WO2023128617A1 - Oil drop cosmetic composition having excellent stability, and preparation method therefor - Google Patents

Abstract

The present invention relates to: a cosmetic composition containing, in a continuous aqueous phase, oil drops; and a preparation method therefor, and according to the present invention, provided is a cosmetic composition in which oil drops form a stable dispersed phase in a continuous aqueous phase even without a surfactant, and thus provide a differentiated appearance.

Description

Oil drop cosmetic composition having excellent stability and manufacturing method thereof

The present invention relates to a cosmetic composition comprising oil drops in a continuous phase, which is an aqueous phase, and a method for preparing the same. Specifically, it relates to a cosmetic composition having a differentiated appearance by forming a stable dispersed phase in the continuous phase, which is an aqueous phase, without including a surfactant, and a method for manufacturing the same.

Recently, with the rise of functional cosmetics in the cosmetic market, demand for visual aesthetics and differentiated feeling of use is increasing. Reflecting this emotional demand, attempts have been made to provide users with visual enjoyment, aesthetic sensibility, and cosmetic pleasure by modifying the unique shape, color, or texture of a bead formulation.

Traditional cosmetic compositions are provided in formulations such as skin, toner, lotion, and cream, but interest in oil drops is increasing to provide a new texture, visual differentiation, and new aesthetic sensibility when applied to the skin. However, since the size of the oil drop is at least 10 μm or more, it is difficult to ensure colloidal stability, and various process variables exist such as the difference in refractive index between the oil phase and the aqueous phase must be considered in order to maintain a translucent phase.

In particular, in cosmetic compositions, oil has only a difference in content and is widely used in most products, but surfactants have been added to solve the disadvantages of feeling of use such as oil shine and to have the stability of emulsion formulations. However, synthetic surfactants are limited in use in products as skin safety becomes increasingly important, and development of new surfactant-free cosmetic compositions is required according to skin irritation concerns and consumer avoidance.

In response to this demand, Prior Art 1 discloses a cosmetic composition containing spherical droplets in which oil is present in a spherical form in an aqueous alcohol solution by dispersing oil in an aqueous alcohol solution using an appropriate powder without using a surfactant. However, prior art 1 has a problem of skin safety caused by aluminum using aluminum oxide powder, and has a limitation that it cannot be applied to users who do not prefer alcohol because it contains a large amount of alcohol.

Prior Art 2 discloses spherical droplets dispersed in an oil phase, and uses a silicone elastomer and a silicone-based surfactant to stabilize the spherical droplets. However, prior art 2 has a limitation that it cannot be applied to a product group that does not contain a surfactant because it uses a silicone-based synthetic surfactant to stabilize the droplet.

Therefore, it is necessary to develop a novel cosmetic composition that includes spherical liquid droplets (oil droplets) having a particle size of at least 10 μm or more without using a surfactant, and has excellent colloidal stability and a transparent or translucent phase.

An object of the present disclosure is to provide a novel oil drop composition having excellent colloidal stability, transparent or translucent, including oil droplets of at least 10 μm or more without using a surfactant, and a manufacturing method thereof.

The present invention is a composition comprising oil drops having an average particle diameter of 10 to 1000 μm in an aqueous phase, which is a continuous phase, wherein the oil phase includes a hydrophobic polymer and oil, and the aqueous phase includes an acrylic acid-based polymer and water, The viscosity of the water phase (η _w ) and the viscosity of the oil phase (η _o ) satisfy Equation 1 below.

[Equation 1]

log(η _o ) < alog(η _w )+b

In Equation 1, a is 1 to 1.18 and b has a value of 0.8 or less.

In one example of the present invention, the viscosity of the aqueous phase (η _w ) and the viscosity of the oil phase (η _o ) may further satisfy Equation 2 below.

[Equation 2]

log(η _o ) > clog(η _w )+d

In Equation 2, c is 5.5 to 5.8 and d has a value of -17 or more.

In one example of the present invention, the viscosity of the aqueous phase may be 200 cP or more.

In one example of the present invention, the viscosity of the oil phase may be 50000 cP or less.

In one example of the present invention, the acrylic acid-based polymer may be a crosspolymer of (meth)acrylic acid and C10-C30 alkyl (meth)acrylate.

In one example of the present invention, the hydrophobic polymer may be a siloxane-based polymer or a siloxane-based copolymer.

In one example of the present invention, based on 100 parts by weight of the acrylic acid-based polymer, the hydrophobic polymer may be included in 100 to 2000 parts by weight.

In one example of the present invention, a C4-C16 trihydric to pentahydric alcohol may be further included.

In one example of the present invention, a surfactant for emulsifying the aqueous phase and the oil phase may not be substantially included.

