CN117414305A - Sun protection emulsion for children and preparation method thereof - Google Patents

Sun protection emulsion for children and preparation method thereof Download PDF

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Publication number
CN117414305A
CN117414305A CN202311431836.2A CN202311431836A CN117414305A CN 117414305 A CN117414305 A CN 117414305A CN 202311431836 A CN202311431836 A CN 202311431836A CN 117414305 A CN117414305 A CN 117414305A
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China
Prior art keywords
sun
agent
child
emulsion
skin
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CN202311431836.2A
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Chinese (zh)
Inventor
帅斌
舒鹏
刘昭
蔡智丽
王晨霞
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Shenzhen Hujia Technology Co ltd
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Shenzhen Hujia Technology Co ltd
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Priority to CN202311431836.2A priority Critical patent/CN117414305A/en
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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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27Zinc; Compounds 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
    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585Organosilicon 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
    • A61K8/72Cosmetics 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
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • 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
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/26Optical properties
    • A61K2800/262Transparent; Translucent
    • 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
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

Abstract

The invention relates to a children sun protection emulsion and a preparation method thereof. The children sun-screening emulsion comprises 20-25% by mass of non-nanometer physical sun-screening agent, wherein the non-nanometer physical sun-screening agent is flaky zinc oxide treated by a surface treatment agent, the surface treatment agent is triethoxy octyl siloxane or hydrogenated polydimethylsiloxane, and the particle size D50 of the flaky zinc oxide is 0.1-0.4 mu m. The material also comprises the following raw materials in percentage by mass: an emollient: 30-40% of an emulsifier: 3-7% of thickener: 0.4-1.0%, humectant: 4-15% of preservative: 0.5-1.0%, filler: 0.5-1.0%, skin feel modifier: 0.5-5% of a dispersant: 0.5-2%. The invention provides the children sun-screening emulsion which can effectively block ultraviolet rays, has excellent stability and good transparency and skin feel.

Description

Sun protection emulsion for children and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a children sun-proof emulsion and a preparation method thereof.
Background
Ultraviolet rays in sunlight cause serious injury to human beings, wherein medium-wave ultraviolet rays (UVB) with the wavelength of 290-320 nm can cause red swelling, blisters, peeling and inflammation of skin; long wave Ultraviolet (UVA) light of 320-400 nm causes skin tanning, aging, skin cancer and DNA damage.
According to the publication of the suggestion of the technical guidelines for children's cosmetics (the suggestion draft) published by month 11 of 2022, the development of sun protection products for children does not allow the use of raw materials prepared by new technologies such as nanotechnology, in principle, the types of chemical sun protection agents should not be more than 3 (not contain 3) and should be used in an amount lower than that of adults, wherein when titanium dioxide and zinc oxide are used simultaneously as sun protection agents or for other purposes, the total use amount should not be more than 25%, and the SPF value should not be higher than 30. Wherein, SPF is the English abbreviation of sun protection factor Sun Protection Factor, sun Protection Factor (SPF) is the ability of representing the product to defend medium wave ultraviolet rays by specific numerical values, is a protection index for evaluating the ability of a sun-proof cosmetic to protect skin from occurrence of sunburn erythema/sunburn, and the higher the SPF value, the better the sun-proof erythema/sunburn effect. When 3 or more chemical sunscreens are used, the sunscreens are used in a formulation similar to that of an adult and the SPF value is higher than 30, the scientificity and necessity of the raw materials used should be sufficiently confirmed, and if necessary, the study data of the formulation optimization process is submitted as evidence support.
In sun-screening milk, physical sun-screening agents are generally less sensitive to skin than chemical sun-screening agents, but traditional non-nano physical sun-screening agents cannot reach higher values of sun-screening index when in use, so that sun-screening effect is not ideal, and meanwhile, physical sun-screening agents with large particle sizes may have the phenomenon of pseudo-white occurrence, so that the sun-screening agents are not attractive when in use.
