Composition, method and application for reducing free radicals on the surface of titanium dioxide powder

Abstract

The present invention relates to the technical field of cosmetics, and in particular to a composition, method and application for reducing free radicals on the surface of titanium dioxide powder. The composition comprises polymethylsilsesquioxane and triethoxyoctylsilane; the mass ratio of polymethylsilsesquioxane to triethoxyoctylsilane is 1-4:1-3. The surface of titanium dioxide powder is reduced by the sealing effect of condensation of hydroxyl free radicals on the surface of the powder and polymethylsilsesquioxane by triethoxyoctylsilane groups. The reduction of free radicals can improve the stability of active ingredients in the formula, be skin-friendly, delay aging caused by powder free radicals, increase the effective period of functional ingredients, and prevent free radicals from inducing skin aging.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and in particular to a composition, method and application for reducing free radicals on the surface of titanium dioxide powder. Background Art

[0002] Free radicals, also known as "free radicals" in chemistry, refer to atoms or groups with unpaired electrons formed by homolytic cleavage of covalent bonds in the molecules of a compound under external conditions such as light and heat. Free radicals are very active because they contain unpaired electrons, so they are extremely unstable (especially hydroxyl radicals), so they will steal electrons from neighboring molecules (including fats, proteins, and DNA) to keep themselves in a stable state. In this way, the neighboring molecule becomes a new free radical, which then steals electricity. As a result of such a chain reaction, the structure of the cell is damaged, causing loss of cell function, gene mutation, and even death.

[0003] Therefore, many cosmetics on the market add antioxidant ingredients to maintain the stability of active ingredients. They can also reduce free radicals on the skin and reduce the aging and damage caused by free radicals to the skin.

[0004] However, in recent years, the demand for skin care foundation products has been increasing. Active ingredients are added to foundations, and there are more and more functional products. However, the titanium dioxide content of foundation products is very high. If the titanium dioxide packaging in the foundation powder is not properly handled and free radicals are generated, some functional ingredients in the product will be inactivated faster and fail to achieve the desired effect. Due to the high activity and strong oxidation reaction ability of free radicals, they can attack any molecules they encounter through oxidation. Free radicals can directly destroy collagen, make cell membranes lose elasticity and flexibility, reduce the immunity of skin cells, make the skin lose elasticity and luster, and the skin color will become dull, gray and yellow, and wrinkles will appear, which will promote skin aging.

[0005] In order to solve the problem of free radicals in the above-mentioned makeup products causing skin aging, minimizing the free radicals produced by titanium dioxide is an urgent issue that needs to be addressed. Summary of the invention

[0006] In order to solve the above problems, the present invention provides a composition, method and application for reducing free radicals on the surface of titanium dioxide powder. The composition and method provided by the present invention can reduce free radicals on the surface of titanium dioxide powder.

[0007] In order to achieve the above object, the present invention provides the following technical solutions: The present invention provides a composition for reducing free radicals on the surface of titanium dioxide powder, comprising polymethylsilsesquioxane and triethoxyoctylsilane; The mass ratio of the polymethylsilsesquioxane to triethoxyoctylsilane is 1-4:1-3; The molecular formula of the polymethylsilsesquioxane is (CH3-SiO 3 / 2 )x, x is 315.78.

[0008] The present invention also provides a method for reducing free radicals on the surface of titanium dioxide powder using the composition described in the above technical solution, comprising the following steps: 1) mixing the triethoxyoctylsilane with a dispersant to obtain a triethoxyoctylsilane solution; 2) spraying the triethoxyoctylsilane solution obtained in step 1) on the surface of titanium dioxide powder, and drying to obtain silane-treated powder; The mass ratio of the titanium dioxide powder to triethoxyoctylsilane is 97-99:1-3; 3) mixing the polymethylsilsesquioxane with a dispersion to obtain a polymethylsilsesquioxane solution; The mass ratio of the titanium dioxide powder to the polymethylsilsesquioxane is 96-99:1-4; 4) mixing the silane-treated powder obtained in step 2) and the polymethylsilsesquioxane solution obtained in step 3), and allowing the mixture to stand to obtain a standing product; 5) The solid-liquid separation of the static product obtained in step 4) is carried out, and the obtained solid is dried to obtain treated titanium dioxide powder.

