CN109199879A - A kind of sun-proof creams of O/W/O multiplet and preparation method thereof - Google Patents

A kind of sun-proof creams of O/W/O multiplet and preparation method thereof Download PDF

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Publication number
CN109199879A
CN109199879A CN201811249731.4A CN201811249731A CN109199879A CN 109199879 A CN109199879 A CN 109199879A CN 201811249731 A CN201811249731 A CN 201811249731A CN 109199879 A CN109199879 A CN 109199879A
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oil
alcohol
ester
peg
sun
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CN109199879B (en
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朱海洋
梁小智
朱卓奇
张婉萍
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Shanghai Ruxi Biotechnology Co Ltd
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Shanghai Ruxi 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
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/066Multiple emulsions, e.g. water-in-oil-in-water
    • 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
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27Zinc; Compounds thereof
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    • A61K8/29Titanium; Compounds thereof
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    • 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
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    • A61K8/34Alcohols
    • A61K8/342Alcohols having more than seven atoms in an unbroken chain
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/35Ketones, e.g. benzophenone
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/361Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides thereof
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
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    • 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
    • A61K8/39Derivatives containing from 2 to 10 oxyalkylene groups
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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    • 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
    • A61K8/4966Triazines or their condensed derivatives
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/604Alkylpolyglycosides; Derivatives thereof, e.g. esters
    • AHUMAN NECESSITIES
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    • 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
    • A61K8/86Polyethers
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    • 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
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    • 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
    • A61K8/893Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by an alkoxy or aryloxy group, e.g. behenoxy dimethicone or stearoxy dimethicone
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    • 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
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    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • 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
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    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns
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    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

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Abstract

The present invention provides a kind of sun-proof creams of O/W/O multiplet, comprise the following components in parts by weight: interior 4~25 parts of phase of oil, 1~8 part of interior emulsifier phase, 1~10 part of polyalcohol, 10~40 parts of water, outer 26~88 parts of phase of oil, 1~10 part of outer emulsifier phase, 0.1~2 part of preservative.The existing certain water-resistance of the sun-proof creams of O/W/O multiplet provided by the invention, again mainly disperse chemical sun in interior oily phase, reduce the direct contact with skin, reduces sun-screening agent to the irritation and greasy feeling of skin, there is apparent advantage in cosmetic product system.

Description

A kind of sun-proof creams of O/W/O multiplet and preparation method thereof
Technical field
The present invention relates to cosmetic technical field, in particular to the sun-proof creams of a kind of O/W/O multiplet and its preparation side Method.
Background technique
The sun-proof creams of high SPF are the technological difficulties of cosmetic product exploitation, because its high SPF depends on body The addition of a large amount of sun-screening agents in system, and in a large amount of sun-screening agents mainly based on chemical ultraviolet absorbers, chemical ultraviolet absorbers exist Belong in cosmetic material and limits the use of raw material, it is a large amount of to add phenomena such as causing the sensitization and poor skin sense of sunscreen cosmetic.
The new technique for solving the problems, such as this at present is with coated carrier (Solid lipid carrier, nano-lipid carrier, micro- glue Capsule, organic micro-spheres etc.) cladding sun-screening agent, to form the carrier structure of cladding chemical ultraviolet absorbers.The carrier structure coated It is contacted applied to chemical ultraviolet absorbers in formula system, have been obstructed with the direct of skin, the physics of carrier structure is ultraviolet shielded Effect and the absorption of chemical ultraviolet absorbers form synergy;But this is only an intermediate, in being added to system Whether carrier structure, which is stabilized, has been limited to its application.
Sun-proof creams can be divided into O/W type emulsion and w/o type emulsion from the structure of emulsion.O/W type emulsion As sunscreen product, there is certain salubrious property, but do not have good water-resistance;And w/o type emulsion has good resist It is aqueous, but chemical ultraviolet absorbers are mostly Oil soluble materials, need to dissolve and be scattered in outer oily phase, so chemical ultraviolet absorbers with The compatibility of outer oil phase will affect the skin sense and stability of product, in addition, chemical ultraviolet absorbers directly contact skin on the skin Skin can promote its irritation to skin.Moreover, existing whether O/W type or w/o type product system, are developing high SPF When being worth sunscreen product, there may be being precipitated because of sun-screening agent caused by sun-screening agent poor compatibility, to increase the thorn to skin Swash property and thus bring greasy feeling.
Therefore, develop it is a kind of can obstruct sun-screening agent and skin directly contact and good skin sense and stability Novel sunscreen creams, become cosmetic industry technical problem urgently to be resolved.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of sun-proof creams of O/W/O multiplet and preparation method thereof.This The existing certain water-resistance of the sun-proof creams of O/W/O multiplet provided is provided, and disperses interior oily phase for sun-screening agent, is avoided Skin is directly contacted, sun-screening agent is reduced to skin bring irritation and greasy feeling, has in cosmetic product system bright Aobvious advantage.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of sun-proof creams of O/W/O multiplet, comprise the following components in parts by weight:
The interior oil mutually includes solid oil phase and liquid oil phase;The solid oil mutually includes solid-state sun-screening agent and solid-state fat Matter;The liquid oil phase includes liquid sun-screening agent and liquid fatty substance.
Preferably, the mass ratio of solid oil phase and liquid oil phase is 1:5~9:1 in the interior oily phase.
Preferably, solid-state sun-screening agent includes Unisol S-22,4- methyl benzyl subunit camphor, hexichol in the interior oily phase Ketone -3, UVNUL MS-40, bis-ethylhexoxyphenol methoxyphenyl triazine, butylmethoxydibenzoylmethane, diethylamino oxybenzene The own ester of formylbenzoate, Diethylhexyl Butamido Triazon, Ethylhexysalicylate, dimethyl PABA ethylhexyl With the mixture of one or more of Uvinul T 150.
Preferably, Solid lipid includes solid grease, chain saturated fatty acids, long-chain saturated fat in the interior oily phase The mixture of one or more of alcohol, solid-state esters, long chain alkane and wax class;
The solid grease includes the mixture of one or more of vaseline, Butyrospermum parkii fruit rouge and rilanit special;
The chain saturated fatty acids include lauric acid, myristic acid, palmitinic acid, stearic acid, behenic acid and behenic acid One or more of mixture;
The long-chain saturated fatty alcohol includes cetanol, stearyl alcohol, cetostearyl alcohol, docosyl alcohol, laruyl alcohol, lauryl alcohol, Myristyl alcohol, tetradecyl alchohol, one in hexadecanol, octadecyl alcolol, palmityl alcohol, docosanol, isooctadecanol, cholesterine and phytosterol Kind or several mixtures;
The solid-state esters include palmitin, stearine, glycerol tristearate, three (behenyl of glycerol Acid) ester, glycerol three (isostearic acid) ester, glycerol three (eicosane diacid) ester, glyceryl behenate, glyceryl monostearate, whale Ceryl alcohol stearate, cetanol palmitate, cetyl dimethicone, stearoxyl trimethyl silane, C30~C45 Alkyl methicone, C30~C45 alkanol dimethyl silane, poly- propyl silsesquioxane, the poly- methyl silicon of cetearyl Oxygen alkane, stearyl dimethione and acrylic acid/stearyl alcohol acrylate/dimethyl silicone polymer methacrylate copolymers The mixture of one or more of object;
The long chain alkane is vaseline;
The wax class includes beeswax, spermaceti, Brazil wax, candelila wax, rice bran wax, rice wax, lacca, ceresine, pure The mixture of one or more of ceresine, lignite wax, paraffin and microwax.
