CN111991243A

CN111991243A - Double-layer multi-effect coagulated bead and preparation method and application thereof

Info

Publication number: CN111991243A
Application number: CN202010895394.7A
Authority: CN
Inventors: 陈宇霞; 陈庆生; 龚盛昭; 吴知情
Original assignee: Guangzhou Huanya Cosmetic Science and Technology Co Ltd
Current assignee: Guangzhou Huanya Cosmetic Science and Technology Co Ltd
Priority date: 2020-08-31
Filing date: 2020-08-31
Publication date: 2020-11-27
Anticipated expiration: 2040-08-31
Also published as: CN111991243B

Abstract

The invention provides a double-layer multi-effect bead and a preparation method and application thereof, wherein the double-layer multi-effect bead comprises the following components: the skin conditioner comprises a surfactant, a thickening agent, polyhydric alcohol, a skin conditioning agent, grease and water, wherein the thickening agent comprises any one or the combination of at least two of gellan gum, agarose or carrageenan. The preparation method of the double-layer multi-effect coagulated bead comprises the following steps: (1) mixing a polyol, a surfactant, a thickener and water; (2) adding a stabilizer and a skin conditioner, controlling the temperature to be 40-60 ℃, mixing at 300-1500 rpm/min, standing, cooling to form solid gel, crushing and mixing; (3) adding oil and fat, and mixing to obtain the double-layer multi-effect coagulated beads. One layer of the double-layer multi-effect coagulated beads is transparent solution, and the other layer of the double-layer multi-effect coagulated beads is transparent or opaque coagulated bead particles, so that the double-layer multi-effect coagulated beads not only have novel appearance, but also have multiple effects of makeup removal, moisture preservation and skin care.

Description

Double-layer multi-effect coagulated bead and preparation method and application thereof

Technical Field

The invention belongs to the technical field of cosmetics, and particularly relates to a double-layer multi-effect coagulated bead as well as a preparation method and application thereof.

Background

With the development of cosmetic technology, cosmetics play an increasingly important role in people's daily life. After the face is made up, if not removed completely, the residual cosmetics can cause the pore blockage of the face skin, leading to the imbalance of the oil secretion of the skin, and further causing skin problems such as acne, comedo and blackhead. Therefore, consumers have increasingly demanded facial cleansing products which are not only fast cleansing, deep cleansing, and all-in-one effects of cleansing, makeup removal, and skin care, but also mild, non-irritating, convenient to use, and novel and beautiful in appearance.

The existing makeup removing cosmetics mainly comprise makeup removing oil, makeup removing water and a double-layer makeup removing liquid combined with the makeup removing oil and the makeup removing water, wherein the makeup removing oil mainly comprises grease and an emulsifier, and a certain amount of makeup removing oil stains remained on the face are removed according to the principle that the grease is dissolved mutually, so that the effect of dissolving stains is achieved; the makeup remover mainly comprises water, has light skin feel and small irritation, can supplement water for the skin while removing the makeup, and is suitable for various skin types, particularly sensitive skin and oily skin; the double-layer makeup remover can effectively combine the advantages of the makeup removing oil and the makeup removing water, and has the advantages of refreshing and no stimulation of the makeup removing water and strong makeup removing capability of the makeup removing oil.

CN110420152A discloses a refreshing and mild double-layer cleansing liquid, which comprises an oil phase and a water phase, wherein the mass ratio of the oil phase to the water phase is 2:8, the oil phase comprises 80-98% of synthetic oil, 2-20% of natural oil and 0.1-0.5% of antioxidant by mass percent, and the water phase comprises 2-10% of humectant, 0.1-1% of surfactant, 0.05-0.2% of chelating agent, 0.5-5% of skin conditioner and the balance of deionized water by mass percent. The makeup remover has good makeup removing effect and is fresh, cool and mild.

CN108524322A discloses a double-layer cleansing lotion, which comprises the following components: 25-40 wt% of grease, 5-15 wt% of humectant, 15-35 wt% of surfactant, 0.05-0.15 wt% of chelating agent, 0.01-0.5 wt% of acid-base regulator, 0.3-2.2 wt% of additive, 1.0-1.5 wt% of inulin lauryl carbamate and the balance of water. The makeup remover has a cleaning effect besides a makeup removing effect.

CN103505381A discloses a two-layer makeup removing emulsion, which is composed of olive oil, silicone oil, mineral oil, vitamin E, poloxamer, a humectant, water, a preservative and the like, can remove most of oil paint, and has good moisturizing and nourishing effects.

In summary, the current double-layer makeup cosmetics have a single effect, and the appearance of the products of the type is not updated in the market for a long time. Therefore, how to provide a makeup remover cosmetic with various effects of makeup removal, moisture retention and skin care, and a novel appearance has become one of the hot points of interest in the field of cosmetics.

Disclosure of Invention

Aiming at the defects and actual needs of the prior art, the invention provides a double-layer multi-effect coagulated bead and a preparation method and application thereof.

