Pearlescent pigment that does not contain titanium dioxide

Abstract

The present invention relates to: a pearlescent pigment capable of implementing a pearlescent effect without containing titanium dioxide (TiO2); and a cosmetic composition containing same, and, more specifically, to: a pearlescent pigment on which a coating layer that is applied to a plate-shaped substrate and comprises zinc sulfide (ZnS) is formed; and a cosmetic composition containing same. The pearlescent pigment of the present invention exhibits various interference colors so as to have a pearlescent effect, without containing TiO2, which has recently been classified as an inhalation carcinogen and is banned from use. In addition, the cosmetic composition containing the pearlescent pigment, of the present invention, has excellent gloss, color development, texture, adherence, spreadability, lasting power and the like, and can ensure stability in terms of pH, odor and the like.

Description

Pearlescent pigments that do not contain titanium dioxide

[0001] The present invention relates to a pearlescent pigment capable of implementing a pearlescent effect without including titanium dioxide (TiO2) and a cosmetic composition comprising the same, and more particularly, to a pearlescent pigment having a coating layer comprising zinc sulfide (ZnS) formed while covering a plate-shaped substrate, and a cosmetic composition comprising the same.

[0002] This application claims priority to Korean Patent Application No. 10-2024-0038534, filed March 20, 2024, the entire disclosure of which is incorporated herein by reference.

[0003]

[0004] Cosmetics are products applied to the skin, such as by spraying or applying them, to cleanse or beautify it. Specifically, cosmetics are applied topically to exposed areas of the skin to protect them from external factors like sunlight, wind, and rain.

[0005] These cosmetics can be categorized into basic cosmetics for cleansing or beautifying the human body and keeping the skin healthy; makeup cosmetics such as loose powder, two-way cake, and foundation used to enhance attractiveness; hair cosmetics such as hair lotion and hair cream used to keep hair healthy and beautiful; and perfumes.

[0006] However, titanium dioxide (TiO2), which is widely used as a high-refractive material for effective pigments in cosmetic compositions, has recently been classified as an inhalable carcinogen in Europe and its use as a food additive is prohibited.

[0007] Korean Patent Publication No. 2023-0068379 discloses a layered pigment composition including a porous inorganic substrate and a porous inorganic shell as a TiO2-free pigment, but it is difficult to expect a pearlescent effect exhibiting various interference colors, and there are problems such as insufficient gloss, color development, usability, adhesion, spreadability, and durability.

[0008]

[0009] [Prior Art Literature]

[0010] [Patent Document]

[0011] Korean Patent Publication No. 2023-0068379

[0012]

[0013] Accordingly, the inventors of the present invention have conducted research and made efforts to develop a pigment material capable of implementing a pearlescent effect without including titanium dioxide (TiO2), which is widely used as a high-refractive-index material, and as a result, they have discovered that a pearlescent pigment formed with a coating layer including zinc sulfide (ZnS) as a high-refractive-index layer while covering a plate-shaped substrate can exhibit various interference colors, thereby completing the present invention.

[0014] Accordingly, an object of the present invention is to provide a pearlescent pigment capable of exhibiting various interference colors by covering a plate-shaped substrate with a coating layer containing zinc sulfide (ZnS).

[0015]

[0016] The present invention

[0017] plate-shaped substrate; and

[0018] A pearlescent pigment comprising a first coating layer containing ZnS while covering the above plate-shaped substrate is characterized.

[0019] The above plate-shaped substrate may be at least one selected from synthetic mica, natural mica, glass flake, plate-shaped iron oxide, plate-shaped alumina, aluminum flake, plate-shaped silica, talc, illite, sericite, and bismuth.

[0020] The above plate-shaped substrate may have an average diameter of 5 to 250 μm and a thickness of 50 to 1,000 nm.

[0021] The above first coating layer may have a thickness of 50 to 350 nm.

[0022] The above ZnS may be included in an amount of 1 to 200 parts by weight per 100 parts by weight of the plate-shaped substrate.

[0023] In addition, the pearlescent pigment of the present invention may further include a second coating layer formed on the surface of the first coating layer and including an oxide or hydroxide of an element selected from Si, Al, Zr, and Fe.

[0024] The second coating layer may include SiO2 and may have a thickness of 10 to 100 nm.

