CN114948796B - Cosmetic composition - Google Patents

Cosmetic composition Download PDF

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CN114948796B
CN114948796B CN202210629915.3A CN202210629915A CN114948796B CN 114948796 B CN114948796 B CN 114948796B CN 202210629915 A CN202210629915 A CN 202210629915A CN 114948796 B CN114948796 B CN 114948796B
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silicone oil
weight
containing silicone
shellac resin
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CN114948796A (en
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陈琛
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Shanghai John Jeff Cosmetics Co ltd
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Shanghai John Jeff Cosmetics Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/896Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/368Carboxylic acids; Salts or anhydrides thereof with carboxyl groups directly bound to carbon atoms of aromatic rings
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55Phosphorus compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/676Ascorbic acid, i.e. vitamin C
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/927Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of insects, e.g. shellac
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention belongs to the technical field of cosmetics, and particularly relates to a composition for cosmetics. The composition consists of modified hydrogen-containing silicone oil, shellac resin, microcrystalline wax, glycerin fatty acid ester, sodium carboxymethyl cellulose, fructose, p-aminobenzoic acid, ascorbic acid, salicylic acid, humectant and solvent, and the prepared cosmetic has better stability, lasting moisturizing effect and good skin-friendly property by grafting 2-methacryloyloxyethyl phosphorylcholine onto the hydrogen-containing silicone oil and matching with the shellac resin.

Description

Cosmetic composition
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a composition for cosmetics.
Background
In recent years, there have been various demands for cosmetic products, and the cosmetic products have been widely divided into various forms, such as lipstick, foundation, cosmetic powder, nail polish, and the like, by adding elements in the forms of liquid, powder, solid, emulsion, and the like, in addition to the forms of further divided forms. Meanwhile, the cosmetics are distributed and stored until all consumers use up, and a long period of time is needed, and the shelf life of the cosmetics is generally 2-3 years. Due to different conditions of placement, delamination is likely to occur after long-term placement, and phase separation is eventually generated, thereby requiring good stability of the cosmetic.
The Chinese patent with application number 2016105953718 discloses a cosmetic with pore-refining effect and a preparation method thereof, wherein the cosmetic is prepared from witch hazel extract, N-methyl-beta-aminopropionic acid, hydrolyzed collagen, lecithin, cholesterol, tween, preservative and PBS buffer solution, and the cosmetic has the effects of refining pores, astringing and resisting bacteria by the synergistic compatibility of the compound, can quickly permeate into skin, and can comprehensively regulate the skin from inside to outside.
The Chinese patent with application number 2018107535015 discloses an antipollution cosmetic composition and cosmetics applied by the same, which are composed of skin protection factors, skin detoxification factors, energy supplementing factors, polyalcohol and water, can effectively protect skin against physical and chemical attack, and also has the effects of expelling toxins and supplementing energy.
However, the stability of the related cosmetics is not examined in the above prior art.