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

in a first aspect, the present invention provides a dual-layer multieffect bead comprising: the skin conditioner comprises a surfactant, a thickening agent, polyhydric alcohol, a skin conditioning agent, grease and water, wherein the thickening agent comprises any one or combination of at least two of gellan gum, agarose or carrageenan, and is preferably the gellan gum and/or the agarose.

The preparation method of the double-layer multi-effect coagulated bead comprises the following steps:

(1) mixing a polyol, a surfactant, a thickener and water;

(2) adding a stabilizer and a skin conditioner, controlling the temperature to be 40-60 ℃, stirring and mixing at 300-1500 rpm/min, standing and cooling until solid gel is formed, and then smashing and mixing;

(3) adding oil and fat, and mixing to obtain the double-layer multi-effect coagulated beads.

In the double-layer multi-effect coagulated bead, the thickening agent gellan gum, agarose or carrageenan interacts with water phase to provide a foundation for preparing the appearance of the coagulated bead; the surfactant has certain capability of dissolving the makeup dirt, forms micelle groups in a system, and has good mildness and low irritation to skin; the oil dissolves the color cosmetics by a similar compatibility mechanism to form a thin ester film on the skin to nourish the skin; the skin conditioner has good moisturizing effect; the polyalcohol has skin-friendly effect and mild property.

According to the invention, the interaction of the thickener gellan gum, the agarose or carrageenan and the water phase of the double-layer multi-effect coagulated bead provides a foundation for preparing the appearance of the coagulated bead, the temperature control temperature in the step (2) of the preparation method is limited to 40-60 ℃, the mixed rotating speed is limited to 300-1500 rpm/min, the double-layer multi-effect coagulated bead with the novel appearance of coagulated bead particles is obtained, the surfactant and the grease act together, the good makeup removing effect is ensured, the irritation is reduced, the skin conditioner has the moisture preserving effect, the polyol promotes the overall mildness of the double-layer multi-effect coagulated bead, and the components are mutually matched to play a synergistic effect, so that the double-layer multi-effect coagulated bead has the multiple effects of makeup removing, moisture preserving and skin caring while having the novel appearance.

Preferably, the surfactant comprises any one of decyl glucoside, lauryl glucoside, sodium lauryl glucarate, disodium cocoyl amphodiacetate, or potassium cocoyl hydrolyzed avenin, or a combination of at least two of which typical but non-limiting combinations are: a combination of decyl glucoside and lauryl glucoside, a combination of disodium cocoyl amphodiacetate and sodium lauryl glucarate, or a combination of sodium lauryl glucarate and potassium cocoyl hydrolyzed avenin.

Preferably, the polyhydric alcohol comprises any one of glycerol, butylene glycol, propylene glycol, dipropylene glycol, 1, 2-hexanediol, 1, 2-pentanediol, or 1, 3-propanediol, or a combination of at least two of these, with typical but non-limiting combinations being: a combination of glycerol and dipropylene glycol, a combination of glycerol and 1, 2-hexanediol, or a combination of dipropylene glycol and 1, 2-hexanediol.

Preferably, the skin conditioning agent comprises any one of or a combination of at least two of PEG-8 caprylic/capric glycerides, PEG-6 caprylic/capric glycerides, PEG-75 shea glycerides, or a glycine max seed extract, wherein typical but non-limiting combinations are: a combination of PEG-8 caprylic/capric glycerides and a extract of Glycine max seed, a combination of PEG-6 caprylic/capric glycerides and a extract of Glycine max seed, or a combination of PEG-75 shea butter glycerides and PEG-6 caprylic/capric glycerides.

Preferably, the fat or oil comprises any one or a combination of at least two of white oil, olive oil, cetyl ethylhexanoate, meadowfoam oil, isononyl isononanoate, glycerol tri (ethylhexanoate) or cyclopentadimethylsiloxane, with typical but non-limiting combinations being: a combination of white oil and cetyl ethylhexanoate, a combination of cetyl ethylhexanoate and pentamethylsiloxane or a combination of olive oil and meadowfoam oil.

Preferably, the raw materials for preparing the double-layer multi-effect coagulated bead also comprise a stabilizer.

Preferably, the stabilizer comprises calcium chloride.

Preferably, the surfactant is present in the bilayer multieffect beading in an amount of 0.10% to 5.00% by mass, and may be present in an amount of 0.30%, 0.50%, 0.70%, 1.00%, 2.00%, 3.00%, 4.00%, 4.20%, 4.40%, 4.60% or 4.80% by mass, but not limited to the recited values, and values within the range of values apply, preferably 0.10% to 2.00%.

Preferably, the mass percentage of the thickener in the double-layer multi-effect condensed bead is 0.05% to 1.00%, and may be 0.07%, 0.09%, 0.11%, 0.13%, 0.20%, 0.30%, 0.40%, 0.60%, 0.80%, 0.85%, or 0.95%, but is not limited to the enumerated values, and the numerical values in the numerical range apply, and preferably 0.05% to 0.80%.

