Background
The water aqua has the advantages of moisturizing, nourishing, softening skin and the like, and is one of the common formulations of cosmetics. The common water aqua products are always transparent or semitransparent, the formula limitation is larger, the components dissolved in the water cannot be added, the appearance is single, and the requirements of consumers on novel appearance cannot be met. There are also double-layer water aqua on the market, the lower layer is water phase, the upper layer is oil phase, shake the use after even, the shortcoming is not contained emulsifying agent, and the two-phase layering speed is too fast, leads to the consumer in the use can very easily pour the oil phase on upper layer, experiences the sense not good.
There are also some water emulsion double-layer products on the market, chinese patent CN107929229B discloses a double-layer emulsion, wherein the emulsifier comprises inulin lauryl carbamate with the weight percentage of 0.1-1%, other components of 5-30% of oil phase, 0.3-10% of humectant and 0.01-0.2% of stabilizer. The bilayer emulsion of this application begins to delaminate for 5-30 minutes and completely delaminates for 60-17280 minutes. While the appearance is beautiful, spreadability is good, and skin feel is fresh, some of the examples add silicone oil components, some consumers now pursue natural components, and do not like to use cosmetics containing silicone oil. And the layering time of most embodiments is longer, and the requirements of consumers on the appearance of the product cannot be met.
Chinese patent CN105147528A discloses a water emulsion double-layer essence emulsion and a preparation method thereof, the double-layer essence emulsion has novel and beautiful appearance, can realize rapid layering, has stable emulsion property and good moisturizing performance. The double-layer essence emulsion comprises cyclopentadimethicone, ruba glue, isododecane, pentaerythritol tetra (ethyl caproate), butanediol, propylene glycol, glycereth-26, glycerol, oat beta-glucan, witch hazel water, phenyl trimethicone, phenoxyethanol, PEG-6 caprylic/capric glyceride, a thickener, caprylic glycol/ethylhexyl glycerol, methylparaben, butylhydroxytoluene, sodium hyaluronate, a pigment and water. The emulsifier used in the application is PEG-6 caprylic/capric glyceride, and the oil component contains two silicone oil components. PEG-6 caprylic/capric glycerides may have dioxane residues due to the PEG groups. Dioxane readily penetrates the skin and is considered by the U.S. environmental protection agency to be a possible human carcinogen. Thus, consumers dislike products that may contain dioxane.
The layered emulsions described in the above patents should be in the form of lotions, since the cosmetic emulsion national standard GB/T29665-2013 specifies that the appearance of the emulsion is not layered, and the cosmetic lotion national standard QB/T2660-2004 has a multi-layered appearance.
The double-layer water aqua on the market at present has the following problems: (1) The water-oil two-phase layering speed is too high, and only the upper oil phase is easily poured out in the use process, so that the experience is poor; (2) The components contain silicone oil or emulsifying agent containing PEG groups, so that consumers can resist the components; (3) The stabilizer or the thickener is added, the layering time is too long, and the appearance is bad; (4) Unstable properties, oil precipitation or thick emulsion on the surface, and no fineness.
Content of the application
The embodiment of the application provides a water emulsion double-layer aqueous solution agent which does not contain silicone oil, does not contain a thickening agent, has safe components, can be rapidly layered and has stable emulsion property and a preparation method thereof, so as to solve the problems in the related art, and the technical scheme is as follows:
in a first aspect, the embodiment of the application provides a water emulsion double-layer aqueous agent, which comprises the following components in percentage by weight: 60.9 to 96.19 percent of water, 0.1 to 2.5 percent of emulsifying agent, 3 to 15 percent of emollient, 0.3 to 10 percent of humectant, 0.3 to 10 percent of skin conditioning agent, 0.01 to 0.1 percent of pH regulator and 0.1 to 1.5 percent of preservative;
wherein the emulsifier comprises sodium bis (lauramide glutamine) lysine and wild soybean seed extract.
