KR102641156B1 - Emulsion composition - Google Patents

Abstract

The present invention relates to an emulsion composition, and the emulsion composition according to the present invention is a silicone resin containing R ₃ SiO _1/2 unit and SiO ₂ unit (wherein R is a straight or branched hydrocarbon group having 1 to 6 carbon atoms, or , an aryl group having 6 to 12 carbon atoms) and an acrylic modified silicone copolymer.

Description

Emulsion composition {EMULSION COMPOSITION}

The present invention relates to emulsion compositions.

When applied to skin care products and hair care products, emulsions for cosmetics are required to form a film on the applied surface, do not have the stickiness characteristic of silicone, and have excellent effects such as gloss and feeling of use. Accordingly, the conventional emulsion composition for hair was prepared by mixing various ingredients to give flexibility and wettability to hair, protect hair, and improve texture when applied to hair care products. Conventional emulsion compositions for hair generally contain a silicone resin represented by dimethylpolysiloxane polymer, which is soft and has excellent lubricity compared to alcohol, glyceride, liquid paraffin, and esters. In addition, the emulsion composition for hair containing the silicone resin is known to be effective in protecting hair by forming a strong film on the hair.

Specifically, Korean Patent Publication No. 938,050 (Patent Document 1) discloses an organopolysiloxane hair treatment agent represented by R ¹ _a R ² _b R ³ _c SiO _(4-abc)/2 . However, the emulsion composition for hair containing organopolysiloxane, as in Patent Document 1, forms a strong film on the hair after application and washing and has excellent durability, but has the disadvantage of lacking a feeling of use, such as the texture and gloss of the hair after washing. In particular, when using an emulsion composition containing a silicone resin with a high degree of polymerization, there was a disadvantage in that silicone's unique stickiness remained on the hair even after application and washing.

Therefore, there is a need for research and development of an emulsion composition for hair that has excellent durability of the manufactured film after application and washing, does not leave behind the stickiness characteristic of silicone, and provides excellent feeling of use, such as hair texture and gloss.

Korean Patent Publication No. 938,050 (Publication Date: December 23, 2005)

Accordingly, the present invention seeks to provide an emulsion composition with excellent durability and feeling of use.

The present invention relates to a silicone resin containing an R ₃ SiO _1/2 unit and a SiO ₂ unit (where R is a straight-chain or branched hydrocarbon group having 1 to 6 carbon atoms, or an aryl group having 6 to 12 carbon atoms) and an acrylic modified silicone. An emulsion composition comprising a copolymer and comprising 25 to 100 parts by weight of an acrylic modified silicone copolymer based on 100 parts by weight of the silicone resin is provided.

The emulsion composition according to the present invention has excellent durability by creating a strong coating film on hair or skin after application and washing, and the coating film improves texture and gloss on hair or skin, providing excellent feeling of use.

Hereinafter, the present invention will be described in detail.

The emulsion composition according to the present invention comprises a silicone resin and an acrylic modified silicone copolymer.

silicone resin

The silicone resin serves to maintain the effect of the composition by forming a strong film on hair or skin after application and washing.

The silicone resin includes R ₃ SiO _1/2 units (M units) and SiO ₂ units (Q units) (wherein R is a straight or branched hydrocarbon group having 1 to 6 carbon atoms, or a hydrocarbon group having 6 to 12 carbon atoms) aryl group). Specifically, the silicone resin may be an MQ resin composed of R ₃ SiO _1/2 units (M units) and SiO ₂ units (Q units).

The R is a linear or branched hydrocarbon group having 1 to 6 carbon atoms, or an aryl group having 6 to 12 carbon atoms. The hydrocarbon group may be, for example, one selected from the group consisting of methyl, ethyl, isopropyl and vinyl groups, and the aryl group may be, for example, one selected from the group consisting of phenyl and naphthyl groups.

