CN109620756B - Organosilicon composite powder for cosmetics and preparation method thereof - Google Patents
Organosilicon composite powder for cosmetics and preparation method thereof Download PDFInfo
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- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
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Abstract
The invention provides an organosilicon composite powder for cosmetics, which is characterized by being prepared from the following components: hydrogen-containing silicone oil, unsaturated compounds, catalysts, inorganic nano powder, organosilicon spherical resin powder and organosilicon dispersants. The average particle size range of the composite powder is 3-100 microns, and the composite powder is in a multilayer wrapping structure: the organosilicon spherical resin powder wraps the organosilicon spherical rubber powder, and the inorganic nanometer powder is uniformly dispersed in the organosilicon spherical rubber powder. The nano powder can not agglomerate to influence the skin feel and the ultraviolet protection effect during the processing or the use of cosmetics, can not contact with the skin to conduct free radicals to the skin, improves the efficacy of the nano physical sun-screening agent through the integral wrapping technology, simultaneously eliminates the adverse effect of the nano physical sun-screening agent on the skin, and is mild and does not stimulate the skin.
Description
Technical Field
The invention belongs to the technical field of organic silicon materials, and particularly relates to organic silicon composite powder for cosmetics and a preparation method thereof.
Background
The organosilicon elastic microsphere powder is widely used in cosmetics due to the characteristics of good oil absorption, dryness, smoothness and the like, and can be used as a skin feeling promoting additive; methods for preparing silicone elastic microspheres have been reported (e.g. US 4761454, US 4742142, US 4962165, US 6497894B1, US 8133586B2, CN 103122070).
The methods disclosed in US 4761454, US 4742142, US 4962165, US 6497894B1 and the like for preparing silicone elastic microspheres all utilize a large amount of small molecular surfactants (such as polyoxyethylene alkyl ether and the like) as emulsifiers to emulsify vinyl-containing silicone oil and hydrogen-containing silicone oil to form emulsions, and then crosslink the emulsions to obtain the silicone elastic microspheres. The organic silicon microspheres are easy to agglomerate and difficult to disperse in application, and a large amount of micromolecule surfactants are adsorbed on the surfaces of the organic silicon elastic microspheres, so that the organic silicon elastic microspheres have certain irritation to limit the application of the organic silicon elastic microspheres in cosmetics.
Patents US 8133586B2 and CN103122070, etc. report silicone microspheres having surfaces coated with polyorganosilsesquioxane, which have excellent anti-coagulation properties and dispersibility, and a method for preparing the same; the preparation method comprises preparing organosilicon elastic microsphere by the method of the above patent (such as US 4761454), and hydrolyzing silane coupling agent in the presence of alkali and surfactant to deposit polyorganosilsesquioxane on the organosilicon microsphere; the method is complicated, has high cost, can bring small molecular surfactant, and can not avoid pungent odor after drying. Patents US5948469 and US7648766B2 disclose methods for preparing silicone elastic microspheres coated with inorganic fine particles such as silica and titanium dioxide, which also require preparing a stable aqueous dispersion of silicone elastic microspheres in advance, and then adsorbing inorganic fine particles such as silica and titanium dioxide on the surface of the microspheres, which is complicated in preparation method, and it is difficult to avoid using surfactants or other emulsion stabilizers, and the odor is not mild enough. Other patents report that the elastic microsphere powder coated with inorganic nanoparticles prepared by the Pickering emulsion technology (the inorganic nanoparticles can play the role of a small molecular surfactant or other emulsion stabilizers and can be coated on the surface of the organic silicon elastic microspheres) has the defects of poor powder dispersion fluidity, adverse effect on human skin caused by the inorganic nanoparticles remained on the surface of the powder and the like.
Disclosure of Invention
The invention provides novel organic silicon multifunctional composite powder for cosmetics and a preparation method thereof, the preparation method can be used for directly and continuously preparing various and multifunctional organic silicon spherical composite micro powder, the obtained organic silicon composite powder has uniform and true spherical appearance, fine and smooth skin feel, good powder dispersion and fluidity, no odor and stimulation, mildness and high safety, repeated polymerization is not needed, special manufacturing equipment is not needed, the process is simple, the production efficiency is high, the manufacturing process is safe and environment-friendly, and industrial production can be stably carried out.