In one embodiment, the emollient comprises one or more of isohexadecane, squalane, hydrogenated polydecene, neopentyl glycol diheptanoate, ethylhexyl palmitate, C13-16 isoparaffin, tri (ethylhexanoate) glycerol, cetyl ethylhexanoate, isononyl isononanoate, mineral oil, prinsepia utilis oil, octyldodecanol, jojoba seed oil, grape seed oil, isopropyl myristate.
In one embodiment, the humectant comprises one or more of glycerin, butylene glycol, 1, 3-propanediol, betaine, dipropylene glycol, glycerin polyether-26, erythritol, methyl propylene glycol, hydroxyethyl urea, sodium polyglutamate, levan, trehalose.
In one embodiment, the skin conditioning agent comprises one or more of bisabolol, tocopherol, beta-glucan, nicotinamide, biogel-1, sodium polyaspartate, glyceroglycosides, dipotassium glycyrrhizinate, glutathione, matrine, corn gluten amino acids, purslane extract, carnosine, chitosan, aloe vera leaf juice.
In one embodiment, the pH adjuster comprises one or more of triethanolamine, potassium hydroxide, arginine, sodium hydroxide, citric acid, sodium citrate.
In one embodiment, the preservative comprises one or more of methylparaben, propylparaben, chlorophenylglycol, phenoxyethanol, ethylhexyl glycerol, hexamidine bis (isethionate), benzyl alcohol.
In one embodiment, the composition comprises the following: 0.1 to 0.3 percent of sodium di (lauramide glutamine) lysine, 0.2 to 0.6 percent of wild soybean seed extract, 2 to 4 percent of isohexadecane, 2 to 4 percent of squalane, 2 to 4 percent of C13-16 isoparaffin, 0.1 to 0.3 percent of tocopherol, 1 to 4 percent of butanediol, 2 to 4 percent of glycerol, 0.01 to 0.1 percent of sodium polyglutamate, 1 to 4 percent of purslane extract, 1 to 4 percent of beta-glucan, 1 to 3 percent of glyceroglycoside, 0.01 to 0.05 percent of arginine, 0.3 to 1.0 percent of phenoxyethanol, 0.1 to 0.5 percent of ethylhexyl glycerol and the balance of water.
In a second aspect, an embodiment of the present application provides a method for preparing a water emulsion bilayer aqua, which is used for preparing the water emulsion bilayer aqua, including:
(1) Sequentially mixing the phase A raw materials: adding water, butanediol, glycerol, sodium polyglutamate, sodium di (lauramide glutamine) lysine and wild soybean seed extract into an emulsifying pot, stirring, heating and preserving heat;
(2) B, raw materials of phase B: adding isohexadecane, squalane, C13-16 isoparaffin and tocopherol into an oil phase pot, stirring and mixing uniformly, and heating;
(3) Vacuumizing to suck the mixture in the step (2) into the mixture in the step (1), homogenizing, stirring, cooling and reducing the temperature;
(4) C phase raw materials: adding phenoxyethanol and ethylhexyl glycerol into an emulsifying pot, stirring and cooling;
(5) Sequentially mixing the phase D raw materials: adding beta-glucan, glyceroglycosides, purslane extract and arginine into an emulsifying pot, uniformly stirring, filtering and discharging after the inspection is qualified.
In one embodiment, the method comprises:
(1) Sequentially mixing the phase A raw materials: adding water, butanediol, glycerol, sodium polyglutamate, sodium di (lauramide glutamine) lysine and wild soybean seed extract into an emulsifying pot, stirring and heating to 80 ℃, and preserving heat for 20 minutes;
(2) B, raw materials of phase B: adding isohexadecane, squalane, C13-16 isoparaffin and tocopherol (vitamin E) into oil phase pot, stirring, mixing, and heating to 80deg.C;
(3) Vacuumizing to suck the mixture in the step (2) into the mixture in the step (1), homogenizing for 5-10 min, stirring and cooling to 60 ℃;
(4) C phase raw materials: adding phenoxyethanol and ethylhexyl glycerol into an emulsifying pot, stirring and cooling to below 45 ℃;
(5) Sequentially mixing the phase D raw materials: adding beta-glucan, glyceroglycosides, purslane extract and arginine into an emulsifying pot, uniformly stirring, filtering and discharging after the inspection is qualified.
