CN115919668A - Oil-coagulated bead composition stably existing in emulsifying system - Google Patents

Oil-coagulated bead composition stably existing in emulsifying system Download PDF

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CN115919668A
CN115919668A CN202211676533.2A CN202211676533A CN115919668A CN 115919668 A CN115919668 A CN 115919668A CN 202211676533 A CN202211676533 A CN 202211676533A CN 115919668 A CN115919668 A CN 115919668A
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oil
mass
phase
stirring
later use
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陈惟妙
冯春波
蒋昕楠
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Shanghai Jahwa United Co Ltd
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Shanghai Jahwa United Co Ltd
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Abstract

The invention discloses an oil coagulated bead composition stably existing in an emulsifying system, which comprises the following components in percentage by weight: (1) an aqueous base; and (2) oil globules dispersed in the aqueous matrix; wherein the aqueous base comprises a thickener, wherein the oil globules comprise one or more humectants, the humectants comprising C 16 ‑C 24 The saturated fatty alcohol according to (2), wherein the oil globule comprises a liquid oil, the liquid oil being a polar oil, wherein the oil globule composition comprises 1 to 10 wt.% of oil globules based on the total weight of the oil globule composition, wherein the weight ratio of the humectant to the liquid oil in the oil globule is 0.1 to 1. The invention also relates to a composition comprising said oil-binding beadAn emulsifying system and a preparation method thereof.

Description

Oil globule composition stable in emulsion system
Technical Field
The invention relates to the field of cosmetics, in particular to an oil coagulated bead composition stably existing in an emulsifying system.
Background
With the development of cosmetic formulation technology, dosage forms of skin care cosmetics added with particles are more and more popular with consumers, and the particles can be added with more active ingredients, so that the interestingness of use is brought to the consumers, and a new development direction is brought to the cosmetics. The particles in these products can be divided into two categories: 1. the cellulose-coated particles, such as vitamin c particles added in hand cream, adopt cellulose to coat vitamin c, maintain the stability of the vitamin c, are damaged in the coating process, and release nutrient substances; 2. oily particles, such as encapsulated oily particles added in the series of essences of Kaempferol, diao and the like, provide a very high-end appearance of the product and have the effects of moistening and moisturizing the skin.
However, both of the above-mentioned types of particles have limitations in use:
1) Cellulose-coated particles: the cellulose is hard and is difficult to be rapidly damaged in the smearing process, the experience of consumers is poor, and the content of active substances wrapped by the cellulose is very low, so that the efficacy of the granules is weak;
2) Oily particles, which are currently used in the market, are particles prepared and molded by raw material manufacturers, and the preparation process of the particles is very complex, the technology is not mature, so that the cost is high, and the oily particles are difficult to be used in a large amount in products. The particles prepared by the process are soft and need to be stored in liquid with a thickening suspension system, so that the uniformity of the particles is ensured, the whole suspension system mixed with oily particles is added into a finished product when the process is used, the operation difficulty is high, the skin feel is poor due to the introduction of a thickening agent, and the expected effect is difficult to achieve.
For example, chinese patent application CN201711457925 discloses a base composition containing suspended particles, which successfully produces oily particles using conventional cosmetic production equipment and raw materials, and studies the effect of thickener type, oil phase component ratio on oily particle stability, hardness, etc.
However, in practical application, the oil gel beads prepared by the method are difficult to apply to an emulsifying system containing an emulsifier, and researches show that the oil gel beads in the emulsifying formula containing the oil gel beads have the instability problems of whitening color, small size of the oil beads, reduced quantity and the like after the emulsifying formula is stored at 25 ℃ for 1 month and at 48 ℃ for 2 weeks. Further research shows that the unstable phenomenon is caused by the change of the component didodecanol in the oil condensation bead, the oil condensation bead is composed of behenyl alcohol and liquid grease, the oil condensation bead is liquid oil bead when the temperature exceeds 70 ℃, in the preparation process, the temperature is gradually reduced from 70 ℃ to room temperature, the behenyl alcohol in the liquid oil bead is gradually crystallized and solidified, and finally the oil condensation bead is generated. When the preparation of the oil coagulated beads is completed and the oil coagulated beads are added into a matrix containing certain emulsifiers, the behenyl alcohol in the oil coagulated beads is influenced by the emulsifiers and is recrystallized, and the behenyl alcohol gradually migrates to an interface and even migrates to a water phase, so that the oil coagulated beads are whitened in color, reduced in quantity and even disappear.
Thus, there remains a need in the art to find suitable techniques to improve the stability of oil globules in emulsified systems. The present inventors have surprisingly found that in an emulsified system, the oily particles produced in one piece by the oil phase can be individually stabilized in the emulsified formulation.
Disclosure of Invention
In one aspect, the present invention provides an oil beading composition stably existing in an emulsifying system, comprising:
(1) An aqueous base; and
(2) Oil-gelling beads dispersed in the aqueous matrix;
wherein the aqueous base comprises a thickening agent,
wherein the oil droplets comprise one or more humectants, the humectants comprising C 16 -C 24 The saturated fatty alcohol (a) of (b),
wherein the oil globules comprise liquid grease, the liquid grease being polar grease,
wherein the oil-gel bead composition comprises 1-10 wt.% of oil-gel beads based on the total weight of the oil-gel bead composition,
wherein the weight ratio of the humectant to the liquid oil in the oil condensate beads is 0.1-1.
