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CN119326672A - Preparation method and application of refreshing composition - Google Patents

Preparation method and application of refreshing composition Download PDF

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Publication number
CN119326672A
CN119326672A CN202411900791.3A CN202411900791A CN119326672A CN 119326672 A CN119326672 A CN 119326672A CN 202411900791 A CN202411900791 A CN 202411900791A CN 119326672 A CN119326672 A CN 119326672A
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parts
stirring
skin
comfort
feed liquid
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CN119326672B (en
Inventor
晏永球
杨卫平
熊菲菲
方娅妮
袁媛
王彩霞
叶玲君
陈羽薇
马云龙
贾福怀
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Ningbo Yufangtang Biotechnology Co ltd
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Ningbo Yufangtang Biotechnology 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
    • A61K8/19Cosmetics 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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; 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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; 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
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • 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
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/494Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/4953Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom containing pyrimidine ring derivatives, e.g. minoxidil
    • 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
    • A61K8/63Steroids; 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
    • A61K8/72Cosmetics 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
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/005Preparations for sensitive skin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/06Preparatory processes
    • 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
    • A61K2800/56Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

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  • Health & Medical Sciences (AREA)
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  • Medicinal Chemistry (AREA)
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  • Emergency Medicine (AREA)
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  • Biotechnology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to a preparation method and application of a comfort-assisting composition, wherein the polydimethylsiloxane can be used as a carrier or a matrix, and organic sunscreens are uniformly dispersed in cosmetics, so that the sun-proof effect and the use experience of the product are improved, the direct contact opportunity of the stimulated organic sunscreens and skin is reduced to the greatest extent, the unique performances of embedding and anti-inflammatory comfort-assisting of a composite structure of a polyorganosiloxane chain and gel aluminum hydroxide/gamma-aluminum oxide fusion are further utilized, the contact of the organic sunscreens with the skin, which have sensitization risks, and the inorganic sunscreens with the skin bad astringent feeling, with the skin care effect substances are greatly reduced, and the sun-proof and skin-care products with the high sun-proof index/long wave ultraviolet protection index, which are comfortable in skin feel and are not easy to be allergic, are prepared.

Description

Preparation method and application of comfort-assisting composition
Technical Field
The invention relates to the technical field of daily chemical skin care products, in particular to a preparation method and application of a comfort-assisting composition for skin care products.
Background
With the improvement of living standard of people, consumers pay more attention to outdoor activities. However, how to prevent the skin from being damaged by ultraviolet rays while enjoying the sun bath is a problem to be solved at present.
At present, the combined sun protection product of the organic synthetic sun protection agent and the inorganic sun protection agent meets the requirements because the sun protection product has quick and durable effect. However, organic sunscreens are affected by human body secretion and illumination environment, have short relative action time, sticky and thick skin feel, are difficult to adapt to high-strength outdoor activities, and have long-term exposure to skin allergy hidden trouble, inorganic sunscreens with nanometer titanium dioxide and nanometer zinc oxide as main angles have long sunscreening time, but have relatively inferior effect to the organic sunscreens, and the cosmetic market is sensitive to the nanometer concept in skin care products, the restrictive regulation is frequent, different adjustment is required in production standard, in addition, the limitation of dispersion conditions in the preparation process of the product containing nanometer components leads to easy formation of aggregation to generate granular feel, and the product presents bad astringent feel on skin, especially the product with high sun protection index, and the uncomfortable feel after being smeared often leads to pain of consumers (especially allergic constitution) for the first time.
In order to solve the above problems, the industry has searched for anti-sensitization and skin feel improvement of the organic/inorganic sunscreen skin care products by using a smooth component such as starch octenyl aluminum succinate, lauroyl lysine, modified mica, cyclopenta silicone oil, and dimethicone and a combination thereof as additives, but no sunscreen care products with a pleasant skin feel and a non-sensitized high sun protection index/long wave ultraviolet protection index have been found so far.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a preparation method of a comfort-assisting composition capable of greatly reducing the irritation of an organic sunscreen agent and the bad astringent feel of an inorganic sunscreen agent so as to meet the requirement of allergic physique.
The second technical problem to be solved by the invention is to provide an application of the comfort-assisting composition in a sun-proof skin care product aiming at the current state of the art, wherein the sun-proof skin care product can be efficiently absorbed, is comfortable in skin feel after being smeared, is not easy to be allergic and has a skin care effect.
The third technical problem to be solved by the invention is to provide a preparation method of the sun-proof skin care product aiming at the current state of the art.
The invention solves at least one of the technical problems by adopting the following technical proposal:
A method of preparing a comfort-aid composition comprising the steps of:
(1) Preparation of superacid catalyst
Uniformly mixing phosphorus pentoxide and crystalline aluminum sulfate, and calcining to obtain a super acidic catalyst;
(2) Preparation of organic sunscreen dispersions
Uniformly mixing ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyl oxyphenol methoxyphenyl triazine, ethylhexyl triazone and dibasic acid ester with butyl hydroxy toluene after heating to obtain a feed liquid A;
(3) Preparation of coated polydimethylsiloxane
Mixing octamethyl cyclotetrasiloxane with the feed liquid A to obtain a feed liquid B;
sequentially reacting the feed liquid B with a super acidic catalyst and hexamethyldisiloxane to obtain an adhesive polydimethylsiloxane finished product liquid, and naming the adhesive polydimethylsiloxane finished product liquid as feed liquid C;
(4) Preparation of hydrated alumina Dispersion slurry
Reacting high-purity sodium aluminum carbonate with sodium hydroxide aqueous solution to obtain hydrated alumina dispersion slurry containing sodium aluminate, and naming the slurry as feed liquid D;
(5) Preparation of smooth modified inorganic powder
Adding nano-scale titanium dioxide and nano-scale zinc oxide into the feed liquid D in batches, depositing a layer of gel Al (OH) 3 on the surfaces of the nano-scale titanium dioxide and zinc oxide particles, and further performing post-treatment to obtain modified nano-scale titanium dioxide/zinc oxide slip inorganic sun-screening agent powder uniformly loaded with gel aluminum hydroxide/gamma-aluminum oxide fusion composite structure, wherein the powder is named as powder E;
(6) Preparation of a comfort-aid composition
And (3) adding the powder E into the feed liquid C, adding cetyl PEG/PPG-10/1 polydimethylsiloxane and dextrin palmitate, and stirring to obtain the target product comfort-assisting composition.
