CN115105430A - Powder surface composite treating agent, surface modified powder and application thereof - Google Patents

Powder surface composite treating agent, surface modified powder and application thereof Download PDF

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CN115105430A
CN115105430A CN202210565235.XA CN202210565235A CN115105430A CN 115105430 A CN115105430 A CN 115105430A CN 202210565235 A CN202210565235 A CN 202210565235A CN 115105430 A CN115105430 A CN 115105430A
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powder
polydimethylsiloxane
coupling agent
polyethylene glycol
organic silicon
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CN115105430B (en
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陈宗乐
吴建军
杨小娟
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Shanghai Co Fun Biotech Co ltd
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Shanghai Co Fun Biotech Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A61K8/894Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
    • 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
    • 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
    • A61K8/23Sulfur; Selenium; Tellurium; 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
    • A61K8/25Silicon; 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
    • A61K8/27Zinc; 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
    • A61K8/29Titanium; 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8176Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • 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
    • A61K8/895Polysiloxanes containing silicon bound to unsaturated aliphatic groups, e.g. vinyl 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
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/12Face or body powders for grooming, adorning or absorbing
    • 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
    • A61K2800/60Particulates further characterized by their structure or composition
    • A61K2800/61Surface treated
    • A61K2800/614By macromolecular compounds

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Abstract

The invention relates to a powder surface composite treating agent, surface modified powder and application thereof. The powder surface composite treating agent comprises a coupling agent, an organic silicon elastomer and a film forming agent, wherein the coupling agent is selected from a coupling agent with an alkoxy group and an organic silicon chain, the organic silicon elastomer is selected from a polydimethylsiloxane cross-linked polymer with hydroxyl, and the mass ratio of the coupling agent to the organic silicon elastomer to the film forming agent is 1:0.1:0.1-1:1: 0.7. The surface modified powder obtained by the powder surface composite treating agent has good dispersion stability and skin-sticking property, and can be widely applied to cosmetics of powder systems and various oil phase systems.

Description

Powder surface composite treating agent, surface modified powder and application thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a powder surface composite treating agent, surface modified powder and application thereof.
Background
The powder is an important component of cosmetics and has the functions of skeleton support, color endowment, skin feeling improvement, flaw covering, ultraviolet shielding and the like. The base powder has good hydrophilicity and excellent dispersibility in an aqueous phase system, and is suitable for cosmetics in an aqueous phase system. In order to improve the dispersion effect of the powder in the oil phase system, the surface of the base powder can be modified by adopting an organic surface modifier, so that the modified powder has good lipophilicity.
Conventional organic surface modifiers include coupling agents, surfactants, silicones, high molecular weight polymers, and the like. Wherein, the coupling agent can improve the hydrophobicity and the grease compatibility of the basic powder, the surfactant can enhance the emulsification and dispersion effects, the compatibility of the organic silicon and the basic powder is good, so that the surface modified powder has smooth and light skin feel, and the high molecular polymer can endow the powder with excellent grease compatibility. However, the traditional organic surface modifier has single performance, cannot enable the surface modified powder to have good dispersion stability and skin-adhering property at the same time, and has great limitation in practical application.
Disclosure of Invention
In view of the above, it is necessary to provide a powder surface composite treating agent, a surface modified powder thereof and applications thereof; the surface modified powder obtained by the powder surface composite treating agent has good dispersion stability and skin-sticking property, and can be widely applied to cosmetics of powder systems and oil phase systems.
The powder surface composite treating agent comprises a coupling agent, an organic silicon elastomer and a film forming agent, wherein the coupling agent is selected from coupling agents with alkoxy groups and organic silicon chains, the organic silicon elastomer is selected from polydimethylsiloxane cross-linked polymers with hydroxyl groups, and the mass ratio of the coupling agent to the organic silicon elastomer to the film forming agent is 1:0.1:0.1-1:1: 0.7.