In a preferred embodiment, the polar oil is selected from the group consisting of: pentaerythritol tetrakis (ethyl hexanoate), octyldodecanol, isopropyl palmitate, isopropyl myristate, or combinations thereof. In a preferred embodiment, the thickener is a polyacrylate thickener, more preferably an acrylic acid/C10-30 alkanol acrylate crosspolymer. In a preferred embodiment, the humectant comprises behenyl alcohol.
In another aspect, the present invention provides an emulsification system comprising: (1) an emulsion-type base; and (2) the oil-beading composition of the present invention, wherein the emulsification type base comprises an aqueous phase comprising an emulsifier and an oil phase comprising an oil, wherein the emulsification system comprises 10 to 50 wt% of the oil-beading composition.
In a preferred embodiment, the emulsifier is sucrose laurate. In a preferred embodiment, the aqueous phase further comprises a thickener. In a preferred embodiment, the emulsifying system comprises 0.5 to 2 weight percent pentaerythritol tetrakis (ethyl hexanoate) ester and 0.5 to 2 weight percent octyldodecanol. In a preferred embodiment, the emulsifying system comprises a combination of 2 to 2.5% by weight of octyldodecanol of pentaerythritol tetrakis (ethyl hexanoate) ester and 0.5% by weight or less of squalane.
In yet another aspect, the present invention provides a method of preparing an emulsification system comprising:
(i) Preparing an oil beading composition comprising:
(1a) Dispersing the thickener homogeneously in water to form an aqueous phase 1;
(1b) Mixing one or more humectants to a homogeneous liquid to form oil phase 1; and
(1c) Adding said oil phase 1 to said water phase 1 to form a desired oleogel composition;
(ii) Preparing an emulsified base comprising:
(2a) Dissolving an emulsifier and optionally a thickener in the aqueous phase to form aqueous phase 2;
(2b) Heating the grease to be transparent to form an oil phase 2; and
(2c) Adding the oil phase 2 into the water phase 2 to form a required emulsified matrix;
(iii) (iii) adding the oil globule composition of step (i) to the emulsified base of step (ii) to obtain the desired emulsified system.
In a preferred embodiment, the method further comprises adjusting the pH to between 5 and 7 after step (iii).
In yet another aspect, the present invention provides a formulation comprising the emulsifying system of the present invention.
Brief description of the drawings
Fig. 1 shows a photograph of the oil droplet stability index.
Fig. 2 shows the DSC curve of example 1.
Detailed Description
The invention surprisingly finds that the polarity of the liquid grease determines the long-term stability of the oil coagulated beads, the larger the polarity of the liquid grease, the better the compatibility with the behenyl alcohol, the more uniform the behenyl alcohol is when cooling and crystallizing, even if the behenyl alcohol is stored at 48 ℃, the crystallization is more uniform, and the oil coagulated beads with uneven and whitish crystallization are not easy to form. On the contrary, if the polarity of the liquid oil is low, the liquid oil has poor compatibility with the behenyl alcohol, the behenyl alcohol is unevenly distributed during cooling crystallization and is easily distributed on the surface of the oil condensation bead with high polarity, so that the oil condensation bead is whitened, and even after the liquid oil is stored at 48 ℃ for 2 weeks, the behenyl alcohol is recrystallized and gradually migrates to the water phase, and the phenomenon that the oil condensation bead disappears appears.
According to the invention, the liquid oil with different polarities is compatible with the behenyl alcohol, and the oil with better compatibility with the behenyl alcohol is found out, so that the behenyl alcohol is not easy to recrystallize and migrate in a system, and oil droplets containing the behenyl alcohol are stabilized and stably exist in an emulsifying system containing an emulsifying agent.
Specifically, the 12 liquid oils and fats are researched, and the invention unexpectedly finds that pentaerythritol tetra (ethyl hexanoate), octyldodecanol, isopropyl palmitate, isopropyl myristate and the like have better effects on stabilizing oil condensation beads.
Oil-gelled-bead composition
The present invention provides an oil globule composition stably present in an emulsification system, the oil globule composition comprising: an aqueous base and oil globules dispersed in the aqueous base.
In some examples of the invention, the aqueous matrix is a solid or semi-solid. In one or more examples, the aqueous matrix is a gel. In some embodiments, the matrix is a hydrogel. In one or more examples, the aqueous base comprises a thickening agent. In one or more examples, the thickener can be a natural (e.g., polysaccharides, etc.) or synthetic (e.g., polyacrylates, polyacrylamides, etc.) thickener. In one or more specific examples, the thickener is selected from TR-1, U21, U30, carbomer 980, AVC, ZEN, sepigel 305, sepiplus 400, gellan gum, or a combination of two or more thereof. In one or more preferred examples, the thickener is selected from TR-1, U21, U30, carbomer 980, AVC, ZEN, or a combination of two or more thereof. In a specific embodiment, the thickener is an acrylic acid/C10-30 alkanol acrylate crosspolymer.
In some examples of the invention, the oil coalescing beads comprise one or more humectants. In one or more examples, the oil gelling beads comprise an alcohol and/or lipid humectant. In one or more examples, the oil globules comprise C16-C24 saturated fatty alcohols. In some preferred examples, the oil globules comprise behenyl alcohol.
In one or more examples, the oil droplets further comprise one or more other humectants. In some embodiments, the one or more additional humectants can be selected from a lipid containing alkyl chain structure. In some embodiments, the one or more additional humectants can be selected from: cetyl/stearyl alcohol, white oil, olive oil, sunflower oil, squalane, jojoba esters, shea butter, silicone oil, or a combination of two or more thereof. In some embodiments, the one or more additional humectants are preferably selected from: white oil, olive oil, sunflower oil, squalane, or a combination of two or more thereof.
