CN102228412A - Oil phase dispersion sunblocking concentrate of nanometer titania and preparation method thereof - Google Patents
Oil phase dispersion sunblocking concentrate of nanometer titania and preparation method thereof Download PDFInfo
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- CN102228412A CN102228412A CN 201110120186 CN201110120186A CN102228412A CN 102228412 A CN102228412 A CN 102228412A CN 201110120186 CN201110120186 CN 201110120186 CN 201110120186 A CN201110120186 A CN 201110120186A CN 102228412 A CN102228412 A CN 102228412A
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Abstract
The invention discloses an oil phase dispersion sunblocking concentrate of nanometer titania and a preparation method as well as application thereof. The concentrate of the invention comprises the following materials by weight: (a) 35-60% of nanometer titania; (b) 30-62% of organic solvent which is one or more of dimethyl polysiloxane, cyclopentasiloxane, alkyl benzoate, caprylic triglyceride and capric triglyceride; (c) 1-10% of dispersing accessory which is one or more of polyhydroxystearate, polyhydroxystearic acid and polyglyceryl polysiloxane. Characterized by uniformity and stability, small viscosity, high content of effective components, obvious blocking effect against ultraviolet rays and complete permeability to visible light, the concentrate provided in the invention is beneficial for the production and processing of various sunblocking cosmetics.
Description
Technical field
The invention belongs to the sunscreen field, particularly oil phase dispersion sunscreen concentrate of a kind of nano titanium oxide and preparation method thereof.
Background technology
The radiation of sunlight middle-ultraviolet lamp has very big injury to skin, and various now artificial and unartificial factors, the atmosphere of depending on for existence to the mankind has caused destruction in various degree, causes ultraviolet amount of radiation constantly to increase, and human beings'health in serious threat.At present typical sunscreens mainly contains two kinds of ultraviolet absorber and ultraviolet light screeners.Wherein, ultraviolet absorber is mainly the organic sunscreen agent, and the molecular energy of this class sunscreen absorbs ultraviolet energy, maybe forms such as light can be discharged with heat energy, thereby minimizing is to the injury of skin again.Though this class sunscreen is to the transparency of products height, ultraviolet absorption effect is good, but skin had certain zest, UV Absorption narrow range to different wave length, when mixing cosmetic base, can contact for a long time and run off because of heating or with profit, under the irradiation of high-intensity ultraviolet, can produce chemical change, reduce or lose character such as sun-proof result, can not resist the injury of ultraviolet for a long time all sidedly skin.
Nano titanium oxide is a kind of inorganic powder material with high refractive index, as the agent of used for cosmetic physical sunscreen, have that chemical property is stable, nontoxic non-stimulated, no sensitization, high-efficiency shielding ultraviolet, to the characteristics of visible light high permeability, approved and widely used physical sunscreen agent at present.
Yet, nano titanium oxide is directly made an addition in the cosmetic formulations, it is inhomogeneous to be easy to cause sun-proof component to disperse, and the cream kind product has influences such as granular sensation, rough, no mercerization effect, skin sense difference.
At present, existing multiple disclosed method and technology preparation are the dispersion concentration thing of physical sunscreen agent with the nanometer-level inorganic powder, for example Chinese patent ZL 98811050.4, Chinese patent CN 1739480A, Japan Patent JP 160541/96 etc.Above-mentioned patented technology and products thereof influences result of use all there being certain defective aspect solid content, flowability, stability and the dispersibility.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is exactly the deficiency that exists at existing nano titanium oxide sunscreen, oil phase dispersion sunscreen concentrate of a kind of nano titanium oxide and its production and application is provided, the oil phase dispersion sunscreen concentrate solid content height of this nano titanium oxide, viscosity is low, can make nano titanium oxide more even as the physical sunscreen component, be added in the various cosmetics with sun-proof result more easily.
One aspect of the present invention provides a kind of oil phase dispersion sunscreen concentrate of nano titanium oxide, is made up of following material by weight:
(a) 35～60% nano titanium oxide;
(b) 30～62% organic solvent, described organic solvent are to be selected from dimethyl polysiloxane, ring penta siloxanes, alkyl benzoate, Trivent OCG and the tricaprin one or more;
(c) 1～10% dispersing aid, described dispersing aid are to be selected from poly-hydroxy stearic acid ester, poly-hydroxy stearic acid and the polyglyceryl polysiloxanes one or more.
Among the present invention, the preferred weight content of each component of oil phase dispersion sunscreen concentrate of described nano titanium oxide is: nano titanium oxide 40%～55%, organic solvent 40%～55% and dispersing aid 3%～5%.
