CN116199885A - Reactive organopolysiloxane, process for producing the same, modified powder, and base cosmetic containing the modified powder - Google Patents

Abstract

The invention discloses reactive organopolysiloxane, a preparation method thereof, modified powder and base makeup containing the modified powder. The reactive organopolysiloxane has a structure shown in formula I; the preparation method of the reactive organopolysiloxane comprises the following steps: mixing unsaturated silane, unsaturated fatty acid ester, optionally monovinyl polysiloxane and hydrogenated polydialkylsiloxane, and reacting in the presence of a catalyst to obtain the reactive organopolysiloxane; the modified powder comprises a powder and a treating agent attached to the powder, wherein the treating agent comprises the reactive organopolysiloxane and/or a partial (hydrolytic) condensate thereof; the base cosmetic comprises the modified powder and the water-in-silicone oil emulsion. The reactive organopolysiloxane provided by the invention can be used as a powder treatment agent, and the modified powder provided by the invention has excellent dispersibility, lipophilicity and lipophilicity, and the color uniformity of a base makeup containing the modified powder is good and the color difference before and after application is small.

Description

Reactive organopolysiloxane, process for producing the same, modified powder, and base cosmetic containing the modified powder

Technical Field

The invention belongs to the technical field of daily chemicals, and particularly relates to reactive organopolysiloxane, a preparation method thereof, modified powder and base makeup containing the modified powder.

Background

The powder used in the make-up base is mainly metal oxide powder for improving skin color and porous microsphere powder for providing oil control effect. In order to improve the dispersion effect of these powders in the base makeup, the modification is generally carried out with a surface treatment agent. The treating agent is covered on the surface of the powder to be treated, so that the powder can be endowed with the characteristics of hydrophobicity, easy dispersion, different skin feel and the like. The treating agents used for modifying these powders mainly include fatty acids, fatty alcohols, silane coupling agents, and some small-molecule surfactants, etc., while the powders used in water-in-silicone type make-up bases are generally modified with hydrophobic silane coupling agents, such as octyltriethoxysilane, decyltriethoxysilane, etc. Although these small molecule treatments are excellent in improving the lipophilicity of powder, they are slightly inferior in dispersion effect and skin feel performance and poor in silicone oil affinity, and the base cosmetic products obtained by using these small molecule treatments as powder modifier, especially the base cosmetic products of silicone oil type, generally have the problems of poor color uniformity, large color change before and after application, relatively low long-term storage stability of the products, especially the problems of color bands of the products and color change before and after application, and are all the time pain points of the base cosmetic products.

At present, there are many reports about powder treatments.

For example, CN114224747a discloses a modified powder and a preparation method thereof, and a cosmetic comprising the modified powder, the preparation method of the modified powder comprises the following steps: mixing the basic powder with a solution containing a film forming agent to obtain a mixture, and drying the mixture to obtain modified powder; when the modified powder is used in cosmetics, the modified powder has excellent compatibility with other components and can be uniformly dispersed in the cosmetics.

CN115105430a discloses a powder surface composite treating agent and its surface modified powder and application, the powder surface composite treating agent includes coupling agent, organosilicon elastomer and film forming agent, the powder surface composite treating agent is used for treating modified basic powder, the obtained surface modified powder has better and stable performance, and the cosmetic has good grease compatibility and stability, good skin adhesion and good skin feel when applied in cosmetics.

Although the powder treatment agent disclosed in the above patent has improved dispersibility and skin feel of the obtained modified powder as compared with the small molecule treatment agent, it has not been able to solve the problems of poor color uniformity of the base makeup product, large color change before and after application, relatively low long-term storage stability of the product, and the like.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide reactive organopolysiloxane, a preparation method thereof, modified powder and base makeup containing the modified powder. The reactive organopolysiloxane has active groups, can be connected to the surface of powder through chemical bonds, introduces a fatty acid ester chain segment and a long siloxane chain segment into a side chain, can be used as a powder treating agent, especially as a powder treating agent for cosmetics, has excellent dispersibility, lipophilicity and lipophilicity, and has fine and smooth color uniformity, small color difference before and after application and excellent skin feel.

To achieve the purpose, the invention adopts the following technical scheme:

in a first aspect, the present invention provides a reactive organopolysiloxane having the structure of formula I:

wherein a is an integer of 1-100, b is an integer of 0-100, c is an integer of 1-100, and d is an integer of 0-100; e is an integer from 1 to 100; n is an integer of 0 to 2; each X represents a divalent organic group; each R ¹ 、R ² 、R ³ 、R ⁴ 、R ⁵ 、R ⁶ Independently selected from any one of 1-30 carbon atom substituted or unsubstituted, and straight or branched alkyl groups, 6-30 carbon atom substituted or unsubstituted aryl or aralkyl groups, 1-30 carbon atom substituted or unsubstituted alkyl groups; q independently of one another represents a hydroxyl group or a hydrolyzable group.

Preferably, each R ¹ 、R ³ Each independently selected from the group consisting of substituted or unsubstituted carbon atoms of 1 to 30,And a linear or branched alkyl group, or an aryl group or an aralkyl group having 6 to 30 carbon atoms.

Preferably, each R ² 、R ⁴ Each independently selected from the group consisting of substituted or unsubstituted, and straight or branched alkyl groups of 1 to 18 carbon atoms.

Preferably, each R ⁵ Independently selected from the group consisting of substituted or unsubstituted, and straight or branched alkyl groups of 1 to 20 carbon atoms.