Preferably, liquid sun-screening agent includes Neo Heliopan E1000, methoxy cinnamic acid second in the interior oily phase The mixture of one or more of the own ester of base, octyl salicylate, Ao Likelin and Homosalate;
In the interior oily phase liquid fatty substance include olive oil, castor oil, peanut oil, palm oil, palm-kernel oil, coconut oil, Sunflower oil, sesame oil, soybean oil, safflower oil, apricot kernel oil, avocado oil, evening primrose oil, rice chaff oil, Queensland nut seed oil, wheat Embryo oil, thorn A Gan tree benevolence oil, candlenut tree macadamia nut oil, rice germ oil, almond oil, olive oil, maize germ oil, rapeseed oil, Persic oil, grape seed oil, peony seed oil, linseed oil, mango oil, white pond flower seed oil, jojoba seed oil, cocoa seed oil, rose Fruit oil, dormant oil, isooctane, Permethyl 99A, isohexadecane, Isoeicosane, polyisobutene, C13~C15 alkane, C12~C20 are different Alkane, synthesis saualane, sucrose saualane, vegetalitas saualane, saualane, octyl dodecanol, isopropyl myristate, palm fibre Palmitic acid isopropyl propionate, ethyl stearte, butyl stearate, ethyl oleate, ethyl linoleate, linoleic acid isopropyl ester, cetanol isopropyl Ester, myristic acid certain herbaceous plants with big flowers ester, oleic acid certain herbaceous plants with big flowers ester, oleyl alcohol oleate, cetanol ricinoleate ester, isoocanol laurate, different tristearin Alcohol laurate, different tridecanol myristinate, 2- hexyl certain herbaceous plants with big flowers alcohol myristinate, isooctadecanol myristinate, 2- octyl Lauryl alcohol myristinate, 2-Ethylhexyl Alcohol palmitate, octanol palmitate, isoocanol palmitate, 2- hexyl certain herbaceous plants with big flowers alcohol Palmitate, different cetanol palmitate, isooctadecanol palmitate, 2-Ethylhexyl Alcohol stearate, octanol stearate, 2- Hexyl certain herbaceous plants with big flowers alcohol stearate, iso-spermaceti ester alcohol stearic acid, the different certain herbaceous plants with big flowers ester of oleic acid, 2- octyl dodecanol oleate and isostearic acid isopropyl The mixture of one or more of ester.
Preferably, the interior emulsifier phase includes that isomery spermaceti alcohol ether, ceteareth -25, cetostearyl alcohol are poly- Ether -6, ceteareth -12, ceteareth -20, ceteareth -30, stereth -2, tristearin Hard -4 phosphate of ester alcohol ether of alcohol polyethers -21, -6 pairs of stearates of polyglycereol, three spermaceti, PEG-20 tribehenin acid glyceride, PEG- One of 8 beeswaxs, PEG-40 stearate, PEG-32 stearate, C16~C18 alkyl glycosides and C22 alkyl glycosides are several The mixture of kind.
Preferably, the outer oil mutually includes dimethyl silicone polymer and its derivative and liquid fatty substance;
The dimethyl silicone polymer and its derivative include ring five dimethyl silicone polymer, cyclohexasiloxane, poly- diformazan Radical siloxane, dimethiconol, diphenyl dimethicone, aminomethyl phenyl dimethyl silicone polymer, poly- diformazan Radical siloxane cross-linking agent, alkyl dimethicone, dimethicone copolyol, dimethiconol ester, benzene The poly- trimethicone of base, sesquialter dimethyl silicone polymer, amino polydimethyl siloxane, dimethyl silicone polymer/divinyl Base dimethione/silsesquioxane cross-linked polymer, dimethyl silicone polymer/phenyl vinyl dimethione crosslinking Polymer, dimethyl silicone polymer/silsesquioxane copolymer, dimethyl silicone polymer/methyl polysilicone alkyl copolymer, poly- two Methylsiloxane/vinyl dimethicone cross polymer, dimethyl silicone polymer/vinyl trimethylsilane oxygroup Esters of silicon acis cross-linked polymer, dimethiconol/silsesquioxane copolymer, dimethiconol/methyl-monosilane One of alcohol/esters of silicon acis cross-linked polymer, polydimethylsiloxanes ethyl dimethyl silicone polymer/methyl polysilicone alkyl copolymer Or several mixture;
The liquid fatty substance include olive oil, castor oil, peanut oil, palm oil, palm-kernel oil, coconut oil, sunflower oil, Sesame oil, soybean oil, safflower oil, apricot kernel oil, avocado oil, evening primrose oil, rice chaff oil, Queensland nut seed oil, wheat-germ oil, thorn A Gan tree benevolence oil, candlenut tree macadamia nut oil, rice germ oil, almond oil, olive oil, maize germ oil, rapeseed oil, persic oil, Portugal Grape seed oil, peony seed oil, linseed oil, mango oil, white pond flower seed oil, jojoba seed oil, cocoa seed oil, rose hip oil, dormant oil, Isooctane, Permethyl 99A, isohexadecane, Isoeicosane, polyisobutene, C13~C15 alkane, C12~C20 isoparaffin, synthesis Saualane, sucrose saualane, vegetalitas saualane, saualane, octyl dodecanol, isopropyl myristate, isopropyl palmitate, Ethyl stearte, butyl stearate, ethyl oleate, ethyl linoleate, linoleic acid isopropyl ester, cetanol isopropyl ester, myristic acid Certain herbaceous plants with big flowers ester, oleic acid certain herbaceous plants with big flowers ester, oleyl alcohol oleate, cetanol ricinoleate ester, isoocanol laurate, isooctadecanol laurate, Different tridecanol myristinate, 2- hexyl certain herbaceous plants with big flowers alcohol myristinate, isooctadecanol myristinate, 2- octyl dodecanol nutmeg Acid esters, 2-Ethylhexyl Alcohol palmitate, octanol palmitate, isoocanol palmitate, 2- hexyl certain herbaceous plants with big flowers alcohol palmitate, different whale Ceryl alcohol palmitate, isooctadecanol palmitate, 2-Ethylhexyl Alcohol stearate, octanol stearate, 2- hexyl certain herbaceous plants with big flowers alcohol are stearic The different certain herbaceous plants with big flowers ester of acid esters, iso-spermaceti ester alcohol stearic acid, oleic acid, 2- octyl dodecanol oleate, isopropyl isostearate, carbonic acid two are pungent Ester, Neo Heliopan E1000, ethylhexyl methoxy cinnamate, octyl salicylate, Ao Likelin, in Homosalate One or more of mixtures.
Preferably, the outer emulsifier phase include the smooth olive oleate of sorb, PEG-30 dimerization hydroxy stearic acid ester, gather it is sweet Oily -3 diisopstearates, glyceryl oleate, -3 polyricinoleate of polyglycereol, PEG-11 methyl ether dimethicone, PEG/PPG-20/22 butyl ether dimethyl silicone polymer, PEG-9 dimethyl silicone polymer, PEG-3 dimethyl silicone polymer, PEG-9 methyl ether dimethicone, PEG-10 Polydimethylsiloxane, PEG-9 polydimethylsiloxanes ethyl poly dimethyl silicon Oxygen alkane, lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone, lauryl PEG-10 tri- (trimethylsiloxy group) silicon Ethyl polymethyl siloxane, PEG-12 dimethyl silicone polymer, ring five dimethyl silicone polymer, lauryl PEG/PPG-18/18 Polymethyl siloxane, PEG/PPG-19/19 dimethyl silicone polymer, PEG/PPG-10/3 oleyl ether dimethyl silicone polymer, PEG/PPG-12/16 dimethyl silicone polymer, PEG/PPG-12/18 dimethyl silicone polymer, PEG/PPG-14/4 poly dimethyl One or more of siloxanes, PEG/PPG-15/15 dimethyl silicone polymer, PEG/PPG-17/18 dimethyl silicone polymer Mixture.
The present invention provides the preparation method of the sun-proof creams of O/W/O multiplet described in above-mentioned technical proposal, including following step It is rapid:
(1) interior oily phase raw material is mixed, obtains interior oil-based system;
(2) interior emulsifier phase, water and polyalcohol are mixed, obtains aqueous phase system;
(3) outer oil is mutually mixed with outer oil phase emulsifier, obtains outer oil-based system;
(4) the interior oil-based system that the step (1) obtains is added in the aqueous phase system that step (2) obtains and carries out first Emulsification, obtains O/W type colostric fluid;
(5) the O/W type colostric fluid for obtaining the step (4) carries out the first homogenization, obtains O/W type nanoemulsions;
(6) by the O/W type nanoemulsions that the step (5) obtains be added in the outer oil-based system that step (3) obtains into Row second emulsifies, and obtains O/W/O type colostric fluid;
(7) the O/W/O type colostric fluid for obtaining the step (6) carries out the second homogenization, obtains O/W/O type lotion;
(8) preservative is added into the O/W/O type lotion that the step (7) obtains, obtains the sun-proof creams of O/W/O type;
The limitation of the not no time sequencing in step (1)~(3).
