CN104127335B - A kind of UV controlled release medicinal ingredient and the preparation technology of easy cleaning Pickering emulsion-type sunscreen cream - Google Patents
A kind of UV controlled release medicinal ingredient and the preparation technology of easy cleaning Pickering emulsion-type sunscreen cream Download PDFInfo
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Abstract
The invention discloses a kind of UV controlled release medicinal ingredient and the preparation technology of easy cleaning Pickering emulsion-type sunscreen cream.Through UV photoresponse type TiO2After nano grain surface activating agent, oil-phase component and water-phase component are blended, high-speed homogenization dispersion and emulsion prepares.First pass through alkyl silane modification and prepare a kind of TiO stablizing Pickering emulsion2Nano grain surface activating agent, and emulsifying mixed with water prepares object Water-In-Oil (W/O) emulsion-type sunscreen cream after being added into oil phase.Nano-particle has UV response characteristics to light, can make emulsion breaking split-phase release medicinal composition after sunlight a period of time.The inventive method is easy, and products obtained therefrom has that sun-proof result is strong, photoresponse controlled release medicinal ingredient, easy cleaned feature after sun exposure a period of time, has a good application prospect in cosmetics industry field.
Description
Technical field
The present invention relates to field of fine chemical, especially sun care preparations field.
Background technology
Sunscreen cream have the good reputation of " skin patron saint in summer ".It can not only be effectively isolated ultraviolet, pre-anti-melanin and the generation of skin carcinoma, but also has the miraculous effects such as sterilization, speckle dispelling, whitening and anti-aging.Along with development and public's enhancing to sun-proof consciousness of society, the characteristic of sunscreen cream, application and safety increasingly become focus of concern.
In current daily sunscreen cream, sunscreen mostly is the Organic substance such as benzophenone, methoxy cinnamate derivative, thus has certain toxic and side effects and zest, containing TiO2The inorganic sunscreen of nano-particle etc. substitutes Orangic sunscreen has become development trend.At present containing TiO2The sunscreen cream of nano-particle is only to utilize TiO2Nano-particle is to the reflection of ultraviolet and scattering process, and preparation technology unavoidably adds organic compound and serves as surfactant.If expecting more preferable sun-proof result, TiO just certainly will be increased2The content of nano-particle or the concentration of increase Orangic sunscreen.And organic sunscreen agent concentration is the highest, the burden causing skin can be the heaviest, TiO2Content increases, it is likely that affect stability of emulsion.The toxic and side effects of the inevitable organic additive of this preparation technology (surfactant and Orangic sunscreen) and zest, in micelle shape inside sunscreen cream mastic, be difficult to after using clean and the most do not possess medicine controlled releasing ability.Therefore, sun care preparations industry is in the urgent need to a nanoparticles stable emulsion of only using, and, easy cleaning, controlled medicinal ingredient less to skin irritation discharge, sun-proof result more preferable inorganic sunscreens frost.With ultraviolet light response TiO2The inorganic sunscreens frost of Water-In-Oil (W/O) emulsion is stablized in granule surface activity agent can effectively solve an above-mentioned difficult problem.Compared with conventional preparation techniques, the TiO of parcel dispersed as emulsions2Nano-particle good dispersion, be difficult to reunite, there is more excellent sun-proof result；And this emulsion has optical Response, after ultra-vioket radiation, particle surface chemical property changes and causes emulsion breaking release medicinal composition；Aqueous phase contact skin after emulsion breaking split-phase, containing medicinal ingredient, it is easy to clean；Additionally it is also with the TiO of doped chemical2The formula of sun screen of nanoparticles stable emulsion adapts to the ultraviolet of varying strength, and controls it and cause medicinal ingredient release in sun-exposed different time sections, excite easy cleaning ability etc..This process of preparing will become, by advantages such as its sun-proof result having is good, be readily cleaned, controllable release medicinal ingredients, the new lover preparing sun sports protection cream, and provides new thinking for the application in fields such as biologic medical, cosmetic industry, pharmaceutical engineerings of the Pickering emulsion.
