JP2006327961A - Cosmetic - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a cosmetic capable of being controlled in an abrasive feeling, while keeping a function of adsorbing or removing waste matter derived from bacteria, viruses, etc., or from sebum. <P>SOLUTION: This cosmetic is compounded from 0.1-50 mass% of amorphous calcium phosphate-coated sericite particles which are formed by coating sericite particles with amorphous calcium phosphate, wherein the amorphous calcium phosphate-coated sericite particles are produced by a production method in which an acid treatment process, a washing process, an alkali process, and calcium phosphate-coating process are conducted. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a cosmetic using amorphous calcium phosphate composite particles.

  Conventionally, natural or man-made clay minerals such as talc, kaolin (white clay), bentonite, mica group minerals (sericite, muscovite, phlogopite, biotite), calcined kaolin, etc., which have a scaly or plate-like particle shape. And processed products thereof, or surface treated products (hereinafter collectively referred to as “clay minerals”) are excellent in slipperiness to the skin due to their particle shape, so that powder white powder, solid white powder, foundation, etc. As a main ingredient of so-called powder base makeup cosmetics, in particular, extender pigments that diminish the color of color pigments, or adsorbents that adsorb sebum (oil) and sweat (moisture) that are secretions from the skin It has been widely used as a component having several functions.

  Of these, talc is transparent, and has a characteristic that the touch when applied to the skin is particularly smooth and has excellent adhesion. Kaolin is inferior to talc in terms of smoothness, but has a relatively large adsorption power for adsorbing secretions from the skin and a concealing power for concealing the foundation, and it exhibits weak acidity suitable for skin health. It has the characteristic.

  Therefore, until now, these two parties have often been used in combination as main ingredients of base makeup cosmetics. Recently, however, sericite, which has a highly transparent makeup effect even with mica group minerals, and titanium oxide-coated particles with pearly luster (such as titanium mica) are also used for base makeup cosmetics with a new cosmetic feel. The demand is expanding.

Especially for sericite, it is popular among clay minerals, and domestic high-purity raw materials are scarce or expensive, and raw materials with low purity from overseas are imported, refined and used. This is the current situation. For this reason, sericite and other mica group minerals are usually distinguished by the names “sericite” and “mica”.
Titanium oxide-coated particles such as titanium mica are processed products in which fine particles of titanium oxide with a high refractive index are coated on the surface of pulverized materials such as muscovite and phlogopite, sericite, talc, synthetic mica, etc. Depending on the thickness of the titanium layer, various interference colors are produced, which are preferred as pearl luster. Furthermore, in recent years, products that have been coated with iron oxide or chromium oxide instead of titanium oxide, titanium oxide that has been further coated with iron oxide or chromium oxide, or those that are combined with dyes or pigments have been developed. It is called pearl pigment or pearl luster pigment. This pearl pigment is titanium mica, bengara-coated mica, bengara-coated titanium mica, black iron oxide-coated titanium mica, carmine-coated titanium mica, conjugate-coated titanium mica, carmine-conjugate-coated titanium mica, chromium oxide-coated titanium mica, bengara-black Iron oxide coated titanium mica, black iron oxide carmine coated titanium mica, black iron oxide conger coated titanium mica, titanium mica + yellow 4, titanium mica + red 202, titanium mica + blue 1, titanium mica + blue 1 + Yellow 4 and so on.

  In actual use, these clay minerals, that is, mineral particles having a scaly or plate-like particle shape, are appropriately blended according to the purpose, and a small amount of oily components, coloring pigments, and the like. A base makeup cosmetic is produced by mixing with the above ingredients.

The inventor previously incorporated amorphous calcium phosphate with excellent functions to adsorb and remove excess sebum on the skin, bacteria and viruses that live there, and viruses, thereby causing rough skin and inflammation caused by acne. Has been proposed to maintain the skin in a normal state and to prevent makeup loss due to waste products and to make the makeup last longer (Patent Document 1).
Patent Document 2 discloses that in a water system in which a pigment is dispersed, a water-soluble calcium salt and water-soluble phosphoric acid or water-soluble phosphate are gradually reacted to form hydroxyapatite and / or phosphoric acid on the pigment surface. A coated pigment for depositing tricalcium and a cosmetic using the coated pigment are described.