Preferably, the preparation method of the comfort-assisting composition specifically comprises the following steps:
(1) Preparation of superacid catalyst
Mixing phosphorus pentoxide and crystalline aluminum sulfate according to a certain proportion (ensuring that the ratio of phosphorus to sulfur in a final finished product is 1:0.5-0.7), dispersing in liquid carbon dioxide into fine powder by ultrasonic waves, recovering to room temperature within 1 hour, reacting for at least 5 hours under a rapid stirring condition, transferring the mixture after preliminary reaction into a high-temperature furnace, heating to 150-160 ℃ within 1 hour, dehydrating for 2 hours, heating to 850-880 ℃ within 2 hours, calcining for at least 3 hours, fully reacting the mixture and generating a super acid catalyst, naturally cooling the product to room temperature, and granulating to obtain micron-sized fine particles;
(2) Preparation of organic sunscreen dispersions
Uniformly mixing organic sunscreens such as ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyl oxyphenol methoxyphenyl triazine and ethylhexyl triazone, dispersing in 1-1.5 times of dibasic acid ester, heating to 50-60 ℃ to enable the materials to be in a homogeneous state, adding antioxidant butylhydroxytoluene accounting for 0.5-0.8% of the total amount of the materials, and uniformly stirring for later use to obtain a feed liquid A;
(3) Preparation of coated polydimethylsiloxane
Mixing 40-60 parts by weight of octamethyl cyclotetrasiloxane with 30-50 parts by weight of the feed liquid A for 20-30 minutes to obtain a feed liquid B;
Adding 4-5 parts by weight of the super acidic catalyst into the feed liquid B under the stirring condition, controlling the temperature to be 60-65 ℃ and stirring and reacting for 6-8 hours to obtain hydroxyl-terminated polydimethylsiloxane wrapped with the organic sunscreen agent, adding 5-10 parts by weight of hexamethyldisiloxane, controlling the temperature to be 60-70 ℃ and stirring and reacting for 2-3 hours to obtain a crude product wrapped with the polydimethylsiloxane as the sunscreen agent, adding 200-300 parts by weight of purified water, rapidly stirring for 20-30 minutes and then washing, standing for 2-3 hours for layering, discarding a lower water phase, removing impurities such as the catalyst, dehydrating an upper material in the temperature of 60-70 ℃ and obtaining a low-boiling-point hexamethyldisiloxane material for 1.5-3 hours under the pressure of 0.01MPa to obtain a finished product wrapped with the polydimethylsiloxane as the sunscreen agent, and naming the feed liquid C;
(4) Preparation of hydrated alumina Dispersion slurry
5-10 Parts by weight of high-purity sodium aluminum carbonate white powder (the mass content of aluminum oxide is 40%) is added into 50-100 parts by weight of sodium hydroxide aqueous solution with the volume concentration of 2% -5% under the stirring condition, and the mixture is stirred and reacted for 1-2 hours at 70-80 ℃ until the system is nearly transparent, so that hydrated aluminum oxide dispersion slurry containing sodium aluminate is obtained, and the hydrated aluminum oxide dispersion slurry is named as feed liquid D;
(5) Preparation of smooth modified inorganic powder
The material liquid D is added with nanoscale titanium dioxide and nanoscale zinc oxide in batches under the bubbling condition of high-purity carbon dioxide, and nanoscale titanium dioxide and zinc oxide particles with gel Al (OH) 3 deposited on the surfaces are dehydrated, dissociated and homogenized in sequence to obtain the powder E, wherein the following steps are more specific:
Under the stirring condition, 5-10 parts by weight of nano-scale titanium dioxide and 3-8 parts by weight of nano-scale zinc oxide are added into the water-containing alumina dispersion slurry D in batches, the temperature is controlled to be 60-70 ℃, high-purity carbon dioxide is introduced into the bottom of a reactor in a multi-way to be bubbled, the reaction is carried out for 15-20 hours, the pH value of the material reaches 7.2-7.5, a layer of gel Al (OH) 3 is deposited on the surfaces of the nano-scale titanium dioxide and zinc oxide particles, composite particles with micrometer particle diameters are prepared, the finished solution is subjected to plate-frame filter pressing and dehydration, then is conveyed into a colloid mill JML-50 for 3 times, is dried for 1-2 hours in a baking oven at 90-100 ℃, is baked for 0.5-1 hour at 450 ℃, and is then subjected to impact dissociation homogenization by high-pressure air flow of 0.6-0.9 MPa, and the modified micrometer-scale titanium dioxide/nanometer zinc oxide slip type inorganic powder with the uniform loading of gel aluminum hydroxide/gamma-aluminum oxide fusion composite structure is obtained;
(6) Preparation of a comfort-aid composition
13-28 Parts by weight of the slip modified inorganic sun-screening agent powder E is dispersed and put into 50-90 parts by weight of sun-screening agent coated polydimethylsiloxane finished product liquid C under the stirring condition, 1-3 parts by weight of cetyl PEG/PPG-10/1 polydimethylsiloxane is added, the temperature is raised to 60-70 ℃ after uniform stirring, the rotating speed is controlled to 280-350 rpm, stirring is carried out for at least 2 hours until the mixture is in a homogeneous high-viscosity state, 0.3-0.5 part by weight of dextrin palmitate is dispersed and put into the mixture, the rotating speed is controlled to 80-120 rpm, stirring is carried out for at least 1 hour, and cooling is carried out to room temperature, thus obtaining the target product comfort-assisting composition.
Preferably, in the step (1), the ratio of phosphorus to sulfur of the super acidic catalyst is 1 (0.5-0.7).
Preferably, in the step (2), the ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyl oxyphenol methoxyphenyl triazine and ethylhexyl triazone are mixed according to the mass ratio of 8 (5-6) (2.5-3) (1.5-2), the dibasic acid ester is a mixture of dibutyl adipate and diisopropyl sebacate, and the mass ratio of dibutyl adipate to diisopropyl sebacate is 6 (5-8).
Preferably, the comfort-aid composition comprises the following components:
13-28 parts by weight of powder E,
50-90 Parts by weight of feed liquid C,
1-3 Parts by weight of cetyl PEG/PPG-10/1 polydimethylsiloxane,
0.3-0.5 Parts by weight of dextrin palmitate.
Preferably, the powder E is prepared from the following components:
55-110 parts by weight of feed liquid D,
5-10 Parts by weight of nano-scale titanium dioxide,
3-8 Parts of nanoscale zinc oxide;
Wherein the feed liquid D is prepared from the following components:
5 to 10 parts by weight of high-purity sodium aluminum carbonate (the high-purity sodium aluminum carbonate is white powder and is converted into aluminum oxide with the mass content of 40 percent),
50-100 Parts by weight of sodium hydroxide aqueous solution with volume concentration of 2% -5%.
Preferably, the feed liquid C is prepared from the following components:
70-110 parts by weight of feed liquid B,
4-5 Parts by weight of super acid catalyst,
5-10 Parts by weight of hexamethyldisiloxane,
200-300 Parts of water;
wherein, the feed liquid B is prepared from the following components:
30-50 parts by weight of feed liquid A,
40-60 Parts of octamethyl cyclotetrasiloxane.
The sun-proof skin care product applying the comfort-assisting composition comprises the following components in parts by weight:
45-55 parts of a comfort assisting composition,
1-3 Parts of vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer,
1-2 Parts of cetyl PEG/PPG-10/1 polydimethylsiloxane,
2-3 Parts of diethyl aminohydroxybenzoyl hexyl benzoate,
2-4 Parts of triethoxy octyl silane,
1-3 Parts of isostearic acid,
4-7 Parts of butanediol,
2-3 Parts of methyl methacrylate cross-linked polymer,
1-3 Parts of distearyl dimethyl ammonium hectorite,
1-2 Parts of triethyl citrate,
0.5 To 0.8 part of VP/hexadecene copolymer,
1-3 Parts of PEG-10 polydimethylsiloxane,
0.1 To 0.3 part of phenoxyethanol,
1-2 Parts of ethylhexyl glycerin,
1-2 Parts of 1, 3-propylene glycol,
0.3-0.6 Part of extract of flos mori (MAGNOLIA BIONDII),
0.1 To 0.3 part of bisabolol,
0.1 To 0.2 part of dipotassium glycyrrhizinate,
0.2 To 0.3 part of p-hydroxyacetophenone,
0.1 To 0.2 part of tetrahydropyrimidine carboxylic acid,
0.08-0.12 Parts of xanthan gum,
20-25 Parts of water.