The invention is realized by adopting the following modes: a cosmetic silicone composite powder comprising the following components: hydrogen-containing silicone oil, unsaturated compounds, catalysts, inorganic nano powder, organic silicon spherical resin powder and organic silicon dispersing agents;
the hydrogen-containing silicone oil has at least two silicon hydrogen bonding alkanes in the molecule, and the hydrogen content is 0.01-1.5%;
the unsaturated compound is polydimethylsiloxane or an alpha, omega-diene compound containing at least two vinyl groups per molecule, and the content of the vinyl groups is 0.1-3%;
the catalyst is an isopropanol solution of chloroplatinic acid or a vinyl platinum complex of a catalyst for hydrosilylation, and the dosage of the catalyst is 1-100 ppm (calculated by platinum atomic mass fraction);
the inorganic nano powder is oleophylic silicon-treated nano titanium dioxide, silicon-treated nano zinc oxide or silicon-treated nano barium sulfate and the like, and the dosage of the inorganic nano powder is 2-20% of the total weight of all the substances participating in the preparation process;
the organic silicon spherical resin powder is polymethyl silsesquioxane spherical powder, and the average particle size of the organic silicon spherical resin powder is 0.5-10 microns;
the organic silicon dispersing agent is polyether modified silicone oil or polyglycerol modified silicone oil, and the dosage of the organic silicon dispersing agent is 0.1-0.6% of the total weight of all the materials participating in the preparation process.
Preferably, the average particle size of the composite powder is in the range of 3-100 microns.
Preferably, the composite powder is in a multilayer wrapping structure: the organosilicon spherical resin powder is coated with organosilicon spherical rubber powder which is polymerized by hydrogen-containing silicone oil, unsaturated compounds and catalysts, and inorganic nano powder is uniformly dispersed in the organosilicon spherical rubber powder.
The invention also provides a preparation method of the organic silicon composite powder for cosmetics, which comprises the following steps:
(1) adding the organic silicon spherical resin powder, the organic silicon dispersing agent and a proper amount of water into a reactor, uniformly mixing, and stirring at a low speed to prepare an aqueous dispersion;
(2) uniformly mixing an unsaturated compound, hydrogen-containing silicone oil and inorganic nano powder, adding a catalyst, and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at the temperature of below 30 ℃ for 1-5min to form emulsion, heating to 60-100 ℃, reacting for 2-6 h, and performing vacuum drying or spray drying on the emulsion after the reaction is finished to obtain dry powder;
(4) and (4) grinding and dispersing the dry powder obtained in the step (3), and screening the powder by using a 100-200-mesh screen to obtain the organic silicon composite multifunctional spherical powder for cosmetics, wherein the average particle size is 3-100 microns.
The invention has the beneficial effects that:
the invention adopts pre-stirring to disperse nano inorganic powder in an organic silicon rubber intermediate mixture, and through catalytic crosslinking, the anti-ultraviolet inorganic nano powder is uniformly dispersed and fixed in an elastic silicon rubber body in the composite powder, so that no nano powder agglomeration occurs to influence skin feel and anti-ultraviolet effect in cosmetic processing or use, and no contact with skin to conduct free radicals to the skin, the efficacy of the nano physical sun-screening agent is improved through an integral wrapping technology, and the adverse effect of the nano physical sun-screening agent on the skin is eliminated.
The invention adopts small-particle-size organosilicon spherical resin powder and a trace amount of organosilicon dispersant, the dosage of which is less than one tenth of that of an emulsion stabilizer adopted by the common emulsion polymerization technology, and the organosilicon spherical resin powder is skillfully compounded to be used as the emulsion stabilizer in the emulsion polymerization process, after the reaction is finished, the organosilicon spherical resin powder is uniformly and tightly adsorbed on the outer surface layer of the composite powder, so that the silicon rubber elastic composite powder has dispersion fluidity, and meanwhile, the inorganic nano-powder dispersed in an internal elastomer is interrupted to be contacted with the outside, so that the free radicals generated in sun protection are effectively prevented from contacting the skin, thereby achieving multiple purposes.
The outer layer of the multilayer-structure composite powder is uniformly wrapped by micron-sized spherical organic silicon resin powder, so that the contact of free radicals generated by the nano sun-screening powder photocatalyst with skin is effectively isolated, the negative effect of a nano inorganic sun-screening agent on the skin is reduced, and the flowability, the dispersibility and the effectiveness of the composite powder are improved.
Because a trace amount of organic silicon dispersing agent is used as an emulsifying aid, and the organic silicon dispersing agent can be cleaned by a water washing process after the reaction is finished, the product has no odor residue of a common emulsifier, and the composite powder is mild, non-irritant and smooth in skin feel, and completely meets the requirements of cosmetics on high performance, safety and mildness of raw materials.
