patent documents]

[0023] [Patent Document 1] Japanese Patent Application Publication No. 05-214257 [Patent Document 2] Japanese Patent Application Laid-Open No. 2005-270955 Summary of the Invention [Problem to be solved by the invention]

[0024] One of the skin problems commonly caused by cosmetics is pigmentation on the skin. However, composite pigments, which have a base material coated with an organic pigment, have the problem of causing pigmentation on the skin when used in cosmetics.

[0025] Therefore, some aspects of the present disclosure aim to provide a composite pigment that is less likely to cause pigmentation on the skin when used as a cosmetic, and a method for producing the same. [Means for solving the problem]

[0026] The inventors of the present disclosure have discovered that the above problems can be solved by using a composite pigment having specific bleeding performance, and have arrived at the present disclosure.

[0027] Some aspects of the present disclosure provide the following [1] to [7].

[0028] [1] A composite pigment comprising a substrate and a pigment covering a surface of the substrate, The pigment includes an organic pigment, A composite pigment, wherein 0.05 g of the composite pigment is dispersed in 20 mL of ethyl acetate, and the resulting dispersion is allowed to stand for 24 hours to separate into a precipitate and a supernatant, and the absorbance of the supernatant at the maximum absorption wavelength is 0.15 or less.

[0029] [2] The composite pigment according to [1], having a strong coverage of 80% or more.

[0030] [3] The composite pigment according to [1] or [2], wherein the base material and the pigment are combined by a mechanochemical treatment.

[0031] [4] The composite pigment according to any one of [1] to [3], wherein the substrate is a flaky substrate containing at least one selected from the group consisting of mica, aluminum, alumina, and glass.

[0032] [5] The substrate comprises a core and a shell covering the surface of the core, The composite pigment according to any one of [1] to [4], wherein the shell contains at least one selected from the group consisting of a resin, a metal, and a metal oxide.

[0033] [6] A method for producing a composite pigment comprising a substrate and a pigment covering a surface of the substrate, a coating step of coating a surface of the base material with the pigment by compounding the base material with the pigment including an organic pigment using a dry particle compounding device; A method for producing a composite pigment, wherein P1 is the load power amount consumed by the dry particle composite device in the coating step, P2 is the load power amount consumed by the dry particle composite device when the coating step is carried out in a state where the raw materials are excluded, and m is the mass of the raw materials used in the coating step, and (P1-P2) / m is 0.2 to 0.5 W·h / g.

[0034] [7] [6] The method for producing a composite pigment according to [6], wherein, in a volume-based particle size distribution of the pigment measured by a wet laser diffraction / scattering method, when the particle sizes at which the integrated values ​​from small particle sizes reach 10% and 90% of the total are defined as D10 and D90, respectively, D90-D10 is 300 μm or less. [Effects of the Invention]

[0035] According to the present disclosure, it is possible to provide a composite pigment that is less likely to cause pigmentation on the skin when used as a cosmetic, and a method for producing the same. [Brief explanation of the drawings]

[0036] [Figure 1] FIG. 1 is a partial cross-sectional front view showing the structure of a processing apparatus according to the invention described in Patent Document 2. [Figure 2] 2 is a diagram showing a rotating shaft and a stirring member in the processing apparatus of FIG. 1. FIG. [Figure 3] FIG. 1 is a side cross-sectional view showing the structure of a processing apparatus according to the invention described in Patent Document 2. DETAILED DESCRIPTION OF THE INVENTION

[0037] In this specification, a numerical range indicated using "to" indicates a range that includes the numerical values ​​before and after "to" as the minimum and maximum values, respectively. Furthermore, unless specifically stated otherwise, the units of the numerical values ​​before and after "to" are the same. Furthermore, in the numerical ranges described in this specification, the upper or lower limit of the numerical range may be replaced with a value shown in the examples. Furthermore, the upper and lower limit values ​​described individually can be combined arbitrarily. Furthermore, "A or B" may include either A or B, or may include both.

[0038] Hereinafter, exemplary embodiments of the present disclosure will be described, but the present disclosure is not limited to the following embodiments.

[0039] <Composite pigment> One embodiment of the present disclosure is a composite pigment including a substrate and a pigment (hereinafter also referred to as a "coated pigment") coating the surface of the substrate, wherein the coated pigment contains an organic pigment, and when 0.05 g of the composite pigment is dispersed in 20 mL of ethyl acetate and the resulting dispersion is allowed to stand for 24 hours to separate into a precipitate and a supernatant, the supernatant has an absorbance at the maximum absorption wavelength (hereinafter referred to as "absorbance A") of 0.15 or less.

[0040] A composite pigment having the above characteristics is less likely to cause pigmentation on the skin when used as a cosmetic. In other words, a composite pigment having the above characteristics can be said to have excellent pigmentation resistance. Therefore, the composite pigment is suitable for use as a pigment for cosmetics. The pigmentation resistance of a composite pigment can be evaluated by the following method.

[0041] Apply composite pigment (approximately 50 mg) to a 5 mm x 5 mm section of a 100 x 100 mm urethane No. 132 series (No. 132#W, Viewlux) Bioskin Plate and spread it with your fingers. Lightly blow off excess pigment with air, then apply an appropriate amount (approximately 0.1 g) of cleansing oil (e.g., Deve OLIVE & ARGAN, Viewer Products Co., Ltd.) to the pigmented area. Rub the pigmented area with your fingers for 2 seconds, wipe off the oil with a Kimwipe, and wipe the pigmented area. After wiping, measure the color of the pigmented area using a colorimeter (e.g., eXact Advanced (x-rite)) (illuminant: D50, standard observer: 2°). The smaller the C* value of the obtained colorimetric data, the better the stainless and pigmentation resistance.

[0042] The C* value of the composite pigment measured by the above method is, for example, 3.0 or less, and can be as low as about 0.0. That is, the C* value of the composite pigment measured by the above method can be, for example, 0.0 to 3.0 or 0.9 to 3.0.