Among the present invention, described nano titanium oxide is a hydrophobic nano-titanium dioxide, preferred surface covers organic hydrophobic nano titanium oxide, and preferably the model that is provided by last marine favour nanosecond science and technology company limited is SHU-103 type nano titanium oxide and SHU-108 type nano titanium oxide.The grain size of described nano titanium oxide is generally 30～100nm with conventional, and preferred 30～50nm can guarantee effectively intercepting the ultraviolet while, and visible light is had transmitance more than 90%.
Among the present invention, described organic solvent is to be selected from one or more of dimethyl polysiloxane, ring penta siloxanes, alkyl benzoate, Trivent OCG and tricaprin, a kind of in preferred alkyl benzoate and ring penta siloxanes.C12～C15 alkyl benzoate of the preferred commodity of described alkyl benzoate AB by name, the caprylic/capric triglyceride of the preferred commodity of described Trivent OCG and tricaprin GTCC by name has effect preferably.
Among the present invention, described dispersing aid is to be selected from poly-hydroxy stearic acid ester, poly-hydroxy stearic acid, methylsiloxane copolymer and the polyglyceryl polysiloxanes one or more, one or more in preferably poly-hydroxy stearic acid ester, poly-hydroxy stearic acid and the polyglyceryl polysiloxanes.
A second aspect of the present invention provides a kind of preparation method of oil phase dispersion sunscreen concentrate of described nano titanium oxide, may further comprise the steps:
1) with dispersing aid heating fusing fully;
2) in whipping process, in organic solvent, add successively the step 1) gained fully the fusing dispersing aid and nano-titanium dioxide powder, mix, oily dispersion;
3) with step 2) oily dispersion of gained adopts the method for ball milling or sand milling to carry out attrition process, and separating and removing impurities and abrasive media then promptly obtain the oil dispersion sunscreen concentrate of nano titanium oxide.
Among the present invention, the described dispersing aid of step 1) preferable 50 ℃～80 ℃ fusions.Step 2) describedly mixes preferable carrying out with high-speed mixer.What the time of the described attrition process of step 3) was preferable is 1 hour, and the method for described separating and removing impurities and abrasive media is preferably by 300～500 eye mesh screen isolated by filtration.The oil dispersion sunscreen concentrate that obtains nano titanium oxide that obtains is to have the blue glossy white oiliness dispersion concentration thing that applies.
The dynamic viscosity of the oil dispersion sunscreen concentrate of nano titanium oxide of the present invention is 30～370mPas, preferred 50～200mPas.In use, only need this concentrate is added in the sun care preparations by proportioning, and agitation as appropriate gets final product.
Related raw material among the present invention as organic solvent, dispersing aid and nano titanium oxide, is the raw material commonly used of cosmetic field.Technology is simple, and process is controlled easily.Dispersions obtained concentrate is uniform and stable, and viscosity is little, and active component content height has significant barriering effect to ultraviolet, and visible light is seen through fully.This nano titanium oxide dispersion concentration thing can be used as the physical sunscreen component and is added in the various cosmetics with sun-proof result, wherein nano titanium oxide disperse more evenly, more convenient, be beneficial to very much the production and processing of various sun care preparationss.
Description of drawings
Below in conjunction with description of drawings feature of the present invention and beneficial effect.
Fig. 1 is scanning electron microscope (SEM) photo of nano titanium oxide in the described dispersion concentration thing.
Fig. 2 is the ultraviolet-visible absorbance test pattern of nano titanium oxide in the described dispersion concentration thing.
The specific embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
Take by weighing the poly-hydroxy stearic acid ester of 15g, 135g C12～C15 alkyl benzoate (AB respectively, Britain Croda) and the 150g modified nano-titanium dioxide (go up the SHU-103 type nano titanium oxide that marine favour nanosecond science and technology company limited is produced, grain size 30～50nm), and will gather hydroxy stearic acid ester and place under 80 ℃ it is melted fully; Then load weighted poly-hydroxy stearic acid fat and modified nano-titanium dioxide are joined in whipping process in C12～C15 alkyl benzoate successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle was at last processed 1 hour with ball mill grinding, and separated with 300 purpose strainer filterings, obtained having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 50%, and dynamic viscosity is 230 ± 10mPas (25 ℃).
Embodiment 2
Take by weighing the C12～C15 alkyl benzoate of the poly-hydroxy stearic acid of 20g, 115g and the modified nano-titanium dioxide of 165g respectively and (go up the SHU-103 type nano titanium oxide that marine favour nanosecond science and technology company limited is produced, grain size 30～50nm), and will gather hydroxy stearic acid and place under 80 ℃ it is melted fully; Then load weighted poly-hydroxy stearic acid and nano titanium oxide are joined in whipping process in C12～C15 alkyl benzoate successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle is at last used grinder attrition process 1 hour, and separates with 300 purpose strainer filterings, obtains having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 55%, and dynamic viscosity is 320 ± 10mPas (25 ℃).