Disclosure of Invention
In order to solve the problems, the invention prepares a cosmetic composition which has better stability, lasting moisturizing effect and good skin-friendly property.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the cosmetic composition is prepared from the following raw materials in parts by weight: 8-12 parts of modified hydrogen-containing silicone oil, 6-8 parts of shellac resin, 12-15 parts of microcrystalline wax, 5-8 parts of glycerin fatty acid ester, 8-12 parts of sodium carboxymethyl cellulose, 5-8 parts of fructose, 3-6 parts of p-aminobenzoic acid, 2-5 parts of ascorbic acid, 2-4 parts of salicylic acid, 10-15 parts of humectant and 45-56 parts of solvent;
the modified hydrogen-containing silicone oil is prepared by grafting 2-methacryloyloxyethyl phosphorylcholine onto hydrogen-containing silicone oil, and has the structural formula:
Figure GDA0003767875150000021
/>
wherein R is C a H 2a+1 ,a=2-17。
The invention has the following beneficial effects:
1. the carboxyl in the shellac structure is effectively inhibited from undergoing esterification reaction in high-temperature preservation by adopting N-methyldiethanolamine to neutralize the carboxyl, so that the shellac structure can maintain good performance at high temperature;
2. the 2-methacryloyloxyethyl phosphorylcholine is grafted to the hydrogen-containing silicone oil, the existence of long-chain alkyl in the hydrogen-containing silicone oil increases the affinity with skin, and meanwhile, the long-chain alkyl and a silicone oil molecular chain are mutually combined to form a network structure, so that the hydrogen-containing silicone oil has better ductility;
3. the mesh structure formed by the modified hydrogen-containing silicone oil is matched with the elastic mesh provided in the shellac resin, so that the stability of the prepared cosmetic is further improved;
4. the existence of the 2-methacryloyloxyethyl phosphorylcholine in the cosmetics can improve the stability of the cosmetics and simultaneously has better skin-friendly property, so that the prepared cosmetics can uniformly cover and protect the skin at the coating position, and can keep better moisturizing effect for a long time.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be made clearly and completely in connection with the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The hydrogen-containing silicone oil used in the invention is purchased from Ji nan nation chemical industry Co., ltd (GB-202).
Example 1
A cosmetic composition is prepared from the following raw materials in parts by weight: 8 parts of modified hydrogen-containing silicone oil, 6 parts of shellac resin, 12 parts of microcrystalline wax, 5 parts of glycerin fatty acid ester, 8 parts of sodium carboxymethyl cellulose, 5 parts of fructose, 3 parts of p-aminobenzoic acid, 2 parts of ascorbic acid, 2 parts of salicylic acid, 10 parts of humectant and 45 parts of solvent.
The modified hydrogen-containing silicone oil is prepared by grafting 2-methacryloyloxyethyl phosphorylcholine onto hydrogen-containing silicone oil, and the preparation method comprises the following steps: adding 2 parts by weight of catalyst platinum into 10 parts by weight of hydrogen-containing silicone oil, raising the temperature to 75 ℃, starting stirring, and adding 15 parts by weight of 2-methacryloyloxyethyl phosphorylcholine in the stirring process; the adding method of the 2-methacryloyloxyethyl phosphorylcholine comprises the following steps: 15 parts by weight of 2-methacryloyloxyethyl phosphorylcholine are divided into 5 parts by weight, 1 part is added each time, stirring is carried out for 20min after each addition is completed, then the next addition is carried out, the 2-methacryloyloxyethyl phosphorylcholine is dissolved more uniformly by a small amount of repeated addition, the 2-methacryloyloxyethyl phosphorylcholine contacts with hydrogen-containing silicone oil more fully, and the reaction between the 2-methacryloyloxyethyl phosphorylcholine and the hydrogen-containing silicone oil is more thorough; after the addition is completed, continuously increasing the temperature to 85 ℃, and performing reduced pressure distillation after the reaction is completed, wherein the reaction process is as follows:
Figure GDA0003767875150000031
wherein R is C a H 2a+1 ,a=2-17。
The method for preprocessing the shellac resin comprises the following steps: adding shellac resin into N-methyldiethanolamine, heating to 85 ℃, and stirring for 20min to obtain shellac resin pretreatment liquid.
Wherein the humectant is sorbitol; the solvent is deionized water.