[0043] The reason why the above effect is obtained is not clear, but is presumed as follows. First, one possible cause of pigmentation on the skin when a composite pigment is used as a cosmetic is the bleeding phenomenon, in which color components (organic pigments, etc.) bleed out from the composite pigment. In contrast, the absorbance A indirectly indicates the amount of color components (organic pigments, etc.) that bleed from the composite pigment into the dispersion. The lower the absorbance A, the less likely the composite pigment is to bleed, and the better its bleeding resistance. In this regard, since the absorbance A of the composite pigment is 0.15 or less, it is presumed that the pigment has good bleeding resistance and, as a result, is less likely to cause pigmentation on the skin when used as a cosmetic.

[0044] The absorbance A can be measured using a spectrophotometer (for example, Hitachi's U-3900). From the viewpoint of enhancing the above-mentioned effects, the absorbance A may be 0.10 or less, 0.06 or less, or 0.03 or less. The lower limit of the absorbance A is not particularly limited, but may be 0.00 or 0.01. That is, the absorbance A may be, for example, 0.00 to 0.15, 0.01 to 0.10, 0.01 to 0.06, or 0.01 to 0.03.

[0045] The composite pigment may be a so-called core-shell particle. That is, the composite pigment may have a core made of a mother particle and a shell made of a child particle. In the composite pigment, the substrate may form the core as the mother particle, and the coated pigment may form the shell as the child particle.

[0046] In the composite pigment, the substrate and the coated pigment may be composited by mechanochemical treatment. Here, mechanochemical treatment refers to a treatment that can induce a mechanochemical phenomenon between the substrate and the coated pigment. For example, a treatment using a dry particle composite device is a mechanochemical treatment. Mechanochemical phenomena are caused by mechanical energy (e.g., compression, shear, impact, etc.), and include chemical reactions (mechanochemical reactions) such as the formation and rupture of chemical bonds, and activation (mechanical activation) caused by particle refinement or changes in crystal structure.

[0047] When the substrate and the coated pigment are composited by mechanochemical treatment, the coated pigment is physically fixed and pressed onto the surface of the substrate by a mechanochemical phenomenon, and the substrate and the coated pigment are more strongly bonded than when the coated pigment is simply attached to the substrate. Therefore, with such a composite pigment, bleeding of the color component is less likely to occur, and pigmentation on the skin can be further suppressed when used as a cosmetic.

[0048] The composite pigment may have a strong coverage of 80% or more, or may have a strong coverage of 87% or more. The higher the strong coverage of the composite pigment, the less likely the pigment components are to bleed, and the more effectively pigmentation on the skin can be suppressed when used as a cosmetic. The upper limit of the strong coverage of the composite pigment is not particularly limited, but may be, for example, 95%. That is, the strong coverage of the composite pigment may be, for example, 80 to 95% or 87 to 95%. Here, the strong coverage indicates the proportion of the coated pigment in the composite pigment that is strongly adhered to the substrate. It can be said that the higher the strong coverage, the more the coated pigment is strongly bonded to the substrate.

[0049] The strong coverage can be calculated based on the following formula (a) by measuring the absorbance A1 and the absorbance A2 according to the following conditions 1 and 2. Formula (a): Strong coverage [unit: %]=(1-[absorbance A1] / [absorbance A2])×100

[0050] [Condition 1] After weighing 0.05 g of composite pigment into a 30 mL vial, add 20 mL of a 5% aqueous ethanol solution. The vial is then shaken for 1 minute using a paint conditioner (Toyo Seiki) to disperse the liquid in the vial. After allowing the vial to stand, 1 mL of the resulting supernatant is sampled and diluted with 9 mL of dilution solvent to obtain a diluted solution. The absorbance of the diluted solution is measured using a spectrophotometer (e.g., Hitachi U-3900) to determine the absorbance at the maximum absorption wavelength (absorbance A1).

[0051] [Condition 2] Weigh 0.05 g of composite pigment into a 30 mL vial and add 20 mL of dilution solvent. The vial is then shaken for 1 minute in a paint conditioner (Toyo Seiki) to disperse the liquid. The vial is then allowed to stand, after which 1 mL of the resulting supernatant is sampled and diluted with 9 mL of dilution solvent to obtain a diluted solution. The absorbance of the diluted solution is measured using a spectrophotometer (e.g., Hitachi U-3900) to determine the absorbance at the maximum absorption wavelength (absorbance A2).

[0052] The dilution solvent used in conditions 1 and 2 is a solvent capable of completely dissolving 0.005 g of organic pigment in a volume of 20 mL. Here, "complete dissolution" refers to the amount of residue remaining after adding 20 mL of solvent to 0.005 g of the organic pigment and thoroughly stirring the resulting mixture through a 0.45 μm pore size membrane filter (e.g., DISMIC-13HP, Advantec Toyo Co., Ltd.). Examples of dilution solvents that can be used include those listed in the "Quantitative Methods" section of the "Legal Colorant Handbook, Revised Edition, compiled by the Japan Cosmetic Industry Association" for the organic pigments contained in coated pigments. When the organic pigment contained in the coated pigment is Red No. 202, dilute acidic ethanol can be used. When the organic pigment contained in the coated pigment is Red No. 104 Aluminum Lake, dilute sodium hydroxide TS can be used. When the organic pigment contained in the coated pigment is Blue No. 1 Aluminum Lake, dilute sodium hydroxide TS can be used.

[0053] The maximum absorption wavelength under conditions 1 and 2 is the maximum absorption wavelength of the organic pigment corresponding to the dilution solvent. If the organic pigment contained in the coated pigment consists of only one type listed in the "Legal Colorant Handbook, Revised Edition, compiled by the Japan Cosmetic Industry Association," the maximum absorption wavelength under conditions 1 and 2 will be the maximum absorption wavelength listed for that organic pigment in the "Quantitative Method" section of the handbook. For example, if the organic pigment contained in the coated pigment is only Red No. 202, the maximum absorption wavelength will be 521 nm; if the organic pigment contained in the coated pigment is only Red No. 104 Aluminum Lake, the maximum absorption wavelength will be 538 nm; and if the organic pigment contained in the coated pigment is only Blue No. 1 Aluminum Lake, the maximum absorption wavelength will be 630 nm.