Embodiment 3
The modified nano-titanium dioxide that takes by weighing the poly-hydroxy stearic acid ester of 15g, the C12 of 150g～C15 alkyl benzoate and 135g respectively (is gone up the SHU-103 type nano titanium oxide that marine favour nanosecond science and technology company limited is produced, grain size 30～50nm), and will gather hydroxy stearic acid and place under 80 ℃ it is melted fully; Then load weighted poly-hydroxy stearic acid and nano titanium oxide are joined in whipping process in C12～C15 alkyl benzoate successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle is at last used grinder attrition process 1 hour, and separates with 300 purpose strainer filterings, obtains having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 45%, and dynamic viscosity is 80 ± 10mPas (25 ℃).The granular size of the nano titanium oxide in this dispersion concentration thing as shown in Figure 1.As seen from Figure 1, there is aggregate hardly in nano titanium oxide in the dispersion concentration thing, and particle scale between 30～50nm, is evenly distributed substantially.The assimilation effect of ultraviolet light and visible light as shown in Figure 2.As seen from Figure 2, the titanium dioxide of nanoscale sees through fully to visible light when having high ultraviolet shielded effect, so product has the transparency after coating.
Embodiment 4
Take by weighing the poly-hydroxy stearic acid of 25g, the poly-hydroxy stearic acid ester of 5g, C12～C15 alkyl benzoate of 90g and the modified nano-titanium dioxide of 180g respectively and (go up the SHU-103 type nano titanium oxide that marine favour nanosecond science and technology company limited is produced, grain size 30～50nm), and will gather hydroxy stearic acid and poly-hydroxy stearic acid and place under 80 ℃ it is melted fully; Then load weighted poly-hydroxy stearic acid, poly-hydroxy stearic acid ester and nano titanium oxide are joined in whipping process in C12～C15 alkyl benzoate successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle is at last used grinder attrition process 1 hour, and separates with 300 purpose strainer filterings, obtains having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 60%, and dynamic viscosity is 370 ± 10mPas (25 ℃).
Embodiment 5
Take by weighing the polyglyceryl polysiloxanes of 15g, ring penta siloxanes of 165g and the modified nano-titanium dioxide of 120g respectively and (go up the SHU-108 type nano titanium oxide that marine favour nanosecond science and technology company limited is produced, grain size 50～100nm), and the polyglyceryl polysiloxanes places under 80 ℃ it is melted fully; Then load weighted polyglyceryl polysiloxanes and nano titanium oxide are joined in whipping process in ring penta siloxanes successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle is at last used grinder attrition process 1 hour, and separates with 300 purpose strainer filterings, obtains having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 40%, and dynamic viscosity is 160 ± 10cp (25 ℃).
Embodiment 6
Take by weighing the poly-hydroxy stearic acid of 10g, the caprylic/capric triglyceride (GTCC of 185g respectively, the Germany peaceful Cognis of section) and the modified nano-titanium dioxide of 105g (go up the SHU-103 type nano titanium oxide of marine favour nanosecond science and technology company limited production, grain size 30～50nm), and will gather hydroxy stearic acid and place under 80 ℃ it is melted fully; Then load weighted poly-hydroxy stearic acid and nano titanium oxide are joined in the caprylic/capric triglyceride in whipping process successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle is at last used grinder attrition process 1 hour, and separates with 300 purpose strainer filterings, obtains having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 35%, and dynamic viscosity is 30 ± 10mPas (25 ℃).
Embodiment 7
Take by weighing the polyglyceryl polysiloxanes of 3g, the dimethyl polysiloxane of 185g and the modified nano-titanium dioxide of 112g respectively and (go up the SHU-108 type nano titanium oxide that marine favour nanosecond science and technology company limited is produced, grain size 50～100nm), and the polyglyceryl polysiloxanes placed it is melted fully; Then load weighted polyglyceryl polysiloxanes and nano titanium oxide are joined in the dimethyl polysiloxane in whipping process successively, and mix with high-speed mixer; The oily dispersion that will contain nano-particle is at last used grinder attrition process 1 hour, and separates with 300 purpose strainer filterings, obtains having the blue glossy white oiliness dispersion concentration thing that applies.Concentrate is uniform and stable, and solid content is 35%, and dynamic viscosity is 130 ± 10mPas (25 ℃).
