WO2014084423A1 - Pressure sensitive destructible microcapsule containing scrubbing agents, preparation method therefor, and use therefor - Google Patents

Abstract

According to the present invention, provided is a core-shell structured pressure sensitive destructible microcapsule containing scrubbing agents, comprising: a scrub core (A) comprising disintegrable or non-disintegrable scrubbing particles or granules; and a pressure sensitive destructible wall layer (B) encompassing the same, wherein the pressure sensitive destructible wall layer (B) comprises a wall-forming material, a binder and optional solid fine particles. The microcapsule containing the scrub core (A) according to the present invention has high storage durability, maintenance durability and aesthetic value, can prevent the swelling, dissolution and disintegration of scrubbing agents caused by a carrier, and can be easily destroyed by pushing, rubbing, polishing or scrubbing with the hands or a tool (cotton fabric, sponge or paper) so as to readily and rapidly supply fresh scrubbing particles with no swelling, dissolution and disintegration into a carrier, thereby improving scrubbing effects, that is, exfoliation effects.

Description

Scrub-containing destructible microcapsules, preparation method and use thereof

FIELD OF THE INVENTION The present invention relates to scrub-containing decomposable microcapsules, methods of making and uses thereof, and more particularly, to microcapsules having scrub cores containing scrub particles or granules, and microcapsules having reduced pressure destructible wall layers, To its use.

Microencapsulation is known in many fields. Microencapsulation means capturing the active ingredient or active substance in a shell and breaking or dissolving the shell under ambient conditions or under certain conditions so that the active ingredient can be released. In general, however, microencapsulation has been used in the pharmaceutical and quasi-pharmaceutical arts to slowly release or sustain the active ingredients by encapsulating the active ingredients such as drugs, vitamins or minerals in a shell which dissolves over a long time in the stomach.

The use of encapsulated materials to control release and improve the stability of the composition is well known. Encapsulation efficiency can be improved by reducing the relative percentage of protective wall material and increasing the content of encapsulated cores. It is important to maximize the absolute delivery of the encapsulated core material.

Recently, microcapsules having a pressure-destructive wall layer which can be easily destroyed or dissolved by pressing, rubbing, wiping or rubbing with a hand or a tool (cotton, sponge, paper) have been proposed in the cosmetic field and the household goods field. For example, color-changing microcapsules proposed in the cosmetic field, including cores containing colorants and pressure-destructive wall layers, include colorant cores and pressure-destructive wall layer shells, which hide or show the color of the colorants when not in use. Although not used, they are destroyed when used or applied on the skin to reveal or express the color of the colorant.

On the other hand, in modern society, due to hormonal abnormalities due to excessive stress and sudden changes in external environment, the keratin layer of the stratum corneum does not fall off or become uniform due to the effects of air pollutants or ultraviolet rays that surpass the normal defense mechanism of the skin. By falling apart, the stratum corneum is abnormally expressed.

Due to the abnormally expressed stratum corneum, the skin tone becomes uneven and the skin becomes rough and dull. In addition, the makeup looks uneven because of the uneven stratum corneum, and the so-called exhilarating makeup is performed.

In order to solve these problems various cosmetics for exfoliation have been developed. If the skin for exfoliating cosmetics is largely classified, it can be divided into chemical exfoliating cosmetics and physical exfoliating cosmetics according to the method of removing exfoliation.

Chemical exfoliation method is to remove and remove keratin with chemicals such as Alpha Hydroxy Acid (AHA) or Beta HydroxyAcid (BHA), and physical exfoliation method is to formulate a scrub and the like. It is added to the inside of the cosmetics to remove the exfoliation to remove the keratin by rubbing using a hand or a tool.

The physical exfoliation method involves scrubbing selected particles from artificial scrubs such as polyethylene, disintegrating natural scrubs such as salt or sugar, and non-disintegrating natural scrubs made by grinding seeds of fruit with seeds such as walnut shells and peaches or apricots. It is a physical removal method.

Korean Laid-Open Publication Nos. 10-1996-021004 and 10-2007-0091758 have proposed scrub formulations using a large amount of natural salt. Specifically, non-aqueous (water-containing formulations) polar solvents without water are used. The liquid crystal emulsification method using phosphorus polyol is used in excess of salt, and the scrub function is provided. However, as mentioned in the specification of the above document, in the case of oil-in-water type or water-in-oil type emulsions using water, the salt component is dissociated to drastically reduce the solubility of the surfactant. have.

Republic of Korea Patent Application No. 10-2004-0064312 and Patent Application No. 10-2007-0044437 discloses a scrub cosmetic composition comprising an excess of sugar as a natural scrub agent, where no surfactant is used to clean and rinse There is a problem with this drop and as a result there is a disadvantage of using separate face washes and other cleaning products separately.

In common scrub-containing exfoliating formulations, non-disintegrating scrubs such as fruit seed powder, rock powder or metal oxides are used. Carriers to which such non-disintegrating scrubs have a black dot appearance appear messy or esthetic Value can be low. In addition, disintegrating scrubs such as salts, sugars, sugar alcohols or other crystalline natural substances are usually white or transparent, which can be of high aesthetic value when added to a carrier and are easy to remove after use, but reduce the solubility of the surfactant and the carrier There have been many difficulties in use as scrub particles due to swelling, dissolution or disintegration.

Accordingly, there has been a need to provide a scrub-containing formulation that can enhance aesthetic value, be free of swelling, dissolution or disintegration by the carrier and prevent the reduction in solubility of the surfactant.

Provided are new scrub-containing formulations which can prevent the deterioration of the aesthetic value of the carrier by the scrub particles, prevent the swelling, dissolution or disintegration of the scrub particles by the carrier, and can prevent a decrease in the solubility of the surfactant. I would like to.