However, the amorphous calcium phosphate particles, especially when used in the above-mentioned base makeup cosmetics, or cosmetics such as eye shadows and lipsticks that are applied to the skin, may cause a tingling sensation and may be uncomfortable. It may not be possible to add a large amount.
In view of this, the inventor provided amorphous calcium phosphate composite particles characterized by coating the surface of scaly or plate-like substrate particles such as sericite with fine particles of amorphous calcium phosphate and cosmetics using the same. It has been proposed (Patent Document 3).
However, such amorphous calcium phosphate composite particles also tend to generate a squeaking feeling compared to the case of only the base particles, and have a problem that squeaking sensation occurs when incorporated in a large amount in cosmetics. On the other hand, the function of adsorbing and removing so-called waste products such as sebum, bacteria, and viruses may not be fully satisfactory unless a large amount of such amorphous calcium phosphate composite particles are added to the cosmetic. ing.
That is, the conventional cosmetics have a problem that it is difficult to suppress the feeling of squeaking while maintaining the function of adsorbing and removing so-called waste products such as sebum, bacteria, and viruses.

JP-A-8-133842 Japanese Patent No. 2914460 JP 2000-169122 A

  It is an object of the present invention to provide a cosmetic material that has a function of adsorbing and removing so-called waste products such as sebum, bacteria, viruses, and the like, while suppressing the squeaky feeling.

The present inventor has found that the surface of the amorphous calcium phosphate-coated particles is covered with the amorphous calcium phosphate and the squeakiness is related, that is, there is a part that is not coated with the amorphous calcium phosphate. It has been found that a feeling of squeaking can be suppressed by suppressing non-uniformity of the amorphous calcium phosphate covering the surface of the particles. Moreover, it discovered that adsorption | suction performance could be improved compared with the thing which is not uniformly coat | covered by coat | covering the surface of a base particle uniformly with an amorphous calcium phosphate.
Therefore, as a result of intensive studies on more uniformly covering the surface of scaly or plate-like substrate particles such as sericite with fine particles of amorphous calcium phosphate, amorphous calcium phosphate was applied to sericite by a predetermined method. As a result of the coating, it was found that the portion not coated with amorphous calcium phosphate can be reduced as compared with conventional amorphous calcium phosphate composite particles, and the present invention has been completed.

  That is, in order to solve the above-mentioned problems, the present invention contains 0.1 to 50% by mass of amorphous calcium phosphate-coated sericite particles obtained by coating sericite particles with amorphous calcium phosphate, and the amorphous calcium phosphate. An acid treatment step in which the coated sericite particles are (1) mixed with sericite particles and an acid having a pH of 1.5 or less to wash the surface of the sericite particles with an acid having a pH of 1.5 or less; (2) sericite Washing for washing the sericite particles treated in the acid treatment step so that the pH of the suspension in which the site particles are dispersed in water at a solid concentration of 0.1 to 50% by mass is 2.0 or more. Step, (3) an alkaline step of preparing an alkaline suspension in which the sericite particles washed by the washing step and calcium hydroxide are mixed, and (4) produced in the alkaline step. Provided is a cosmetic manufactured by a manufacturing method in which a calcium phosphate coating step of coating the surface of sericite particles with amorphous calcium phosphate by adding phosphoric acid to an alkaline suspension is provided. To do.

According to the present invention, the amorphous calcium phosphate-coated sericite particles wash the surface of the sericite particles with an acid having a pH of 1.5 or less by mixing the sericite particles with an acid having a pH of 1.5 or less. Acid treatment step, sericite treated in the acid treatment step so that the pH of a suspension in which sericite particles are dispersed in water at a solid content concentration of 0.1 to 50% by mass is 2.0 or more A washing step for washing particles, an alkaline step for preparing an alkaline suspension in which calcium hydroxide is mixed with sericite particles washed by the washing step, phosphoric acid in the alkaline suspension created in the alkaline step Since the calcium phosphate coating process in which the surface of the sericite particles is coated with amorphous calcium phosphate is added and added, amorphous calcium phosphate Surface not coated with amorphous calcium phosphate portion of the coated sericite particles can be prevented from being generated.
Therefore, the cosmetic containing the amorphous calcium phosphate-coated sericite particles can have a feeling of squeaking while maintaining the function of adsorbing and removing so-called waste products such as sebum, bacteria, and viruses.