Preferably, the mass percentage of the polyol in the double-layer multi-effect bead is 1.00% to 20.00%, and may be 1.00%, 2.00%, 3.00%, 4.00%, 10.00%, 12.00%, 14.00%, 16.00%, 17.00%, 18.00% or 19.00%, but is not limited to the enumerated values, and all values within the numerical range apply, and are preferably 1.00% to 15.00%.

Preferably, the mass percentage of the stabilizer in the double-layer multi-effect condensed bead is 0.00-0.50%, and may be 0.01%, 0.02%, 0.03%, 0.05%, 0.10%, 0.20%, 0.30%, 0.35%, 0.38%, 0.40%, or 0.45%, but is not limited to the listed values, and the values in the numerical range apply, and are preferably 0.01-0.20%.

Preferably, the skin conditioning agent is present in the bilayer multieffect beading in an amount of 0.01% to 5.00% by weight, and may be present in an amount of 0.03%, 0.05%, 0.07%, 0.15%, 0.50%, 1.00%, 2.00%, 3.00%, 3.50%, 4.50% or 4.80% by weight, but not limited to the recited values, and values within the range of values apply, preferably 0.01% to 3.00%.

Preferably, the mass percentage of the grease in the double-layer multi-effect bead is 1.00-50.00%, and may be 2.00%, 4.00%, 6.00%, 10.00%, 15.00%, 20.00%, 30.00%, 35.00%, 40.00%, 42.00% or 48.00%, but is not limited to the listed values, and all the values in the numerical range are applicable, and are preferably 1.00-40.00%.

Preferably, the double-layer multi-effect beads comprise the following components in percentage by mass: 0.10-5.00 percent of surfactant, 0.05-1.00 percent of thickening agent, 1.00-20.00 percent of polyol, 0.00-0.50 percent of stabilizer, 0.01-5.00 percent of skin conditioner, 1.00-50.00 percent of grease and the balance of water.

Preferably, the double-layer multi-effect beads comprise the following components in percentage by mass: 0.10-2.00 percent of surfactant, 0.05-0.80 percent of thickening agent, 1.00-15.00 percent of polyol, 0.01-0.20 percent of stabilizer, 0.01-3.00 percent of skin conditioner, 1.00-40.00 percent of grease and the balance of water.

In a second aspect, the present invention provides a method for preparing the bilayer multieffect bead of the first aspect, the method comprising the steps of:

(1) mixing a polyol, a surfactant, a thickener and water;

(2) adding a stabilizer and a skin conditioner, controlling the temperature to be 40-60 ℃, mixing at 300-1500 rpm/min, standing, cooling to form solid gel, crushing and mixing;

Preferably, the temperature controlled is 40-60 ℃, and may be 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 56 ℃ or 58 ℃, but is not limited to the recited values, and the values in the numerical range are all applicable.

Preferably, the mixing speed in step (2) is 300-1500 rpm/min, and may be 500rpm/min, 600rpm/min, 700rpm/min, 800rpm/min, 900rpm/min, 1000rpm/min, 1200rpm/min or 1300rpm/min, but is not limited to the enumerated values, and the numerical values in the numerical range are all applicable.

Preferably, the mixing in steps (1), (2) and (3) is performed by stirring.

Preferably, the temperature of the mixing in the step (1) is 60-80 ℃, and can be 62 ℃, 64 ℃, 66 ℃, 68 ℃, 70 ℃, 72 ℃, 76 ℃ or 78 ℃, but is not limited to the enumerated values, and the numerical values in the numerical range are all applicable.

Preferably, the mixing speed in step (1) is 300-1500 rpm/min, preferably 500-1200 rpm/min, and may be 600rpm/min, 700rpm/min, 800rpm/min, 900rpm/min, 1000rpm/min or 1100rpm/min, but is not limited to the listed values, and the values in the numerical range are all applicable.

Preferably, the mixing time in the step (1) is 1-10 min, and may be 2min, 4min, 6min or 8min, but is not limited to the listed values, and the values in the range are all applicable, and are preferably 3-8 min.

Preferably, the mixing time in the step (2) is 1-10 min, and may be 2min, 4min, 6min or 8min, but is not limited to the listed values, and the values in the range are all applicable, and preferably 2-5 min.

Preferably, the temperature of the standing solution in the step (2) is reduced to 20-40 ℃, and the temperature can be 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃, 32 ℃, 36 ℃ or 38 ℃, but is not limited to the listed values, and the values in the numerical range are all applicable.

Preferably, the time for smashing and mixing in the step (2) is 2-10 min, and may be 2min, 4min, 6min or 8min, but is not limited to the listed values, and the values in the value range are all applicable, and are preferably 3-8 min.