We use scrub particles or scrub granules to form a scrub-containing core and protect and hide the core with a shell comprising a pressure-destructive wall layer, any outer color layer, and an outermost protective layer. The scrub particles are not scattered in the carrier to prevent deterioration of aesthetic value and to prevent swelling, dissolution and disintegration of the scrub by the carrier, and for example, when applied or applied to the skin, the hand or tool Since the decompression-destructive wall layer can be easily destroyed by pressing, rubbing, wiping or rubbing with (cotton, sponge, paper), fresh, free of swelling, dissolution and disintegration when the microcapsules are applied or applied to the skin. The scrub particles can be easily and quickly fed into the carrier, thereby providing a scrubbing effect, i.e. The removal effect was found that could be improved.

In addition, the present inventors can further increase the storage durability, handling durability and aesthetic value of the microcapsules as well as in the carrier by further coating the outer color layer and / or the protective coating layer on the obtained microcapsules. The present invention has been found to be able to provide microcapsules that are stable and have a high aesthetic value even when added.

The scrub-containing microcapsules according to the present invention have high storage durability, handling durability and aesthetic value, can prevent swelling, dissolution and disintegration of the scrub by a carrier, and can be pressed with a hand or a tool (cotton, sponge, paper), Fresh scrub particles that are easily broken by rubbing, wiping or rubbing and are free of swelling, dissolution and disintegration can be easily and quickly supplied into the carrier, thereby improving the scrubbing effect, ie exfoliation effect.

1 is a schematic view showing a typical structure of a scrub-containing decomposable microcapsules according to the present invention,

The first object of the present invention is to include a scrub core (A) containing scrub particles or granules and a pressure-destructive wall layer (B) surrounding it, an optional outer color layer (C) and an outermost protective layer (D). In providing a scrub-containing decomposable microcapsule, the above-mentioned decompression-destroying wall layer (B) comprises a wall forming material, a binder and any micro solid particles.

It is a second object of the present invention to provide a method for preparing a scrub core-containing pressure-sensitive destructible microcapsules comprising the following steps:

(a) preparing a scrub core (A) comprising scrub particles or scrub granules,

(b) the scrub core (A) prepared in step (a) is coated with a pressure-sensitive destructive wall layer coating solution in which the wall-forming substance, the binder and any micro solid particles are dispersed or dissolved to form a pressure-destructive wall layer (B),

(c) optionally, the particles obtained in step (b) are coated with an outer color side coating solution in which the colorant, wall forming material and binder are dispersed or dissolved to form an outer color layer (C), and

(d) optionally, the particles obtained in step (b) or (c) are coated with a solution in which the shell-forming polymer is dispersed or dissolved to form the outermost protective layer (D).

The invention is explained in more detail below with reference to the drawings.

In the present invention, a scrub core-containing decomposable microcapsule comprising a pressure-destructive wall layer comprises a scrub core-containing core (A), a pressure-decomposable wall layer (B) surrounding it, an optional outer color layer (C) and an outermost layer. An outer protective layer (D) is included.

1 is a schematic view showing the structure of the particles of the color change microcapsules according to the present invention, where A is a scrub-containing core, B is a pressure-destructive wall layer, C is an outer color layer, and E is an outermost protective layer, respectively. .

1 shows particles of a scrub-containing decomposable microcapsules having a size of approximately 100-2000 μm, wherein microcapsules according to the invention are generally at least about 100 μm, preferably at least 150 μm, more preferably Is a particle size of 200 μm or more, particularly 250 μm or more, more particularly 300 μm or more, and about 2000 μm or less, preferably 1600 μm or less, more preferably 1400 μm or less, particularly 1200 μm or less, More particularly, it may have a (average) particle size of 1000 μm or less.

Alternatively, the color change microcapsules according to the present invention have an average particle size of 14 to 150 mesh (about 1300 μm to 104 μm), particularly 18 to 65 mesh (about 980 μm to 203 μm).

1. Scrub

In the context of the present invention, the term "scrub" or "scrub particles" means a granular material which is added to the exfoliating cosmetic of the skin and used to physically detach the dead skin by rubbing using a hand or a tool after application.

Scrubs can be divided into disintegratable scrubs that disintegrate or dissolve into smaller particles in the medium and, in use, non-disintegratable scrubs that can swell but not disintegrate in the medium. Disintegratable scrubs include, for example, inorganic salts such as chlorides, carbonates, hydrogencarbonates, sulfates and phosphates of alkali or alkaline earth metals; Sugar (sugar); Or erythritol (4-carbon), tracer, arabitol (5-carbon), xylitol, ribitol, mannitol (6-carbon), sorbitol, galactitol, iditol, inositol, bolitol (7-carbon) Sugar alcohols such as sugar alcohols of peat sugars; Other crystalline natural substances may be mentioned. Non-disintegrating scrubs include artificial scrubs such as polyethylene, nut shell powder, natural scrubs such as fruit seed powder, carbon black, graphite, metal oxides (e.g. silica, titania, zirconia, zinc oxide, or composite oxides thereof), rocks Mention may be made of inorganic scrubs such as powders (eg garnet powder).

Since the size of the scrub particles is rubbed directly on the skin, the particles are uniform and the size of the scrub particles is used so that the effect of exfoliation and the size of the scratches or unnecessary irritation can be minimized or minimized. If the particle size is too small, the effect of exfoliating the skin keratin is weak, if the particle size is too large, even if the peeling effect is excellent, the skin irritation is severe, causing side effects.

The size of one scrub particle is usually 20 to 200 μm, especially 30 to 150 μm, preferably 40 to 120 μm, more preferably 50 to 100 μm for non-disintegrating scrubs, and the disintegratable scrub is disintegrated or Depending on the ease of dissolution it may have a larger size than this.

However, the size of the scrub granules may be 50 to 1000 μm, particularly 60 to 900 μm, preferably 70 to 800 μm, and more preferably 80 to 600 μm.

When the size of one scrub particle acting on the skin is 200 μm or more, especially 150 μm or more, it may cause a lot of irritation to the skin. Therefore, the size of the non-disintegrating scrub or the size of the particles after the disintegrating scrub is disintegrated Care must be taken in the decision.