The preferred embodiments of the present invention will be described below.
First, a method for producing amorphous calcium phosphate-coated sericite particles used in the cosmetic of the present embodiment will be described.
Sericite particles are used as the base particles of the amorphous calcium phosphate-coated sericite particles in the present embodiment.
Further, in the method for producing amorphous calcium phosphate-coated particles of the present embodiment, an acid treatment step of mixing the sericite particles and an acid and washing the surface of the sericite particles with an acid having a pH of 1.5 or less; A washing step for washing the sericite particles treated in the acid treatment step so that the pH of the suspension in which the site particles are dispersed in water at a solid content concentration of 0.1 to 50% by mass is 2.0 or more. An alkaline step of preparing an alkaline suspension obtained by mixing sericite particles and calcium hydroxide washed in the washing step, and adding phosphoric acid to the alkaline suspension prepared in the alkaline step. The surface of the sericite particles is coated with amorphous calcium phosphate by performing a calcium phosphate coating process in which the surface of the sericite particles is coated with amorphous calcium phosphate. That.

In the acid treatment step, deposits such as iron, titanium, calcium, silicon, aluminum, potassium, and magnesium adhering to the surface of the sericite particles by acid are removed as deposit ions from the surface of the sericite particles. Suppresses aggregation of sericite particles. As this acid treatment step, it is possible to employ a general granular washing method such as a method of showering acidic liquid on sericite particles or a method of immersing and washing sericite particles in acidic liquid. From the viewpoint that the site particles can be uniformly and sufficiently treated as a whole, it is preferable to perform a method of immersing and washing the sericite particles in an acidic liquid.
In this respect, the solid content concentration of the sericite particles dispersed in the acid during pickling is preferably 0.1 to 50% by mass, more preferably 1 to 50% by mass. More preferably, it is 5-30 mass%. The solid content concentration is preferably within such a range. When the solid content concentration exceeds 50% by mass, the effects such as the removal of the adhering ions and the suppression of the aggregation described above are uniformly and sufficiently applied to the entire substrate material. Even if the solid content concentration is less than 0.1% by mass, not only can the above-mentioned effects be expected to be more uniform and sufficient, but also the equipment to be used becomes large. This is because there is a possibility that productivity may be lowered, for example, the amount of amorphous calcium phosphate-coated sericite particles obtained with respect to the amount of acid used is reduced.

The acid used in the method of immersing and washing sericite particles in this acidic liquid is not particularly limited, but is usually a strong acid such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, etc. used for iron removal, citric acid, etc. Weak acids such as malic acid, acetic acid and oxalic acid can be used alone or in combination. Further, these acids can be used in the same concentration or diluted. In addition, as such an acid, it can suppress that the calcium ion added at a latter alkali process is consumed by anions other than a phosphate ion, and in the calcium phosphate coating | coated process, on the surface of a sericite particle | grain. It is preferable to use phosphoric acid because it can produce amorphous calcium phosphate more efficiently.
Furthermore, when phosphoric acid is used, the surface of sericite can be coated with finer amorphous calcium phosphate than when using an acid other than phosphoric acid, and the amorphous calcium phosphate-coated sericite can be coated. This is preferable in that the structure of the amorphous calcium phosphate covering the particles can be made close to a sphere, and the feeling of squeaking can be further reduced (slidability can be improved).

As the sericite particles, at least one selected from untreated sericite particles and sericite particles made into pearl pigments is used. As such sericite particles, those having an average particle diameter of 1 to 100 μm can be used. In addition, the said average particle diameter in this specification means the value of 50 vol% of the curve which shows the cumulative particle size distribution calculated | required by the laser diffraction method, for example, the brand name of "Rodos" from Japan Laser Corporation. It can be measured by a commercially available laser diffraction type particle size distribution measuring device.
In addition, such sericite particles are not particularly limited in terms of dimensions, but in order to maintain the above-mentioned slipperiness to the skin and to give a good feel without causing a squeaking feeling when used in cosmetics. The average value of the major axis in the flat plate plane is about 1 to 1000 μm, the average value of the minor axis is ½ times or more of the mean value of the major axis, and the thickness is 1/1000 or more times of the mean value of the major axis. , Preferably less than 1/2 times.
In addition, it is preferable that the average value of a major axis is about 3-500 micrometers especially also in said range. Needless to say, the upper limit of the ratio of the minor axis is one time the major axis. Further, the thickness is preferably about 1/100 to 1/5 times the average value of the major axis, even in the above range. If the average value of the major axis in the flat plate plane is less than the above range, the overall size is too small, and even if the overall shape is maintained as a scale or plate, it was produced using such sericite particles. When amorphous calcium phosphate-coated sericite particles are used in cosmetics, the feeling of slipping on the skin may be insufficient. On the other hand, if this range is exceeded, excessively large sericite particles are cracked or broken, and the size tends to decrease. When the composite particles produced using such sericite particles are used in cosmetics because the ratio is out of the above range and it is no longer scaly or plate-like, There is a risk that the feeling of slipping will be insufficient.