In one embodiment, the silicone elastomer is selected from at least one of a polydimethylsiloxane crosspolymer having a polyethylene glycol chain, a polydimethylsiloxane crosspolymer having a polypropylene glycol chain, and a polydimethylsiloxane crosspolymer having a polyglycerol chain.
In one embodiment, the silicone elastomer is selected from the group consisting of polyethylene glycol-12 dimethicone crosspolymer, polyethylene glycol-12 dimethicone crosspolymer with polypropylene glycol-20, dimethicone crosspolymer with bis-isobutylpolypropylene glycol-20, bis-isobutylpolyethylene glycol/polypropylene glycol-20/35/dimethicone crosspolymer, bis-isobutylpolyethylene glycol/polypropylene glycol-10/7/dimethicone crosspolymer, polyethylene glycol/polypropylene glycol/butylene/dimethicone crosspolymer, polyethylene glycol/lauryl dimethicone crosspolymer, dimethicone polyethylene glycol-10/15 crosspolymer, At least one of polydimethylsiloxane polyethylene glycol-15 cross-linked polymer, bis-polyethylene glycol-15 polydimethylsiloxane/isophorone diisocyanate cross-linked polymer, methoxy polyethylene glycol-23 methacrylate/glycerol diisostearate methacrylate cross-linked polymer and polydimethylsiloxane/polyglycerol-3 cross-linked polymer.
In one embodiment, the alkoxy group in the coupling agent is selected from at least one of methoxy group and ethoxy group.
In one embodiment, the coupling agent is selected from at least one of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, triethoxysilylethylpolydimethylsiloxyethyldimethicone, trimethoxysilylpolydimethylsiloxane.
In one embodiment, the film former is selected from at least one of trimethylsiloxysilicate, polymethylsilsesquioxane, polypropylsilsesquioxane, acrylate/trimethicone methacrylate copolymer, acrylate/polydimethylsiloxane copolymer, diphenylsiloxyphenyltrimethicone, polyvinylpyrrolidone/hexadecene copolymer.
The surface modified powder obtained by adopting the powder surface composite treating agent comprises base powder and an organic layer coated on the surface of the base powder.
In one embodiment, the mass fraction of the base powder in the surface-modified powder is 85% -99%.
In one embodiment, the base powder is at least one selected from titanium dioxide, zinc oxide, iron oxide, chromium oxide, ultramarine, talc, mica, clay, boron nitride, pearly luster, barium sulfate, calcium sulfate, pearl powder, magnesium sulfate, aluminum sulfate, bismuth oxychloride, zinc carbonate, magnesium carbonate, calcium carbonate and calcium phosphate.
The application of the surface modified powder in cosmetics of powder system and oil phase system.
In the powder surface composite treating agent, on one hand, the coupling agents can be chemically bonded to form a film with a net structure on the surface of the basic powder, so that the surface of the basic powder is organized and hydrophobic effect is achieved, and on the other hand, the coupling agents can also be chemically bonded with the basic powder and the organic silicon elastomer, so that not only can an organic silicon elastomer chain segment be introduced into the film, but also the coupling agents can be stably combined with the basic powder. Meanwhile, the film-forming agent can be recrystallized and deposited on the surface of the basic powder in the surface treatment process of the basic powder and is combined with the film to form an organic layer, so that a three-dimensional organic net structure is formed on the surface of the basic powder through the synergistic effect of the film-forming agent, the coupling agent, the organic silicon elastomer and the organic silicon elastomer, the steric hindrance effect is further enhanced, and the surface modified powder obtained by the powder surface composite treatment agent can have good dispersion stability and skin-adhering property.
Therefore, the surface modified powder can be widely applied to cosmetics of powder systems and oil phase systems as a raw material, so that the cosmetics have good grease compatibility and stability, and are good in skin adhesion and skin feel.
Detailed Description
The powder surface composite treating agent and the surface-modified powder and the use thereof provided by the present invention will be further described below.
