Oil bead composition for moistening and repairing skin and preparation method thereof

Abstract

The invention relates to an oil bead composition for moistening and repairing skin and a preparation method thereof. The oil bead composition comprises the following components: a phase A: water, a humectant 1, a thickener, a chelating agent, an emulsifier 1 and a preservative 1; phase B: alkali; the phase C comprises a humectant and a preservative 2; phase D: emulsifier 2 and essence; phase E: modified oil beads; wherein the modified oil bead has a core-shell structure, the shell structure is an acrylate cross-linked polymer, and the core structure comprises a humectant 3, an emulsifier 3 and a preservative 3; the acrylate cross-linked polymer is obtained by carrying out esterification reaction on polylactic acid modified chitosan and acrylic acid and then carrying out free radical polymerization on the polylactic acid modified chitosan, acrylic acid and acrylate. The stability of the oil bead composition is improved, absorption and effectiveness of effective components can be promoted, good skin moistening and repairing effects are achieved, a certain slow release function is achieved, the effective time of a product can be prolonged, and the problems existing in the prior art are solved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of skin care, in particular to an oil bead composition for moisturizing and repairing skin and a preparation method thereof. BACKGROUND

[0002] The oil bead essence is a new type of essence product, which has a unique microcapsule wrapping function compared with ordinary skin care essence. It can also separate and store water-soluble and oil-soluble active ingredients, and release them when used, which not only ensures the stability of high active ingredients, but also avoids the degradation of ingredients caused by long-term mixing of ordinary essence. In terms of skin feel, the oil bead essence can meet the moisturizing needs of dry skin by adjusting the water-oil ratio, and will not make oily skin feel heavy. At the same time, the oil component can soften the stratum corneum and promote the absorption of water-soluble components, thereby improving the penetration efficiency. In addition, the oil bead essence can be used to adjust the water-oil ratio according to the season or skin quality to achieve customized care, and the rapid moisturizing effect is more prominent.

[0003] However, the existing oil bead essence has the problem of unstable emulsion system after long-term storage, which leads to obvious stratification of water and oil phases. This instability directly affects the use effect: when the lipophilic component is preferentially absorbed by the skin, the penetration efficiency of the hydrophilic component will be greatly reduced. Because the water-soluble active substance cannot effectively penetrate the stratum corneum, a large amount of unabsorbed active ingredient will remain on the skin surface and gradually volatilize, which not only weakens the immediate moisturizing ability of the product, but also affects the long-term moisturizing and repairing function, significantly restricting the effect of the product, and needs to be improved.

[0004] Therefore, it is urgent to develop a new technical solution to solve the problems existing in the prior art. SUMMARY

[0005] Therefore, the present application provides an oil bead composition for moisturizing and repairing skin and a preparation method thereof. The modified oil bead obtained by compounding specific acrylate cross-linked polymer, humectant and other substances not only improves the stability of the composition, promotes the absorption and effect of active ingredients, realizes good moisturizing and repairing effect of the skin, but also has a certain slow-release function, which is beneficial to prolong the effective time of the product and overcomes the problems existing in the prior art.

[0006] One object of the present application is to provide an oil bead composition for moisturizing and repairing skin, which comprises the following components in mass fraction:

[0007] A phase:

[0008]

[0009]

[0010] B phase:

[0011] alkali 0.1-0.5 parts

[0012] C phase:

[0013] moisturizer 2 1-4 parts

[0014] preservative 2 0.01-0.1 parts

[0015] D phase:

[0016] emulsifier 2 0.01-0.05 parts

[0017] fragrance 0.001-0.01 parts

[0018] E phase:

[0019] modified oil beads 20-25 parts;

[0020] The modified oil beads have a core-shell structure, the shell structure is an acrylate cross-linked polymer, and the core structure includes moisturizer 3, emulsifier 3 and preservative 3.

[0021] The acrylate cross-linked polymer is polylactic acid modified chitosan, which is subjected to esterification with acrylic acid and then subjected to free radical polymerization with acrylic acid and acrylate.

[0022] Further, the mass ratio of the acrylate cross-linked polymer, moisturizer 3, emulsifier 3 and preservative 3 is (4-10):(3-10):(3-10):(0.01-0.1).