The present invention comprises the steps of preparing an aqueous phase containing an acrylic acid-based polymer, a basic compound and water; preparing an oil phase containing a hydrophobic polymer and an oil; And mixing the aqueous phase and the oil phase to prepare a composition in which an oil phase, which is a dispersed phase, is distributed in an oil drop form in an aqueous phase, which is a continuous phase; wherein the viscosity of the oil phase and the aqueous phase satisfy Equation 1 below To provide a method for producing an oil drop composition.

[Equation 1]

log(η _o ) < alog(η _w )+b

(η _w is the viscosity of the aqueous phase, η _o is the viscosity of the oil phase, a is 1 to 1.18, and b has a value of 0.8 or less.)

In one example of the present invention, the oil phase may further include a protonated acrylic acid-based polymer.

In one example of the present invention, the protonated acrylic acid-based polymer may move from the oil phase to the interface between the water phase and stabilize the oil drop by a base in the water phase when the water phase and the oil phase are mixed.

In one example of the present invention, the acrylic acid-based polymer included in the oil phase may be included in an amount of 1 to 5% by weight based on the total weight of the acrylic acid-based polymer included in the oil drop composition.

The present disclosure provides a novel oil drop composition that is transparent or translucent in the visible ray region and has excellent colloidal stability while containing an oil drop of at least 10 μm or more without using a surfactant. The oil drop composition according to the present disclosure can be gently rolled when applied to the skin, and can improve skin moisturizing while preventing skin drying.

1 shows an apparatus for producing an oil drop composition.

Figure 2 shows optical micrographs of oil drop compositions according to Examples and Comparative Examples.

Hereinafter, the present invention will be described in detail so that those skilled in the art can easily implement the present invention. However, this invention may be implemented in many different forms, and is not limited to the embodiments described herein. Also, it is not intended to limit the scope of protection defined by the claims.

In addition, technical terms and scientific terms used in the description of the present invention, unless otherwise defined, have meanings commonly understood by those of ordinary skill in the art to which this invention belongs, and in the following description of the present invention Descriptions of well-known functions and configurations that may unnecessarily obscure the gist are omitted.

Numerical ranges, as used herein, include lower and upper limits and all values within that range, increments logically derived from the form and breadth of the range being defined, all values defined therein, and the upper and lower limits of the numerical range defined in different forms. includes all possible combinations of Unless otherwise specifically defined in the specification of the present invention, values outside the numerical range that may occur due to experimental errors or rounding of values are also included in the defined numerical range.

Unless otherwise specifically defined in the present invention, that a part "includes" a certain component means that it may further include other components, not excluding other components unless otherwise stated. Also, the singular forms used in the specification and appended claims may be intended to include the plural forms as well, unless the context dictates otherwise.

Units used herein without special mention are based on weight, and as an example, the unit of % or ratio means weight% or weight ratio, and unless otherwise defined, weight% means that any one component of the entire composition is included in the composition. It means the weight percent occupied by

As used herein, the term "substantially unused" means that other elements, materials or processes not listed with a specified element, material or process are inadmissible to at least one basic and novel technical idea of the invention. It means that it can be present in an amount that does not have a significant effect on

As used herein, the term "siloxane-based elastomer" refers to a polymer exhibiting high viscosity at room temperature, and may have a crosslinked structure in which a network is formed through crosslinking points in a high molecular weight polymer chain. Accordingly, the siloxane-based elastomer may mean a siloxane-based crosspolymer.

Viscosity in the present specification has a unit of cP (centipoise) unless otherwise specified.

The present inventors have found that oil drops of at least 10 μm or more in oil phase can have excellent colloidal stability in the aqueous phase, and are transparent or translucent in the visible light region, despite not using a surfactant when the oil phase and the aqueous phase form a specific viscosity relationship. The discovery of the formation of phases completed the present invention.

Hereinafter, the present invention will be specifically described.

The present disclosure provides an oil drop composition, wherein the oil drop composition includes oil drops having an average particle diameter of 10 to 1000 μm in an aqueous phase that is a continuous phase, the oil phase includes a hydrophobic polymer and an oil, and the aqueous phase comprises It includes an acrylic acid-based polymer and water, and the viscosity of the aqueous phase (η _w ) and the viscosity of the oil phase (η _o ) satisfy the following formula 1.

[Equation 1]

log(η _o ) < alog(η _w )+b

At this time, in Equation 1, a is 1 to 1.18 and b has a value of 0.8 or less.