Preferably, the breaking up and mixing in step (2) is performed at a speed of 500-3000 rpm/min, which may be 600rpm/min, 700rpm/min, 800rpm/min, 900rpm/min, 1000rpm/min, 1500rpm/min, 1700rpm/min, 2000rpm/min, 2200rpm/min, 2500rpm/min, or 2800rpm/min, but is not limited to the listed values, and the values in the range are all applicable.

Preferably, the mixing time in the step (3) is 1-5 min, and may be 2min, 3min or 4min, but is not limited to the listed values, and the values in the range are all applicable, and preferably 1-3 min.

Preferably, the mixing speed in step (3) is 100-1500 rpm/min, and may be 200rpm/min, 300rpm/min, 400rpm/min, 500rpm/min, 800rpm/min, 1000rpm/min, 1100rpm/min, 1200rpm/min, 1300rpm/min or 1400rpm/min, but is not limited to the listed values, and the values in the numerical range are all applicable.

In the present invention, as a preferred preparation method, the method comprises:

(1) putting polyalcohol, a surfactant, a thickening agent and water into a pot, stirring and mixing at the temperature of 60-80 ℃, wherein the stirring speed is 300-1500 rpm/min, and the stirring and mixing time is 1-10 min;

(2) adding a stabilizer and a skin conditioner, cooling to 40-60 ℃, stirring, mixing, defoaming, stirring at the rotating speed of 300-1500 rpm/min for 1-10 min, standing, cooling to 20-40 ℃, forming a solid gel, stirring, smashing, and mixing, wherein the stirring at the rotating speed of 1500-3000 rpm/min, and the smashing and mixing time is 5-10 min;

(3) adding grease, stirring and mixing to obtain the double-layer multi-effect coagulated beads, wherein the stirring speed is 100-1500 rpm/min, and the stirring and mixing time is 1-5 min.

In a third aspect, the present invention provides a use of the bilayer multieffect bead of the first aspect in the preparation of a cosmetic.

In a fourth aspect, the present invention provides a cosmetic comprising the double-layered multi-effect bead of the first aspect.

Preferably, the cosmetic further comprises any one or a combination of at least two of a chelating agent, a preservative, a pigment or an aromatizer.

Preferably, the formulation of the cosmetic includes any one of a water agent, an emulsion, a essence, a gel or a spray.

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

(1) the components of the double-layer multi-effect condensed bead are matched with each other, the thickening agent gellan gum, the agarose or carrageenan and the water phase are interacted, a foundation is provided for preparing the appearance of the condensed bead, the surfactant and the grease are interacted, the good makeup removing effect is guaranteed, the irritation is reduced, the skin conditioner has a moisturizing effect, the polyalcohol promotes the overall mildness of the double-layer multi-effect condensed bead, and the double-layer multi-effect condensed bead has multiple effects of makeup removing, moisturizing and skin care while having a novel appearance;

(2) the preparation process of the double-layer multi-effect coagulated beads is simple, the equipment cost is low, the efficiency is high, and the preparation method is suitable for large-scale production;

(3) the cosmetics prepared by the double-layer multi-effect condensed bead have novel appearance, have multiple effects of makeup removal, moisture preservation and skin care, and are specifically characterized in that a subject has fresh skin feel after makeup removal, the skin still has high moisture content after 8 hours of use, the average hydration rate reaches more than 42 percent, and the double-layer multi-effect condensed bead has important application prospect in the field of cosmetics.

Drawings

FIG. 1 is a double-layered multi-effect bead prepared in example 1;

FIG. 2 shows the results of the hemolysis rate test for different concentrations of each sample;

FIG. 3 is a graph showing the particle size distribution of the double-layer multi-effect beads prepared in example 1;

FIG. 4 is a graph showing the particle size distribution of the double-layer multi-effect beads prepared in example 2;

FIG. 5 is a graph showing the particle size distribution of the double-layer multi-effect beads prepared in example 3;

FIG. 6 is a particle size distribution diagram of the double-layer multi-effect beads prepared in example 10;

FIG. 7is a particle size distribution diagram of the double-layer multi-effect coagulated beads prepared in example 11;

FIG. 8 is a graph showing the particle size distribution of the double-layered multi-effect coagulated beads prepared in example 12;

FIG. 9 is a particle size distribution diagram of the double-layer multi-effect beads prepared in example 13;

FIG. 10 is a graph showing the particle size distribution of comparative example 7 (a commercially available and well-known brand double-layer cleansing liquid);

FIG. 11 is a graph showing the particle size distribution of comparative example 8 (a commercially preferred double-layer essence water of a certain known brand).

Detailed Description

To further illustrate the technical means adopted by the present invention and the effects thereof, the present invention is further described below with reference to the embodiments and the accompanying drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention.

The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or apparatus used are conventional products commercially available from normal sources, not indicated by the manufacturer.

Example 1

The embodiment provides a double-layer multi-effect bead, which comprises the following components in percentage by mass: 0.10% of cocoyl amphodiacetate disodium, 1.00% of gellan gum, 1.00% of glycerol, 0.50% of calcium chloride, 5.00% of PEG-8 glyceryl isostearate and 1.00% of cetyl ethylhexanoate, and the balance of water.