[0054] When the covering pigment contains multiple organic pigments, the strong coverage rate is determined for each organic pigment, and the lowest strong coverage rate is taken as the strong coverage rate of the composite pigment. For example, when the covering pigment contains two organic pigments (organic pigments A and B), first, dilution solvents for organic pigments A and B are selected. Next, absorbances A1 and A2 are measured using the dilution solvent for organic pigment A as the dilution solvent under conditions 1 and 2, and the strong coverage rate for organic pigment A is determined. Similarly, absorbances A1 and A2 are measured using the dilution solvent for organic pigment B as the dilution solvent under conditions 1 and 2, and the strong coverage rate for organic pigment B is determined. The lower of the strong coverage rates determined in this way is taken as the strong coverage rate of the composite pigment.

[0055] Next, the constituent materials of the composite pigment will be described.

[0056] (base material) The substrate is, for example, an inorganic substrate made of an inorganic material. The inorganic substrate may be made of at least one metal or metal oxide. Examples of metals include silicon (Si), iron (Fe), aluminum (Al), sodium (Na), calcium (Ca), magnesium (Mg), potassium (K), copper (Cu), manganese (Mn), titanium (Ti), silver (Ag), gold (Au), platinum (Pt), lead (Pb), chromium (Cr), tin (Sn), molybdenum (Mo), gallium (Ga), and indium (In). Examples of metal oxides include oxides of these metals. The substrate may also contain an organic material as long as it does not impair the effects of the present disclosure.

[0057] The substrate may be, for example, a particle. The shape of the substrate is not particularly limited, but may be flaky (flake-like) from the viewpoint of easily bonding to the coated pigment. Examples of flaky substrates include mica, aluminum, alumina, glass, titanium dioxide, red iron oxide, iron oxide, yellow iron oxide, black iron oxide, zinc oxide, Prussian blue, ultramarine, chromium oxide, kaolin, clay, bentonite, bismuth oxychloride, zirconium oxide, and magnesium oxide. These substrates may be used alone or in combination of two or more. Among the above, at least one selected from the group consisting of mica, aluminum, alumina, and glass may be used from the viewpoint of enhancing the radiance desired in cosmetics.

[0058] Examples of mica include natural mica, synthetic mica, synthetic phlogopite, titanium mica, synthetic titanium mica, iron oxide-coated mica, iron oxide-coated synthetic mica, chromium hydroxide mica, etc. Commercially available products that can be used include SunMICA (trademark, manufactured by SunChemical) and IRIODIN (registered trademark, manufactured by Merck).

[0059] Examples of aluminum (Al) include aluminum itself, as well as aluminum hydroxide, aluminum chloride, aluminum nitride, aluminum phosphate, aluminum sulfate, etc. Commercially available products that can be used include Hydrolan (registered trademark, manufactured by Eckart Co., Ltd.).

[0060] The glass may be silicate glass containing silicon dioxide (SiO2) as a main component. Examples of glass include soda-lime glass, lead glass, soda-lime glass, A-glass, C-glass, E-glass, borosilicate glass, and aluminosilicate glass. Commercially available products that can be used include Glass Flake, Metashine, and Lumigran (all registered trademarks, manufactured by Nippon Sheet Glass Co., Ltd.).

[0061] The substrate may be a core-shell particle comprising a core (mother particle) and a shell (coating layer) covering the surface of the core. The core may be composed of the materials described above. The core may be, for example, flaky. From the viewpoint of enhancing the radiance desired in cosmetics, the flaky core may contain at least one selected from the group consisting of mica, aluminum, alumina, and glass. The shell may contain at least one component selected from the group consisting of resin, metal, and metal oxide. From the viewpoint of further enhancing the radiance desired in cosmetics, the substrate may comprise a flaky core and a shell covering the surface of the core and containing at least one selected from the group consisting of resin, metal, and metal oxide.

[0062] Examples of the resin include acrylic resin, urethane resin, styrene resin, ether resin, epoxy resin, etc. Examples of the metal and metal oxide include the same metals and metal oxides as those described above.

[0063] The core and shell may be composed of different materials from the viewpoint of enhancing the brilliance desired in cosmetics. In particular, from the viewpoint of further enhancing the brilliance desired in cosmetics, the core may contain mica and the shell may contain titanium oxide. An example of a substrate having such a configuration is a pearl pigment. The hue of the pearl pigment is not particularly limited.

[0064] The size of the substrate may be larger than that of the coated pigment (single particle). The average particle diameter of the substrate may be 1 to 80 μm, 5 to 50 μm, or 10 to 45 μm, from the viewpoint of the efficiency of treating the substrate with the coated pigment during composite pigment production. Here, the average particle diameter of the substrate refers to the particle diameter (median diameter D50) at which the cumulative value from the smallest particle size reaches 50% of the total in the volume-based particle size distribution of the substrate measured by wet laser diffraction / scattering. The average particle diameter is measured, for example, using a particle size distribution analyzer MT3000II (Microtrack Bell Corporation).

[0065] When the substrate is flaky, the thickness of the substrate is, for example, 0.1 to 5 μm, and may be 0.2 to 3 μm. The length of the flaky substrate in the long side direction is, for example, 3 to 100 μm, and may be 5 to 50 μm. The average aspect ratio (length / thickness) of the flaky substrate is, for example, 10 to 200, and may be 20 to 150. When the size and average aspect ratio of the flaky substrate are within the above ranges, when the composite pigment is used in cosmetics, the applied cosmetic product tends to feel smooth to the touch, spread well during application, and also tend to have good color development and luster.

[0066] The content of the base material may be 20 to 98% by mass, or 30 to 95% by mass, based on the total amount of the composite pigment. When the content of the base material is within the above range, when the composite pigment is used in a cosmetic, the applied cosmetic tends to have a smooth feel, good spreadability upon application, and good color development and luster.

[0067] The ratio of the content of the substrate to the content of the coated pigment (substrate / pigment), in mass ratio, may be 0.3 to 20, or may be 0.5 to 15, or 1 to 10. When the ratio (substrate / pigment) is within the above range, when the composite pigment is used in a cosmetic, the applied cosmetic tends to feel smooth to the touch, spreads well during application, and also tends to have good color development and luster.

[0068] (coated pigment) The coated pigment coats the surface of the substrate. The coated pigment may coat at least a part of the surface of the substrate, but may also completely coat the entire surface of the substrate.