[0023] Further, the moisturizer 1, moisturizer 2 and moisturizer 3 are selected from one or more of glycerol, glycerol polyether, sodium hyaluronate, panthenol, butanediol, sorbitol and hexanediol.

[0024] Further, the thickening agent is selected from one or more of carbomer, xanthan gum and starch derivatives.

[0025] Further, the emulsifier 1, emulsifier 2 and emulsifier 3 are selected from one or more of PPG / PEG copolymer, PEG-40 castor oil, glyceryl tri(ethylhexanoate) and caprylic / capric triglyceride.

[0026] Further, the preservative 1, preservative 2 and preservative 3 are selected from one or more of p-hydroxyacetophenone and caprylhydroxamic acid.

[0027] Further, the chelating agent is EDTA-disodium.

[0028] Further, the core structure further comprises an active ingredient selected from one or more of retinol, astaxanthin, guaiazulene, comfrey extract, and giant kelp extract.

[0029] Another object of the present application is to provide a preparation method of the above-mentioned skin-moisturizing and repairing oil bead composition, which comprises the following steps:

[0030] S1, blending polylactic acid, an activating agent, and carboxymethyl chitosan, and stirring and reacting to obtain an intermediate product 1;

[0031] S2, blending the intermediate product 1, acrylic acid, a catalyst, and a polymerization inhibitor, and heating to react to obtain an intermediate product 2;

[0032] S3, blending the intermediate product 2, acrylic acid, an acrylic ester, and an initiator, and heating to react under inert gas protection to obtain an acrylic ester crosslinked polymer;

[0033] S4, blending the acrylic ester crosslinked polymer, a humectant 3, an emulsifier 3, and a preservative 3 to obtain a modified oil bead, i.e., an E phase;

[0034] S5, heating and mixing the A phase, the B phase, and the C phase, and then adding the D phase and the E phase to obtain the skin-moisturizing and repairing oil bead composition.

[0035] Further, the mass ratio of the polylactic acid and the carboxymethyl chitosan is (1-3):5.

[0036] Further, the mass ratio of the intermediate product 1 and the acrylic acid is 5:(0.5-4).

[0037] Further, the mass ratio of the intermediate product 2, the acrylic acid, and the acrylic ester is (1-3):(1-3):(3-6).

[0038] Further, the acrylic ester is selected from C10-30 alkyl acrylate.

[0039] Further, the activating agent is EDC (1-ethyl-3-(3-dimethylaminopropyl) carbodiimide) and NHS (N-hydroxysuccinimide).

[0040] The present application has the following beneficial effects:

[0041] The oil bead composition for moisturizing and repairing skin of the present application contains modified oil beads obtained by compounding a specific acrylate cross-linked polymer and a humectant, an emulsifier and the like, wherein the acrylate cross-linked polymer is obtained by first reacting chitosan with polylactic acid through the amino functional group to obtain intermediate product 1, then esterifying the intermediate product 2 through the hydroxyl group and acrylic acid, and finally polymerizing with acrylic acid and acrylate to obtain the cross-linked polymer. The acrylate cross-linked polymer of the present application serves as the shell layer of the oil bead, and the chitosan introduced therein has good affinity with active ingredients such as retinol, astaxanthin and polysaccharides in plant extracts and the like, and the long chain of polylactic acid further plays a role of winding and cross-linking, so as to fully coat the active ingredients; and after the polylactic acid grafted chitosan is polymerized with the hydrophilic acrylic acid and the hydrophobic acrylate alkyl ester, the obtained product has excellent film-forming property and emulsifying property, and after being combined with the active ingredients and the humectant and the emulsifier, stable oil bead particles can be formed, which are persistently dispersed in the aqueous system of the composition, so as to ensure the effectiveness after long-term storage, reduce the possibility of precipitation and stratification of the oil phase and the water phase components, and endow the product with better appearance and use experience. Moreover, after the oil bead microparticles of the present application contact the skin, the contents can be continuously and controllably released, and also have a certain sustained-release effect, so that the active substances and oily and aqueous components can be fully absorbed by the skin, thereby realizing the simultaneous performance of barrier repair and deep moisturizing, improving the use effect of the product, and overcoming the problems in the prior art. DETAILED DESCRIPTION

[0042] In order to more clearly illustrate the technical solutions of the present application, the following examples are listed. The raw materials, reactions and post-treatment means appearing in the examples are all common raw materials on the market and technical means well known to those skilled in the art, unless otherwise stated.