The preparation method of the cosmetic composition comprises the following steps:
s1, respectively weighing raw materials according to parts by weight;
s2, preprocessing 6 parts by weight of shellac resin to obtain shellac resin preprocessing liquid;
s3, sequentially adding 8 parts by weight of modified hydrogen-containing silicone oil, 12 parts by weight of microcrystalline wax and 5 parts by weight of glycerin fatty acid ester weighed in the step S1 into 22.5 parts by weight of solvent, wherein the solvent consumption is half of the total weight, raising the temperature to 50 ℃, and starting stirring to fully dissolve for later use;
s4, respectively adding 5 parts by weight of fructose, 3 parts by weight of p-aminobenzoic acid, 2 parts by weight of ascorbic acid, 2 parts by weight of salicylic acid and 10 parts by weight of humectant into 22.5 parts by weight of solvent, wherein the solvent dosage is half of that of the medium, and uniformly stirring for later use;
and S5, mixing the solutions obtained in the step S3 and the step S4, adding the shellac resin pretreatment liquid prepared in the step S2, uniformly stirring, ultrasonically dispersing, and adding 8 parts by weight of sodium carboxymethylcellulose to adjust the viscosity of the solution until a stable emulsion is formed, thus obtaining the shellac resin emulsion.
Example 2
Compared with the example 1, the raw materials are different in selection and weight parts, the raw materials are different in dosage and preparation conditions in the preparation process, and the preparation method is specifically as follows with reference to the example 1:
a cosmetic composition is prepared from the following raw materials in parts by weight: 12 parts of modified hydrogen-containing silicone oil, 8 parts of shellac resin, 15 parts of microcrystalline wax, 8 parts of glycerin fatty acid ester, 12 parts of sodium carboxymethyl cellulose, 8 parts of fructose, 6 parts of p-aminobenzoic acid, 5 parts of ascorbic acid, 4 parts of salicylic acid, 15 parts of humectant and 56 parts of solvent.
The modified hydrogen-containing silicone oil is prepared by grafting 2-methacryloyloxyethyl phosphorylcholine onto hydrogen-containing silicone oil, and the preparation method comprises the following steps: adding 3 parts by weight of rhodium catalyst into 15 parts by weight of hydrogen-containing silicone oil, raising the temperature to 75 ℃, starting stirring, and adding 20 parts by weight of 2-methacryloyloxyethyl phosphorylcholine in the stirring process; the adding method of the 2-methacryloyloxyethyl phosphorylcholine comprises the following steps: 20 parts by weight of 2-methacryloyloxyethyl phosphorylcholine are divided into 5 parts by weight, 1 part is added each time, stirring is carried out for 30min after each addition is completed, then the next addition is carried out, the 2-methacryloyloxyethyl phosphorylcholine is dissolved more uniformly by a small amount of repeated addition, the 2-methacryloyloxyethyl phosphorylcholine contacts with hydrogen-containing silicone oil more fully, and the reaction between the 2-methacryloyloxyethyl phosphorylcholine and the hydrogen-containing silicone oil is more thorough; after the addition is completed, the temperature is continuously increased to 85 ℃, and the reaction is completed, and then the catalyst is obtained through reduced pressure distillation.
The method for preprocessing the shellac resin comprises the following steps: adding shellac resin into N-methyldiethanolamine, heating to 85 ℃, and stirring for 20min to obtain shellac resin pretreatment liquid.
Wherein the humectant is glycine; the solvent is distilled water.
The preparation method of the cosmetic composition comprises the following steps:
s1, respectively weighing raw materials according to parts by weight;
s2, pretreating 8 parts by weight of shellac resin to obtain shellac resin pretreatment liquid;
s3, sequentially adding 12 parts by weight of the modified hydrogen-containing silicone oil, 15 parts by weight of microcrystalline wax and 8 parts by weight of glycerin fatty acid ester weighed in the step S1 into 28 parts by weight of solvent, wherein the solvent consumption is half of the total parts, raising the temperature to 55 ℃, and starting stirring to fully dissolve for later use;
s4, respectively adding 8 parts by weight of fructose, 6 parts by weight of p-aminobenzoic acid, 5 parts by weight of ascorbic acid, 4 parts by weight of salicylic acid and 15 parts by weight of humectant into 28 parts by weight of solvent, wherein the solvent dosage is half of the medium weight, and uniformly stirring for later use;
and S5, mixing the solutions obtained in the step S3 and the step S4, adding the shellac resin pretreatment liquid prepared in the step S2, uniformly stirring, ultrasonically dispersing, and adding 12 parts by weight of sodium carboxymethylcellulose to adjust the viscosity of the solution until a stable emulsion is formed, thus obtaining the shellac resin emulsion.