The preparation method of the sun-proof skin care product comprises the following steps:
(1) Mixing and stirring vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and cetyl PEG/PPG-10/1 polydimethylsiloxane uniformly, adding diethylamino hydroxybenzoyl hexyl benzoate, and stirring and mixing uniformly at room temperature to obtain an oil phase G;
Mixing triethoxyoctyl silane, triethyl citrate and isostearic acid under stirring, heating to 60-65 ℃, stirring and mixing to be liquid, adding VP/hexadecene copolymer and methyl methacrylate cross-linked polymer in batches, stirring and mixing for at least 1H to be homogeneous thick liquid, dispersing distearyl dimethylammonium hectorite under stirring and mixing for at least 2H to be homogeneous, then adding into a comfort-assisting composition, controlling the rotating speed to be 200-300 rpm, and stirring for at least 3H to be homogeneous high thick state, thus obtaining an oil phase H;
(2) Adding PEG-10 polydimethylsiloxane into two thirds of water under the stirring condition, dissolving to be semitransparent, adding dipotassium glycyrrhizinate, stirring to be nearly transparent, adding phenoxyethanol ethylhexyl glycerol and p-hydroxyacetophenone, and heating to 60-70 ℃ for standby to obtain a water phase I;
(3) Dispersing xanthan gum in 1, 3-propylene glycol and butanediol, stirring to obtain a nearly transparent high-viscosity state, adding one third of water, stirring, adding tetrahydropyrimidine carboxylic acid, flos Hemerocallis (MAGNOLIA BIONDII) extract and bisabolol, stirring, and collecting water phase J;
(4) Under the stirring condition, slowly adding the water phase I into the oil phase H at the temperature of 60-75 ℃, stirring for at least 10 minutes until the system is in an initial state of high-viscosity W/O emulsion, homogenizing for at least 15 minutes at the rotating speed of 3000-5000 rpm, obtaining homogenized high-gloss Gao Chou W/O emulsion, cooling to 35-38 ℃, adding the water phase J under the stirring condition, homogenizing for at least 10 minutes at the rotating speed of 3000-5000 rpm, stirring until the mixture is in a high-gloss homogenized emulsion state, adding the oil phase G, stirring for at least 30 minutes at the rotating speed of 300-400 rpm, homogenizing the high-gloss high-viscosity W/O emulsion, and aging for 24 hours to obtain the target product of the sun-proof skin care product.
Compared with the prior art, the invention has the advantages that the unique performances of embedding, anti-inflammatory and smoothness of a composite structure of the gel aluminum hydroxide/gamma-aluminum oxide fusion, which are easily led into a spiral structure by a polyorganosiloxane chain, are utilized to greatly reduce the contact between an organic sunscreen agent with sensitization risk to skin and an inorganic sunscreen agent with easy bad astringent feel to skin, and the invention combines skin care effect substances to prepare the sunscreen care product with comfortable skin feel and difficult allergy and high sun protection index/long wave ultraviolet protection index.
The specific mechanism of the invention is detailed as follows:
(1) In the organosiloxane compound, a 3d empty orbit on Si in the Si-O bond and a non-covalent electron pair of an O atom form a dpi p pi covalent bond, so that the Si-O bond has partial double bond property and is active. The bond length of the Si-O bond is longer, so that the steric hindrance of the side group rotation is smaller, and the Si-O bond is easy to attack. The electronegativity of Si and O differs greatly, and Si-O bonds have 50% ionic character, making polyorganosiloxanes very sensitive to reactions with ionic character. The bond angle of the Si-O bonds is large, so that the Si-O bonds are easy to rotate. The polyorganosiloxane chains form a helical structure due to the mutual compensation of dpi p pi bonds between Si-O and the mutual compensation between Si-O dipoles, each spiro ring consists of about 6 siloxane units, and the methyl groups are outwards used for shielding (see figure 1). The specific arrangement of the molecular chains of the dimethicone during polymerization maintains a balance of rigidity and flexibility, as well as intermolecular interactions (e.g., van der waals forces, hydrogen bonding, etc.), such that the dimethicone backbone can also form more complex three dimensional structures including helices. Such structures with entrapment characteristics make it very easy to package electronic cloud-offset polar organic compounds including ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyl oxyphenol methoxyphenyl triazine, ethylhexyl triazone, and organic sunscreens containing delocalized pi-bond organic compounds during further polymerization. In addition, the organic sun-screening agent is an oil-soluble substance and has certain compatibility with the polydimethylsiloxane in chemical property. Can be more easily embedded by polydimethylsiloxane. The polydimethylsiloxane can be used as a carrier or a matrix to uniformly disperse the organic sunscreen agent in the cosmetics, so that the sun-screening effect and the use experience of the product are improved, and the direct contact opportunity of the stimulated organic sunscreen agent and skin is reduced to the greatest extent.
(2) The nano titanium dioxide and zinc oxide are used as physical sun-screening agents in sun-screening cosmetics, and have high ultraviolet screening efficiency. However, due to its small particle size, large specific surface area, and extremely high surface energy, agglomerates are easily formed, thereby affecting the dispersibility and transparency of the product, and at the same time, electron-hole pairs generated after absorbing ultraviolet rays may cause discoloration and off-flavor of the product. The gel aluminum hydroxide/gamma-aluminum oxide fusion has various properties beneficial to skin as a coating material, and the astringency of the gel aluminum hydroxide/gamma-aluminum oxide fusion helps to reduce greasy feel and uncomfortable feel of the skin due to the capability of absorbing excessive moisture on the surface of the skin. The antipruritic effect is reduced by combining with acidic substances on the skin surface, and can relieve skin pruritus. The antipruritic effect is also achieved by reducing the release of inflammatory mediators by neutralizing acidic substances on the skin surface.
After the gel aluminum hydroxide/gamma-aluminum oxide fusion is coated outside the nanoscale titanium dioxide and zinc oxide, the agglomeration of the nanoparticles can be reduced, so that the dispersibility of the nanoparticles in cosmetics is improved. The coating layer can protect the nano particles from the external environment, such as illumination, humidity and the like, so that the stability of the nano particles is improved. The astringent, antipruritic and anti-inflammatory effects of gel aluminum hydroxide in the fusion may help reduce the undesirable irritation of the skin by the nanoparticles. The gel aluminum hydroxide has excellent oil absorption and hygroscopicity, can effectively adsorb grease and sweat on the surface of skin, and keeps the skin fresh and dry. This feature allows the cosmetic containing gel aluminum hydroxide to reduce the greasy feel of the skin and make the makeup more durable and fresh. The gel aluminum hydroxide can help to adjust the viscosity of the cosmetics, so that the cosmetics are lighter and smoother in texture, easy to push evenly, and free from heavy feeling. The regulating function makes the cosmetic smooth and easy to pull skin, so as to reduce skin irritation and damage. The particle structure of the gel aluminum hydroxide can increase the smoothness between the skin and the cosmetics, so that the application process is easier and more pleasant. The smooth feel not only improves the use experience, but also is beneficial to the even distribution of cosmetics on the skin. Gel aluminum hydroxide is a substance with stable chemical property, is not easy to chemically react with skin, and does not cause irritation or allergy to the skin. Meanwhile, due to the moderate molecular size, pores are not blocked, and the potential risk to skin is further reduced. The skeleton structure formed by coating gel aluminum hydroxide/gamma-aluminum oxide fusion outside the nanoscale titanium dioxide and zinc oxide can provide certain support and stability, so that the crushed fine powder forms a uniform coating on the skin. The coating can reduce the direct contact area of titanium dioxide and zinc oxide nano particles and skin, thereby reducing astringent feel and other adverse reactions. The smooth modified inorganic sun-screening agent powder containing gel aluminum hydroxide/gamma-aluminum oxide fusion compound structure not only maintains excellent physical sun-screening effect, but also greatly increases the anti-allergy and comfort of the composite powder.