[0043] The words "preferred", "preferably", "more preferred" and the like in the present application refer to the embodiments of the present application which can provide certain beneficial effects in certain cases. However, other embodiments can also be preferred in the same or other cases. In addition, the description of one or more preferred embodiments does not imply that other embodiments are not usable, nor is it intended to exclude other embodiments from the scope of the present application.

[0044] It should be understood that, except in any operating examples, or otherwise indicated, expressions of amount or all numbers in the specification and claims, such as, for example, amounts of ingredients, are understood as being modified by the term "about". Therefore, unless otherwise indicated, the numerical parameters set forth in the following description and attached claims are approximations that can vary depending on the desired properties sought to be obtained by the present application.

[0045] The concentration of the sodium hydroxide solution in the embodiments of the present application is 10wt%.

[0046] The sodium polyacrylate grafted starch in the embodiment of the present application is MAKIMOUSSE 25.

[0047] The PEG / PPG-17 / 6 copolymer in the embodiment of the present application is purchased from Haian Petrochemical in Jiangsu Province.

[0048] The PEG-40 castor oil in the embodiment of the present application is purchased from BASF, and the model number is CO-40.

[0049] The comfrey extract in the embodiment of the present application is comfrey essential oil, which is purchased from Henan Qianshengtang Pharmaceutical Co., Ltd.

[0050] The “parts” in the embodiment of the present application all refer to mass parts.

[0051] Example 1

[0052] A skin-moisturizing and repairing oil bead composition, comprising the following components in mass parts:

[0053] Phase A:

[0054]

[0055] Phase B:

[0056] Sodium hydroxide solution 0.25 parts

[0057] Phase C:

[0058] Butylene glycol 2 parts

[0059] Caprylhydroxamic acid 0.06 parts

[0060] Phase D:

[0061] PEG-40 castor oil 0.02 parts

[0062] Fragrance 0.005 parts

[0063] Phase E:

[0064] Acrylate crosspolymer 9.35 parts

[0065] Retinol 0.6 parts

[0066] Sorbitol 3 parts

[0067] 1,2-Hexanediol 3 parts

[0068] Glyceryl triethylhexanoate 4 parts

[0069] p-Hydroxyacetophenone 0.05 parts

[0070] The preparation method of the skin-moisturizing and repairing oil bead composition comprises the following steps:

[0071] S0, mixing D, L-lactide and zinc lactate with a mass ratio of 10:0.01 in water as a solvent, reacting for 72 h at 180°C in a nitrogen environment, then dissolving the product in dichloromethane, then adding anhydrous ether for precipitation, and drying after filtration to obtain polylactic acid with a hydroxyl end group;

[0072] S1, mixing polylactic acid, EDC and NHS in dimethyl sulfoxide as a solvent, stirring and reacting for 3 h to obtain a polylactic acid solution;

[0073] adding carboxymethyl chitosan in water as a solvent, dissolving, then continuously stirring to add the polylactic acid solution, reacting for 12 h, then extracting with dichloromethane, then adding ice ethanol for precipitation, and drying after filtration to obtain intermediate product 1;

[0074] The mass ratio of the polylactic acid, EDC, NHS and carboxymethyl chitosan is 1.5:0.6:0.36:5;

[0075] S2, blending intermediate product 1, acrylic acid, p-toluenesulfonic acid and hydroquinone with a mass ratio of 5:1:0.01:0.01 in toluene as a solvent, heating at 80°C for 6 h, then removing the solvent to obtain intermediate product 2;

[0076] S3, blending intermediate product 2, acrylic acid, decyl acrylate and potassium persulfate with a mass ratio of 2:1:3:0.03 in water as a solvent, heating at 90°C for 5 h in a nitrogen environment, then removing the solvent to obtain an acrylate crosslinked polymer;

[0077] S4, blending and stirring the acrylate crosslinked polymer, humectant 3, emulsifier 3 and preservative 3 in the above mass proportions to obtain modified oil beads, i.e. phase E;

[0078] S5, blending the components of phase A in the above mass proportions, stirring uniformly at 85°C, then cooling to 60°C, adding the blended phase B and phase C, stirring uniformly, then cooling to 40°C, adding the blended phase D and phase E, and stirring uniformly to obtain the oil bead composition for moisturizing and repairing the skin.