[0009] Preferably, in step 1), the mass ratio of triethoxycaprylylsiloxane to the dispersant is 1:1; The dispersant includes one or more of acetone, isododecane, cyclopentasiloxane and ethanol; The mixing conditions include: mixing at a rotation speed of 200 rpm for 30 minutes.

[0010] Preferably, in step 2), the triethoxyoctylsilane solution is sprayed on the surface of the titanium dioxide powder 3 to 4 times, and after each spraying, the mixture is mixed at a rotation speed of 2000 rpm for 5 to 10 minutes; The drying conditions include: temperature of 80° C. and time of 3 hours.

[0011] Preferably, in step 3), the mass ratio of polymethylsilsesquioxane to the dispersion is 1:1; The dispersion liquid comprises one or more of acetone, isododecane, cyclopentasiloxane and ethanol; The mixing conditions include: mixing at a rotation speed of 200 rpm for 30 minutes.

[0012] Preferably, in step 4), the mass ratio of the silane-treated powder solution to the polymethylsilsesquioxane solution is 1:1-2; The standing time is 12 hours.

[0013] Preferably, the drying conditions in step 5) include: temperature of 100° C. and time of 5 hours.

[0014] The present invention also provides the use of the treated titanium dioxide powder obtained by the method described in the above technical solution in reducing free radicals in base makeup products.

[0015] The present invention also provides the use of the composition described in the above technical solution in reducing free radicals on the surface of titanium dioxide powder.

[0016] In the present invention, the surface of titanium dioxide powder reduces the release of free radicals on the powder surface through the condensation of triethoxyoctylsilane groups and the sealing effect of polymethylsilsesquioxane. The reduction of free radicals can improve the stability of active ingredients in the formula, be skin-friendly, delay aging caused by powder free radicals, increase the shelf life of effective ingredients, and prevent free radicals from inducing skin aging.

[0017] Beneficial effects of the present invention: The total free radical release content of titanium dioxide treated with triethoxycaprylylsiloxane + polymethylsilsesquioxane is less than that of untreated titanium dioxide and triethoxycaprylylsiloxane treated titanium dioxide, and the amount of triethoxycaprylylsiloxane and polymethylsilsesquioxane used also has a significant difference in the total free radical release content. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments are briefly introduced below.

[0019] Figure 1 The laboratory test results of titanium dioxide powder are shown in Figure 1, which are untreated titanium dioxide powder, titanium dioxide powder treated with triethoxycaprylylsiloxane (Example 1), and titanium dioxide powder treated with triethoxycaprylylsiloxane + polymethylsilsesquioxane (Example 2). Figure 2 It is a parameter for testing the total free radical content of titanium dioxide powder on the machine. DETAILED DESCRIPTION

[0020] The invention provides a composition for reducing free radicals on the surface of titanium dioxide powder, comprising polymethylsilsesquioxane and triethoxyoctylsilane; the mass ratio of the polymethylsilsesquioxane to the triethoxyoctylsilane is 1-4:1-3; the molecular formula of the polymethylsilsesquioxane is (CH3-SiO 3 / 2)x, x is 315.78. Manufacturer: In the present invention, the polymethylsilsesquioxane is from Momentive (Shanghai) Trading Co., Ltd., origin: Japan, product model: SilFormFlexible™ fluid. In the present invention, the polymethylsilsesquioxane and triethoxyoctylsilane in the composition are preferably packaged separately.

[0021] The present invention provides a method for reducing free radicals on the surface of titanium dioxide powder using the composition described in the above technical solution, comprising the following steps: 1) mixing the triethoxyoctylsilane with a dispersant to obtain a triethoxyoctylsilane solution; 2) spraying the triethoxyoctylsilane solution obtained in step 1) on the surface of titanium dioxide powder, and drying to obtain silane-treated powder; The mass ratio of the titanium dioxide powder to triethoxyoctylsilane is 97-99:1-3; 3) mixing the polymethylsilsesquioxane with a dispersion to obtain a polymethylsilsesquioxane solution; The mass ratio of the titanium dioxide powder to the polymethylsilsesquioxane is 96-99:1-4; 4) mixing the silane-treated powder obtained in step 2) and the polymethylsilsesquioxane solution obtained in step 3), and allowing the mixture to stand to obtain a standing product; 5) The solid-liquid separation of the static product obtained in step 4) is carried out, and the obtained solid is dried to obtain treated titanium dioxide powder.