The molar ratio (M:Q) of the R ₃ SiO _1/2 unit and the SiO ₂ unit of the silicone resin may be 0.3:1 to 1.5:1, 0.5:1 to 1.3:1, or 0.7:1 to 1.2:1.

The silicone resin may have a viscosity of 100 cP to 1,000 cP at 25°C and a weight average molecular weight (Mw) of 1,000 to 8,000 g/mol. Specifically, the silicone resin may have a viscosity of 300 cP to 1,000 cP or 500 cP to 800 cP at 25°C, and a weight average molecular weight (Mw) of 2,000 to 7,000 g/mol or 3,000 to 5,000 g/mol. When the viscosity of the silicone resin is within the above range, the viscosity of the composition containing the silicone resin is appropriate, thereby improving the usability of the composition, and when the weight average molecular weight (Mw) of the silicone resin is within the above range, the coating film manufactured from the composition containing the silicone resin has an appropriate viscosity. Adhesion is improved, which has the effect of improving the sustainability of the coating film.

Acrylic modified silicone copolymer

The acrylic-modified silicone copolymer serves to improve the feeling of use of a composition containing it.

The acrylic modified silicone copolymer may be represented by the following formula (1).

In Formula 1, R ¹ is a straight-chain or branched hydrocarbon group having 1 to 10 carbon atoms, x is an integer from 3 to 20, y is an integer from 3 to 25, and n is an integer from 10 to 30.

Specifically, in Formula 1, R ¹ is an alkyl group of C _{1 to 10} , x is an integer of 5 to 20, y is an integer of 5 to 20, n is an integer of 15 to 30, and the alkyl group is a hydroxyl group or It may be substituted with a halogen atom.

When x, y, and n are within the above range, there is an effect of providing a film feel and improving sustainability and feeling of use.

The acrylic modified silicone copolymer may be prepared by copolymerizing a dimethylpolysiloxane compound represented by the following formula (2) and a radically polymerizable monomer containing at least one functional group selected from the group consisting of an acrylate group and a methacrylate group.

In Formula 2, R ² is C _1-10 alkylene, R ³ is methyl or a hydrogen atom, and m is an integer from 10 to 30.

Specifically, in Formula 2, R ² is C _1-5 alkylene, R ³ is methyl or a hydrogen atom, and m may be an integer of 15 to 30.

If m is within the above range, it has the effect of improving softness and usability.

The radically polymerizable monomer contains at least one functional group selected from the group consisting of an acrylate group and a methacrylate group, for example, C _{1 to 10} alkyl methacrylate, hydroxy-C _{1 to 10} alkyl methacrylate. It may be alkyl acrylate, C _{1 to 10} alkyl acrylate or hydroxy-C _{1 to 10} alkyl acrylate. Specifically, the radical polymerizable monomer includes alkyl methacrylates having _{1 to 10} C atoms, such as methyl methacrylate, ethyl methacrylate, butyl methacrylate, and 2-ethylhexyl methacrylate; Hydroxy-C _{1 to 10} hydroxyalkyl methacrylates such as 2-hydroxyethyl methacrylate and 2-hydroxypropyl methacrylate; and C _{1 to C 10} alkyl acrylates such as methyl acrylate, ethyl acrylate, butyl acrylate, and 2-ethylhexyl acrylate; and hydroxy-C _{1 to 10} alkyl acrylates such as 2-hydroxyethyl acrylate and 2-hydroxypropyl acrylate.

The acrylic-modified silicone copolymer may have a glass transition temperature (Tg) of 35 to 60° C. and a silicone content of 65 to 90% by weight based on the total weight of the acrylic-modified silicone copolymer. Specifically, the acrylic modified silicone copolymer may have a glass transition temperature of 37 to 55°C or 38 to 50°C and a silicone content of 70 to 88% by weight or 75 to 85% by weight based on the total weight of the acrylic modified silicone copolymer. there is. When the glass transition temperature of the acrylic-modified silicone copolymer is within the above range, there is an effect of improving film formation and film sustainability, and when the silicone content of the acrylic-modified silicone copolymer is within the above range, there is an effect of improving the feeling of use.