Specifically, a is 1 to 1.1 and b has a value of 0.75 or less, more specifically, a is 1.01 to 1.06, 1.02 to 1.04 or 1.0322, b is 0.75 or less, 0.7 or less, 0.68 or less, 0.65 or less, 0.6 or less, 0.612 or less or 0.58 or less, and may be 0 or more as a lower limit. Or a is 1 to 1.1, 1.01 to 1.06, 1.02 to 1.04 or 1.0322, and b may be 0 to 0.75, 0 to 0.7, 0 to 0.68, 0 to 0.65, 0 to 0.6, 0 to 0.612 or 0 to 0.58. .

The oil drop of the oil drop composition satisfies the viscosity condition of Equation 1 and forms a stable oil drop without coalescence or phase separation despite having a relatively large average particle diameter of 1 to 1000 μm. can

Specifically, the average particle diameter of the oil drop may be 10 μm or more, 50 μm or more, 100 μm or more, or 150 μm or more as a lower limit, and 1000 μm or less, 600 μm or less, or 500 μm or less as an upper limit. Specifically, it may be 10 to 1000 μm, and more specifically, it may be 100 to 600 μm, or 150 to 500 μm. The oil drop may have a transparent or translucent phase by adjusting the refractive indices of the oil phase and the aqueous phase while having the above-described average particle diameter. In general, although the stability of the dispersed phase decreases significantly as the average particle ^diameter of the oil drop increases, the oil drop composition according to the present disclosure has a very remarkable dispersion stability in the aqueous phase and an excellent appearance.

The volume ratio of the aqueous phase and the oil phase is not limited as long as the aqueous phase is included in the same or larger volume than the oil phase. Specifically, 50:50 to 99:1, 55:45 to 95:5, 55:45 to 90:10, 60:40 to 85:15, 60:40 to 80:20, 60:40 to 80:20 days can

For example, in the oil drop composition according to the present disclosure, the viscosity of the water phase (η _w ) and the viscosity of the oil phase (η _o ) may further satisfy Equation 2 below.

[Equation 2]

log(η _o ) > clog(η _w )+d

In Equation 2, c is 5.5 to 5.8 and d has a value of -17 or more.

Specifically, c may be 5.55 to 5.75, 5.6 to 5.7, 5.62 to 5.66, or 5.644, and d is -19 or more, -18.5 or more, -18.33 or more, -18 or more, -17.5 or more, -17 or more, -16.64 It may be greater than or equal to, and specifically as an upper limit, d may be -15 or less, -16 or less, or -16.5 or less. Alternatively, c may be 5.55 to 5.75, 5.6 to 5.7, 5.62 to 5.66, or 5.644, and d is -19 to -15, -18.5 to -16, -18.5 to -16.5, -18.33 to -16.5, - 18.33 to -16.64, -18 to -16.64, -17.5 to -16.64 or -17 to -16.64.

The oil drop composition of the oil drop composition satisfies the viscosity condition of Equation 2, so that it does not form a fine emulsion of 10 μm or less, forms an oil drop with a relatively large average particle diameter, and maintains excellent dispersion stability. When the average particle diameter of the oil drop is 10 μm or less, the dispersion stability is excellent, but the translucent phase is converted to an opaque phase, which is undesirable because of the poor appearance.

For example, the lower limit of the viscosity of the aqueous phase may be 200 cP or more, 300 cP or more, 400 cp or more, or 500 cP or more, and the upper limit may be 20,000 cP or less, 15,000 cP or less, 12,000 cP or less, 10,000 cP or less, or 8,000 cP may be below. Specifically, the aqueous phase may have a viscosity of 200 to 20,000 cP, 300 to 15,000 cP, 400 to 12,000 cP, or 500 to 8,000 cP.

For example, the lower limit of the viscosity of the oil phase may be 50 cP or more, 75 cP or more, or 100 cP or more, and the upper limit may be 100,000 cP or less, 50,000 cP or less, 40,000 cP or less, or 30,000 cP or less. Specifically, the viscosity of the oil phase may be 50 to 100,000 cP, 75 to 50,000 cP, and more specifically, 100 to 40,000 cP.

As the aqueous phase and the oil phase simultaneously satisfy the above-mentioned degree range, the colloidal stability of the oil drop is high, so that precipitation does not occur and long-term stability can be achieved.

As a preferred example, the viscosity of the aqueous phase satisfies 500 to 8,000 cP, and at the same time, the viscosity of the oil phase may be 30,000 cP or less. As the aqueous phase and the oil phase simultaneously satisfy the above viscosities, the oil drop may have an average particle diameter of 100 μm or more and a relatively uniform distribution, and at the same time, remarkably excellent dispersion stability.