Summary of the invention
In view of the above deficiency of prior art, it is desirable to provide a kind of UV controlled release medicinal ingredient and easy-clean emulsion type sunscreen cream preparation technology, it is allowed to overcome the disadvantage mentioned above of prior art.
The purpose of the present invention is realized by following means.
A kind of UV controlled release medicinal ingredient and the preparation technology of easy cleaning Pickering emulsion-type sunscreen cream, step is as follows:
The first step: TiO2Prepared by nano grain surface activating agent
(a)TiO2The preparation of nano-particle: 1) in reactant liquor each volume components ratio for butyl titanate: ethanol: deionized water: glacial acetic acid=9:36:12:40, dehydrated alcohol is added in butyl titanate, continues stirring until mix homogeneously；The mixed liquor of deionized water and glacial acetic acid is added drop-wise in ethanol and butyl titanate mixed liquor under stirring, continuously stirred, prepare vitreosol；2) vitreosol is transferred to hydrothermal synthesis reaction still and carries out 100～150 DEG C of isothermal reactions, react 2～3 hours, remove clear liquid, it is thus achieved that white TiO2Precipitation；3) by absolute ethanol washing white TiO2Precipitation, collects precipitation, adds dehydrated alcohol fully dispersed, dries, it is thus achieved that TiO2Precipitation；4) TiO that will dry2After precipitation is fully ground, it is placed in Muffle furnace 500 DEG C and calcines 30～60 minutes, prepare the TiO with photoelectric activity2Nano-particle；
(b)TiO2The surface modification of nano-particle: 1) take the TiO with photoelectric activity that (a) step obtains2Nano-particle, ultrasonic disperse 5～10 minutes；2) dispersion liquid is sealed, be placed under dark magnetic agitation 4～after 8 hours, release sealing and be placed in 45～60 DEG C of drying in baking oven；3) it is 1～in the mixed liquor of the trim,ethylchlorosilane of 5% or dodecyltrichlorosilane or silicon fluoride and cosmetics-stage oil phase that the powder after drying joins volume ratio, ultrasonic disperse 5～10 minutes, magnetic agitation 8～12 hours, period is continuously replenished oil phase and maintains initial level；4) by above-mentioned TiO2Dispersion liquid, removes clear liquid, precipitates post-drying；5) drying precipitation being fully ground, be dispersed in cosmetics-stage oil phase, under magnetic agitation state, UV light irradiates 24～32 hours, and period is continuously replenished oil phase to maintain initial soln liquid level；6) standing suspension after illumination terminates, remove oil phase after high speed centrifugation separates under 15000rpm, precipitation is dried, after being fully ground, is TiO2Nano grain surface activating agent；
Second step: oil phase and water-phase component preparation
Being dispersed in cosmetics-stage oil phase by the TiO2 nano grain surface activating agent that the first step prepares, the mass percent concentration of nano grain surface activating agent and oil phase is between 1%～3%；And it is directly mixed with aqueous phase, oil phase and aqueous phase volume ratio are between 3:2～7；
3rd step: prepare the one-tenth breast of Pickering emulsion sunscreen cream
The oil mixing with water solution ultrasonic disperse 1～5min that will obtain in second step, again with high speed disperser to dispersion liquid with 1,5000rpm rotating speed high-speed homogenization dispersion 1～5min, emulsifying adds appropriate amount of auxiliary materials the most afterwards, i.e. prepares object UV controlled release medicinal ingredient and easy cleaning Pickering emulsion-type sunscreen cream.
Aqueous phase in second step there was added one or more of following material: mass percent be 0.25%～0.5% pharmaceutically acceptable addition, glycerol, vitamin E.
Described pharmaceutically acceptable addition is a kind of in following material: the Radix Astragali, apple polyphenol, Radix Notoginseng total arasaponins.