Example 3
A cosmetic composition is prepared from the following raw materials in parts by weight: 10 parts of modified hydrogen-containing silicone oil, 7 parts of shellac resin, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethyl cellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of humectant and 50 parts of solvent.
The modified hydrogen-containing silicone oil is prepared by grafting 2-methacryloyloxyethyl phosphorylcholine onto hydrogen-containing silicone oil, and the preparation method comprises the following steps: adding 2 parts by weight of catalyst platinum into 12 parts by weight of hydrogen-containing silicone oil, raising the temperature to 75 ℃, starting stirring, and adding 17.5 parts by weight of 2-methacryloyloxyethyl phosphorylcholine during stirring; the adding method of the 2-methacryloyloxyethyl phosphorylcholine comprises the following steps: the method comprises the steps of (1) dividing 17.5 parts by weight of 2-methacryloyloxyethyl phosphorylcholine into 5 parts, adding 1 part each time, stirring for 20min after each addition is completed, adding the next part, and enabling the 2-methacryloyloxyethyl phosphorylcholine to be dissolved more uniformly and fully in contact with hydrogen-containing silicone oil through a small amount of repeated addition, wherein the reaction between the two parts is more thorough; after the addition is completed, the temperature is continuously increased to 85 ℃, and the reaction is completed, and then the catalyst is obtained through reduced pressure distillation.
The method for preprocessing the shellac resin comprises the following steps: adding shellac resin into N-methyldiethanolamine, heating to 85 ℃, and stirring for 30min to obtain shellac resin pretreatment liquid.
Wherein the humectant is sorbitol; the solvent is distilled water.
The preparation method of the cosmetic composition comprises the following steps:
s1, respectively weighing raw materials according to parts by weight;
s2, preprocessing 7 parts by weight of shellac resin to obtain shellac resin preprocessing liquid;
s3, sequentially adding 10 parts by weight of modified hydrogen-containing silicone oil, 14 parts by weight of microcrystalline wax and 6 parts by weight of glycerin fatty acid ester weighed in the step S1 into 25 parts by weight of solvent, wherein the solvent consumption is half of the total parts, raising the temperature to 50 ℃, and starting stirring to fully dissolve for later use;
s4, respectively adding 6 parts by weight of fructose, 5 parts by weight of p-aminobenzoic acid, 3 parts by weight of ascorbic acid, 3 parts by weight of salicylic acid and 12 parts by weight of humectant into 25 parts by weight of solvent, wherein the solvent dosage is half of the medium weight, and uniformly stirring for later use;
and S5, mixing the solutions obtained in the step S3 and the step S4, adding the shellac resin pretreatment liquid prepared in the step S2, uniformly stirring, ultrasonically dispersing, and adding 10 parts by weight of sodium carboxymethylcellulose to adjust the viscosity of the solution until a stable emulsion is formed, thus obtaining the shellac resin emulsion.
Comparative example 1
In comparison with example 3, shellac resin was not added to the raw material composition, and the remaining conditions were unchanged.
The raw materials and the compositions in the comparative example are as follows: 10 parts of modified hydrogen-containing silicone oil, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethylcellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of humectant and 50 parts of solvent.