For example, the acrylic acid-based polymer is a water-soluble polymer containing an acrylic acid residue in a structural unit, and may be a hydrophobic substituted acrylic acid-based polymer. The acrylic acid-based polymer substituted with a hydrophobic group may be a long-chain alkyl group-substituted acrylic acid-based polymer, and exemplarily, may be a crosspolymer of (meth)acrylic acid and C _10-30 alkyl (meth)acrylate. The acrylic acid-based polymer may be located in the aqueous phase, and (meth)acrylic acid may be deprotonated by a subsequent neutralization process with a basic compound. The lower limit of the weight average molecular weight of the acrylic acid-based polymer may be 10,000 g/mol or more, 50,000 g/mol or more, 100,000 g/mol or more, or 200,000 g/mol or more, and the upper limit may be 10,000,000 g/mol or less, 5,000,000 g/mol or less. or 1,000,000 g/mol. Specifically, the weight average molecular weight of the acrylic acid-based polymer may be 10,000 to 10,000,000 g/mol, more specifically 100,000 to 5,000,000 g/mol.

For example, the acrylic acid-based polymer may be 0.001 to 20 parts by weight, 0.01 to 10 parts by weight, or 0.03 to 1 part by weight based on 100 parts by weight of water, but if it is within the range that satisfies the numerical range of the viscosity of Formula 1, the above numerical range not limited to

For example, the hydrophobic polymer may be a siloxane-based polymer or a siloxane-based copolymer. Specifically, it may be polydimethylsiloxane, a polydimethylsiloxane-based copolymer, or a siloxane-based elastomer, preferably a siloxane-based elastomer. Specific examples of the hydrophobic polymer may include dimethicone, dimethicone/vinyldimethicone crosspolymer, dimethicone/PEG-10/15 crosspolymer, dimethicone/polyglycerin-3 crosspolymer, or a combination thereof, More specifically, it may be a dimethicone/vinyldimethicone crosspolymer. As the siloxane-based elastomer is selected as the hydrophobic polymer, the oil drop may have remarkably excellent colloidal stability and may have transparency or translucency in the visible light region.

For example, the hydrophobic polymer may be 1 to 200 parts by weight, 2 to 100 parts by weight, or 5 to 50 parts by weight based on 100 parts by weight of oil, but if it is within a range that satisfies the numerical range of the viscosity of Formula 1, the above numerical range Not limited.

In another example, based on 100 parts by weight of the acrylic acid polymer in the oil drop composition, the hydrophobic polymer may be 100 parts by weight or more, 500 parts by weight or more, and 2000 parts by weight or less, 1000 parts by weight or less as a lower limit, Specifically, it may be included in 100 to 2000 parts by weight.

The oil included in the oil phase may be a silicone oil, a hydrocarbon oil, an ester oil, a triglyceride oil, a vegetable oil, an animal oil, a mineral oil, or a combination thereof, specifically, a silicone oil or It may be a mixture of silicone oil and non-silicone oil, an ester oil, or a mixture of ester oil and non-ester oil.

For example, the silicone-based oil may be selected and used without limitation from linear silicone-based oils and cyclic silicone-based oils, but non-limiting examples thereof include dimethicone, phenyldimethicone, phenyltrimethicone, diphenyldimethicone, a Modimethicone, stearyldimethicone, cyclopentasiloxane, cyclohexasiloxane, polydimethylsiloxane, methylphenylpolysiloxane, tetradecamethylhexasiloxane, octamethyltrisiloxane, methylcyclopolysiloxane, octamethylcyclotetrasiloxane, decamethylcyclopenta It may be one or two or more selected from siloxane and dodecamethylcyclohexasiloxane. Preferably, it may contain one or two or more selected from dimethicone, phenyldimethicone, phenyltrimethicone, diphenyldimethicone, amodimethicone, stearyldimethicone, cyclopentasiloxane, cyclohexasiloxane, etc. Not limited to this.

For example, the hydrocarbon-based oil may be one or two or more selected from C _10-20 alkanes, polybutene, hydrogenated polyisobutene, hydrogenated polydecene, and squalane. Preferably, it may include one or two or more selected from C _13-15 alkanes, but is not limited thereto.

For example, the mineral oil may be one or two or more selected from liquid paraffin, vaseline, isoparaffins, etc., but is not limited thereto.

For example, the ester-based oil may be an aliphatic oil containing one or more ester bonds, specifically triethylhexanoin, cetylethylhexanoate, cetyloctanoate, cetylisooctanoate, and isononyl isononanoate. , octyldodecyl myristate, pentaerythrityltetraethylhexanoate, isopropyl palmitate, isopropyl myristate, and may be one or two or more selected from tocopherol acetate, but is not limited thereto.

As the oil phase contains the silicone oil, the stability of the oil drop can be maintained, and when mixed with the water phase and stirred, the phenomenon of oil coating on the wall does not occur, which preferably provides a process advantage. In addition, when the oil is further included in the oil drop composition, when applied to the skin such as hands, it is gently rolled and prevents skin from drying out, while improving skin moisturization.