The process is advanced and ingenious, can directly and continuously prepare the multi-variety and multi-functional organosilicon spherical composite micro powder, and has the advantages of high efficiency, safety, environmental protection and high stability of large-scale production in the production process.
Drawings
FIG. 1 is a schematic diagram showing that nano-scale physical sun-screening agents such as nano titanium dioxide, zinc dioxide and barium sulfate are uniformly dispersed and fixed in organic silicon spherical rubber micro-powder to eliminate adverse effects caused by nano-powder agglomeration.
FIG. 2 is a representation of the organosilicon composite powder of the invention by microscopic electron microscopy.
Fig. 3 is a representation of the inventive silicone composite powder by microscopic electron microscopy (× 700).
FIG. 4 is a representation of the organosilicon composite powder in a microscopic electron microscope (X6500).
Detailed Description
In order to more concisely and clearly demonstrate technical solutions, objects and advantages of the present invention, the following detailed description of the present invention is provided with reference to specific embodiments and accompanying drawings.
Example 1
(1) Adding 9.5g of organic silicon spherical resin powder (with the average particle size of 1.5 microns) and 0.32g of polyether modified silicone oil (with the HLB value of 10-15) into 49.8g of water, and stirring at a low speed to prepare an aqueous dispersion;
(2) mixing 26.8g of vinyl silicone oil (the vinyl content is 1.1%) with the viscosity of 100cSt, 3.2g of hydrogen-containing silicone oil (the hydrogen content is 0.6%) with the viscosity of 60cSt and 10g of silicon-treated nano titanium dioxide, adding 40ppm of catalyst (calculated according to the mass fraction of platinum atoms), and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at a temperature below 30 ℃ to form an emulsion, heating to 60-100 ℃, reacting for 2-6 hours, and carrying out vacuum drying or spray drying on the emulsion after the reaction is finished;
(4) and grinding and dispersing the obtained dry powder, and screening the powder by a screen with 100-200 meshes to obtain the organic silicon composite multifunctional spherical powder for cosmetics, wherein the average particle size is 10-30 microns.
Example 2
(1) Adding 14.6g of organic silicon spherical resin powder (with the average particle size of 1.5 microns) and 0.15g of polyether modified silicone oil (with the HLB value of 10-15) into 56.8g of water, and stirring at a low speed to prepare an aqueous dispersion;
(2) mixing 14.2g of vinyl silicone oil (the vinyl content is 0.75%) with the viscosity of 200cSt, 5.4g of hydrogen-containing silicone oil (the hydrogen content is 0.6%) with the viscosity of 60cSt and 8g of silicon-treated nano titanium dioxide, adding 50ppm of catalyst (calculated according to the mass fraction of platinum atoms), and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at a temperature below 30 ℃ to form an emulsion, heating to 60-100 ℃, reacting for 2-6 hours, and carrying out vacuum drying or spray drying on the emulsion after the reaction is finished;
(4) and grinding and dispersing the obtained dry powder, and screening the powder by a screen with 100-200 meshes to obtain the organic silicon composite multifunctional spherical powder for cosmetics, wherein the average particle size is 10-30 microns.
Example 3
(1) Adding 11g of organic silicon spherical resin powder (with the average particle size of 2 microns) and 0.38g of polyether modified silicone oil (with the HLB value of 10-15) into 54.6g of water, and stirring at a low speed to prepare an aqueous dispersion;
(2) mixing 25.7g of vinyl silicone oil (the vinyl content is 0.75%) with the viscosity of 200cSt, 2.3g of hydrogen-containing silicone oil (the hydrogen content is 0.25%) with the viscosity of 300cSt and 6g of silicon-treated nano zinc oxide, adding 50ppm of catalyst (calculated according to the mass fraction of platinum atoms), and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at a temperature below 30 ℃ to form an emulsion, heating to 60-100 ℃, reacting for 2-6 hours, and carrying out vacuum drying or spray drying on the emulsion after the reaction is finished;
(4) and grinding and dispersing the obtained dry powder, and sieving the powder by a 100-200-mesh sieve to obtain the organic silicon composite multifunctional spherical powder for cosmetics, wherein the average particle size is 30-50 microns.