Preferably, the pressure of step (5) first homogenization is 300bar~1500bar, the first homogenization Cycle-index is 1 time~5 times.
The present invention provides a kind of sun-proof creams of O/W/O multiplet, constituent include interior oily phase, interior emulsifier phase, Polyalcohol, water, outer oily phase, outer emulsifier phase, preservative.The present invention uses O/W/O type emulsion as the matrix of sun-proof creams Sun-screening agent is dissolved in interior oily phase, makes the existing certain water resistant of the sun-proof creams of O/W/O multiplet provided by the invention by system Property, and obstructed sun-screening agent and contacted with the direct of skin, sun-screening agent is reduced to skin bring irritation and greasy feeling.Implement Example the result shows that, the sun-proof creams of O/W/O multiplet provided by the invention have it is good sun protection, it is not oily to skin refreshing It is greasy.
The present invention provides the preparation methods of the sun-proof creams of O/W/O multiplet described in above scheme.The present invention passes through work The control of skill, the particle size and distribution of oily phase particle effectively in control, by interior oily phase particle control between 200~500nm, Good physical shielding effect is generated by the scattering process to ultraviolet light, and realizes the synergy with sun-screening agent.Also, this It is simple to invent the preparation method provided, is suitble to large-scale production, there is apparent advantage in cosmetic product system.
Specific embodiment
The present invention provides a kind of sun-proof creams of O/W/O multiplet, comprise the following components in parts by weight:
The interior oil mutually includes solid oil phase and liquid oil phase;The solid oil mutually includes solid-state sun-screening agent and solid-state fat Matter;The liquid oil phase includes liquid sun-screening agent and liquid fatty substance.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include interior oily 4~25 parts of phase, preferably It is 6 parts~16 parts;The interior oil mutually includes solid oil phase and liquid oil phase, and the mass ratio of the solid oil phase and liquid oil phase is excellent It is selected as 1:5~9:1;The solid oil mutually includes solid-state sun-screening agent and Solid lipid, the solid-state sun-screening agent and Solid lipid Mass ratio is preferably 1:3~5:1;The liquid oil phase includes liquid sun-screening agent and liquid fatty substance, the liquid sun-screening agent and liquid The mass ratio of state lipid is preferably 2:1~9:1.
In the present invention, Solid lipid may make the fusing point of interior oily phase higher, and the present invention passes through solid-state in phase oily in control The proportion of oily phase forms a kind of solid-state phase particle, has stability under sunlight irradiation;It is sun-proof that liquid fatty substance is conducive to solid-state The dissolution of agent.
In the present invention, solid-state sun-screening agent preferably includes Unisol S-22,4- methyl benzyl subunit camphor tree in the interior oily phase Brain, benzophenone-3, UVNUL MS-40, bis-ethylhexoxyphenol methoxyphenyl triazine, butylmethoxydibenzoylmethane, two The own ester of second ammonia oxybenzene formylbenzoate, Diethylhexyl Butamido Triazon, Ethylhexysalicylate, dimethyl PABA The mixture of one or more of ethylhexyl and Uvinul T 150.
In the present invention, to preferably include solid grease, chain saturated fatty acids, long-chain full for Solid lipid in the interior oily phase With the mixture of one or more of fatty alcohol, solid-state esters, long chain alkane and wax class.
In the present invention, solid grease preferably includes vaseline, Butyrospermum parkii fruit rouge and rilanit special in the interior oily phase One or more of mixture.
In the present invention, in the interior oily phase chain saturated fatty acids preferably include lauric acid, myristic acid, palmitinic acid, The mixture of one or more of stearic acid, behenic acid and behenic acid.
In the present invention, long-chain saturated fatty alcohol preferably includes cetanol, stearyl alcohol, cetearyl alcohol in the interior oily phase Alcohol, docosyl alcohol, laruyl alcohol, lauryl alcohol, myristyl alcohol, tetradecyl alchohol, hexadecanol, octadecyl alcolol, palmityl alcohol, docosanol, different tristearin The mixture of one or more of alcohol, cholesterine and phytosterol.
In the present invention, solid-state esters preferably include palmitin, stearine, glycerol in the interior oily phase Tristearate, glycerol three (behenic acid) ester, glycerol three (isostearic acid) ester, glycerol three (eicosane diacid) ester, glycerol behenyl Acid esters, glyceryl monostearate, cetanol stearate, cetanol palmitate, cetyl dimethicone, stearic oxygen Base trimethyl silane, C30~C45 alkyl methicone, C30~C45 alkanol dimethyl silane, poly- propyl silicon sesquialter oxygen Alkane, cetearyl methicone, stearyl dimethione and acrylic acid/stearyl alcohol acrylate/poly dimethyl The mixture of one or more of siloxanes methacrylate copolymer.
In the present invention, long chain alkane is preferably vaseline in the interior oily phase.
In the present invention, wax class preferably includes beeswax, lanolin, spermaceti, Brazil wax, small candle tree in the interior oily phase The mixtures of the one or more of wax, rice bran wax, rice wax, lacca, ceresine, ceresin, lignite wax, paraffin and microwax.
In the present invention, liquid sun-screening agent preferably includes Neo Heliopan E1000, methoxyl group in the interior oily phase The mixture of one or more of 2-Ethylhexyl cinnamate, octyl salicylate, Ao Likelin and Homosalate.
In the present invention, liquid fatty substance preferably includes olive oil, castor oil, peanut oil, palm oil, palm fibre in the interior oily phase Palmitic acid benevolence oil, coconut oil, sunflower oil, sesame oil, soybean oil, safflower oil, apricot kernel oil, avocado oil, evening primrose oil, rice chaff oil, Australia Continent nut seed oil, wheat-germ oil, thorn A Gan tree benevolence oil, candlenut tree macadamia nut oil, rice germ oil, almond oil, olive oil, corn Embryo oil, rapeseed oil, persic oil, grape seed oil, peony seed oil, linseed oil, mango oil, white pond flower seed oil, jojoba seed oil, Cocoa seed oil, rose hip oil, dormant oil, isooctane, Permethyl 99A, isohexadecane, Isoeicosane, polyisobutene, C13~C15 alkane Hydrocarbon, C12~C20 isoparaffin, synthesis saualane, sucrose saualane, vegetalitas saualane, saualane, octyl dodecanol, Pork and beans Cool isopropyl propionate, isopropyl palmitate, ethyl stearte, butyl stearate, ethyl oleate, ethyl linoleate, linoleic acid isopropyl Ester, cetanol isopropyl ester, myristic acid certain herbaceous plants with big flowers ester, oleic acid certain herbaceous plants with big flowers ester, oleyl alcohol oleate, cetanol ricinoleate ester, the isoocanol moon Cinnamic acid ester, isooctadecanol laurate, different tridecanol myristinate, 2- hexyl certain herbaceous plants with big flowers alcohol myristinate, isooctadecanol Pork and beans Cool acid esters, 2- octyl dodecanol myristinate, 2-Ethylhexyl Alcohol palmitate, octanol palmitate, isoocanol palmitinic acid It is ester, 2- hexyl certain herbaceous plants with big flowers alcohol palmitate, different cetanol palmitate, isooctadecanol palmitate, 2-Ethylhexyl Alcohol stearate, pungent Alcohol stearate, 2- hexyl certain herbaceous plants with big flowers alcohol stearate, iso-spermaceti ester alcohol stearic acid, the different certain herbaceous plants with big flowers ester of oleic acid, 2- octyl dodecanol oleate With the mixture of one or more of isopropyl isostearate.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include 1~8 part of interior emulsifier phase, excellent It is selected as 2~5 parts.In the present invention, the interior emulsifier phase preferably includes isomery spermaceti alcohol ether, ceteareth -25, whale Wax stereth -6, ceteareth -12, ceteareth -20, ceteareth -30, stearyl alcohol are poly- Hard -4 phosphate of ester alcohol ether of ether -2, stereth -21, -6 pairs of stearates of polyglycereol, three spermaceti, PEG-20 tribehenin acid are sweet In grease, PEG-8 beeswax, PEG-40 stearate, PEG-32 stearate, C16~C18 alkyl glycosides and C22 alkyl glycosides One or more of mixtures.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include 1~10 part of polyalcohol, preferably It is 3~8 parts.In the present invention, the polyalcohol preferably includes in ethylene glycol, glycerine, 1,3-BDO and dipropylene glycol One or more of mixtures.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include 10~40 parts of water, and preferably 15 ~35 parts.The present invention does not have particular/special requirement to the water, selects water well known to those skilled in the art.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include outer oily 26~88 parts of phase, preferably It is 30~50 parts.In the present invention, the outer oil mutually preferably includes dimethyl silicone polymer and its derivative and liquid fatty substance.