For example, the oil phase may further include natural oil. Non-limiting examples of natural oils include citron seed oil, sunflower seed oil, avocado oil, orange oil, macadamia seed oil, lemon oil, pine nut oil, jojoba seed oil, olive oil, tea tree oil, grape seed oil, and hemp seed. vegetable oils such as oil, MCT oil, green tea seed oil, coconut oil, rosehip oil, damask rose oil, brazil nut seed oil, drumstick seed oil, grapefruit seed oil, soybean oil and vanilla fruit oil; but is not limited thereto.

For example, C _4-16 trivalent to pentavalent alcohol may be further included. As the alcohol is further included, the colloidal stability of the oil drop may be further improved.

The trihydric to pentahydric alcohol may be used without limitation as long as it can be used in an external composition for the skin, and non-limiting examples thereof include dipropylene glycol, butylene glycol, 1,2-butanediol, 1,3-butanediol, 2,3-butanediol, 2-methyl-1,3-propanediol, trimethylolethane, trimethylolpropane, pentaerythritol, sorbitol, mannitol, xylitol, erythritol, adonitol, threitol, arabitol and tallitol It may be one or two or more selected from the like.

The C _4-16 trihydric to pentahydric alcohol may be included in an amount of 0 to 5 wt%, specifically 0.01 to 4 wt%, and more specifically 0.1 to 2 wt%, based on the total weight of the oil drop composition.

As described above, conventional emulsification systems and oil drop compositions must contain a large amount of alcohol or a surfactant to ensure colloidal stability, but the oil drop composition according to the present disclosure is an interface for emulsifying the aqueous phase and the oil phase. It may be substantially free of active agents. As it does not contain a surfactant, it can have remarkably excellent skin safety, and consumer preference can be further improved.

In the present disclosure, substantially not containing a surfactant means that it is not included within a range that substantially affects the functional effect of the oil drop composition, and is contained in a small amount for impurities or other known additional functional effects. What is included is not excluded. Specifically, the surfactant may be included in an amount of 0.1% by weight or less, 0.01% by weight or less, 0.001% by weight or less, or 0.0001% by weight or less based on the total weight of the oil drop composition, and the lower limit may be 0% by weight or more.

The surfactant for the emulsification may be a component used for the purpose of stabilizing the emulsified phase, and specifically, may be a low molecular weight cationic, anionic or nonionic surfactant, exemplarily having a molecular weight of 5000 g/mol or less and a molecular weight of 2000 g /mol or less or a molecular weight of 1000 g/mol or less.

The oil drop composition according to the present disclosure prevents coalescence between oil drops so that the oil drops are stably dispersed in the water phase, and can maintain a stable dispersed phase without adversely changing with time even at low temperatures as well as high temperatures.

The present disclosure provides a method for preparing an oil drop composition, which includes preparing an aqueous phase containing an acrylic acid-based polymer, a basic compound and water; preparing an oil phase containing a hydrophobic polymer and an oil; And mixing the aqueous phase and the oil phase to prepare a composition in which the dispersed oil phase is distributed in the form of an oil drop in a continuous aqueous phase; characterized in that it satisfies Formula 1 below.

[Equation 1]

log(η _o ) < alog(η _w )+b

At this time, in Equation 1, a is 1 to 1.18 and b has a value of 0.8 or less.

Specifically, a is 1 to 1.1 and b has a value of 0.75 or less, more specifically, a is 1.01 to 1.06, 1.02 to 1.04 or 1.0322, b is 0.75 or less, 0.7 or less, 0.68 or less, 0.65 or less, 0.6 or less, 0.612 or less or 0.58 or less, and may be 0 or more as a lower limit. Or a is 1 to 1.1, 1.01 to 1.06, 1.02 to 1.04 or 1.0322, and b may be 0 to 0.75, 0 to 0.7, 0 to 0.68, 0 to 0.65, 0 to 0.6, 0 to 0.612 or 0 to 0.58. .

For example, the viscosity of the aqueous phase (η _w ) and the viscosity of the oil phase (η _o ) may further satisfy Equation 2 below.

[Equation 2]

log(η _o ) > clog(η _w )+d

In Equation 2, c is 5.5 to 5.8 and d has a value of -17 or more.

Specifically, c may be 5.55 to 5.75, 5.6 to 5.7, 5.62 to 5.66, or 5.644, and d is -19 or more, -18.5 or more, -18.33 or more, -18 or more, -17.5 or more, -17 or more, -16.64 It may be greater than or equal to, and specifically as an upper limit, d may be -15 or less, -16 or less, or -16.5 or less. Alternatively, c may be 5.55 to 5.75, 5.6 to 5.7, 5.62 to 5.66, or 5.644, and d is -19 to -15, -18.5 to -16, -18.5 to -16.5, -18.33 to -16.5, - 18.33 to -16.64, -18 to -16.64, -17.5 to -16.64 or -17 to -16.64.