[0022] The present invention mixes the triethoxyoctylsilane with a dispersant to obtain a triethoxyoctylsilane solution. In the present invention, the mass ratio of the triethoxyoctylsiloxane to the dispersant is preferably 1:1. In the present invention, the dispersant preferably includes one or more of acetone, isododecane, cyclopentasiloxane and ethanol. In the present invention, the mixing conditions preferably include: mixing for 30 minutes at a rotation speed of 200 rpm.

[0023] The present invention sprays the obtained triethoxyoctylsilane solution on the surface of titanium dioxide powder, and obtains silane-treated powder after drying. The present invention has no special limitation on the titanium dioxide powder, and the titanium dioxide powder conventionally used in base makeup products can be used. In the present invention, the triethoxyoctylsilane solution is preferably sprayed on the surface of titanium dioxide powder 3 to 4 times, and after each spraying, it is mixed at a speed of 2000 rpm for 5 to 10 minutes, so that the triethoxyoctylsilane solution is evenly attached to the surface of the powder. In the present invention, the drying conditions preferably include: a temperature of 80°C and a time of 3 hours.

[0024] The present invention mixes the polymethylsilsesquioxane with a dispersion to obtain a polymethylsilsesquioxane solution. In the present invention, the mass ratio of the polymethylsilsesquioxane to the dispersion is preferably 1:1. In the present invention, the dispersion preferably includes one or more of acetone, isododecane, cyclopentasiloxane and ethanol. In the present invention, the mixing conditions preferably include: mixing for 30 minutes at a rotation speed of 200 rpm.

[0025] In the present invention, the mass ratio of the silane-treated powder solution to the polymethylsilsesquioxane solution is preferably 1:1 to 2. In the present invention, the standing time is preferably 12 hours.

[0026] The present invention separates the solid and liquid of the static product, dries the solid, and obtains the treated titanium dioxide powder. In the present invention, the drying conditions preferably include: a temperature of 100° C. and a drying time of 5 hours.

[0027] The present invention also provides the use of the treated titanium dioxide powder obtained by the method described in the above technical solution in reducing free radicals in base makeup products. The present invention has no special limitation on the base makeup products, and conventional base makeup products in the art can be used.

[0028] The present invention also provides the use of the composition described in the above technical solution in reducing free radicals on the surface of titanium dioxide powder.

[0029] In order to further illustrate the present invention, the present invention is described in detail below in conjunction with embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0030] Example 1 A method for reducing free radicals on the surface of titanium dioxide powder, comprising the steps of: (1) triethoxyoctylsilane was mixed with ethanol in a mass ratio of 1:1, and the mixture was stirred at 200 rpm for 30 min to obtain a transparent and uniform mixed solution; (2) spraying the transparent uniform mixed solution obtained in step (1) evenly on the surface of the titanium dioxide powder using a sprayer three times, mixing at 2000 rpm for 10 minutes after each spraying, until the transparent uniform mixed solution is evenly attached to the surface of the titanium dioxide powder; wherein the mass ratio of titanium dioxide powder to triethoxyoctylsilane is 98:2; (3) Dry the treated powder in an oven at 80°C for 3 hours to obtain silane-treated powder.

[0031] Example 2 The difference from Example 1 is that the mass ratio of titanium dioxide powder to triethoxyoctylsilane is 99:1, and the rest is the same as Example 1, to obtain silane-treated powder.

[0032] Example 3 The difference from Example 1 is that the mass ratio of titanium dioxide powder to triethoxyoctylsilane is 97:3, and the rest is the same as Example 1, to obtain silane-treated powder.

[0033] Comparative Example 1 The difference from Example 1 is that the mass ratio of titanium dioxide powder to triethoxyoctylsilane is 99.5:0.5, and the rest is the same as Example 1, to obtain silane-treated powder.

[0034] Comparative Example 2 The difference from Example 1 is that the mass ratio of titanium dioxide powder to triethoxyoctylsilane is 96:4, and the rest is the same as Example 1, to obtain silane-treated powder.