In some examples of the invention, the oil globules comprise liquid grease. In one or more examples, the oil globules comprise polar grease. In one or more examples, the polar grease is selected from: tri (ethyl hexanoate) glyceride, cetyl ethylhexanoate, pentaerythritol tetra (ethyl hexanoate), octyldodecanol, isopropyl palmitate, isopropyl myristate, caprylic/capric triglyceride, or combinations thereof. In a preferred embodiment, the polar oil is selected from: pentaerythritol tetrakis (ethyl hexanoate), octyldodecanol, isopropyl palmitate, isopropyl myristate, or combinations thereof.
In some examples of the invention, the oil globule composition comprises from 1 wt% to 10 wt% oil globules. In a preferred embodiment, the oil globule composition comprises from 1 wt% to 5 wt% oil globules.
In one or more examples, the weight ratio of humectant to liquid grease in the oil globules is between 0.1 and 1. In a preferred embodiment, the weight ratio of the humectant to the liquid oil or fat in the oil-gel beads is 0.1 to 0.2.
In some examples of the invention, the oil condensate beads may further comprise one or more efficacy additives. In other examples, one or more other humectants in the oil droplets are partially replaced by one or more efficacy additives. In one or more examples, the efficacy additive is present in an amount that does not exceed the amount of humectant present in the oil droplet. In some illustrative examples, the mass of the efficacy additive is no more than 95%, 90%, 85%, or 80% of the mass of the humectant contained in the oil gel bead. In some examples, the one or more performance additives are oil soluble performance additives. In one or more examples, the efficacy additive can be a cosmetic additive (e.g., a skin makeup additive, a hair cosmetic additive), a pharmaceutical additive, a food additive, or a combination of two or more thereof. Examples of the efficacy additive may include (but are not limited to): oil-soluble licorice, vitamin C tetraisopalmitate, vitamin E acetate, bisabolol, grape extract complex oil, tea seed oil, turmeric root extract, resveratrol, rhodiola rosea oil, safflower seed oil, ganoderma lucidum extract, indomethacin, methyl salicylate, colorless lycopene, or a combination of any two or more thereof.
In some embodiments of the invention, the oil droplets have a particle size in the range of 0.3 to 1 mm. In the present invention, "particles" and "microbeads" are used interchangeably and each means macroscopic particulate matter having a particle size in the millimeter or sub-millimeter range. By adjusting the type of the grease in the formula of the grease coagulated beads, the invention stabilizes grease microbeads with the diameter of 0.3-1mm in an emulsifying system containing an emulsifier and the grease.
Emulsification system comprising oil globule composition
The present invention provides an emulsification system comprising an oil globule composition, the emulsification system comprising an emulsification-type matrix and an oil globule composition.
In some examples of the invention, the emulsified base comprises an aqueous phase and an oil phase. In some examples, the aqueous phase comprises an emulsifier. In one or more embodiments of the present invention, the emulsifier is sucrose laurate. In some examples, the aqueous phase comprises a thickening agent. In one or more embodiments of the present invention, the thickener is polyacrylate crosspolymer-6. In some examples of the invention, the oil phase comprises a lipid. In one or more examples of the invention, the oil or fat comprises polydimethylsiloxane, glycerol tri (ethylhexanoate), or a combination thereof. In some examples of the invention, the emulsified base comprises 1-5 wt% of an oil phase.
In some examples of the invention, the emulsification system comprises 10 to 50 wt% of the oil globule composition. In a preferred embodiment, the emulsification system comprises 20 to 40 wt% of the oil globule composition. In a most preferred embodiment, the emulsification system comprises 30 to 35 wt% of the oil globule composition.
In some examples of the invention, the emulsification system comprises 0.5 to 2 weight percent pentaerythritol tetrakis (ethyl hexanoate) ester and 0.5 to 2 weight percent octyldodecanol, based on the total weight of the emulsification system.
In some examples of the invention, the emulsification system comprises a combination of 2 to 2.5 weight percent octyldodecanol of pentaerythritol tetrakis (ethyl hexanoate) ester and equal to or less than 0.5 weight percent squalane, based on the total weight of the emulsification system.
Preparation of the emulsifying SystemMethod
The present invention provides a method of preparing an emulsification system comprising:
(i) Preparing an oil droplet composition;
(ii) Preparing an emulsion type matrix;
(iii) (iii) adding the oil globule composition of step (i) to the emulsified base of step (ii) to obtain the desired emulsified system.
In some embodiments of the invention, the invention provides a method of making an oil beading composition, comprising:
(1a) Dispersing the thickener homogeneously in water to form an aqueous phase 1;
(1b) Mixing one or more humectants to a homogeneous liquid to form oil phase 1; and
(1c) The desired oleogel composition is formed by adding the above oil phase 1 to the above water phase 1.
In one or more examples, in step (1 a), the thickener dispersed in water is warmed to a temperature greater than 70 ℃, e.g., 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, or a range formed by endpoints of any two of the foregoing. In some embodiments, the water used in step (1 a) is purified water, distilled water, preferably deionized water. In some examples, the dispersing in step (1 a) is performed with stirring or shaking.
In one or more examples, the mixing in step (1 b) is performed at a temperature greater than 70 ℃, e.g., 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, or a range formed by endpoints of any two of the foregoing. In some examples, the one or more humectants include alcohol and/or lipid humectants. In some examples, the one or more humectants include C16-C24 saturated fatty alcohols. In some preferred examples, the one or more humectants include behenyl alcohol. In some examples, one or more other humectants are also employed. In some embodiments, the one or more additional humectants can be selected from: cetyl/stearyl alcohol, white oil, olive oil, sunflower oil, squalane, jojoba esters, shea butter, silicone oil, or a combination of two or more thereof. In some preferred examples, the one or more additional humectants are selected from: white oil, olive oil, sunflower oil, squalane, or a combination of two or more thereof. In some examples, the mixing in step (1 b) is performed with stirring or shaking.