In one embodiment, the method further comprises:
(6) Filling, packaging and code spraying;
(7) And (5) warehousing after the inspection is qualified.
The advantages or beneficial effects in the technical scheme at least comprise:
1. the application adopts the combination of sodium bis (lauramide glutamine) lysine and the wild soybean (Glycine SOJA) seed extract as the emulsifier, does not contain PEG group, and has good safety. The emulsion capability is strong, and the prepared water emulsion double-layer aqueous agent can still keep very good stability after standing for quite a long time without adding a thickening agent, and the quality problems of other similar products, such as oil separation on the upper layer, oil-water separation phenomenon, thick emulsion and the like, can not occur. Sodium lysine bis (lauramide glutamine) is of a double-chain structure, a double-layer arrangement structure is formed on the surface of emulsified particles, and the formed emulsified particle interfacial film is loose in structure and general in stability. After the wild soybean (Glycine SOJA) seed extract is added, the single-chain structure can lead molecules in a double-layer structure formed by sodium bis (lauramide glutamine) lysine to be polymerized and arranged, so that a more compact structure is formed, and the strength of an emulsion particle interface film is enhanced. Therefore, after the sodium bis (lauramide glutamine) lysine and the wild soybean (GLYCINE SOJA) seed extract are compounded, the prepared emulsified particles have smaller and more uniform particle size and good stability, and are obviously superior to the sodium bis (lauramide glutamine) lysine or the wild soybean (GLYCINE SOJA) seed extract which are singly used.
2. The application does not contain silicone oil component and can meet the personalized demands of consumers. By using C13-16 isoparaffin instead of silicone oil component, the smooth skin feeling similar to that of silicone oil is achieved on the premise of not containing silicone oil.
3. After the water emulsion double-layer aqua is uniformly shaken, the water emulsion double-layer aqua is left for about 3 minutes to start layering, and is completely divided into two layers about 15 minutes to realize rapid layering, wherein the upper layer is emulsion, the lower layer is aqua, the aqua part is in a semitransparent state temporarily, the layering interface is clear, and the lower layer is transparent and clear aqua about 12 hours. After the double-layer emulsion disclosed in Chinese patent CN107929229B is uniformly shaken, layering is started within 5-30 minutes, and the double-layer emulsion is completely layered within 60-17280 minutes, so that the layering time is too long, and the appearance of the product is affected.
4. The water emulsion double-layer water agent can be used for replacing toning lotion and emulsion, so that the skin care steps are reduced, the time is saved, and the current tension life rhythm is met. And various nourishing components such as beta-glucan, glyceroglycosides and purslane extract are added, so that the skin is healthier and plump and has high elasticity.
5. The formula system can be added with various water phase or oil phase active ingredients, has much higher flexibility than the conventional water agent products, and is suitable for being applied as various functional product matrixes.
6. All raw materials of the water emulsion double-layer water agent formula provided by the application have low component safety scores (higher represents larger risk) on the beauty repair APP, are green marks, and are a beauty repair full-green product. In recent years, many consumers can inquire the safety of cosmetics by using beautiful repair lines, and the beautiful repair lines have good safety of all-green products and can be used safely.
The foregoing summary is for the purpose of the specification only and is not intended to be limiting in any way. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features of the present application will become readily apparent by reference to the following detailed description.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in various different ways without departing from the spirit or scope of the present application. Accordingly, the description is to be regarded as illustrative in nature and not as restrictive.
In a first aspect, the embodiment of the application provides a water emulsion double-layer aqueous agent, which comprises the following components in percentage by weight: 60.9 to 96.19 percent of water, 0.1 to 2.5 percent of emulsifying agent, 3 to 15 percent of emollient, 0.3 to 10 percent of humectant, 0.3 to 10 percent of skin conditioning agent, 0.01 to 0.1 percent of pH regulator and 0.1 to 1.5 percent of preservative;
wherein the emulsifier comprises sodium bis (lauramide glutamine) lysine and Glycine max (Glycine max) extract.