[0035] Example 4 (1) triethoxyoctylsilane was mixed with acetone in a mass ratio of 1:1, and the mixture was stirred at 200 rpm for 30 min to obtain a transparent and uniform mixed solution; (2) spraying the transparent uniform mixed solution obtained in step (1) evenly on the surface of the titanium dioxide powder using a sprayer three times, mixing at 2000 rpm for 10 minutes after each spraying, until the transparent uniform mixed solution is evenly attached to the surface of the titanium dioxide powder; wherein the mass ratio of titanium dioxide powder to triethoxyoctylsilane is 98:2; (3) drying the treated powder in an oven at 80°C for 3 hours to obtain silane-treated powder; (4) Polymethylsilsesquioxane (molecular formula: (CH3-SiO 3 / 2 )x, x is 315.78) and cyclopentasiloxane in a mass ratio of 1:1, and stirred at 200 rpm for 30 min to obtain a transparent and uniform mixed solution 1; (2) adding the silane-treated powder obtained in step (3) to the mixed solution 1 obtained in step 4) and stirring at 1500 rpm for 4 h to allow the polymethylsilsesquioxane to fully adhere to the surface of the powder, and standing for 12 h; wherein the mass ratio of titanium dioxide powder to polymethylsilsesquioxane is 98:2; (4) The cyclopentasiloxane in the supernatant of the material after the reaction is completed is recovered, and the solvent and powder are separated from the remaining material by a suction filter. The filtered powder is passed through an oven at 100°C for 5 hours to dry the material to obtain a powder with multiple surface treatments.

[0036] Example 5 The difference from Example 4 is that the mass ratio of titanium dioxide powder to polymethylsilsesquioxane is 97:3, and the rest is the same as Example 2, to obtain a powder with multiple surface treatments.

[0037] Example 6 The difference from Example 4 is that the mass ratio of titanium dioxide powder to polymethylsilsesquioxane is 99:1, and the rest is the same as Example 2, to obtain a powder with multiple surface treatments.

[0038] Example 7 The difference from Example 4 is that the mass ratio of titanium dioxide powder to polymethylsilsesquioxane is 96:4, and the rest is the same as Example 2, to obtain a powder with multiple surface treatments.

[0039] Comparative Example 3 The difference from Example 4 is that the mass ratio of titanium dioxide powder to polymethylsilsesquioxane is 99.5:0.5, and the rest is the same as Example 2, to obtain a powder with multiple surface treatments.

[0040] Comparative Example 4 The difference from Example 4 is that the mass ratio of titanium dioxide powder to polymethylsilsesquioxane is 95:5, and the rest is the same as Example 2, to obtain a powder with multiple surface treatments.

[0041] Lab Tests: Experimental method: prepare untreated titanium dioxide powder, triethoxycaprylylsiloxane treated titanium dioxide powder (Example 1), triethoxycaprylylsiloxane + polymethylsilsesquioxane treated titanium dioxide powder (Example 4), mix them evenly with pure alcohol, pour them into a transparent container after mixing evenly, continue to add 10% potassium iodide aqueous solution by mass percentage, and stir quickly and evenly, wherein the mass ratio of titanium dioxide powder: pure alcohol: 10% potassium iodide aqueous solution is 9:3:1, try to avoid air residue in the container, cover it with a lid to seal it, and then expose it to natural light for one week to promote chemical reaction.

[0042] Experimental principle: Hydroxyl free radicals will oxidize iodine ions to form elemental I2, making the solution yellow. The more free radicals released by titanium dioxide, the more elemental I2 is formed and the darker the color.

[0043] Experimental results: Results Figure 1 ,from Figure 1 It can be seen that the titanium dioxide powder treated with triethoxycaprylylsiloxane + polymethylsilsesquioxane has the lightest color, indicating that the free radical release content is less than that of untreated titanium dioxide and triethoxycaprylylsiloxane treated titanium dioxide.

[0044] Tested by a third-party testing agency: Test method: Weigh 20 mg of titanium dioxide powder and test the total free radical content. The instrument is a paramagnetic resonance spectrometer, the instrument model is Bruker A300, the parameters are shown in Figure 2 .

[0045] Testing organization: Fuda Testing Technology Group Co., Ltd.