In the present invention, dimethyl silicone polymer and its derivative preferably include five poly dimethyl silicon of ring in the outer oily phase Oxygen alkane, cyclohexasiloxane, dimethyl silicone polymer, dimethiconol, diphenyl dimethicone, aminomethyl phenyl Dimethyl silicone polymer, dimethyl silicone polymer cross-linking agent, alkyl dimethicone, dimethicone copolyol, Dimethiconol ester, phenyl trimethicone, sesquialter dimethyl silicone polymer, amino polydimethyl siloxane, Dimethyl silicone polymer/divinyl dimethione/silsesquioxane cross-linked polymer, dimethyl silicone polymer/phenyl Vinyl dimethione cross-linked polymer, dimethyl silicone polymer/silsesquioxane copolymer, dimethyl silicone polymer/ Methyl polysilicone alkyl copolymer, Dimethicone/Vinyl Dimethicone cross-linked polymer, polydimethylsiloxanes Alkane/vinyl trimethylsilane oxygroup esters of silicon acis cross-linked polymer, gathers dimethiconol/silsesquioxane copolymer Dimethyl silica alkanol/methyl-monosilane alcohol/esters of silicon acis cross-linked polymer, polydimethylsiloxanes ethyl dimethyl silicone polymer/poly- The mixture of one or more of Methylpolysiloxane Copolymer.
In the present invention, liquid fatty substance preferably includes olive oil, castor oil, peanut oil, palm oil, palm fibre in the outer oily phase Palmitic acid benevolence oil, coconut oil, sunflower oil, sesame oil, soybean oil, safflower oil, apricot kernel oil, avocado oil, evening primrose oil, rice chaff oil, Australia Continent nut seed oil, wheat-germ oil, thorn A Gan tree benevolence oil, candlenut tree macadamia nut oil, rice germ oil, almond oil, olive oil, corn Embryo oil, rapeseed oil, persic oil, grape seed oil, peony seed oil, linseed oil, mango oil, white pond flower seed oil, jojoba seed oil, Cocoa seed oil, rose hip oil, dormant oil, isooctane, Permethyl 99A, isohexadecane, Isoeicosane, polyisobutene, C13~C15 alkane Hydrocarbon, C12~C20 isoparaffin, synthesis saualane, sucrose saualane, vegetalitas saualane, saualane, octyl dodecanol, Pork and beans Cool isopropyl propionate, isopropyl palmitate, ethyl stearte, butyl stearate, ethyl oleate, ethyl linoleate, linoleic acid isopropyl Ester, cetanol isopropyl ester, myristic acid certain herbaceous plants with big flowers ester, oleic acid certain herbaceous plants with big flowers ester, oleyl alcohol oleate, cetanol ricinoleate ester, the isoocanol moon Cinnamic acid ester, isooctadecanol laurate, different tridecanol myristinate, 2- hexyl certain herbaceous plants with big flowers alcohol myristinate, isooctadecanol Pork and beans Cool acid esters, 2- octyl dodecanol myristinate, 2-Ethylhexyl Alcohol palmitate, octanol palmitate, isoocanol palmitinic acid It is ester, 2- hexyl certain herbaceous plants with big flowers alcohol palmitate, different cetanol palmitate, isooctadecanol palmitate, 2-Ethylhexyl Alcohol stearate, pungent Alcohol stearate, 2- hexyl certain herbaceous plants with big flowers alcohol stearate, iso-spermaceti ester alcohol stearic acid, the different certain herbaceous plants with big flowers ester of oleic acid, 2- octyl dodecanol oleate, Isopropyl isostearate, carbonic acid dioctyl ester, Neo Heliopan E1000, ethylhexyl methoxy cinnamate, bigcatkin willow are misery The mixture of one or more of ester, Ao Likelin, Homosalate.
In the present invention, it is also preferable to include in physics ultraviolet light screener, skin sense regulator and film forming agent in the outer oily phase One or more.
In the present invention, physics ultraviolet light screener preferably includes titanium dioxide and/or zinc oxide in the outer oily phase;It is described Skin sense regulator preferably includes silica, polyamide fibre -12, vinyldimethicone/polymethylsilsesquioxane cross-linked polymeric The mixture of one or more of object, polymethyl methacrylate and polymethylsilsesquioxane.
In the present invention, film forming agent preferably includes polymethylsilsesquioxane, trimethyl silicane alkoxy in the outer oily phase The mixture of one or more of esters of silicon acis and acrylic acid/polydimethylsiloxanecopolymer copolymer.
In the present invention, when the outer oil mutually includes that dimethyl silicone polymer and its derivative, liquid fatty substance, physics are ultraviolet When screener, skin sense regulator and film forming agent, dimethyl silicone polymer and its derivative and liquid fatty substance in the outer oily phase Mass fraction is preferably 80~99 parts;The mass fraction of physics ultraviolet light screener is preferably 2~10 parts in the outer oily phase;It is described The mass fraction of skin sense regulator is preferably 1~3 part in outer oil phase;The mass fraction of film forming agent is preferably in the outer oily phase 0.5~2 part.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include 1~10 part of outer emulsifier phase, Preferably 2~6 parts.In the present invention, the outer emulsifier phase preferably includes the smooth olive oleate of sorb, PEG-30 dimerization hydroxyl Stearate, polyglyceryl-3 diisostearate, glyceryl oleate, -3 polyricinoleate of polyglycereol, PEG-11 methyl ether poly- two Methylsiloxane, PEG/PPG-20/22 butyl ether dimethyl silicone polymer, PEG-9 dimethyl silicone polymer, the poly- diformazan of PEG-3 Radical siloxane, PEG-9 methyl ether dimethicone, PEG-10 Polydimethylsiloxane, PEG-9 polydimethylsiloxanes ethyl are poly- Dimethyl siloxane, lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone, tri- (trimethyl of lauryl PEG-10 Siloxy) silica ethyl polymethyl siloxane, PEG-12 dimethyl silicone polymer, ring five dimethyl silicone polymer, lauryl PEG/ PPG-18/18 polymethyl siloxane, PEG/PPG-19/19 dimethyl silicone polymer, PEG/PPG-10/3 oleyl ether poly dimethyl Siloxanes, PEG/PPG-12/16 dimethyl silicone polymer, PEG/PPG-12/18 dimethyl silicone polymer, PEG/PPG-14/4 are poly- One of dimethyl siloxane, PEG/PPG-15/15 dimethyl silicone polymer and PEG/PPG-17/18 dimethyl silicone polymer Or several mixture.