The powder surface composite treating agent provided by the invention comprises a coupling agent, an organic silicon elastomer and a film forming agent, wherein the coupling agent is selected from coupling agents with alkoxy groups and organic silicon chains, the organic silicon elastomer is selected from polydimethylsiloxane cross-linked polymers with hydroxyl groups, and the mass ratio of the coupling agent to the organic silicon elastomer to the film forming agent is 1:0.1:0.1-1:1: 0.7.
The invention selects the coupling agent simultaneously having alkoxy groups and organosilicon chains, wherein the alkoxy groups in the coupling agent can be hydrolyzed to generate silanol, on one hand, the silanol can react with each other to generate a siloxane bond, and a film with a net structure is formed on the surface of the basic powder, so that the surface of the basic powder is organized and hydrophobic, on the other hand, the silanol can also react with hydroxyl on the surface of the basic powder and hydroxyl in an organosilicon elastomer structure, and further generates the siloxane bond through dehydration condensation, thus not only introducing organosilicon elastomer chain segments into the film, but also being stably combined with the basic powder.
Meanwhile, compared with the traditional coupling agent containing an ethoxy active group, the coupling agent provided by the invention can enable the basic powder to have wider grease compatibility and more excellent skin feel and skin sticking performance, so that the actual application range of the coupling agent is expanded.
Specifically, the alkoxy group in the coupling agent is selected from at least one of methoxy group and ethoxy group.
Further, the coupling agent is at least one selected from triethoxysilylethyl polydimethylsiloxyethyl hexyl polydimethylsiloxane, triethoxysilylethyl polydimethylsiloxyethyl polydimethylsiloxane and trimethoxysilyldimethyl polysiloxane, and is preferably triethoxysilylethyl polydimethylsiloxyethyl hexyl polydimethylsiloxane.
The silicone elastomer is at least one selected from the group consisting of a polydimethylsiloxane crosspolymer having a polyethylene glycol chain, a polydimethylsiloxane crosspolymer having a polypropylene glycol chain, and a polydimethylsiloxane crosspolymer having a polyglycerol chain.
In one embodiment, the silicone elastomer is selected from the group consisting of polyethylene glycol-12 polydimethylsiloxane (PEG-12 polydimethylsiloxane) crosspolymer, polyethylene glycol-12 polydimethylsiloxane (PEG-12 polydimethylsiloxane) crosspolymer with polypropylene glycol-20 (PPG-20), polydimethylsiloxane crosspolymer with bis-isobutyl polypropylene glycol-20 (bis-isobutyl PPG-20), bis-isobutyl polyethylene glycol/polypropylene glycol-20/35/polydimethylsiloxane (bis-isobutyl PEG/PPG-20/35/polydimethylsiloxane) crosspolymer, bis-isobutyl polyethylene glycol/polypropylene glycol-10/7/polydimethylsiloxane (bis-isobutyl PEG/PPG-10/7/polydimethylsiloxane) Alkyl) crosspolymer, polyethylene glycol/polypropylene glycol/butylene/polydimethylsiloxane (PEG/PPG/butylene/polydimethylsiloxane) crosspolymer, polyethylene glycol-15/lauryl polydimethylsiloxane (PEG-15/lauryl polydimethylsiloxane) crosspolymer, polydimethylsiloxane polyethylene glycol-10/15 (polydimethylsiloxane PEG-10/15) crosspolymer, polydimethylsiloxane polyethylene glycol-15 (polydimethylsiloxane PEG-15) crosspolymer, bis-polyethylene glycol-15 polydimethylsiloxane/isophorone diisocyanate (bis-PEG-15 polydimethylsiloxane/IPDI) crosspolymer, methoxy polyethylene glycol-23 methacrylate/glycerol diisostearate methacrylate (methoxy PEG-23) Methacrylate/glyceryl diisostearate methacrylate), polydimethylsiloxane/polyglyceryl-3 crosspolymer, preferably PEG-12 polydimethylsiloxane crosspolymer.