[0025] In addition, the pearlescent pigment of the present invention may include one or more silane compounds selected from hydrogen dimethicone, dimethicone, triethoxy caprylysilane, and polymethylsilsesquioxane on the surface of the second coating layer.

[0026] Additionally, the pearl luster pigment of the present invention may further include a pigment layer on the surface of the second coating layer.

[0027] In addition, the pearl luster pigment of the present invention,

[0028] A third coating layer formed on the surface of the second coating layer and containing ZnS; and

[0029] The third coating layer may further include a fourth coating layer formed on the surface thereof and containing an oxide or hydroxide of an element selected from among Mg, Si, Al, and Zr.

[0030] In addition, the pearl luster pigment of the present invention,

[0031] It can be used in paints, coatings, automotive paints, powder coatings, printing inks, security printing inks, plastics, ceramic materials, glass or paper, or in paper coatings, toners for electrophotographic printing processes, seeds, greenhouse sheeting or tarpaulins, or as an absorbent in laser marking of paper or plastics, or as an absorbent in laser welding of plastics, or in cosmetic formulations, or in the preparation of pigment pastes using water, organic and / or aqueous solvents, or in the preparation of pigment formulations or dry formulations.

[0032] Meanwhile, the present invention is characterized by a cosmetic composition comprising the pearlescent pigment in an amount of 0.01 to 95 wt% in the total composition.

[0033] In addition, the cosmetic composition of the present invention may include one or more components selected from the group consisting of water, polyol, polar or non-polar oil, fat, wax, film former, polymer, copolymer, surfactant, free-radical scavenger, antioxidant, stabilizer, odor improving agent, silicone oil, emulsifier, solvent, preservative, thickener, flow additive, flavoring agent, colorant, effect pigment, UV absorber, surface active agent and / or cosmetically active compound, filler, binder, pearlescent pigment, color pigment and organic dye.

[0034]

[0035] The pearlescent pigment of the present invention exhibits a pearlescent effect by displaying interference colors of various colors, while not containing TiO2, which has recently been classified as an inhalation carcinogen and is prohibited from use.

[0036] In addition, a cosmetic composition including the pearl luster pigment of the present invention has excellent gloss, color development, usability, adhesion, spreadability, and durability, and can secure stability in terms of pH and odor.

[0037]

[0038] Figure 1 is a micrograph (X 500) of the pearl luster pigment of Example 1.

[0039] Figure 2 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 1.

[0040] Figure 3 is a micrograph (X 500) of the pearl luster pigment of Example 2.

[0041] Figure 4 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 2.

[0042] Figure 5 is a micrograph (X 500) of the pearl luster pigment of Example 3.

[0043] Figure 6 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 3.

[0044] Figure 7 is a micrograph (X 500) of the pearlescent pigment of Example 4.

[0045] Figure 8 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 4.

[0046] Figure 9 is a micrograph (X 500) of the pearl luster pigment of Example 5.

[0047] Figure 10 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 5.

[0048] Fig. 11 is a micrograph (X 500) of the pearl luster pigment of Example 6.

[0049] Figure 12 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 6.

[0050] Figure 13 is a colorimetric coordinate image of the pearl luster pigments of Examples 1 to 6.

[0051] Figure 14 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 7.

[0052] Figure 15 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 8.

[0053] Figure 16 is a scanning electron microscope (SEM) photograph of the pearlescent pigment of Example 9.

[0054]

[0055] Hereinafter, the present invention will be described in detail. Prior to this, it should be noted that the terms and words used in this specification and claims should not be interpreted as limited to their conventional or dictionary meanings. Rather, they should be interpreted with meanings and concepts that conform to the technical spirit of the present invention, based on the principle that the inventor can appropriately define the concept of the term to best explain his or her invention. Accordingly, the configurations described in the embodiments described in this specification are merely the most preferred embodiments of the present invention and do not represent the entire technical spirit of the present invention. Therefore, it should be understood that various equivalents and modified examples may exist as of the time of this application.

[0056]

[0057] The pearlescent pigment of the present invention comprises a plate-shaped substrate and a first coating layer containing ZnS while covering the plate-shaped substrate.

[0058] In the present invention, pearlescent pigment refers to a pigment that produces a pearlescent, iridescent, or metallic color and has a special color and luster effect by utilizing the characteristics of light and the refraction of a material.