In addition, when using sericite particles that are pearl pigments as sericite particles, various interference colors such as blue, yellow, green, red, and purple can be selected as the interference color. This makes it possible to achieve a natural and beautiful finish while correcting various shortcomings. For example, dull skin and dark circles around the eyes usually have melanin or congestion that absorbs and lacks yellow to red light as the skin color, so sericite that has a red to orange reflective interference color. By using particles (pearl pigments), the skin can be made healthy, bright and transparent. In addition, for sensitive skin, atopy, acne skin, etc., which are often seen in recent years, sericite particles having a green reflection interference color that is insufficiently absorbed by the hemoglobin pigment are used to soften the redness. A natural and beautiful finish is possible. In addition, skin with a lot of uneven color such as spots and freckles should be corrected with sericite particles that have a yellow interference color that is absorbed by the dark melanin pigment, and the skin is naturally made uniform. Can do.
In general, such sericite particles can be used as they are on the market, but classification may be performed if necessary. The amorphous calcium phosphate covering the surface of the sericite particles is tricalcium phosphate containing crystal water as represented by the general formula: Ca ₃ (PO ₄ ) ₂ .nH ₂ O, The crystal structure is amorphous. Note that the amorphous crystal structure means that amorphous calcium phosphate has a large amount of water of crystallization, so that the powder X-ray diffraction pattern is broader than crystalline calcium phosphate as illustrated in FIG. Can be confirmed.
As long as the effects of the present invention are not impaired, an element such as barium, strontium, zinc, magnesium, sodium, potassium, iron, aluminum, titanium, or the like is dissolved in a part of the calcium of the amorphous calcium phosphate. Alternatively, it may be ion-exchanged or substituted, and a part of PO ₄ may be substituted with one kind of atomic group such as VO ₄ , SiO ₄ , and CO ₄ .
Furthermore, calcium phosphate may be combined with one or more metal oxides. Although it does not specifically limit as a metal oxide, For example, a titanium oxide, a zinc oxide, a cerium oxide etc. are mention | raise | lifted.

In the washing step, the concentration of deposit ions removed from the surface of the sericite particles during the acid treatment described above is reduced, and in the subsequent calcium phosphate coating step, the deposit ions are amorphous on the surface of the sericite particles. Inhibiting the coating of calcium phosphate.
At this time, the washed sericite particles are washed so that the suspension in which water is dispersed in water at a solid concentration of 0.1 to 50% by mass, preferably 1 to 50% by mass, has a pH of 2.0 or more.
As a washing method in this washing step, washing may be performed by simply adding water to the above-described pickled sericite particles, and from the pickled sericite particles together with an acidic liquid by centrifugal dehydration as described above. A method of rinsing by adding water until the pH of the suspension in which the sericite particles are dispersed is discharged to a pH of 2.0 or more after dehydrating the extraneous matter ions out of the system and dehydrating can be used. A method of repeatedly performing dehydration / rinsing can also be employed.

In addition, when hydrochloric acid, nitric acid, sulfuric acid, or citric acid is used as the acid, it is possible to suppress consumption of calcium ions by anions other than phosphate ions such as chloride ions and sulfate ions. The washing step is preferably carried out until the suspension in which the sericite particles are dispersed in water at a solid content concentration of 0.1 to 50% by mass, preferably 1 to 50% by mass, has a pH of 6.0 or more. .
In the alkali step, an alkaline suspension is prepared by mixing the sericite particles washed in the aforementioned washing step and calcium hydroxide. Here, the sericite particles and calcium hydroxide are mixed to make the suspension alkaline. When the subsequent calcium phosphate coating step is performed in an acidic state, the added phosphoric acid is composed of calcium hydrogen phosphate. This is because it is consumed for formation and it becomes difficult to coat the surface of sericite particles with amorphous calcium phosphate.