[0069] The coated pigment contains at least one organic pigment. Organic pigments are broadly classified into synthetic organic pigments and natural organic pigments. The coated pigment may contain only one of synthetic organic pigments and natural organic pigments, or may contain both. It may contain multiple organic pigments depending on the desired hue. Because the coated pigment contains an organic pigment, it is easy to obtain high coloring strength and vivid colors.

[0070] Examples of synthetic organic pigments include azo-based, phthalocyanine-based, anthraquinone-based, perylene-based, perinone-based, quinacridone-based, thioindigo-based, dioxazine-based, isoindolinone-based, quinophthalone-based, azomethine-based, diketopyrrolopyrrole-based, and isoindoline-based synthetic organic pigments.

[0071] Specific examples of synthetic organic pigments include Red No. 3, Red No. 104, Red No. 106, Red No. 201, Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 223, Red No. 226, Red No. 227, Red No. 228, Red No. 230, Red No. 401, Red No. 405, Red No. 505, Orange No. 203, Orange No. 204, Orange No. 205, Yellow No. 4, Yellow No. 5, Yellow 401, Blue No. 1, Blue No. 404, and CI Pigment Red 1, 2, 3, 4, 5, 6, 7, 8, 9, 12, 14, 15, 16, 17, 21, 22, 23, 31, 32, 37, 38, 41, 47, 48, 48:1, 48:2, 48:3, 48:4, 49, 49:1, 49:2, 50:1, 52:1, 52:2, 53, 53:1, 53:2, 53:3, 57, 57:1, 57:2, 58:4, 60, 63, 63:1 , 63:2, 64, 64:1, 68, 69, 81, 81:1, 81:2, 81:3, 81:4, 83, 88, 90:1, 101, 101:1, 104, 108, 108:1, 109, 112, 113, 114, 122, 123, 144, 146, 147, 149, 151, 166, 168, 169, 170, 172, 173, 174, 175, 176 , 177, 178, 179, 181, 184, 185, 187, 188, 190, 193, 194, 200, 202, 206, 207, 208, 209, 210, 214, 216, 220, 221, 224, 230, 231, 232, 233, 235, 236, 237, 238, 239, 242, 243, 245, 247, 249, 250, 251, 253, 254, 255, 256, 257, 258, 259, 260, 262, 263, 264, 265, 266, 267, 268, 269, 270, 271, 272, 27 3, 274, 275, 276, 277, 278, 279, 280, 281, 282, 283, 284, 285, 286, 287, 291, 295, 296, CIPigment Blue 1, 1:2, 9, 14, 15, 15:1, 15:2, 15:3, 15:4, 15:6, 16, 17, 19, 25, 27, 28, 29, 33, 3 5, 36, 56, 56:1, 60, 61, 61:1, 62, 63, 66, 67, 68, 71, 72, 73, 74, 75, 76, 78, 79, CIPigment Yellow 1, 2, 3, 4, 5, 10, 12, 13, 14, 15, 16, 17, 18, 24, 31, 32, 34, 35, 35:1, 36, 36:1, 37, 37:1, 40, 42, 43, 53, 55, 60, 61, 62 , 63, 65, 73, 74, 77, 81, 83, 93, 94, 95, 97, 98, 100, 101, 104, 106, 108, 109, 110, 113, 114, 115, 116, 117, 118, 119, 1 20, 123, 126, 127, 128, 129, 139, 147, 150, 151, 152, 153, 154, 155, 156, 161, 162, 164, 166, 167, 168, 169, 170, 171 , 172, 173, 174, 175, 176, 177, 179, 180, 181, 182, 185, 187, 188, 192, 193, 194, 196, 198, 199, 213, 214, CIPigment Examples of synthetic organic pigments include Violet 1, 1:1, 2, 2:2, 3, 3:1, 3:3, 5, 5:1, 14, 15, 16, 19, 23, 25, 27, 29, 31, 32, 37, 39, 42, 44, 47, 49, and 50; and CI Pigment Green 1, 2, 4, 7, 8, 10, 13, 14, 15, 17, 18, 19, 26, 36, 37, 45, 48, 50, 51, 54, 55, 58, and 59. Tar dyes other than those listed above can also be used as synthetic organic pigments. These synthetic organic pigments can be used alone or in combinations of two or more depending on the desired hue.

[0072] Examples of natural organic pigments (natural colorants) include carotenoid-based, anthocyanin-based, flavonoid-based, quinone-based, porphyrin-based, diketone-based, betacyanin-based, and azaphilone-based natural organic pigments.

[0073] Specific examples of natural organic pigments include β-carotene, norbixin, bixin, capsanthin, lutein, lycopene, crocin, crocetin, astaxanthin, cyanidin acylglucoside, cyanidin, peonidin aglycone, anidine glucoside, delphinidin glucoside, anthocyanin, shisonin, malonylshisonin, pelargonidin acylglucoside, cocoa polyphenols, apigeninidin, luteolinidin, polymerized proanthocyanidin, saflomin, carthamin, carminic acid, laccaic acid, chlorophyll, phycocyanin, curcumin, betanin, isobetanin, ankaflavin, monascorubrin, iridoid glycosides, ester hydrolysates of iridoid glycosides, and eumelanin. These natural organic pigments may be used alone or in combination depending on the desired hue.

[0074] The organic pigment may be a lake pigment insolubilized with a metal ion, such as aluminum lake, calcium lake, or barium lake.

[0075] The coated pigment may contain components other than the organic pigment, such as an extender pigment.

[0076] The content of the organic pigment in the coated pigment may be 5% by mass or more, 10% by mass or more, 20% by mass or more, 40% by mass or more, or 60% by mass or more, based on the total amount of the coated pigment, from the viewpoint of achieving both saturation and smoothness when the composite pigment is formed. The content of the organic pigment in the coated pigment may be 100% by mass or less, 80% by mass or less, or 60% by mass or less, based on the total amount of the coated pigment, from the viewpoint of easily maintaining the brilliance of the base material. From these viewpoints, the content of the organic pigment in the coated pigment may be, for example, 5 to 100% by mass, 5 to 80% by mass, 10 to 80% by mass, 20 to 80% by mass, 40 to 60% by mass, or 60 to 100% by mass, based on the total amount of the coated pigment. The content of the organic pigment can be determined, for example, by quantitative analysis using high-performance liquid chromatography. Specifically, a calibration curve is prepared using a standard sample of the organic pigment, and the content is calculated based on the calibration curve.