[0059] The above plate-shaped substrate may use at least one selected from synthetic mica, natural mica, glass flake, plate-shaped iron oxide, plate-shaped alumina, aluminum flake, plate-shaped silica, talc, illite, sericite, and bismuth.

[0060] At this time, the plate-shaped substrate may exhibit an average diameter of 5 to 250 ㎛ and a thickness of 100 to 1,000 nm, preferably an average diameter of 10 to 150 ㎛ and a thickness of 100 to 800 nm, and more preferably an average diameter of 20 to 100 ㎛ and a thickness of 200 to 500 nm.

[0061] What is meant by the first coating layer containing ZnS being coated on the plate-like substrate is that the first coating layer may be formed in a form in which the entire surface of the plate-like substrate is coated and completely surrounds it, or the first coating layer may be coated on only a portion of the surface of the plate-like substrate, or the first coating layer may be coated in an island form on the surface of the plate-like substrate.

[0062] The first coating layer including the above ZnS may have a thickness of 50 to 350 nm. In this case, the thickness refers to the thickness of each coating layer when the first coating layer is formed on both the upper and lower portions of the plate-shaped substrate.

[0063] The interference color may vary depending on the thickness of the first coating layer. Specifically, when the thickness is 50 to 80 nm, a white interference color is exhibited, when the thickness is 80 to 110 nm, a gold interference color is exhibited, when the thickness is 110 to 130 nm, a red interference color is exhibited, when the thickness is 130 to 150 nm, a violet interference color is exhibited, when the thickness is 150 to 180 nm, a blue interference color is exhibited, and when the thickness is 180 to 200 nm, a green interference color is exhibited.

[0064] In addition, when the thickness is 200 to 220 nm, it can exhibit interference colors of gold color again, and as the thickness of the coating layer increases, it can exhibit interference colors of red, violet, blue, and green colors.

[0065] The first coating layer including the above ZnS can be formed using a zinc precursor solution and a sulfur precursor solution. At this time, it is preferable to form the layer while adjusting the pH to a range of 3 to 7 using a pH adjuster, and more preferably, it is preferable to adjust the pH to a range of 3.5 to 6.

[0066] In addition, the coating of the ZnS is preferably performed at 40 to 100°C, more preferably at 50 to 90°C, and most preferably at 60 to 80°C.

[0067] The above zinc precursors include ZnCl2, ZnCl4, ZnSO4·7H2O, and Zn(CH3COO). 2, Zn(NO3)2, etc. can be used.

[0068] As the above sulfur precursor, Na2S, Na2S, Na2S2O4, Na2S2O7, C2H5NS, C2H4O2S, C2H4OS, etc. can be used.

[0069] ZnS formed in this way may be included in an amount of 1 to 200 parts by weight per 100 parts by weight of the plate-shaped substrate, preferably 5 to 150 parts by weight, and more preferably 10 to 120 parts by weight.

[0070]

[0071] In addition, the pearlescent pigment of the present invention may further include a second coating layer formed on the surface of the first coating layer and including an oxide or hydroxide of an element selected from Si, Al, Zr, and Fe.

[0072] The second coating layer may include silicon dioxide (SiO2), aluminum oxide (Al2O3), zirconium dioxide (ZrO2), or iron oxide (Fe2O3), and preferably may include silicon dioxide (SiO2).

[0073] The second coating layer including the above silicon dioxide (SiO2) can be formed by adding a Si precursor compound, stirring, and then adding a basic solution and further stirring. As the Si precursor compound, tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate (TMOS), etc. can be used.

[0074] Additionally, the second coating layer including the silicon dioxide (SiO2) can be formed using water glass.

[0075] The second coating layer may have a thickness of 10 to 100 nm, preferably 20 to 80 nm, and more preferably 30 to 60 nm.

[0076] In particular, when the pearlescent pigment of the present invention is dispersed in water, the atomic ratio of Zn and S cannot be 1:1 due to the elution of Zn ions from ZnS in the first coating layer, and a state in which Zn atoms are insufficient occurs, causing problems such as an increase in pH and the generation of odor. However, the second coating layer serves to protect the first coating layer, and can bring about effects such as pH stability of the pigment, improvement of brittleness, and clear trance color.

