A composition, its application and powder phase-liquid phase double-layer product

Through the chelation or adsorption effect of component I and component II of the composition, the problem of uneven sedimentation of zinc oxide in cosmetics is solved, rapid stratification and uniform dispersion are achieved, and product quality and usage experience are improved.

CN115944554BActive Publication Date: 2025-10-03AO YE JI SHI YAN SHI XI TONG GONG CHENG (SHANG HAI) YOU XIAN GONG SI
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Patent Information

Application Number
CN202211743630.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-29
Publication Date
2025-10-03
Estimated Expiration
2042-12-29

AI Technical Summary

Technical Problem

Powdered zinc oxide tends to settle and is difficult to remix evenly in cosmetic products with a high liquid content, affecting product quality and consumer satisfaction.

Method used

The composition comprises components I and II, wherein component I comprises a C8-C10 weak acid and a C4-C10 alcohol, and component II comprises a skin conditioning agent A and adenosine. Component I and component II are chelated or adsorbed on the surface of zinc oxide to reduce the zeta potential, thereby achieving rapid sedimentation and uniform dispersion.

Benefits of technology

It achieves rapid sedimentation and stratification of zinc oxide, keeps the water phase clear, avoids agglomeration, and can quickly mix into a suspension when shaken, improving the product experience.

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Abstract

The present application discloses a composition comprising component I and component II; component I comprises the following raw materials: a C8-C10 weak acid and a C4-C10 alcohol; component II comprises the following raw materials: a skin conditioner A, a skin conditioner B, and adenosine; wherein the skin conditioner A comprises yeast glycoprotein and a neutral or acidic compound with an amino group; and the skin conditioner B comprises a neutral or acidic compound with an amino group. The present application also provides applications of the above-mentioned combination and a powder-liquid phase bilayer product. When the composition provided by the present application is added to a powder-liquid phase bilayer product containing zinc oxide, the zinc oxide can have a better sedimentation rate and can be quickly separated into layers during storage; at the same time, the zinc oxide can maintain a dispersed state without agglomeration or aggregation, and can be quickly mixed with the liquid phase to form a suspension when shaken.
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Description

Technical Field

[0001] The present application relates to the field of cosmetic technology, and in particular to a composition, its application, and a powder phase-liquid phase double-layer product. Background Art

[0002] Zinc oxide is a non-toxic, odorless, amphoteric oxide belonging to Group VI. It is abundant and relatively inexpensive. Its most common crystal structure is the regular hexagonal zirconite, which is thermodynamically stable at room temperature. Zinc oxide has a wide band gap, a large surface area (surface area / volume), small particle size, good dispersibility, and excellent stability. It exhibits excellent optical, chemical, electrical, and biological properties. It possesses anti-inflammatory, hemostatic, and somewhat astringent properties, and also has the ability to absorb oil secreted by human skin.

[0003] Zinc oxide is widely used in products such as sunscreen, foundation, powders, and lotions. As consumers' demand for efficacy continues to rise, its application in cosmetics is becoming increasingly widespread. However, powdered zinc oxide in most products, especially those with high liquid content, settles to the bottom. Therefore, issues such as settling speed and the ability to remix after settling affect the performance of gouache-based layered products, impacting product quality and consumer satisfaction. Summary of the Invention

[0004] To solve the above technical problems, the first object of the present invention is to provide a composition; the second object of the present invention is to provide a use of the composition in preparing a powder phase-liquid phase dual-layer product containing zinc oxide; and the third object of the present invention is to provide a powder phase-liquid phase dual-layer product containing zinc oxide. When the composition provided in this application is added to a powder phase-liquid phase dual-layer product containing zinc oxide, the zinc oxide can have a good sedimentation rate, allowing for rapid stratification during storage; at the same time, the zinc oxide can maintain a dispersed state without agglomeration or aggregation, and can be quickly mixed with the liquid phase to form a suspension when shaken.

