阅读说明：本技术 一种有机硅凝胶组合物及其制备方法和应用 (Organic silicon gel composition and preparation method and application thereof ) 是由 王莉 沈佳 卓胜池 宋小禹 赵浩伟 于 2021-06-23 设计创作，主要内容包括：本发明公开了一种有机硅凝胶组合物及其制备方法和应用,该有机硅凝胶组合物为凝胶状,其组分包括油脂、有机硅弹性微球和活性功能颗粒；并且该有机硅凝胶组合物的制备方法包括如下步骤：制备有机硅弹性微球；采用油脂稀释溶胀有机硅弹性微球,在稀释溶胀过程中,将活性功能颗粒分散在油脂中,制成有机硅凝胶组合物；同时还公开了上述有机硅凝胶组合物在个人护理组合物中的应用。本发明的新型的有机硅凝胶组合物应用于终产品中,使得终产品中的活性功能颗粒分散性好且稳定性佳,能够充分发挥活性功能颗粒的作用。(The invention discloses an organic silicon gel composition and a preparation method and application thereof, wherein the organic silicon gel composition is in a gel shape, and comprises the components of grease, organic silicon elastic microspheres and active functional particles; and the preparation method of the silicone gel composition comprises the following steps: preparing organic silicon elastic microspheres; adopting grease to dilute and swell the organic silicon elastic microspheres, and dispersing active functional particles in the grease in the diluting and swelling process to prepare an organic silicon gel composition; also disclosed is the use of the above silicone gel composition in a personal care composition. The novel organic silicon gel composition is applied to final products, so that the active functional particles in the final products have good dispersibility and good stability, and the functions of the active functional particles can be fully exerted.)

1. The organic silicon gel composition is characterized by being in a gel shape, and the components of the organic silicon gel composition comprise grease, organic silicon elastic microspheres and active functional particles.

2. The silicone gel composition according to claim 1, wherein the active functional particles are added in an amount of 0.5 to 50% by mass of the silicone gel composition.

3. The silicone gel composition according to claim 1, wherein the silicone elastic microspheres are added in an amount of 10 to 30% by mass of the silicone gel composition.

4. The silicone gel composition of claim 1, wherein the oil is a combination of one or more selected from the group consisting of linear dimethicone, cyclic dimethicone, isododecane, isohexadecane, white oil, squalane, isononyl isononanoate, cetyl ethylhexanoate, caprylic/capric triglyceride, diisostearyl malate, tri (ethyl hexanoate) glycerol, and propylene glycol dicaprylate/caprate.

5. The silicone gel composition of claim 1, wherein the active functional particles are personal care ingredients including skin care ingredients and hair care ingredients.

6. The silicone gel composition of claim 5, wherein the skin care ingredients comprise skin feel modifiers, emollients, fragrances, ultraviolet absorbers, sunscreens, toners, herbal extracts, preservatives, light diffusers, and combinations thereof.

7. The silicone gel composition of claim 5, wherein the hair care ingredients comprise conditioners, surfactants, pearlescers, colorants, dyes, and combinations thereof.

8. A method of making the silicone gel composition of any of claims 1-7, comprising the steps of:

grease is adopted to dilute and swell the organic silicon elastic microspheres, and active functional particles are dispersed in the grease in the diluting and swelling process to prepare the organic silicon gel composition.

9. Use of the silicone gel composition of any one of claims 1-7 in a personal care composition.

10. A personal care composition comprising the silicone gel composition of any one of claims 1-7.

Technical Field

The invention particularly relates to an organic silicon gel composition and a preparation method and application thereof.