[0077] In addition, the surface of the second coating layer may include one or more silane compounds selected from hydrogen dimethicone, dimethicone, triethoxy caprylysilane, and polymethylsilsesquioxane. The silane compound improves the protective effect of the first coating layer of the second coating layer, and may exhibit the effect of forming a negative charge on the surface of the second coating layer to block particles exhibiting a negative charge by repulsion.

[0078] Additionally, the pearl luster pigment of the present invention may further include a pigment layer on the surface of the second coating layer.

[0079] The pigment layer may include various color pigments, but preferably may include a colored gloss pigment including a natural dye.

[0080] In addition, the pearl luster pigment of the present invention,

[0081] A third coating layer formed on the surface of the second coating layer and containing ZnS; and

[0082] The third coating layer may further include a fourth coating layer formed on the surface thereof and containing an oxide or hydroxide of an element selected from among Mg, Si, Al, and Zr.

[0083] The fourth coating layer may include magnesium oxide (MgO), silicon dioxide (SiO2), aluminum oxide (Al2O3), or zirconium dioxide (ZrO2), and preferably may include silicon dioxide (SiO2).

[0084] The pearlescent pigment of the present invention is

[0085] It can be used in paints, coatings, automotive paints, powder coatings, printing inks, security printing inks, plastics, ceramic materials, glass or paper, or in paper coatings, toners for electrophotographic printing processes, seeds, greenhouse sheeting or tarpaulins, or as an absorbent in laser marking of paper or plastics, or as an absorbent in laser welding of plastics, or in cosmetic formulations, or in the preparation of pigment pastes using water, organic and / or aqueous solvents, or in the preparation of pigment formulations or dry formulations.

[0086] Preferably, all plastics and films known to those skilled in the art can be colored using the pearlescent pigments according to the present invention. The pearlescent pigments according to the present invention can be mixed with organic dyes and / or pigments, such as transparent or opaque white, colored and black pigments and conventional transparent, colored and black luster pigments based on flake-shaped iron oxides, organic pigments, holographic pigments, LCPs (liquid crystal polymers) and metal oxide-coated flakes based on mica, glass, Al2O3, Fe2O3, SiO2, etc.

[0087] Meanwhile, the present invention is characterized by a cosmetic composition comprising the pearlescent pigment in an amount of 0.01 to 95 wt% in the total composition.

[0088] The cosmetic composition of the present invention may include one or more components selected from the group consisting of water, polyol, polar or non-polar oil, fat, wax, film former, polymer, copolymer, surfactant, free-radical scavenger, antioxidant, stabilizer, odor improving agent, silicone oil, emulsifier, solvent, preservative, thickener, flow additive, flavoring agent, colorant, effect pigment, UV absorber, surface active agent and / or cosmetically active compound, filler, binder, pearlescent pigment, color pigment and organic dye.

[0089] In addition, the cosmetic composition of the present invention may include raw materials for general cosmetics, including color cosmetics and basic cosmetics.

[0090] At this time, color cosmetics may include base makeup products such as BB cream, foundation, makeup base, primer, skin cover, powder pact, two-way cake, and loose powder; eye makeup products such as eye shadow, eyeliner, mascara, and eyebrow; cheek touch products such as blusher, highlighter, and shading; and lip products such as lipstick, lip gloss, lip tint, lip balm, lip lacquer, and liquid rouge.

[0091] Basic cosmetics can include sunscreen, toner, emulsion, cream, essence, ampoule, mist, cleansing foam, and hair products such as shampoo and conditioner.

[0092] The above cosmetic composition can secure usability by exhibiting stability in terms of pH, fragrance, etc. while exhibiting various interference colors without using titanium dioxide (TiO2) with a high refractive index, which is classified as an inhalation carcinogen.

[0093]

[0094] Hereinafter, the present invention will be described in detail using examples and experimental examples. However, the examples according to the present invention may be modified in various ways, and the scope of the present invention should not be construed as being limited to the examples described below. The examples of the present invention are provided to more fully explain the present invention to those of average skill in the art.