Use that the inventive method obtains be readily cleaned, sun-proof result is good, controlled release medicinal ingredient effect obvious invention product, has that more traditional organic sunscreen frost easy cleaning, sun-proof result be higher, controlled release drug effect extremely significantly ability.Stable W/O emulsion starts breakdown of emulsion, about 12h complete breakdown of emulsion split-phase after irradiating UV about 4h, and oil reservoir floats, and medicinal ingredient discharges, and water layer directly contacts skin and makes it easier to clean.Skin is played a very good protection by the medicinal ingredient with free radical, anti-aging effects etc..The made sunscreen cream of this preparation technology has above advantage and mainly relies on the irradiation of UV light to cause TiO2Nano grain surface chemical fundamental change.This transformation causes the aggravation of emulsion unstability and then makes emulsion breaking split-phase.TiO2Nano-particle is grafted chemical group in modifying process and has sympathy to oil phase, and UV irradiates rear surface and produces hydroxyl so that this nano-particle hydrophilic strengthens, the unstability aggravation of emulsion, finally realizes stable Pickering emulsion breaking split-phase.
Accompanying drawing is described as follows:
Fig. 1 is product UV controlled release medicinal ingredient of the present invention and easy cleaning Pickering emulsion-type sunscreen cream operation principle schematic diagram:
The TiO of this research preparation2The W/O emulsion-type sunscreen cream that nano grain surface activating agent is stable, after being excited by sunlight middle-ultraviolet lamp, TiO2The surface chemical property of nano-particle changes, and ultimately results in emulsion breaking split-phase, and medicinal ingredient is released.Upper strata is mainly oil phase, and lower floor is that the aqueous phase having dissolved medical substance directly contacts skin.
Detailed description of the invention
Enforcement to the present invention is further described below in conjunction with the accompanying drawings.But it should be emphasized that embodiments below is exemplary rather than in order to limit the scope of the present invention and application.In processing step, involved chemical raw material is conventional commercial technical pure with reagent.
Embodiment 1
The first step: TiO2Nano grain surface activating agent preparation method
(a)TiO2The preparation of nano-particle: 36mL dehydrated alcohol is joined in 9mL butyl titanate, continuously stirred, obtain mixed liquor A；12mL deionized water is joined in 40mL glacial acetic acid, continuously stirred, obtain mixed liquid B.Mixed liquid B is dropwise added drop-wise in the mixed liquor A under stirring, prepares vitreosol (the regulation photoresponse time and intensity such as N element of can adulterating in colloidal sol).Vitreosol being transferred to hydrothermal synthesis reaction still and carries out 150 DEG C of isothermal reactions, the response time is 2 hours, removes the supernatant, it is thus achieved that white TiO2Precipitation.By absolute ethanol washing white TiO2Precipitation, 15000rpm high speed centrifugation 10 minutes, repeats above operation 3 times, abandoning supernatant, collects precipitation, add dehydrated alcohol and carry out fully dispersed, be placed in 60 DEG C of drying in baking oven, it is thus achieved that purer TiO2Precipitation.The TiO that will dry2Precipitation is fully ground, and is placed in 500 DEG C of Muffle furnaces calcining 30 minutes, prepares the TiO with photoelectric activity2Nano-particle.
(b)TiO2The surface modification of nano-particle: will have the TiO of photoelectric activity2Nano-particle, is poured into appropriate H2O2In, it is ensured that H2O2Solution is totally submerged TiO2Nano-particle, ultrasonic disperse 5 minutes.Dispersion liquid is sealed, is placed in magnetic agitation under dark and, after 4 hours, releases sealing and be placed in 45 DEG C of drying in baking oven.Powder after drying joins in the mixed liquor of 1mL dodecyltrichlorosilane and 20mL normal hexane, and ultrasonic disperse is after 5 minutes, then magnetic agitation 12 hours, prepares modified TiO2Dispersion liquid.Modified TiO will be stood2Dispersion liquid, 15000rpm high speed centrifugation 10 minutes, remove the supernatant, lower sediment is placed in 50 DEG C of drying in baking oven.Being dispersed in normal hexane after being fully ground by drying powder, under magnetic agitation state, UV light irradiates 24 hours (uviol lamp wavelength 254nm, power 12W, solution distance uviol lamp 10～15cm), and period is continuously replenished normal hexane to maintain initial level.Illumination stands suspension, 15000rpm high speed centrifugation 10 minutes after terminating, remove upper strata normal hexane, and lower sediment is dried, and after being fully ground, is TiO2Nano grain surface activating agent.