In the manufacturing method of the oil drop composition according to the present disclosure, detailed descriptions of ingredients and contents included in the water phase and the oil phase are the same as those described in the oil drop composition, so detailed descriptions are omitted.

Referring to FIG. 1 , the oily raw material stored in the hydrophobic raw material supply unit 300 is continuously supplied to the cooling and constant temperature bath 400 through the transport pipe 200 at a constant pressure. The supplied raw material of the oil phase falls, and oil drops are produced by the agitator 100 according to preset conditions.

The basic compound included in the aqueous phase may serve to help increase the viscosity of the acrylic acid-based polymer. Non-limiting examples thereof include one or two or more selected from sodium hydroxide, potassium hydroxide, ammonium hydroxide, and triethanolamine.

As a preferred example, the oil phase may further include a protonated acrylic acid-based polymer. The acrylic acid-based polymer may be the same as the acrylic acid-based polymer included in the aqueous phase, and since specific examples are the same as those described above, a detailed description thereof will be omitted.

As the acrylic acid-based polymer is protonated, it may not completely dissolve in the oil phase, but may have a certain level of dispersibility. When the water phase and the oil phase are mixed, the protonated acrylic acid-based polymer can move from the oil phase to the interface between the water phase and stabilize the oil drop by the base in the water phase. The acrylic acid-based polymer dispersed in the oil phase by mixing with the aqueous phase may be completely deprotonated or partially deprotonated, and preferably, at least a part of the structural unit is substituted with a hydrophobic group to form an interface between the aqueous phase and the oil phase. stabilization more effectively. It is difficult to achieve such interface stabilization and thus a stable oil drop composition only by the acrylic acid-based polymer dissolved in the aqueous phase.

For example, the acrylic acid-based polymer included in the oil phase has a lower limit of 1% by weight or more and 2% by weight or more, and an upper limit of 5% by weight or less and 4% by weight based on the total weight of the total acrylic acid-based polymers included in the oil drop composition. May include the following. Specifically, the acrylic acid-based polymer included in the oil phase may be included in 1 to 5% by weight and 2 to 4% by weight.

Hereinafter, Examples and Experimental Examples will be specifically exemplified and described. However, the examples and experimental examples to be described below are merely illustrative of a part, and the technology described herein is not limited thereto.

[Group I: Examples and Comparative Examples]

EZ-4U (Acrylates/C10-30 Alkyl Acrylate Crosspolymer (INCI)) was used as an acrylic acid-based polymer, and an aqueous phase containing potassium hydroxide and water was prepared. The pH of the aqueous phase was adjusted to 5-7. For the preparation of the oil phase, an elastomer-type polymer was used as a hydrophobic polymer, silicone oil and ester-based oil were used as oil, and 3% by weight of the total weight of EZ-4U was used as an acrylic acid-based polymer included in the oil drop composition. It was additionally dispersed in the aqueous phase. Accordingly, an oil phase was prepared by stirring the hydrophobic polymer, oil, and acrylic acid-based polymer in a combination as described later at 25 °C. The aqueous phase and oil phase prepared respectively are shown in the following table, the volume ratio of the aqueous phase and the oil phase was set to 60:40, and the contents of the components included in the aqueous phase and the oil phase were appropriately adjusted to have the viscosity shown in Table 1.

Specifically, Sam. 1 to 10 used Cyclopentasiloxane (and) Dimethicone/Vinyl Dimethicone Crosspolymer (KSG15-Shin Etsu) as an elastomer and Isononyl Isononanoate as an oil. Sam. 11 to Sam. 20 used C13-15 Alkane/Vinyl Dimethicone Crosspolymer (C13-15 Alkane (and) Dimethicone/Vinyl Dimethicone Crosspolymer: PURESIL ORG01 - Elkem) as an elastomer and Diphenylsiloxy Phenyl Trimethicone oil as an oil. Sam. 21 to Sam. 30 used Isododecane (and) Dimethicone/Vinyl Dimethicone Crosspolymer (USG106 - ShinEtsu) elastomer as an elastomer and mixed oil of Isononyl Isononanoate and olive oil as an oil.

Viscosity was measured at 25 ° C using BROOKFIELD AMETEK (#62 to #64, 12 RPM, 1 min).

While slowly adding the aqueous phase and the oil phase to the aqueous phase, the mixture was stirred for 10 minutes to prepare an oil drop composition in which the dispersed oil phase was distributed in the form of fine droplets in the continuous aqueous phase.