Accordingly, improvements are needed in the art.
Disclosure of Invention
In the prior art, when the traditional non-nanometer physical sun-screening agent is used, the sun-screening index cannot reach a higher value, so that the sun-screening effect is not ideal, and meanwhile, the physical sun-screening agent with large particle size can be pseudo-white, so that the sun-screening agent is not attractive when being used and is not suitable for being used as child sun-screening milk, so that the invention provides the child sun-screening milk and the preparation method thereof for solving the problems.
To achieve the above object, in a first aspect, the present invention provides a child sun protection emulsion comprising 20 to 25% by mass of a non-nano physical sun protection agent, wherein the non-nano physical sun protection agent is a sheet zinc oxide treated with a surface treatment agent, the surface treatment agent is triethoxy octyl siloxane or hydrogenated polydimethylsiloxane, and the particle size D50 of the sheet zinc oxide is 0.1 μm to 0.4 μm.
In one implementation, the child sun protection milk further comprises the following raw materials in percentage by mass:
an emollient: 30-40%,
emulsifying agent: 3 to 7 percent,
and (3) a thickening agent: 0.4 to 1.0 percent,
humectant: 4-15 percent,
preservative: 0.5 to 1.0 percent,
filler: 0.5 to 1.0 percent,
skin feel modifier: 0.5-5%
Dispersing agent: 0.5-2%.
In one implementation, the humectant includes any one or more of glycerin, propylene glycol, butylene glycol, 1, 3-propylene glycol, pentylene glycol, and 1, 2-hexylene glycol.
In one implementation, the filler is sodium chloride or magnesium sulfate and the preservative is phenoxyethanol or p-hydroxyacetophenone.
In one implementation, the emollient is any one or more of coco caprylic/capric acid ester, polydimethylsilane, isohexadecane, caprylic/capric triglyceride, isononyl isononanoate, C9-12 alkane, squalane, and jojoba oil.
In one implementation, the dispersant is any one or more of sorbitan sesquiisostearate, sorbitan sesquioleate, and acrylic acid (ester)/ethylhexyl acrylate/polydimethylsiloxane methacrylate copolymer.
In one implementation, the emulsifier is any one or more of polyglycerol-2-dimer hydroxystearate, polyglycerol-4-diisostearate/polyhydroxystearate/sebacate, lauryl PEG-9-dimethicone ethyl dimethicone, cetyl PEG/PPG-10/1-dimethicone, and PEG-9-dimethicone ethyl dimethicone.
In one implementation, the thickener is distearyldimethylammonium hectorite or quaternary salt-18 bentonite.
In one implementation, the skin feel modifier is silica or polymethylsilsesquioxane.
In a second aspect, the present invention also provides a method for preparing a child sun protection milk, which is used for preparing the child sun protection milk according to any one of the above, and specifically includes the following steps:
s1, weighing the raw materials with the mass fractions, sequentially adding the solvent, the humectant and the filler into a water pot, heating to 85 ℃, uniformly stirring, cooling to 25-30 ℃, and adding the preservative to obtain a water phase mixture A;
s2, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s3, stirring is started, the water phase mixture A obtained in the step S1 is added into an emulsifying pot, stirring is carried out for 5 minutes, and then homogenization is started for 1 minute;
and S4, continuously stirring until the mixture is uniform and vacuum defoamation is carried out, and obtaining the child sun-proof emulsion.
The beneficial effects are that: according to the invention, the flaky zinc oxide treated by the surface treatment agent is used as a sun-screening agent, so that the children sun-screening emulsion meeting the requirements of children cosmetics is obtained, the provided children sun-screening emulsion has good transparency and skin feel performance while sun-screening is ensured, and the children sun-screening emulsion which has excellent ultraviolet resistance and stability performance and good transparency and skin feel performance is provided.