Preferably, each R ⁶ Independently of one another, from alkyl groups of 1 to 4 carbon atoms.

Preferably, each X is independently selected from divalent substituted or unsubstituted hydrocarbon groups having 1 to 20 carbon atoms.

Preferably, Q independently of each other represent hydroxy or alkoxy.

Preferably, n is 0.

Preferably, the preparation raw materials of the reactive organopolysiloxane include: hydrogenated polydialkylsiloxanes, unsaturated silanes, unsaturated fatty acid esters, optionally monovinylpolysiloxanes, and catalysts.

Preferably, the weight average molecular weight of the reactive organopolysiloxane is 1000 to 35000, further preferably, the weight average molecular weight of the reactive organopolysiloxane is 3000 to 20000.

Preferably, the unsaturated fatty acid ester is a monounsaturated fatty acid ester.

Preferably, the unsaturated fatty acid ester is one or more of methyl oleate, ethyl oleate, propyl oleate, butyl oleate, 2-octyl dodecyl oleate, methyl 10-undecylenate, ethyl 10-undecylenate, methyl palmitoleate, ethyl palmitoleate, methyl eicosenoate, ethyl eicosenoate, methyl erucate and ethyl erucate.

Preferably, the unsaturated silane is one or more of vinyl trimethoxysilane, vinyl triethoxysilane, vinyl-tris (2-methoxyethoxy) silane, methacryloxypropyl trimethoxysilane, allyl triethoxysilane, 7-octenyl trimethoxysilane, and 3- (methacryloxy) propyl trimethoxysilane.

Preferably, the monovinyl polysiloxane has a number average molecular weight of 500 to 2000.

In a second aspect, the present invention provides a method for preparing the reactive organopolysiloxane described above, the method comprising the steps of:

The reactive organopolysiloxane is obtained by mixing an unsaturated silane, an unsaturated fatty acid ester, optionally a monovinyl polysiloxane, and a hydrogenated polydialkylsiloxane, and reacting them in the presence of a catalyst.

Preferably, the molar ratio between the unsaturated silane and the unsaturated fatty acid ester is (1 to 8.5): (1.5-9.5); for example, 1 to 8.5 may be 1, 2, 3, 4, 5, 6, 7, 8.5;1.5 to 9.5 may be 1.5, 2, 3, 4, 5, 6, 7, 8, 9.5, etc.

Preferably, the molar ratio between the unsaturated silane and the unsaturated fatty acid ester is (2-6.5): (3-7.5).

Preferably, the molar ratio between the unsaturated silane and the monovinyl polysiloxane is (1 to 8.5): (0-2); for example, 1 to 8.5 may be 1, 2, 3, 4, 5, 6, 7, 8.5;0 to 2 may be 0, 0.5, 1, 1.5, 2, etc.

Preferably, the molar ratio between the unsaturated silane and the monovinyl polysiloxane is (2 to 6.5): (0.1-1.5).

Preferably, the catalyst is a platinum-based catalyst.

Preferably, the temperature of the reaction is 60-120 ℃.

In a third aspect, the present invention provides the use of a reactive organopolysiloxane as described above in the field of powder treatment.

In a fourth aspect, the present invention provides a modified powder comprising a powder and a treating agent attached to the powder, the treating agent comprising a reactive organopolysiloxane and/or a partial (hydrolytic) condensate thereof as described above.

Preferably, the powder comprises an inorganic powder and/or an organic powder.

In the present invention, the inorganic powder is exemplified by one or more selected from the group consisting of synthetic mica, sericite, iron oxide (such as iron oxide), titanium oxide, zinc oxide, zirconium oxide, magnesium oxide, aluminum oxide, chromium oxide, iron ferrocyanide, chrome green, manganese violet, kaolin, talc, calcium sulfate, magnesium sulfate, barium sulfate, boron nitride, silica, pearlescent pigment, metallic pigment, glass, ultramarine blue; the organic powder is one or more selected from organic lake, high molecular polymer, wax powder, surfactant, and metal soap (such as zinc stearate, aluminum stearate, calcium stearate, magnesium stearate, zinc myristate, and magnesium myristate).

Preferably, the weight ratio between the reactive organopolysiloxane and the powder is (1 to 50): 100.

further preferably, the weight ratio between the reactive organopolysiloxane and the powder is (1 to 10): 100; for example, 1:100;2:100;3:100;4:100;5:100;6:100;7:100;8:100;9:100;10:100, etc.

In a fifth aspect, the present invention provides a method for preparing the modified powder, which comprises the following steps:

adding the reactive organopolysiloxane and optionally a first solvent into the powder, uniformly mixing, and drying to obtain modified powder;

preferably, the mixing means is one or more of mechanical stirring, homogenizing, grinding, and centrifugal mixing.

Preferably, the first solvent is at least one selected from water, alkanols, esters, ethers, olefins, and siloxanes solvents; more preferably, the solvent is selected from one or more of water, ethanol, isopropanol, isododecane, cyclopentadimethicone, and dimethicone having a viscosity of 0.5 to 2 CPS.

Preferably, the drying temperature is 40-200 ℃, and the drying time is 0.5-8 h.

Further preferably, the drying temperature is 60-100 ℃ and the drying time is 1-4 h.

In a sixth aspect, the present invention provides a make-up base comprising the modified powder described above and a water-in-silicone oil emulsion.

Preferably, the mass ratio of the modified powder to the silicone oil water emulsion is (9-15): (80-83).