The preparation method comprises the following steps:

(1) putting glycerol, disodium cocoyl amphodiacetate, gellan gum and water into a pot according to a proportion, stirring and mixing at 60 ℃, wherein the stirring speed is 1500rpm/min, and the stirring and mixing time is 1 min;

(2) adding calcium chloride and PEG-8 glyceryl isostearate in proportion, cooling to 50 deg.C, stirring, mixing, defoaming at stirring speed of 1000rpm/min for 1min, standing, cooling to 20 deg.C to form solid gel, stirring, crushing, and mixing at stirring speed of 500rpm/min for 10 min;

(3) adding cetyl ethylhexanoate in a ratio, stirring and mixing to obtain the double-layer multi-effect coagulated beads, wherein the stirring speed is 100rpm/min, and the stirring and mixing time is 5 min.

The prepared double-layer multi-effect coagulated beads are shown in figure 1 and have obvious coagulated bead appearance.

Example 2

The embodiment provides a double-layer multi-effect bead, which comprises the following components in percentage by mass: decyl glucoside 5.00%, agarose 0.05%, 1, 2-hexanediol 20.00%, wild soybean seed extract 0.01%, cyclopenta dimethyl silicone polymer 50.00%, and water in balance.

The preparation method comprises the following steps:

(1) putting 1, 2-hexanediol, decyl glucoside, agarose and water into a pot according to a proportion, stirring and mixing at 80 ℃, wherein the stirring speed is 300rpm/min, and the stirring and mixing time is 10 min;

(2) adding the extract of wild soybean seeds in proportion, cooling to 40 deg.C, stirring at 300rpm/min for 10min, standing, cooling to 40 deg.C to form solid gel, stirring at 3000rpm/min, crushing, and mixing for 2 min;

(3) adding cyclopentadimethylsiloxane according to a proportion, stirring and mixing to obtain the double-layer multi-effect coagulated beads, wherein the stirring speed is 1500rpm/min, and the stirring and mixing time is 1 min.

Example 3

The embodiment provides a double-layer multi-effect bead, which comprises the following components in percentage by mass: 2.00 percent of sodium lauryl glucose carboxylate, 0.80 percent of carrageenan, 15.00 percent of propylene glycol, 3.00 percent of PEG-6 glyceryl isostearate, 40.00 percent of olive oil and the balance of water.

The preparation method comprises the following steps:

(1) putting propylene glycol, sodium lauryl glucose carboxylate, carrageenan and water into a pot according to a proportion, stirring and mixing at 75 ℃, wherein the stirring speed is 1000rpm/min, and the stirring and mixing time is 6 min;

(2) adding PEG-6 glyceryl isostearate according to a proportion, cooling to 60 ℃, stirring, mixing, defoaming, stirring at a rotation speed of 1500rpm/min for 3min, standing, cooling to 35 ℃, forming solid gel, stirring, smashing, mixing, stirring at a rotation speed of 1500rpm/min for 7 min;

(3) adding olive oil in proportion, stirring and mixing to obtain the double-layer multi-effect coagulated beads, wherein the stirring speed is 600rpm/min, and the stirring and mixing time is 2 min.

Example 4

This example is compared with example 1 except that in step (2) of the preparation method, calcium chloride and PEG-8 glyceryl isostearate are added proportionally and cooled to 40 ℃, and the rest is the same as example 1.

Example 5

This example is compared with example 1 except that in step (2) of the preparation method, calcium chloride and PEG-8 glyceryl isostearate are added proportionally and cooled to 60 ℃, and the rest is the same as example 1.

Example 6

The present example is different from example 1 only in that the defoaming was performed after stirring and mixing in step (2) in the preparation method, and the stirring speed was 300rpm/min, and the other steps are the same as example 1.

Example 7

The present example is different from example 1 only in that the defoaming was performed after stirring and mixing in step (2) in the preparation method, and the stirring speed was 1500rpm/min, and the other steps were the same as example 1.

Example 8

This example is similar to example 1 except that gellan gum was replaced with carrageenan, which is the same as example 1.

Example 9

This example is compared with example 1 except that gellan gum was replaced with agarose, and the rest was the same as example 1.

Example 10

In this example, a two-layer beading cosmetic was prepared, and the mass percentages of the components are shown in table 1.

TABLE 1

Note: "QS" means a small amount of addition, and the amount of addition is selected according to the actual formulation and production environment, and the following "QS" is the same as that of the above.

The preparation method comprises the following steps:

(1) putting the phase A into a pot in turn, heating to 75 ℃, stirring at the speed of 1000rpm/min for 5min, and dissolving uniformly;

(2) sequentially adding the phase B, the phase C and the phase D, cooling to 55 ℃, uniformly stirring at the speed of 800rpm/min for 3min, defoaming, standing, cooling to 35 ℃ to form solid gel, crushing, uniformly mixing, stirring at the speed of 2000rpm/min for 6 min;

(3) adding the phase F, and homogenizing uniformly at a homogenizing speed of 500rpm/min for 1-3 min.