Drawings
FIG. 1 is a graph showing the absorbance contrast of a sheet zinc oxide provided by the present invention;
FIG. 2 is a schematic view of an electron microscope of the sheet zinc oxide provided by the present invention;
FIG. 3 is a graph comparing sun protection efficiency of a sheet zinc oxide provided by the present invention with that of a conventional zinc oxide raw material;
fig. 4 is a graph showing the transparency of the children's sun-protection milk according to the present invention compared with the existing children's sun-protection milk made of zinc oxide.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. Furthermore, the descriptions of the terms "one embodiment," "some embodiments," "examples," "particular examples," or "some examples," etc., described below mean 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 invention. In this specification, schematic representations of the above terms are not necessarily for the same embodiment or example. The technical features of the respective embodiments of the present invention may be combined with each other as long as they do not collide with each other.
The invention provides a child sun protection emulsion, which comprises 20-25% by mass of non-nanometer physical sun protection agent, wherein the non-nanometer physical sun protection agent is flaky zinc oxide treated by a surface treatment agent, the surface treatment agent is triethoxy octyl siloxane or hydrogenated polydimethylsiloxane, and the particle size D50 of the flaky zinc oxide is 0.1-0.4 mu m. Wherein, the sheet zinc oxide is treated by the surface treating agent, and the smoothness and the dispersibility of the sheet zinc oxide are improved. The use of a surface treatment agent such as triethoxy octyl siloxane or hydrogenated polydimethyl siloxane can form a protective film on the surface of zinc oxide. This helps reduce the likelihood of powder coalescence and hard block formation, improves the stability of the product and allows for better dispersion in cosmetics or sunscreens.
Wherein the child sun cream further comprises an emulsifier, a thickener, an emollient, a humectant, a preservative, a filler, a skin feel modifier, and a dispersant. Specifically, the children sun protection emulsion further comprises the following raw materials in percentage by mass:
an emollient: 30-40%,
emulsifying agent: 3 to 7 percent,
and (3) a thickening agent: 0.4 to 1.0 percent,
humectant: 4-15 percent,
preservative: 0.5 to 1.0 percent,
filler: 0.5 to 1.0 percent,
skin feel modifier: 0.5-5%
Dispersing agent: 0.5-2%.
Further, the humectant comprises any one or more of glycerin, propylene glycol, butylene glycol, 1, 3-propylene glycol, pentylene glycol and 1, 2-hexylene glycol.
The filler is sodium chloride or magnesium sulfate.
The preservative is phenoxyethanol or p-hydroxyacetophenone.
The emollient is any one or more of coco caprylic/capric acid ester, polydimethyl silane, isohexadecane, caprylic/capric triglyceride, isononyl isononanoate, C9-12 alkane, squalane and jojoba oil.
The dispersing agent is any one or more of sorbitan sesquiisostearate, sorbitan sesquioleate and acrylic acid (ester)/ethylhexyl acrylate/polydimethylsiloxane methacrylate copolymer. Among them, acrylic acid (esters)/ethylhexyl acrylate/polydimethylsiloxane methacrylate copolymer is a synthetic material, and is generally used as a thickener, thickener and emulsifier in cosmetics. They can increase the tackiness and consistency of the product, making it easier to use and apply. The concentration of such copolymers in cosmetics is generally low and therefore the skin irritation is also low.
The emulsifier is any one or more of polyglycerol-2 dipolyhydroxystearate, polyglycerol-4 diisostearate/polyhydroxystearate/sebacate, lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, cetyl PEG/PPG-10/1 polydimethylsiloxane and PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane.
The thickener is disteardimonium hectorite (CAS 94891-31-3) or quaternary salt-18 bentonite.
The skin feel modifier is silica or polymethylsilsesquioxane.