Wherein 9 to 15 may be 9, 10, 11, 12, 13, 14, 15, etc.; 80 to 83 may be 80, 81, 82, 83, etc.

Preferably, the preparation raw materials of the water-in-silicone oil emulsion comprise an A component and a B component, wherein the A component comprises the following components in parts by weight: 17-25 parts of moisturizing grease, 2-6 parts of organic silicon elastomer, 2-6 parts of water-in-oil emulsifier and 0.7-1.1 parts of mineral thickener; the component B comprises the following components in parts by weight: 7.5 to 15.5 parts of moisturizing component, 37 to 41 parts of water and 0.7 to 1.1 parts of electrolyte.

Preferably, the moisturizing grease comprises phenyl trimethicone and/or polydimethylsiloxane.

Preferably, the silicone elastomer comprises a polydimethylsiloxane cross-linked polymer.

Preferably, the water-in-oil emulsifier comprises PEG/PPG-20/15 polydimethylsiloxane and/or PEG-10 polydimethylsiloxane.

Preferably, the mineral thickener comprises a mixture of quaternary ammonium salt-18 bentonite and/or distearyldimethylammonium lithium montmorillonite.

Preferably, the moisturizing component comprises glycerin and/or propylene glycol.

Preferably, the electrolyte is sodium chloride and/or potassium chloride.

Preferably, the preservative is one or more of phenoxyethanol, benzoic acid, sodium benzoate, dehydroacetic acid, sodium dehydroacetate, sorbic acid and salts thereof, octanol, octanoyl hydroxamic acid.

In a seventh aspect, the present invention provides a method for preparing the base makeup, which includes the following steps:

s1, mixing the modified powder, a second solvent and a surfactant, and grinding the mixture into modified powder slurry;

s2, uniformly mixing the modified powder slurry and the water-in-silicone oil emulsion, and filling the mixture into a container to obtain the base makeup.

Preferably, the second solvent is at least one selected from water, alkanols, esters, ethers, olefins, and siloxanes solvents; more preferably, the solvent is selected from one or more of water, ethanol, isopropanol, isododecane, cyclopentadimethicone, and dimethicone having a viscosity of 0.5 to 2 CPS;

the surfactant of the present invention is not particularly limited, and one or more of anionic surfactant, cationic surfactant and nonionic surfactant may be selected.

Compared with the prior art, the invention has the beneficial effects that:

the reactive organopolysiloxane provided by the invention has reactive groups, can be bonded on the surface of powder through chemical bonds, so that the reactive organopolysiloxane is firmly combined with the surface of the powder, and fatty acid ester chain segments and long siloxane chain segments are introduced into side chains, so that the modified powder obtained by modifying the reactive organopolysiloxane has excellent dispersibility, has very high affinity with various oil agents such as silicone oil, ester oil, hydrocarbon oil and the like, has good color uniformity of a base makeup containing the modified powder, has small color difference before and after application, and has good spreadability, fineness and excellent skin feel.

Detailed Description

The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art. In the present specification, "part" and "%" respectively mean "part by mass" and "% by mass" unless otherwise specified.

The method for measuring the active hydrogen comprises the following steps:

accurately weighing 0.1g (accurate to 0.0001 g) of the product in a 250mL iodometric bottle, fully dissolving the object to be measured in 10mL carbon tetrachloride, and then adding 5mL of Br with the concentration of 10% ₂ -CH ₃ The COOH solution is vibrated to be uniformly mixed, and is placed in a dark place to react for half an hour, and then is added10mL of 10% potassium iodide solution. Starting with a calibrated concentration of Na ₂ S ₂ O ₃ And (3) titrating the standard solution, adding 2-4 drops of 10g/L starch indicator solution near the end point, immediately stopping titration when the blue color of the solution system disappears, and simultaneously performing a blank control experiment.

The active hydrogen content was calculated using the following calculation formula: c (C) _H ％＝[(V ₀ -V ₁ )×C _Na2S2O3 ×0.5/(m×1000)]×100％

In the above, C _H For the content of active hydrogen in the product, m is the product mass, C is Na ₂ S ₂ O ₃ Concentration of standard solution (mol.L) ^-1 )，V ₀ Na consumed for blank experiment reaction ₂ S ₂ O ₃ Volume (mL), V ₁ Na consumed for the product experimental reaction ₂ S ₂ O ₃ Volume (mL).

Synthesis example 1

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

s2, uniformly mixing methyl oleate, triethoxyallylsilane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight of 1250), isopropyl alcohol accounting for 20% of the total mass of the raw materials and hydroquinone accounting for 0.1% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

s3, putting the hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle, carrying out heat preservation reaction for 5 hours at 90 ℃ after the dropwise adding is finished, stopping the reaction after detecting the content of silicon hydrogen to be less than 10ppm, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A1).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between methyl oleate, triethoxyallylsilane and mono-blocked alkenyl silicone oil was 3.5:6:0.5.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the methyl oleate, the triethoxy allyl silane, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example are subjected to hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 9288.