Example 4
(1) Adding 13.6g of organic silicon spherical resin powder (with the average particle size of 5 microns) and 0.35g of polyether modified silicone oil (with the HLB value of 10-15) into 51.8g of water, and stirring at a low speed to prepare an aqueous dispersion;
(2) mixing 21.4g of vinyl silicone oil (the vinyl content is 0.75%) with the viscosity of 200cSt, 8.6g of hydrogen-containing silicone oil (the hydrogen content is 0.6%) with the viscosity of 60cSt and 5g of silicon-treated nano titanium dioxide, adding 30ppm of catalyst (calculated according to the mass fraction of platinum atoms), and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at a temperature below 30 ℃ to form an emulsion, heating to 60-100 ℃, reacting for 2-6 hours, and carrying out vacuum drying or spray drying on the emulsion after the reaction is finished;
(4) and grinding and dispersing the obtained dry powder, and sieving the powder by a 100-200-mesh sieve to obtain the organic silicon composite multifunctional spherical powder for cosmetics, wherein the average particle size is 20-40 microns.
Example 5
(1) Adding 13.2g of organic silicon spherical resin powder (with the average particle size of 3.5 microns) and 0.25g of polyether modified silicone oil (with the HLB value of 10-15) into 56.8g of water, and stirring at a low speed to prepare an aqueous dispersion;
(2) mixing 23.8g of vinyl silicone oil (the vinyl content is 0.26%) with the viscosity of 1500cSt, 2.2g of hydrogen-containing silicone oil (the hydrogen content is 0.25%) with the viscosity of 300cSt and 4g of silicon-treated nano zinc oxide, adding 40ppm of catalyst (calculated according to the mass fraction of platinum atoms), and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at a temperature below 30 ℃ to form an emulsion, heating to 60-100 ℃, reacting for 2-6 hours, and carrying out vacuum drying or spray drying on the emulsion after the reaction is finished;
(4) and grinding and dispersing the obtained dry powder, and sieving the powder by a 100-200-mesh sieve to obtain the organic silicon composite multifunctional spherical powder for cosmetics, wherein the average particle size is 40-90 microns.
The composite powders prepared in examples 1 to 5 were subjected to effect evaluation
1. The results of the physical and chemical tests carried out on the silicone composite powders prepared in examples 1 to 5 of the present invention are shown in table 1:
table 1: index data for Silicone composite powders prepared in examples 1-5
2. Evaluation of ultraviolet absorbance
The measurement of UV wavelength absorbance of the silicone composite powder according to examples 1 to 5 was measured using a UV/VIS spectrophotometer model V-550(JASCO, japan) as follows. As a control, a commercially available composite powder containing silica and titanium dioxide (containing no silicone spherical resin powder and silicone dispersant) in which fine particles of titanium oxide were distributed in solid silica particles was used, and the particle size of the composite powder of the control was 4 μm.
Table 2: UV absorbance values of examples 1 to 5 and comparative example
As a result, as shown in table 2, since titanium dioxide or zinc oxide nanoparticles easily form aggregates which hardly exhibit good UV absorption, it was surprisingly observed that a relatively large amount of titanium dioxide or zinc oxide nanoparticles are used in examples 1 and 2, whose ultraviolet absorbance values were still higher than those of examples 3, 4, and 5, indicating that a relatively large amount of titanium dioxide or zinc oxide nanoparticles did not form aggregates, and were uniformly dispersed in the silicone composite powder and were fixedly wrapped therein. Compared with a control group, the commercial composite powder which does not contain the organic silicon spherical resin powder and the organic silicon dispersing agent has lower ultraviolet absorbance value, so that the effective sun-screening effect can not be achieved.
3. Security assessment
Patch test on human skin
Number of test population: 100 persons; age: between 20-50 years old; health condition: the tested skin is healthy, has no allergic history of the skin disease and meets the voluntary selection standard of the tested subject. The total number was 5 groups of 20 people each.
The spot pasting method comprises the following steps: selecting a qualified spot tester, coating about 0.020 g-0.025 g of a tested object in the spot tester in a closed spot patch experiment mode, externally coating the back of the tested object with a special adhesive tape, removing the tested object after 24 hours, observing skin reactions after 0.5, 6, 12, 24 and 48 hours after the tested object is removed respectively, and recording the results according to the skin reaction grading standard in the cosmetic hygiene Specification.