The scrub may be used in an amount of 95 to 30% by weight, preferably 90 to 40% by weight, more preferably 85 to 50% by weight, especially 80 to 60% by weight, based on the total weight of the microcapsules.

2. Scrub core or scrub-containing core

In the present invention, "scrub core" or scrub-containing core means a core of scrub particles or scrub granules or a core containing scrub particles or scrub granules. Specifically, it is possible to form a scrub core with a single scrub particle prepared by pulverizing the scrub raw material, and to form a scrub core with scrub granules granulated with these wall scrubbing particles and / or a binder. it means.

The scrub particles in the scrub granules may be in the form of aggregates or in a form in which the scrub particles are dispersed in a matrix of the wall forming material.

Granulation of the scrub particles can be accomplished by conventional particle forming methods, for example compression granulation (drying), spray drying, spray coagulation, emulsion, fluid bed granulation.

The amount of binder in the scrub granules is not particularly limited and may be selected from an amount such that the scrub does not detach during the coating process and / or after solvent evaporation. The amount of binder used is generally from 0.5 to 15% by weight, preferably from 1 to 10% by weight, particularly from 1.5 to 9% by weight and more particularly from 2 to 8% by weight, based on the total weight of the core.

3. Binder

Binders or coating bases are usually used to facilitate the coating process, to prevent detachment of the coating material and to improve the durability of the coating layer.

In general, as the binder or coating base, a hydrophilic coating base, a hydrophobic coating base, or a lipid-based coating base may be used. The hydrophilic coating base may be released from the pigment with the coating base to the cosmetic carrier, the hydrophobic coating base is too strong film property may cause a foreign object upon use, it is preferable to use a lipid-based coating base.

In the present invention, the binder is selected from sticky polymeric materials, lipid-based materials or mixtures thereof.

Sticky polymeric materials that can be used as binders include, for example, gelatin, starch (starch), glucose syrup, povidone (PVP), cellulose derivatives, and the like, preferably starch (eg corn star). Iii) cellulose derivatives may be used.

Lipid-based materials that can be used as binders are materials that exhibit amphiphilic properties with both polar and non-polar portions, such as stearic acid, palmitic acid, oleic acid, linoleic acid, linolenic acid, and these It may include a C ₁₂ -C ₂₂ fatty acid chain selected from the group consisting of a mixture of. The chain of fatty acids may be hydrogenated and, in some cases, form a nonpolar portion of the lipid-based material.

According to a particular embodiment of the invention, the lipid-based material is a sphingolipid such as, for example, phospholipid such as phosphatidylcholine, phosphatidylethanolamine, phosphatidic acid or phosphatidylserine, sphingosine-1-phosphate or sphingomyelin And ceramides, preferably lecithin or ceramide, which is a phospholipid mixture, particularly hydrogenated lecithin.

According to a particular variant of the present invention, since the binder can act as a wall forming material, it is possible to form the coating layer using only the binder without using a separate wall forming material. For example, corn starch may be used as a binder in the form of a corn starch binder, but may itself be used as a wall forming material.

The amount of binder used may be determined by considering the type and amount of the wall forming material as well as other components such as colorants and / or titanium dioxide particles. In general, however, the content of the lipid-based material is, based on the weight of each layer containing it, from 0.1 to 30% by weight, particularly from 0.2 to 25% by weight, preferably from 0.3 to 20% by weight and more preferably. Preferably from 0.4 to 20% by weight. When the content of the binder is less than 0.1% by weight, the fracture characteristics or dissolving ability may be lowered. When the content of the binder is 25.0% by weight or more, the durability may be degraded or the durability and stability during processing and storage may be reduced.

4. Wall Forming Material

In the present invention, since the microcapsules are often used in an aqueous medium, the wall forming material can be preferably selected from hydrophilic polymers. The term hydrophilic polymer means a (co) polymer capable of forming a hydrogen bond with water or an alcohol compound (particularly selected from lower alcohols, glycols, polyols), especially those having OH, NH and SH bonds. .

The hydrophilic polymer can be selected from the following polymers or mixtures thereof:

Acrylic or methacrylic acid homopolymers or copolymers or salts and esters thereof, in particular the product sold under the name Versicol F or Versicol K by the company Allied Colloid, the product sold as Ultrahold 8 by the company Ciba-Geigy, and Synthalen. Type K polyacrylic acids, and salts of polyacrylic acids, in particular sodium salts (corresponding to the INCI name sodium acrylate copolymer) and more particularly crosslinked sodium polyacrylates (INCI name sodium acrylate copolymers (and) Caprylic / capric triglycerides) (available under the name Luvigel EM);

Copolymers of acrylic acid and acrylamide (its sodium salt form being marketed under the name Reten by the company Hercules), sodium polymethacrylate (available under the name Darvan No. 7 by the company Vanderbilt), and polyhydroxycarboxylic acids Sodium salt of (available under the name Hydagen F from the company Henkel);

Polyacrylic acid / alkylacrylate copolymers, preferably modified or unmodified carboxyvinyl polymers; The most particularly preferred copolymers according to the invention are acrylic / C _10-30 alkylacrylate copolymers (INCI name: acrylate / C _10-30 alkylacrylate crosspolymers) under the trade name Pemulen TR1, Pemulen by the company Lubrizol. Products marketed as TR2, Carbopol 1382 and Carbopol ETD2020, more preferably Pemulen TR2;

-Copolymers of alkylacrylic acid / alkylmethacrylic acid copolymers and derivatives thereof, especially salts and esters thereof, such as ethyl acrylate, methyl methacrylate and low content methacrylic acid esters with quaternary ammonium groups ( Sold under the trade name EUDRAGIT RSPO by Evonik Degussa;

AMPS (polyacrylamidomethylpropanesulfonic acid, partially neutralized with ammonia water and highly crosslinked) (commercially available from the company Clariant);