[0079] Example 2

[0080] An oil bead composition for moisturizing and repairing the skin, the oil bead composition for moisturizing and repairing the skin comprising components in the following mass proportions:

[0081] Phase A:

[0082]

[0083] Phase B:

[0084] Sodium hydroxide solution 0.25 parts

[0085] C phase:

[0086] Butanediol 2 parts

[0087] Octanohydroxamic acid 0.06 parts

[0088] D phase:

[0089] PEG-40 castor oil 0.02 parts

[0090] Fragrance 0.005 parts

[0091] E phase:

[0092]

[0093]

[0094] The method for preparing the skin-moisturizing and repairing oil bead composition comprises the following steps:

[0095] S0, mixing D, L-lactide and zinc lactate in a mass ratio of 10:0.01 with water as a solvent, reacting at 180°C for 72h in a nitrogen environment, then dissolving the product in dichloromethane, adding anhydrous ether for precipitation, filtering and drying to obtain polylactic acid with a hydroxyl end group;

[0096] S1, mixing polylactic acid, EDC and NHS with dimethyl sulfoxide as a solvent, stirring and reacting for 3h to obtain a polylactic acid solution;

[0097] With water as a solvent, carboxymethyl chitosan is stirred and added, after dissolution, the polylactic acid solution is continuously stirred and added, and reacts for 12h, then extracted with dichloromethane, and precipitated by adding ice ether, and after filtering and drying, an intermediate product 1 is obtained;

[0098] The mass ratio of the polylactic acid, EDC, NHS and carboxymethyl chitosan is 1.5:0.6:0.36:5;

[0099] S2, blending the intermediate product 1, acrylic acid, p-toluenesulfonic acid and hydroquinone in a mass ratio of 5:1:0.01:0.01 with toluene as a solvent, heating at 80°C for 6h, and then removing the solvent to obtain an intermediate product 2;

[0100] S3, blending the intermediate product 2, acrylic acid, decyl acrylate and potassium persulfate in a mass ratio of 2:1:3:0.03 with water as a solvent, heating at 90°C for 5h in a nitrogen environment, and then removing the solvent to obtain an acrylate crosslinked polymer;

[0101] S4, blend and stir the acrylate cross-linked polymer, humectant 3, emulsifier 3 and preservative 3 according to the above mass fractions to obtain a modified oil bead, i.e. phase E;

[0102] S5, mix the components of phase A, stir uniformly at 85°C, then cool to 60°C, add the mixed phases B and C, stir uniformly, then cool to 40°C, add the mixed phases D and E, stir uniformly to obtain the oil bead composition for moisturizing and repairing skin.

[0103] Example 3

[0104] An oil bead composition for moisturizing and repairing skin, comprising the following components in mass fractions:

[0105] Phase A:

[0106]

[0107]

[0108] Phase B:

[0109] Sodium hydroxide solution 0.25 parts

[0110] Phase C:

[0111] Butanediol 2 parts

[0112] Caprylhydroxamic acid 0.06 parts

[0113] Phase D:

[0114] PEG-40 castor oil 0.02 parts

[0115] Essence 0.005 parts

[0116] Phase E:

[0117]

[0118] The preparation method of the oil bead composition for moisturizing and repairing skin comprises the following steps:

[0119] S0, mix D, L-lactide and zinc lactate in a mass ratio of 10:0.01 with water as the solvent, react at 180°C for 72h in a nitrogen environment, then dissolve the product in dichloromethane, then add anhydrous ether for precipitation, filter and dry to obtain polylactic acid with a hydroxyl end group;

[0120] S1, mix polylactic acid, EDC and NHS with dimethyl sulfoxide as the solvent, stir and react for 3h to obtain a polylactic acid solution;

[0121] The intermediate product 1 is obtained by dissolving carboxymethyl chitosan in water, stirring and adding the polylactic acid solution, reacting for 12 hours, extracting with dichloromethane, and then precipitating with ethyl ether, and then filtering and drying.