Background

The maintenance and beauty finished products on the market can be roughly divided into three categories according to the efficacy: skin care, sunscreen and cosmetics, and active functional particles are added into the components of the cosmetic, such as: emollients, inorganic sunscreens, toners, pearls, etc., however, the addition of silicone gels is a recent trend toward maintaining cosmetic products in order to increase the feel of the user when applying and the comfort of long-term use; the organic silicon gel is a gel which is formed into a film and has a smooth feeling after most siloxane chains are staggered to form macromolecules with a three-dimensional cross-linked structure and a small molecular solvent or silicone oil is swelled; when the high-viscosity silica gel is mixed with the skin care or beauty active functional particles in the manufacturing process of the actual maintenance and beauty finished products, a machine table with large shearing force and prolonged mixing time are needed to fully and uniformly mix the high-viscosity silica gel and the skin care or beauty active functional particles, and the mixed finished products are difficult to control in stability and easy to settle, so that the adding amount of the active functional particles is small, and the application range is narrow.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a novel organic silicon gel composition, which abandons the prior mode of directly adopting organic silicon gel, adopts organic silicon elastic microspheres to replace the prior organic silicon gel, can fully and uniformly mix active functional particles, the organic silicon elastic microspheres and grease by using smaller shearing force, ensures that the active functional particles in the final product have good dispersibility and good stability, and fully plays the role of the active functional particles.

The invention also discloses a preparation method of the organic silicon gel composition.

The invention also discloses an application of the silicone gel composition in a personal care composition.

In order to achieve the purpose, the invention adopts a technical scheme that:

a silicone gel composition in the form of a gel, wherein the gel is: the space network structure formed by a certain method has the structure gaps filled with liquid serving as a dispersion medium, has uniform appearance and keeps a certain form of elastic semisolid state.

The invention relates to an organic silicon gel composition which comprises grease, organic silicon elastic microspheres and active functional particles.

According to some preferred aspects of the present invention, the active functional particles are added in an amount of 0.5 to 50% by mass of the silicone gel composition. In some preferred embodiments of the present invention, the active functional particles are added in an amount of 3 to 50% by mass of the silicone gel composition. In some more preferred embodiments of the present invention, the active functional particles are added in an amount of 4.5 to 50% by mass of the silicone gel composition.

According to some preferred aspects of the present invention, the silicone elastic microspheres are added in an amount of 10 to 30% by mass of the silicone gel composition. In some preferred embodiments of the present invention, the silicone elastic microspheres are added in an amount of 15 to 30% by mass of the silicone gel composition. In some more preferred embodiments of the present invention, the silicone elastic microspheres are added in an amount of 17 to 26% by mass of the silicone gel composition.

In the past, when silicone gel is mixed with active functional particles, the silicone chain swells small molecular solvent or silicone oil to form high-viscosity silicone gel, so that the mixed active functional particles have poor dispersibility and are easy to settle.

The organic silicon gel composition is prepared by diluting and swelling organic silicon elastic microspheres by grease, and dispersing active functional particles in the grease in the diluting and swelling process.

In the process of diluting and swelling the organic silicon elastic microspheres by the oil, the active functional particles are dispersed in the oil, the active functional particles can be fully and uniformly mixed and are not easy to agglomerate, and the mixed finished product has excellent stability and is not easy to settle, so that the dispersibility and stability of the active functional particles in the formed organic silicon gel are well realized, and the defects of poor dispersibility and difficult long-term stable dispersion in the prior art are avoided.

According to some preferred and specific aspects of the present invention, the active functional particles are personal care ingredients.

According to some specific aspects of the invention, the personal care ingredients include skin care ingredients and hair care ingredients.

Further, the skin care ingredients include skin feel modifiers, emollients, fragrances, ultraviolet absorbers, sunscreens, toners, herbal extracts, preservatives, light diffusers, and combinations thereof.

Further, the hair care ingredients include conditioning agents, surfactants, pearlizing agents, colorants, dyes, and combinations thereof.

According to some preferred and specific aspects of the invention, the oil is a combination of one or more selected from the group consisting of linear dimethicone, cyclic dimethicone, isododecane, isohexadecane, white oil, squalane, isononyl isononanoate, cetyl ethyl hexanoate, caprylic/capric triglyceride, diisostearyl malate, tri (ethyl hexanoate) glycerol, and propylene glycol dicaprylate/caprate.