The preparation method of the cosmetic composition comprises the following steps:
s1, respectively weighing raw materials according to parts by weight;
s2, sequentially adding 10 parts by weight of modified hydrogen-containing silicone oil, 14 parts by weight of microcrystalline wax and 6 parts by weight of glycerin fatty acid ester weighed in the step S1 into 25 parts by weight of solvent, wherein the solvent consumption is half of the total parts, raising the temperature to 50 ℃, and starting stirring to fully dissolve for later use;
s3, respectively adding 6 parts by weight of fructose, 5 parts by weight of p-aminobenzoic acid, 3 parts by weight of ascorbic acid, 3 parts by weight of salicylic acid and 12 parts by weight of humectant into 25 parts by weight of solvent, wherein the solvent dosage is half of the medium weight, and uniformly stirring for later use;
s4, mixing the solutions obtained in the step S2 and the step S3, and adding 10 parts by weight of sodium carboxymethylcellulose after ultrasonic dispersion to adjust the viscosity of the solution until stable emulsion is formed, thus obtaining the emulsion.
The remaining preparation is described in example 3.
Comparative example 2
In comparison with example 3, no modification of the hydrogen-containing silicone oil was carried out, the remaining conditions being unchanged.
The raw materials and the compositions in the comparative example are as follows: 10 parts of hydrogen-containing silicone oil, 7 parts of shellac resin, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethyl cellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of humectant and 50 parts of solvent.
The specific preparation is described in example 3.
Comparative example 3
In comparison with example 3, the modified hydrogen-containing silicone oil was replaced with 2-methacryloyloxyethyl phosphorylcholine, with the remaining conditions unchanged.
The raw materials and the compositions in the comparative example are as follows: 10 parts of 2-methacryloyloxyethyl phosphorylcholine, 7 parts of shellac resin, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethyl cellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of humectant and 50 parts of solvent.
The specific preparation is described in example 3.
Comparative example 4
In comparison with example 3, the modified hydrogen-containing silicone oil was replaced with hydrogen-containing silicone oil and 2-methacryloyloxyethyl phosphorylcholine, with the remaining conditions unchanged.
The raw materials and the compositions in the comparative example are as follows: 12 parts of hydrogen-containing silicone oil, 17.5 parts of 2-methacryloyloxyethyl phosphorylcholine, 7 parts of shellac resin, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethylcellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of humectant and 50 parts of solvent.
The specific preparation is described in example 3.
Comparative example 5
Compared to example 3, shellac resin was replaced with shea resin, and the remaining conditions were unchanged.
The raw materials and the compositions in the comparative example are as follows: 10 parts of modified hydrogen-containing silicone oil, 7 parts of avocado resin, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethylcellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of a humectant and 50 parts of a solvent.
The specific preparation is described in example 3.
Comparative example 6
In comparison with example 3, shellac resin was not pretreated and the remaining conditions were unchanged.
The raw materials and the compositions in the comparative example are as follows: 10 parts of modified hydrogen-containing silicone oil, 7 parts of shellac resin, 14 parts of microcrystalline wax, 6 parts of glycerin fatty acid ester, 10 parts of sodium carboxymethyl cellulose, 6 parts of fructose, 5 parts of p-aminobenzoic acid, 3 parts of ascorbic acid, 3 parts of salicylic acid, 12 parts of humectant and 50 parts of solvent.
The preparation method of the cosmetic composition comprises the following steps:
s1, respectively weighing raw materials according to parts by weight;
s2, sequentially adding 10 parts by weight of modified hydrogen-containing silicone oil, 7 parts by weight of shellac resin, 14 parts by weight of microcrystalline wax and 6 parts by weight of glycerin fatty acid ester which are weighed in the step S1 into 25 parts by weight of solvent, wherein the solvent consumption is half of the total weight, raising the temperature to 50 ℃, and starting stirring to fully dissolve for later use;
s3, respectively adding 6 parts by weight of fructose, 5 parts by weight of p-aminobenzoic acid, 3 parts by weight of ascorbic acid, 3 parts by weight of salicylic acid and 12 parts by weight of humectant into 25 parts by weight of solvent, wherein the solvent dosage is half of the medium weight, and uniformly stirring for later use;
and S4, mixing the solutions obtained in the step S2 and the step S3, uniformly stirring, and adding 10 parts by weight of sodium carboxymethylcellulose after ultrasonic dispersion to adjust the viscosity of the solution until stable emulsion is formed, thus obtaining the emulsion.