And (3) test results:
the result of the human body skin patch test shows that: each group of subjects pass the composite powder patch test of the invention of examples 1-5, and observe skin reactions at 0.5, 6, 12, 24 and 48 hours, wherein 0 case has adverse skin reactions, which indicates that the composite powder is safe to use and mild and non-irritant to human body.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (2)
1. A cosmetic silicone composite powder, characterized by comprising the following components: hydrogen-containing silicone oil, unsaturated compounds, catalysts, inorganic nano powder, organic silicon spherical resin powder and organic silicon dispersing agents;
the hydrogen-containing silicone oil has at least two silicon hydrogen bonding alkanes in the molecule, and the hydrogen content is 0.01-1.5%;
the unsaturated compound is polydimethylsiloxane or an alpha, omega-diene compound containing at least two vinyl groups per molecule, and the content of the vinyl groups is 0.1-3%;
the catalyst is an isopropanol solution of chloroplatinic acid or a vinyl platinum complex, and the dosage of the catalyst is 1-100 ppm in terms of mass fraction of platinum atoms;
the inorganic nano powder is oleophylic silicon-treated nano titanium dioxide, silicon-treated nano zinc oxide or silicon-treated nano barium sulfate, and the dosage of the inorganic nano powder is 2-20% of the total weight of all the substances participating in the preparation process;
the organic silicon spherical resin powder is polymethyl silsesquioxane spherical powder, and the average particle size of the organic silicon spherical resin powder is 0.5-10 microns;
the organic silicon dispersing agent is polyether modified silicone oil or polyglycerol modified silicone oil, and the dosage of the organic silicon dispersing agent is 0.1-0.6% of the total weight of all the substances participating in the preparation process;
the composite powder is in a multilayer wrapping structure: the organosilicon spherical resin powder wraps organosilicon spherical rubber powder which is polymerized by hydrogen-containing silicone oil, unsaturated compounds and catalysts, and inorganic nano powder is uniformly dispersed in the organosilicon spherical rubber powder;
the preparation method of the organosilicon composite powder for cosmetics comprises the following steps:
(1) adding the organic silicon spherical resin powder, the organic silicon dispersing agent and a proper amount of water into a reactor, uniformly mixing, and stirring at a low speed to prepare an aqueous dispersion;
(2) uniformly mixing an unsaturated compound, hydrogen-containing silicone oil and inorganic nano powder, adding a catalyst, and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at the temperature of below 30 ℃ for 1-5min to form emulsion, heating to 60-100 ℃, reacting for 2-6 h, and performing vacuum drying or spray drying on the emulsion after the reaction is finished to obtain dry powder;
(4) and (4) grinding and dispersing the dry powder obtained in the step (3), and screening the powder by using a 100-200-mesh screen to obtain the organic silicon composite powder for cosmetics, wherein the average particle size is 3-100 micrometers.
2. A method for preparing the cosmetic silicone composite powder according to claim 1, comprising the steps of:
(1) adding the organic silicon spherical resin powder, the organic silicon dispersing agent and a proper amount of water into a reactor, uniformly mixing, and stirring at a low speed to prepare an aqueous dispersion;
(2) uniformly mixing an unsaturated compound, hydrogen-containing silicone oil and inorganic nano powder, adding a catalyst, and uniformly stirring to form organosilicon spherical rubber powder;
(3) adding the mixture obtained in the step (2) into the aqueous dispersion obtained in the step (1), stirring and mixing, homogenizing at the temperature of below 30 ℃ for 1-5min to form emulsion, heating to 60-100 ℃, reacting for 2-6 h, and performing vacuum drying or spray drying on the emulsion after the reaction is finished to obtain dry powder;
(4) and (4) grinding and dispersing the dry powder obtained in the step (3), and screening the powder by using a 100-200-mesh screen to obtain the organic silicon composite powder for cosmetics, wherein the average particle size is 3-100 micrometers.
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| CN112545907B (en) * | 2020-12-16 | 2022-02-22 | 江南大学 | Preparation method of wax beads with embedded chemical sun-screening agent and surface loaded with nano titanium dioxide and application of wax beads in sunscreen cream |
| CN114557917B (en) * | 2022-03-30 | 2024-07-26 | 彭氏(惠州)实业发展有限公司 | Sun-proof cosmetic composition |
| CN116509757B (en) * | 2023-04-13 | 2025-03-07 | 上海创美研化妆品科技有限公司 | Mild and non-irritating water-based powder cream and preparation method thereof |
| CN118021628B (en) * | 2024-01-23 | 2024-08-27 | 深圳市羽素生物科技有限公司 | Easily-dispersible sulfur microcapsule and preparation method and application thereof |
| CN117898953B (en) * | 2024-01-23 | 2024-08-30 | 深圳市羽素生物科技有限公司 | Triple-coated colloidal sulfur and preparation method and application thereof |
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