[Comparative Example 17]

In the example corresponding to Sam.14, an aqueous phase having a viscosity of 2,100 cp at room temperature, containing water without potassium hydroxide, using xanthan gum (Xanthan gum, G1253 Korea Caragen) instead of the acrylic acid polymer included in the aqueous phase was prepared and carried out in the same manner as in Example, except that 3% by weight of the total weight of xanthan gum included in the microdroplet composition was additionally dispersed in the oil phase.

[Comparative Example 18]

In the example corresponding to Sam.21, hydroxypropyl methylcellulose (HPMC, H7509 Sigma-Aldrich) was used instead of the acrylic acid-based polymer contained in the aqueous phase, and the aqueous phase containing water was dissolved without potassium hydroxide, An aqueous phase having a viscosity of 3,900 cp at room temperature was prepared and carried out in the same manner as in Example, except that 3% by weight of the total weight of HPMC included in the microdroplet composition was additionally dispersed in the oil phase.

[Group II: Examples and Comparative Examples]

Except for the fact that the volume ratio of the aqueous phase and the oil phase was set to 80:20 in the above Group I Examples and Comparative Examples, the oil drop in which the oil phase, the dispersed phase, is distributed in the form of fine droplets in the aqueous phase, the continuous phase, was carried out in the same manner. A composition was prepared.

[Evaluation of microdroplets]

The evaluation of microdroplets prepared according to Examples and Comparative Examples of Group I is shown in Table 1 below, and the evaluation of microdroplets prepared according to Examples and Comparative Examples of Group II is shown in Table 2 below.

		Oil phase viscosity (cP)
		100	5,000	10,000	25,000	40,000	50,000
Water viscosity (cP)	100	X(Sam.1)	X(Sam.2)	X(Sam.3)	X(Sam.4)	X(Sam.5)	X(Sam.6)
	1,000	○(Sam.7)	○(Sam.8)	X(Sam. 9)	X(Sam.10)	X(Sam.11)	X(Sam.12)
	2,000	○(Sam.13)	○(Sam.14)	○(Sam.15)	X(Sam.16)	X(Sam.17)	X(Sam.18)
	4,000	△(Sam. 19)	○(Sam.20)	○(Sam.21)	○(Sam.22)	X(Sam.23)	X(Sam.24)
	8,000	△(Sam.25)	△(Sam.26)	○(Sam.27)	○(Sam.28)	△(Sam.29)	X(Sam.30)

		Oil phase viscosity (cP)
		100	5,000	10,000	25,000	40,000	50,000
Water viscosity (cP)	100	X(Sam.31)	X(Sam.32)	X(Sam.33)	X(Sam.34)	X(Sam.35)	X(Sam.36)
	1,000	○(Sam.37)	○(Sam.38)	X(Sam.39)	X(Sam.40)	X(Sam.41)	X(Sam.42)
	2,000	○(Sam.43)	○(Sam.44)	○(Sam.45)	X(Sam.46)	X (Sam. 47)	X(Sam.48)
	4,000	△(Sam.49)	○(Sam.50)	○(Sam.51)	○(Sam.52)	X(Sam. 53)	X(Sam.54)
	8,000	△(Sam.55)	○(Sam.56)	○(Sam.57)	○(Sam.58)	○(Sam.59)	X(Sam.60)

In Tables 1 and 2, ○ means that microdroplets are stably formed, △ means that microdroplets are formed but the particle size is very small and an opaque composition is formed, and X means that no microdroplets are formed and phase separation occurs As can be seen in Table 1 and FIG. 2 above, Sam.7, Sam.8, Sam.13, Sam.14, Sam.15, and Sam corresponding to the examples. As .21, Sam.20, Sam.22, Sam.27, and Sam.28 all satisfied Equation 1, it was shown that stable microdroplets were produced. Sam. In the case of Example 1 (Comparative Example 1), the viscosity of the water phase was low, and it was found that phase separation occurred immediately without the formation of fine droplets. In addition, Sam.2 (Comparative Example 2), Sam.3 (Comparative Example 3), Sam.4 (Comparative Example 4), Sam.5 (Comparative Example 5), Sam. 6 (Comparative Example 6), Sam.9 (Comparative Example 7), Sam.10 (Comparative Example 8), Sam.11 (Comparative Example 9), Sam.12 (Comparative Example 10), Sam.16 (Comparative Example 11) ), Sam.17 (Comparative Example 12), Sam.18 (Comparative Example 13), Sam.23 (Comparative Example 14), Sam.24 (Comparative Example 15), and Sam.30 (Comparative Example 16) have fine droplets. It was found to have a semi-continuous phase or band-like shape without formation of spherical microdroplets, a phenomenon in which particles float and agglomerate due to a serious coalescence phenomenon without formation.