(3) The nano-grade titanium dioxide and nano-zinc oxide coated and modified by the gel aluminum hydroxide/gamma-aluminum oxide fusion can be uniformly dispersed in the organic silicone oil to form stable suspension, which is beneficial to reducing agglomeration and deposition of nano particles on skin, thereby reducing bad astringency. The organic silicone oil has excellent lubricity and compatibility, can form good interface interaction with the coated modified nano particles, is favorable for forming a finer and more uniform coating, can better adapt to the surface of skin, reduces friction between inorganic powder particles and the skin, and further reduces astringent feel.
(4) The extract of Wangchun flower (MAGNOLIA BIONDII) exhibits excellent efficacy as an active ingredient in cosmetics and skin care products, particularly in sunscreening and after-sun repair. The extract of the verruca plana is rich in lignans and can provide effective defense effect before skin is sunburned. The release of various cytokines is inhibited by targeted regulation of damage related molecular patterns (DAMPs) of sunburn cells, thereby reducing the sensitivity of the skin to ultraviolet rays. After the skin is damaged by ultraviolet rays, the flos mori extract can accelerate the regression of erythema, lighten inflammatory response of the skin, and has the effects of relieving and repairing, thereby being beneficial to restoring the health state of the skin. Products containing the extract of the flos mori, such as sun cream, spray, gel and the like, can assist in increasing the SPF value of the sun protection index and provide more comprehensive protection for the skin. The extract of the flos mori has remarkable relieving effect and can relieve discomfort such as redness, tingling and the like of skin. For sensitive skin, this is a very mild skin care ingredient. The extract of the flos mori can also be used as an efficacy adjuvant to be added into sun-proof and whitening products, so that the overall effect of the products is improved.
(5) Tetrahydropyrimidine carboxylic acid, also known as ectoine or Ectoin, is an amino acid derivative with multiple effects. The tetrahydropyrimidine carboxylic acid can effectively isolate ultraviolet rays, resist photoaging and prevent DNA and cell damage caused by ultraviolet rays. It has obvious repairing effect on skin cell DNA damage caused by ultraviolet ray.
One molecule of tetrahydropyrimidine carboxylic acid can complex a plurality of skin free water molecules, so that skin cell free water is structured and continuously locks water, thereby maintaining skin osmotic pressure balance. Because the water-soluble skin-care gel has small molecules, is easy to absorb and is dissolved in water, the skin moisture content can be obviously increased, and the higher the concentration is, the more rapidly the skin moisture content is increased. Under the extreme environments of high temperature, high salt, strong ultraviolet rays and the like, the tetrahydropyrimidine carboxylic acid can keep a good active state, and plays a role in protecting cells. And the structure of enzyme protein in organisms can be stabilized, and the normal operation of molecules in cells can be ensured. The tetrahydropyrimidine carboxylic acid can improve the immunity protection capability of skin cells and increase the cell repair capability. It has strong antimicrobial and allergen resisting ability, and also has good antiallergic and antiinflammatory effects. Tetrahydropyrimidine carboxylic acid enhances fibroblast activity, thereby promoting the production of hyaluronic acid, collagen and elastic fibers. In a word, the tetrahydropyrimidine carboxylic acid is mainly used as an antioxidant and a skin conditioner in cosmetics, and has multiple effects of activating skin, resisting aging, moisturizing, preventing sunburn, repairing, resisting inflammation, relaxing sensitization and the like.
Bisabolol and dipotassium glycyrrhizinate are also the first to improve the anti-allergy and soothing aspects.
The skin-nourishing anti-allergic and soothing functional substances have synergistic effect, so that the sun-proof and skin-protecting product with comfortable skin feel and no allergy and high sun-proof index/long-wave ultraviolet protection index is obtained.
Drawings
Fig. 1 is a structural diagram in the summary of the invention.
Detailed Description
The present invention is described in further detail below with reference to examples.
Example 1:
The preparation method of the comfort-assisting composition in the embodiment is as follows:
(1) The super acidic catalyst is prepared by mixing 5000 g of phosphorus pentoxide with 6700 g of anhydrous aluminum sulfate (the ratio of phosphorus to sulfur in the final product is 1:0.6), dispersing into liquid carbon dioxide by ultrasonic wave to form fine powder, recovering to room temperature within 1 hour, and reacting for 6 hours under the condition of rapid stirring. Transferring the mixture after the preliminary reaction into a high-temperature furnace, heating to 155 ℃ within 1 hour, dehydrating for 2 hours, heating to 860 ℃ within 2 hours, calcining for 3 hours, and fully reacting the mixture to generate the super acid catalyst. The product is naturally cooled to room temperature and granulated into 10-micron-sized grains.
(2) 50L of organic sunscreen agent dispersion is prepared by adding 10 kg of dibutyl adipate and 10 kg of diisopropyl sebacate into a stainless steel batching pot with stirring (jacket heating), stirring to obtain a mixed solution, respectively adding 8 kg of organic sunscreen agent ethylhexyl methoxycinnamate, 6 kg of butyl octanol salicylate, 2.5 kg of bis-ethylhexyl oxyphenol methoxyphenyl triazine and 1.5 kg of ethylhexyl triazinone, stirring and mixing uniformly, heating to 55 ℃ to ensure that the materials are in a homogeneous state, adding 2.3 kg of antioxidant butylhydroxytoluene, and stirring uniformly for standby, wherein the total weight of the mixed solution is 38 kg.
(3) The preparation of the coated polydimethylsiloxane comprises the steps of adding 45 kg of octamethyl cyclotetrasiloxane and 38 kg of the feed liquid A into a 100-liter stainless steel batching pot with stirring quality, and stirring for 25min to obtain 83 kg in total to obtain a feed liquid B;
200L of high-quality stainless steel reaction pot (with large-area cold suspicious device and receiver) with stirring, 83 kg of feed liquid B is added under stirring conditions (with the rotation speed controlled at 120 rpm), 5 kg of super acidic catalyst is added, the temperature controlled at 62 ℃ is used for stirring and reacting for 6 hours, the hydroxyl-terminated polydimethylsiloxane wrapped with the organic sunscreen agent is obtained, 6 kg of hexamethyldisiloxane is added, the temperature controlled at 62 ℃ is used for stirring and reacting for 3 hours, and the crude product liquid wrapped with the sunscreen agent polydimethylsiloxane is obtained. Adding 100 kg of purified water, quickly stirring for 25min, washing, standing for 3h for layering, and removing impurities such as catalyst by discarding the lower water phase. Dehydrating the upper material at 60 ℃ under 0.01MPa and low-boiling-point substances for 3 hours to obtain the finished product liquid coated with the sun-screening agent polydimethylsiloxane, wherein the total weight of the finished product liquid is 88 kg, namely the liquid C.