The film forming agent can form a film on the surface of the basic powder, so that the friction force between basic powder particles and between the basic powder particles and the skin is greatly reduced, and the skin feel of the surface modified powder is favorably improved. More importantly, the film-forming agent can be recrystallized and deposited on the surface of the basic powder in the surface treatment process of the basic powder and combined with a film to form an organic layer, so that a three-dimensional organic net structure is formed on the surface of the basic powder through the synergistic effect of the film-forming agent, the coupling agent, the organic silicon elastomer and the organic silicon elastomer, the steric hindrance effect is further enhanced, and the surface modified powder obtained by the powder surface composite treatment agent can have good dispersion stability and skin-adhering property.
Specifically, the film forming agent is selected from at least one of trimethylsiloxysilicate, polymethylsilsesquioxane, polypropylsilsesquioxane, acrylic acid (ester)/polytrimethylsiloxane methacrylate copolymer, acrylic acid (ester)/polydimethylsiloxane copolymer, diphenylsiloxyphenyltrimethicone and polyvinylpyrrolidone/hexadecene copolymer, and is preferably trimethylsiloxysilicate.
The organic silicon elastomer is in a gel state at normal temperature, and a volatile oil solvent can be adopted to prepare the organic silicon elastomer into an organic silicon elastomer solution. Wherein, in the organic silicon elastomer solution, the mass ratio of the organic silicon elastomer to the volatile oil solvent is 1:3-1:15, preferably 1:3-1: 10; the viscosity of the silicone elastomer solution is 5 mPas-1000 mPas, preferably 5 mPas-600 mPas.
Because the film forming agent is solid at normal temperature, the film forming agent can also be prepared into a film forming agent solution by adopting a volatile oily solvent. Wherein in the film forming agent solution, the mass ratio of the film forming agent to the volatile oily solvent is 1:1-1:10, preferably 1:1-1: 5; the viscosity of the film-forming agent solution is 3 mPas-500 mPas, preferably 3 mPas-200 mPas.
In order to provide a hydrolysis reaction environment required by an alkoxy group in the coupling agent and improve the bonding rate of the coupling agent on the surface of the base powder, water can be used as one of the solvents to prepare the coupling agent into a coupling agent solution.
Furthermore, in order to reduce the viscosity of the coupling agent solution and thereby improve the dispersion efficiency of the coupling agent in the base powder and make it sufficiently contact with the surface of the base powder, the solvent for preparing the coupling agent solution may further contain a volatile oil solvent.
Since ethanol can further enhance the compatibility between the volatile oil-based solvent, the coupling agent, and water, in one embodiment, the solvent in which the coupling agent solution is formulated is preferably a volatile oil-based solvent, ethanol, and water. Wherein, in the coupling agent solution, the mass ratio of the coupling agent, the volatile oily solvent and the ethanol to the water is 3:3:1:0.5-3:10:3:0.5, preferably 3:3:1:0.5-3:5:1: 0.5; the viscosity of the coupling agent solution is 5 mPas-600 mPas, preferably 5 mPas-500 mPas.
In order to completely mix the coupling agent, the organic silicon elastomer and the film forming agent in the powder surface composite treating agent, the prepared coupling agent solution, the organic silicon elastomer solution and the film forming agent solution can be mixed, so that the powder surface composite treating agent is obtained.
Specifically, the volatile oil solvent is at least one selected from volatile silicone oil and volatile alkane. Wherein the volatile silicone oil is selected from at least one of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane and polydimethylsiloxane, preferably at least one of decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane and polydimethylsiloxane; the volatile alkane is selected from at least one of C8 alkane, C9 alkane, C10 alkane, C11 alkane, C12 alkane, C13 alkane, C14 alkane, C15 alkane, C16 alkane, C17 alkane, C18 alkane, C19 alkane and C20 alkane.
The invention also provides surface modified powder obtained by adopting the powder surface composite treating agent, and the surface modified powder comprises base powder and an organic layer covered on the surface of the base powder.
The surface modified powder can be obtained by carrying out surface treatment on the basic powder by using the powder surface composite treating agent provided by the invention. In the surface modified powder, because the powder surface composite treating agent and the surface of the basic powder have rich chemical bonding, the surface modified powder has better and more stable performance.