On the other hand, in the case of Sam.19, Sam.25, Sam.26, and Sam.29, stable microdroplets were obtained, but microdroplets with very small particle diameters were obtained, resulting in an opaque phase. This characteristic is due to the fact that the samples do not satisfy Equation 2.

Referring to FIG. 4, FIG. 4 shows an optical micrograph of a microdroplet, in which microdroplets of 10 μm or more are produced by an embodiment according to the present disclosure, and the average particle diameter is also easily adjusted by adjusting Equations 1 and 2 This indicates that it can be regulated.

In the case of Comparative Examples 17 and 18, although the viscosity of the aqueous phase and the viscosity of the oil phase satisfied Equation 1, fine droplets were formed after stirring, but phase separation occurred after 20 minutes.

On the other hand, the evaluation results of the microdroplets of Group II, which were tested by varying the volume ratio of the aqueous phase and the oil phase, were the same as Group I, and through this, by adjusting Equations 1 and 2, regardless of the volume ratio of the aqueous phase and the oil phase, It can be seen that the stability of the three droplets can be easily controlled.

As described above, the present invention has been described with specific details and limited examples, but this is only provided to help a more general understanding of the present invention, the present invention is not limited to the above examples, and the field to which the present invention belongs Those skilled in the art can make various modifications and variations from these descriptions.

Therefore, the spirit of the present invention should not be limited to the described embodiments, and it will be said that not only the claims to be described later, but also all modifications equivalent or equivalent to these claims belong to the scope of the present invention. .

explanation of code

100: stirring unit 200: transport pipe

300: supply unit 400: thermostat

Claims (13)

1. A composition comprising oil drops having an average particle diameter of 10 to 1000 μm in an aqueous phase, which is a continuous phase,

   The oil phase includes a hydrophobic polymer and an oil,

   The aqueous phase includes an acrylic acid-based polymer and water,

   An oil drop composition, characterized in that the viscosity of the aqueous phase (η _w ) and the viscosity of the oil phase (η _o ) satisfy Equation 1 below.

   [Equation 1]

   log(η _o ) < alog(η _w )+b

   In Equation 1, a is 1 to 1.18 and b has a value of 0.8 or less.
2. According to claim 1,

   The oil drop composition, wherein the viscosity of the aqueous phase (η _w ) and the viscosity of the oil phase (η _o ) further satisfy Equation 2 below.

   [Equation 2]

   log(η _o ) > clog(η _w )+d

   In Equation 2, c is 5.5 to 5.8 and d has a value of -17 or more.
3. According to claim 1,

   The viscosity of the aqueous phase is 200 cP or more, the oil drop composition.
4. According to claim 1,

   The viscosity of the oil phase is 50000 cP or less, the oil drop composition.
5. According to claim 1,

   The acrylic acid-based polymer is a crosspolymer of (meth)acrylic acid and C10-C30 alkyl (meth)acrylate, oil drop composition.
6. According to claim 1,

   The hydrophobic polymer,

   An oil drop composition which is a siloxane-based polymer or a siloxane-based copolymer.
7. According to claim 1,

   Based on 100 parts by weight of the acrylic acid-based polymer, the hydrophobic polymer is included in 100 to 2000 parts by weight, the oil drop composition.
8. According to claim 1,

   An oil drop composition further comprising a C4-C16 trihydric to pentahydric alcohol.
9. According to claim 1,

   An oil drop composition that does not substantially contain a surfactant for emulsifying the aqueous phase and the oil phase.
10. preparing an aqueous phase containing an acrylic acid-based polymer, a basic compound and water;

    preparing an oil phase containing a hydrophobic polymer and an oil; and

    Mixing the aqueous phase and the oil phase to prepare a composition in which an oil phase, a dispersed phase, is distributed in an oil drop form in an aqueous phase, which is a continuous phase;

    A method for producing an oil drop composition, characterized in that the viscosity of the oil phase and the aqueous phase satisfies the following formula 1.

    [Equation 1]

    log(η _o ) < alog(η _w )+b

    (η _w is the viscosity of the aqueous phase, η _o is the viscosity of the oil phase, a is 1 to 1.18, and b has a value of 0.8 or less.)
11. According to claim 10,

    The method of producing an oil drop composition, wherein the oil phase further comprises a protonated acrylic acid-based polymer.
12. According to claim 11,

    The method of producing an oil drop composition, wherein the protonated acrylic acid-based polymer moves from the oil phase to the interface of the aqueous phase by a base in the aqueous phase when mixing the aqueous phase and the oil phase to stabilize the oil drop.
13. According to claim 11,

    The acrylic acid-based polymer included in the oil phase is included in an amount of 1 to 5% by weight based on the total weight of the acrylic acid-based polymer included in the oil drop composition.

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