Correlation performance test:
1. temperature resistance test
The cosmetic compositions prepared in examples 1 to 3 and comparative examples 1 to 6 were placed in 50ml test tubes with stoppers, and placed in a 40℃thermostat water bath for 24 hours, and the water-out condition was observed and the water cut rate was calculated. The calculation formula of the water division rate is as follows: f= (v) 1 /v 2 ) X 100%, where f: a water division rate; v 1 : separating out the volume of water, ml; v 2 : total volume of aqueous phase, ml. The test results are shown in Table 1.
TABLE 1
Group of Water cut rate/%
Example 1 0
Example 2 0
Example 3 0
Comparative example 1 20
Comparative example 2 65
Comparative example 3 25
Comparative example 4 12
Comparative example 5 18
Comparative example 6 15
As can be seen from the data in Table 1, the cosmetic compositions prepared in examples 1 to 3 did not show water division, and the sample prepared in comparative example 2 had a maximum water division of 65% and the cosmetics prepared in examples 1 to 3 had higher stability and higher emulsifying property as can be seen from the temperature resistance test.
2. Cold resistance test
According to cosmetic national Standard GB/T29665-2013 skin care emulsion, the cosmetic compositions prepared in examples 1-3 and comparative examples 1-6 were placed in a 50ml test tube with a stopper, placed in a low temperature thermostatic water bath at-8deg.C for 24 hours, taken out, placed at room temperature for 2 hours, and then the state change of the sample was observed, and the water cut rate was calculated. The test results are shown in Table 2.
TABLE 2
Figure GDA0003767875150000091
Figure GDA0003767875150000101
As can be seen from the data of Table 2, the cosmetic compositions prepared in examples 1 to 3, comparative example 4 and comparative example 6 do not show water division, and the sample prepared in comparative example 2 shows the greatest degree of water division, so that the samples prepared in examples 1 to 3, comparative example 4 and comparative example 6 have a certain stability at low temperature.
3. Centrifugal stability test
According to cosmetic national Standard GB/T29665-2013 skin care emulsion, a proper amount of samples prepared in examples 1-3 and comparative examples 1-6 are placed into a centrifuge tube (2/3 of the volume of the centrifuge tube), and test conditions are as follows: 2000r/min, and centrifuging for 30min. After the test is finished, the centrifuge tube is taken out to observe the state change of the sample. The test results are shown in Table 3.
TABLE 3 Table 3
Figure GDA0003767875150000102
Figure GDA0003767875150000111
As can be seen from the test results of Table 3, examples 1 to 3 and comparative examples 4 to 6 were free from water separation after the centrifugation test, and comparative example 1 and comparative example 3 were slightly water-separated, and comparative example 2 was water-separated to a greater extent. Examples 1-3 and comparative examples 4-6 are illustrated to have higher stability performance in the centrifugation test.
4. Moisture retention performance test
Test conditions: the ambient temperature is 20-22 ℃ and the ambient humidity is 40% -60% in the test.
The testing steps are as follows:
(1) Marking a plurality of 3cm multiplied by 3cm tested areas on the inner side of the forearm of a subject, so that the cosmetic application area and the blank control area are randomly distributed;
(2) Before using the sample, using a skin moisture meter to measure in the smeared area and the blank area, recording the initial measurement value;
(3) Immediately, 8mg of cosmetics are applied to the application area by a pipette once, and the cosmetics are uniformly applied by wearing latex gloves. Measuring skin moisture content of all areas at a set time, each area being measured 3 times, the test time not exceeding 24 hours;
(4) After the measurement is finished, the measured values of all the test areas are counted, and the moisturizing effect of the cosmetics is judged.