[0122] The mass ratio of the polylactic acid, EDC, NHS and carboxymethyl chitosan is 1.5:0.6:0.36:5.

[0123] S2, the intermediate product 1, acrylic acid, p-toluenesulfonic acid and hydroquinone are blended in a mass ratio of 5:1:0.01:0.01, heated at 80°C for 6 hours, and then the solvent is removed to obtain the intermediate product 2.

[0124] S3, the intermediate product 2, acrylic acid, decyl acrylate and potassium persulfate are blended in a mass ratio of 2:1:3:0.03, heated at 90°C for 5 hours under nitrogen, and then the solvent is removed to obtain the acrylate cross-linked polymer.

[0125] S4, the acrylate cross-linked polymer, humectant 3, emulsifier 3 and preservative 3 are blended in the above mass ratio, and then stirred uniformly to obtain the modified oil beads, i.e. the E phase.

[0126] S5, the components of the A phase are mixed, stirred uniformly at 85°C, then cooled to 60°C, the mixed B phase and C phase are added, stirred uniformly, then cooled to 40°C, the mixed D phase and E phase are added, and then stirred uniformly to obtain the oil bead composition for moisturizing and repairing skin.

[0127] Based on Example 1, Comparative Examples 1-2 are set.

[0128] Comparative Example 1 differs from Example 1 in that step S1-2 is deleted, and in step S3, the intermediate product 2 is replaced by acrylic acid, and the other components and preparation methods are the same as those of Example 1.

[0129] Comparative Example 2 differs from Example 1 in that step S1-2 is deleted, and in step S3, the intermediate product 2 is replaced by decyl acrylate, and the other components and preparation methods are the same as those of Example 1.

[0130] Test Example

[0131] The oil bead compositions for moisturizing and repairing skin prepared in Examples 1-3 and Comparative Examples 1-2 are tested for performance.

[0132] Test Method:

[0133] Stability Test: The samples prepared in Examples and Comparative Examples are sealed in containers and placed at 40°C for 60 days, and then observed for precipitation and stratification after returning to room temperature.

[0134] Moisturizing test: 25-35 year-old female volunteers were selected, 25 in total, and divided into 5 groups, 5 in each group, and each group was applied with the sample prepared in the example or the comparative example. Each person applied 2 g of the composition on the face after cleaning, and rubbed for 1 min for absorption. The skin water content before application, 1 h after application, and 6 h after application was detected, and the average value of each group was calculated. During the test, each volunteer was kept in a room with constant temperature and humidity.

[0135] Repair test: 25-35 year-old female volunteers were selected, 50 in total, and divided into 5 groups, 10 in each group, and each group was applied with the sample prepared in the example or the comparative example, 2 g of the composition was applied on the face in the morning and evening, and rubbed for 1 min for absorption, for 30 days. Each person scored the effect of improving fine lines on the skin, with a score of 1-10, and 10 was the best, and the average value of each group was calculated.

[0136] The test results are shown in Table 1.

[0137] Table 1 Performance test results

[0138]

[0139] According to Table 1, it can be concluded that the oil bead composition prepared in Examples 1-3 of the present application has good stability, maintains good dispersion and uniformity after long-term high-temperature placement, and has excellent skin care effect, long-acting time, and strong moisturizing and repairing effect. The oil beads of Comparative Examples 1-2, which replace the ingredients, are difficult to exist persistently and stably in the aqueous system, resulting in reduced stability of the composition, relatively short maintenance time of active ingredients and emollient ingredients after use, and different degrees of decline in moisturizing and repairing effect, and the performance is not ideal.

[0140] It is apparent to those skilled in the art that the present application is not limited to the details of the foregoing exemplary embodiments, and the present application can be implemented in other specific forms without departing from the spirit or essential characteristics of the present application. Therefore, the embodiments should be considered in all respects as illustrative and not restrictive, and the scope of the present application is defined by the appended claims rather than the foregoing description, and all changes falling within the meaning and range of equivalents of the claims are intended to be encompassed by the present application.