Second step: oil phase and water-phase component preparation and ratio
Take and there is response characteristics to light and make the TiO of emulsion breaking split-phase2Nano grain surface activating agent 0.09g adds and has dissolved in the 9mL normal hexane of the sunscreen cream compositions such as appropriate olive oil, then takes the appropriate cosmetics-stage Radix Astragali, glycerol, vitamin E etc. and be dissolved in the deionized water of 9mL.Water-oil phase is directly mixed.
3rd step: prepare the one-tenth breast method of Pickering emulsion sunscreen cream
Dispersion liquid is disperseed 3 minutes with 1,5000rpm rotating speed high-speed homogenization by the oil mixing with water solution ultrasonic disperse obtained in second step for 3 minutes again with Portable high speed disperser.Emulsifying adds the adjuvant such as appropriate amount of essence, preservative the most afterwards, i.e. prepares UV controlled release medicinal ingredient and easy cleaning Pickering emulsion-type sunscreen cream.
Embodiment 2
The first step: TiO2Nano grain surface activating agent preparation method
(a)TiO2The preparation of nano-particle: 36mL dehydrated alcohol is joined in 9mL butyl titanate, continuously stirred, obtain mixed liquor A；12mL deionized water is joined in 40mL glacial acetic acid, continuously stirred, obtain mixed liquid B.Mixed liquid B is dropwise added drop-wise in the mixed liquor A under stirring, prepares vitreosol.Vitreosol being transferred to hydrothermal synthesis reaction still and carries out 150 DEG C of isothermal reactions, the response time is 2 hours, removes the supernatant, it is thus achieved that white TiO2Precipitation.By absolute ethanol washing white TiO2Precipitation, 15000rpm high speed centrifugation 10 minutes, repeats above operation 3 times, abandoning supernatant, collects precipitation, add dehydrated alcohol and carry out fully dispersed, be placed in 60 DEG C of drying in baking oven, it is thus achieved that purer TiO2Precipitation.The TiO that will dry2Precipitation is fully ground, and is placed in 500 DEG C of Muffle furnaces calcining 30 minutes, prepares the TiO with photoelectric activity2Nano-particle.
(b)TiO2The surface modification of nano-particle: will have the TiO of photoelectric activity2Nano-particle, is poured into appropriate H2O2In, it is ensured that H2O2Solution is totally submerged TiO2Nano-particle, ultrasonic disperse 5 minutes.Dispersion liquid is sealed, is placed in magnetic agitation under dark and, after 4 hours, releases sealing and be placed in 45 DEG C of drying in baking oven.Powder after drying joins in the mixed liquor of 1mL dodecyltrichlorosilane and 20mL kerosene, and ultrasonic disperse is after 5 minutes, and magnetic agitation 12 hours prepares modified TiO2Dispersion liquid.Modified TiO will be stood2Dispersion liquid, 15000rpm high speed centrifugation 10 minutes, remove the supernatant, lower sediment is placed in 50 DEG C of drying in baking oven.Being dispersed in kerosene after being fully ground by drying powder, under magnetic agitation state, UV light irradiates 24 hours (uviol lamp wavelength 254nm, power 12W, solution distance uviol lamp 10～15cm), and period is continuously replenished kerosene to maintain initial level.Illumination stands suspension, 15000rpm high speed centrifugation 10 minutes after terminating, remove upper strata kerosene, and lower sediment is dried, and after being fully ground, is TiO2Nano grain surface activating agent.
Second step: oil phase and water-phase component preparation and ratio
Take and there is response characteristics to light and make the TiO of emulsion breaking split-phase2Nano grain surface activating agent 0.09g adds and has dissolved in the 9mL kerosene of the sunscreen cream compositions such as appropriate olive oil, then takes the appropriate cosmetics-stage Radix Astragali, glycerol, vitamin E etc. and be dissolved in the deionized water of 9mL.Water-oil phase is directly mixed.