The invention also provides a technical scheme that: a method of making the silicone gel composition described above, the method comprising the steps of:

grease is adopted to dilute and swell the organic silicon elastic microspheres, and active functional particles are dispersed in the grease in the diluting and swelling process to prepare the organic silicon gel composition.

In some embodiments of the present invention, the specific embodiments of the above-described preparation of the silicone gel composition are as follows: stirring the active functional particles, the organic silicon elastic microspheres and the grease together, mixing at the temperature of 10-50 ℃, diluting and swelling the organic silicon elastic microspheres by the grease, and dispersing the active functional particles in the grease in the diluting and swelling process to prepare the organic silicon gel composition.

In some embodiments of the present invention, the specific embodiments of the above-described preparation of the silicone gel composition are as follows: mixing and stirring the organic silicon elastic microspheres and grease at the temperature of 10-50 ℃, diluting and swelling the organic silicon elastic microspheres by using the grease, adding active functional particles in the process of dilution and swelling, and dispersing the active functional particles in the grease to prepare the organic silicon gel composition.

According to the method for preparing the organic silicon gel composition, active functional particles are dispersed in the oil in the process of diluting and swelling the organic silicon elastic microspheres by the oil, and because the volume in the oil expands, the active functional particles can be uniformly dispersed in the oil and are not easy to agglomerate, and the mixed finished product has excellent stability and is not easy to settle.

According to the present invention, the silicone elastic microspheres are commercially available.

According to some preferred aspects of the present invention, the silicone elastic microspheres can be prepared by the following preparation method:

mixing a compound containing at least two double bonds, hydrogen-containing polysiloxane and a catalyst, then mixing the mixture with an emulsifier and water, homogenizing the mixture to form emulsion, and heating and curing the emulsion; and drying and crushing after the reaction is finished to obtain the organic silicon elastic microspheres.

According to some preferred aspects of the invention, the compound containing at least two double bonds comprises a vinyl terminated dimethylsilicone oil, a vinyl terminated olefin, a vinyl terminated polyether, and combinations of two or more thereof.

According to some preferred aspects of the present invention, the hydrogen-containing polysiloxane comprises hydrogen-containing silicone oil.

According to some preferred aspects of the present invention, the catalyst comprises chloroplatinic acid, a chloroplatinate salt, an alcohol-modified chloroplatinic acid, a complex of chloroplatinic acid with an olefin, chloroplatinic acid, or a complex of a chloroplatinic acid salt with a vinyl-containing siloxane.

According to some preferred aspects of the invention, the emulsifier comprises a combination of one or more of an anionic emulsifier, a cationic emulsifier, an amphoteric emulsifier, and a non-ionic emulsifier; wherein the anionic emulsifier comprises alkyl sulfate, alkyl sulfonate, fatty acid ester sulfonate, alkyl succinic acid sulfonate, alkyl phosphate and alkyl carboxylate;

the cationic emulsifier comprises alkyl ammonium salts, alkyl quaternary ammonium salts and polyamine;

the amphoteric emulsifier comprises lecithin, amino acid type and betaine type;

the non-ionic emulsifier comprises polyoxyethylene, fatty alcohol polyoxyethylene ether, alkyl glycoside, span and tween series, polyol series, polyether modified silicone oil, and sorbitan monolaurate.

The invention also provides a technical scheme that: use of the silicone gel composition described above in a personal care composition.

The invention also provides a technical scheme that: a personal care composition comprising the silicone gel composition described above.

According to some specific aspects of the invention, the personal care composition comprises a sunscreen cream, a skin cream, a serum-upgraded cream, an eye cream, a lipstick, an eye shadow, a foundation, a compact, an eyeliner, an eye shadow, a blush, a mascara, and the like.

Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:

based on the problem that active functional particles are difficult to be uniformly dispersed in organic silicon gel in a short time in the prior art, the invention innovatively provides a novel intermediate composition, namely organic silicon gel composition, which directly comprises organic silicon elastic microspheres, active functional particles and grease and is in a gel state, the invention abandons the prior mode of directly adopting organic silicon gel, but adopts the organic silicon elastic microspheres to replace the organic silicon gel in the prior art, can fully and uniformly mix the active functional particles, the organic silicon elastic microspheres and the grease by using smaller shearing force, and in the process of diluting and swelling the organic silicon elastic microspheres by the grease, the active functional particles are dispersed in the grease, namely the active functional particles are dispersed in the grease before the organic silicon elastic microspheres are completely in the gel state, thereby realizing unexpected excellent dispersibility and lasting stability of the dispersed state, furthermore, the composition can replace the prior organic silicon gel and active functional particles to be applied to final products, so that the active functional particles in the final products have good dispersibility and good stability, and the functions of the active functional particles are fully exerted.

Drawings

FIG. 1 is a microscopic view of a paste-type silicone gel obtained in example 2 of the present invention;

FIG. 2 is a microscopic view of the toner-dispersed silica gel obtained in comparative example 1 of the present invention;

FIG. 3 is a microscopic view of the toner-dispersed silica gel obtained in comparative example 2 of the present invention;

FIG. 4 is a graph showing the effect of the sunscreen agent obtained in example 6 of the present invention after stability test (placing in an oven at 40 ℃ C. for 15 days) (the body opening is substantially upward)

FIG. 5 is a graph showing the effect of the sunscreen obtained in example 6 of the present invention after a stability test (placing in an oven at 40 ℃ for 15 days) was carried out (in a poured state, the body opening was substantially horizontal);

FIG. 6 is a graph showing the effect of the sunscreen composition of comparative example 2 after stability testing (oven at 40 ℃ C. for 15 days) according to the present invention (body opening substantially facing upward);

FIG. 7 is a graph showing the effect of the sunscreen composition of the present invention after stability test (oven at 40 ℃ C. for 15 days) using the sunscreen composition obtained in comparative example 2 (in a poured state, the body opening is substantially horizontal).

Detailed Description

The above-described scheme is further illustrated below with reference to specific examples; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.

Not specifically illustrated in the following examples, all starting materials are commercially available or may be prepared by methods conventional in the art.

Example 1

The embodiment provides a preparation method of an organic silicon elastic microsphere and the organic silicon elastic microsphere prepared by the method, which comprises the following steps:

(1) 20g of vinyl-terminated dimethylsilicone oil (Mw ═ 1.9. + -. 0.1X 10)⁴Commercially available with a vinyl content of 0.4 ± 0.1% wt) and 80g of hydrogen-containing silicone oil (Mw ═ 2.1 ± 0.1 × 10⁴Hydrogen content 0.07 ± 0.01% wt, commercially available) were mixed and a calculated amount of chloroplatinic acid (10 ppm in terms of Pt in the mixture) was added and mixed well.

(2) Adding 4g polyoxyethylene sorbitan fatty acid ester (purchased from Chinese medicine, Tween-20) into 200g water to prepare a solution;

(3) mixing the mixture obtained in the step (1) with the solution obtained in the step (2), homogenizing to form emulsion, reacting at 50 ℃ for 4h, drying the emulsion, and grinding to obtain the organosilicon elastic microspheres, wherein the particle size of the organosilicon elastic microspheres is about 5-20 μm.

Example 2

This example provides a silicone gel composition and method of preparation, the silicone gel composition being a cream-type silicone gel comprising 20g of the silicone elastic microspheres prepared in example 1, 25g of toner (KREMER, germany, designation C25060) and 55g of 5cst dimethicone (DOW, PMX-200);

the preparation method comprises the following steps: 20g of the silicone elastic microspheres prepared in example 1, 25g of toner C25060 and 55g of 5cst simethicone were mixed, and the mixture was swelled at 60 ℃ under a stirring condition (50rpm) for 6 hours, and the microscopic image thereof was measured as shown in FIG. 1, whereby it was found that a color paste type silicone gel having uniform dispersion and uniform color was obtained in this example.