Synthesis example 2

S1, 39.4g of high-hydrogen silicone oil (202, the hydrogen content is 1.58%), 258.5g of octamethyl cyclotetrasiloxane and 2.05g of hexamethyldisiloxane are put into a reaction kettle, 4g of concentrated sulfuric acid is slowly added, the temperature is raised to 60 ℃ for heat preservation and reaction for 6 hours, then sodium bicarbonate is slowly added for neutralization after the temperature is raised to 40 ℃, and the mixture is filtered, heated to 140 ℃ for removing micromolecular substances, cooled and cooled to obtain hydrogenated polydialkylsiloxane (the hydrogen content is 0.16%);

s2, uniformly mixing methyl palmitoleate, vinyl trimethoxy silane, single-end capped alkenyl silicone oil (Silok 3821F21, molecular weight of 500), isopropyl alcohol accounting for 30% of the total mass of the raw materials and hydroquinone accounting for 0.2% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

S3, putting the hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser according to a metering ratio, starting stirring, introducing nitrogen, heating to 95 ℃, dropwise adding 10ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle, carrying out heat preservation reaction for 5 hours at the temperature of 95 ℃ after the dropwise adding is finished, stopping the reaction after detecting the content of silicon hydrogen to be less than 10ppm, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A2).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) = 1.1.15; the molar ratio of methyl palmitoleate to vinyltrimethoxysilane to the mono-blocked alkenyl silicone oil was 5:4:1.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the methyl palmitoleate, the vinyl trimethoxy silane, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example are subjected to hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 18118.5.

Synthesis example 3

S1, adding 41g of high-hydrogen silicone oil (202, the hydrogen content is 1.58%), 240g of octamethyl cyclotetrasiloxane and 3.7g of hexamethyldisiloxane into a reaction kettle, slowly adding 4 parts of concentrated sulfuric acid, heating to 60 ℃, keeping the temperature for reaction for 6 hours, cooling to 40 ℃, slowly adding sodium bicarbonate for neutralization, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane (the hydrogen content is 0.21%);

s2, uniformly mixing propyl oleate, vinyl triethoxysilane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight 1250), isopropyl alcohol accounting for 30% of the total mass of the raw materials and hydroquinone accounting for 0.2% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

s3, putting the hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser according to a metering ratio, starting stirring, introducing nitrogen, heating to 85 ℃, dropwise adding 10ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle, carrying out heat preservation reaction for 6 hours at 85 ℃ after the dropwise adding is finished, stopping the reaction after detecting the content of silicon hydrogen to be less than 10ppm, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A3).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.3; the molar ratio between the propyl oleate, the vinyl triethoxysilane and the single-end capped alkenyl silicone oil is 6.5:3:0.5.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the propyl oleate, the vinyl triethoxysilane, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example are subjected to hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 3827.

Synthesis example 4

S1, adding 37.5g of high-hydrogen silicone oil (202, the hydrogen content is 1.58%), 250.7g of octamethyl cyclotetrasiloxane and 11.8g of hexamethyldisiloxane into a reaction kettle, slowly adding 4g of concentrated sulfuric acid, heating to 60 ℃, keeping the temperature for reaction for 6 hours, cooling to 40 ℃, slowly adding sodium bicarbonate for neutralization, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane (the hydrogen content is 0.20%);

s2, uniformly mixing ethyl oleate, allyl trimethoxysilane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight 1250), isopropyl alcohol accounting for 30% of the total mass of the raw materials and hydroquinone accounting for 0.2% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

S3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 95 ℃, dropwise adding 10ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture liquid into the reaction kettle, after dropwise adding the raw material mixture liquid into the reaction kettle for 1.5h, carrying out heat preservation reaction for 4h at 100 ℃, after detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and carrying out reduced pressure distillation to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A4).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.1; the mol ratio of the ethyl oleate to the allyl trimethoxysilane to the single-end capped alkenyl silicone oil is 2:7.5:0.5;

the product obtained by the synthesis example is tested by adopting a Fourier transform infrared spectrometerThe result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the ethyl oleate, the allyl trimethoxy silane, the single end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example are subjected to hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 5343.

Synthesis example 5

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

s2, uniformly mixing methyl oleate, triethoxyallylsilane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight is 1250), isopropyl alcohol accounting for 20% of the total mass of the raw materials and hydroquinone accounting for 0.1% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

s3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle for 1.5h, carrying out heat preservation reaction for 5h at 90 ℃, detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A5).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between methyl oleate, triethoxyallylsilane and mono-blocked alkenyl silicone oil was 1:9.5:0.5.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the Si-H bond is basically disappeared, which proves that in the synthesis exampleThe methyl oleate, triethoxyallyl silane, single-end capped alkenyl silicone oil and hydrogenated polydialkylsiloxane undergo hydrosilylation reaction to obtain the reactive organopolysiloxane shown in the formula (I).

Weight average molecular weight (M) by GPC _w ) 9134.

Synthesis example 6

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

s2, uniformly mixing methyl oleate, triethoxyallylsilane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight is 1250), isopropyl alcohol accounting for 20% of the total mass of the raw materials and hydroquinone accounting for 0.1% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

S3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle for 1.5h, carrying out heat preservation reaction for 5h at 90 ℃, detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A6).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between methyl oleate, triethoxyallylsilane and mono-blocked alkenyl silicone oil was 8.5:1.5:0.5.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the methyl oleate, the triethoxy allyl silane, the single end-capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example generate silicon-hydrogen addition is provedThe reaction is carried out to obtain the reactive organopolysiloxane shown in the formula (I).

Weight average molecular weight (M) by GPC _w ) 9841.

Synthesis example 7

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

s2, uniformly mixing methyl oleate, triethoxyallylsilane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight is 1250), isopropyl alcohol accounting for 20% of the total mass of the raw materials and hydroquinone accounting for 0.1% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

s3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle for 1.5h, carrying out heat preservation reaction for 5h at 90 ℃, detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A7).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between methyl oleate, triethoxyallylsilane and mono-blocked alkenyl silicone oil is 3:5:2.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the methyl oleate, the triethoxy allyl silane, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example are subjected to hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average by GPC testMolecular weight (M) _w ) 6708.