[0077] In the volumetric particle size distribution of the coated pigment measured by wet laser diffraction / scattering, the particle sizes at which the cumulative values ​​from the smallest particle sizes reach 10% and 90% of the total are defined as D10 and D90, respectively. The difference between these (D90 - D10) may be 300 μm or less (0 to 300 μm). The smaller the difference (D90 - D10), the less variation there is in the particle size of the coated pigment. When D90 - D10 is 300 μm or less, when the composite pigment is used in cosmetics, the applied cosmetic product tends to feel smooth to the touch, spread well upon application, and also tend to have good color development and luster. From the same perspective, the difference (D90 - D10) may be 100 μm or less, 10 μm or less, or 5 μm or less. The difference (D90 - D10) may be 0 μm or more, 3 μm or more, 3.5 μm or more, or 4 μm or more, or may be 0 to 300 μm, 3 to 300 μm, 3.5 to 100 μm, 4 to 10 μm, or 0 to 5 μm. D10 and D90 are measured, for example, using a particle size distribution analyzer MT3000II (Microtrac BEL Corporation).

[0078] The content of the coated pigment may be 1 to 50 parts by mass or 5 to 20 parts by mass relative to 100 parts by mass of the base material, from the viewpoint of achieving both the design properties of the base material and the saturation when made into a composite pigment.

[0079] (Other ingredients) The composite pigment may contain, in addition to the substrate and the coated pigment, inorganic powder or organic powder as other components.

[0080] Examples of inorganic powders include zirconium oxide, zinc oxide, cerium oxide, magnesium oxide, barium sulfate, calcium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate, talc, sericite, silicic acid, silicic acid anhydride, aluminum silicate, magnesium silicate, aluminum magnesium silicate, calcium silicate, barium silicate, strontium silicate, metal tungstate, hydroxyapatite, vermiculite, higilite, bentonite, montmorillonite, hectorite, zeolite, ceramic powder, dibasic calcium phosphate, alumina, aluminum hydroxide, boron nitride, and silica.

[0081] Examples of organic powders include polyamide powder, polyester powder, polyethylene powder, polypropylene powder, polystyrene powder, polyurethane powder, benzoguanamine powder, polymethylbenzoguanamine powder, tetrafluoroethylene powder, polymethyl methacrylate powder, cellulose powder, silk powder, nylon powder (12 nylon, 6 nylon), styrene-acrylic acid copolymer powder, divinylbenzene-styrene copolymer powder, vinyl resin powder, urea resin powder, phenolic resin powder, fluororesin powder, silicon resin powder, acrylic resin powder, melamine resin powder, epoxy resin powder, polycarbonate resin powder, microcrystalline fiber powder, rice starch, and lauroyl lysine.

[0082] When an organic powder and an inorganic powder are used, the content of the organic powder and the content of the inorganic powder may be 0.1 to 10% by mass, or 0.5 to 5% by mass, respectively, relative to the total amount of the composite pigment. The total content of the organic powder and the inorganic powder may be within the above range.

[0083] The composite pigment may contain an oily base as another component for the purpose of stabilizing the dispersion of the coated pigment. Examples of such an oily base include waxes that are solid at room temperature (25°C) and liquid oily components that are liquid.

[0084] Examples of the waxes include vegetable waxes such as candelilla wax, carnauba wax, rice wax, Japan wax, and sunflower wax; animal waxes such as beeswax; mineral waxes such as ozokerite, ceresin, and microcrystalline wax; petroleum waxes such as solid paraffin; and synthetic waxes such as silicone wax and synthetic beeswax.

[0085] Examples of the liquid oily component include vegetable oils such as olive oil, castor oil, jojoba oil, macadamia nut oil, crab rose fruit oil, cocoa butter, rose oil, and lanolin; animal oils such as horse oil, turtle oil, wild boar oil, mink oil, and shark oil; hydrocarbon oils such as petrolatum, liquid paraffin, isodecane, isododecane, octyldodecyl, diisostearyl malate, and hydrogenated polyisobutene; isotridecyl isononanoate, isopropyl isostearate, neopentyl glycol dicaprate, isotridecyl isononanoate, and diisostearic acid Examples of suitable oils include ester oils such as glyceryl, glyceryl triisostearate, diisostearyl malate, octyldodecanol, and di(phytosteryl / 2-octyldodecyl) N-lauroyl-L-glutamate; silicone oils such as dimethylpolysiloxane and phenylmethylpolysiloxane; dimer acid esters, dimer diol derivatives, cholesterol fatty acid esters, phytosterol fatty acid esters, polyglycerin fatty acid esters, pentaerythritol fatty acid esters, and glyceryl tri-2-ethylhexanoate.

[0086] The total content of the waxes and the liquid oil component in the composite pigment may be 0.1 to 10% by mass, or may be 0.5 to 5% by mass, based on the total amount of the composite pigment.

[0087] The composite pigment described above can be used in cosmetics as well as inks, paints, toners, materials for forming molded articles, and the like.

[0088] <Method of manufacturing composite pigments> Another embodiment of the present disclosure is a method for producing a composite pigment including a substrate and a pigment coating the surface of the substrate, the method including a coating step of coating the surface of the substrate with the coating pigment by using a dry particle compositing device to composite the substrate and a pigment including an organic pigment (hereinafter referred to as a "coating pigment"). Where P1 is the load power consumed by the dry particle compositing device in the coating step, P2 is the load power consumed by the dry particle compositing device when the coating step is performed without the raw materials, and m is the mass (charge amount) of the raw materials used in the coating step, (P1-P2) / m is 0.2 to 0.5 W·h / g.

[0089] Here, "raw material" refers to the materials used to produce the composite particles, specifically a mixture of the substrate, coating pigment, and other optional components. The details of the substrate, coating pigment, and other components are the same as those of the substrate, coating pigment, and other components described above for the composite pigment. For example, in the volume-based particle size distribution of the coating pigment measured by wet laser diffraction / scattering, if the particle sizes at which the integrated values ​​from small particle sizes reach 10% and 90% of the total are defined as D10 and D90, respectively, the difference between these (D90 - D10) may be 300 μm or less, 100 μm or less, 10 μm or less, or 5 μm or less; or 3 μm or more, 3.5 μm or more, or 4 μm or more; or may be 0 to 300 μm, 3 to 300 μm, 3.5 to 100 μm, 4 to 10 μm, or 0 to 5 μm.