[0005] The technical solutions provided by the present invention are as follows:

[0006] A composition comprising component I and component II;

[0007] Component I includes the following raw materials: C8-C10 weak acid, C4-C10 alcohol;

[0008] Component II includes the following raw materials: skin conditioning agent A, skin conditioning agent B and adenosine;

[0009] Wherein, the skin conditioning agent A comprises yeast glycoprotein and a neutral or acidic compound with an amino group;

[0010] Skin conditioning agents B include neutral or acidic compounds having an amino group.

[0011] Preferably, component I comprises the following raw materials: a C8-C10 weak acid, a C4 alcohol, and a C10 alcohol;

[0012] Component II includes the following raw materials: skin conditioning agent A, skin conditioning agent B and adenosine;

[0013] Wherein, the skin conditioning agent A comprises yeast glycoprotein, and neutral amino acids and / or acidic amino acids;

[0014] The skin conditioning agent B includes a neutral amino acid derivative and / or an acidic amino acid derivative.

[0015] Preferably, component I comprises the following raw materials: 10-hydroxydecanoic acid; 1,10-decanedioic acid; 1,10-decanediol; 1,3-butanediol;

[0016] Component II includes the following raw materials: skin conditioning agent A, skin conditioning agent B and adenosine;

[0017] Wherein, the skin conditioning agent A comprises yeast glycoprotein, glutamic acid, valine, and threonine;

[0018] Skin Conditioning Agent B includes glutamylaminoethylimidazole.

[0019] Preferably, component I comprises the following raw materials: 1.8-2.4 parts by weight of 10-hydroxydecanoic acid; 1.8-2.4 parts by weight of 1,10-decanedioic acid; 1.0-1.5 parts by weight of 1,10-decanediol; 94-96 parts by weight of 1,3-butanediol;

[0020] Component II comprises the following raw materials: 0.2-1.0 parts by weight of skin conditioning agent A, 0.2-2.0 parts by weight of skin conditioning agent B, and 0.1-2.0 parts by weight of adenosine;

[0021] Wherein, the skin conditioning agent A comprises, by mass fraction, 1-5% yeast glycoprotein, 1-5% glutamic acid, 0.1-1% valine, 0.1-1% threonine, and the balance is water;

[0022] Calculated by mass fraction, the skin conditioner B comprises 1% of glutamylaminoethylimidazole and the balance is water.

[0023] Preferably, component I comprises the following raw materials: 2.1 parts by weight of 10-hydroxydecanoic acid; 2.1 parts by weight of 1,10-decanedioic acid; 1.3 parts by weight of 1,10-decanediol; 94.5 parts by weight of 1,3-butanediol;

[0024] The skin conditioning agent A used in component II comprises, by mass fraction, 3% yeast glycoprotein, 3% glutamic acid, 0.55% valine, 0.55% threonine, and the balance being water.

[0025] Preferably, the skin conditioner A further comprises 0.2-2% of a preservative and <0.1% of a stabilizer, sodium metabisulfite, wherein the preservatives are phenoxyethanol and ethylhexylglycerin, and the mass ratio of phenoxyethanol to ethylhexylglycerin is 1:1;

[0026] Skin Conditioner B also includes a preservative (0.4%), wherein the preservatives are sorbic acid and phenoxyethanol, with the mass ratio of sorbic acid to phenoxyethanol being 1:3. More preferably, the preservatives used in Skin Conditioner A are phenoxyethanol (0.55%) and ethylhexylglycerin (0.55%). The stabilizer, sodium metabisulfite, is preferably used in an amount of 0.01-0.09%.

[0027] Preferably, the mass ratio of component I to component II is (1-4):(0.25-1.75).

[0028] Use of any of the above-described compositions in preparing a powder-liquid bilayer product containing zinc oxide, wherein the liquid phase comprises water and ethanol, and wherein the composition functions to accelerate zinc oxide sedimentation, reduce zinc oxide aggregation, and maintain clarity of the aqueous phase. Without the addition of other raw materials, the aqueous phase is colorless and clear. Even when the addition of other raw materials causes a color change in the aqueous phase, the composition provided herein can maintain clarity of the aqueous phase.