(4) The preparation of the hydrated alumina dispersion slurry comprises the steps of adding 60 kg of 3% sodium hydroxide aqueous solution into a 100-liter high-quality stainless steel reaction kettle with stirring, dispersing 8 kg of high-purity sodium aluminum carbonate white powder with 40% aluminum oxide content into the kettle in three batches, and carrying out speed-control stirring at 72 ℃ for 80rpm reaction for 2 hours, wherein the system is almost transparent and transparent, and 68 kg of hydrated alumina dispersion slurry containing sodium aluminate and named feed liquid D are obtained.
(5) The preparation of the smooth modified inorganic powder comprises the steps of adding 6 kg of nano-grade titanium dioxide and 4 kg of nano-grade zinc oxide into the hydrated alumina dispersion slurry liquid D in five batches under the condition of controlling the speed and stirring at 180rpm in a 100-liter stainless steel reaction kettle, controlling the temperature to be 60-70 ℃, introducing high-purity carbon dioxide into the bottom of the reactor for bubbling, reacting for 18 hours to ensure that the PH value of the material reaches 7.3, and depositing a layer of gel Al (OH) 3 on the surfaces of the nano-grade titanium dioxide and zinc oxide particles to prepare the composite particles with the particle size of about 50 micrometers. The solution is subjected to plate-frame filter pressing dehydration, then is conveyed into a colloid mill JML-50, is treated under the action of mechanochemical force, is dried for 1h in a 100 ℃ oven, is baked for 0.5h at 500 ℃, and is then subjected to high-pressure airflow impact dissociation homogenization at 0.6MPa, so that 18 kg of uniformly-loaded gel aluminum hydroxide/gamma-aluminum oxide fusion composite structure modified nanoscale titanium dioxide/zinc oxide smooth inorganic sun-screening agent powder, namely powder E, is obtained.
(6) Preparation of a comfort-aid composition:
Adding 88 kg of sun-screening agent polydimethylsiloxane wrapped finished product liquid C into a 120-liter stainless steel reaction kettle, dispersing 18 kg of the slip modified inorganic sun-screening agent powder E into three batches, uniformly stirring, adding 2 kg of cetyl PEG/PPG-10/1 polydimethylsiloxane, uniformly stirring, heating to 62 ℃, stirring for 3h at a speed of 280rpm to a homogeneous high-consistency state, dispersing 0.4 kg of dextrin palmitate, stirring for 1h at a speed of 100rpm, and cooling to room temperature to obtain the high-efficiency sun-screening skin care product comfort-assisting composition of 108.5 kg.
Example 2:
the preparation method of the sun-proof skin care emulsion in the embodiment comprises the following steps:
The formula comprises the following components:
50 kg of the product-assisted comfort composition of example 1,
Vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer 1 kg,
Cetyl PEG/PPG-10/1 polydimethylsiloxane 2 kg,
3 Kg of diethyl aminohydroxybenzoyl hexyl benzoate,
2Kg of triethoxy octyl silane was used,
1 Kg of isostearic acid was used,
4 Kg of butanediol, the weight of the butanediol,
3 Kg of methyl methacrylate cross-linked polymer,
3 Kg of distearyl dimethylammonium hectorite,
2 Kg of triethyl citrate is added to the mixture,
VP/hexadecene copolymer 0.6 kg,
PEG-10 polydimethylsiloxane 2 kg,
0.3 Kg of phenoxyethanol,
2 Kg of ethylhexyl glycerin,
2 Kg of 1, 3-propanediol,
0.6 Kg of extract of flos Wallichii (MAGNOLIA BIONDII) flowers,
0.2 Kg of bisabolol,
Dipotassium glycyrrhizinate 0.2 kg,
0.3 Kg of p-hydroxyacetophenone,
0.2 Kg of tetrahydropyrimidine carboxylic acid,
0.1 Kg of xanthan gum, and the weight of the xanthan gum,
24 Kg of purified water was used for the purification of the water,
The materials are all commercial products and cosmetic grades.
Technological conditions and operation steps:
(1) 10L of stainless steel batching pot with stirring, adding 1 kg of vinyl polydimethylsiloxane/polymethyl siloxane silsesquioxane cross-linked polymer and 2 kg of cetyl PEG/PPG-10/1 polydimethylsiloxane, stirring and mixing uniformly, adding 3 kg of diethylhydroxybenzoyl hexyl benzoate in three batches, stirring and mixing uniformly at room temperature to obtain an oil phase G, wherein the total amount is 6 kg.
Adding 2 kg of triethoxyoctylsilane, 2 kg of triethyl citrate and 1 kg of isostearic acid into a 15-liter stainless steel batching pot with stirring (jacket heating), stirring and mixing until the temperature reaches 62 ℃, stirring and mixing until the mixture is liquid, adding 3 kg of VP/hexadecene copolymer and methyl methacrylate cross-linked polymer in batches, stirring for 1H until the mixture is in a homogeneous thick liquid state, scattering 3 kg of distearyldimethylammonium hectorite into three batches, stirring for 2H until the mixture is in a homogeneous state, and then pumping the materials into a 100-liter belt stirring (jacket heating) stainless steel batching pot containing 50 kg of the efficient sun-screening skin care product comfort assisting composition F, controlling the temperature to 62 ℃, and stirring at 200-300 rpm for 3H until the mixture is in a homogeneous high thick state, thus obtaining an oil phase H, and the total 61 kg.
(2) Adding 16kg of purified water into 30L of stainless steel batching pot with stirring (jacket heating), adding 2 kg of PEG-10 polydimethylsiloxane under stirring, dissolving to be semitransparent, adding 0.2 kg of dipotassium glycyrrhizinate, stirring to be almost transparent, adding 0.3 kg of phenoxyethanol, 2 kg of ethylhexyl glycerol and 0.3 kg of p-hydroxyacetophenone, and heating to 60-70 ℃ for standby, thus obtaining a water phase I, wherein the total amount of the water phase I is 20.8 kg.
Adding 2kg of 1, 3-propylene glycol and 4 kg of butanediol into a 20-liter stainless steel batching pot with stirring (jacket heating), uniformly stirring, scattering into 0.1 kg of xanthan gum in three batches, stirring to be in a nearly transparent high-thick state, adding 8 kg of purified water, uniformly stirring, adding 0.2 kg of tetrahydropyrimidine carboxylic acid, 0.6kg of flos mori (MAGNOLIA BIONDII) extract and 0.2 kg of bisabolol, and uniformly stirring for standby to obtain a water phase J, wherein the total amount is 15.1 kg.
(3) In a 150L stainless steel homogenizing emulsifying pot (with a homogenizer at the bottom), 61 kg of oil phase H is pumped under the stirring condition (with the rotation speed of 50 rpm), the temperature is controlled to 70 ℃, 20.8 kg of water phase I is slowly pumped in within 10 minutes, the stirring is carried out for 15 minutes until the system is in a high-viscosity W/O emulsion initial state, the rotation speed is controlled to 5000rpm for homogenizing for 25 minutes, so as to obtain a homogenized high-gloss Gao Chou W/O emulsion, the homogenized high-gloss water phase J is cooled to 37 ℃, the stirring condition (with the rotation speed of 100 rpm) is controlled, 15.1 kg of water phase J is pumped, the rotation speed is controlled to 3000rpm for homogenizing for 10 minutes, the homogenized high-gloss emulsion is stirred until the homogenized high-gloss water phase is in a liquid state, 6 kg of oil phase G is pumped, the rotation speed is controlled to 300-400 rpm for stirring for 40 minutes, the homogenized high-gloss W/O emulsion is homogenized for 24 hours, and the high-efficiency skin care emulsion product is obtained, and the total of 103 kg is obtained.