[0090] In the above production method, (P1-P2) / m means the load power amount applied per 1 g of raw material in the coating process. A dry particle compositing device requires load power even during idle operation, but the load power amount P2 consumed during idle operation is measured in advance, and the load power amount consumed to composite the base material and coating pigment can be determined by subtracting P2 from the load power amount P1 consumed in the coating process.

[0091] Organic pigments tend to have poorer bleeding resistance than inorganic pigments. However, with the above-described production method, (P1-P2) / m is 0.2 to 0.5 W·h / g, and therefore the base material and the coating pigment are successfully combined. As a result, a composite pigment with excellent bleeding resistance can be obtained. Specifically, for example, a composite pigment having an absorbance A of 0.15 or less in the above-described embodiment can be obtained. Therefore, it can be said that the above-described production method can produce a composite pigment that is less likely to cause pigmentation on the skin when used in cosmetics.

[0092] (Coating process) In the coating process, the raw materials are loaded into a dry particle compositing device and processed in the device to composite the substrate and the coating pigment. The order in which the raw materials are loaded is not particularly limited. For example, the substrate and the coating pigment may be loaded into the dry particle compositing device sequentially or simultaneously. When the substrate and the coating pigment are mixed in advance to prepare a premix and then the premix is ​​loaded into the dry particle compositing device, higher raw material mixability is likely to be achieved.

[0093] The amounts of raw materials charged in the coating step may be such that the content of each constituent material in the resulting composite pigment falls within the ranges indicated for the content of each constituent material in the composite pigment of the above embodiment. Specifically, for example, the amount of the coating pigment charged may be 1 to 50 parts by mass or 5 to 20 parts by mass per 100 parts by mass of the base material.

[0094] The dry-type composite device used in the coating step may be the device described in the above-mentioned Patent Document 2 (for example, the device described with reference to FIGS. 1 to 3). Specific examples of such devices include the Nobilta / NOB type manufactured by Hosokawa Micron Corporation ("Nobilta" is a registered trademark) and the "Hybridization System NHS-O type" manufactured by Nara Machinery Works, Ltd.

[0095] The dry-type compounding device includes a rotor that is made up of, for example, the rotating shaft of the device described in Patent Document 2 and an agitating blade as an agitating member. The rotor is, for example, cylindrical.

[0096] The diameter (φ) of the rotating part may be 80 mm or more (e.g., 80 to 300 mm), or may be 100 to 150 mm. Here, the diameter (φ) of the rotating part refers to the length of a line segment that connects the end of one agitator to the end of the other agitator on the opposite side of the agitator, among the imaginary lines that pass through the center of the rotating part (center of the rotating shaft) when viewed from the axial direction of the rotating shaft. If the length of the line segment varies depending on the measurement location, the length of the longest line segment is taken as the diameter of the rotating part. The diameter of the rotating part is usually equal to twice the distance from the center of the rotating part to the farthest end of the agitator, and is equal to the value calculated by subtracting the diameter of the inner periphery of the casing (D1 in Figure 3), described below, by twice the size of the clearance, described below.

[0097] The wider the agitating member, the larger the area that can be treated, so the width of the agitating member may be 15 mm or more, 25 mm or more, or 30 mm or more. The width of the agitating member may be 15 to 60 mm, 25 to 55 mm, or 30 to 55 mm. Here, the width of the agitating member means the length from one end to the other end of the agitating member when viewed in a direction intersecting the axial direction of the rotation shaft (for example, the distance between L1 and L3 in Figure 2).

[0098] The number of stirring members lined up in the axial direction of the rotating shaft is, for example, 2 or more, and may be 2 to 10, or 3 to 9, or 4 to 8. The number of stirring members lined up in the circumferential direction of the rotating shaft when viewed from the axial direction of the rotating shaft is, for example, 4 or less, and may be 1 to 4, or 2 to 3. The total number of stirring members is, for example, 2 to 40, or may be 10 to 20.

[0099] The length of the casing may be 30 mm or more (for example, 30 to 300 mm), or may be 200 to 300 mm. Here, the length of the casing means the length along the direction of the rotation axis of the casing.

[0100] The diameter of the inner periphery of the casing (D1 in FIG. 3) may be 50 mm or more (for example, 50 to 300 mm), or may be 100 to 200 mm.

[0101] The size of the gap (clearance) between the casing and the stirring member (the shortest distance between the casing and the stirring member) may be 2 mm or more, or may be 3 mm or more, from the viewpoint of suppressing crushing of the base material. The size of the clearance may be 10 mm or less, or may be 6 mm or less, from the viewpoint of smoothly progressing the compounding treatment. From these viewpoints, the size of the clearance may be, for example, 2 to 10 mm or 3 to 6 mm.

[0102] The effective processing volume of the dry particle composite device may be 0.015 L or more (for example, 0.015 to 0.50 L), or may be 0.15 L or more (for example, 0.15 to 0.45 L).

[0103] In the coating step, the above-mentioned (P1-P2) / m is set to 0.2 to 0.5 W·h / g. From the viewpoint of improving the bleed resistance of the resulting composite pigment, (P1-P2) / m may be 0.3 W·h / g or more. From the viewpoint of improving the bleed resistance of the resulting composite pigment, (P1-P2) / m may be 0.5 W·h / g or less, 0.45 W·h / g or less, or 0.4 W·h / g or less. From the above viewpoint, (P1-P2) / m may be, for example, 0.3 to 0.5 W·h / g, 0.3 to 0.45 W·h / g, or 0.3 to 0.4 W·h / g.

[0104] (P1-P2) / m can be adjusted by the amount of raw materials charged, as well as the shape and number of stirring members, the clearance of the device, the peripheral speed of the stirring members, the rotation speed of the stirring members, the mixing time, etc.

[0105] The peripheral speed of the stirring member in the coating step may be 5.0 to 20.0 m / s, 5.0 to 15.0 m / s, 10.0 to 15.0 m / s, or 10.0 to 13.0 m / s, from the viewpoints of preventing cracking of the substrate and smoothing the surface condition of the composite pigment.