50 volunteers 18-30 years old were randomly selected for trial, no product was used 2-3 days before the test, no water was contacted 1-2 hours before the test, the test sites of the volunteers were wiped clean by using a dry paper towel before the test, the moisturizing effect of the cosmetics prepared in examples 1-3 and comparative examples 1-6 was measured, and the moisturizing ability of the skin itself was measured by setting a control group, and the experimental results are shown in table 4.
TABLE 4 Table 4
Figure GDA0003767875150000112
Figure GDA0003767875150000121
As can be seen from the data in Table 4, the skin moisture content gradually decreases with time, wherein the initial moisturizing effect of the sample prepared in example 3 is best, and the skin moisture content can be maintained close to 10 hours after application, and the moisturizing effect of the samples prepared in examples 1-3 is higher than that of the samples prepared in comparative examples 1-6 in comprehensive comparison, and is higher than that of the control group, namely, the moisturizing ability of the skin can be effectively improved after the cosmetic samples prepared by application.
5. Safety test
Test article: samples prepared in example 3.
Control group: deionized water.
The subject: 40 volunteers 18-30 years old.
The patch method comprises the following steps: the test object and the control group are dripped into a plaque tester by a closed plaque test method from about 0.020mL to 0.025mL (semi-fluid), the test object is removed after being externally applied to the back of a subject for 24 hours, skin reactions are observed after being removed for 0.5 hour, 24 hours and 48 hours respectively, and test results are recorded, and are shown in table 5.
TABLE 5
Figure GDA0003767875150000122
Figure GDA0003767875150000131
The results of the human skin patch test show that no adverse reaction of skin occurs in volunteers, which indicates that the cosmetics prepared by the invention are safe to use, and the samples prepared in examples 1-3 are subjected to the human skin patch test according to the method, so that the test results similar to the test results are obtained.
Compared with the prior art, shellac resin is obtained from the secretion of lac worm and is the only known animal resin, the resin is a solid formed by lactone and gum ester of hydroxy carboxylic acid, and the resin is an elastic grid formed by hydroxy fatty acid and sesquiterpene acid, and the gaps contain a mixture of low-molecular fatty acid esters, so that the shellac resin has good stability and film forming property. The carboxyl and hydroxyl in the shellac structure gradually undergo esterification reaction in high-temperature storage, the film forming performance of the shellac is affected, and the carboxyl is neutralized by adopting N-methyldiethanolamine, so that the occurrence of the esterification reaction is effectively inhibited, and the shellac can maintain good performance at high temperature.
Introducing long-chain alkyl groups into silicone oils (wherein R is C a H 2a+1 A=2-17), can enhance the lipophilicity of the cosmetic, enable the cosmetic to be more similar to the fat component of a human body, have better affinity with skin, and effectively improve the skin care property, the hydrophobic air permeability, the softness, the smoothness, the crease resistance and the anti-sticking property of the cosmetic; the use of organic acid can reduce the generation of insoluble matters, but cosmetics containing the components can increase sticky feeling in the use process, and influence the use experience; in order to prepare the cosmetics with high stability while keeping good use experience, the invention mixes hydrogen-containing silicone oil with 2-methacryloyloxyethyl phosphorylcholine, reacts under the action of a catalyst, and grafts the 2-methacryloyloxyethyl phosphorylcholine onto the hydrogen-containing silicone oil to obtain the modified hydrogen-containing silicone oil. The cell membrane takes two layers of lipid molecules as a framework, the main component is phospholipid amphiphilic molecules, phosphorylcholine is a hydrophilic end group of a basic unit forming the cell membrane, is the outermost layer group in the outer cell membrane, and is copolymerized with hydrophobic acrylic ester monomers to obtain a copolymer with hydrophilic and oleophilic amphiphilic properties, so that 2-methacryloyloxyethyl phosphorylcholine contains zwitterionic groups