Claims (9)
1. the oil phase dispersion sunscreen concentrate of a nano titanium oxide is characterized in that, is made up of following material by weight:
(a) 35～60% nano titanium oxide;
(b) 30～62% organic solvent, described organic solvent are to be selected from dimethyl polysiloxane, ring penta siloxanes, alkyl benzoate, Trivent OCG and the tricaprin one or more; With
(c) 1～10% dispersing aid, described dispersing aid are to be selected from poly-hydroxy stearic acid ester, poly-hydroxy stearic acid and the polyglyceryl polysiloxanes one or more.
2. the oil phase dispersion sunscreen concentrate of nano titanium oxide as claimed in claim 1 is characterized in that the weight content of described each component is: nano titanium oxide 40%～55%, organic solvent 40%～55% and dispersing aid 3%～5%.
3. the oil phase dispersion sunscreen concentrate of nano titanium oxide as claimed in claim 1 is characterized in that, the mean diameter of described nano titanium oxide is 10～100nm.
4. the oil phase dispersion sunscreen concentrate of nano titanium oxide as claimed in claim 1 is characterized in that described nano titanium oxide is a hydrophobic nano-titanium dioxide.
5. the oil phase dispersion sunscreen concentrate of nano titanium oxide as claimed in claim 1 is characterized in that, described alkyl benzoate is C12～C15 alkyl benzoate of commodity AB by name.
6. the oil phase dispersion sunscreen concentrate of nano titanium oxide as claimed in claim 1 is characterized in that, described Trivent OCG and tricaprin are the caprylic/capric triglyceride of commodity GTCC by name.
7. the oil phase dispersion sunscreen concentrate of nano titanium oxide as claimed in claim 1 is characterized in that, dynamic viscosity is 30～370mPas.
8. the preparation method as claim 1～7 oil phase dispersion sunscreen concentrate of nano titanium oxide as described in each is characterized in that, may further comprise the steps:
1) with dispersing aid heating fusing fully;
2) in whipping process, in organic solvent, add successively the step 1) gained fully the fusing dispersing aid and nano-titanium dioxide powder, mix, oily dispersion;
3) with step 2) oily dispersion of gained adopts the method for ball milling or sand milling to carry out attrition process, and separating and removing impurities and abrasive media then promptly obtain the oil dispersion sunscreen concentrate of nano titanium oxide.
9. as the application in the preparation sun care preparations of the oil phase dispersion sunscreen concentrate of the described nano titanium oxide of claim 1～7.
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| CN103520024A (en) * | 2013-10-30 | 2014-01-22 | 东南大学 | Titanium dioxide nanostructure lipid carrier and preparation method thereof |
| CN105209010A (en) * | 2013-03-14 | 2015-12-30 | 雅芳产品公司 | Long-wearing glossy lipcolor |
| CN106333867A (en) * | 2016-10-27 | 2017-01-18 | 广州市玮弘祺生物科技有限责任公司 | Sun-screening composition and preparation method and application thereof |
| CN115463054A (en) * | 2022-09-30 | 2022-12-13 | 上海臻臣化妆品有限公司 | Sunscreen composition and preparation method thereof |
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| CN101330898A (en) * | 2005-12-14 | 2008-12-24 | 株式会社资生堂 | Dispersion of fine titanium oxide particles and cosmetic preparation containing the same |
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| CN1732886A (en) * | 2005-08-09 | 2006-02-15 | 安徽大学 | Inorganic nanometer sunshade emulsion of maniod eibish and its preparation process |
| US20090191273A1 (en) * | 2005-09-23 | 2009-07-30 | Croda International Plc | Metal Oxide Dispersion |
| CN101330898A (en) * | 2005-12-14 | 2008-12-24 | 株式会社资生堂 | Dispersion of fine titanium oxide particles and cosmetic preparation containing the same |
| US20090098206A1 (en) * | 2005-12-23 | 2009-04-16 | Croda International Plc | Particulate Metal Oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105209010A (en) * | 2013-03-14 | 2015-12-30 | 雅芳产品公司 | Long-wearing glossy lipcolor |
| US11077049B2 (en) | 2013-03-14 | 2021-08-03 | New Avon Llc | Long-wearing glossy lipstick |
| CN103520024A (en) * | 2013-10-30 | 2014-01-22 | 东南大学 | Titanium dioxide nanostructure lipid carrier and preparation method thereof |
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| CN115463054A (en) * | 2022-09-30 | 2022-12-13 | 上海臻臣化妆品有限公司 | Sunscreen composition and preparation method thereof |
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Application publication date: 20111102 |