(4) And (5) qualified stirring and discharging after detection.

Example 11

In this example, a two-layer beading cosmetic was prepared, and the mass percentages of the respective components are shown in table 2.

TABLE 2

The preparation method is the same as that of example 10.

Example 12

In this example, a two-layer beading cosmetic was prepared, and the mass percentages of the respective components are shown in table 3.

TABLE 3

The preparation method is the same as that of example 10.

Example 13

In this example, a two-layer beading cosmetic was prepared, and the mass percentages of the respective components are shown in table 4.

TABLE 4

The preparation method is the same as that of example 10.

Comparative example 1

This comparative example is the same as example 1 except that calcium chloride and PEG-8 glyceryl isostearate were added in proportion in step (2) of the preparation method and cooled to 30 ℃.

Comparative example 2

This comparative example is the same as example 1 except that calcium chloride and PEG-8 glyceryl isostearate were added in proportion in step (2) of the preparation method and cooled to 70 ℃.

Comparative example 3

The comparative example is the same as example 1 except that in the preparation method, the defoaming is performed after the stirring and mixing in step (2), and the stirring speed is 100 rpm/min.

Comparative example 4

The comparative example is different from example 1 only in that the defoaming is performed after the stirring and mixing in the step (2) in the preparation method, the stirring speed is 1700rpm/min, and the rest is the same as example 1.

Comparative example 5

This comparative example compares to example 1, except that gellan gum is replaced with xanthan gum, otherwise the same as example 1.

Comparative example 6

This comparative example is compared to example 1, except that gellan gum was replaced with pectin, otherwise the same as example 1.

Comparative example 7 commercially available double-layer cleansing liquid of a certain brand name

Comprises the following components: cyclopentadimethylsiloxane, water, glycerol, decyl glucoside, propylene glycol, PEG-6 caprylic/capric glycerides, polysorbate-60, disodium EDTA, dipotassium glycyrrhizinate, and phenoxyethanol.

Comparative example 8 commercially available double-layer essence water of certain well-known brand

Comprises the following components: water, glycerin, agar, xanthan gum, cyclopentadimethylsiloxane, dimethicone/vinyl dimethicone crosspolymer, polysorbate-60, decyl glucoside, disodium EDTA, cornflower (CENTAUREA CYANUS) floral water, p-hydroxyacetophenone, phenoxyethanol, and a fragrance.

Experimental example 1 different process conditions experiment

The appearance of the double-layered multi-effect beads prepared in example 1, examples 4 to 9 and comparative examples 1 to 6 was compared, and the results are shown in table 5.

TABLE 5

Case(s)	Appearance of coagulated beads
		Example 1	Is provided with
Example 4	Is provided with
		Example 5	Is provided with
Example 6	Is provided with
		Example 7	Is provided with
Example 8	Is provided with
		Example 9	Is provided with
Comparative example 1	Is free of
		Comparative example 2	Is free of
Comparative example 3	Is free of
		Comparative example 4	Is free of
Comparative example 5	Is free of
		Comparative example 6	Is free of

As can be seen from table 5, the double-layer multi-effect beads prepared in examples 1 and 4 to 9 have bead appearance, while the double-layer multi-effect beads prepared in comparative examples 1 to 6 do not have bead appearance, it is described that 3 factors, namely the type of carrageenan, the temperature reduction temperature in step (2) and the stirring and mixing speed in step (2), play a key role in the formation process of bead appearance, and the application prepares the double-layer multi-effect beads with bead appearance by studying the interaction among the 3 factors and the influence of the interaction on bead formation.

Test example 2 erythrocyte hemolysis test

The samples of examples 1 to 3, examples 10 to 13 and comparative examples 7 and 8 were subjected to hemolysis test of erythrocytes, and the irritation of the test samples to the skin surface was evaluated based on the principle that lipids and proteins on the surface of human skin are similar to the cell membrane of erythrocytes. The test results were evaluated according to the RBC test method and the classification standard (ECVAM. ECVAM DB-ALM: INVITIONX Protoco, Red blood cells test system. INVITOX No.37Ispra. Italy: ECVAM,1994.) of the European Alternatives verification center, the classification standard being shown in Table 6.

TABLE 6

L/D	Grading
		>100	Has no irritation
10<L/D<100	Micro-stimulation
		1<L/D<10	Mild stimulation
0.1<L/D<1	Moderate stimulation
		L/D≦1	Severe stimulation

The results of the experiment are shown in table 7 and fig. 2.