3rd step: prepare the one-tenth breast method of Pickering emulsion sunscreen cream
Dispersion liquid is disperseed 3 minutes with 1,5000rpm rotating speed high-speed homogenization by the oil mixing with water solution ultrasonic disperse obtained in second step for 3 minutes again with Portable high speed disperser.Emulsifying adds the adjuvant such as appropriate amount of essence, preservative the most afterwards, i.e. prepares UV controlled release medicinal ingredient and easy cleaning Pickering emulsion-type sunscreen cream.
Embodiment 3
Oil phase replaces with No. 26 white oils of cosmetics-stage, and other steps are with described in embodiment 1 and embodiment 2.
Self-control Pickering emulsion-type sunscreen cream is measured its absorbance after the tradition organic sunscreen identical multiple of frost dilution respectively, according to the ultraviolet wavelength section scanning figure drawn, obtains making Pickering emulsion-type sunscreen cream sun-proof result by oneself and be better than tradition organic sunscreen frost.This is due to the TiO in self-control Pickering emulsion-type sunscreen cream2Nano-particle can not only specular scattering ultraviolet, and ultraviolet is had strong Absorption.Meanwhile, with tradition organic sunscreen frost equal dose, self-control Pickering emulsion-type sunscreen cream being applied to same vehicle, after waiting time, equal strength illumination, residue is carried out experiment and compares, self-control Pickering emulsion-type sunscreen cream easy cleaning effect is obvious.Mainly in tradition organic sunscreen frost, the content of organics such as Orangic sunscreen and emulsifying agent is higher, and makes Pickering emulsion-type sunscreen cream by oneself to have the TiO of sun-proof result2Emulsion stablized by nano grain surface activating agent, after sunlight, and TiO2Nano grain surface chemical property changes, and this transformation causes emulsion breaking split-phase, and oil phase floats, aqueous phase contact skin, it is easy to clean.TiO2Nano-particle is grafted chemical group in modifying process and has sympathy to oil phase, and UV irradiates rear surface and produces hydroxyl so that this nano-particle hydrophilic strengthens, the unstability aggravation of emulsion, finally realizes stable Pickering emulsion breaking split-phase.Finally, it be observed that breakdown of emulsion split-phase effect after self-control Pickering emulsion-type sunscreen cream illumination, and study the medicinal ingredient burst size discovery with irradiation time, self-control Pickering emulsion-type sunscreen cream about irradiates the thorough split-phase of 12h, and medicinal ingredient burst size is up to more than 90%.
The self-control Pickering emulsion-type sunscreen cream that the present invention obtains will become, by advantages such as its sun-proof result having is good, be readily cleaned, controllable release medicinal ingredients, the new lover preparing sun sports protection cream, and for Pickering emulsion in the new thinking of the application offer in the fields such as biologic medical, cosmetic industry, pharmaceutical engineering.
Claims (1)
1. a UV controlled release medicinal ingredient and the preparation work of easy cleaning Pickering emulsion-type sunscreen cream
Skill, step is as follows:
The first step: TiO2Prepared by nano grain surface activating agent
(a)TiO2The preparation of nano-particle: 1) in reactant liquor each volume components than for butyl titanate:
Ethanol: deionized water: glacial acetic acid=9:36:12:40, adds dehydrated alcohol in butyl titanate, holds
Continuous stirring is to mix homogeneously；Under stirring, the mixed liquor of deionized water and glacial acetic acid is dripped
In ethanol and butyl titanate mixed liquor, continuously stirred, prepare vitreosol；2) by transparent
Colloidal sol is transferred to hydrothermal synthesis reaction still and carries out 100～150 DEG C of isothermal reactions, reacts 2～3 hours,
Remove clear liquid, it is thus achieved that white TiO2Precipitation；3) by absolute ethanol washing white TiO2Precipitation,
Collect precipitation, add dehydrated alcohol fully dispersed, dry, it is thus achieved that TiO2Precipitation；4) will
The TiO dried2After precipitation is fully ground, it is placed in Muffle furnace 500 DEG C and calcines 30～60 minutes,
Prepare the TiO with photoelectric activity2Nano-particle；
(b)TiO2The surface modification of nano-particle: 1) take that (a) step obtains there is photoelectric activity
TiO2Nano-particle, ultrasonic disperse 5～10 minutes；2) dispersion liquid is sealed, be placed in black
Secretly descend magnetic agitation 4～after 8 hours, release sealing and be placed in 45～60 DEG C of drying in baking oven；3)
It is 1～the trim,ethylchlorosilane of 5% or dodecyl three that powder after drying joins volume ratio
In the mixed liquor of chlorosilane or silicon fluoride and cosmetics-stage oil phase, ultrasonic disperse 5～10 minutes,
Magnetic agitation 8～12 hours, period is continuously replenished oil phase and maintains initial level；4) by above-mentioned
TiO2Dispersion liquid, removes clear liquid, precipitates post-drying；5) drying precipitation is fully ground, all
Even being scattered in cosmetics-stage oil phase, under magnetic agitation state, UV light irradiates 24～32 hours,
Period is continuously replenished oil phase to maintain initial soln liquid level；6) suspension is stood after illumination terminates,
Removing oil phase after high speed centrifugation separates under 15000rpm, precipitation is dried, after being fully ground, i.e.