In one embodiment, the mass fraction of the base powder in the surface-modified powder is 85% to 99%.
Specifically, the base powder is at least one selected from titanium dioxide, zinc oxide, iron oxide, chromium oxide, ultramarine, talc, mica, clay, boron nitride, pearly luster, barium sulfate, calcium sulfate, pearl powder, magnesium sulfate, aluminum sulfate, bismuth oxychloride, zinc carbonate, magnesium carbonate, calcium carbonate and calcium phosphate. The titanium dioxide is selected from at least one of micron-sized titanium dioxide and nano-sized titanium dioxide, the iron oxide is selected from at least one of yellow iron oxide, red iron oxide and black iron oxide, the chromium oxide is selected from green chromium oxide, the mica is selected from at least one of sericite, synthetic fluorophlogopite and crystal mica, the clay is selected from at least one of bentonite and kaolin, the calcium sulfate is selected from calcium sulfate hydrate, the zinc carbonate is selected from basic zinc carbonate, the magnesium carbonate is selected from basic magnesium carbonate, and the calcium phosphate is selected from calcium pyrophosphate.
The invention also provides application of the surface modified powder in cosmetics of powder systems and oil phase systems.
The surface modified powder provided by the invention can be widely applied to cosmetics of powder systems and oil phase systems as a raw material, so that the cosmetics have good grease compatibility and stability, and are good in skin adhesion and skin feel.
Hereinafter, the powder surface composite treating agent, the surface-modified powder thereof and the use thereof will be further described with reference to the following specific examples.
Example 1
3g of triethoxysilylethylpolysiloxyethylhexylpolydimethylsiloxane, 3g of polydimethylsiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 596 mPas. 2g of a crosslinked polymer of PEG-12 polydimethylsiloxane and PPG-20 was mixed with 6g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 587 mPas. 1g of trimethylsiloxysilicate was mixed with 1g of polydimethylsiloxane to give a film-forming solution having a viscosity of 195 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of titanium dioxide, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the titanium dioxide in the surface modified powder is 94.3%.
Example 2
3g of triethoxysilylethylpolydimethylsilyloxyethyl polydimethylsiloxane, 4g of dodecamethylcyclohexasiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 521 mPas. 2g of a polydimethylsiloxane/bis-isobutyl PPG-20 crosslinked polymer was mixed with 8g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 535 mPas. 1g of polymethylsilsesquioxane was mixed with 2g of polydimethylsiloxane to give a film-forming agent solution having a viscosity of 174 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide red, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide red in the surface modified powder is 95.3%.
Example 3
3g of trimethoxysilylpolydimethylsiloxane, 5g of polydimethylsiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 446 mPas. 1g of a crosslinked polymer of PEG-12 polydimethylsiloxane and PPG-20 was mixed with 5g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 481 mPas. 0.5g of diphenylsiloxyphenyl trimethicone was mixed with 2g of decamethylcyclopentasiloxane to obtain a film-forming agent solution having a viscosity of 131 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide yellow, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide yellow in the surface modified powder is 95.8%.
Example 4
3g of triethoxysilylethylpolyethoxyhexylpolydimethylsiloxane, 5g of polydimethylsiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 446 mPas. 1g of a crosslinked polymer of PEG-12 polydimethylsiloxane and PPG-20 was mixed with 6g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 429 mPas. 1g of trimethylsiloxysilicate was mixed with 3g of polydimethylsiloxane to give a film-forming agent solution having a viscosity of 152 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide black, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide black in the surface modified powder is 95.9%.
Example 5
3g of triethoxysilylethylpolydimethylsilyloxyethyl polydimethylsiloxane, 6g of dodecamethylcyclohexasiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 371 mPas. 1g of a polydimethylsiloxane/bis-isobutyl PPG-20 crosslinked polymer was mixed with 7g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 367 mPas. 1g of polymethylsilsesquioxane was mixed with 4g of polydimethylsiloxane to give a film-forming agent solution having a viscosity of 132 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of talcum powder, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain the surface modified powder, wherein the mass fraction of the talcum powder in the surface modified powder is 96.4%.