AMPS / acrylamide copolymers, for example the product Sepigel or Simulgel, commercially available from the company SEPPIC, especially copolymers of the INCI name polyacrylamide (and) C13-14 isoparaffin (and) Laureth-7;

Polyoxyethylenated AMPS / alkylmethacrylate copolymers (crosslinked or uncrosslinked), for example types of Aristoflex HMS available from the company Clariant;

Anionic, cationic, amphoteric or nonionic chitin or chitonic acid polymers;

-Cellulose polymers and derivatives, preferably those other than alkylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxymethylcellulose, ethylhydroxyethylcellulose and carboxymethylcellulose, and also quaternized cellulose derivatives; In a preferred embodiment, the cellulose polymer is carboxymethylcellulose;

Starch polymers and derivatives, optionally modified; In a preferred embodiment, the starch polymer is a natural starch;

Vinyl polymers such as copolymers of polyvinylpyrrolidone, methylvinylether and malic anhydride, copolymers of vinylacetate and crotonic acid, copolymers of vinylpyrrolidone and vinylacetate; Copolymers of vinylpyrrolidone and caprolactam; Polyvinyl alcohol;

Optional modified polymers of natural polymers, such as kalactomannan and derivatives thereof such as konjac gum, gellan gum, locust bean gum, phenugrik gum, caraba gum, gum tragaganth, gum arabic , Acacia gum, guar gum, hydroxypropyl guar, hydroxypropyl guar modified with sodium methylcarboxylate group (Jaguar XC97-1, Rhodia), hydroxypropyltrimethylammonium guar chloride, and xanthan derivatives;

Alginates and carrageenans;

Glycoaminoglycans, hyaluronic acid and derivatives thereof;

Mucopolysaccharides such as hyaluronic acid and chondroitin sulfate, and mixtures thereof.

Preferably, the hydrophilic polymer according to the present invention may be selected from the group consisting of polysaccharides and derivatives thereof, homo / copolymers of (meth) acrylic acid or salts or esters thereof, and mixtures thereof. The aforementioned polysaccharides and derivatives may be selected from the group consisting of chitosan polymers, chitin polymers, cellulose polymers, starch polymers, galactomannan, alginate, carrageenan, mucopolysaccharides and derivatives thereof and mixtures thereof. .

In a preferred embodiment, the hydrophilic polymer contains cellulose and derivatives thereof, such as corn starch, polymethyl methacrylate, carboxymethylcellulose (CMC), cellulose esters and ethers, and aminocelluloses.

Preferred methacrylic acid and / or methacrylic acid esters alone and / or copolymers are copolymers of methyl methacrylate and ethyl acrylate having a molecular weight of 750-850 kDa.

It may be preferred that the hydrophilic polymer as wall forming material according to the invention be uncrosslinked.

5. Decompression-destructive wall layer

As used in the present specification, the term "pressure friable or pressure breakable" means easily broken by pressing, rubbing, wiping or rubbing with a hand or a tool (cotton, sponge, paper). .

In the present invention, the pressure-destructive wall layer may comprise a wall forming material and / or a binder, and in some cases may contain microsolid particles.

The thickness of the pressure-destructive wall layer varies depending on the type and content of the binder and the fine solid particles, but is usually 10 μm or more, preferably 30 μm or more, more preferably 50 μm or more, especially 80 μm or more, and more particularly Preferably it is 100 micrometers or more, Usually 300 micrometers or less, Preferably it is 250 micrometers or less, More preferably, it is 200 micrometers or less, Especially 180 micrometers or less, More specifically, it is 150 micrometers or less.

Alternatively, the pressure-destructive wall layer may be present in an amount of 5 to 70% by weight, preferably 10 to 60% by weight, more preferably 15 to 50% by weight, especially 20 to 40% by weight, based on the total weight of the microcapsules. Can be used as

6. Fine solid particles

The pressure-destructive wall layer of the present invention may contain microsolid particles, which microparticles serve to rupture or destroy the pressure-destructive wall layer, specifically the wall forming material layer, in an irreversible manner. To promote or increase disintegration or dissolution. Furthermore, these microsolid particles are believed to play an important role in the strength, durability, decompression fracture, and post-peelability of the decompression-destructive wall layer.

The microsolid particles include, for example, inorganic salts such as chlorides, carbonates, hydrogen carbonates, sulfates, and phosphates of alkali or alkaline earth metals; Sugar (sugar); Or erythritol (4-carbon), tracer, arabitol (5-carbon), xylitol, ribitol, mannitol (6-carbon), sorbitol, galactitol, iditol, inositol, bolitol (7-carbon) Sugar alcohols such as sugar alcohols of peat sugars; Other crystalline natural substances; Polymeric particles such as polyethylene; Natural vegetable particles such as nut shell powder, fruit seed powder; Inorganic particles such as carbon black, graphite, metal oxides (eg silica, titania, zirconia, zinc oxide, or composite oxides thereof), rock powders (eg garnet powder) may be mentioned.

The average particle size or size of the fine solid particles is not particularly limited, but is usually 10 nm to 20 μm, preferably 50 nm to 10 μm, more preferably 100 nm to 5 μm, and particularly 150 nm to 2 μm. If the average particle size or size of the microsolid particles is 10 nm or less, the decompression performance is reduced. Titanium dioxide particles having a primary particle size smaller than the above range but having a secondary particle size corresponding to the above range may also be used in the present invention.

The amount of the fine solid particles in the pressure-destructive wall layer is 5 to 99% by weight, preferably 10 to 95% by weight, more preferably 15 to 90% by weight, particularly 20 to 85% by weight, based on the total weight of the wall layer. Can be used as

According to one embodiment of the invention, the microsolid particles can be made of the same material as the above-described scrub, preferably in metal oxides such as alumina, silica, titania, zirconia, zinc oxide, or composite oxides thereof. The microcapsules can be colored white by including the selected microsolid particles in the pressure-destructive wall layer.