Example 3

This example provides a silicone gel composition and method of making, which is a polydimethylsiloxane-dispersed silicone gel comprising 25.5g of the silicone elastomeric microspheres prepared in example 1, 4.5g of polydimethylsiloxane (ex chang, designation WJ450) and 70g of 5cst dimethicone (DOW, PMX-200);

the preparation method comprises the following steps: 25.5g of the silicone elastic microspheres prepared in example 1, 4.5g of polydimethylsiloxane, and 70g of 5cst dimethyl silicone oil were mixed and swollen at 60 ℃ under a stirring condition (50rpm) for 6 hours to obtain a polydimethylsiloxane-dispersed silicone gel having uniform dispersion and excellent smoothness.

Example 4

This example provides a silicone gel composition and method of preparation, the silicone gel composition being a physical sunscreen dispersed silicone gel comprising 17.5g of the silicone elastic microspheres prepared in example 1, 50g of nano ZnO powder and 32.5g of 5cst dimethicone (DOW, PMX-200);

the preparation method comprises the following steps: 17.5g of the silicone elastic microspheres prepared in example 1, 50g of nano ZnO powder and 32.5g of 5cst simethicone are mixed and swelled at 60 ℃ under the stirring condition (50rpm) for 6h to obtain dispersed silica gel which is uniformly dispersed and stabilized by a physical sunscreen agent.

Comparative example 1

The embodiment provides a process for mixing silica gel and toner, which comprises the following specific preparation processes: stirring 25g of toner (KREMER, Germany, brand C25060) and 37.5g of octyldodecanol for 30min until the toner is uniform, and transferring the mixture to a three-roller machine for strong shearing and dispersing for many times to obtain the color paste. 20g of silica gel (self-made: 25g of the silicone elastic microspheres prepared in example 1 and 75g of 5cst dimethicone are mixed and swelled at 60 ℃ under a stirring condition (50rpm) for 6 hours), and 17.5g of 50cst dimethicone (DOW, PMX-200) are stirred and mixed uniformly. The dispersed color paste is added into the dispersed silica gel, and is stirred and mixed evenly with strong force to prepare toner dispersed silica gel, and a microscopic picture is obtained by testing as shown in figure 2.

Comparative example 2

The embodiment provides a toner dispersing silica gel, and the specific preparation process comprises the following steps: 20g of vinyl-terminated dimethylsilicone oil (Mw ═ 1.9. + -. 0.1X 10)⁴Commercially available with a vinyl content of 0.4 ± 0.1% wt) and 80g of hydrogen-containing silicone oil (Mw ═ 2.1 ± 0.1 × 10⁴Hydrogen content 0.07 ± 0.01% wt, commercially available), 5g C250 toner (KREMER, germany, designation C25060), mixed well, added chloroplatinic acid (10 ppm in terms of Pt in the mixture) in calculated amounts under stirring, and mixed well with 50g 5cst simethicone. Simultaneously, the temperature is increased, the reaction is carried out for 3h at 70 ℃, the rotating speed is 100rpm, and the reaction is stopped. Transferring the mixture to a blender, adding 450g of 5cst dimethyl silicone oil, mixing for 4h under high shear force to obtain toner dispersed silica gel, and testing to obtain a microscopic image shown in FIG. 3, which shows that the toner has poor dispersibility.

Example 5

This example provides a lipstick made from the color paste type silicone gel prepared in example 2, having the components and amounts shown in table 1 below.

TABLE 1

The preparation method of the lipstick comprises the following steps:

(1) mixing the components of phase A at 90 +/-5 ℃, and stirring and dispersing the components uniformly;

(2) mixing the components of the phase B at 90 +/-5 ℃, and stirring and dispersing the components until the components are uniform;

(3) adding the phase A into the phase B at the temperature of 90 +/-5 ℃, and stirring and dispersing the mixture to be uniform;

(4) cooling to 80 +/-5 ℃, adding the phase D into the mixture obtained in the step (3), and uniformly mixing;

(5) adding the phase C into the mixture obtained in the step (4) at the temperature of 80 +/-5 ℃, and fully stirring and mixing for 10-15 minutes at a high speed (about 700 rpm);

(6) cooling to 75 +/-5 ℃, adding the phase E, stirring at medium speed (about 400rpm) and uniformly mixing (keeping the temperature);

(7) preheating a mould, pouring a material body into the mould, cooling to room temperature, and then putting the mould into a refrigerator for cooling for about 15 minutes;

(8) and taking out the die from the refrigerator, removing the upper die, inserting the packing material, demolding and extracting paste, screwing the paste to the bottom of the tube, and finishing the lipstick.