[0029] A powder phase-liquid phase double-layer product containing zinc oxide, characterized by comprising any one of the above-mentioned compositions.

[0030] Preferably, the addition amount of the combination is 0.5-15%, preferably 1-10%, more preferably 2-6%, more preferably 3-4%, calculated on a mass fraction basis.

[0031] For zinc oxide-containing products with a powder-liquid dual-layer structure, achieving a clear liquid upper layer and solid powder lower layer, while avoiding the appearance of a suspended state that would affect the appearance, the sedimentation rate of the solid powder must be considered. However, the settled powder must not aggregate and must disperse quickly when shaken for ease of use.

[0032] In response to the above problems, the present application provides a composition comprising component I and component II; component I comprises the following raw materials: a C8-C10 weak acid and a C4-C10 alcohol; component II comprises the following raw materials: a skin conditioner A, a skin conditioner B, and adenosine; wherein the skin conditioner A comprises yeast glycoprotein, as well as neutral amino acids and / or acidic amino acids; and the skin conditioner B comprises neutral amino acid derivatives and / or acidic amino acid derivatives. The composition provided in the present application is added to a powder phase-liquid phase double-layer product containing zinc oxide, which can give the zinc oxide a good sedimentation rate and allow for rapid stratification during storage; at the same time, the zinc oxide can maintain a dispersed state without agglomeration or aggregation, and can be quickly mixed with the liquid phase to form a suspension when shaken.

[0033] The present application abandons the traditional method of surface-coating zinc oxide or introducing other powdered raw materials to increase sedimentation. Instead, zinc oxide is chelated or adsorbed on the surface of zinc oxide by using compounds containing carboxyl groups, amino groups and alkylated amino groups, thereby reducing the Zeta potential of zinc oxide and allowing it to sediment quickly. In addition, the dispersion slurry can be repeatedly dispersed and sedimented by shaking.

[0034] In the present application, component I consisting of 10-hydroxydecanoic acid; 1,10-decanedioic acid; 1,10-decanediol; and 1,3-butanediol is purchased from the market with the trade name Acnacidol™ BG.

[0035] Component II includes 0.2-1.0 parts by weight of skin conditioning agent A (1-5% yeast glycoprotein, 1-5% glutamic acid, 0.1-1% valine, 0.1-1% threonine, 0.2-2% preservative, <0.1% sodium metabisulfite stabilizer, wherein the preservatives are phenoxyethanol and ethylhexylglycerin in a 1:1 ratio, and the balance is water), 0.2-2.0 parts by weight of skin conditioning agent B (1% glutamylaminoethylimidazole, 0.4% preservative, wherein the preservatives are sorbic acid and phenoxyethanol in a 1:3 ratio, and the balance is water), and 0.1-2.0 parts by weight of adenosine. This component, named CLOCK-F, is a composite raw material developed by the applicant, as shown in patent CN110448478B.

[0036] Among them, skin conditioner A and skin conditioner B are also purchased from the market, with the trade names of REVITALIN PF and CHRONOCYCLIN respectively.

[0037] CHRONOCYCLIN is also known as skin rhythm peptide. The structure of glutamylaminoethylimidazole it contains is shown in the figure below:

[0038]

[0039] Adenosine is a nucleotide composed of ribose (ribofuranose) and adenine, linked by a β-N9 glycoside bond. The structure is as follows:

[0040]

[0041] This application also provides the use of the above-mentioned composition in preparing a powder-liquid phase bilayer product containing zinc oxide; wherein the liquid phase comprises water and ethanol. The composition functions to accelerate zinc oxide sedimentation, reduce zinc oxide aggregation, and maintain a colorless and clear aqueous phase. The water and ethanol in the liquid phase can be mixed in any proportion; preferably, the amount of ethanol in the liquid phase is 20-40%.