Synthesis example 8

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

s2, uniformly mixing methyl oleate, triethoxyallylsilane, isopropanol accounting for 20% of the total mass of the raw materials and hydroquinone accounting for 0.1% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

S3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle for 1.5h, carrying out heat preservation reaction for 5h at 90 ℃, detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A8).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between methyl oleate and triethoxyallylsilane was 4:6.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the methyl oleate, the triethoxy allyl silane, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example are subjected to hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 8594.

Synthesis of comparative example 1

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

S2, uniformly mixing methyl oleate, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight 1250, of Guangzhou, and the like), isopropyl alcohol accounting for 20% of the total mass of the raw materials and hydroquinone accounting for 0.1% of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

s3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle for 1.5h, carrying out heat preservation reaction for 5h at 90 ℃, detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A9).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between methyl oleate and the mono-blocked alkenyl silicone oil was 3.5:0.5.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the methyl oleate, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example generate hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 10687.

Synthesis of comparative example 2

S1, adding 256.3g of octamethyl cyclotetrasiloxane, 37.5g of high hydrogen silicone oil (202, hydrogen content is 1.58%) and 6.1g of hexamethyldisiloxane and 4g of concentrated sulfuric acid into a reaction kettle, heating to 55 ℃, carrying out heat preservation reaction for 6 hours, adding a sodium carbonate neutralizer, filtering, heating to 140 ℃ to remove micromolecule substances, and cooling to obtain hydrogenated polydialkylsiloxane, wherein the hydrogen content of the hydrogenated polydialkylsiloxane is 0.20%;

s2, uniformly mixing triethoxy allyl silane, single-end capped alkenyl silicone oil (Silok 3821F8, molecular weight of 1250, guangzhou, and the like), isopropyl alcohol accounting for 20 percent of the total mass of the raw materials, and hydroquinone accounting for 0.1 percent of the total mass of the raw materials according to a metering ratio to obtain a raw material mixed solution;

s3, putting hydrogenated polydialkylsiloxane into a reaction kettle provided with a stirrer, a thermometer and a condenser tube according to a metering ratio, starting stirring, introducing nitrogen, heating to 90 ℃, dropwise adding 20ppm of a Karster catalyst into the reaction kettle, dropwise adding a raw material mixture into the reaction kettle, dropwise adding the raw material mixture into the reaction kettle for 1.5h, carrying out heat preservation reaction for 5h at 90 ℃, detecting that the content of silicon hydrogen is less than 10ppm, stopping the reaction, and distilling under reduced pressure to remove low-boiling substances to obtain reactive organopolysiloxane (marked as A10).

Wherein, n (Si-H) in the reaction raw materials: n (c=c) =1.1.2; the molar ratio between triethoxyallylsilane and mono-blocked alkenylsilicone oil was 6:0.5.

The product obtained in this synthesis example was tested by using a Fourier transform infrared spectrometer, and the test result shows that the wavelength is 2150cm ^-1 Near, the infrared characteristic peak of the silicon-hydrogen bond is basically disappeared, and the fact that the triethoxyallylsilane, the single-end capped alkenyl silicone oil and the hydrogenated polydialkylsiloxane in the synthesis example generate hydrosilylation reaction proves that the reactive organopolysiloxane shown in the formula (I) is obtained.

Weight average molecular weight (M) by GPC _w ) 9155.

2. A preparation method of modified powder.

Examples 1 to 10 and comparative examples 1 to 3 below are methods for producing modified powders.

The raw material model and manufacturer information are as follows:

iron red powder: shanghai ShengKun chemical Co., ltd;

iron oxide yellow powder: shanghai ShengKun chemical Co., ltd;

iron black powder: shanghai ShengKun chemical Co., ltd;

silicone oil: hunan Sirocco hasSilicone Co Ltd

201-1.5, having a viscosity of 1.5cps;

porous silica powder: jin Sanjiang (culprit) silicon materials stock limited,

319。

example 1

Mixing 100g of iron oxide red, 3g of reactive organopolysiloxane (A1) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 100 ℃ for 2 hours to obtain modified iron oxide red;

Replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Example 2

This example differs from example 1 in that the reactive organopolysiloxane (A1) is replaced with a reactive organopolysiloxane (A2). Modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium white powder and modified porous silica powder were each produced in the same manner as in example 1.

Example 3

This example differs from example 1 in that the reactive organopolysiloxane (A1) is replaced with a reactive organopolysiloxane (A3). Modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium white powder and modified porous silica powder were each produced in the same manner as in example 1.

Example 4

This example differs from example 1 in that the reactive organopolysiloxane (A1) is replaced with a reactive organopolysiloxane (A4). Modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium white powder and modified porous silica powder were each produced in the same manner as in example 1.

Example 5

This example is different from example 1 in that the reactive organopolysiloxane (A1) was replaced with the reactive organopolysiloxane (A5), and modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium oxide powder, and modified porous silica powder were each produced in the same manner as in example 1.

Example 6

This example differs from example 1 in that the reactive organopolysiloxane (A1) is replaced with a reactive organopolysiloxane (A6). Modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium white powder and modified porous silica powder were each produced in the same manner as in example 1.