TABLE 7

As can be seen from Table 7, the double-layer multi-effect beads prepared in examples 1-3 and 10-13 have much reduced irritation, approaching or reaching the level of no irritation, compared to comparative example 7 (a commercially good double-layer makeup remover with a certain brand name) and comparative example 8 (a commercially good double-layer essence water with a certain brand name); as can be seen from FIG. 2, the concentrations of the double-layer multi-effect beads prepared in examples 1 to 3 and examples 10 to 13 are not hemolyzed at the concentration of less than 0.5%, and the concentrations of comparative examples 7 and 8 are not hemolyzed at the concentration of less than 0.01%; in summary, it is demonstrated that the double-layered multi-effect beads prepared in examples 1 to 3 and examples 10 to 13 are much less irritant than comparative examples 7 and 8.

Test example 3 evaluation of makeup removal Effect

20 female volunteers, aged 25-50 years, were selected and applied to full-face makeup with equal amounts of BB cream (W/O type), eye shadow and eyeliner lipstick, and then equal amounts of the double-layer multi-effect beading prepared in examples 1-3, the double-layer beading cosmetics prepared in examples 10-13, comparative example 7 (commercially good double-layer makeup remover of certain brand) and comparative example 8 (commercially good double-layer essence water of certain brand) were taken and applied together with makeup remover cotton, the products prepared in examples were applied to the left face, and the comparative examples 7 and 8 were applied to the right face, and skin feel after cleansing and makeup removing effects were evaluated, with the results shown in Table 8.

TABLE 8

As can be seen from Table 8, the double-layer multi-effect beading prepared in examples 1-3 and examples 10-13 has better makeup removing effect than that of comparative example 7 and comparative example 8, the skin of the volunteers is fresh after use, the eyes hardly feel irritating sensation when the eyes are subjected to makeup removing, the skin of the comparative example 7 and comparative example 8 is greasy after use, the eyes of the volunteers have very irritating sensation after use, and partial makeup residues still exist after cleaning, so that the double-layer multi-effect beading disclosed by the invention has better makeup removing effect and very fresh use sensation, is mild and has no irritation, and can be used for makeup removing and cleaning.

Test example 4 evaluation of moisturizing Effect

Skin moisture content test the moisture content of the skin was measured as a change in the capacitance of the stratum corneum of the skin using a Corneometer test probe (CourageKhazaka, germany) whose principle is based on the fact that the dielectric constant of water (81) is significantly different from that of other substances (< 7). In this experiment, the double-layered multi-effect beads prepared in examples 1 to 3, the double-layered beading cosmetics prepared in examples 10 to 13, comparative example 7 and comparative example 8 were tested to compare the change in skin moisture content of subjects before and after use, 20 subjects including 15 women and 5 men, and the average age was 28 years.

The specific method comprises the following steps: the subjects washed the forearms of both hands, sat in a humidity environment for 30min, and drawn out 3X 3cm from the left and right forearms²The test area of (1) was measured by using the left arm as the test area of the sample and the symmetrical area of the right arm as a blank control, measuring the moisture content of each test site with a Corneometer CM825 probe, repeating the procedure 5 times to obtain an average value, recording the data, and calculating the skin hydration rate at different time intervals according to the formula (1), with the results shown in table 9.

TABLE 9

Numbering	0h	1h	4h	8h
					Example 1	0.62	83.51	53.78	44.68
Example 2	0.61	82.75	54.55	45.25
					Example 3	0.61	83.65	55.32	44.18
Example 10	0.62	83.51	53.21	43.13
					Example 11	0.61	81.69	53.52	42.98
Example 12	0.62	81.22	56.26	45.54
					Example 13	0.63	81.13	56.88	45.12
Comparative example 7	0.60	50.36	35.17	21.36
					Comparative example 8	0.62	55.15	36.86	23.07

As can be seen from the data in Table 9, the skin of the subject still has high moisture content after 8 hours using the double-layer multi-effect beadlets prepared in examples 1-3 and examples 10-13, and the average hydration rate reaches over 42%, while the skin of the subject has an average hydration rate below 25% after 8 hours using the products of comparative examples 7 and 8, which indicates that the double-layer multi-effect beadlets of the present invention have good moisturizing effect.

Test example 5 particle diameter measurement

By using SZ-100 and based on a laser diffraction-scattering particle size distribution determination method, particle size characterization is carried out on the double-layer multi-effect beads prepared in examples 1-3, the double-layer multi-effect bead cosmetics prepared in examples 10-13, the comparative example 7 and the comparative example 8, and the results are shown in figures 3-11, wherein the particle size of the double-layer multi-effect bead micelle prepared by the invention is 8-100 nm, most of the double-layer multi-effect bead micelle is distributed around 10nm, even if the contents of the components in the formula are different, the particle size of the double-layer multi-effect bead micelle is not obviously changed, the double-layer multi-effect beads can be stably present in the system, in addition, the particle size distribution of the double-layer multi-effect beads prepared in examples 1-3 and the double-layer multi-effect bead cosmetics prepared in examples 10-13 is different from that of the comparative example 7 and the comparative example 8, and the particle size of the double-layer multi-effect beads prepared in examples 1-3 and the distribution is more concentrated, while the particle size distributions of comparative example 7 and comparative example 8 are more dispersed.