Comparative example 1:
preparation of a sunscreen silicone oil physical composition:
By bypassing the process of preparing silicone oil by blending and polymerizing octamethyl cyclotetrasiloxane and organic sunscreens, the organic sunscreens are directly and physically blended by using dimethyl silicone oil and carrier esters with theoretical conversion amount, meanwhile, the process of embedding nano inorganic sunscreens in gel aluminum hydroxide/gamma-aluminum oxide fusion composite structure is omitted, and the physical blending is directly and physically blended by using aluminum hydroxide fine powder with theoretical conversion amount, nano titanium dioxide and nano zinc oxide, thus preparing the silicone oil physical composition of the sunscreens, which is prepared by referring to the formula (scaled down) of the example 1, and is detailed as follows:
(1) The preparation of the organic sunscreen dispersion comprises the steps of adding 10 g of dibutyl adipate and 10 g of diisopropyl sebacate into a 50 ml stainless steel batching cup with stirring (jacket heating), stirring to obtain a mixed solution, adding 8g of ethylhexyl methoxycinnamate, 6g of butyl octanol salicylate, 2.5 g of bis-ethylhexyl oxyphenol methoxyphenyl triazine and 1.5 g of ethylhexyl triazinone serving as the organic sunscreen agents, stirring and mixing uniformly, heating to 55 ℃ to enable the materials to be in a homogeneous state, adding 2.3 g of butyl hydroxy toluene serving as an antioxidant, and stirring uniformly for standby, wherein the total weight of the material liquid A is 38 g.
(2) The preparation of the organic sun-screening agent polydimethylsiloxane physical blending liquid comprises the steps of adding 45 g of simethicone and 38 g of the feed liquid A into a 100 ml stainless steel batching cup with stirring quality, stirring for 25min, and mixing for 83 kg in total to obtain a feed liquid B;
In a 200 ml high-quality stainless steel batching cup with stirring, 83 g of feed liquid B is added under the stirring condition (the rotation speed is controlled to 120 rpm), 6 g of simethicone is added, and stirring and mixing are carried out for 1h at the temperature of 42 ℃ to obtain the organic sun-screening agent polydimethylsiloxane physical blending liquid, 88 g in total, and the name of feed liquid C.
(3) Preparation of inorganic sunscreening powder of aluminium hydroxide cosmetic grade aluminium hydroxide is treated with colloidal mill JML-50 to prepare about 50 μm of fine powder, 12 g of powder D is weighed.
(5) The preparation of the inorganic sun-screening agent powder containing aluminum hydroxide, namely, 12g of micron-sized fine powder aluminum hydroxide, 6g of nano-sized titanium dioxide and 4 g of nano-sized zinc oxide are conveyed into a colloid mill JML-50, mixed treatment is carried out under the action of mechanochemical force, a 100 ℃ oven is used for baking for 1h, then the baking is carried out for 0.5h at 500 ℃ for dehydration, and then the high-pressure air flow of 0.6MPa is used for impact dissociation homogenization, so that 18 g of inorganic sun-screening agent powder containing aluminum hydroxide with extremely high uniformity is obtained, namely, powder E.
(6) Preparation of a sunscreen silicone oil physical composition:
Adding 88 kg of an organic sunscreen agent polydimethylsiloxane physical blending solution C into a 120 ml high-quality stainless steel reactor with stirring, dispersing 18 kg of an inorganic sunscreen agent powder E containing aluminum hydroxide in three batches, stirring uniformly, adding 2 g of cetyl PEG/PPG-10/1 polydimethylsiloxane, heating to 62 ℃ after stirring uniformly, stirring for 3h at a speed of 280rpm to a homogeneous high-viscosity state, dispersing and adding 0.4 g of dextrin palmitate, stirring for 1h at a speed of 100rpm, and cooling to room temperature to obtain the sunscreen agent silicone oil physical composition, wherein the total weight of the sunscreen agent silicone oil physical composition F is 108.5 kg.
Comparative example 2:
the preparation method of the sun protection skin care emulsion comprises the following steps:
The formulation of example 2 was changed to the sunscreen silicone oil physical composition F of comparative example 1 as follows:
the sunscreen silicone oil of comparative example 1 was 50 grams of physical composition F,
Vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer 1 g,
Cetyl PEG/PPG-10/1 polydimethylsiloxane 2 g,
3 G of diethyl aminohydroxybenzoyl hexyl benzoate,
2 G of triethoxy octyl silane,
1 G of isostearic acid, and the total weight of the mixture,
4 G of butanediol, the weight of the butanediol,
Methyl methacrylate cross-linked polymer 3 g,
3 G of distearyl dimethylammonium hectorite,
2G of triethyl citrate, which is prepared from the following components,
VP/hexadecene copolymer 0.6 g,
PEG-10 polydimethylsiloxane 2 g,
0.3 G of phenoxyethanol,
2G of ethylhexyl glycerin,
2G of 1, 3-propanediol,
0.6 G of extract of flos Wallichii (MAGNOLIA BIONDII) flowers,
0.2 G of bisabolol,
0.2 G of dipotassium glycyrrhizinate,
0.3 G of p-hydroxyacetophenone,
0.2 G of tetrahydropyrimidine carboxylic acid,
0.1 Gram of xanthan gum, and the like,
24 G of purified water was used, which was then washed with water,
Process conditions and procedure referring to example 1, a sunscreen skin care emulsion was prepared.
The products prepared in inventive example 2 and comparative example 2 were subjected to performance tests.
Evaluation one, sun-screening Effect test
Human body test of sun protection effect:
The Sun Protection Factor (SPF), also known as sun protection factor, shows the level of sun protection performance that a sunscreen product can exert. The greater the SPF value, the better the sunscreen effect. It is determined based on the Minimum Erythema Dose (MED) of the skin. The minimum erythema dose of the skin increases after the use of the sunscreen.
Sun protection factor (Sun protection factor, SPF) the ratio of MED required to cause erythema in skin protected by the sunscreen cosmetic to MED required to cause erythema in skin not protected is the SPF of the sunscreen cosmetic. This can be expressed as follows:
SPF = MED for skin protected/MED for unprotected skin using sunscreen cosmetics.
Note that the Minimum Erythema Dose (MED) directs the erythema that is clearly visible to the skin in a range up to the minimum dose (J/m 2) or minimum time (seconds) of uv radiation required to irradiate the majority of the area of the spot.
The SPF index is suitable for evaluating the protective effect against UVB.
The long-wave ultraviolet protection index (PFA value) of sunscreen cosmetics is also called UVA protection index. UVA in sunlight irradiates the skin, mainly producing a physiological effect of skin darkening, measured as the minimum sustained blackening amount (MPPD). MPPD is the minimum ultraviolet radiation dose or the shortest radiation time required for generating slight blackening on the skin of the whole irradiation part 2-4 hours after irradiation.
PFA = MPPD of skin protected using sun protection cosmetics/MPPD of unprotected skin.
The sun protection skin care cream of example 2 and comparative example 2 was selected, and the sun protection effect of the product was tested according to the sun protection cosmetic sun protection index test method (human body method) of cosmetic safety technical Specification (2015 edition), and the test results are shown in Table 1.
TABLE 1 Sun protection Effect test results
Sample of SPF PFA
Inventive example 2 high efficiency sun-screening skin care emulsion 50.8 16.5
Comparative example 2 Sun-protection skin care emulsion 42.2 11.2
As can be seen from Table 1, the sun protection factor of the high-efficiency sun protection skin care emulsion prepared in the embodiment 2 of the invention can reach SPF50+PA++, and the sun protection factor of the sun protection skin care emulsion in the comparative example 2 is obviously reduced compared with that in the embodiment 2.