Example 7

This example differs from example 1 in that the reactive organopolysiloxane (A1) is replaced with a reactive organopolysiloxane (A7). Modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium white powder and modified porous silica powder were each produced in the same manner as in example 1.

Example 8

Mixing 100g of iron oxide red, 5g of reactive organopolysiloxane (A1) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 60 ℃ for reaction for 4 hours to obtain modified iron oxide red;

replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

Replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Example 9

Mixing 100g of iron oxide red, 1g of reactive organopolysiloxane (A1) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 100 ℃ for 2 hours to obtain modified iron oxide red;

replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Example 10

Mixing 100g of iron oxide red, 3g of reactive organopolysiloxane (A1) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 40 ℃ for reaction for 8 hours to obtain modified iron oxide red;

replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

Replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Example 11

Mixing 100g of iron oxide red, 3g of reactive organopolysiloxane (A8) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 100 ℃ for 2 hours to obtain modified iron oxide red;

replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Comparative example 1

Mixing 100g of iron oxide red, 3g of reactive organopolysiloxane (A9) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 100 ℃ for 2 hours to obtain modified iron oxide red;

replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

Replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Comparative example 2

Mixing 100g of iron oxide red, 3g of reactive organopolysiloxane (A10) and 5g of silicone oil (viscosity of 1.5 cps), and baking at 100 ℃ for 2 hours to obtain modified iron oxide red;

replacing the iron oxide red powder with iron oxide yellow powder, and preparing modified iron oxide yellow powder by the same method;

replacing the iron oxide red powder with iron oxide black powder, and preparing modified iron oxide black powder by the same method;

replacing the iron oxide red powder with titanium dioxide, and preparing a modified titanium dioxide body by the same method;

the iron oxide red powder is replaced by porous silica powder, and the modified porous silica powder is prepared by the same method.

Comparative example 3

The present embodiment differs from example 1 in that: the iron oxide red powder, the iron oxide yellow powder, the iron oxide black powder, the titanium pigment and the porous silica powder are not modified.

Comparative example 4

The present embodiment differs from example 1 in that: the reactive organopolysiloxane (A1) is replaced by octyl triethoxysilane, and modified iron oxide red powder, modified iron oxide yellow powder, modified iron oxide black powder, modified titanium pigment and modified porous silica powder are respectively prepared by the same method.

3. A preparation method of base cosmetic is provided.

The following application example 1-application example 11 and application comparative example 1-application comparative example 4 are preparation methods of base cosmetics.

The composition and the weight thereof are shown in Table 1, and application example 1 to application example 11 and application comparative example 1 to application comparative example 4 were prepared by the same preparation method except that the composition of the modified color paste used in the A phase was different, and the composition and the addition amount of the B phase and the C phase were the same.

(1) And (3) preparing phase A color paste:

s1, respectively weighing 65g of the modified iron oxide red powder prepared in the above examples 1-11 and comparative examples 1-4, respectively mechanically stirring and mixing with 2g of PEG-10 polydimethylsiloxane (SiCare 2215) and 33g of silicone oil (viscosity of 1.5 cps), and grinding for three times in a three-roller grinder to obtain the corresponding modified iron oxide red color paste. The modified iron oxide red pastes obtained in examples 1-11 and comparative examples 1-4 were sequentially designated as B1-1, B1-2, B1-3, B1-4, B1-5, B1-6, B1-7, B1-8, B1-9, B1-10, B1-11, B1-12, B1-13, B1-14, and B1-15.

S2, respectively weighing 65g of the modified iron oxide yellow powder prepared in the examples 1-11 and the comparative examples 1-4, respectively mechanically stirring and mixing with 2g of PEG-10 polydimethylsiloxane (Hunan Sirocco, siCare 2215) and 33g of silicone oil (viscosity of 1.5 cps), and grinding for three times in a three-roller grinder to obtain corresponding modified iron oxide yellow paste respectively. The modified iron oxide yellow pastes obtained in examples 1 to 10 and comparative examples 1 to 5 were sequentially designated as B2-1, B2-2, B2-3, B2-4, B2-5, B2-6, B2-7, B2-8, B2-9, B2-10, B2-11, B2-12, B2-13, B2-14, and B2-15.

S3, respectively weighing 50g of the modified iron black powder prepared in the examples 1-11 and the comparative examples 1-4, respectively mechanically stirring and mixing with 2g of PEG-10 polydimethylsiloxane (Hunan Sirocco, siCare 2215) and 48g of silicone oil (viscosity of 1.5 cps), and grinding for three times in a three-roller grinder to obtain corresponding modified iron black paste respectively. The modified iron black pastes obtained in examples 1 to 10 and comparative examples 1 to 5 were sequentially designated as B3-1, B3-2, B3-3, B3-4, B3-5, B3-6, B3-7, B3-8, B3-9, B3-10, B3-11, B3-12, B3-13, B3-14, and B3-15.

S4, respectively weighing 80g of the modified titanium dioxide bodies prepared in the examples 1-11 and the comparative examples 1-4, respectively carrying out mechanical stirring and mixing with 2g of PEG-10 polydimethylsiloxane (SiCARE 2215) and 18g of silicone oil (with the viscosity of 1.5 cps), and then placing the mixture in a three-roller grinding machine for three times to respectively obtain the corresponding modified titanium dioxide paste. The modified titanium white pastes obtained in examples 1 to 10 and comparative examples 1 to 5 were sequentially designated as B4-1, B4-2, B4-3, B4-4, B4-5, B4-6, B4-7, B4-8, B4-9, B4-10, B4-11, B4-12, B4-13, B4-14, and B4-15.