Application comparative example 1

This example provides a lipstick having the components and amounts shown in table 2 below.

TABLE 2

The preparation method of the lipstick comprises the following steps:

(1) mixing and stirring the C25060 toner and the octyl dodecanol for 30 minutes, and strongly shearing, dispersing and grinding for 2-3 times by using a three-roller machine to obtain color paste;

(2) mixing the components of phase A at 90 +/-5 ℃, and stirring and dispersing the components uniformly;

(3) mixing the components of the phase B at 90 +/-5 ℃, and stirring and dispersing the components until the components are uniform;

(4) adding the phase A into the phase B at the temperature of 90 +/-5 ℃, and stirring and dispersing the mixture to be uniform;

(5) cooling to 80 +/-5 ℃, adding the phase D into the mixture obtained in the step (3), and uniformly mixing;

(6) adding the color paste obtained in the step (1) into the mixture obtained in the step (5) at the temperature of 80 +/-5 ℃, and fully stirring and mixing for 20-25 minutes at a high speed (about 700 rpm);

(7) cooling to 75 +/-5 ℃, adding the phase E, stirring at medium speed (about 400rpm) and uniformly mixing (keeping the temperature);

(8) preheating a mould, pouring a material body into the mould, cooling to room temperature, and then putting the mould into a refrigerator for cooling for about 15 minutes;

(9) and taking out the die from the refrigerator, removing the upper die, inserting the packing material, demolding and extracting paste, screwing the paste to the bottom of the tube, and finishing the lipstick.

Compared with the embodiment 5, in the embodiment 5, the color paste type silica gel only needs to be directly put into the oil phase and the wax phase which are uniformly mixed, and extra strong shearing equipment is not needed; in this case, the toner must first be mixed with the oil, mixed with a powerful shearing device, and then introduced into the formulation, and the time required for mixing the silicone gel with the wax is lengthened, or else there is a risk of uneven dispersion.

Example 6

This example provides a sunscreen made using the physical sunscreen dispersion silicone gel prepared in example 4, and having the components and amounts shown in table 3 below.

TABLE 3

The preparation method comprises the following steps: step 1: mixing and stirring the components of the phase A for 3 minutes; step 2: mixing and dispersing the phase B uniformly, slowly dripping the phase A under the stirring condition, finishing dripping within 30 minutes, then stirring for 30 minutes, and homogenizing at a low speed (about 3000rpm) for 1 minute; and step 3: adding phase C, stirring at low speed (about 150rpm) to obtain sunscreen agent; the resulting sunscreen was tested for stability (in a 40 ℃ oven for 15 days) and still showed high viscosity, no delamination or particle mura, and still maintained good viscosity, as shown in figures 4-5.

Comparative application example 2

This example provides a sunscreen having the components and amounts shown in table 4 below.

TABLE 4

The preparation method comprises the following steps: step 1: mixing and stirring the components of the phase A for 3 minutes; step 2: mixing and dispersing the phase B uniformly, slowly dripping the phase A under the stirring condition, finishing dripping within 30 minutes, then stirring for 30 minutes, and homogenizing at a low speed (about 3000rpm) for 1 minute; and step 3: adding phase C, stirring at low speed (about 150rpm) to obtain sunscreen agent; the stability test of the prepared sunscreen agent (placing in a 40 ℃ oven for 15 days) shows that many particles are adhered to the bottle wall, obvious particles are not uniformly dispersed, and meanwhile, the bottle body has obvious flowing property and insufficient viscosity after being poured, as shown in figures 6-7.

The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.