In one or more functional examples, one or more performance additives are further added in step (1 b) and mixed with the one or more humectants to form an oil phase. In some examples, one or more efficacy additives are added to partially replace one or more other humectants in the oil phase. In one or more examples, the quality of the efficacy additive does not exceed the quality of the humectant contained in the oil phase. In some illustrative examples, the mass of the efficacy additive does not exceed 95%, 90%, 85%, or 80% of the mass of the humectant contained in the oil phase. In some examples, the one or more performance additives are oil soluble performance additives. In one or more embodiments, the efficacy additive can be a cosmetic additive (e.g., a skin makeup additive, a hair cosmetic additive), a pharmaceutical additive, a food additive, or a combination of two or more thereof. Examples of the efficacy additive may include (but are not limited to): oil-soluble licorice, vitamin C tetraisopalmitate, vitamin E acetate, bisabolol, grape extract complex oil, tea seed oil, turmeric root extract, resveratrol, rhodiola rosea oil, safflower seed oil, ganoderma lucidum extract, indomethacin, methyl salicylate, colorless lycopene, or a combination of any two or more thereof.
In one or more examples, step (1 c) comprises adding the oil phase to the aqueous phase with stirring to obtain a dispersion. In one or more examples, the agitation is at a speed of 200 to 600RPM, for example, 250 to 550RPM, 300 to 500RPM, 350 to 450 RPM. In one or more examples, the stirring is continued for more than 5 minutes, e.g., more than 8 minutes, more than 10 minutes. In one or more examples, the stirring in step (1 c) is performed at a temperature greater than 70 ℃, e.g., 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, or a range formed by any two of the foregoing values as endpoints. In one or more examples, step (1 c) further comprises cooling the dispersion to room temperature. In some examples, the dispersion obtained as described above is allowed to stand to cool to room temperature. In one or more examples, the dispersion is allowed to stand to cool until a solid or semi-solid matrix having oil globules dispersed therein is obtained. In one or more examples, the dispersion is placed into a corresponding container (e.g., a container having a desired shape or desired composition) and subsequently cooled to obtain a solid or semi-solid matrix having oil globules dispersed therein.
In some embodiments of the invention, the invention provides a method of making an emulsified base comprising:
(2a) Dissolving an emulsifier and a thickener in an aqueous phase to form an aqueous phase 2;
(2b) Heating the grease to be transparent to form an oil phase 2; and
(2c) The oil phase 2 is added to the water phase 2 to form the desired emulsion-type base.
In one or more examples, step (2 a) is performed at a temperature equal to or greater than 70 ℃, e.g., 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, or a range formed by endpoints of any two of the foregoing. In some embodiments, the water used in step (2 a) is purified water, distilled water, preferably deionized water. In some examples, step (2 a) is performed with stirring or shaking.
In one or more examples, step (2 b) is performed at a temperature equal to or greater than 70 ℃, e.g., 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, or a range formed by any two of the foregoing values as endpoints. In some examples, step (2 b) is performed with stirring or shaking.
In one or more examples, step (2 c) comprises the addition of oil phase 2 to water phase 2 under homogeneous conditions. In one or more examples, the homogenization conditions last equal to or greater than 5 minutes, e.g., equal to or greater than 8 minutes, equal to or greater than 10 minutes. In one or more examples, step (2 c) further comprises cooling to room temperature to form an emulsion-type matrix.
In some embodiments of the invention, the prepared oil bead composition is added to the prepared emulsified base to provide the desired emulsified system. In one or more preferred embodiments, the method of preparing an emulsification system of the present invention further comprises: a step of adjusting the pH after adding the oil globule composition to the emulsion type base. In some examples, tromethamine is used to adjust the pH of the emulsification system. In some examples, the pH of the emulsification system is adjusted to between 5 and 7.
Formulations containing an emulsifying system
The present invention provides formulations comprising the above-described emulsifying system. In some examples, the formulation can be a cosmetic formulation (e.g., a skin makeup formulation, a hair cosmetic formulation), a pharmaceutical formulation, a food formulation, or a combination of two or more thereof. In one or more examples, the formulation may be in a semi-solid or solid form. In one or more examples, the formulation may also include other additives such as, but not limited to, pigments, flavors, fragrances, and the like.
Use of an emulsifying system comprising an oil beading composition
The invention also provides the use of the above-described suspension oil globule-containing matrix composition in cosmetic products, pharmaceuticals and/or food products.
Examples
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Those skilled in the art can make appropriate modifications and alterations to the present invention, which fall within the scope of the invention.
Unless otherwise indicated, percentages and parts are by weight. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
Experimental Material
The raw materials and sources used in the present invention are as follows:
Figure BDA0004017156970000101
Figure BDA0004017156970000111
laboratory apparatus
The following instruments are mainly adopted in the following embodiments of the invention:
1. a fixed agitator IKA RW20;
2. HWS 28 model of constant temperature water bath Shanghai-Hengscientific instruments Co., ltd;
3. a weighing balance METTLER TOLEDO PL602-S;
DSC thermal differential analyzer
5. Viscometer Brookfield RVDV-C
6. Wet film preparation apparatus, 1 micron height
Experimental process
The oil globule composition can be prepared by the following process:
dispersing the thickener homogeneously in water and subsequently heating to a temperature above 70 ℃ to form an aqueous phase 1;
mixing one or more humectants at a temperature above 70 ℃ to a homogeneous liquid to form an oil phase 1;
the oil phase 1 was added to the water phase 1, stirring was continued to obtain a homogeneous dispersion, and the mixture was cooled to room temperature with stirring.