  In the calcium phosphate coating step, the surface of sericite particles is coated with amorphous calcium phosphate by adding phosphoric acid to the alkaline suspension prepared in the alkaline step. At this time, as described above, if the suspension is in an acidic state, in particular, a pH of less than 5.0, there is a possibility that calcium hydrogen phosphate may be formed. The addition of the acid is preferably performed in a state where the pH is maintained at 5.0 or higher. In addition, if necessary, the pH may be maintained at 5.0 or higher and the formation of calcium hydrogen phosphate may be suppressed while alternately performing the alkali process and the calcium phosphate coating process. In the calcium phosphate coating step, the liquid temperature is preferably maintained at 50 ° C. or lower. At this time, if the liquid temperature exceeds 50 ° C., the crystallinity of calcium phosphate is increased and the water of crystallization is dropped. As a result, the activity of the obtained amorphous calcium phosphate-coated sericite particles such as the waste adsorbing performance may be reduced. Because.

  As described above, the produced amorphous calcium phosphate-coated particles can employ general drying means such as spray drying and cake drying, but do not require a step such as crushing, and are amorphous at the time of crushing. It is preferable to employ a drying means by spray drying from the viewpoint that the calcium phosphate-coated particles can be rubbed together and the amorphous calcium phosphate can be prevented from falling off from the surface of the amorphous calcium phosphate-coated sericite particles.

Next, a cosmetic containing the thus-produced amorphous calcium phosphate-coated sericite particles will be described.
As cosmetics of this embodiment, for example, emulsifying foundation, powder foundation, oily foundation, solid emulsifying foundation, lipstick, eye shadow, makeup cosmetics such as teak and nail color, shampoo, rinse, conditioner, hair treatment Hair cosmetics such as hair powder, body powder, perfume powder, baby powder, face powder, and other basic cosmetics such as emulsions, lotions, creams, cleansings, packs, sunscreens, and makeup bases.
Moreover, 0.1-50 mass% of said amorphous calcium phosphate coating | coated sericite particles are mix | blended with these cosmetics.

  The blending amount of the amorphous calcium phosphate-coated sericite particles is within such a range when the blending amount of the amorphous calcium phosphate-coated sericite particles is less than 0.1% by mass, sebum, bacteria, and virus. This is because the effect of adsorbing and removing so-called waste products such as the above cannot be obtained, and when the blending amount exceeds 50% by mass, a squeaky feeling is generated in the cosmetic.

  The amorphous calcium phosphate-coated sericite particles to be blended in the cosmetic may be surface-treated in advance. Examples of surface treatments include, for example, fluorine compound treatment, silicone treatment, metal soap treatment, acylated lysine treatment, oil agent treatment, silane treatment, amino acid treatment, wax treatment, and metal oxide treatment. Any processing that is used can be adopted. Of course, the amorphous calcium phosphate-coated sericite particles may be used in cosmetics without surface treatment.

  In addition to amorphous calcium phosphate-coated sericite particles, the cosmetics include oils, powders (pigments, pigments), resins, surfactants, stickers, preservatives, fragrances, ultraviolet rays that are commonly used in cosmetics. Various components such as an absorbent (including organic and inorganic), a humectant, a physiologically active ingredient, salts, a solvent, an antioxidant, a chelating agent, a neutralizing agent, and a pH adjusting agent can be blended. Examples of oils include higher alcohols such as cetyl alcohol, isostearyl alcohol, lauryl alcohol, hexadecyl alcohol, octyldodecanol, fatty acids such as isostearic acid, undecylenic acid, oleic acid, glycerin, sorbitol, ethylene glycol, Polyhydric alcohols such as propylene glycol and polyethylene glycol, myristyl myristate, hexyl laurate, decyl oleate, isopropyl myristate, hexyl decyl dimethyloctanoate, glyceryl monostearate, diethyl phthalate, ethylene glycol monostearate, oxy Esters such as octyl stearate, hydrocarbons such as liquid paraffin, isoparaffin, petrolatum, squalane, lanolin, reduced Phosphorus, waxes such as carnauba wax, mink oil, cacao butter, coconut oil, palm kernel oil, camellia oil, sesame oil, castor oil, oils and fats such as olive oil and the like.

  Examples of other forms of oil include dimethylpolysiloxane, methylhydrogenpolysiloxane, methylphenylpolysiloxane, polyether-modified organopolysiloxane, alkyl-modified organopolysiloxane, sugar-modified silicone, glyceryl-modified silicone, and amodimethicone. And silicone compounds such as amino-modified organopolysiloxane, silicone gel, acrylic silicone, trimethylsiloxysilicic acid, and silicone RTV rubber.