[0106] The rotation speed of the stirring member in the coating step may be 500 rpm or more (for example, 500 to 5000 rpm), or may be 1000 to 5000 rpm, 1500 to 3500 rpm, or 1500 to 2500 rpm, from the viewpoint of efficiently progressing the composite treatment.

[0107] The mixing time in the coating step may be 1 to 10 minutes or 2 to 10 minutes, from the viewpoint of being able to prevent the base material from being crushed while allowing the composite treatment to proceed smoothly.

[0108] The amount of power used by the dry particle composite device in the coating step may be 100 to 2000W.

[0109] (Other processes) The method for producing a composite pigment may further include, in addition to the coating step, steps of sterilization, sieving, and the like.

[0110] <Cosmetics, inks, paints, toners, or molded products> Other embodiments of the present disclosure are cosmetics, inks, paints, toners, or molded articles containing the composite pigment of the above embodiment. These may contain, in addition to the composite pigment, general components suitable for the respective uses and purposes.

[0111] Examples of cosmetics include foundations (face colors, concealers, etc.), makeup bases (makeup bases, pre-makeup, etc.), face powders, lipsticks (lipstick, lip rouge, lip color, lip pencil, rouge paste, lip gloss, lip liner, etc.), eye makeup (eye shadow, eye color, eyeliner, eyebrow pencil, eyebrow pencil, eyebrow blush, mascara, eyelash cosmetics, etc.), cheek cosmetics (blush, cheek color, cheek rouge, etc.), nail cosmetics (nail enamel, nail polish, nail color, nail polish, pedicure, nail lacquer, top coat, base coat, etc.), and hair colorants (hair dye, hair color spray, hair color stick, color rinse, hair manicure, etc.).

[0112] The ink may be a printing ink, such as lithographic (offset) ink, letterpress ink, gravure ink, screen ink, flexographic ink, UV-curable ink, water-based ink, oil-based ink, vegetable oil ink, newspaper ink, or inkjet ink.

[0113] Examples of paints include powder paints, water-based (water-based) paints, epoxy resin paints, urethane resin paints, fluororesin paints, polyester resin paints, melamine resin paints, and synthetic resin paints such as acrylic resin paints.

[0114] Toner is a micro-sized powder made of electrostatically charged plastic particles with color particles attached thereto, used in laser printers and copiers. In toner, composite pigments may be blended as color particles.

[0115] The molded product may be one molded using a resin composition containing the composite pigment as a plastic colorant. The plastic colorant may be in the form of a masterbatch (MB), color pellets, color compound, dry color, paste color, liquid masterbatch, or the like. [Example]

[0116] The contents of the present disclosure will be described in more detail below using examples and comparative examples, but the present disclosure is not limited to the following examples.

[0117] <Materials and equipment used> In the examples and comparative examples, the following base materials 1 to 5, pigments (coating pigments) 1 to 5, and devices (dry composite devices) 1 and 2 were used.

[0118] [Base material] ·Base material 1 Titanium dioxide-coated mica particles (red, flake-shaped, manufactured by Sun Chemical, D50: 23 μm) ·Base material 2 Titanium dioxide-coated mica particles (red, flake-shaped, manufactured by Sun Chemical, D50: 20 μm) ·Base material 3 Titanium dioxide-coated mica particles (gold, flake-like, manufactured by Sun Chemical, D50: 23 μm) ·Base material 4 Titanium dioxide-coated mica particles (green, flake-like, manufactured by Sun Chemical, D50: 23 μm) ·Base material 5 Titanium dioxide-coated mica particles (silver, flakes, Colors & Effects, D50: 40 μm)

[0119] [Coating pigments] Pigment 1 Pigment (C19-7703, manufactured by Sun Chemical, organic pigment content: 60% by mass, D90-D10: 3.90 μm) containing organic pigment (Red No. 202, azo-based, CI Pigment Red 57:1) Pigment 2 Pigment (C19-7720, manufactured by Sun Chemical, organic pigment content: 100% by mass, D90-D10: 3.28 μm) consisting of an organic pigment (Red No. 202, azo-based, CI Pigment Red 57:1) Pigment 3 Pigment containing organic pigment (Red No. 202, azo-based, CI Pigment Red 57:1) (C19-003, manufactured by Sun Chemical, organic pigment content: 60% by mass, D90-D10: 87.06 μm) Pigment 4 Pigment containing organic pigment (Red No. 104 Aluminum Lake, tar dye) (C14-7723, manufactured by Sun Chemical Co., Ltd., organic pigment content: 22% by mass, D90-D10: 6.59 μm) Pigment 5 Pigment containing organic pigment (Blue No. 1 Aluminum Lake, tar pigment) (C39-7733, manufactured by Sun Chemical Co., Ltd., organic pigment content: 17% by mass, D90-D10: 4.76 μm)

[0120] [Dry compounding equipment] Device 1 (Nobilta (registered trademark) NOB-130) Blade diameter (φ): 124 mm Blade width: 49mm Number of blades: 16 in total (6 axial blades, 2 circumferential blades) Casing length: 230mm Casing inner diameter: 130mm Clearance: 3mm Effective processing volume: 0.269L Device 2 (Nobilta (registered trademark) NOB-mini) Blade diameter (φ): 86mm Blade width: 20mm Number of blades: 8 in total (2 axial blades, 4 circumferential blades) Casing length: 60mm Casing inner diameter: 92mm Clearance: 2mm Effective processing volume: 0.033L

[0121] <Examples 1 to 7 and Comparative Example 1> (Manufacturing composite pigments) A premix was prepared by premixing the base material and the coating pigment in the amounts listed in Table 1. The premix was then fed into a dry particle compositing apparatus (apparatus 1 or apparatus 2) listed in Table 1 and processed under the conditions (electrical energy, mixing time, applied power, rotation speed, and peripheral speed) listed in Table 1 to obtain a composite pigment. The applied power in Table 1 refers to the applied power per gram of raw materials (base material and coating pigment) and corresponds to the above-mentioned (P1-P2) / m. The rotation speed and peripheral speed in Table 1 refer to the rotation speed and peripheral speed of the blade.