The invention also provides a preparation method of the children sun protection milk, which specifically comprises the following steps:
s1, weighing the raw materials with the mass fractions, sequentially adding the solvent, the humectant and the filler into a water pot, heating to 85 ℃, uniformly stirring, cooling to 25-30 ℃, and adding the preservative to obtain a water phase mixture A;
s2, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s3, stirring is started, the water phase mixture A obtained in the step S1 is added into an emulsifying pot, stirring is carried out for 5 minutes, and then homogenization is started for 1 minute;
and S4, continuously stirring until the mixture is uniform and vacuum defoamation is carried out, and obtaining the child sun-proof emulsion.
Referring to fig. 1-4 in combination, fig. 1 is a graph showing absorbance contrast of the flaky zinc oxide provided by the present invention, fig. 2 is a schematic view of an electron microscope of the flaky zinc oxide provided by the present invention, fig. 3 is a graph showing sun protection efficiency contrast of the flaky zinc oxide provided by the present invention and the existing zinc oxide raw material, and fig. 4 is a graph showing transparency contrast of the child sun protection emulsion provided by the present invention and the child sun protection emulsion prepared by the existing zinc oxide.
As can be seen from fig. 1, the flaky zinc oxide provided by the invention has absorbance in both UVA and UVB, and has a wider-spectrum sun-screening function compared with conventional zinc oxide. The zinc oxide with the flaky structure adopted by the invention can be obtained from figure 2, and the size of the flaky structure is 0.1-0.4 mu m, and the thickness of the flaky structure is large, so that the flaky structure has good transparency and skin feel performance while ensuring sun protection when being used as a sun-screening agent. In FIG. 3, ZS-1004B (B) is 20nm zinc oxide surface treated with triethoxyoctylsilane, NZD60AB20 (A) is 20nm zinc oxide surface treated with triethoxyoctylsilane at C12-15 alkyl benzoate is ground into a slurry of 60% content, BSZP (C) is triethoxyoctylsilane surface treated flake zinc oxide, ZS94B (D) is current micron grade zinc oxide. The graph shows that the flaky zinc oxide used in the patent of the invention has the same sun-proof efficiency as the nanometer zinc oxide. As can be seen from fig. 4, the transparency of the flaky zinc oxide (BSZP) provided by the present invention is higher than that of the common zinc oxide-made child sun cream.
Example 1
In this example, a child sun cream is provided comprising a solvent, a sunscreen, an emulsifier, a thickener, an emollient, a humectant, a preservative, a filler, a skin feel modifier, and a dispersant.
Specifically, the solvent is water accounting for 25% of the total mass;
the sun-screening agent is zinc oxide/triethoxy octyl silane accounting for 20 percent of the total mass;
the emulsifier comprises polyglycerol-2 dimer hydroxystearate 2% by weight and cetyl PEG/PPG-10/1 polydimethylsiloxane 1% by weight;
the thickener is distearyl dimethyl ammonium hectorite accounting for 0.8 percent of the total mass;
the emollient comprises 15% by total mass of coco caprylic/capric acid ester, 8% by total mass of polydimethylsiloxane, 7% by total mass of isohexadecane and 4.8% by total mass of isononyl isononanoate;
the humectant comprises 8% of 1, 3-propylene glycol, 5% of butanediol and 0.5% of hexanediol by total mass;
the preservative is p-hydroxyacetophenone accounting for 0.4% of the total mass;
the filler is magnesium sulfate with the total mass of 0.5 percent;
the skin feel modifier is silica accounting for 1.0 percent of the total mass;
the dispersant is sorbitan sesquiisostearate with the total mass of 0.5%.
The embodiment provides a preparation method of a children sun block, comprising the following steps:
s11, weighing the raw materials with the mass fractions, sequentially adding the solvent, the humectant, the filler and the preservative into a water pot, heating to 85 ℃, uniformly stirring, and then cooling to 25-30 ℃ to obtain a water phase mixture A;
s12, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s13, stirring is started, the water phase mixture A obtained in the step S11 is added into an emulsifying pot, stirring is performed for 5 minutes, and then homogenization is started for 1 minute;
and S14, continuously stirring until the mixture is uniformly vacuum defoamed, and obtaining the child sun-proof emulsion.