According to one embodiment of the present invention, the microsolid particles may preferably use water-soluble or water-dispersible microsolid particles.

7. Outer Color Layer

The microcapsules according to the present invention may further have an outer color layer (hereinafter referred to as an outer color layer) outside the pressure-destructive wall layer. The outer color layer (outer color layer) is a solution containing a colorant and a binder and is formed by coating the pressure-sensitive destructible wall layer, for example, by fluidized bed coating.

The wall forming material and binder contained in the outer color layer may be the same or different from that of the core and / or pressure-destructive wall layer.

Generally, it can be installed to impart to the microcapsules a color other than the color expressed by the decompression destructive wall layer, so that the colorant in an amount such that it does not disturb the color of the medium itself when the microcapsules are applied to the skin and used. May be contained, or if necessary, in an amount capable of expressing a desired color by disturbing the color of the medium itself.

The content of the outer layer may be selected from 1 to 60 parts by weight, preferably 2 to 50 parts by weight, more preferably 3 to 40 parts by weight, particularly 4 to 30 parts by weight based on the total weight of the core. The content of the outer layer colorant may be selected from 10 to 90 parts by weight, preferably 15 to 85 parts by weight, more preferably 20 to 80 parts by weight, and particularly 25 to 75 parts by weight based on the weight of the outer layer. Can be.

8. Outermost protective layer

The microcapsules according to the present invention further install a protective outermost protective layer on the outside of the decompression decomposable wall layer or an additional outer color layer to protect the microcapsules from moisture in the air during storage or in a cosmetic carrier medium such as water or alcohol. Long-term stability of the microcapsules can be ensured.

The outermost protective layer may be made of a shell-forming polymer selected from the group consisting of shellac, polyacrylates, polymethacrylates, cellulose ethers, cellulose esters, polystyrene maleic hydride copolymers or mixtures thereof. Can be.

The outermost protective layer is preferably included in an amount of 0.1 to 20.0% by weight, preferably 0.5 to 15% by weight relative to the total weight of the microcapsules. If the content of the outermost protective layer is less than 0.1% by weight, there is no meaning of coating, and when it exceeds 20.0% by weight, foreign matter may occur.

9. Colorant or Pigment

In the present invention, "colorants" or pigments include organic or inorganic pigments, dyes or lakes of synthetic or natural origin, and colorants approved for use in cosmetics by CTFA and FDA used in cosmetic formulations.

In the present invention, the colorant may be water soluble or water dispersible, or may be oil-soluble or oil-phase or limited solubility in water.

In the present invention, the colorants are organic pigments such as well-known FD & C or D & C dyes, inorganic pigments such as metal oxides, or rakes such as cochineal carmine, barium, strontium, calcium or aluminum and these Mention may be made of those based on any combination of.

In the present invention, the following may be mentioned as colorants:

-Carmin of cochenille;

Organic pigments such as azo, anthraquinone, indigo, xanthene, pyrene, quinoline, triphenylmethane, fluorane colorants;

Insoluble in sodium, potassium, calcium, barium, aluminum, zirconium, strontium, titanium of acid colorants such as azo, anthraquinone, indigo, xanthene, pyrene, quinoline, triphenylmethane, and fluorane colorants Salts, these colorants may comprise at least one carboxyl or sulfonic acid group.

As specific examples of the organic pigments, those having the following trade names may be mentioned:

-D & C Blue No.4, D & C Brown No.1, D & C Green No.5,

-D & C Green No.6, D & C Orange No.4, D & C Orange No.5, D & C Orange No.10,

-D & C Orange No.11, D & C Red No.6, D & C Red No.7, D & C Red No.17, D & C Red No.21, D & C Red No.22, D & C Red No.27, D & C Red No.28, D & C Red No.30, D & C Red No. 31, D & C Red No.33, D & C Red No.34, D & C Red No.36, D & C Violet No.2, D & C Yellow No.7, D & C Yellow No.8, D & C Yellow No.10, D & C Yellow No.11, FD & C Blue No.1,

-FD & C Green No.3, FD & C Red No.40, FD & C Yellow No.5, FD & C Yellow No.6.

In one embodiment, the colorant is an inorganic pigment, preferably a metal oxide selected from iron oxide, specifically iron oxide, titanium dioxide, aluminum oxide, zirconium oxide, cobalt oxide, cerium oxide, nickel oxide, tin oxide or zinc oxide Oxide, or a complex oxide, more preferably iron oxide selected from red iron oxide, yellow iron oxide or black iron oxide, or mixtures thereof.

One skilled in the art knows how to choose a colorant and colorant combination that can give the desired color effect or color change.

On the other hand, some colors can be realized by one colorant, but most colors are realized by changing the composition ratio of a mixture of various colorants. Thus, in the present specification, the colorant or one colorant may be used in the sense encompassing not only one colorant but also one or more colorant mixtures, unless specifically limited.

10.COLOR-CHANGING MICROCAPSULES

According to the present invention, the term microcapsule is a substantially spherical microcapsule containing at least one layered coating containing at least one colorant and a core surrounded by and chemically different from the coating. Means.

The term multi-layer microcapsule means a microcapsule consisting of an inner core and one outer layer surrounded by a coating based on one or a plurality of inner layer (s). One or multiple inner layer (s) forming a multilayer coating of multilayer microcapsules and a single outer layer of multilayer microcapsules may be formed of the same or different wall-forming organic compounds.

The microcapsules of the present invention are pressure friable that are easily destroyed, ruptured, dissolved and / or disintegrated (hereinafter referred to as breaking) by hand, by means of pressing, rubbing, wiping, or rubbing with a hand or a tool (cotton, sponge, paper). or pressure breakable).

Microcapsules having a pressure-destructive wall layer according to the present invention may be prepared by a fluidized bed process or a similar process. Granulation by spray drying leads to granulation by agglomeration of particles, while fluid bed processes lead to capsules of layered core-shell structures in the form of concentric circles.