[0122] (Measurement of absorbance A) The absorbance A was measured for the composite pigments of Examples 1 to 7 and Comparative Example 1. Specifically, 0.05 g of the composite pigment was dispersed in 20 mL of ethyl acetate, and the resulting dispersion was allowed to stand for 24 hours to separate into a precipitate and a supernatant. The absorbance of the supernatant was measured in the wavelength range of 300 to 800 nm using a Hitachi U-3900 spectrophotometer, and the absorbance at the maximum absorption wavelength (absorbance A) was determined. The results are shown in Table 1. The maximum absorption wavelength was read around 515 nm for Examples 1 to 4 and 7 and Comparative Example 1, around 560 nm for Example 5, and around 670 nm for Example 6.

[0123] (Measurement of strong coverage) The strong coverage ratio was measured for the composite pigments of Examples 1 to 7 and Comparative Example 1. Specifically, first, the absorbance A1 and absorbance A2 were measured according to the above-mentioned conditions 1 and 2, and the strong coverage ratio was calculated based on the above-mentioned formula (a). The results are shown in Table 1. Note that, as the dilution solvent under conditions 1 and 2, ethanol (dilute acid) was used in Examples 1 to 4 and 7 and Comparative Example 1, and sodium hydroxide test solution (dilute) was used in Examples 5 and 6. Furthermore, the maximum absorption wavelength was read around 521 nm in Examples 1 to 4 and 7 and Comparative Example 1, around 538 nm in Example 5, and around 630 nm in Example 6.

[0124] <Evaluation> The pigmentation resistance of the composite pigments of Examples 1 to 7 and Comparative Example 1 was evaluated. Specifically, first, a composite pigment (approximately 50 mg) was applied to a 5 mm x 5 mm or larger section of a 100 x 100 mm Bioskin Plate, Urethane No. 132 Series (No. 132#W, manufactured by Viewlux) and spread with a finger. After that, excess pigment was lightly blown off with air, and an appropriate amount (approximately 0.1 g) of cleansing oil (Deve OLIVE & ARGAN, Viewer Products Co., Ltd.) was applied to the pigment-applied area. Next, the pigment-applied area was rubbed with a finger for 2 seconds, the oil was wiped off with a Kimwipe, and the pigment-applied area was wiped up and wiped off. The pigment-applied area after wiping was measured using a colorimeter (eXact Advanced, manufactured by X-Rite) to determine the C* value. The color measurement conditions were illuminant: D50, standard observer: 2°. The results are shown in Table 1.

[0125] [Table 1]

Claims

1. A composite pigment comprising a substrate and a pigment covering a surface of the substrate, the base material and the pigment are combined by a mechanochemical treatment, the content of the pigment is 1 to 50 parts by mass relative to 100 parts by mass of the base material, The pigment includes an organic pigment, the substrate is a flaky substrate containing at least one selected from the group consisting of mica, aluminum, alumina, and glass, the organic pigment comprises at least one selected from the group consisting of azo-based synthetic organic pigments, thioindigo-based synthetic organic pigments, Red No. 3, Red No. 104, Red No. 106, Red No. 223, Red No. 230, Red No. 401, Blue No. 1, and lake pigments thereof; The composite pigment is such that, when 0.05 g of the composite pigment is dispersed in 20 mL of ethyl acetate and the resulting dispersion is allowed to stand for 24 hours to separate into a precipitate and a supernatant, the absorbance of the supernatant at the maximum absorption wavelength is 0.15 or less.

2. The composite pigment according to claim 1 , wherein the strong coverage is 80% or more.

3. 3. The composite pigment according to claim 1, wherein the content of the organic pigment in the pigment is 5 to 100% by mass.

4. The organic pigment comprises the azo-based synthetic organic pigment, 3. The composite pigment according to claim 1 or 2, wherein the azo-based synthetic organic pigment comprises at least one selected from the group consisting of Red No. 201, Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 227, Red No. 228, Red No. 405, Red No. 505, Orange No. 203, Orange No. 204, Orange No. 205, Yellow No. 4, Yellow No. 5, and Yellow No.

401.

5. The organic pigment comprises the lake pigment, 3. The composite pigment according to claim 1, wherein the lake pigment comprises at least one selected from the group consisting of aluminum lake, calcium lake, and barium lake.

6. The substrate comprises a core and a shell covering the surface of the core, The composite pigment according to claim 1 or 2, wherein the shell comprises at least one selected from the group consisting of a resin, a metal, and a metal oxide.

7. A method for producing a composite pigment comprising a substrate and a pigment covering a surface of the substrate, a coating step of coating a surface of the base material with the pigment by compounding the base material with the pigment including an organic pigment using a dry particle compounding device; the substrate is a flaky substrate containing at least one selected from the group consisting of mica, aluminum, alumina, and glass, the organic pigment comprises at least one selected from the group consisting of azo-based synthetic organic pigments, thioindigo-based synthetic organic pigments, Red No. 3, Red No. 104, Red No. 106, Red No. 223, Red No. 230, Red No. 401, Blue No. 1, and lake pigments thereof; the peripheral speed of the stirring member in the coating step is 5.0 to 20.0 m / s; a method for producing a composite pigment, wherein P1 denotes a load power amount consumed by the dry particle composite device in the coating step, P2 denotes a load power amount consumed by the dry particle composite device when the coating step is carried out in a state where the raw materials are excluded, and m denotes a mass of the raw materials used in the coating step, and (P1-P2) / m is 0.2 to 0.5 W·h / g.

8. 8. The method for producing a composite pigment according to claim 7, wherein, in a volume-based particle size distribution of the pigment measured by a wet laser diffraction / scattering method, when the particle sizes at which integrated values ​​from small particle sizes reach 10% and 90% of the total are defined as D10 and D90, respectively, D90 - D10 is 300 μm or less.

Citation Information

Patent Citations

  • Organic pigment adhered thin flaky pigment and its production

    JP1987101662A

  • New flaky pigment

    JP1993214257A

  • Pigment composition for traffic paint and preparation thereof

    JP1995331113A

  • Composite pigment and cosmetic containing the same

    JP1996059434A

  • Organic / Inorganic composite particle and its manufacturing method, and pigment composed of the powder, coating material and resin composition pigment dispersion and masterbatch using the pigment

    JP2002356625A