Evaluation II skin smoothness
The basic performances of the high-efficiency sun-proof skin care emulsion prepared in the example 2 and the sun-proof skin care emulsion sample in the aspect of skin feel of the comparative example 2 are measured, and the measurement results are shown in table 2. From the test results of Table 2, the sample of example 2 of the present invention was superior to comparative example 2 in terms of skin feel smoothness.
TABLE 2 determination of skin Shu Huashuang core index
Evaluation of greasy skin blocking Property
The combing property related mechanical data of the high-efficiency sun-proof skin care emulsion of the embodiment 2 and the sun-proof skin care emulsion of the comparative embodiment 2 after soaking and drying the hair are tested by a tensile force measuring instrument method, and the viscosity and greasy resistance of the skin are indirectly estimated.
(1) Summary of the invention
The tensile tester is a special tester for evaluating hair combing performance, simulates the action of combing hair by a person through a standard comb, and combing a bundle of hair and recording the hair by a terminal. When the comb passes through the hair fibers, it shows the force (in gf) that is loaded in a specified displacement (in mm) when it is stretched against the resistance of the hair. The adhesive greasiness of aloe is indirectly estimated by detecting the change index of the combing force of the hair bundles before and after the sample is soaked.
(2) Materials and methods
(2.1) Main instruments and materials
A tension meter;
A constant temperature and humidity incubator;
a plurality of hair bundles with the length of 50cm and the weight of about 16g;
The high-efficiency sun-proof skin care emulsion of the embodiment 2 and the sun-proof skin care emulsion of the comparative example 2 are prepared into 10% water diluted dispersion diluted emulsion by an ultrasonic dispersion device.
(2.2) Pretreatment of hair strands
Several hair strands of the same length (50 cm) and weight (about 16 g) were prepared. Firstly, washing twice with tap water at 40 ℃, then placing the hair bundle in a beaker filled with 5g of sodium dodecyl sulfate and 1000mL of water, heating to 80 ℃ for soaking, then placing the beaker in a constant temperature and humidity box at 45 ℃ for two hours, and finally, washing with tap water until no foam exists, and naturally airing.
And (3) treating a sample of the sun-proof skin care emulsion, namely weighing 4g of a sample of the sun-proof skin care emulsion, diluting and dispersing the diluted emulsion, rubbing the sample onto the treated hair bundle, standing the hair bundle for 30 minutes, flushing the hair bundle with tap water, and blowing the hair bundle for thirty minutes by a natural wind blower until the hair bundle is nearly dried.
(2.3) Test of combing Property
The dry comb properties of the hair bundles after the sun-proof skin care lotion is diluted, dispersed and diluted emulsion sample treatment are respectively measured on a tension meter.
① Connecting a host power supply, turning on a computer, and preheating an instrument for more than half an hour;
② All the samples forming the test sample are collected together, each sample is identified, software is opened, a new sample is created, a test method is selected, and the new sample is named;
③ Firstly combing hair by using a plastic comb, then fixing a hair sample to be tested by using a proper clamp, and naturally placing the hair bundle in the middle of the comb;
④ After the calibration and zeroing of the instrument are completed, the test of the hair bundle is started, the hair bundle is stretched at the speed of 300mm/min, the displacement is 200ram, and the load value between 100 mm and 200mm of displacement is taken. To reduce measurement errors due to hair-strand differences, the same hair-strand was repeated 5 times and averaged (the program automatically recorded the data and calculated the average).
(3) Results and discussion
The test mainly examines the influence degree of the high-efficiency sun-proof skin care emulsion of the invention example 2 and the sun-proof skin care emulsion of the invention comparative example 2 on the hair comb property, and the average value (gf) of the load of the hair bundles after the two types of the sun-proof skin care emulsion are diluted and dispersed by the sun-proof skin care emulsion sample are tested and recorded by a tension meter to compare the dry hair comb physical property, and the data result is shown in Table 3 in detail.
TABLE 3 Table 3
As can be seen from Table 3, the average load value (gf) of the hair drying comb after treatment with the skin care lotion of example 2 of the present invention is significantly smaller than that of the skin care lotion of comparative example 2, which indirectly indicates that the product of the present invention has very little blocking force on the greasy skin after being applied to the skin, and the skin has no coarse-grained and astringent feel.
Evaluation of Patch test
Test article A plaque test was performed on the sample prepared in example 2 to detect the potential for adverse effects on human skin.
The total number of subjects is 38, wherein 18 men and 20 women are aged 20-40 years, and the subjects accord with the admission of tested volunteers. The standard test method is that 0.03mL of sample is taken by a syringe and placed in a medicine chamber of the spot test adhesive tape, the spot test adhesive tape with the sample is immediately and longitudinally stuck on the normal skin of the left forearm from the lower part, and the medicine chambers are simultaneously lightly pressed one by one to expel air and uniformly distribute test objects. The test sites were marked for observation. The blank group was subjects without product.
Analysis of results the plaque tape was removed after 24 hours, the skin reactions were observed after half an hour, 24 hours and 48 hours, respectively, and the results of the skin reactions were recorded according to CTFA guidelines for analysis.
The criteria for the identification of skin irritation test are shown in Table 4 below.
TABLE 4 skin irritation test identification criteria
The test results are shown in Table 5 below.
TABLE 5 skin irritation test results Table
As can be seen from Table 5, the high-efficiency sunscreen skin care cream prepared in example 2 of the present invention does not cause irritation reaction, and has good safety.
Evaluating five improvement of skin after application in terms of elasticity improvement, pore refinement, reduction of number of fish tail lines, reduction of volume of fish tail lines, and the like of cosmetic core data
The skin-improving elasticity/wrinkle resistance/pore shrinkage/moisture retention index of the high-efficiency sun-protecting skin cream of example 2 of the present invention and the skin-protecting skin cream of comparative example 2 were compared by using a test instrument (VISIA-CR Corneometer CM825 Cutometer MPA585 Primos), and are shown in Table 6.
TABLE 6
It is noted that the subject population (16 persons) used the example 2 high-efficiency sun-screening skin care cream of the present invention on the left side of the face in a single time, while the comparative example 2 sun-screening skin care cream was used on the right side of the face.
In conclusion, the high-efficiency sun-proof skin care emulsion of the embodiment 2 of the invention is obviously superior to the sun-proof skin care emulsion of the comparative embodiment 2 in the skin-care and beauty core data of elasticity improvement, pore refinement, reduction of the quantity of fish tail lines, reduction of the volume of fish tail lines and the like.