and has good hydrophilicity and conservationAqueous, at the same time its good biocompatibility makes it safer during the application of cosmetics. The 2-methacryloyloxyethyl phosphorylcholine is grafted to the hydrogen-containing silicone oil, the existence of long-chain alkyl in the hydrogen-containing silicone oil increases the affinity with skin, and meanwhile, the long-chain alkyl and a silicone oil molecular chain are mutually combined to form a network structure, so that the hydrogen-containing silicone oil has better ductility; furthermore, the formed reticular structure is matched with the elastic grids in the shellac resin, so that the stability of the prepared cosmetic is further improved, and the test results of temperature resistance, cold resistance and centrifugal stability show that the prepared cosmetic is better in stability; in addition, the existence of the 2-methacryloyloxyethyl phosphorylcholine can improve the stability of the cosmetics and simultaneously has better skin-friendly property, so that the prepared cosmetics can uniformly cover and protect the skin at a coating position, and can keep better moisturizing effect for a long time.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the application, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. The cosmetic composition is characterized by being prepared from the following raw materials in parts by weight: 8-12 parts of modified hydrogen-containing silicone oil, 6-8 parts of shellac resin, 12-15 parts of microcrystalline wax, 5-8 parts of glycerin fatty acid ester, 8-12 parts of sodium carboxymethyl cellulose, 5-8 parts of fructose, 3-6 parts of p-aminobenzoic acid, 2-5 parts of ascorbic acid, 2-4 parts of salicylic acid, 10-15 parts of humectant and 45-56 parts of solvent;
the modified hydrogen-containing silicone oil is prepared by grafting 2-methacryloyloxyethyl phosphorylcholine onto hydrogen-containing silicone oil, and has the structural formula:
Figure DEST_PATH_IMAGE001
wherein R is C a H 2a+1 ,a=2-17;
The humectant is sorbitol or glycine;
the solvent is deionized water or distilled water;
the shellac resin is shellac resin pretreatment liquid, and the pretreatment method comprises the following steps: adding shellac resin into N-methyldiethanolamine, heating to 85 ℃, and stirring for 20min to obtain shellac resin pretreatment liquid.
2. The cosmetic composition according to claim 1, wherein the modified hydrogen-containing silicone oil is prepared by the process of: adding a catalyst into hydrogen-containing silicone oil, raising the temperature, starting stirring, adding 2-methacryloyloxyethyl phosphorylcholine in the stirring process, continuously raising the temperature after the addition is finished, and performing reduced pressure distillation after the reaction is finished.
3. The cosmetic composition according to claim 2, wherein the addition method of 2-methacryloyloxyethyl phosphorylcholine is: the 2-methacryloyloxyethyl phosphorylcholine is divided into 5 parts, 1 part is added each time, and after each addition is completed, the mixture is stirred for 20 to 30 minutes, and then the next addition is performed.
4. The cosmetic composition according to claim 2, wherein the catalyst is one or a mixture of platinum, palladium, rhodium, silver and ruthenium.
5. The method for producing a cosmetic composition according to any one of claims 1 to 4, wherein the method for producing is:
s1, respectively weighing raw materials according to parts by weight;
s2, preprocessing shellac resin to obtain shellac resin preprocessing liquid;
s3, sequentially adding the modified hydrogen-containing silicone oil, the microcrystalline wax and the glycerol fatty acid ester which are weighed in the step S1 into a solvent, wherein the solvent consumption is half of the total part, heating to 50-55 ℃, and starting stirring to fully dissolve for standby;
s4, respectively adding fructose, p-aminobenzoic acid, ascorbic acid, salicylic acid and a humectant into a solvent, wherein the solvent dosage is half of the medium part, and uniformly stirring for later use;
and S5, mixing the solutions obtained in the step S3 and the step S4, adding the shellac resin pretreatment liquid prepared in the step S2, uniformly stirring, and adding sodium carboxymethylcellulose after ultrasonic dispersion to adjust the viscosity of the solution until stable emulsion is formed, thus obtaining the shellac resin.
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