The acrylic modified silicone copolymer may have a weight average molecular weight (Mw) of 7,000 to 48,000 g/mol and a viscosity of 100 to 300 cP at 25°C. Specifically, the acrylic modified silicone copolymer may have a weight average molecular weight (Mw) of 8,000 to 45,000 g/mol or 10,000 to 45,000 g/mol and a viscosity at 25°C of 150 to 250 cP or 180 to 200 cP. When the weight average molecular weight (Mw) of the acrylic modified silicone copolymer is within the above range, it has the effect of providing sustainability and gloss to the film after drying, and when the viscosity at 25°C is within the above range, it has the effect of providing a film feel. .

The acrylic modified silicone copolymer is included in an amount of 25 to 100 parts by weight based on 100 parts by weight of the silicone resin. Specifically, the acrylic modified silicone copolymer may be included in an amount of 30 to 95 parts by weight, 40 to 80 parts by weight, or 40 to 60 parts by weight based on 100 parts by weight of the silicone resin. When the acrylic modified silicone copolymer is included in the above content range, it has the effect of improving the sustainability and feeling of use of the film after applying the emulsion.

additive

The emulsion composition may further include one or more additives selected from the group consisting of diluents, solvents, emulsifiers, and thickeners.

The diluent serves to improve the usability of the emulsion composition by controlling the viscosity of the emulsion composition.

The diluent may be silicone oil. The silicone oil includes, for example, organopolysiloxane such as dimethylpolysiloxane and a copolymer of dimethylsiloxane and methylphenylsiloxane; Cyclic siloxanes such as octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, tetramethyltetrahydrogencyclotetrasiloxane, and tetramethyltetraphenylcyclotetrasiloxane; etc. can be mentioned.

The diluent may have a viscosity of 0.1 to 100 cP at 25°C. Specifically, the diluent may have a viscosity of 0.5 to 100 cP or 1 to 100 cP at 25°C. If the viscosity of the diluent at 25°C is within the above range, it has the effect of improving emulsion stability.

The diluent may be included in an amount of 200 to 300 parts by weight based on 100 parts by weight of the silicone resin. Specifically, the diluent may be included in an amount of 200 to 280 parts by weight or 200 to 250 parts by weight based on 100 parts by weight of the silicone resin. When the diluent is included within the above content range, it has the effect of improving the dilution stability and emulsion stability of the emulsion.

The solvent serves to improve the usability of the emulsion composition by controlling the viscosity of the emulsion composition.

The solvent is not particularly limited as long as it is a common solvent that can be included in an emulsion composition, and may specifically be water. Examples of the water include ionized water, rose water, and lavender water.

The solvent may be included in an amount of 200 to 300 parts by weight based on 100 parts by weight of the silicone resin. Specifically, the solvent may be included in an amount of 230 to 300 parts by weight or 250 to 300 parts by weight based on 100 parts by weight of the silicone resin. When the solvent is included within the above content range, it has the effect of improving emulsion stability and feeling of use.

The emulsifier serves to evenly mix each component of the composition.

The emulsifier may specifically be a cationic, nonionic and anionic emulsifier. More specifically, the emulsifier may be a nonionic emulsifier.

The nonionic emulsifiers include, for example, polyoxyethylene alkyl ether, polyoxyethylene allylalkyl ether, polyoxyalkylene alkylphenol ether, polyoxyalkylene aryl ester, polyoxyalkylene sorbic acid alkyl ester, sodium lauryl ether sulfate. and stearyl trimethyl ammonium chloride. Specifically, the nonionic surfactant may be a block copolymer of ethylene oxide and propylene oxide. The ethylene oxide and propylene oxide block copolymer is preferably used as a mixture of one type of ethylene oxide or propylene oxide, or two or more different types of ethylene oxide and propylene oxide block copolymers.