  Furthermore, examples of fluorine-based oils include, for example, fluorocarbons such as perfluorodecalin, alcohols such as perfluoropolyether, fluorinated pitch and fluoroalcohol having a perfluoroalkyl chain, and perfluoroalkyl phosphate triethanolamine salts. And phosphoric acid esters such as carboxylic acids having a fluoroalkyl chain, fluoroalkyl-modified silicones, fluorine / polyether co-modified silicones, and fluorinated silicone resins.

  Examples of powders include sericite (unprocessed), mica (muscovite, phlogopite, saucite, biotite, lithia mica, synthetic mica), talc, kaolin, vermiculite, smectite, titanium oxide-coated mica. (Titanium mica), pearl pigments such as titanium oxide-coated sericite, titanium oxide-coated talc, fish scale foil, boron nitride, and other resin powders such as nylon beads, silicone beads, PTFE powder, silicone elastomer, and yellow Iron oxide, red iron oxide, black iron oxide, chromium oxide, cobalt oxide, carbon black, ultramarine, bitumen, zinc oxide, titanium oxide, zirconium oxide, silicon oxide, aluminum oxide, cerium oxide, barium sulfate, calcium carbonate, magnesium carbonate , Aluminum silicate, magnesium silicate, silicon carbide, organic dye, Yellow, particulate titanium oxide, particulate zinc oxide, particulate iron oxide, etc. plate-like barium sulfate.

  These powders are fluorine compound treatment, silicone treatment, metal soap treatment, acylated lysine treatment, oil agent treatment, silane treatment, amino acid treatment, wax treatment, metal oxide treatment, silane coupling agent treatment, organic titanate treatment, You may use it in the state which gave surface treatments, such as a fatty-acid treatment. As the surfactant, any of an anionic surfactant, a cationic surfactant, a nonionic surfactant, and a betaine surfactant can be used.

  Examples of the physiologically active component include anti-inflammatory agents, blood circulation promoters, vitamins, tyrosinase activity inhibitors, urea and the like. Examples of the solvent include purified water, methanol, ethanol, isopropyl alcohol, ether, LPG, volatile silicone, light liquid isoparaffin, and alternative chlorofluorocarbon. Mineral water can also be used instead of purified water.

  As such cosmetics, in powder white powder, solid white powder, foundation, the average particle diameter of the amorphous calcium phosphate-coated sericite particles to be blended is preferably 1 to 50 μm in terms of touch, In the eye shadow, teak, lipstick, and nail color, the average particle size of the amorphous calcium phosphate-coated sericite particles to be blended is 50 in that they can give a sparkle to the site where makeup is applied and improve the aesthetic appearance. It is preferable that it is -100micrometer.

  EXAMPLES Next, although an Example is given and this invention is demonstrated in more detail, this invention is not limited to these.

(Production of amorphous calcium phosphate-coated sericite particles)
(Production Example 1)
To 1 liter of ion-exchanged water, sericite manufactured by Sanshin Mining Co., Ltd. (trade name “FSE”: average particle diameter of about 8.17 μm, flat plate major axis average value of about 8 μm, minor axis average value of about 5 μm, thickness average value) 450 g of about 0.1 μm) was added, 1500 g of a 7.5% by mass phosphoric acid aqueous solution was added with stirring, and the mixture was stirred for 10 minutes to form a suspension. Carried out. The pH of the suspension at this time was measured with a pH meter and found to be pH 2.68.
Further, the sericite was separated by suction filtration, and the washing step was carried out by adding ion-exchanged water to prepare a resuspension until the pH became 2.0 or more at a solid content concentration of 20%.
Next, using a homomixer, a calcium hydroxide suspension in which 37.3 g of calcium hydroxide is dispersed in 1 liter of ion-exchanged water is prepared, and the pH of the resuspension is compared to the resuspension. This calcium hydroxide suspension was added until 12.5 to carry out an alkaline step to prepare an alkaline suspension.
Furthermore, while maintaining the liquid temperature of this alkaline suspension at 50 ° C. or lower, a 7.5% by mass aqueous phosphoric acid solution was added until the final pH was 6.5 and stirred for 30 minutes, followed by a calcium phosphate coating step. Carried out.
Further, spray drying (Okawara Kako Machinery Co., Ltd. “L-8”) was used for spray drying to perform the above-mentioned alkali process and this calcium phosphate coating process alternately twice (total 3 times each). Granules were produced to produce amorphous calcium phosphate coated sericite particles.