Based on parts by weight, the sun-proof creams of O/W/O multiplet provided by the invention include 0.1~2 part of preservative, preferably It is 0.3~1.2 part.In the present invention, the preservative is preferably bromo- 2- nitropropane -1,3 glycol of 2-, the bromo- 5- nitro-of 5- 1,3- dioxanes, the bicyclic oxazolidine of 7- ethyl, benzalkonium chloride, benzalkonium bromide, benzene prick ammonium saccharin, benzethonium chloride, benzoic acid, benzene first Sour sodium, benzyl alcohol, formaldehyde benzylalcohol hemiacetal, bromine chlorine sweet smell, two sodium acetates, anesin, benzyl chloride phenol, dichloroxylenol, chlorobenzene are sweet The own amidine hydroxyethyl sulfonate of ether, Climbazole, dehydroactic acid, dehydroactic acid sodium, Bis(hydroxymethyl)imidazolidinyl urea, dibromo, dichloro Benzene first, dimethyl oxazolidine, DMDM hydantoin, dimethyl hydantoin, formaldehyde, paraformaldehyde, formic acid, sodium formate, penta 2 Aldehyde, hexamidine P-hydroxybenzoic acid sodium, Hexetidine, imidazolidinyl urea, iodine propilolic alcohol butyl mephenesin Carbamate, the different Anthelvet of methyl Mixture (the methyl chloride isothiazoline of quinoline ketone, methylchloroisothiazandnone and methylisothiazolinone and magnesium chloride and magnesium nitrate Ketone: methylisothiazolinone 3:1), o-cymene -5- alcohol, o-phenyl phenol, 4-HBA, parachlorometacresol, benzene oxygen Ethyl alcohol, benzene oxygen isopropanol, piroctone, polyaminopropyl biguanide, propionic acid, sodium propionate, salicylic acid, sodium hydroxy methyl glycinate, sorb Acid, sodium sorbate, potassium sorbate, thimerosal, triclocarban, triclosan, pungent glycol, hexylene glycol, decoyl hydroximic acid, para hydroxybenzene Ethyl ketone, anisic acid, quaternary ammonium salt -15, polyamidopropyl ether, gum arabic, xanthan gum, propylene glycol/bis- (methylols) imidazolidine Base urea/methyl hydroxybenzoate iodine propilolic alcohol butyl mephenesin Carbamate, propylene glycol/Bis(hydroxymethyl)imidazolidinyl urea/iodine propilolic alcohol butyl ammonia Formic acid esters, propylene glycol/Bis(hydroxymethyl)imidazolidinyl urea/methyl hydroxybenzoate/Nipasol, the chloro- 2- dihydroxy diphenyl ether of 2,2,4- tri-, 5-Chloro-2-methyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, 1,3- dihydroxymethyl, 5- dimethyl receive acyl Iodo- 2 propynylbutylcarbamate of urea, dimethyloldimethylhydantoin, 3-, 5- chloro -2- methyl -4- isothiazoline - Two between 3- ketone/2-methyl-4-isothiazolin-3-one, dimethyloldimethylhydantoin/isothiazolinone, pentanediol, fourth The mixture of one or more of alcohol, methyl propanediol and zinc pyrithione.
The present invention provides the preparation method of the sun-proof creams of O/W/O multiplet described in above-mentioned technical proposal, including it is following Step:
(1) interior oily phase raw material is mixed, obtains interior oil-based system;
(2) interior emulsifier phase, water and polyalcohol are mixed, obtains aqueous phase system;
(3) outer oil is mutually mixed with outer oil phase emulsifier, obtains outer oil-based system;
(4) the interior oil-based system that the step (1) obtains is added in the aqueous phase system that step (2) obtains and carries out first Emulsification, obtains O/W type colostric fluid;
(5) the O/W type colostric fluid for obtaining the step (4) carries out the first homogenization, obtains O/W type nanoemulsions;
(6) by the O/W type nanoemulsions that the step (5) obtains be added in the outer oil-based system that step (3) obtains into Row second emulsifies, and obtains O/W/O type colostric fluid;
(7) the O/W/O type colostric fluid for obtaining the step (6) carries out the second homogenization, obtains O/W/O type lotion;
(8) preservative is added into the O/W/O type lotion that the step (7) obtains, obtains the sun-proof creams of O/W/O type;
The limitation of the not no time sequencing in step (1)~(3).
The present invention mixes interior oily phase raw material, obtains interior oil-based system.In the present invention, in the present invention, the interior oil The mixing temperature of phase raw material is preferably 70~90 DEG C, and more preferably 80 DEG C;The mixing preferably carries out under stiring, the stirring Speed be preferably 300~600rpm, the time of stirring is preferably 5~15min.In a specific embodiment of the present invention, preferably Liquid oil phase is heated to 70~90 DEG C, then solid oil is added in liquid oil phase mixes under agitation.
The present invention mixes interior emulsifier phase, water and polyalcohol, obtains aqueous phase system.In the present invention, the interior phase cream The mixing temperature of agent, water and polyalcohol is preferably 70~90 DEG C, and more preferably 80 DEG C;It is described mixing preferably under stiring into Row, the speed of the stirring is preferably 300~600rpm, and the time of stirring is preferably 5~15min.
The present invention mutually mixes outer oil with outer oil phase emulsifier, obtains outer oil-based system.In the present invention, the outer oily phase Mixing temperature with outer oil phase emulsifier is preferably 40~60 DEG C, and more preferably 50 DEG C;The mixing preferably carries out under stiring, The speed of the stirring is preferably 300~600min, and the time of stirring is preferably 5~15min.
After obtaining interior oil-based system and aqueous phase system, the interior oil-based system is added in the aqueous phase system by the present invention The first emulsification is carried out, O/W type colostric fluid is obtained.The present invention preferably passes through stirring shearing and carries out the first emulsification, and the stirring turns Speed is preferably 300~600rpm, and the time of stirring is preferably 5~15min.
After the completion of first emulsification, the O/W type colostric fluid is preferably carried out the first homogenization by the present invention, obtains O/W type Nanoemulsions.In the present invention, the pressure of first homogenization is preferably 300bar~1500bar, the first homogenization Cycle-index be preferably 1 time~5 times.Present invention preferably uses high pressure homogenizers to carry out homogenization.
After the completion of first homogenization, the present invention preferably under stiring cools down the O/W type nanoemulsions, The speed of the stirring is preferably 300~600rpm, and the present invention preferably cools the O/W type nanoemulsions to 40~60 ℃。
After the completion of cooling, the O/W type nanoemulsions are added in the outer oil-based system and carry out second by the present invention Emulsification, obtains O/W/O type colostric fluid.The present invention preferably passes through stirring shearing and carries out the second emulsification, and the speed of the stirring is preferred For 300~600rpm, the time of stirring is preferably 6~10min.
After the completion of second emulsification, the O/W/O type colostric fluid is preferably carried out the second homogenization by the present invention, obtains O/W/ O-shaped lotion.In the present invention, the speed of second homogenization is preferably 3000~19000rpm, at second homogeneous The time of reason is preferably 3~10min.
After the completion of second homogenization, the present invention preferably under stiring cools down the O/W/O type lotion, institute The speed for stating stirring is preferably 200~800rpm, and described cool preferably cools to 40 DEG C or less.
After the completion of cooling, preservative is added in the O/W/O type lotion in the present invention, and it is anti-to obtain O/W/O type for mixing Shine creams.In the present invention, the mixing preferably carries out under stiring, and it is special that the present invention does not have the speed of stirring and time It is required that O/W/O type lotion and preservative can be made to be uniformly mixed.After mixing, the present invention is preferably by O/W/O type lotion It is cooled to room temperature with the mixed emulsion of preservative composition, obtains the sun-proof creams of O/W/O type.
Sun-proof creams of O/W/O multiplet provided by the invention and preparation method thereof are carried out below with reference to embodiment detailed Explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
In terms of 100g formula material, concrete composition is as follows:
Interior oil phase 8g, wherein solid-state sun-screening agent is 4- methyl benzyl subunit camphor, dosage 2g;Solid lipid is docosyl alcohol, Dosage is 1.5g;Liquid sun-screening agent is ethylhexyl methoxy cinnamate, dosage 4g;Liquid fatty substance is isopropyl palmitate, Dosage is 0.5g;
Interior emulsifier phase is PEG-40 stearate, dosage 1.5g;
Polyalcohol is glycerol, dosage 3g;
Water, dosage 13g;
Outer oil phase 67.5g, wherein dimethyl silicone polymer and its derivative are ring five dimethyl silicone polymer, hexamethylene silicon oxygen The mixture of alkane and dimethyl silicone polymer, dosage 42g;Liquid fatty substance is the mixture of isohexadecane and avocado oil, dosage For 19.5g;Physics ultraviolet light screener is titanium dioxide, dosage 6g in outer oil phase.