[0042] This application also provides a zinc oxide-containing powder-liquid dual-layer product. Adding the aforementioned composition can accelerate zinc oxide sedimentation, reduce zinc oxide aggregation, and maintain a colorless and clear aqueous phase. The powder-liquid dual-layer product can be a lotion, sunscreen, or other product, and can be formulated with other reagents known in the art as needed. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments recorded in this application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0044] Figure 1 is the particle size distribution curve of zinc oxide used in the embodiments of the present invention;

[0045] Figure 2 : is an electron microscope photograph of the zinc oxide particles used in the examples of the present invention;

[0046] Figure 3 This is a photo showing the color change of the system after adding EDTA 2Na Ca in the examples of the present invention;

[0047] Figure 4 The following is a photograph of the experimental results of the combination ratio optimization in the embodiment of the present invention. DETAILED DESCRIPTION

[0048] In order to help those skilled in the art better understand the technical solutions in this application, the technical solutions in the embodiments of this application will be clearly and completely described below. Obviously, the embodiments described are only part of the embodiments of this application, not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without making any creative efforts shall fall within the scope of protection of this application.

[0049] 1. Experimental Verification

[0050] 1 Preparation of nano zinc oxide dispersion

[0051] Weigh 18g of zinc oxide powder in a 100mL beaker, add 42g of deionized water, and stir until uniformly dispersed. Then, homogenize at 4000 rpm for 3min at room temperature to fully disperse the zinc oxide powder. Then, add 30g of ethanol (75% by volume) while stirring and stir for 30min to obtain zinc oxide-water-ethanol dispersion A. The average particle size of the zinc oxide used is ≤1μm (distribution curve shown in Figure 1 , photos such as Figure 2 ), non-volatile matter content ≥98.0%.

[0052] 2. Raw material screening test

[0053] Add the alternative component to dispersion slurry A to obtain the final dispersion slurry of the alternative component. After standing and stratifying under the same dispersion conditions, measure the ratio of the total liquid level height to the height of the settled zinc oxide in the final dispersion slurry after 12 hours and record it as the solid-liquid ratio.

[0054] 2.1. Add water to dispersion slurry A to 100 g to obtain blank zinc oxide-water-ethanol final dispersion slurry Ta1;

[0055] 2.2. When preparing dispersion slurry A, add 40 g of ethanol (75% by volume) to obtain blank zinc oxide-water-ethanol final dispersion slurry Ta2;

[0056] 2.3. When preparing dispersion slurry A, add 32 g of deionized water and 50 g of ethanol (75% by volume) to obtain blank zinc oxide-water-ethanol final dispersion slurry Ta3;

[0057] 2.4. Add salicylic acid to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0058] 2.5. Add KCl to dispersion slurry A and add water to 100g to obtain the final dispersion slurry;

[0059] 2.6. Add EDTA-2Na Ca to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0060] 2.7. Add pyrrolidone carboxylic acid (PCA-H) to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0061] 2.8. Add nicotinamide to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0062] 2.9. Add CLOCK-F to dispersion A and add water to 100g to obtain the final dispersion;

[0063] 2.10. Add Acnacidol BG to dispersion A and add water to 100g to obtain the final dispersion;

[0064] 2.11. Add glycerol to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0065] 2.12. Add PE9010 (phenoxyethanol and ethylhexylglycerin in a mass ratio of 1:1) to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0066] 2.13. Add arginine to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0067] 2.14. Add PEG400 to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry;

[0068] 2.15. Add diethoxyethyl succinate (EDS) to dispersion slurry A and add water to 100 g to obtain the final dispersion slurry.

[0069] The amount of the above raw materials added (unit: g) and the measured solid-liquid ratio are shown in Table 1

[0070] Table 1

[0071]

[0072] The smaller the solid-to-liquid ratio, the greater the difference between the settled zinc oxide height and the total liquid level (the combined height of the liquid phase and the powder phase), indicating more thorough zinc oxide sedimentation. The solid-to-liquid ratio data in Table 1 show that the experimental groups containing salicylic acid, the chelating agent EDTA-2Na Calcium, pyrrolidone carboxylic acid (PCA-H), Acnacidol BG, CLOCK-F, and glycerol had even lower solid-to-liquid ratios, indicating that these agents have a certain effect on the sedimentation rate of zinc oxide.