For TiO2Nano grain surface activating agent；
Second step: oil phase and water-phase component preparation
The TiO that the first step is prepared2Nano grain surface activating agent is dispersed in cosmetics-stage
In oil phase, the mass percent concentration of nano grain surface activating agent and oil phase 1%～3% it
Between；And it is directly mixed with aqueous phase, oil phase and aqueous phase volume ratio are between 3:2～7；
3rd step: prepare the one-tenth breast of Pickering emulsion sunscreen cream
The oil mixing with water solution ultrasonic disperse 1～5min that will obtain in second step, then with dividing at a high speed
Dissipating device to dispersion liquid with 1,5000rpm rotating speed high-speed homogenization dispersion 1～5min, after emulsifying completely
Add appropriate amount of auxiliary materials, i.e. prepare object UV controlled release medicinal ingredient and easy cleaning Pickering
Emulsion-type sunscreen cream；
Oil phase in second step there was added appropriate olive oil；
Aqueous phase in second step there was added one or more of following material: mass percent is
The pharmaceutically acceptable addition of 0.25%～0.5%, glycerol, vitamin E；
Described pharmaceutically acceptable addition is a kind of in following material: the Radix Astragali, apple polyphenol, Radix Notoginseng total arasaponins.
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| CN105496799B (en) * | 2015-12-28 | 2018-04-13 | 西北工业大学 | Stablize Pickering lotions and preparation method with optical Response by emulsifying agent of photosensitive POSS hybrid particulates |
| BR102015032897B1 (en) * | 2015-12-29 | 2021-07-20 | Natura Cosméticos S.A. | PRODUCTION PROCESS OF THIN FILM NANOSTRUCTURE OF POLYMER AMPHILICAL BLENDA WITH HIGH CONCENTRATION OF ORGANIC NUCLEUS AS AN ULTRAVIOLET RADIATION FILTER |
| CN107970137A (en) * | 2017-11-14 | 2018-05-01 | 湖南博隽生物医药有限公司 | A kind of cyclo-dextrin-modified organosilicon Pickering lotions and preparation method thereof |
| CN108641204A (en) * | 2018-05-17 | 2018-10-12 | 姚子巍 | A kind of preparation method of MPP power pipes |
| CN114129461A (en) * | 2021-11-29 | 2022-03-04 | 广州凡岛网络科技有限公司 | Sunscreen skin care product containing composite titanium dioxide and preparation method thereof |
| CN116236409A (en) * | 2023-04-14 | 2023-06-09 | 山东理工大学 | Preparation method of novel oil-in-water emulsion with antioxidant and ultraviolet-resistant activities |
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| CN101496779B (en) * | 2009-02-27 | 2011-05-04 | 深圳清华大学研究院 | Titanic oxide solid lipid nano granule, fluid dispersion and preparation method thereof |
| CN103881422B (en) * | 2014-03-21 | 2015-04-22 | 西南交通大学 | Light-operated switch type TiO2 nano-particles surfactant and preparation method thereof |
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