[0095]

[0096] Example 1: Preparation of ZnS coated pearlescent pigment (white)

[0097] 100 g of plate-shaped alumina having a 5-50 ㎛ particle size distribution was placed in a beaker containing 1,000 g of deionized water, and stirred at 450 rpm to prepare a slurry. The slurry was heated to 80°C, and when it reached 80°C, the pH of the slurry was adjusted to 4.0 using 10 wt% hydrochloric acid. Next, a 13.3 wt% ZnCl2 solution and a 7.8 wt% Na2S H2O solution were simultaneously titrated at a constant rate to maintain the pH at 4.0, and a total of 300 g of the ZnCl2 solution was added, followed by stirring for an additional 30 minutes. The product was then dehydrated, washed with water, and dried at 80°C for 12 hours.

[0098] Finally, ZnS was coated on plate-shaped alumina to obtain a pearlescent pigment exhibiting a white interference color, and its microscopic images are shown in Figs. 1 and 2.

[0099] In particular, as a result of measuring the thickness of ZnS shown in Fig. 2, it was confirmed that the upper part (D1) was 70 nm (±5 nm) and the lower part (D2) was 72 nm (±5 nm).

[0100]

[0101] Example 2: Preparation of ZnS coated pearlescent pigment (gold)

[0102] The procedure was the same as Example 1, except that a total of 600 g of the above ZnCl2 solution was added.

[0103] As a result, a pearlescent pigment exhibiting a gold interference color was obtained by coating ZnS on plate-shaped alumina, and its microscopic images are shown in Figs. 3 and 4.

[0104] In particular, as a result of measuring the thickness of ZnS shown in Fig. 4, it was confirmed that the upper part (D1) was 106 nm (±5 nm) and the lower part (D2) was 101 nm (±5 nm).

[0105]

[0106] Example 3: Preparation of ZnS coated pearlescent pigment (red)

[0107] The procedure was the same as Example 1, except that a total of 900 g of the above ZnCl2 solution was added.

[0108] As a result, a pearlescent pigment exhibiting a red interference color was obtained by coating ZnS on plate-shaped alumina, and its microscopic images are shown in Figs. 5 and 6.

[0109] In particular, as a result of measuring the thickness of ZnS shown in Fig. 6, it was confirmed that the upper part (D1) was 124 nm (±5 nm) and the lower part (D2) was 125 nm (±5 nm).

[0110]

[0111] Example 4: Preparation of ZnS coated pearlescent pigment (purple)

[0112] The procedure was the same as Example 1, except that a total of 1,200 g of the above ZnCl2 solution was added.

[0113] As a result, a pearlescent pigment exhibiting a violet interference color was obtained by coating ZnS on plate-shaped alumina, and its microscopic images are shown in Figs. 7 and 8.

[0114] In particular, as a result of measuring the thickness of ZnS shown in Fig. 8, it was confirmed that the upper part (D1) was 136 nm (±5 nm) and the lower part (D2) was 135 nm (±5 nm).

[0115]

[0116] Example 5: Preparation of ZnS coated pearlescent pigment (blue)

[0117] The procedure was the same as Example 1, except that a total of 1,500 g of the above ZnCl2 solution was added.

[0118] As a result, a pearlescent pigment exhibiting a blue interference color was obtained by coating ZnS on plate-shaped alumina, and its microscopic images are shown in Figs. 9 and 10.

[0119] In particular, as a result of measuring the thickness of ZnS shown in Fig. 10, it was confirmed that the upper part (D1) was 153 nm (±5 nm) and the lower part (D2) was 161 nm (±5 nm).

[0120]

[0121] Example 6: Preparation of ZnS coated pearlescent pigment (green)

[0122] The same procedure as Example 1 was followed, except that a total of 1,800 g of the above ZnCl2 solution was added.

[0123] As a result, a pearlescent pigment exhibiting a green interference color was obtained by coating ZnS on plate-shaped alumina, and its microscopic images are shown in Figs. 11 and 12.

[0124] In particular, as a result of measuring the thickness of ZnS shown in Fig. 12, it was confirmed that the upper part (D1) was 190 nm (±5 nm) and the lower part (D2) was 188 nm (±5 nm).

[0125]

[0126] Experimental Example 1: Color difference measurement of pearlescent pigments

[0127] The pearlescent pigments obtained in Examples 1 to 6 were mixed with nitrocellulose resin at a pigment concentration of 6 wt%, and a film was formed using a 100 μm doctor blade. The color difference was measured using BYK maci, and the results are shown in Fig. 13.

[0128]

[0129] Example 7: Preparation of ZnS coated pearlescent pigment (gold)

[0130] The procedure was the same as Example 1, except that a total of 2,100 g of the above ZnCl2 solution was added.