Example 6
3g of triethoxysilylethylpolysiloxyethylhexylpolydimethylsiloxane, 7g of decamethylcyclopentasiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 296 mPas. 1g of a polydimethylsiloxane/bis-isobutyl PPG-20 crosslinked polymer was mixed with 8g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 309 mPas. 1g of diphenylsiloxyphenyl trimethicone was mixed with 5g of decamethylcyclopentasiloxane to obtain a film-forming agent solution having a viscosity of 114 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide yellow, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide yellow in the surface modified powder is 96.8%.
Example 7
3g of triethoxysilylethylpolydimethylsilyloxyethyl polydimethylsiloxane, 8g of decamethylcyclopentasiloxane, 1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 221 mPas. 1g of a crosslinked polymer of PEG-12 polydimethylsiloxane and PPG-20 was mixed with 9g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 262 mPas. 1g of diphenylsiloxyphenyl trimethicone was mixed with 6g of decamethylcyclopentasiloxane to obtain a film-forming agent solution having a viscosity of 95 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide yellow, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide yellow in the surface modified powder is 97.1%.
Example 8
A coupling agent solution having a viscosity of 146 mPas was obtained by mixing 3g of trimethoxysilylpolydimethylsiloxane, 9g of polydimethylsiloxane, 1g of ethanol and 0.5g of water. 1g of a polydimethylsiloxane/bis-isobutyl PPG-20 crosslinked polymer was mixed with 10g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 215 mPas. 1g of the polypropylsilsesquioxane was mixed with 7g of decamethylcyclopentasiloxane to give a film-forming agent solution with a viscosity of 76 mPas. And uniformly mixing the coupling agent solution, the organic silicon elastomer solution and the film forming agent solution to obtain 15g of the powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide yellow, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide yellow in the surface modified powder is 97.4%.
Comparative example 1
5.1g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 5.1g of polydimethylsiloxane, 1.7g of ethanol and 0.8g of water were mixed to obtain 12.7g of a coupling agent solution having a viscosity of 596 mPas.
Under the condition of stirring, spraying the coupling agent solution on 85g of titanium dioxide, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the titanium dioxide in the surface modified powder is 94.3%.
Comparative example 2
4.2g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 5.6g of polydimethylsiloxane, 1.4g of ethanol and 0.7g of water were mixed to obtain 11.9g of a coupling agent solution having a viscosity of 521 mPas.
Under the condition of stirring, spraying the coupling agent solution on 85g of iron oxide red, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide red in the surface modified powder is 95.3%.
Comparative example 3
3.8g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 6.3g of polydimethylsiloxane, 1.3g of ethanol and 0.6g of water were mixed to obtain 12g of a coupling agent solution having a viscosity of 446 mPas.
Under the condition of stirring, spraying the coupling agent solution on 85g of iron oxide yellow, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide yellow in the surface modified powder is 95.8%.
Comparative example 4
3.2g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 6.4g of polydimethylsiloxane, 1.1g of ethanol and 0.5g of water were mixed to obtain 11.2g of a coupling agent solution having a viscosity of 371 mPas.
Under the condition of stirring, spraying the coupling agent solution on 85g of iron oxide black, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide black in the surface modified powder is 96.4%.
Comparative example 5
2.8g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 6.5g of polydimethylsiloxane, 0.9g of ethanol and 0.5g of water were mixed to obtain 10.7g of a coupling agent solution having a viscosity of 296 mPas.
Under the condition of stirring, spraying the coupling agent solution on 85g of talcum powder, uniformly stirring, transferring to a drying box, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the talcum powder in the surface modified powder is 96.8%.