The preparation process of the matrix containing the emulsifier comprises the following steps:
dissolving emulsifier and thickener, etc. in water phase at 70 deg.C to form water phase 2;
heating the grease to 70 ℃ until the grease is transparent to form an oil phase 2;
adding the water phase 2 into the oil phase 2 under the condition of homogenization, homogenizing for 10 minutes, and cooling to room temperature to form an emulsified matrix.
The preparation process of the cream containing the oil condensation beads comprises the following steps:
adding the oil bead composition into an emulsion type matrix, uniformly mixing, adding tromethamine, and uniformly stirring.
Examples 1 to 6
Figure BDA0004017156970000121
Example 1: oil phase component-behenyl alcohol, glycerol tri (ethyl hexanoate)
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of glycerol tri (ethyl hexanoate) and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 2: oil phase Components-behenyl alcohol, cetyl Ethyl hexanoate
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of cetyl ethyl hexanoate and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 3: oil phase component-behenyl alcohol, pentaerythritol tetra (ethyl hexanoate)
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of pentaerythritol tetra (ethyl hexanoate) and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 4: oil phase component-behenyl alcohol, octyl dodecanol
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of octyldodecanol and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 5: oil phase components-behenyl alcohol, isopropyl palmitate
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of isopropyl palmitate and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 6: oil phase components-behenyl alcohol, isopropyl myristate
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of isopropyl myristate and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative examples 1 to 6 formulations
Figure BDA0004017156970000161
Comparative example 1: oil phase component-behenyl alcohol, squalane
Weighing 0.4 parts by mass of behenyl alcohol and 2.5 parts by mass of squalane, 0.00006 parts by mass of CI61650, uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 2: oil phase component-behenyl alcohol, dioctyl carbonate
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of dioctyl carbonate and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 3: oil phase component-behenyl alcohol, mineral oil
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of mineral oil and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 4: oil phase Components-behenyl alcohol, cetyl Ethyl hexanoate
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of cetyl ethyl hexanoate and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 5: oil phase component-behenyl alcohol, olive fruit oil
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of olive fruit oil and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 6: oil phase component-behenyl alcohol, sunflower seed oil
Weighing 0.4 part by mass of behenyl alcohol, 2.5 parts by mass of sunflower seed oil and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotation speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to obtain a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Test example 1: viscosity test, oil bead tensile film stability test, DSC thermal difference analysis test
And (3) viscosity testing: the viscosity change of the sample after standing stability was measured by a Brookfield RVDV-C viscosity tester, and the viscosity change ratio was calculated. If the viscosity is obviously increased, the fact that the behenyl alcohol migrates to the water phase is proved, the viscosity of the continuous phase is improved by recrystallization of the water phase, and the comparison with an oil drop sample shows that when the viscosity is increased by less than 10%, the shape and the color stability of the oil drop are better, and the oil drop is judged to be 'V'; when the viscosity increased by more than 10%, the oil globule morphology was poor, and it was judged to be "x".
Testing the stability of the oil drop stretched film: taking 2g of sample, placing the sample in a film drawing die, pulling down the sample on a black paper card at a constant speed to form a film with the thickness of 1mm, standing for 48 hours, volatilizing moisture of the face cream to form a transparent phase, uniformly distributing oil droplets on the black paper, observing the quantity and color of the oil droplets on a fixed area, and evaluating the stability of the oil droplets in a system, wherein the more the quantity of the oil droplets in the same area is, the more the color is, and the better the stability of the system is. The stability evaluation criteria were set as follows:
oil droplet stability index 5: the number of oil globules was reduced by <10%, the oil globules were blue;
oil droplet stability index 4:10% < the number of oil globules decreased by <20%, the oil globules were blue;
oil droplet stability index 3: the number of oil globules is reduced by less than 30%, the oil globules are white;
oil droplet stability index 2: the number of oil globules is reduced by less than 50%, the oil globules are white;
oil droplet stability index 1: the number of oil globules is reduced by less than 70%, the oil globules are white;
oil droplet stability index 0: substantially free of visible oil globules.
Fig. 1 shows a photograph of the oil droplet stability index.
The stability index is above 3, and the product is judged to be qualified.
Oil drop DSC test: taking 20g of a sample, placing the sample in a screen, washing the sample with deionized water for 5 minutes, screening out oil drop particles, placing the sample in an oven for drying for 24 hours, taking 0.01g of dried oil drop for DSC test, and setting the temperature as follows: and (3) raising the temperature from 25 ℃ to 100 ℃ at 15 ℃/min, then reducing the temperature to 25 ℃ at 10 ℃/min, analyzing the change of the phase transition temperature after the oil drop is placed and stabilized, comparing the DSC temperature reduction crystallization peak just after the preparation of the sample and the position change of the crystallization peak after the sample is placed and placed at 48 ℃ for 2 weeks, and if the temperature difference of the crystallization peak is less than 10 ℃, laterally proving that the crystallization of the behenyl alcohol is less changed, the oil drop is more stable, and marking as &. If the change is more than 10 ℃, it is indicated that the crystallization and position of behenyl alcohol in the oil globule structure are changed, and the stability of the oil globule is reflected laterally to be poor, and is evaluated as "Δ". As shown in the DSC curve of fig. 2, the DSC crystallization peak of example 1 varied from 58 ℃ to 66 ℃, with a variation of less than 10 ℃, evaluated as o.