Claims (10)

1. A method for preparing a comfort-aid composition, which is characterized by comprising the following steps:
(1) Preparing a super acid catalyst, namely uniformly mixing phosphorus pentoxide and crystalline aluminum sulfate, and calcining to obtain the super acid catalyst;
(2) Preparing organic sunscreen agent dispersion materials, namely heating ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyl oxyphenol methoxyphenyl triazine, ethylhexyl triazone and dibasic acid ester, and uniformly mixing with butyl hydroxy toluene to obtain a feed liquid A;
(3) Preparing coated polydimethylsiloxane, namely stirring and mixing octamethyl cyclotetrasiloxane with the feed liquid A to obtain feed liquid B, and sequentially reacting the feed liquid B with a super acidic catalyst and hexamethyldisiloxane to obtain coated polydimethylsiloxane finished product liquid which is named as feed liquid C;
(4) Preparing hydrated alumina dispersion slurry, namely reacting high-purity sodium aluminum carbonate with sodium hydroxide aqueous solution to obtain hydrated alumina dispersion slurry containing sodium aluminate, and naming the hydrated alumina dispersion slurry as feed liquid D;
(5) Preparing smooth modified inorganic powder, namely adding nano-scale titanium dioxide and nano-scale zinc oxide into the feed liquid D in batches, depositing a layer of gel Al (OH) 3 on the surfaces of the nano-scale titanium dioxide and zinc oxide particles, and further performing post-treatment to obtain modified nano-scale titanium dioxide/zinc oxide smooth inorganic sun-screening agent powder uniformly loaded with gel aluminum hydroxide/gamma-aluminum oxide fusion, wherein the powder is named as powder E;
(6) The preparation method of the comfort assisting composition comprises the steps of adding powder E into feed liquid C, adding cetyl PEG/PPG-10/1 polydimethylsiloxane and dextrin palmitate, and stirring to obtain the target product of the comfort assisting composition.
2. The method for preparing a comfort-aid composition according to claim 1, wherein the ratio of phosphorus to sulfur of the super acid catalyst obtained in the step (1) is 1 (0.5-0.7).
3. The method for preparing the comfort-assisting composition according to claim 1, wherein in the step (2), the mass ratio of the ethylhexyl methoxycinnamate, the butyl octanol salicylate, the bis-ethylhexyl oxyphenol methoxyphenyl triazine and the ethylhexyl triazone is 8 (5-6): 2.5-3): 1.5-2.
4. The method for preparing a comfort-assisting composition according to claim 1, wherein in the step (2), the dibasic acid ester is a mixture of dibutyl adipate and diisopropyl sebacate, and the mass ratio of dibutyl adipate to diisopropyl sebacate is 6 (5-8).
5. The method for preparing a comfort-assisting composition according to claim 1, wherein in the step (5), the feed liquid D is fed with nano-sized titanium dioxide and nano-sized zinc oxide in batches under the bubbling condition of high-purity carbon dioxide, and the nano-sized titanium dioxide and zinc oxide particles with gel Al (OH) 3 deposited on the surfaces are dehydrated, dissociated and homogenized in sequence to obtain the powder E.
6. The method for preparing a comfort-aid composition according to any one of claims 1 to 5, characterized in that:
The comfort-aid composition comprises the following components:
13-28 parts by weight of powder E,
50-90 Parts by weight of feed liquid C,
1-3 Parts by weight of cetyl PEG/PPG-10/1 polydimethylsiloxane,
0.3-0.5 Parts by weight of dextrin palmitate.
7. A process for preparing a comfort-aid composition according to claim 6, characterized in that:
the powder E is prepared from the following components:
55-110 parts by weight of feed liquid D,
5-10 Parts by weight of nano-scale titanium dioxide,
3-8 Parts of nanoscale zinc oxide;
Wherein the feed liquid D is prepared from the following components:
5-10 parts by weight of high-purity sodium aluminum carbonate,
50-100 Parts by weight of 2-5% sodium hydroxide aqueous solution.
8. A process for preparing a comfort-aid composition according to claim 6, characterized in that:
The feed liquid C is prepared from the following components:
70-110 parts by weight of feed liquid B,
4-5 Parts by weight of super acid catalyst,
5-10 Parts by weight of hexamethyldisiloxane,
200-300 Parts of water;
wherein, the feed liquid B is prepared from the following components:
30-50 parts by weight of feed liquid A,
40-60 Parts of octamethyl cyclotetrasiloxane.
9. A sunscreen skin care product to which the comfort-aid composition of any one of claims 1 to 8 is applied, characterized in that:
the coating comprises the following components in parts by weight:
45-55 parts of a comfort assisting composition,
1-3 Parts of vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer,
1-2 Parts of cetyl PEG/PPG-10/1 polydimethylsiloxane,
2-3 Parts of diethyl aminohydroxybenzoyl hexyl benzoate,
2-4 Parts of triethoxy octyl silane,
1-3 Parts of isostearic acid,
4-7 Parts of butanediol,
2-3 Parts of methyl methacrylate cross-linked polymer,
1-3 Parts of distearyl dimethyl ammonium hectorite,
1-2 Parts of triethyl citrate,
0.5 To 0.8 part of VP/hexadecene copolymer,
1-3 Parts of PEG-10 polydimethylsiloxane,
0.1 To 0.3 part of phenoxyethanol,
1-2 Parts of ethylhexyl glycerin,
1-2 Parts of 1, 3-propylene glycol,
0.3 To 0.6 part of extract of the flos mori,
0.1 To 0.3 part of bisabolol,
0.1 To 0.2 part of dipotassium glycyrrhizinate,
0.2 To 0.3 part of p-hydroxyacetophenone,
0.1 To 0.2 part of tetrahydropyrimidine carboxylic acid,
0.08-0.12 Parts of xanthan gum,
20-25 Parts of water.
10. A method of preparing a sunscreen skin care product according to claim 9, comprising the steps of:
(1) Mixing and stirring vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer and cetyl PEG/PPG-10/1 polydimethylsiloxane uniformly, adding diethylamino hydroxybenzoyl hexyl benzoate, and stirring and mixing uniformly at room temperature to obtain an oil phase G;
Mixing triethoxyoctyl silane, triethyl citrate and isostearic acid under stirring, heating to 60-65 ℃, stirring and mixing to be liquid, adding VP/hexadecene copolymer and methyl methacrylate cross-linked polymer in batches, stirring and mixing for at least 1H to be homogeneous thick liquid, dispersing distearyl dimethylammonium hectorite under stirring and mixing for at least 2H to be homogeneous, then adding into a comfort-assisting composition, controlling the rotating speed to be 200-300 rpm, and stirring for at least 3H to be homogeneous high thick state, thus obtaining an oil phase H;
(2) Adding PEG-10 polydimethylsiloxane into two thirds of water under the stirring condition, dissolving to be semitransparent, adding dipotassium glycyrrhizinate, stirring to be nearly transparent, adding phenoxyethanol ethylhexyl glycerol and p-hydroxyacetophenone, and heating to 60-70 ℃ for standby to obtain a water phase I;
(3) Dispersing xanthan gum in 1, 3-propylene glycol and butanediol, stirring until the mixture is in a nearly transparent high-viscosity state, adding one third of water, stirring uniformly, adding tetrahydropyrimidine carboxylic acid, flos Hedyotidis Diffusae extract and bisabolol, and stirring uniformly for standby to obtain a water phase J;
(4) Under the stirring condition, slowly adding the water phase I into the oil phase H at the temperature of 60-75 ℃, stirring for at least 10 minutes until the system is in an initial state of high-viscosity W/O emulsion, homogenizing for at least 15 minutes at the rotating speed of 3000-5000 rpm, obtaining homogenized high-gloss Gao Chou W/O emulsion, cooling to 35-38 ℃, adding the water phase J under the stirring condition, homogenizing for at least 10 minutes at the rotating speed of 3000-5000 rpm, stirring until the mixture is in a high-gloss homogenized emulsion state, adding the oil phase G, stirring for at least 30 minutes at the rotating speed of 300-400 rpm, homogenizing the high-gloss high-viscosity W/O emulsion, and aging for 24 hours to obtain the target product of the sun-proof skin care product.
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