11. Fluidized Bed Coating Process

Microencapsulation by fluid bed coating processes is described, for example, in Fluid-Bed Coating, Teunou, E .; Poncelet, 2005, D. Food Science and Technology (BocaRaton, FL, United States), Volume 146 Issue Encapsulated and Powdered Foods, Pages 197-212.

The fluidized bed coating process is called the Wurster process and / or tangential spray process and is commonly used for the preparation of microcapsules with particle size of 50 to 500 μm and microencapsulation with particle size of 35 to 5000 μm. It is known that it is possible to manufacture. Fluidized bed coating processes are cost effective and standardized on some encapsulated foods or drugs. Not only is it possible to produce large particles, but also has the advantage that the particle size and shape are constant.

One skilled in the art can know the amount of air, liquid amount and temperature which makes it possible to produce reproducibly the microcapsules according to the invention.

Preferably, the fluidized bed process carried out is a Wuster process and / or a tangential spray process. These processes make it possible to lead to spherical capsules with a core surrounded by one or more outer layers as opposed to a pelletization process.

The coating liquid used in the fluidized bed process of the present invention may use water, preferably purified water, or a low boiling point organic solvent. In the present invention, a low boiling point organic solvent means an organic solvent having a boiling point of about 100 ° C. or lower, and for example, methylene chloride, methanol, ethanol, or a mixture thereof may be mentioned. In the present invention, as the organic solvent, any solvent capable of dissolving or dispersing the wall-forming material and / or the lipid-based material, having a boiling point lower than water and having low residual toxicity can be used.

*****

In the present invention, according to a preferred embodiment, the microcapsules comprise a lipid-based material selected from a lipid-based material selected from phospholipids, advantageously phosphoacylglycerols such as lecithin.

In a particularly preferred embodiment, the core may comprise cosmetic substances such as vitamins, perfumes, etc., in addition to the scrub.

The prepared microcapsules are all types of emulsion formulations, such as water in oil (W / O), oil in water (O / W), water in silicone (W / S), and silicone in water (S / W). It can be used in emulsion formulations of the type.

Traditional non-disintegrating scrubs such as fruit seed powder, rock powder or metal oxides are commonly used in conventional scrub-containing exfoliating formulations. Carriers added with such non-disintegrating scrubs have a blackish appearance and appear dirty. Aesthetic value can be low. However, in the present invention, the aesthetic value of the carrier may be high because the scrub particles are collected and concealed in the microcapsules, and thus, the aesthetic value of the carrier may be high. Since it is supplied into the carrier, the exfoliation effect may be high.

Disintegratable scrubs, such as salt, sugar, sugar alcohols or other crystalline natural substances, are usually white or transparent, which can be of aesthetic value when added to a carrier and are easy to remove after use, but may be caused by swelling, dissolution or disintegration by the carrier. Due to this, there are many difficulties in use as the scrub particles, so the use thereof has been limited.

According to the present invention, such disintegrable scrub particles or particles can be collected and concealed in microcapsules to prevent swelling, dissolution or disintegration by carriers, as well as breaking microcapsules in use to swell, dissolve or Since the fresh scrub particles without disintegration can be supplied into the carrier, the exfoliation effect can be enhanced.

In addition, conventional scrub formulations may retain particles intact initially due to the surfactant when including the disintegratable scrub formulation, but over time the disintegratable scrub formulation will dissolve or disperse in a water based carrier. Therefore, due to the disintegratable scrub component dissolved into the carrier, there is a high possibility that the phase separation of the surfactant occurs during storage or the foaming of the surfactant does not occur properly in use. On the other hand, according to the present invention, the scrub-containing microcapsules do not have a disintegratable scrub component dissolved into the carrier, and since the scrub particles are supplied into the carrier during use, no phase separation of the surfactant occurs during storage, and the scrub even when used Even if the particles disintegrate, it takes time to dissolve into the carrier, so that the foaming of the surfactant is hardly disturbed.

The microcapsules according to the present invention are added to a water-based carrier and are not destroyed even after prolonged swelling. The microcapsules according to the present invention can be decomposed by a suitable physical stimulus such as rubbing, rubbing, pressing, etc., when using the swollen microcapsules. This disintegrates or dissolves and disappears into the carrier, leaving only the scrub core inside. When the scrub core is in the form of granules, the disintegrating or dissolving step of the wall forming material of the scrub core proceeds after the pressure-destructive wall layer disappears, so that the scrub particles are present with little influence on the carrier or the surfactant. Interact with. Thus, the scrub particles have a form that is freshly provided in the carrier and can act for the maximum time as a scrub agent.

In the following, the present invention is explained in more detail based on Examples, but the present invention is not limited by the following Examples. Unless otherwise specified in the examples, the percentages and ratios are based on weight, and the trade names are indicated as they are if the substance or substance contained is clear.

Example 1 :

First, charcoal powder was pulverized and classified to obtain 30 to 40 mesh (420 to 590 μm) of hard graphite particles, which were used as a scrub core.

Zea mays corn starch is gelatinized in purified water at 80 ℃ or higher to make corn starch binder coating liquid, and then soft graphite powder (smaller particle size than hard graphite used as scrub core), corn starch (Zea) mays corn starch) was added and dissolved or dispersed at 40 ° C. to prepare a pressure-sensitive destructive wall coating solution.

The obtained hard graphite particles were introduced into a fluidized bed coating system (Glatt GPOG 1, Rotor spray system) and coated with the obtained pressure-degradable wall layer coating liquid to obtain pressure-destructive microcapsules containing graphite particles as a scrub-particle core. .

The obtained microcapsules have a particle size of approximately 650 ~ 850㎛ and the composition of Table 1 below.