TABLE 1
Figure BDA0004017156970000211
From the test results, it was found that the stability of oil droplets formed by behenyl alcohol and different liquid greases showed differences in the emulsified system, wherein: the oil globule has the best stability when being compatible with pentaerythritol tetra (ethyl hexanoate) and octyl dodecanol, and the oil globule is formed through stability investigation when being compatible with isopropyl palmitate and isopropyl myristate; the oil beads formed by the compatibility of the oil beads with squalane, dioctyl carbonate, mineral oil, cetyl ethyl hexanoate, olive oil and sunflower seed oil do not pass stability investigation.
These experiments prove that the behenyl alcohol has good crystallization stability when being compatible with liquid oil with higher polarity, and the phenomenon of instability of recrystallization, oil bead whitening and disappearance is not easy to occur in the stability period.
Examples 7 to 11
Figure BDA0004017156970000221
Example 7: oil phase components-behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester, glycerol tri (ethyl hexanoate)
Weighing 0.4 part by mass of behenyl alcohol, 2 parts by mass of pentaerythritol tetra (ethyl hexanoate), 1 part by mass of glycerol tri (ethyl hexanoate) and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 8: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol
Weighing 0.4 mass part of behenyl alcohol, 2 mass parts of pentaerythritol tetra (ethyl hexanoate), 1 mass part of octyl dodecanol and 0.00006 mass part of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotation speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to obtain a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 9: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and isopropyl palmitate
Weighing 0.4 mass part of behenyl alcohol, 2 mass parts of pentaerythritol tetra (ethyl hexanoate), 1 mass part of isopropyl palmitate and 0.00006 mass part of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 10: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester, isopropyl myristate
Weighing 0.4 mass part of behenyl alcohol, 2 mass parts of pentaerythritol tetra (ethyl hexanoate), 1 mass part of isopropyl myristate and 0.00006 mass part of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 11: oil phase Components-Twenediol, pentaerythritol Tetrakis (ethylhexanoate), caprylic/capric triglyceride
Weighing 0.4 part by mass of behenyl alcohol, 2 parts by mass of pentaerythritol tetra (ethyl hexanoate), 1 part by mass of caprylic/capric triglyceride and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Examples 12 to 16
Figure BDA0004017156970000251
Figure BDA0004017156970000261
Example 12: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol
Weighing 0.4 part by mass of behenyl alcohol, 2 parts by mass of pentaerythritol tetra (ethyl hexanoate), 0.5 part by mass of octyldodecanol and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 13: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol
Weighing 0.4 mass part of behenyl alcohol, 1.5 mass parts of pentaerythritol tetra (ethyl hexanoate), 1 mass part of octyl dodecanol and 0.00006 mass part of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 14: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol
Weighing 0.4 part by mass of behenyl alcohol, 1.25 parts by mass of pentaerythritol tetra (ethyl hexanoate), 1.25 parts by mass of octyldodecanol and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 15: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol
Weighing 0.4 part by mass of behenyl alcohol, 1 part by mass of pentaerythritol tetra (ethyl hexanoate), 1.5 parts by mass of octyl dodecanol and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 16: oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol
Weighing 0.4 mass part of behenyl alcohol, 0.5 mass part of pentaerythritol tetra (ethyl hexanoate), 2 mass part of octyl dodecanol and 0.00006 mass part of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Examples of the embodiments 17-21
Figure BDA0004017156970000291
Example 17: the oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester, octyldodecanol and squalane
Weighing 0.4 part by mass of behenyl alcohol, 1 part by mass of pentaerythritol tetra (ethyl hexanoate), 1 part by mass of octyldodecanol, 0.5 part by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 18: the oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate), octyl dodecanol and squalane
Weighing 0.4 part by mass of behenyl alcohol, 1.2 parts by mass of pentaerythritol tetra (ethyl hexanoate), 0.8 part by mass of octyldodecanol, 0.5 part by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 19: the oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate), octyl dodecanol and squalane
Weighing 0.4 part by mass of behenyl alcohol, 1 part by mass of pentaerythritol tetra (ethyl hexanoate), 0.8 part by mass of octyldodecanol, 0.7 part by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 20: the oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate), octyl dodecanol and squalane
Weighing 0.4 part by mass of behenyl alcohol, 0.8 part by mass of pentaerythritol tetra (ethyl hexanoate), 1 part by mass of octyldodecanol, 0.7 part by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Example 21: the oil phase components of behenyl alcohol, pentaerythritol tetra (ethyl hexanoate) ester, octyldodecanol and squalane
Weighing 0.4 part by mass of behenyl alcohol, 1 part by mass of pentaerythritol tetra (ethyl hexanoate), 0.5 part by mass of octyldodecanol, 1 part by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative examples 7 to 11 formulations
Figure BDA0004017156970000321
Figure BDA0004017156970000331
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Comparative example 7: the oil phase components of behenyl alcohol, mineral oil, caprylic/capric triglyceride, squalane
Weighing 0.4 part by mass of behenyl alcohol, 0.5 part by mass of pentaerythritol tetra (ethyl hexanoate), 0.5 part by mass of octyl dodecanol, 2 parts by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 8: the oil phase components of behenyl alcohol, mineral oil, caprylic/capric triglyceride, squalane
Weighing 0.4 part by mass of behenyl alcohol, 0.3 part by mass of pentaerythritol tetra (ethyl hexanoate), 0.7 part by mass of octyl dodecanol, 2 parts by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 9: the oil phase components of behenyl alcohol, mineral oil, caprylic/capric triglyceride, squalane