(Production Example 2)
Amorphous calcium phosphate-coated sericite particles were produced in the same manner as in Production Example 1 except that the calcium phosphate coating step was carried out until the final pH was 8.5.

(Production Example 3)
Amorphous calcium phosphate-coated sericite particles were produced in the same manner as in Production Example 1 except that the calcium phosphate coating step was performed until the final pH reached 10.5.

(Production Example 4)
Except that the acid treatment step was not carried out, and in the calcium phosphate coating step, an 8.5% by mass phosphoric acid aqueous solution was used until the final pH was 9.0 to 10.0, and Production Example 1 Similarly, amorphous calcium phosphate-coated sericite particles were produced.

(Production Example 5)
Without carrying out the acid treatment step, sericite particles were dispersed in 3 liters of ion-exchanged water at 90 ° C., that an alkaline suspension was prepared using an alkaline aqueous solution of 25 g / liter of calcium acetate in the alkaline step, calcium phosphate In the coating step, the same procedure as in Production Example 1 was conducted, except that the alkaline suspension was added to a final pH of 7.0 using an aqueous sodium hydrogen phosphate solution while maintaining the liquid temperature at 90 ° C. Amorphous calcium phosphate coated particles were produced. In this production example, amorphous calcium phosphate-coated sericite particles were produced according to the production method described in Patent Document 2.

(Oleic acid adsorption amount)
First, a blank sample prepared by drying amorphous calcium phosphate-coated particles under conditions of 350 ° C. × 1 h was prepared. Next, 4.5 g of oleic acid was added to 0.5 g of this blank sample and allowed to stand at 37 ° C. for 24 hours to adsorb oleic acid. Further, the sample was washed three times with 15 ml of diethyl ether and air-dried to obtain an adsorption sample.
About 14 to 17 mg each of the blank sample and the adsorbed sample were collected, and the oil absorption amount was obtained by performing TG-DTA measurement at a heating rate of 20 ° C./min from 30 ° C. to 600 ° C. in a nitrogen gas stream. .
More specifically, the difference between the residual heating rate (%) at 30 to 600 ° C. and the residual heating rate (%) at 30 to 150 ° C. is obtained as a weight loss rate (%), and each of the blank sample and the adsorption sample is obtained. The difference in weight loss rate (%) was taken as the adsorption rate (%), and this adsorption rate (%) was multiplied by 10 to obtain the oil adsorption amount (mg / g). The results are shown in Table 1.

(Kishimi test)
Table 2 shows the results of having the subjects evaluated the feel when the amorphous calcium phosphate-coated sericite particles prepared in Production Examples 1 to 5 were spread on the face in 10 stages. .
Good: There is no tingling feeling and the touch is good.
Poor: There is a feeling of squeaking and the touch is bad.
Normal: Neither good nor bad, in between.

(Microscopic observation)
Scanning electron micrographs of Production Examples 3 and 5 are shown in FIGS.
From this figure, in Production Example 3, the amorphous calcium phosphate-coated sericite particles A have fine spherical amorphous calcium phosphate B uniformly attached to the entire surface of the sericite particles, but in Production Example 5, A large particle E having a diameter of about 100 μm, in which many sericite particles are aggregated, has been formed. Further, the surface of the giant particle E is roughly covered with a large rod-like amorphous calcium phosphate C, and a substrate exposed portion D in which the sericite particles are exposed is seen partially.
As described above, the amorphous calcium phosphate-coated sericite particles obtained in Production Examples 1 to 3 are more amorphous than the amorphous calcium phosphate-coated sericite particles obtained in Production Examples 4 and 5. It can be seen that calcium phosphate is uniform, adsorbing performance (function of adsorbing and removing waste products) is high, and the feeling of squeaking is also reduced. That is, by mixing sericite particles and an acid having a pH of 1.5 or less, an acid treatment step of treating the surface of the sericite particles with an acid having a pH of 1.5 or less, A washing step for washing the sericite particles treated in the acid treatment step so that the pH of the suspension dispersed in water at 50% by mass is 2.0 or more, and the sericite washed in the washing step An alkaline process for preparing an alkaline suspension in which site particles and calcium hydroxide are mixed, and phosphoric acid is added to the alkaline suspension prepared in the alkaline process so that the surface of the sericite particles is made of amorphous calcium phosphate. By using the amorphous calcium phosphate-coated sericite particles produced by the production method in which the calcium phosphate coating step is performed, Bacteria adsorbing a so-called waste, such as virus, the ability to remove can be assumed with suppressed creaking feeling while suppressing a decrease.