[0046] Test sample: 1. Untreated titanium dioxide; 2. Triethoxycaprylylsiloxane treated titanium dioxide (Example 1); 3. Triethoxycaprylylsiloxane treated titanium dioxide (Example 2); 4. Triethoxycaprylylsiloxane treated titanium dioxide (Example 3); 5. Triethoxycaprylylsiloxane treated titanium dioxide (Comparative Example 1); 6. Triethoxycaprylylsiloxane treated titanium dioxide (Comparative Example 2); 7. Triethoxycaprylylsiloxane + polymethylsilsesquioxane treated titanium dioxide (Example 4); 8. Triethoxycaprylylsiloxane + polymethylsilsesquioxane treated titanium dioxide (Example 5); 9. Triethoxycaprylylsiloxane + polymethylsilsesquioxane treated titanium dioxide (Example 6); 10. Triethoxycaprylylsiloxane + polymethylsilsesquioxane treated titanium dioxide (Example 7); 11. Titanium dioxide treated with triethoxycaprylylsiloxane + polymethylsilsesquioxane (Comparative Example 3); 12. Titanium dioxide treated with triethoxycaprylylsiloxane + polymethylsilsesquioxane (Comparative Example 4); The test results are shown in Table 1.

[0047] Table 1 Titanium dioxide free radical test results

[0048] It can be concluded from Table 1 that the total free radical release content of titanium dioxide treated with triethoxycaprylylsiloxane + polymethylsilsesquioxane is less than that of untreated titanium dioxide and triethoxycaprylylsiloxane treated titanium dioxide, and the amount of triethoxycaprylylsiloxane and polymethylsilsesquioxane used also has a significant difference in the total free radical release content.

[0049] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. People can also obtain other embodiments based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A composition for reducing free radicals on the surface of titanium dioxide powder, characterized in that: Includes polymethylsilsesquioxane and triethoxycaprylylsilane; The mass ratio of the polymethylsilsesquioxane to triethoxyoctylsilane is 1-4:1-3; The molecular formula of the polymethylsilsesquioxane is (CH3-SiO 3 / 2 )x, x is 315.

78.

2. A method for reducing free radicals on the surface of titanium dioxide powder using the composition of claim 1, characterized in that: The following steps are involved: 1) mixing the triethoxyoctylsilane with a dispersant to obtain a triethoxyoctylsilane solution; 2) spraying the triethoxyoctylsilane solution obtained in step 1) on the surface of titanium dioxide powder, and drying to obtain silane-treated powder; The mass ratio of the titanium dioxide powder to triethoxyoctylsilane is 97-99:1-3; 3) mixing the polymethylsilsesquioxane with a dispersion to obtain a polymethylsilsesquioxane solution; The mass ratio of the titanium dioxide powder to the polymethylsilsesquioxane is 96-99:1-4; 4) mixing the silane-treated powder obtained in step 2) and the polymethylsilsesquioxane solution obtained in step 3), and allowing the mixture to stand to obtain a standing product; 5) The solid-liquid separation of the static product obtained in step 4) is carried out, and the obtained solid is dried to obtain treated titanium dioxide powder.

3. The method according to claim 2, characterized in that In the step 1), the mass ratio of triethoxycaprylylsiloxane to the dispersant is 1:1; The dispersant includes one or more of acetone, isododecane, cyclopentasiloxane and ethanol; The mixing conditions include: mixing at a rotation speed of 200 rpm for 30 minutes.

4. The method according to claim 2, characterized in that: In the step 2), the triethoxyoctylsilane solution is sprayed on the surface of the titanium dioxide powder 3 to 4 times, and after each spraying, the mixture is mixed at a speed of 2000 rpm for 5 to 10 minutes; The drying conditions include: temperature of 80° C. and time of 3 hours.

5. The method according to claim 2, characterized in that: In step 3), the mass ratio of polymethylsilsesquioxane to the dispersion is 1:1; The dispersion liquid comprises one or more of acetone, isododecane, cyclopentasiloxane and ethanol; The mixing conditions include: mixing at a rotation speed of 200 rpm for 30 minutes.

6. The method according to claim 2, characterized in that In step 4), the mass ratio of the silane-treated powder solution to the polymethylsilsesquioxane solution is 1:1-2; The standing time is 12 hours.

7. The method according to claim 2, characterized in that The drying conditions in step 5) include: a temperature of 100° C. and a drying time of 5 hours.

8. Use of the treated titanium dioxide powder obtained by the method according to any one of claims 2 to 7 in reducing free radicals in base makeup products.

9. Use of the composition according to claim 1 in reducing free radicals on the surface of titanium dioxide powder.

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