Weighing 0.4 part by mass of behenyl alcohol, 0.5 part by mass of pentaerythritol tetra (ethyl hexanoate), 1 part by mass of octyl dodecanol, 1.5 parts by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotation speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to obtain a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 10: the oil phase components of behenyl alcohol, mineral oil, caprylic/capric triglyceride, squalane
Weighing 0.4 part by mass of behenyl alcohol, 0.3 part by mass of pentaerythritol tetra (ethyl hexanoate), 1.2 parts by mass of octyldodecanol, 1.5 parts by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotation speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to obtain a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Comparative example 11: the oil phase components of behenyl alcohol, mineral oil, caprylic/capric triglyceride, squalane
Weighing 0.4 part by mass of behenyl alcohol, 0.2 part by mass of pentaerythritol tetra (ethyl hexanoate), 1.3 parts by mass of octyl dodecanol, 1.5 parts by mass of squalane and 0.00006 part by mass of CI61650, and uniformly mixing at 70 ℃ until transparent liquid is used as an oil phase 1 for later use; weighing 30.00 parts by mass of deionized water, adding 0.40 part by mass of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, uniformly dispersing, and heating to 70 ℃ to serve as a water phase 1 for later use; adding the oil phase 1 into the water phase 1 under stirring, keeping stirring for 10 minutes at the rotating speed of 400RPM, stirring to form oil droplets, and cooling to room temperature to be used as a mixed phase 1 for later use; weighing 1 part by mass of polydimethylsiloxane and 2 parts by mass of glycerol tri (ethyl hexanoate), uniformly mixing, and heating to 70 ℃ to be transparent to serve as an oil phase 2 for later use; weighing 0.5 mass part of sucrose laurate and 0.5 mass part of polyacrylate crosslinked polymer-6, adding 60 mass parts of deionized water, heating to 70 ℃ to uniformly disperse the mixture to form a water phase 2 for later use, adding the oil phase 2 into the water phase 2 under the homogenizing condition, keeping the homogenization for 10 minutes, cooling to room temperature to form a mixed phase 2 for later use, adding the mixed phase 2 into a mixed phase 1 under the stirring condition, stirring for 2 minutes until oil beads are uniformly dispersed, dissolving tromethamine containing 0.2 mass part, adding the mixture into the mixture of the mixed phase 1+2, stirring for 10 minutes, and discharging.
Test example 2: viscosity test, oil bead tensile film stability test, DSC thermal difference analysis test
And (3) viscosity testing: the viscosity change of the sample after standing stability was measured by a Brookfield RVDV-C viscosity tester, and the viscosity change ratio was calculated. If the viscosity is obviously increased, the fact that the behenyl alcohol migrates to the water phase is proved, the viscosity of the continuous phase is improved by recrystallization of the water phase, and the comparison with an oil drop sample shows that when the viscosity is increased by less than 10%, the shape and the color stability of the oil drop are better, and the oil drop is judged to be 'V'; when the viscosity increased by more than 10%, the oil globule morphology was poor, and it was judged to be "x".
Testing the stability of the oil drop stretched film: taking 2g of sample, placing the sample in a film drawing die, pulling down the sample on a black paper card at a constant speed to form a film with the thickness of 1mm, standing for 48 hours, volatilizing moisture of the face cream to form a transparent phase, uniformly distributing oil droplets on the black paper, observing the quantity and color of the oil droplets on a fixed area, and evaluating the stability of the oil droplets in a system, wherein the more the quantity of the oil droplets in the same area is, the more the color is, and the better the stability of the system is. The stability evaluation criteria were set as follows:
oil droplet stability index 5: the number of oil globules was reduced by <10%, the oil globules were blue;
oil droplet stability index 4:10% < the number of oil globules decreased by <20%, the oil globules were blue;
oil droplet stability index 3: the number of oil globules is reduced by less than 30%, the oil globules are white;
oil droplet stability index 2: the number of oil globules is reduced by less than 50%, the oil globules are white;
oil droplet stability index 1: the quantity of oil droplets is reduced by less than 70 percent, and the oil droplets are white;
oil droplet stability index 0: substantially free of visible oil globules.
The stability index is above 3, and the product is judged to be qualified.
Oil drop DSC test: taking 20g of a sample, placing the sample in a screen, washing the sample with deionized water for 5 minutes, screening out oil drop particles, placing the sample in an oven for drying for 24 hours, taking 0.01g of dried oil drop for DSC test, and setting the temperature as follows: and (3) raising the temperature from 25 ℃ to 100 ℃ at a speed of 15 ℃/min, then lowering the temperature to 25 ℃ at a speed of 10 ℃/min, analyzing the change of the phase transition temperature after the oil drop is placed and stable, and comparing the DSC temperature-lowering crystallization peak when the sample is just prepared with the position change of the crystallization peak after the sample is placed at 48 ℃ for 2 weeks. If the crystallization peak temperature difference is less than 10 ℃, the side surface proves that the crystallization change of the behenyl alcohol is small, the oil drop is stable, and is marked as o; if the change is more than 10 ℃, it is indicated that the crystallization and position of behenyl alcohol in the oil globule structure are changed, and the stability of the oil globule is reflected laterally to be poor, and is evaluated as "Δ".
TABLE 2
Figure BDA0004017156970000361
Figure BDA0004017156970000371
From the results of examples 7-11, it was found that different combinations of fats and oils have different effects on the stability of oil droplets, with the proviso that behenyl alcohol and pentaerythritol tetra (ethyl hexanoate) ester are fixed, wherein: pentaerythritol tetra (ethyl hexanoate) ester and octyl dodecanol are the best in matching stability, and are better than isopropyl palmitate and isopropyl myristate, and stability is examined. However, the collocation with caprylic/capric triglyceride failed stability studies.