Comparative example 6
5.1g of PEG-12 polydimethylsiloxane, the crosslinked polymer of PPG-20 and 15.4g of polydimethylsiloxane were mixed to give 20.5g of a silicone elastomer solution having a viscosity of 195 mPas.
Under the condition of stirring, spraying the organic silicon elastomer solution on 85g of titanium dioxide, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the titanium dioxide in the surface modified powder is 94.3%.
Comparative example 7
4.2g of trimethylsiloxysilicate were mixed with 8.4g of polydimethylsiloxane to give 12.6g of a film-forming agent solution having a viscosity of 174 mPas.
Spraying the film-forming agent solution on 85g of iron oxide red under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide red in the surface modified powder is 95.3%.
Comparative example 8
A coupling agent solution having a viscosity of 446 mPas was obtained by mixing 2.8g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 4.7g of polydimethylsiloxane, 0.9g of ethanol and 0.5g of water. 0.9g of a crosslinked polymer of PEG-12 polydimethylsiloxane and PPG-20 was mixed with 4.5g of polydimethylsiloxane to obtain a silicone elastomer solution having a viscosity of 131 mPas. And uniformly mixing the coupling agent solution and the organic silicon elastomer solution to obtain 3g of powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 85g of iron oxide yellow, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide yellow in the surface modified powder is 95.8%.
Comparative example 9
3.2g of triethoxysilylethylpolydimethylsiloxyethylhexylpolydimethylsiloxane, 5.3g of polydimethylsiloxane, 1.1g of ethanol and 0.5g of water were mixed to obtain a coupling agent solution having a viscosity of 446 mPas. 0.5g of trimethylsiloxysilicate was mixed with 2g of polydimethylsiloxane to give a film-forming agent solution having a viscosity of 131 mPas. And (3) uniformly mixing the coupling agent solution and the film forming agent solution to obtain 3g of powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 97g of iron oxide black, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and performing jet milling to obtain surface modified powder, wherein the mass fraction of the iron oxide black in the surface modified powder is 95.8%.
Comparative example 10
2.5g of a crosslinked polymer of PEG-12 polydimethylsiloxane and PPG-20 and 12.5g of polydimethylsiloxane were mixed to obtain a silicone elastomer solution having a viscosity of 481 mPas. 1.2g of trimethylsiloxysilicate was mixed with 4.8g of polydimethylsiloxane to give a film-forming agent solution having a viscosity of 131 mPas. And uniformly mixing the organic silicon elastomer solution and the film forming agent solution to obtain 21g of powder surface composite treating agent.
Under the condition of stirring, spraying the powder surface composite treating agent on 97g of talcum powder, uniformly stirring, transferring to a drying oven, drying at 105 ℃ for 3h, and carrying out jet milling to obtain the surface modified powder, wherein the mass fraction of the talcum powder in the surface modified powder is 95.8%.
The surface-modified powders prepared in examples 1 to 5 and comparative examples 1 to 10 were subjected to a performance test, and the test results are shown in table 1 below.
TABLE 1
Figure BDA0003657845590000151
Figure BDA0003657845590000161
Application example 1
The surface-modified powders prepared in examples 1 to 5 of the present invention were prepared according to the formulation shown in Table 2, to obtain sample A.
TABLE 2
Figure BDA0003657845590000162
Application comparative example 1
The surface-modified powders prepared in comparative examples 1 to 5 of the present invention were prepared according to the formulation shown in Table 3 to obtain sample B.
TABLE 3
Figure BDA0003657845590000171
Comparative application example 2
The surface-modified powders prepared in comparative examples 6 to 10 of the present invention were prepared according to the formulation shown in Table 4 to obtain sample C.
TABLE 4
Figure BDA0003657845590000172
Figure BDA0003657845590000181
And (3) carrying out stability test on the prepared samples A-C, wherein the test method comprises the following steps: freeze-thaw cycle test (one cycle test including low temperature-8 + -2 deg.C, 24 hr and high temperature 40 + -1 deg.C, 24 hr) and normal temperature stability test (15 deg.C-25 deg.C).