Example 2
Unlike in example 1, specific raw materials of the child sun milk provided in this example include:
the solvent is water accounting for 25 percent of the total mass;
the sun-screening agent is zinc oxide/triethoxy octyl silane accounting for 22 percent of the total mass;
the emulsifier comprises 3% of polyglycerol-4 diisostearate/polyhydroxystearate/sebacate by total mass and 1.0% of PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane by total mass;
the thickener is distearyl dimethyl ammonium hectorite accounting for 0.5 percent of the total mass;
the emollient comprises 10% by total mass of coco caprylic/capric ester, 15% by total mass of polydimethylsiloxane, 8% by total mass of isohexadecane and 5% by total mass of caprylic/capric triglyceride;
the humectant comprises butanediol 3% of the total mass, glycerol 2.7% and hexanediol 0.5%;
the preservative is phenoxyethanol with the total mass of 0.3 percent;
the filler is sodium chloride accounting for 1% of the total mass;
the skin feel modifier is polymethyl silsesquioxane accounting for 1% of the total mass;
the dispersing agent is sorbitan sesquioleate accounting for 1.0% of the total mass.
The embodiment provides a preparation method of a children sun block, comprising the following steps:
s21, weighing the raw materials with the mass fractions, sequentially adding the solvent, the humectant and the filler into a water kettle, heating to 85 ℃, uniformly stirring, cooling to 25-30 ℃, and adding the preservative to obtain a water phase mixture A;
s22, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s23, stirring is started, the water phase mixture A obtained in the step S1 is added into an emulsifying pot, stirring is performed for 5 minutes, and then homogenization is started for 1 minute;
and S24, continuously stirring until the mixture is uniformly vacuum defoamed, and obtaining the child sun-proof emulsion.
Example 3
Unlike in example 1, specific raw materials of the child sun milk provided in this example include:
the solvent is 21% of water by total mass;
the sun-screening agent is zinc oxide/triethoxy octyl silane accounting for 24 percent of the total mass;
the emulsifier comprises 3% of lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane and 2% of polyglycerol-2 dimer hydroxystearate by total mass;
the thickener is quaternary plating salt-18 bentonite accounting for 0.4% of the total mass;
the emollient comprises 5% by total mass of coco caprylic/capric acid ester, 15% by total mass of polydimethylsiloxane, 13% by total mass of isohexadecane and 6.1% by total mass of squalane;
the humectant comprises 3% of butanediol and 3% of glycerol by total mass;
the preservative comprises p-hydroxyacetophenone accounting for 0.3 percent of the total mass and phenoxyethanol accounting for 0.4 percent of the total mass;
the filler is magnesium sulfate with the total mass of 0.8%;
the skin feel modifier comprises 1% of polymethylsilsesquioxane and 0.5% of silica by total mass;
the dispersing agent is acrylic acid (ester)/ethylhexyl acrylate/polydimethylsiloxane methacrylate copolymer with the total mass of 1.5 percent.
The embodiment provides a preparation method of a children sun block, comprising the following steps:
s31, weighing the raw materials with the mass fractions, sequentially adding the solvent, the humectant, the filler and the preservative into a water pot, heating to 85 ℃, uniformly stirring, and then cooling to 25-30 ℃ to obtain a water phase mixture A;
s32, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s33, stirring is started, the water phase mixture A obtained in the step S31 is added into an emulsifying pot, stirring is performed for 5 minutes, and then homogenization is started for 1 minute;
and S34, continuously stirring until the mixture is uniformly vacuum defoamed, and obtaining the child sun-proof emulsion.
Example 4
Unlike in example 1, specific raw materials of the child sun milk provided in this example include:
the solvent was water at 23% by mass of the total.