[0131] As a result, a pearlescent pigment exhibiting a gold interference color was obtained by coating ZnS on plate-shaped alumina, and a microscope photograph thereof is shown in Fig. 14.

[0132] In particular, as a result of measuring the thickness of ZnS shown in Fig. 14, it was confirmed that the upper part (D1) was 205 nm (±5 nm) and the lower part (D2) was 201 nm (±5 nm).

[0133]

[0134] Example 8: Preparation of ZnS coated pearlescent pigment (green)

[0135] The procedure was the same as Example 1, except that a total of 3,300 g of the above ZnCl2 solution was added.

[0136] As a result, a pearlescent pigment exhibiting a green interference color was obtained by coating ZnS on plate-shaped alumina, and a microscope photograph thereof is shown in Fig. 15.

[0137] In particular, as a result of measuring the thickness of ZnS shown in Fig. 15, it was confirmed that the upper part (D1) was 310 nm (±5 nm) and the lower part (D2) was 306 nm (±5 nm).

[0138]

[0139] Example 9: Preparation of pearlescent pigment with protective layer formed using TEOS

[0140] 100 g of the pearlescent pigment exhibiting the interference color of gold of Example 2 was added to 490 g of isopropyl alcohol (IPA) to prepare a slurry. Then, tetraethyl orthosilicate (TEOS) was added to the dispersed slurry and stirred at 400 rpm. After the temperature was raised to 50°C, 145 g of 0.89 wt% ammonia water was added and stirred for about 10 hours while maintaining the temperature. Thereafter, after dehydration and washing with isopropyl alcohol (IPA), the slurry was dried to obtain a pearlescent pigment having a SiO2 protective layer formed thereon.

[0141] A microscope photograph of the pearl luster pigment manufactured in this manner is shown in Fig. 16.

[0142] As shown in the above Figure 16, it was confirmed that a ZnS layer was located on the upper and lower parts of the plate-shaped aluminum, and a SiO2 protective layer was formed on the outside.

[0143]

[0144] Example 10: Preparation of pearlescent pigment with a protective layer formed using water glass

[0145] 100 g of the pearlescent pigment exhibiting the interference color of gold of Example 2 was added to 1 L of deionized water and stirred to form a slurry. The slurry was heated to 80°C, and when it reached 80°C, the pH was adjusted to 6.5 using 5 wt% NaOH. 100 g of 5 wt% water glass was titrated into the slurry at a constant rate over 4 hours, while maintaining the pH constant with a 5 wt% HCl dilution solution. After titration, the mixture was refluxed for 60 minutes, and the final slurry was filtered, dehydrated, washed with water, and dried at 80°C for 12 hours. The dried powder was heat-treated at 350°C / 30 min to obtain a pearlescent pigment having a SiO2 protective layer formed thereon.

[0146]

[0147] Example 11: Preparation of pearlescent pigment having a natural pigment coating layer formed thereon.

[0148] 100 g of the red natural pigment prepared by the method described in Patent Publication No. 10-2015-0048588 and 1,000 g of deionized water were placed in a beaker and stirred at 300 rpm to form a slurry. Next, the pearlescent pigment of Example 9 and CaCl2 were added, the pH of the mixed solution was adjusted to 5, and the mixture was stirred and refluxed for 30 minutes. The final slurry after refluxing was washed and dehydrated, and dried at 80°C. After drying, it was screened using a 325 mesh sieve to remove aggregated particles formed during the reaction, thereby obtaining a red powder coated with the final red natural pigment.

[0149]

[0150] Example 12: Preparation of pearlescent pigment treated with silane compound

[0151] 100 g of the pearlescent pigment of Example 9 and 1,000 g of deionized water were placed in a beaker and stirred at 450 rpm to form a slurry. Next, the slurry was heated to 80°C, and when it reached 80°C, the pH was adjusted to 6.0 using 10 wt% caustic soda. Next, while maintaining the pH at 6.0, 5 wt% silane was slowly titrated. Hydrogen dimethicone was used as the silane. After the titration, the coated silane was stabilized through reflux for 30 minutes. After reflux, dehydration was performed, and after washing with water, it was sufficiently dried in an oven at 100°C to obtain a pearlescent pigment having a silane compound treated on the final surface.