Table 1

Microcapsules	matter	Content (% by weight)
Scrub-Containing Core (A)	Hard graphite particles	20
Decompression Wall Layers (B)	Soft graphite particles	50
	Corn starch	22.3
	Corn starch binder	7.7

When the obtained decomposable microcapsules are added to a water-based carrier, applied to the skin and rubbed by hand, it can be seen that the decomposable wall layer disappears and the hard graphite particles remain in the carrier to act as scrub particles.

Example 2 :

Except for using hydrogenated lecithin instead of corn starch binder (corn starch aid), the same procedure as in Example 1 was carried out to obtain a pressure-destructive microcapsules containing graphite particles as a scrub-particle core.

Example 3 :

Except for using titanium dioxide particles in place of soft graphite particles, the same procedure as in Example 1 was carried out to obtain a pressure-sensitive destructible microcapsules containing graphite particles as a scrub-particle core. The microcapsules obtained in this example have white color.

It can be seen that when the obtained decomposable microcapsules are added into a water-based carrier, applied to the skin and rubbed by hand, the white decomposable wall layer disappears and black hard graphite particles remain in the carrier to act as scrub particles.

Comparative Example 1 :

The same procedure was followed as in Example 1 except that the core composed of microcrystalline cellulose, mannitol and corn starch was used in place of hard graphite, to obtain a pressure-destructive microcapsules containing no scrub-particles.

The obtained pressure-sensitive destructible microcapsules were added in a carrier and applied to the skin and rubbed by hand, all disappearing without leaving any grains.

Example 4 :

Corn starch and hydrogenated lecithin were added to a mixed solvent of methylene chloride and ethanol and dissolved at 40 ° C. Iron oxide, red iron oxide, and black iron oxide were added thereto in a weight ratio of 1.26: 0.252: 45.36, and homogeneously dispersed to prepare an outer color layer solution having a brown color.

Graphite-containing pressure-sensitive destructible microcapsules prepared in Example 1 were introduced into a fluidized bed coating system (Glatt GPCG 1, Rotor system) and coated with the prepared external color layer solution, A capsule (outer brown) was obtained.

When the obtained pressure-sensitive destructible microcapsules were added in the carrier and applied to the skin and rubbed by hand, it can be seen that the brown outer color layer disappeared and the black hard graphite particles remained in the carrier to act as scrub particles.

Example 5 :

Corn starch was gelatinized in purified water at 80 ° C. or higher to form a corn starch binder coating solution, and then corn starch and hydrogenated lecithin were added and dissolved or dispersed at approximately 40 ° C., and titanium dioxide (TiO ₂₎ having an average particle size of 200 to 400 nm. ) Was added and dispersed well with a homogenizer to prepare a pressure-degradable wall layer coating solution.

The graphite-containing pressure-sensitive destructible microcapsules (external color black) prepared in Example 1 were introduced into a fluidized bed coating system (Glatt GPCG 1, bottom spray) and coated with the pressure-sensitive decomposable wall layer coating liquid prepared above, thereby preparing the graphite-containing pressure-sensitive destructible microcapsules. A capsule (outer color white) was obtained.

Example 6 :

Corn starch was gelatinized in purified water at 80 ° C. or higher to prepare a corn starch binder coating solution, and then corn starch and hydrogenated lecithin were added and dissolved or dispersed at approximately 40 ° C. to prepare a pressure-sensitive breakable wall coating.

The pulverized sun salt (NaCl) powder was introduced into the fluidized bed coating system (Glatt GPCG 1) as a scrub particle and coated with the prepared pressure-degradable wall layer coating solution, thereby obtaining sodium chloride-containing pressure-sensitive destructible microcapsules.

When the obtained pressure-sensitive destructible microcapsules were added in a carrier and applied to the skin and rubbed by hand, all of the microcapsules appeared to be lost, but the texture of sodium chloride particles in the carrier was felt for a while and acted as scrub particles until disappeared. Can be.

Example 7 :

In the same manner as in Example 1 except using commercially available polyethylene (INDUCOS 13/3, Lipo Chemicals) having a particle size of 20 ~ 200㎛ instead of hard graphite particles, a reduced pressure having a composition shown in Table 2 Destructive microcapsules were obtained. The obtained microcapsules have a particle size of approximately 200 ~ 400㎛.

TABLE 2

Microcapsules	matter	Content (% by weight)
Scrub-Containing Core (A)	Polyethylene beads	9
Decompression Wall Layers (B)	Microcrystalline cellulose	22
	Mannitol	28
	Titanium dioxide	35
	Hydrogenated Lecithin	One
	Corn starch binder	5

Example 8 :

First, charcoal powder was pulverized and classified to obtain hard graphite microparticles having a diameter of 50 to 100 µm.

Corn starch is gelatinized in purified water at 80 ° C. or higher to form a corn starch binder coating solution, and then corn starch and hydrogenated lecithin are added and melted at about 40 ° C. to prepare a coating liquid. Granulated to a size 300-500 μm.

Corn starch was gelatinized in purified water at 80 ° C. or higher to form a corn starch binder coating solution, and titanium dioxide particles, zea mays corn starch, and hydrogenated lecithin were added and dissolved at about 40 ° C. Titanium dioxide (TiO ₂ ) having a particle size of 200-400 nm was added thereto and dispersed well with a homogenizer to prepare a titanium dioxide particle layer coating solution.

The obtained graphite granules were coated with the obtained titanium dioxide particle layer coating solution in a fluidized bed coating system (Glatt GPCG 1, Rotor spray system) to obtain a pressure-destructive microcapsules having a graphite-containing core and a titanium dioxide particle layer. The microcapsules obtained had the composition shown in Table 3 below and had an average size of 500-700 μm.