In summary, the invention provides a double-layer multi-effect coagulated bead and a preparation method and application thereof, and by optimizing components and process conditions, one layer of the double-layer multi-effect coagulated bead is a transparent solution, and the other layer is transparent or opaque coagulated bead particles, so that the double-layer multi-effect coagulated bead is novel in appearance and has multiple effects of makeup removal, moisture preservation and skin care.

The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims

1. A dual-layer multi-effect bead, comprising: surfactants, thickeners, polyols, skin conditioners, oils and water;

the thickening agent comprises any one or the combination of at least two of gellan gum, agarose or carrageenan;

(1) mixing a polyol, a surfactant, a thickener and water;

2. The dual-layer multi-effect beadlets of claim 1 wherein the surfactant comprises any one or a combination of at least two of decyl glucoside, lauryl glucoside, sodium lauryl glucarate, disodium cocoyl amphodiacetate, or potassium cocoyl hydrolyzed avenin;

preferably, the polyhydric alcohol comprises any one of glycerol, butanediol, propylene glycol, dipropylene glycol, 1, 2-hexanediol, 1, 2-pentanediol or 1, 3-propanediol or a combination of at least two thereof;

preferably, the skin conditioning agent comprises any one of or a combination of at least two of PEG-8 caprylic/capric glycerides, PEG-6 caprylic/capric glycerides, PEG-75 shea glycerides, or a glycine max seed extract;

preferably, the oil comprises any one or a combination of at least two of white oil, olive oil, cetyl ethylhexanoate, meadowfoam seed oil, isononyl isononanoate, glycerol tri (ethylhexanoate) or cyclopentadimethylsiloxane;

preferably, the raw materials for preparing the double-layer multi-effect coagulated bead also comprise a stabilizer;

preferably, the stabilizer comprises calcium chloride.

3. The dual-layer multi-effect bead according to claim 1 or 2, wherein the surfactant is present in the dual-layer multi-effect bead in a mass percentage of 0.10% to 5.00%, preferably 0.10% to 2.00%;

preferably, the mass percentage of the thickening agent in the double-layer multi-effect condensed bead is 0.05-1.00%, preferably 0.05-0.80%;

preferably, the mass percentage of the polyhydric alcohol in the double-layer multi-effect condensed bead is 1.00-20.00%, and preferably 1.00-15.00%;

preferably, the mass percentage of the stabilizer in the double-layer multi-effect condensed bead is 0.00-0.50%, preferably 0.01-0.20%;

preferably, the mass percentage of the skin conditioner in the double-layer multi-effect condensed bead is 0.01-5.00%, preferably 0.01-3.00%;

preferably, the mass percentage of the grease in the double-layer multi-effect condensation bead is 1.00-50.00%, and preferably 1.00-40.00%.

4. The dual-layer multieffect bead according to any one of claims 1-3, wherein the dual-layer multieffect bead comprises, in mass percent: 0.10-5.00% of surfactant, 0.05-1.00% of thickening agent, 1.00-20.00% of polyol, 0.00-0.50% of stabilizer, 0.01-5.00% of skin conditioner, 1.00-50.00% of grease and the balance of water;

5. A method of preparing the bilayer multieffect beading according to any one of claims 1-4, comprising the steps of:

(1) mixing a polyol, a surfactant, a thickener and water;

6. The method according to claim 5, wherein the mixing in the step (1), the step (2) and the step (3) is carried out by stirring;

preferably, the mixing temperature in the step (1) is 60-80 ℃;

preferably, the rotation speed of the mixing in the step (1) is 300-1500 rpm/min;

preferably, the mixing time in the step (1) is 1-10 min;

preferably, the mixing time in the step (2) is 1-10 min;

preferably, the standing and cooling in the step (2) is carried out to 20-40 ℃;

preferably, the time for smashing and mixing in the step (2) is 2-10 min;

preferably, the crushing and mixing in the step (2) are carried out at a rotating speed of 500-3000 rpm/min;

preferably, the mixing time in the step (3) is 1-5 min;

preferably, the rotation speed of the mixing in the step (3) is 100-1500 rpm/min.

7. The method for preparing according to claim 5 or 6, characterized in that the method comprises:

(2) adding a stabilizer and a skin conditioner, cooling to 40-60 ℃, stirring, mixing, defoaming, stirring at the rotating speed of 300-1500 rpm/min for 1-10 min, standing, cooling to 20-40 ℃, forming a solid gel, stirring, smashing, and mixing, wherein the stirring at the rotating speed of 500-3000 rpm/min, and the smashing and mixing time is 5-10 min;

8. Use of the dual-layer multi-effect beads according to any one of claims 1 to 4 for the preparation of a cosmetic product.

9. A cosmetic comprising the double-layered multi-effect bead of any one of claims 1 to 4;

10. The cosmetic according to claim 9, wherein the formulation of the cosmetic comprises any one of a water agent, an emulsion, a essence, a jelly, or a spray.