From the results of examples 12 to 16, it was found that the compatibility between pentaerythritol tetra (ethyl hexanoate) 0.5% and 2% and octyl dodecanol 0.5% and 2% were good and the oil drop stability was high.
From the results of examples 17 to 21, it was found that when pentaerythritol tetrakis (ethyl hexanoate) ester, octyldodecanol and squalane were combined, the oil droplet stability passed when the total amount of pentaerythritol tetrakis (ethyl hexanoate) ester and octyldodecanol was more than 2% to 2.5% and the squalane content was 0.5% or less; when the total amount of pentaerythritol tetra (ethyl hexanoate) and octyl dodecanol is less than 2 percent and the squalane accounts for 0.7 to 1 percent, the oil drop stability is not passed.
The preparations of examples 1 to 21 and the like were used for the preparation of external preparations for skin. The skin external preparation is preferably a cosmetic composition such as essence, cream, etc. The weight percentage of the mixture in the skin external preparation is 1-100% (w/w). The preferred weight percentage is 20% to 100% (w/w). More preferably 30% to 90% (w/w). The most preferred weight percentage is 50% to 90% (w/w).
The following are examples of specific applications of the preparations in skin external preparations, and formulations and preparation methods of these dosage forms. In the tables, "-" indicates no addition.
Example 22: preparation of face cream
Figure BDA0004017156970000381
Example 23: preparation of the emulsion
Figure BDA0004017156970000382
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Figure BDA0004017156970000391
Example 24: preparation of jelly
Figure BDA0004017156970000392
Example 25: preparation of essence
Figure BDA0004017156970000401
Example 26: preparation of facial mask
Figure BDA0004017156970000402
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Figure BDA0004017156970000411
Example 27: preparation of eye cream
Figure BDA0004017156970000412
It will be appreciated that various alterations and modifications of the invention will occur to those skilled in the art upon reading the above teachings, and that such equivalents are intended to fall within the scope of the invention as defined by the appended claims.

Claims (14)

1. An oil beading composition stabilized in an emulsifying system, comprising:
(1) An aqueous base; and
(2) Oil-gelling beads dispersed in the aqueous matrix;
wherein the aqueous base comprises a thickening agent,
wherein the oil droplets comprise one or more humectants, the humectants comprising C 16 -C 24 The saturated fatty alcohol (a) of (b),
wherein the oil globules comprise liquid grease, the liquid grease being polar grease,
wherein the oil-gel bead composition comprises 1-10 wt.% of oil-gel beads based on the total weight of the oil-gel bead composition,
wherein the weight ratio of the humectant to the liquid oil in the oil condensate beads is 0.1-1.
2. The oil beading composition of claim 1 wherein the polar grease is selected from the group consisting of: pentaerythritol tetrakis (ethyl hexanoate), octyldodecanol, isopropyl palmitate, isopropyl myristate, or combinations thereof.
3. The oil gelling bead composition of claim 1, wherein the thickener is a polyacrylate thickener.
4. The oil gelling bead composition of claim 3, wherein the thickener is an acrylic acid/C10-30 alkanol acrylate crosspolymer.
5. The oil coalescing composition of claim 1, wherein the humectant comprises behenyl alcohol.
6. The oil beading composition according to claim 1 wherein the grease beads further comprise one or more efficacy additives.
7. An emulsification system comprising:
(1) An emulsion-type base; and
(2) The oil beading composition according to any one of claims 1 to 6,
wherein the emulsified base comprises an aqueous phase and an oil phase, the aqueous phase comprises an emulsifier, and the oil phase comprises an oil,
wherein the emulsification system comprises 10-50 wt% of the oil globule composition.
8. The emulsification system of claim 7, wherein the emulsifier is sucrose laurate.
9. The emulsification system of claim 7, wherein the aqueous phase further comprises a thickener.
10. The emulsifying system of claim 7, wherein the emulsifying system comprises 0.5-2% by weight pentaerythritol tetrakis (ethyl hexanoate) and 0.5-2% by weight octyldodecanol.
11. The emulsification system of claim 7, wherein the emulsification system comprises a combination of 2-2.5 wt% octyldodecanol of pentaerythritol tetrakis (ethyl hexanoate) ester and 0.5 wt% or less squalane.
12. A method of making the emulsification system of any one of claims 7-11 comprising:
(i) Preparing an oil beading composition comprising:
(1a) Dispersing the thickener homogeneously in water to form an aqueous phase 1;
(1b) Mixing one or more humectants to a homogeneous liquid to form oil phase 1; and
(1c) Adding said oil phase 1 to said water phase 1 to form a desired oil gel composition;
(ii) Preparing an emulsified base comprising:
(2a) Dissolving an emulsifier and optionally a thickener in the aqueous phase to form aqueous phase 2;
(2b) Heating the grease to be transparent to form an oil phase 2; and
(2c) Adding the oil phase 2 into the water phase 2 to form a required emulsified matrix;
(iii) (iii) adding the oil globule composition of step (i) to the emulsified base of step (ii) to obtain the desired emulsified system.
13. The method of claim 12, wherein the method further comprises adjusting the pH to between 5 and 7 after step (iii).
14. A formulation comprising the emulsification system of any one of claims 7-11.
CN202211676533.2A 2022-12-26 2022-12-26 Oil-coagulated bead composition stably existing in emulsifying system Pending CN115919668A (en)

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