Sodium bis (lauramide glutamine) lysine is commercially available under the name: PELLICER TM LB-10, 10% active, is a product of ASAHI KASEI FINECHEM CO., LTD. Sodium di (lauramide glutamine) lysine is an anionThe son double lock has surface activity, a plurality of hydrophobic groups and a plurality of hydrophilic groups, has super-strong emulsifying capacity, has skin care effect because the molecular structure is similar to that of ceramide, and can recover the skin barrier function.
The wild soybean (Glycine SOJA) seed extract is commercially available under the name: TXBIO SOYBEAN SEED EXTRACT the wild soybean seed extract has an active matter content of 20%, and is a product of Xingan Tianxing biotechnology Co. The wild soybean (Glycine SOJA) seed extract adopts low temperature formulation process, and is prepared from enzymolysis lecithin of non-transgenic soybean, with HLB value of 14.9, good hydrophilicity, good emulsifying property, mild skin, and no irritation.
In one embodiment, the emollient comprises one or more of isohexadecane, squalane, hydrogenated polydecene, neopentyl glycol diheptanoate, ethylhexyl palmitate, C13-16 isoparaffin, tri (ethylhexanoate) glycerol, cetyl ethylhexanoate, isononyl isononanoate, mineral oil, prinsepia utilis oil, octyldodecanol, jojoba seed oil, grape seed oil, isopropyl myristate.
In one embodiment, the humectant comprises one or more of glycerin, butylene glycol, 1, 3-propanediol, betaine, dipropylene glycol, glyceryl polyether-26, erythritol, methyl propylene glycol, hydroxyethyl urea, sodium polyglutamate, levan, trehalose.
In one embodiment, the skin conditioning agent comprises one or more of bisabolol, tocopherol (or vitamin E), beta-glucan, nicotinamide, biogel-1, sodium polyaspartate, glucosyl glycerogelatin, dipotassium glycyrrhizinate, glutathione, matrine, corn gluten amino acids, purslane extract, carnosine, chitosan amine, aloe vera leaf juice.
In one embodiment, the pH adjuster comprises one or more of triethanolamine, potassium hydroxide, arginine, sodium hydroxide, citric acid, sodium citrate.
In one embodiment, the preservative comprises one or more of methylparaben, propylparaben, chlorophenylglycol, phenoxyethanol, ethylhexyl glycerol, hexamidine bis (isethionate), benzyl alcohol.
In one embodiment, the composition comprises the following: 0.1 to 0.3 percent of sodium di (lauramide glutamine) lysine, 0.2 to 0.6 percent of wild soybean seed extract, 2 to 4 percent of isohexadecane, 2 to 4 percent of squalane, 2 to 4 percent of C13-16 isoparaffin, 0.1 to 0.3 percent of tocopherol, 1 to 4 percent of butanediol, 2 to 4 percent of glycerol, 0.01 to 0.1 percent of sodium polyglutamate, 1 to 4 percent of purslane extract, 1 to 4 percent of beta-glucan, 1 to 3 percent of glyceroglycoside, 0.01 to 0.05 percent of arginine, 0.3 to 1.0 percent of phenoxyethanol, 0.1 to 0.5 percent of ethylhexyl glycerol and the balance of water.