The emulsifier may be included in an amount of 10 to 50 parts by weight based on 100 parts by weight of the silicone resin. Specifically, the emulsifier may be included in an amount of 20 to 50 parts by weight or 30 to 50 parts by weight based on 100 parts by weight of the silicone resin. When the content of the emulsifier is within the above range, there is an effect of improving emulsion stability.

The thickener serves to increase the viscosity of the emulsion and improve emulsion stability. In addition, examples of the thickener include polyacrylic acid, polymer xanthan gum, and guar gum.

The thickener may be included in an amount of 0.1 to 1 part by weight based on 100 parts by weight of the silicone resin. Specifically, the thickener may be included in an amount of 0.1 to 0.8 parts by weight or 0.1 to 0.5 parts by weight based on 100 parts by weight of the silicone resin. When the content of the thickener is within the above range, the viscosity increases and storage stability is improved.

In addition, the emulsion composition includes ingredients used in conventional cosmetics to the extent that they do not interfere with the effect of the present invention, including organically modified clay minerals, resins, ultraviolet absorbers, ultraviolet absorbing scattering agents, moisturizers, preservatives, antibacterial agents, fragrances, salts, and oxidizing agents. Preventative agents, pH adjusters, chelating agents, refreshing agents, anti-inflammatory agents, skin care ingredients (whitening agents, cell revitalizers, skin roughness improvers, blood circulation promoters, skin astringents, antiseborrheic agents, etc.), vitamins, amino acids, hexane, hormones, It may additionally include a hair solidifying agent, etc.

The emulsion composition may have a viscosity of 5,000 to 100,000 cP at 25°C. Specifically, the emulsion composition may have a viscosity of 5,000 to 50,000 cP, 5,000 to 30,000 cP, 5,000 to 20,000 cP, or 5,000 to 15,000 cP at 25°C. When the viscosity of the emulsion composition at 25°C is within the above range, it has the effect of improving feeling of use, such as softness and spreadability.

The emulsion composition according to the present invention can be included in conventional cosmetic compositions and can be formulated in the form of solutions, suspensions, emulsions, pastes, gels, creams, lotions, and sprays. For example, the emulsion composition may be in the form of aqueous, solubilized, O/W emulsified, W/O emulsified, oil-based, etc. In addition, the emulsion composition can be mixed with a propellant and provided in a foam type using an aerosol foam or pump foam container, and can be used outside of the bathroom, such as styling spray, styling mousse, hair mist, hair wax, hair cream, and hair essence. It can be included in a cosmetic composition for hair. Furthermore, the emulsion composition may be included in hair cosmetic compositions for use in bathrooms, such as shampoos, conditioners, bleaching or perm products, rinse-out products, intensive care masks, shower gels, or lotions or creams for scalp treatment.

Specifically, the emulsion composition may be an emulsion composition for hair cosmetics.

As described above, the emulsion composition according to the present invention has excellent durability by creating a strong coating film on the hair after application and washing, and the coating film improves the texture and gloss of the hair, providing an excellent feeling of use.

The present invention will be described in more detail below with reference to the following examples. However, the description using the following examples is only intended to specify and explain specific embodiments of the present invention, and is not intended to limit or interpret the scope of the present invention to the contents described in these examples.

[Example]

The ingredients and product names of each component used in the following examples and comparative examples are shown in Table 1 below.