[0073] Further observation of the experimental group revealed the following issues:

[0074] Salicylic acid is acidic and has carboxyl groups that can adsorb to the surface of zinc oxide powder, and has the ability to significantly increase the sedimentation effect of zinc oxide powder. However, while salicylic acid promotes sedimentation, it will produce agglomeration and cannot be repeatedly shaken for use.

[0075] The chelating agent represented by EDTA 2Na Ca has excellent sedimentation improvement ability due to its strong binding ability with zinc oxide. However, in the subsequent stability study, it was found that it would cause the system to change color, and the color gradually deepened with the increase of light exposure time. The color change photos are shown in Table 2 and Figure 3 , which is not conducive to maintaining the colorless and clear state of the liquid phase and is not suitable for products with lighter colors.

[0076] Pyrrolidone carboxylic acid (PCA-H) is a strong acid that can be adsorbed on the surface of zinc oxide powder and has a strong binding ability with zinc oxide. However, it will also react with zinc oxide and consume some of the zinc oxide powder. It is not suitable for products that require a quantitative amount of zinc oxide powder.

[0077] The amount of glycerol added in the experimental group was relatively high, which would have a greater application limitation on the composition. Considering that the additive used to promote the precipitation of zinc oxide needs to have a smaller impact on the entire formula system, glycerol was excluded from subsequent experiments.

[0078] In summary, Acnacidol BG and CLOCK-F, which contain weak acids, amino acids, and amino acid derivatives as main ingredients, were selected for subsequent investigation.

[0079] Table 2

[0080]

[0081] 3. Combination Ratio Optimization

[0082] The preparation method is the same as above, the reagent dosage (unit: g) and the results are shown in Table 3, and the photos are shown in Figure 4 .

[0083] Table 3

[0084]

[0085] From Table 3 and Figure 4 It can be seen that Acnacidol TM The addition of BG 3% and CLOCK-F 0.25% have a better solid-liquid ratio.

[0086] That is to say, the solid-liquid ratio of Acnacidol BG 3% and CLOCK-F 0.25% is the smallest, which is smaller than other ratios of Acnacidol BG and CLOCK-F, and smaller than the same ratios of Acnacidol BG and CLOCK-F, proving that Acnacidol BG 3% and CLOCK-F 0.25% have a synergistic effect.

[0087] Because zinc oxide and water are hydrated in the zinc oxide-water-ethanol dispersion, the surface charge of zinc oxide is dense, resulting in a high electrostatic effect. This results in optimal dispersion stability of the zinc oxide particles. Simultaneously, the system's viscosity is also high, making zinc oxide difficult to precipitate. Substances containing carboxyl and amino groups, such as amino acids and amino acid derivatives (in this application's experiments, 3% Acnacidol BG and 0.25% CLOCK-F), are composed of negatively charged carboxyl groups and molecules containing lone pairs of electrons (or π bonds). These molecules readily undergo physical and chemical adsorption to zinc oxide particles through van der Waals forces, ionic bonds, and hydrogen bonds, increasing the negative charge on the surface of the zinc oxide particles, lowering their zeta potential, and causing sedimentation.

[0088] 4. Verification of combination effect

[0089] The ability of the aminocarboxyl structure to promote sedimentation was further verified using the same preparation method as above. The results are shown in Table 4 (unit: g).

[0090] Table 4

[0091]

[0092] Pga-h80 is a complex composed of 86.7% water, 7.5% butylene glycol, 5% sodium polyglutamate, 0.72% phenoxyethanol, and 0.08% ethylhexylglycerin. It's manufactured by Taiwan VEDAN. GLDA-30 is tetrasodium glutamate diacetate.