S5, the modified porous silica prepared in the above examples 1-11 and comparative examples 1-4 is weighed for standby, and sequentially marked as B5-1, B5-2, B5-3, B5-4, B5-5, B5-6, B5-7, B5-8, B5-9, B5-10, B5-11, B5-12, B5-13, B5-14 and B5-15.

(2) Preparing a base finished product:

s1, weighing each component of the B phase and each component of the C phase according to a feeding ratio, respectively mechanically stirring and mixing, slowly adding the composition of the C phase into the composition of the B phase under homogenization, and continuously homogenizing for 15min after the addition is finished to obtain a mixed phase;

s2, weighing the components of the phase A in proportion, adding the components into the mixed phase obtained in the step S1, continuously stirring for 15min at 500 rpm after the components are added, cooling to room temperature, and filling to obtain the base makeup.

TABLE 1

/>

The performances of the base makeup were evaluated, and the evaluation results are shown in table 2. The specific evaluation method is as follows:

dispersibility: grading the appearance of the base makeup according to the uniformity of the color and the size of the internal and external chromatic aberration, wherein the grade 1 is uniform in color, free of color bands and free of obvious internal and external chromatic aberration; the level 2 is slightly uneven in color, slightly has internal and external chromatic aberration, slightly observes color bands, but does not affect the use; grade 3 is color unevenness, color bands are observed; the level 4 is that the color is obviously uneven and color bands are obviously observed; the grade 5 is a visible color band and cannot be used as a base makeup.

Color change before and after application: the colors before and after the base make-up are compared, the color is divided into 1-5 grades according to the change degree of the colors before and after the base make-up is coated, wherein the 1 grade is small in color difference before and after the base make-up is coated, the 2 grade is slightly chromatic difference, and the 3 grade is capable of showing chromatic difference; the level 4 is obvious in chromatic aberration; the grade 5 is a color difference with larger value.

Stability: the above base cosmetics were subjected to a freeze thawing (-15 ℃) and heat stability (48 ℃) cross-cycle test for 15 days and were classified into 1 to 5 grades according to the following evaluation criteria:

stage 1: no demulsification, oil drift and layering phenomena exist, and the viscosity is not obviously changed;

2 stages: the emulsion breaking and oil drifting phenomena are slight, and the viscosity is slightly changed;

3 stages: the emulsion breaking and oil drifting phenomena and the viscosity changes;

4 stages: obvious demulsification and oil drift phenomena are caused, and the viscosity change is large;

5 stages: has very obvious demulsification and oil drift phenomena and obvious layering.

Evaluation of feel in use: the sensory evaluation was performed using a scoring test method, the full scale of each sensory index was classified into 5 grades, and the sensory evaluation panel included 10 panel members, and the spreadability and uniformity and fineness were evaluated according to the following scoring criteria:

stage 1: the method is very good; 2 stages: the method is good; 3 stages: medium; 4 stages: slightly worse; 5 stages: and (3) difference.

TABLE 2

As can be seen from Table 2, the base cosmetics obtained in the present invention application examples 1 to 4 and 8 were uniform in color, excellent in dispersibility and spreadability, small in color difference before and after application, uniform and fine in application, good in spreadability, and excellent in storage stability.

As is clear from the comparison between application example 9 and application example 1, when the addition amount of the reactive organopolysiloxane is too low, the content of the reactive organopolysiloxane contained on the surface of the modified powder is too low, resulting in deterioration in the properties such as the dispersibility of the base makeup, spreadability, feel in use, and color change before and after coating film obtained from the modified powder.

As is clear from the comparison between application example 10 and application example 1, when the reaction temperature of the reactive organopolysiloxane with the powder is too low, it is difficult to completely react, and the dispersibility, spreadability, feel in use, color change before and after coating, and the like of the base makeup obtained from the modified powder are degraded.

As is clear from comparison of application comparative example 1 to application comparative example 3 with application example 1, when the reactive organopolysiloxane is not the structure provided by the present invention, the resulting modified powder and the base makeup containing the modified powder are inferior in dispersibility, spreadability, feel in use, color change before and after coating, and the like.

As is clear from comparison of application comparative example 4 with application example 1, when the powder is modified without adding the reactive organopolysiloxane, the properties such as dispersibility, spreadability, feel in use and the like of the base makeup containing the powder do not meet the use requirements.

As is clear from the comparison between application comparative example 5 and application example 1, the use of octyltriethoxysilane as a modified powder resulted in a base coating film having inferior color change, dispersibility, spreadability, feel in use, and the like to application example 1.

In summary, the reactive organopolysiloxane provided by the invention has good reactivity and modification performance on powder, the modified powder modified by the reactive organopolysiloxane has good dispersibility, and the color change before and after the base coating film obtained by the modified powder is small, and the spreadability, the usability and the storage stability are good.

While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.

Claims (10)

1. A reactive organopolysiloxane characterized in that the reactive organopolysiloxane has a structure represented by formula I:

wherein a is an integer of 1-100, b is an integer of 0-100, c is an integer of 1-100, and d is an integer of 0-100; e is an integer from 1 to 100; n is an integer of 0 to 2;

each X represents a divalent organic group;

each R ¹ 、R ² 、R ³ 、R ⁴ 、R ⁵ 、R ⁶ Independently selected from any one of 1-30 carbon atom substituted or unsubstituted, and straight or branched alkyl groups, 6-30 carbon atom substituted or unsubstituted aryl or aralkyl groups, 1-30 carbon atom substituted or unsubstituted alkyl groups;

Q independently of one another represents a hydroxyl group or a hydrolyzable group.