ingredient Physical properties or manufacturer and product name silicone resin MQ resin M:Q = 0.8 to 1.1:1, viscosity at 25°C: 700cP, Mw: 4,000g/mol Acrylic modified silicone copolymer 1 Tg: 45℃, Mw: 25,000g/mol, silicon content: 81% by weight,
In Formula 1, x=y=11, n=25, R ¹ =CH ₃ Acrylic modified silicone copolymer 2 Tg: 40℃, Mw: 43,000g/mol, silicon content: 87% by weight,
In Formula 1, x=5, y=20, n=25, R ¹ = CH ₃ Acrylic modified silicone copolymer 3 Tg: 48℃, Mw: 28,000g/mol, silicon content: 72% by weight,
In Formula 1, x=5, y=5, n=15, R ¹ = CH ₃ Acrylic modified silicone copolymer 4 Tg: 48℃, Mw: 9,200g/mol, silicon content: 60% by weight,
In Formula 1, x=10, y=5, n=15, R ¹ = CH ₃ Acrylic modified silicone copolymer 5 Tg: 42℃, Mw: 65,000g/mol, silicon content: 91% by weight,
In Formula 1, x=2 y=20, n=40, R ¹ = CH ₃ Acrylic modified silicone copolymer 6 Tg: 65℃, Mw: 6,500g/mol, silicon content: 68% by weight,
In Formula 1, x=10, y=2, n=30, R ¹ = CH ₃ Acrylic modified silicone copolymer 7 Tg: 32℃, Mw: 50,000g/mol, silicon content: 78% by weight,
In Formula 1, x=5, y=30, n=15, R ¹ = CH ₃ diluent Decamethylcyclopentasiloxane menstruum ionized water emulsifier Synperonic PE/F 68, a nonionic emulsifier (CRODA product) thickener TEGO Carbomer 340FD (EVONIK product)

Examples 1 to 12 and Comparative Examples 1 and 2. Preparation of emulsion composition

An emulsion composition was prepared by mixing the silicone resin, acrylic modified silicone copolymer, diluent, solvent, emulsifier, and thickener in the amounts shown in Table 2 below.

(part by weight) silicone resin Acrylic modified silicone copolymer diluent menstruum emulsifier thickener One 2 3 4 5 6 7 Example 1 100 47 - - - - - - 220 267 33 0.3 Example 2 100 51 - - - - - - 220 267 33 0.3 Example 3 100 58 - - - - - - 220 267 33 0.3 Example 4 100 31 - - - - - - 220 267 33 0.3 Example 5 100 72 - - - - - - 220 267 33 0.3 Example 6 100 92 - - - - - - 220 267 33 0.3 Example 7 100 - 47 - - - - - 220 267 33 0.3 Example 8 100 - - 47 - - - - 220 267 33 0.3 Example 9 100 - - - 47 - - - 220 267 33 0.3 Example 10 100 - - - - 47 - - 220 267 33 0.3 Example 11 100 - - - - - 47 - 220 267 33 0.3 Example 12 100 - - - - - - 47 220 267 33 0.3 Comparative Example 1 100 22 - - - - - - 220 267 33 0.3 Comparative Example 2 100 106 - - - - - - 220 267 33 0.3

Test example: Evaluation of physical properties of emulsion composition

The physical properties of the emulsion compositions of Examples 1 to 12 and Comparative Examples 1 and 2 were measured and evaluated by the following method, and the results are shown in Table 3.

(1) Appearance

The appearance of the emulsion composition was evaluated by observing color with the naked eye at 25°C.

(2) Viscosity

Viscosity at 25°C was measured using a viscometer (LVT Brookfield viscometer, spindle #64, 30 rpm).

(3) Average particle size

Ionized water was added to the emulsion composition to dilute the solution to a concentration of 5% by weight, and then the average particle size of the emulsion composition was measured using a laser particle size analyzer (manufacturer: Malvern, model name: mastersizer 3000).

(4) Stability

The stability of the emulsion composition was evaluated after being stored at 25°C or 50°C for 7 days. At this time, if the emulsion composition after storage was uniform like the initial emulsion composition and there was no layer separation, it was evaluated as 'good', and if the emulsion composition was not uniform and layer separation was visible to the naked eye, it was evaluated as 'separation'.

(5) Feeling of use (sensory evaluation)

The feeling of use of the emulsion composition was evaluated by 10 people using the following evaluation items, and the results were averaged.