In a second aspect, an embodiment of the present application provides a method for preparing a water emulsion bilayer aqua, which is used for preparing a water emulsion bilayer aqua, including:
(1) Sequentially mixing the phase A raw materials: adding water, butanediol, glycerol, sodium polyglutamate, sodium di (lauramide glutamine) lysine and wild soybean seed extract into an emulsifying pot, stirring, heating and preserving heat;
(2) B, raw materials of phase B: adding isohexadecane, squalane, C13-16 isoparaffin and tocopherol into an oil phase pot, stirring and mixing uniformly, and heating;
(3) Vacuumizing to suck the mixture in the step (2) into the mixture in the step (1), homogenizing, stirring, cooling and reducing the temperature;
(4) C phase raw materials: adding phenoxyethanol and ethylhexyl glycerol into an emulsifying pot, stirring and cooling;
(5) Sequentially mixing the phase D raw materials: adding beta-glucan, glyceroglycosides, purslane extract and arginine into an emulsifying pot, uniformly stirring, filtering and discharging after the inspection is qualified.
In one embodiment, the method for preparing the aqueous emulsion bilayer aqua comprises the following steps:
(1) Sequentially mixing the phase A raw materials: adding water, butanediol, glycerol, sodium polyglutamate, sodium di (lauramide glutamine) lysine and wild soybean seed extract into emulsifying pot, stirring, heating to 80deg.C, and maintaining for 20 min.
(2) B, raw materials of phase B: adding isohexadecane, squalane, C13-16 isoparaffin and tocopherol (vitamin E) into oil phase pot, stirring, mixing, and heating to 80deg.C.
(3) Vacuumizing to suck the mixture in the step (2) into the mixture in the step (1), homogenizing for 5-10 min, stirring and cooling to 60 ℃.
(4) C phase raw materials: adding phenoxyethanol and ethylhexyl glycerol into an emulsifying pot, stirring and cooling to below 45 ℃.
(5) Sequentially mixing the phase D raw materials: adding beta-glucan, glyceroglycosides, purslane extract and arginine into an emulsifying pot, uniformly stirring, filtering and discharging after the inspection is qualified.
(6) Filling, packaging and code spraying.
(7) And (5) warehousing after the inspection is qualified.
Embodiments of the present application will be described in detail below with reference to examples 1 to 3 and comparative examples 1 to 3, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Examples 1-3 and comparative examples 1-3 provide a water emulsion double-layer aqua, and the raw material components are shown in table 1 in parts by weight:
table 1 example and comparative example preparation formulations
The preparation method comprises the following steps:
(1) Sequentially mixing the phase A raw materials: water, butylene glycol, glycerin, sodium polyglutamate, PELLICER TM Adding LB-10 and TXBIO SOYBEAN SEED EXTRACT into an emulsifying pot, stirring and heating to 80 ℃, and preserving heat for 20 minutes;
(2) B, raw materials of phase B: adding isohexadecane, squalane, C13-16 isoparaffin and tocopherol (vitamin E) into oil phase pot, stirring, mixing, and heating to 80deg.C;
(3) Vacuumizing to suck the mixture in the step (2) into the mixture in the step (1), homogenizing for 5-10 min, stirring and cooling to 60 ℃;
(4) C phase raw materials: adding phenoxyethanol and ethylhexyl glycerol into an emulsifying pot, stirring and cooling to below 45 ℃;
(5) Sequentially mixing the phase D raw materials: adding beta-glucan, glyceroglycosides, purslane extract and arginine into an emulsifying pot, uniformly stirring, filtering and discharging after the inspection is qualified;
(6) After the inspection is qualified, filling, packaging and code spraying are carried out;
(7) And (5) warehousing after the inspection is qualified.
Test example one, physical and chemical index detection
And according to QB/T2660, performing physical and chemical index test on the prepared water emulsion double-layer water aqua. The results are shown in Table 2 below:
TABLE 2 physical and chemical indicator detection results
Test example two, application Performance detection
(1) Safety of raw materials
All raw materials of the water emulsion double-layer water agent formula of the application have low component safety scores on the beautiful repair APP, are all green marks, and are beautiful repair full-green products. The safety score of the formulation of the application in the beauty repair app ingredient is shown in table 3:
TABLE 3 safety score for the formulation of the present application in beauty repair app ingredients
(2) Product safety test:
the skin care compositions prepared in examples and comparative examples were subjected to a body patch test according to the method described in cosmetic safety Specification (2015 edition).