Outer emulsifier phase is polyglyceryl-3 diisostearate, dosage 6g;
Preservative is the mixture of methyl hydroxybenzoate and Phenoxyethanol, dosage 1g.
The sun-proof creams of O/W/O multiplet are prepared by above-mentioned raw materials, steps are as follows:
(1) 80 DEG C are heated to after mixing interior oily phase raw material, obtains finely dispersed interior oil phase component;
(2) it is heated to 80 DEG C after mixing interior emulsifier phase, polyalcohol with water, obtains finely dispersed water phase components;
(3) outer oil is mutually mixed and heated to 50 DEG C with outer emulsifier phase, obtains finely dispersed outer oil phase component;
(4) with revolving speed whipping step (2) resulting water phase components of 400rpm, while the resulting interior oil of step (1) is added Phase component stirs 5min, obtains O/W type colostric fluid;
(5) the O/W type colostric fluid for obtaining step (4) carries out high-pressure homogeneous processing, and homogeneous is pressure 400bar, circulation time Number is 1 time, forms O/W type nanoemulsions, this lotion is cooled under the revolving speed stirring of 500rpm to 50 DEG C;
(6) the resulting outer oil phase component of whipping step (3) under the revolving speed of 600rpm receives the resulting O/W type of step (5) Rice milk liquid is added in step (3) system, is stirred 7min, is obtained O/W/O type colostric fluid;
(7) by O/W/O type colostric fluid obtained by (6), it is more to obtain O/W/O by the homogeneous 3min at homogeneous speed 13000r/min Weight structure nanoemulsions;
(8) the O/W/O multiplet nanoemulsions for obtaining step (7) stir cooling with the speed of 400rpm, cool to 40 DEG C, preservative is added and stirs evenly, is subsequently cooled to room temperature to get the sun-proof creams of O/W/O multiplet.
Embodiment 2
In terms of 100g formula material, concrete composition is as follows:
Interior oil phase 13g, wherein solid-state sun-screening agent be the own ester of diethylamino oxybenzene formylbenzoate, Uvinul T 150 and The mixture of UVNUL MS-40, dosage 4g;Solid lipid is the mixture of Butyrospermum parkii fruit rouge, rilanit special, dosage 3g; Liquid sun-screening agent is the mixture of ethylhexyl methoxy cinnamate and octyl salicylate, and dosage 5g, liquid fatty substance is palm Isopropyl propionate, dosage 1g;
Interior emulsifier phase is ceteareth -30, dosage 2.5g;
Polyalcohol is the mixture of glycerol and 1,3-BDO, dosage 7g;
Water, 18.8g;
Outer oil phase 51.5g, wherein dimethyl silicone polymer and its derivative are ring five dimethyl silicone polymer, hexamethylene silicon oxygen The mixture of alkane and alkyl dimethicone, dosage 41g;Liquid fatty substance is different cetanol palmitate, dosage 3g; Physics ultraviolet light screener is the mixture of titanium dioxide and zinc oxide, dosage 5g;Skin sense regulator is silica, dosage 2g; Film forming agent is polymethylsilsesquioxane, dosage 0.5g;
Outer emulsifier phase is PEG-10 Polydimethylsiloxane, dosage 6g;
Preservative is the mixture of methyl hydroxybenzoate, Nipasol and Phenoxyethanol, dosage 1.2g.
The sun-proof creams of O/W/O multiplet are prepared by above-mentioned raw materials, steps are as follows:
(1) 85 DEG C are heated to after mixing interior oily phase raw material, obtains finely dispersed interior oil phase component;
(2) it is heated to 85 DEG C after mixing interior emulsifier phase, polyalcohol with water, obtains finely dispersed water phase components;
(3) outer oil is mutually mixed and heated to 50 DEG C with outer emulsifier phase, obtains finely dispersed outer oil phase component;
(4) with revolving speed whipping step (2) resulting water phase components of 500rpm, while the resulting interior oil of step (1) is added Phase component stirs 5min, obtains O/W type colostric fluid;
(5) the O/W type colostric fluid for obtaining step (4) carries out high-pressure homogeneous processing, and homogeneous is pressure 900bar, circulation time Number is 3 times, forms O/W type nanoemulsions, this lotion is cooled under the revolving speed stirring of 500rpm to 50 DEG C;
(6) the resulting outer oily phase of whipping step (3) under the revolving speed of 600rpm, by the resulting O/W type nano-emulsion of step (5) Liquid is added in (3) system, is stirred 6min, is obtained O/W/O type colostric fluid;
(7) by O/W/O type colostric fluid obtained by (6), it is more to obtain O/W/O by the homogeneous 3min at homogeneous speed 18000r/min Weight structure nanoemulsions;
(8) the O/W/O multiplet nanoemulsions for obtaining step (7) stir cooling with the speed of 400rpm, cool to 40 DEG C, preservative is added and stirs evenly, is subsequently cooled to room temperature to get the sun-proof creams of O/W/O multiplet.
Embodiment 3
In terms of 100g formula material, concrete composition is as follows:
Interior oil phase 22g, wherein solid-state sun-screening agent is butylmethoxydibenzoylmethane and double-ethyl hexyl oxy phenol first The mixture of oxygen phenyl triazine, dosage 7g;Solid lipid is stearine, dosage 3g;Liquid sun-screening agent is difficult to understand vertical The mixture of crin and Homosalate, dosage 10g;Liquid fatty substance is 2-Ethylhexyl Alcohol palmitate, dosage 2g;
Interior emulsifier phase is C16~C18 alkyl glycosides, dosage 4g;
Polyalcohol is 1,3-BDO, dosage 8g;
Water, 26g;
Outer oil phase 31.2g, wherein dimethyl silicone polymer and its derivative are ring five dimethyl silicone polymer, poly dimethyl The mixture of silicone cross-linked object and dimethyl silicone polymer, dosage 23g;Liquid fatty substance is carbonic acid dioctyl ester, dosage 2g; Physics ultraviolet light screener is zinc oxide, dosage 5g;Skin sense regulator is silica, dosage 1.2g;
Outer emulsifier phase is PEG-10 Polydimethylsiloxane, dosage 8g;
Preservative is the mixture of methyl hydroxybenzoate, Nipasol and Phenoxyethanol, dosage 0.8g.
The sun-proof creams of O/W/O multiplet are prepared by above-mentioned raw materials, steps are as follows:
(1) 85 DEG C are heated to after mixing interior oily phase raw material, obtains finely dispersed interior oil phase component;
(2) it is heated to 85 DEG C after mixing interior emulsifier phase, polyalcohol with water, obtains finely dispersed water phase components;
(3) outer oil is mutually mixed and heated to 50 DEG C with outer emulsifier phase, obtains finely dispersed outer oil phase component;
(4) with revolving speed whipping step (2) resulting water phase components of 500rpm, while the resulting interior oil of step (1) is added Phase component stirs 5min, obtains O/W type colostric fluid;
(5) the O/W type colostric fluid for obtaining step (4) carries out high-pressure homogeneous processing, and homogeneous is pressure 900bar, circulation time Number is 3 times, forms O/W type nanoemulsions, this lotion is cooled under the revolving speed stirring of 500rpm to 50 DEG C;
(6) the resulting outer oily phase of whipping step (3) under the revolving speed of 600rpm, by the resulting O/W type nano-emulsion of step (5) Liquid is added in (3) system, is stirred 6min, is obtained O/W/O type colostric fluid;
(7) by O/W/O type colostric fluid obtained by (6), it is more to obtain O/W/O by the homogeneous 4min at homogeneous speed 16000r/min Weight structure nanoemulsions;
(8) the O/W/O multiplet nanoemulsions for obtaining step (7) stir cooling with the speed of 400rpm, cool to 40 DEG C, preservative is added and stirs evenly, is subsequently cooled to room temperature to get the sun-proof creams of O/W/O multiplet.
Measure of merit
The sun-proof creams of O/W/O multiplet of Examples 1 to 3 preparation are carried out SPF test (sun protection test) respectively, are had Body test method is as follows:
Instrument:
UV-2000S ultraviolet transmission analysis tester, PMMAHD6 plate, assay balance, antistatic disposable finger cot, disposably 1mL asepsis injector.