[0152]

[0153] Example 13: Preparation of pearlescent pigment having a third coating layer and a fourth coating layer formed thereon.

[0154] 100 g of the pearl luster pigment of Example 9 and 1,000 g of deionized water were placed in a beaker and stirred at 300 rpm to form a slurry.

[0155] The above slurry was heated to 80°C, and when it reached 80°C, the pH of the slurry was adjusted to 4.0 using 10 wt% hydrochloric acid. Next, a 13.3 wt% ZnCl2 solution and a 7.8 wt% Na2S H2O solution were simultaneously titrated at a constant rate to maintain the pH at 4.0, and a total of 600 g of the ZnCl2 solution was added, followed by stirring for an additional 30 minutes. Thereafter, the product was dehydrated and washed with water, and dried at 80°C for 12 hours to obtain a pigment having a third coating layer formed thereon.

[0156] After that, 100 g of the pigment was added to 490 g of isopropyl alcohol (IPA) to prepare a slurry. Thereafter, tetraethyl orthosilicate (TEOS) was added to the dispersed slurry and stirred at 400 rpm. After the temperature was raised to 50°C, 145 g of 0.89 wt% ammonia water was added and stirred for about 10 hours while maintaining the temperature. Thereafter, the pigment was dehydrated and washed with isopropyl alcohol (IPA) and dried to obtain a pigment having a fourth coating layer formed thereon. It was confirmed that the pigment was a pearlescent pigment with improved saturation and gloss and a gold interference color.

[0157]

[0158] Experimental Example 2: Preparation and property evaluation of cosmetic composition

[0159] Cream eyeshadow cosmetic compositions were prepared using the pearlescent pigment powders of Examples 2 and 9 above. Cream eyeshadows of Preparation Examples 1 and 2 were prepared with the compositions shown in Table 1 below (unit: weight %).

[0160] Classification Ingredient name Manufacturing example 1 Manufacturing example 2 A Caprylic / capric triglyceride Bal. Bal. Hydrogenated polyisobutene 16.00 16.00 Phenyl trimethicone 15.00 15.00 Beeswax 5.00 5.00 Preservative 0.30 0.30 B Example 2 pigment - 40.00 Example 9 pigment 40.00 -

[0161] 1) Manufacturing method

[0162] After weighing the A phase in a beaker, heat it in a constant temperature water bath at 85℃ and mix it evenly using a stirrer.

[0163] Next, add phase B to phase A and mix evenly using a stirrer to prevent clumping of the pearl pigment.

[0164] Next, an appropriate amount of the semi-finished product was placed in a mold, cooled to room temperature, and molded to produce a cream eyeshadow.

[0165]

[0166] 2) Physical property evaluation

[0167] In order to determine the effectiveness of the above manufacturing example, 40 women aged 20 to 40 were subjected to actual use for 15 days, and the average score of the results was evaluated.

[0168] The comparison items were gloss, color development, usability, adhesion, spreadability, and durability, and the results are shown in Table 2 below.

[0169] Distinction Gloss Coloration Feel Adhesion Spreading Durability Manufacturing Example 14.24.13.94.13.63.3 Manufacturing Example 24.54.63.84.03.63.3

[0170] * A higher number means a better score.

[0171] 1: Very bad, 2: Bad, 3: Average, 4: Good, 5: Very good

[0172]

[0173] As shown in Table 2 above, Manufacturing Example 2 was relatively superior to Manufacturing Example 1 in terms of gloss and color development, and other usability, adhesion, spreadability, and durability showed almost similar results.

[0174]

[0175] Experimental Example 3: Stability Evaluation of Cosmetic Compositions

[0176] The stability of the cosmetic composition of the above manufacturing example was tested as follows.

[0177] First, the compositions of Manufacturing Examples 1 and 2 were dispersed in DI water at a concentration of 10 wt% and stored at room temperature (RT) and 45°C. After 60 days, the changes in pH and the occurrence of odor were measured, which are shown in Tables 3 and 4 below. In addition, the compositions of Manufacturing Examples 1 and 2 were dispersed in oil (Caprylic / Capric Triglyceride) at a concentration of 10 wt% and stored at room temperature (RT) and 45°C. After 60 days, the changes in pH and the occurrence of odor were measured, which are shown in Tables 5 and 6 below.