TABLE 3

Microcapsules	matter	Content (% by weight)
Scrub-Containing Core (A)	Graphite granules	68
Decompression Wall Layers (B)	Microcrystalline cellulose	11
	Titanium dioxide	17
	Hydrogenated Lecithin	One
	Corn starch binder	5

Example 9 :

Corn starch was gelatinized in purified water at 80 ° C. or higher to form a corn starch binder coating solution, and titanium dioxide particles, corn starch and hydrogenated lecithin were added and dissolved at about 40 ° C. Polyethylene beads (INDUCOS 13/3, Lipo Chemicals) having a particle size of 50-200 μm were added to the resulting reaction mixture and dispersed well to prepare a scrub-containing solution, and granulated to obtain polyethylene beads dispersed in a matrix. A scrub-containing core granule having a form was obtained.

Hydrogenated lecithin, PMMA (polymethyl methacrylate) and corn starch were added to a mixed solvent of methylene chloride and ethanol (weight ratio 1: 1) and dissolved at approximately 40 ° C. Titanium dioxide particles were added to the resulting reaction mixture and well dispersed to prepare a titanium dioxide particle coating solution.

The obtained scrub-containing core granules were coated with the obtained titanium dioxide particle layer coating liquid in a fluidized bed coating system (Glatt GPCG 1, bottom spray) to obtain a pressure-destructive microcapsules having a scrub-containing core and a titanium dioxide particle layer. The obtained microcapsules had the composition shown in Table 4 below and the average size was 400 to 600 µm.

Table 4

Microcapsules	matter	Content (% by weight)
Scrub-Containing Core (A)	Scrub particles	67.8
	Hydrogenated Lecithin	0.2
	Corn starch binder	2.0
Decompression Wall Layers (B)	Titanium dioxide	24.5
	Hydrogenated Lecithin	2.5
	PMMA	1.5
	Corn starch	1.0

The color scrub-containing decomposable microcapsules according to the present invention can be usefully used in the field of scrub preparation and cosmetics containing the same.

Claims (16)

1. A core-shell structured microcapsule comprising a scrub core (A) containing scrub particles or granules and a pressure-destructive wall layer (B) surrounding it, wherein the pressure-destructive wall layer (B) described above comprises a wall forming material and a binder. A scrub-containing decomposable microcapsule, characterized in that it comprises.
2. 2. The scrub-containing decomposable microcapsule according to claim 1, wherein the aforementioned wall forming material is selected from the group consisting of hydrophilic polymer, hydrophilic modified cellulose and hydrophilic natural material.
3. The scrub-containing decomposable microcapsule of claim 1, wherein the binder described above is a tacky polymeric material, a lipid-based material or a mixture thereof.
4. The scrub-containing decompression-decomposing microstructure according to claim 1, wherein the pressure-decomposable wall layer (B) described above may further include microsolid particles in an amount of 5 to 99% by weight based on the total weight of the wall layer. capsule.
5. The scrub-containing pressure-decomposable microcapsule according to claim 1, wherein the pressure-destructive wall layer (B) has a thickness of 10 to 300 µm.
6. 2. The scrub-containing decomposing microcapsules according to claim 1, further comprising the following outer color layer (C), outermost protective layer (D), or both on the above-described decompression-destructive wall layer (B). :

   (C) an outer color layer comprising a colorant, a wall forming material and a binder

   (D) outermost protective layer comprising shell-forming polymer (D)
7. 7. The shell-forming polymer according to claim 6, wherein the shell-forming polymer described above is selected from the group consisting of shellac, polyacrylate, polymethacrylate, cellulose ether, cellulose ester, polystyrene maleic hydride copolymer or mixtures thereof. Scrub-containing decomposable microcapsules, characterized in that the.
8. The method of claim 1, wherein the scrub is a disintegratable scrub selected from the group consisting of inorganic salt particles, sugar particles, sugar alcohol particles, particles of crystalline natural substances, or polymeric particles, plant particles, metal oxide particles, inorganic particles. Scrub-containing pressure-sensitive destructible microcapsule, characterized in that the non-disintegratable scrub selected from the group consisting of.
9. 9. The method of claim 8, wherein the disintegratable scrub is an inorganic salt particle of chloride, carbonate, hydrogen carbonate, sulfate, phosphate, ammonium salt of alkali metal or alkaline earth metal; Sugar (sugar) particles; Scrub-containing pressure-sensitive destructible microcapsules, characterized in that selected from the group consisting of sugar alcohol particles.
10. 9. The method of claim 8, wherein the non-disintegrating scrubs comprise polyethylene particles; Nut shell powder particles, fruit seed powder particles, cellulose particles, fiber particles; Silica, titania, zirconia, zinc oxide, or composite oxide particles thereof; Scrub-containing pressure-sensitive destructible microcapsules, characterized in that selected from the group consisting of carbon black, graphite, garnet powder, natural rock powder.
11. 2. The scrub-containing decomposable microcapsule having a decompression-destructive wall layer according to claim 1, characterized in that the average particle size is 100-2000 mu m.
12. A process for preparing a scrub-containing decomposable microcapsule according to claim 1, comprising the following steps (a) and (b):

    (a) preparing a scrub core (A) comprising scrub particles or granules, and

    (b) The scrub core (A) prepared in step 1) is coated with a pressure-sensitive destructive wall layer coating solution in which the wall-forming substance and the binder are dispersed or dissolved to form a pressure-destructive wall layer (B).
13. 13. The method of claim 12, further comprising one or both of the following steps (c) and (d):

    (c) coating the particles obtained in step (b) with an outer color coating solution in which the colorant, wall forming material and binder are dispersed or dissolved, to form an outer color layer (C), and

    (d) The particles obtained in step (b) or (c) are coated with a solution in which the shell-forming polymer is dispersed or dissolved to form the outermost protective layer (D).
14. 14. A method according to claim 12 or 13, wherein the coating in each of the aforementioned steps (a), (b), (c) or (d) is carried out in a fluidized bed process. Manufacturing method.
15. The method of claim 12 or 13, wherein the coating liquid described above uses at least one member selected from the group consisting of water, methylene chloride, methanol and ethanol as a solvent.
16. Cosmetics comprising the scrub-containing pressure-destructive microcapsules according to claim 1.

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