- Evaluation items: Glossiness, coating properties, and softness of hair after applying and washing the composition

- Rating: 5 (very good), 4 (excellent), 3 (average), 2 (poor), 1 (very poor)

(6) Continuity

0.2 g of the emulsion composition was applied on the skin and 1 hour later, the removal of the coating film was evaluated when the applied surface of the emulsion composition was pushed with a finger. If the coating film was partially or completely pushed out by the finger, it was marked as Case was evaluated as O.

Exterior viscosity
(cP) average
particle size stability Feeling of use (sensory evaluation) persistence 25℃ 50℃ glossiness Coating properties Soft Example 1 milk white 10,000 3㎛ Good Good 5 5 5 O Example 2 milk white 12,500 3㎛ Good Good 5 5 5 O Example 3 milk white 13,100 3㎛ Good Good 5 5 5 O Example 4 milk white 8,900 3㎛ Good Good 5 3 5 O Example 5 milk white 18,800 4㎛ Good Good 5 4 4 O Example 6 milk white 24,000 6㎛ Good Good 4 5 3 O Example 7 milk white 12,100 3㎛ Good Good 5 3 3 O Example 8 milk white 11,050 3㎛ Good Good 5 3 3 O Example 9 milk white 14,800 3㎛ Good Separated after 7 days 3 4 5 O Example 10 milk white 7,800 3㎛ Good Good 2 3 5 O Example 11 milk white 18,000 3㎛ Good Separated after 7 days 3 4 5 O Example 12 milk white 6,700 3㎛ Good Separated after 7 days 3 3 5 O Comparative Example 1 milk white 4,600 3㎛ Separate within 24 hours 24 hours
separated within 2 One One X Comparative Example 2 milk white 34,500 8㎛ Separate within 24 hours 24 hours
separated within One 2 One X

As shown in Table 3, the emulsion compositions of Examples 1 to 12 had excellent stability, usability, durability, and appearance. On the other hand, the emulsion compositions of Comparative Example 1, which contained a small amount of acrylic-modified silicone copolymer compared to the silicone resin, and Comparative Example 2, which contained an excessive amount of acrylic-modified silicone copolymer, had a viscosity that was too low or high and was used at room temperature (25°C) and high temperature. Due to low stability at (50°C), there was a problem with oil and water components being separated within 24 hours of storage.

As described above, it was confirmed that the emulsion composition according to the present invention has excellent durability by creating a strong coating film on the hair after application and washing, and that the coating film improves the texture and gloss of the hair, providing an excellent feeling of use.

Claims (5)

A silicone resin containing R ₃ SiO _1/2 unit and SiO ₂ unit (where R is a straight or branched hydrocarbon group having 1 to 6 carbon atoms, or an aryl group having 6 to 12 carbon atoms) and an acrylic modified silicone copolymer Contains,
Containing 25 to 100 parts by weight of an acrylic modified silicone copolymer based on 100 parts by weight of the silicone resin,
The acrylic modified silicone copolymer is an emulsion composition represented by the following formula (1):
[Formula 1]

In Formula 1,
R ¹ is a straight-chain or branched hydrocarbon group having 1 to 10 carbon atoms,
x is an integer from 3 to 20,
y is an integer from 3 to 25,
n is an integer from 10 to 30. delete In claim 1,
An emulsion composition wherein the acrylic modified silicone copolymer has a glass transition temperature of 35 to 60°C and a silicone content of 65 to 90% by weight based on the total weight of the acrylic modified silicone copolymer. In claim 1,
The silicone resin is an emulsion composition having a viscosity of 100 cP to 1,000 cP at 25°C and a weight average molecular weight (Mw) of 1,000 to 8,000 g/mol. In claim 1,
The silicone resin is an emulsion composition in which the molar ratio (M:Q) of R ₃ SiO _1/2 unit and SiO ₂ unit is 0.3:1 to 1.5:1.