2. The reactive organopolysiloxane according to claim 1, wherein each R ¹ 、R ³ Each independently selected from the group consisting of substituted or unsubstituted, and linear or unsubstituted, carbon atoms of 1 to 30Branched alkyl, or aryl or aralkyl having 6 to 30 carbon atoms;

preferably, each R ² 、R ⁴ Each independently selected from the group consisting of substituted or unsubstituted, and straight or branched alkyl groups of 1 to 18 carbon atoms;

preferably, each R ⁵ Independently selected from the group consisting of substituted or unsubstituted, and linear or branched alkyl groups of 1 to 20 carbon atoms;

preferably, each R ⁶ Independently of each other, from alkyl groups of 1 to 4 carbon atoms;

preferably, each X is independently selected from divalent substituted or unsubstituted hydrocarbon groups having 1 to 20 carbon atoms;

preferably, Q independently of each other represent hydroxy or alkoxy;

preferably, n is 0.

3. The reactive organopolysiloxane according to claim 1 or 2, characterized in that the preparation raw materials of the reactive organopolysiloxane include: hydrogenated polydialkylsiloxanes, unsaturated silanes, unsaturated fatty acid esters, optionally monovinyl polysiloxanes and catalysts;

preferably, the weight average molecular weight of the reactive organopolysiloxane is 1000-35000;

Preferably, the unsaturated fatty acid ester is a monounsaturated fatty acid ester;

preferably, the unsaturated fatty acid ester is one or more of methyl oleate, ethyl oleate, propyl oleate, butyl oleate, 2-octyl dodecyl oleate, methyl 10-undecylenate, ethyl 10-undecylenate, methyl palmitoleate, ethyl palmitoleate, methyl eicosenoate, ethyl eicosenoate, methyl erucate and ethyl erucate;

preferably, the unsaturated silane is one or more of vinyl trimethoxysilane, vinyl triethoxysilane, vinyl-tri (2-methoxyethoxy) silane, methacryloxypropyl trimethoxysilane, allyl triethoxysilane, 7-octenyl trimethoxysilane, 3- (methacryloxy) propyl trimethoxysilane, vinyl methyl diethoxysilane, allyl methyl dimethoxy silane;

preferably, the monovinyl polysiloxane has a number average molecular weight of 500 to 2000.

4. A process for the preparation of a reactive organopolysiloxane as claimed in any one of claims 1 to 3, comprising the steps of:

the reactive organopolysiloxane is obtained by mixing an unsaturated silane, an unsaturated fatty acid ester, optionally a monovinyl polysiloxane, and a hydrogenated polydialkylsiloxane, and reacting them in the presence of a catalyst.

5. The method according to claim 4, wherein the molar ratio between the unsaturated silane and the unsaturated fatty acid ester is (1 to 8.5): (1.5-9.5);

preferably, the molar ratio between the unsaturated silane and the unsaturated fatty acid ester is (2-6.5):

(3～7.5)；

preferably, the molar ratio between the unsaturated silane and the monovinyl polysiloxane is (1 to 8.5): (0-2);

preferably, the molar ratio between the unsaturated silane and the monovinyl polysiloxane is (2 to 6.5):

(0.1～1.5)；

preferably, the catalyst is a platinum-based catalyst;

preferably, the temperature of the reaction is 60-120 ℃.

6. Use of the reactive organopolysiloxanes according to any of claims 1 to 5 in the field of powder treatment.

7. A modified powder comprising a powder and a treating agent attached to the powder, the treating agent comprising the reactive organopolysiloxane according to any one of claims 1 to 5 and/or a partial (hydrolytic) condensate thereof;

preferably, the powder comprises inorganic powder and/or organic powder;

preferably, the weight ratio between the reactive organopolysiloxane and the powder is (1 to 50): 100;

further preferably, the weight ratio between the reactive organopolysiloxane and the powder is (1 to 10): 100.

8. A method of preparing the modified powder of claim 7, comprising the steps of:

adding the reactive organopolysiloxane and optionally a first solvent into the powder, uniformly mixing, and drying to obtain modified powder;

preferably, the drying temperature is 40-200 ℃ and the drying time is 0.5-8h;

further preferably, the drying temperature is 60-100 ℃ and the drying time is 1-4h.

9. A make-up base comprising the modified powder of claim 7 and a water-in-silicone oil emulsion;

preferably, the mass ratio of the modified powder to the silicone oil water emulsion is (9-15): (80-83);

preferably, the preparation raw materials of the water-in-silicone oil emulsion comprise an A component and a B component, wherein the A component comprises the following components in parts by weight: 17-25 parts of moisturizing grease, 2-6 parts of organic silicon elastomer, 2-6 parts of water-in-oil emulsifier and 0.7-1.1 parts of mineral thickener; the component B comprises the following components in parts by weight: 7.5 to 15.5 parts of moisturizing component, 37 to 41 parts of water and 0.7 to 1.1 parts of electrolyte.

10. A method of preparing a make-up base as defined in claim 9, comprising the steps of:

S1, mixing the modified powder, a second solvent and a surfactant, and grinding the mixture into modified powder slurry;

s2, uniformly mixing the modified powder slurry and the water-in-silicone oil emulsion, and filling the mixture into a container to obtain the base makeup.