The sunscreen agent is zinc oxide/hydrogenated polydimethylsiloxane accounting for 23% of the total mass.
The emulsifier comprises lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane in an amount of 2.5% by weight and cetyl PEG/PPG-10/1 polydimethylsiloxane in an amount of 2% by weight.
The thickener is distearyl dimethyl ammonium hectorite with the total mass of 0.5 percent.
The emollient comprises 8% by total mass of coco caprylic/capric acid ester, 12% by total mass of polydimethylsiloxane, 9.7% by total mass of isohexadecane and 5% by total mass of jojoba oil.
The humectant comprises 5% butanediol and 5% glycerol by total mass.
The preservative is p-hydroxyacetophenone accounting for 0.5% of the total mass.
The filler is magnesium sulfate with the total mass of 0.8%.
The skin feel modifier is polymethylsilsesquioxane with the total mass of 1.5%.
The dispersant comprises sorbitan sesquioleate accounting for 0.5% of the total mass and acrylic acid (ester)/ethylhexyl acrylate/polydimethylsiloxane methacrylate copolymer accounting for 1.0%.
The embodiment provides a preparation method of a children sun block, comprising the following steps:
s41, weighing the raw materials with the mass fractions, sequentially adding the solvent, the humectant and the filler into a water kettle, heating to 85 ℃, uniformly stirring, cooling to 25-30 ℃, and adding the preservative to obtain a water phase mixture A;
s42, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s43, stirring is started, the water phase mixture A obtained in the step S41 is added into an emulsifying pot, stirring is started for 5 minutes, and homogenization is started for 1 minute;
and S44, continuously stirring until the mixture is uniformly vacuum defoamed, and obtaining the child sun-proof emulsion.
The following are various performance tests performed on the child sun protection milks obtained in examples 1-4 provided herein.
1. Skin patch test:
30 adults aged 23-49 years were randomly selected, including 5 men and 25 women, and the test pieces were the child sun-protection milks prepared in examples 1-4, and the negative control was a blank control. Selecting proper patch test equipment, coating about 0.02-0.025g of test object into the patch test device by a closed patch test method, applying the test object onto the forearm flexor side of a subject by using a medical adhesive tape for external use, removing the test object for 24 hours, observing skin reactions respectively in the patch tests for 0.5 hours, 24 hours and 48 hours, and according to the skin reaction grading standard in cosmetic hygiene Specification (2015 edition), wherein the test results are shown in Table 1.
TABLE 1 skin response grading Standard for skin seal Patch test
Table 2 statistical table of skin patch test results
Human body patches showed that 0 cases of suspicious reactions appeared in 30 subjects. It was confirmed that the child sun milk of the present invention did not cause adverse effects on the child's skin.
2. Sun protection SPF value test
The object to be measured: the products produced as in examples 1-4.
Control: SPF value 16.1, according to the standard formulation of cosmetic safety technical Specification (2015 edition).
The subject: 10 people total, 10 people completed, 5 men and 5 women, ages 23-49 years, and average age 28 years, meet the volunteer selection standard of the subjects.
Light source: the xenon arc lamp of the sunlight simulator meets the measurement specification requirements in each performance index.
The inspection method comprises the following steps: the test is performed according to the specific requirements of the current effective technical specifications. The subject was tilted forward and irradiated on the back. The minimum erythema dose (MED value) of the subject's skin to ultraviolet irradiation was predicted 24 hours before the test, and the ultraviolet irradiation dose was adjusted based on the prediction result, for testing the test object. On the day of testing, first, a test subject was selected for a time of not less than 30cm on his back 2 Is used in an amount of (2.00.+ -. 0.05) mg/cm 2 Uniformly coating the object to be detected or the reference substance in the area, selecting the irradiation dose according to the standard requirement, and irradiating in three conditions: (1) the skin of the subject is not coated with the test object; (2) coating a reference substance; (3) coating the measured object. The experimental results were observed after 16-24 hours, and MED values in the three cases were recorded, respectively.