Experimental population: 30 persons total, 30 women, 6 men, age 21-59, 5 persons per group, meet the subject's volunteer inclusion criteria.
The testing method comprises the following steps: the selected area is not more than 50mm 2 A proper patch tester with the depth of about 1mm is provided, and about 0.020 ml to 0.025ml of a test object is added into the patch tester by a closed patch test method; the patch tester is applied to the forearm of a subject, the test object is removed after 24 hours, skin reactions are observed after 0.5 hour, 24 hours and 48 hours respectively, and the results are recorded according to the skin reaction grading standard in cosmetic safety technical Specification (2015 edition).
Test results: the score scale of 0 score (negative response) was 0 at 3 observation time points of 0.5h, 24h, 48h after patch removal of 30 subjects.
(3) Product layering speed test:
the products of the examples and the comparative examples are respectively contained in a scale bottle of 100ml, and after the two phases are completely mixed with the same stirring speed and stirring time, the time required for delamination again is observed by standing, and the setting of the observation time is tested: the first 15 minutes, every 10 seconds is an observation period, the first half hour, every 1 minute is an observation period, after standing for half an hour, the first half hour is a test observation period, the second half hour is a test observation period, and the third half hour is a test observation period, the fourth half hour is a test observation period, and the fourth half hour is a test observation period; a test observation period of every 4 hours from 12 hours to 48 hours; after 48 hours, one test observation period is every 24 hours. Retention of test data: the last bit is an integer multiple of 5. The test results are shown in Table 4.
Table 4 layering speed test results
As can be seen from table 4, the double-layer essence water in examples 1 to 3 starts to be layered in about 3 minutes, and is completely layered in about 20 minutes, the layered interface is clear, the upper layer is emulsion, the lower layer is aqueous solution, and the aqueous solution is temporarily semitransparent. About 12 hours, the lower water agent becomes transparent; the double-layer essence water in comparative examples 1 and 2 starts layering in about 50 seconds, and completely layering in about 7 minutes, so that the layering interface is clear, the upper layer is emulsion, the lower layer is water aqua, and the water aqua is in a semitransparent state temporarily. About 7 hours, the lower water agent becomes transparent; comparative example 3 was an oil-water two-phase system without an emulsifier, and was layered within 10 seconds, and the delamination was completed in 5 minutes.
Examples are the addition of sodium di (lauramide glutamine) lysine and wild soybean (GLYCINE SOJA) seed extract in varying proportions; comparative example 1 with only wild soybean (GLYCINE SOJA) seed extract, comparative example 2 with only sodium bis (lauramide glutamine) lysine, and comparative example 3 with a blank control. As shown in table 4, from the test results, it can be seen that: the bilayer water agent prepared in comparative examples 1-3 had a high layering speed, and may already delaminate when poured out after shaking, which would result in only pouring out the upper layer of liquid, and the use experience was poor. The bilayer water aqua prepared in the embodiment 1-3 has moderate layering speed, and the bilayer water aqua has good uniformity of materials and good use experience when poured out after shaking uniformly. The synergistic effect of the sodium bis (lauramide glutamine) lysine and the wild soybean (Glycine SOJA) seed extract product is obvious, the emulsifying capacity is stronger, and the prepared double-layer water aqua has moderate layering speed and good stability. Is obviously better than the single use of sodium bis (lauramide glutamine) lysine or wild soybean (GLYCINE SOJA) seed extract.
It should be understood that the numerical values disclosed in the embodiments of the present application are approximate values, not determined. Where the error or experimental conditions allow, all values within the error range may be included without limiting the specific values disclosed in the embodiments of the present application.
The numerical ranges disclosed in the examples of the present application are intended to represent relative amounts of the components in the mixture, as well as ranges of temperatures or other parameters recited in the examples of other methods.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The foregoing is merely illustrative of the present application, and the present application is not limited thereto, and any person skilled in the art will readily recognize that various modifications and substitutions are possible within the scope of the present application. Therefore, the protection scope of the application is subject to the protection scope of the claims.