[0178] time(day)135710213160 Manufacturing Example 1 RTpH3.633.653.673.843.934.014.084.24 Take 5554332145℃pH3.843.863.923.984.054.124.234.51 Take 55433211

[0179] time(day)135710213160 Manufacturing Example 2 RTpH5.865.855.875.875.885.895.915.95 Take55555555445℃pH6.526.516.516.526.536.546.596.59 Take55555544

[0180] time(day)135710213160 Manufacturing Example 1 RT Take 5555444445℃ Take 55544433

[0181] time(day)135710213160 Manufacturing Example 2RT Take 5555555545℃ Take 55555554

[0182] * A higher number means a better score.

[0183] 1: Very bad, 2: Bad, 3: Average, 4: Good, 5: Very good

[0184]

[0185] In the case of the cosmetic composition of the above Manufacturing Example 1, it was confirmed that the pH increased over time and some odor was generated, but in the case of the cosmetic composition of the above Manufacturing Example 2, it was confirmed that there was almost no increase in pH in water and oil and no odor was generated.

Claims

1. Plate-shaped substrate; and A first coating layer containing ZnS while covering the above plate-shaped substrate; A pearlescent pigment characterized by comprising:

2. In paragraph 1, A pearl luster pigment characterized in that the plate-shaped substrate is at least one selected from synthetic mica, natural mica, glass flake, plate-shaped iron oxide, plate-shaped alumina, aluminum flake, plate-shaped silica, talc, illite, sericite, and bismuth.

3. In paragraph 1, A pearlescent pigment characterized in that the above plate-shaped substrate exhibits an average diameter of 5 to 250 ㎛ and a thickness of 50 to 1,000 nm.

4. In paragraph 1, A pearlescent pigment characterized in that the first coating layer has a thickness of 50 to 350 nm.

5. In paragraph 1, A pearlescent pigment characterized in that the above ZnS is contained in an amount of 1 to 200 parts by weight per 100 parts by weight of the plate-shaped substrate.

6. In paragraph 1, A pearlescent pigment characterized in that it further comprises a second coating layer formed on the surface of the first coating layer and containing an oxide or hydroxide of an element selected from Si, Al, Zr, and Fe.

7. In paragraph 6, A pearlescent pigment characterized in that the second coating layer comprises SiO2.

8. In paragraph 6, A pearlescent pigment characterized in that the second coating layer has a thickness of 10 to 100 nm.

9. In paragraph 6, A pearlescent pigment characterized in that it comprises one or more silane compounds selected from hydrogen dimethicone, dimethicone, triethoxy caprylysilane, and polymethylsilsesquioxane on the surface of the second coating layer.

10. In paragraph 6, A pearl luster pigment characterized in that it further includes a pigment layer on the surface of the second coating layer.

11. In paragraph 6, A third coating layer formed on the surface of the second coating layer and containing ZnS; and A pearlescent pigment characterized by comprising a fourth coating layer formed on the surface of the third coating layer and containing an oxide or hydroxide of an element selected from among Mg, Si, Al, and Zr.

12. In any one of the clauses 1 to 11 selected, Pearlescent pigments for use in paints, coatings, automotive paints, powder coatings, printing inks, security printing inks, plastics, ceramic materials, glass or paper, or for use in paper coatings, toners for electrophotographic printing processes, seeds, greenhouse sheeting or tarpaulins, or for use as absorbents in laser marking of paper or plastics, or for use as absorbents in laser welding of plastics, or for use in cosmetic preparations, or for use in the preparation of pigment pastes using water, organic and / or aqueous solvents, or for use in the preparation of pigment preparations or dry preparations.

13. A cosmetic composition characterized in that the pearlescent pigment selected from any one of claims 1 to 11 is included in an amount of 0.01 to 95 wt% in the entire composition.

14. In paragraph 13, A cosmetic composition characterized in that it comprises at least one component selected from the group consisting of water, polyol, polar or non-polar oil, fat, wax, film former, polymer, copolymer, surfactant, free-radical scavenger, antioxidant, stabilizer, odor improving agent, silicone oil, emulsifier, solvent, preservative, thickener, flow additive, flavoring agent, colorant, effect pigment, UV absorber, surface active agent and / or cosmetically active compound, filler, binder, pearlescent pigment, color pigment and organic dye.

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