The SPF value calculating method comprises the following steps: the SPF value of the test object or the reference object for protecting the single subject is expressed by the following formula:
SPFi
the SPF value of the individual is required to be accurate to one digit after the decimal point, the arithmetic average of the SPF of all the subjects of the tested object is calculated, and the integer part of the arithmetic average is taken as the SPF value of the tested sample. The sampling error of the estimated mean may calculate the standard deviation and standard error of the shuffled data.
The test results are shown in Table 3:
TABLE 3 Sun-protection SPF value test results Table
The human body test results show that the SPF of the tested children sun-proof milk sample is between 25 and 30, and meets the requirements of regulations.
3. Determination of the Long-wave ultraviolet protection index (PFA) of sunscreen cosmetics
The object to be measured: the finished products of examples 1-4
Control: PFA values of 4.4+ -0.6 were formulated according to the PFA assay standard formulation in cosmetic safety Specification (2015 edition).
The subject: 10 people total, 10 people completed, 5 men and 5 women, ages 23-49 years, and average age 28 years, meet the volunteer selection standard of the subjects.
Light source: the xenon arc lamp of the sunlight simulator meets the measurement specification requirements in each performance index.
The inspection method comprises the following steps: the test was carried out according to the specific requirements of cosmetic safety Specification (2015 edition). The subject was tilted forward and irradiated on the back. The minimum erythema dose (MED value) of the subject's skin to ultraviolet irradiation was predicted 24 hours before the test, and the ultraviolet irradiation dose was adjusted based on the prediction result, for testing the test object. On the day of testing, first, a test subject was selected for a time of not less than 30cm on his back 2 Is used in an amount of (2.00.+ -. 0.05) mg/cm 2 Uniformly coating the object to be detected or the reference substance in the area, and then selecting UVA irradiation according to the standard requirement, and irradiating in three conditions: (1) the skin of the subject is not coated with the test object; (2) coating a reference substance; (3) coating the measured object. After 2-4 hours, the experimental results were observed and the MPPD values were recorded in each of the three cases.
The PFA value calculation method comprises the following steps: the PFA value of the test object or the control object for protecting the single subject is expressed by the following formula:
PFAi
the individual PFA value is required to be accurate to one digit after the decimal point, the arithmetic average of the PFA values of all the subjects of the tested object is calculated, and the integral part of the arithmetic average is taken as the PFA value of the tested sample. The sampling error of the estimated mean may calculate the standard deviation and standard error of the shuffled data. The test results are shown in Table 4.
TABLE 4 Table of results of measurement of the Long-wave ultraviolet protection index (PFA)
The PFA value of the tested sample is 8.8-10.1 as shown by the human body test result.
4. Stability test
The children sun-protection milk prepared in the examples 1-4 is subjected to high and low temperature stability experiments at 48 ℃, 40 ℃, 15 ℃ below zero and 45 ℃ to 25 ℃ below zero to 15 ℃ below zero for 3 months, and the stability of the paste is observed. The specific test method comprises the following steps: the child sun protection emulsion is respectively filled into 5 PET plastic bottles with the weight of 50g for each bottle, the bottle cap is tightly covered, 4 samples are respectively placed in a 48 ℃ constant temperature drying box, a 40 ℃ constant temperature drying box, a refrigerator-15 ℃ and a temperature alternation test box, and the other 1 sample is placed in a room temperature environment as a reference sample for continuous observation for 3 months. The specific test results are shown in table 5.
Table 5 stability test results table
The test results show that: the children sun-proof emulsion prepared in the examples 1-4 can pass the high-low temperature stability experiment, and the sun-proof emulsion paste has excellent stability.