Operating procedure:
Using 1mL one-shot injector pipette samples and be loaded on PMMAHD6 plate, sample is equal with enough and size Even drop is added on plate (1.35mg/cm2), it then puts on fingerstall and is smeared, smearing the time should not the too long but guarantor that do the best Card smears the uniformity of sample, and sample surplus is accurately controlled with assay balance after sample-adding amount and smearing.It has smeared sun-proof The carrier board of sample is placed horizontally at dull thread straight shot places desiccated balance 20min at normal temperature, then ultraviolet with UV-2000S Analysis tester is penetrated to be tested, every piece of carrier board tests 12 different positions, each position carry out respectively 290nm~ The transmitance of 400nm scans.Then the SPF of sample is calculated according to the scan data of 12 positions.The calculation formula of SPF are as follows:
In formula 1, E (λ) --- erythemal effect coefficient (CIE-1987);
I (λ) --- the radiation intensity of the UV light source of the instrument for SPF test;
A0The average monochromatic absorbance of each sample panel before (λ) --- UV irradiates;
The step-length (1nm) of d (λ) --- wavelength.
The spf value that 12 positions calculate is averaged, the spf value as sample to be tested;It respectively will be to Examples 1 to 3 Calculated spf value is listed in Table 1 below after sample test.
Table 1: the sun protection factor of the sun-proof creams of Examples 1 to 3
By 1 data of table this it appears that: the sun-proof creams of O/W/O multiplet provided by the invention have it is good sun-proof Property, to skin refreshing non-greasy.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of sun-proof creams of O/W/O multiplet, which is characterized in that comprise the following components in parts by weight:
The interior oil mutually includes solid oil phase and liquid oil phase;The solid oil mutually includes solid-state sun-screening agent and Solid lipid;Institute Stating liquid oil phase includes liquid sun-screening agent and liquid fatty substance.
2. sun-proof creams according to claim 1, which is characterized in that solid oil phase and liquid oil phase in the interior oily phase Mass ratio is 1:5~9:1.
3. sun-proof creams according to claim 1 or 2, which is characterized in that solid-state sun-screening agent includes 3- in the interior oily phase Benzylidene camphor, 4- methyl benzyl subunit camphor, benzophenone-3, UVNUL MS-40, bis-ethylhexoxyphenol methoxyphenyl triazine, fourth Methoxydibenzoyl-methane, the own ester of diethylamino oxybenzene formylbenzoate, Diethylhexyl Butamido Triazon, first The mixture of one or more of phenol song azoles trisiloxanes, dimethyl PABA ethylhexyl and Uvinul T 150.
4. sun-proof creams according to claim 1 or 2, which is characterized in that Solid lipid includes solid-state in the interior oily phase One or more of grease, chain saturated fatty acids, long-chain saturated fatty alcohol, solid-state esters, long chain alkane and wax class are mixed Close object;
The solid grease includes the mixture of one or more of vaseline, Butyrospermum parkii fruit rouge and rilanit special;
The chain saturated fatty acids include in lauric acid, myristic acid, palmitinic acid, stearic acid, behenic acid and behenic acid One or more of mixtures;
The long-chain saturated fatty alcohol includes cetanol, stearyl alcohol, cetostearyl alcohol, docosyl alcohol, laruyl alcohol, lauryl alcohol, Pork and beans One of cool alcohol, tetradecyl alchohol, hexadecanol, octadecyl alcolol, palmityl alcohol, docosanol, isooctadecanol, cholesterine and phytosterol or Several mixtures;
The solid-state esters include palmitin, stearine, glycerol tristearate, glycerol three (behenic acid) Ester, glycerol three (isostearic acid) ester, glycerol three (eicosane diacid) ester, glyceryl behenate, glyceryl monostearate, cetanol Stearate, cetanol palmitate, cetyl dimethicone, stearoxyl trimethyl silane, C30~C45 alkyl Polymethyl siloxane, C30~C45 alkanol dimethyl silane, poly- propyl silsesquioxane, cetearyl methyl polysilicone Alkane, stearyl dimethione and acrylic acid/stearyl alcohol acrylate/dimethyl silicone polymer methacrylate copolymer One or more of mixture;
The long chain alkane is vaseline;
The wax class include beeswax, spermaceti, Brazil wax, candelila wax, rice bran wax, rice wax, lacca, ceresine, ceresin, The mixture of one or more of lignite wax, paraffin and microwax.
5. sun-proof creams according to claim 1 or 2, which is characterized in that liquid sun-screening agent includes pair in the interior oily phase One of methoxycinnamate isoamyl valerate, ethylhexyl methoxy cinnamate, octyl salicylate, Ao Likelin and Homosalate Or several mixture;
Liquid fatty substance includes olive oil, castor oil, peanut oil, palm oil, palm-kernel oil, coconut oil, sunflower in the interior oily phase Seed oil, sesame oil, soybean oil, safflower oil, apricot kernel oil, avocado oil, evening primrose oil, rice chaff oil, Queensland nut seed oil, wheat embryo Oil, thorn A Gan tree benevolence oil, candlenut tree macadamia nut oil, rice germ oil, almond oil, olive oil, maize germ oil, rapeseed oil, peach kernel Oil, grape seed oil, peony seed oil, linseed oil, mango oil, white pond flower seed oil, jojoba seed oil, cocoa seed oil, rose hip oil, Dormant oil, isooctane, Permethyl 99A, isohexadecane, Isoeicosane, polyisobutene, C13~C15 alkane, the different alkane of C12~C20 Hydrocarbon, synthesis saualane, sucrose saualane, vegetalitas saualane, saualane, octyl dodecanol, isopropyl myristate, palmitinic acid Isopropyl ester, ethyl stearte, butyl stearate, ethyl oleate, ethyl linoleate, linoleic acid isopropyl ester, cetanol isopropyl ester, meat Myristic acid certain herbaceous plants with big flowers ester, oleic acid certain herbaceous plants with big flowers ester, oleyl alcohol oleate, cetanol ricinoleate ester, isoocanol laurate, isooctadecanol laurel Acid esters, different tridecanol myristinate, 2- hexyl certain herbaceous plants with big flowers alcohol myristinate, isooctadecanol myristinate, 2- octyl dodecanol Myristinate, 2-Ethylhexyl Alcohol palmitate, octanol palmitate, isoocanol palmitate, 2- hexyl certain herbaceous plants with big flowers alcohol palmitinic acid Ester, different cetanol palmitate, isooctadecanol palmitate, 2-Ethylhexyl Alcohol stearate, octanol stearate, 2- hexyl certain herbaceous plants with big flowers In the different certain herbaceous plants with big flowers ester of alcohol stearate, iso-spermaceti ester alcohol stearic acid, oleic acid, 2- octyl dodecanol oleate and isopropyl isostearate One or more of mixtures.
6. sun-proof creams according to claim 1, which is characterized in that the interior emulsifier phase include isomery spermaceti alcohol ether, Ceteareth -25, ceteareth -6, ceteareth -12, ceteareth -20, spermaceti are hard Hard -4 phosphorus of ester alcohol ether of lipidol polyethers -30, stereth -2, stereth -21, -6 pairs of stearates of polyglycereol, three spermaceti Acid esters, PEG-20 tribehenin acid glyceride, PEG-8 beeswax, PEG-40 stearate, PEG-32 stearate, C16~C18 alkane The mixture of one or more of base glucosides and C22 alkyl glycosides.