[0093] As can be seen from Table 4, Acnacidol BG, composed of weak acids such as 10-hydroxydecanoic acid and sebacic acid and other raw materials, is a cosmetic raw material derived from royal jelly. It has carboxyl groups and weak acidity, which can bind to the surface of zinc oxide powder to improve the sedimentation effect, and is a priority component.

[0094] CLOCK-F, composed of amino acids and amino acid derivatives, has amino and carboxyl groups that can bind to the surface of zinc oxide powder to improve sedimentation and provide specific efficacy to the product. It is a priority component.

[0095] When salicylic acid is combined with CLOKC-F, CLOCK-F cannot improve the clumping effect of salicylic acid. Acnacidol BG itself has a carboxyl group, which also does not improve the clumping effect of salicylic acid.

[0096] The three raw materials in CLOCK-F (REVITALIN PF, CHRONOCYCLIN, and adenosine) were tested separately and all had little effect on the sedimentation of zinc oxide when used alone.

[0097] In addition, another experiment showed that EDTA-2NaCa

[0098] When mixed with CLOKC-F or Acnacidol BG respectively, neither CLOKC-F nor Acnacidol BG could improve the darkening of the system caused by EDTA-2NaCa.

[0099] Acnacidol BG was tested in combination with the raw materials GLDA-30, betaine, GSH, hydrolyzed royal jelly protein, citric acid, and PGA-H80, but no significant synergistic effect was found to increase zinc oxide precipitation.

[0100] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A powder phase-liquid phase double-layer product containing zinc oxide, characterized in that: comprising a composition comprising component I and component II; Component I includes the following raw materials: 1.8-2.4 parts by weight of 10-hydroxydecanoic acid; 1.8-2.4 parts by weight of 1,10-decanedioic acid; 1.0-1.5 parts by weight of 1,10-decanediol; 94-96 parts by weight of 1,3-butanediol; Component II comprises the following raw materials: 0.2-1.0 parts by weight of skin conditioning agent A, 0.2-2.0 parts by weight of skin conditioning agent B, and 0.1-2.0 parts by weight of adenosine; Wherein, the skin conditioning agent A comprises, by mass fraction, 1-5% yeast glycoprotein, 1-5% glutamic acid, 0.1-1% valine, 0.1-1% threonine, and the balance is water; Calculated by mass, the skin conditioning agent B comprises 1% of glutamylaminoethylimidazole and the balance is water; And, the liquid phase includes water and ethanol.

2. The powder phase-liquid phase double-layer product containing zinc oxide according to claim 1, characterized in that: Component I includes the following raw materials: 2.1 parts by weight of 10-hydroxydecanoic acid; 2.1 parts by weight of 1,10-decanedioic acid; 1.3 parts by weight of 1,10-decanediol; 94.5 parts by weight of 1,3-butanediol; The skin conditioning agent A used in component II comprises, by mass fraction, 3% yeast glycoprotein, 3% glutamic acid, 0.55% valine, 0.55% threonine, and the balance being water.

3. The powder phase-liquid phase double-layer product containing zinc oxide according to any one of claims 1-2, characterized in that: Skin conditioner A also includes 0.2-2% of a preservative and <0.1% of a stabilizer, sodium metabisulfite, wherein the preservatives are phenoxyethanol and ethylhexylglycerin, and the mass ratio of phenoxyethanol to ethylhexylglycerin is 1:1; Skin conditioner B further includes 0.4% of a preservative, wherein the preservatives are sorbic acid and phenoxyethanol, and the mass ratio of sorbic acid to phenoxyethanol is 1:

3.

4. The powder phase-liquid phase double-layer product containing zinc oxide according to any one of claims 1 to 3, characterized in that: The mass ratio of component I to component II is (1-4):(0.25-1.75).

5. The powder phase-liquid phase double-layer product containing zinc oxide according to claim 1, characterized in that: The amount of the composition added is 0.5-15% by mass.

Citation Information

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