In summary, the invention adopts the flaky zinc oxide treated by the surface treatment agent as the sun-screening agent, so that the children sun-screening emulsion meeting the requirements of children cosmetics is obtained, the provided children sun-screening emulsion has better transparency and skin feel performance while ensuring sun screening, and has broad-spectrum sun screening, and the children sun-screening emulsion which can effectively block ultraviolet rays, has excellent stability and has good transparency and skin feel performance can be provided.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes using the descriptions and drawings of the present invention or direct or indirect application in other related technical fields are included in the scope of the present invention.

Claims (10)

1. The children sun protection emulsion is characterized by comprising 20-25% by mass of non-nano physical sun protection agent, wherein the non-nano physical sun protection agent is flaky zinc oxide treated by a surface treatment agent, the surface treatment agent is triethoxy octyl siloxane or hydrogenated polydimethylsiloxane, and the particle size D50 of the flaky zinc oxide is 0.1-0.4 mu m.
2. The child sun milk according to claim 1, further comprising the following raw materials in mass fraction:
an emollient: 30-40%,
emulsifying agent: 3 to 7 percent,
and (3) a thickening agent: 0.4 to 1.0 percent,
humectant: 4-15 percent,
preservative: 0.5 to 1.0 percent,
filler: 0.5 to 1.0 percent,
skin feel modifier: 0.5-5%
Dispersing agent: 0.5-2%.
3. The child sun milk of claim 2, wherein the humectant comprises any one or more of glycerin, propylene glycol, butylene glycol, 1, 3-propanediol, pentylene glycol, and 1, 2-hexanediol.
4. The child sun block of claim 2, wherein the filler is sodium chloride or magnesium sulfate and the preservative is phenoxyethanol or p-hydroxyacetophenone.
5. The child sun emulsion of claim 2, wherein the emollient is any one or more of coco caprylic/capric acid ester, polydimethylsilane, isohexadecane, caprylic/capric triglyceride, isononyl isononanoate, C9-12 alkane, squalane, and jojoba oil.
6. The child sun emulsion according to claim 2, wherein the dispersant is any one or more of sorbitan sesquiisostearate, sorbitan sesquioleate and acrylic acid (ester)/ethylhexyl acrylate/polydimethylsiloxane methacrylate copolymer.
7. The child sun emulsion of claim 1, wherein the emulsifier is any one or more of polyglycerin-2-dimer hydroxystearate, polyglycerin-4-diisostearate/polyhydroxystearate/sebacate, lauryl PEG-9-dimethicone ethyl dimethicone, cetyl PEG/PPG-10/1-dimethicone, and PEG-9-dimethicone ethyl dimethicone.
8. The child sun emulsion of claim 1, wherein the thickener is disteardimethylammonium hectorite or quaternary salt-18 bentonite.
9. The child sun emulsion of claim 1, wherein the skin feel modifier is silica or polymethylsilsesquioxane.
10. A method for preparing the child sun protection milk, which is characterized by being used for preparing the child sun protection milk according to any one of claims 1-9, and specifically comprising the following steps:
s1, weighing the raw materials with mass fractions according to claim 2, sequentially adding the solvent, the humectant and the filler into a water pot, heating to 85 ℃, uniformly stirring, cooling to 25-30 ℃, and adding the preservative to obtain a water phase mixture A;
s2, grinding the sun-screening agent, the skin-moistening agent and the dispersing agent uniformly by using equipment in advance, adding the mixture into an emulsifying pot, adding the emulsifying agent, the thickening agent and the skin-feel regulator, and uniformly stirring the mixture;
s3, stirring is started, the water phase mixture A obtained in the step S1 is added into an emulsifying pot, stirring is carried out for 5 minutes, and then homogenization is started for 1 minute;
and S4, continuously stirring until the mixture is uniform and vacuum defoamation is carried out, and obtaining the child sun-proof emulsion.
CN202311431836.2A 2023-10-31 2023-10-31 Sun protection emulsion for children and preparation method thereof Pending CN117414305A (en)

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