7. sun-proof creams according to claim 1, which is characterized in that it is described it is outer oil mutually include dimethyl silicone polymer and its Derivative and liquid fatty substance;
The dimethyl silicone polymer and its derivative include ring five dimethyl silicone polymer, cyclohexasiloxane, poly dimethyl silicon Oxygen alkane, dimethiconol, diphenyl dimethicone, aminomethyl phenyl dimethyl silicone polymer, poly dimethyl silicon Oxygen alkane cross-linking agent, alkyl dimethicone, dimethicone copolyol, dimethiconol ester, phenyl are poly- Trimethicone, sesquialter dimethyl silicone polymer, amino polydimethyl siloxane, dimethyl silicone polymer/divinyl are poly- Diformazan siloxanes/silsesquioxane cross-linked polymer, dimethyl silicone polymer/phenyl vinyl dimethione cross-linked polymeric Object, dimethyl silicone polymer/silsesquioxane copolymer, dimethyl silicone polymer/methyl polysilicone alkyl copolymer, poly dimethyl Siloxanes/vinyl dimethicone cross polymer, dimethyl silicone polymer/vinyl trimethylsilane oxygroup silicic acid Ester cross-linked polymer, dimethiconol/silsesquioxane copolymer, dimethiconol/methyl-monosilane alcohol/silicon One of acid esters cross-linked polymer, polydimethylsiloxanes ethyl dimethyl silicone polymer/methyl polysilicone alkyl copolymer are several The mixture of kind;
The liquid fatty substance includes olive oil, castor oil, peanut oil, palm oil, palm-kernel oil, coconut oil, sunflower oil, sesame Oil, soybean oil, safflower oil, apricot kernel oil, avocado oil, evening primrose oil, rice chaff oil, Queensland nut seed oil, wheat-germ oil, thorn A Gan Set benevolence oil, candlenut tree macadamia nut oil, rice germ oil, almond oil, olive oil, maize germ oil, rapeseed oil, persic oil, grape pip It is oil, peony seed oil, linseed oil, mango oil, white pond flower seed oil, jojoba seed oil, cocoa seed oil, rose hip oil, dormant oil, different pungent Alkane, Permethyl 99A, isohexadecane, Isoeicosane, polyisobutene, C13~C15 alkane, C12~C20 isoparaffin, synthesis spiny dogfish Alkane, sucrose saualane, vegetalitas saualane, saualane, octyl dodecanol, isopropyl myristate, isopropyl palmitate, tristearin Acetoacetic ester, butyl stearate, ethyl oleate, ethyl linoleate, linoleic acid isopropyl ester, cetanol isopropyl ester, myristic acid certain herbaceous plants with big flowers ester, Oleic acid certain herbaceous plants with big flowers ester, oleyl alcohol oleate, cetanol ricinoleate ester, isoocanol laurate, isooctadecanol laurate, different 13 Alcohol myristinate, 2- hexyl certain herbaceous plants with big flowers alcohol myristinate, isooctadecanol myristinate, 2- octyl dodecanol myristinate, 2-Ethylhexyl Alcohol palmitate, octanol palmitate, isoocanol palmitate, 2- hexyl certain herbaceous plants with big flowers alcohol palmitate, different cetanol Palmitate, isooctadecanol palmitate, 2-Ethylhexyl Alcohol stearate, octanol stearate, 2- hexyl certain herbaceous plants with big flowers alcohol stearate, The different certain herbaceous plants with big flowers ester of iso-spermaceti ester alcohol stearic acid, oleic acid, 2- octyl dodecanol oleate, isopropyl isostearate, carbonic acid dioctyl ester, to first One of oxygroup isoamyl cinnamate, ethylhexyl methoxy cinnamate, octyl salicylate, Ao Likelin and Homosalate or Several mixtures.
8. sun-proof creams according to claim 1, which is characterized in that the outer emulsifier phase includes the smooth olive oleic acid of sorb Ester, PEG-30 dimerization hydroxy stearic acid ester, polyglyceryl-3 diisostearate, glyceryl oleate, the poly- ricinoleic acid of polyglycereol -3 Ester, PEG-11 methyl ether dimethicone, PEG/PPG-20/22 butyl ether dimethyl silicone polymer, PEG-9 poly dimethyl silicon Oxygen alkane, PEG-3 dimethyl silicone polymer, PEG-9 methyl ether dimethicone, PEG-10 Polydimethylsiloxane, PEG-9 are poly- Dimethyl silica ethyl dimethyl silicone polymer, lauryl PEG-9 Polydimethylsiloxyethyl Dimethicone, lauryl (trimethylsiloxy group) silica ethyl of PEG-10 tri- polymethyl siloxane, PEG-12 dimethyl silicone polymer, five poly dimethyl silicon of ring Oxygen alkane, lauryl PEG/PPG-18/18 polymethyl siloxane, PEG/PPG-19/19 dimethyl silicone polymer, PEG/PPG-10/3 Oleyl ether dimethyl silicone polymer, PEG/PPG-12/16 dimethyl silicone polymer, PEG/PPG-12/18 dimethyl silicone polymer, PEG/PPG-14/4 dimethyl silicone polymer, PEG/PPG-15/15 dimethyl silicone polymer and PEG/PPG-17/18 poly dimethyl The mixture of one or more of siloxanes.
9. the preparation method of sun-proof creams described in claim 1~8 any one, comprising the following steps:
(1) interior oily phase raw material is mixed, obtains interior oil-based system;
(2) interior emulsifier phase, water and polyalcohol are mixed, obtains aqueous phase system;
(3) outer oil is mutually mixed with outer emulsifier phase, obtains outer oil-based system;
(4) the interior oil-based system that the step (1) obtains is added in the aqueous phase system that step (2) obtains and carries out the first cream Change, obtains O/W type colostric fluid;
(5) the O/W type colostric fluid for obtaining the step (4) carries out the first homogenization, obtains O/W type nanoemulsions;
(6) the O/W type nanoemulsions that the step (5) obtains are added in the outer oil-based system that step (3) obtains and carry out Two emulsifications, obtain O/W/O type colostric fluid;
(7) the O/W/O type colostric fluid for obtaining the step (6) carries out the second homogenization, obtains O/W/O type lotion;
(8) preservative is added into the O/W/O type lotion that the step (7) obtains, obtains the sun-proof creams of O/W/O type;
The limitation of the not no time sequencing in step (1)~(3).
10. the preparation method of sun-proof creams according to claim 9, which is characterized in that step (5) first homogenization Pressure be 300bar~1500bar, the cycle-index of the first homogenization is 1 time~5 times.
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CN110507550A (en) * 2019-09-19 2019-11-29 广州奥蓓斯化妆品有限公司 A kind of preparation method of Water-In-Oil packet bloom
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CN112891256A (en) * 2021-01-26 2021-06-04 广东丸美生物技术股份有限公司 Concentrated soluble matrix and preparation method and application thereof
CN113208940A (en) * 2021-04-30 2021-08-06 广州市科能化妆品科研有限公司 Refreshing and stable sunscreen composition and preparation method thereof
CN115350099A (en) * 2022-08-26 2022-11-18 广州栋方生物科技股份有限公司 Emulsification method and application of oil-in-water type sunscreen composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110302109A (en) * 2019-07-18 2019-10-08 福建省亚热带植物研究所 A kind of oil/water containing peony seed oil/oil type sunscreen and preparation method thereof
CN110507550A (en) * 2019-09-19 2019-11-29 广州奥蓓斯化妆品有限公司 A kind of preparation method of Water-In-Oil packet bloom
CN110897955A (en) * 2019-12-12 2020-03-24 芭贝拉化妆品(浙江)有限公司 Sunscreen composition and preparation method and application thereof
CN110897955B (en) * 2019-12-12 2022-04-19 芭贝拉化妆品(浙江)有限公司 Sunscreen composition and preparation method and application thereof
CN112891256A (en) * 2021-01-26 2021-06-04 广东丸美生物技术股份有限公司 Concentrated soluble matrix and preparation method and application thereof
CN113208940A (en) * 2021-04-30 2021-08-06 广州市科能化妆品科研有限公司 Refreshing and stable sunscreen composition and preparation method thereof
CN113208940B (en) * 2021-04-30 2022-12-23 广州市科能化妆品科研有限公司 Refreshing and stable sun-screening composition and preparation method thereof
CN115350099A (en) * 2022-08-26 2022-11-18 广州栋方生物科技股份有限公司 Emulsification method and application of oil-in-water type sunscreen composition
CN115350099B (en) * 2022-08-26 2023-12-29 广州栋方生物科技股份有限公司 Emulsification method of oil-in-oil type sun-screening composition and application thereof

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