[0141] In addition, it should be understood that although the present specification is described in terms of embodiments, not every embodiment contains only one independent technical solution, and the description of the specification is only for the sake of clarity, and those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can be appropriately combined to form other embodiments that those skilled in the art can understand.

Claims

1. An oil droplet composition for moisturizing and repairing the skin, characterized in that: The oil droplet composition for moisturizing and repairing the skin comprises the following components in parts by mass: Phase A: Phase B: 0.1-0.5 parts of alkali Phase C: Moisturizer 2 1-4 parts Preservative 2 0.01-0.1 parts Phase D: Emulsifier 2 0.01-0.05 parts 0.001-0.01 parts of flavor Phase E: 20-25 parts of modified oil beads; The modified oil droplets have a core-shell structure, the shell structure is an acrylic acid ester cross-linked polymer, and the core structure includes a moisturizer 3, an emulsifier 3 and a preservative 3; The acrylate cross-linked polymer is chitosan modified with polylactic acid, which is obtained by esterification with acrylic acid and then free radical polymerization with acrylic acid and acrylate.

2. The oil droplet composition for moisturizing and repairing the skin according to claim 1, characterized in that: The moisturizing agent 1, moisturizing agent 2 and moisturizing agent 3 are selected from one or more of glycerin, glycerol polyether, sodium hyaluronate, panthenol, butylene glycol, sorbitol and hexylene glycol.

3. The oil droplet composition for moisturizing and repairing skin according to claim 1, characterized in that: The thickener is selected from one or more of carbomer, xanthan gum, and starch derivatives.

4. The oil droplet composition for moisturizing and repairing skin according to claim 1, characterized in that: The emulsifier 1, emulsifier 2 and emulsifier 3 are selected from one or more of PPG / PEG copolymer, PEG-40 castor oil, triethylhexanoin and caprylic / capric triglyceride.

5. The oil droplet composition for moisturizing and repairing skin according to claim 1, characterized in that: The preservative 1, preservative 2 and preservative 3 are selected from one or more of p-hydroxyacetophenone and octanoylhydroxamic acid.

6. The oil droplet composition for moisturizing and repairing the skin according to claim 1, characterized in that: The core structure further comprises an active ingredient, which is selected from one or more of retinol, astaxanthin, guaiaczul, lithospermum officinale extract, and giant kelp extract.

7. The method for preparing the oil droplet composition for moisturizing and repairing the skin according to any one of claims 1 to 6, characterized in that: The preparation method of the oil droplet composition for moisturizing and repairing the skin comprises the following steps: S1, blending polylactic acid, an activator and carboxymethyl chitosan, stirring and reacting to obtain an intermediate product 1; S2, mixing the intermediate product 1, acrylic acid, a catalyst and a polymerization inhibitor, and heating the mixture for reaction to obtain an intermediate product 2; S3, blending the intermediate product 2, acrylic acid, acrylic ester and an initiator, and heating the mixture under inert gas protection to obtain an acrylic ester cross-linked polymer; S4, blending the acrylic acid ester cross-linked polymer, moisturizer 3, emulsifier 3 and preservative 3 to obtain modified oil droplets, i.e., phase E; S5. Heat and mix phase A, phase B, and phase C, stir, and then add phase D and the phase E to obtain the oil droplet composition for moisturizing and repairing the skin.

8. The method for preparing the oil droplet composition for moisturizing and repairing the skin according to claim 7, characterized in that: The mass ratio of the polylactic acid to carboxymethyl chitosan is (1-3):

5.

9. The method for preparing the oil droplet composition for moisturizing and repairing the skin according to claim 7, characterized in that: The mass ratio of the intermediate product 1 to acrylic acid is 5:(0.5-4).

10. The method for preparing the oil droplet composition for moisturizing and repairing the skin according to claim 7, characterized in that: The mass ratio of the intermediate product 2, acrylic acid, and acrylic ester is (1-3):(1-3):(3-6).

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