TABLE 5
Figure BDA0003657845590000182
The prepared foundation liquid samples a-C were subjected to skin adhesion test, and the test results are shown in table 6 below.
TABLE 6
Figure BDA0003657845590000183
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The powder surface composite treating agent is characterized by comprising a coupling agent, an organic silicon elastomer and a film forming agent, wherein the coupling agent is selected from coupling agents with alkoxy groups and organic silicon chains, the organic silicon elastomer is selected from polydimethylsiloxane cross-linked polymers with hydroxyl groups, and the mass ratio of the coupling agent to the organic silicon elastomer to the film forming agent is 1:0.1:0.1-1:1: 0.7.
2. The powder surface composite treatment agent according to claim 1, wherein the silicone elastomer is at least one selected from the group consisting of a polydimethylsiloxane cross-linked polymer having a polyethylene glycol chain, a polydimethylsiloxane cross-linked polymer having a polypropylene glycol chain, and a polydimethylsiloxane cross-linked polymer having a polyglycerol chain.
3. The powder surface composite treatment agent according to claim 2, wherein the silicone elastomer is selected from the group consisting of polyethylene glycol-12 dimethicone crosspolymer, polyethylene glycol-12 dimethicone crosspolymer with polypropylene glycol-20, dimethicone crosspolymer with bis-isobutylpolypropylene glycol-20, bis-isobutylpolyethylene glycol/polypropylene glycol-20/35/dimethicone crosspolymer, bis-isobutylpolyethylene glycol/polypropylene glycol-10/7/dimethicone crosspolymer, polyethylene glycol/polypropylene glycol/butylene/dimethicone crosspolymer, polyethylene glycol/lauryl dimethicone crosspolymer, Polydimethylsiloxane polyethylene glycol-10/15 cross-linked polymer, polydimethylsiloxane polyethylene glycol-15 cross-linked polymer, bis-polyethylene glycol-15 polydimethylsiloxane/isophorone diisocyanate cross-linked polymer, methoxy polyethylene glycol-23 methacrylate/glycerol diisostearate methacrylate cross-linked polymer, and polydimethylsiloxane/polyglycerol-3 cross-linked polymer.
4. The powder surface composite treating agent according to claim 1, wherein the alkoxy group in the coupling agent is at least one selected from methoxy group and ethoxy group.
5. The powder surface composite treatment agent according to claim 4, wherein the coupling agent is at least one selected from triethoxysilylethyl polydimethylsiloxyethyl hexyl polydimethylsiloxane, triethoxysilylethyl polydimethylsiloxyethyl polydimethylsiloxane, and trimethoxysilylpolydimethylsiloxane.
6. The powder surface composite treating agent according to claim 1, wherein the film forming agent is at least one selected from the group consisting of trimethylsiloxysilicate, polymethylsilsesquioxane, polypropylsilsesquioxane, acrylic acid (ester)/polytrimethylsiloxane methacrylate copolymer, acrylic acid (ester)/polydimethylsiloxane copolymer, diphenylsiloxyphenyltrimethicone, and polyvinylpyrrolidone/hexadecene copolymer.
7. The surface-modified powder obtained by the treatment of the powder surface composite treatment agent according to any one of claims 1 to 6, wherein the surface-modified powder comprises a base powder and an organic layer coated on the surface of the base powder.
8. The surface-modified powder according to claim 7, wherein the base powder has a mass fraction of 85% to 99% in the surface-modified powder.
9. The surface-modified powder according to claim 7, wherein the base powder is at least one selected from the group consisting of titanium dioxide, zinc oxide, iron oxide, chromium oxide, ultramarine, talc, mica, clay, boron nitride, pearl, barium sulfate, calcium sulfate, pearl powder, magnesium sulfate, aluminum sulfate, bismuth oxychloride, zinc carbonate, magnesium carbonate, calcium carbonate, and calcium phosphate.
10. Use of the surface-modified powder according to any one of claims 7 to 9 in cosmetics in powder system and oil phase system.
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