Example 1
Using the amorphous calcium phosphate-coated sericite particles of Production Example 1, a foundation was produced by the following formulation 1.
(Formulation 1)
Ingredient Mass%
Amorphous calcium phosphate coated sericite particles 18
Iron oxide 4.5
Sericite (unprocessed product) 15
Plate-like barium sulfate 34
Titanium oxide 8
Talc 10
Perfluoropolyether 7
Fluorine-modified silicone 3
Preservatives and fragrances 0.5
The foundation was excellent in touch and did not cause a squeaky feeling when applied to the skin.

(Example 2)
Using the amorphous calcium phosphate-coated sericite particles of Production Example 1, a foundation was produced by the following formulation 2. All inorganic powders including amorphous calcium phosphate-coated sericite particles were treated with 3 parts by weight of perfluoroalkyl phosphate ester salt with respect to 100 parts by weight of the inorganic powder.
(Formulation 2)
Ingredient Mass%
Amorphous calcium phosphate coated sericite particles 20
Iron oxide 4.5
Sericite (untreated product) 12
Plate-like barium sulfate 32
Titanium oxide 8
Fine particle titanium oxide 2
Talc 10
Silicone elastomer 3
Organic UV absorber 3
Perfluoropolyether 5.5
Glycerin 0.5
White petrolatum 1
Preservatives and fragrances 0.5
The above foundation was excellent in the effect of preventing ultraviolet rays and excellent in touch, and did not cause a squeaky feeling when applied to the skin.

(Example 3)
Using the amorphous calcium phosphate-coated sericite particles of Production Example 2, a foundation was produced by the following formulation 3. First, component A and component B were mixed, then component C was added and further mixed, the mixture was pulverized and cast into a metal dish using a mold to obtain a product.
In addition, Component A is processed using 3 parts by weight of a perfluoroalkyl phosphate ester salt with respect to 100 parts by weight of each.
(Formulation 3)
Component A mass%
Amorphous calcium phosphate coated sericite particles 10
Iron oxide 4.5
Sericite (untreated product) 20
Plate-like barium sulfate 34
Titanium oxide 8
Talc 10

Component B Mass%
Silicone elastomer 3

Ingredient C
Perfluoropolyether 7
Fluorine-modified silicone 3
Preservatives and fragrances 0.5
The above foundation was excellent in UV prevention effect, sebum resistance (makeup persistence), and also in touch, and did not cause a squeaky feeling when applied to the skin.

Example 4
Using the amorphous calcium phosphate-coated sericite particles of Production Example 3, a body powder foam was produced according to the following formulation 4. First, component A was mixed, then component B was added and further mixed, and a mixed gas of component C was added and filled into a container to obtain a product.
(Formulation 4)
Component A mass%
Squalane 1
Polyoxyethylene cetyl ether 3
1,3-butylene glycol 1
Ethyl alcohol 12
Polymethylsilsesquioxane powder 5

Component B Mass%
Water 33
Amorphous calcium phosphate coated sericite particles 15

Ingredient C
Alternative Freon 22
LPG 8

The body powder foam was particularly refreshing and excellent in sebum adsorption effect.
As described above, the amorphous calcium phosphate-coated sericite particles are mixed with sericite particles and an acid having a pH of 1.5 or less, whereby the surface of the sericite particles is washed with an acid having a pH of 1.5 or less. The sericite particles treated in the acid treatment step so that the pH of the suspension obtained by dispersing the sericite particles in water at a solid concentration of 0.1 to 50% by mass is 2.0 or more. Washing step for washing, alkaline step for preparing an alkaline suspension in which calcium hydroxide is mixed with sericite particles washed by the washing step, and phosphoric acid is added to the alkaline suspension created in the alkaline step. Amorphous calcium phosphate because a calcium phosphate coating process is carried out, in which the surface of sericite particles is coated with amorphous calcium phosphate. The surface of the coated sericite particles can be prevented from generating a portion that is not coated with amorphous calcium phosphate, and cosmetics containing this amorphous calcium phosphate-coated sericite particles can be used for sebum, bacteria, viruses, etc. It can be seen that it is possible to suppress the feeling of squeaking while maintaining the function of adsorbing and removing so-called waste products.

A scanning electron micrograph of amorphous calcium phosphate-coated sericite particles of Production Example 3. An enlarged photograph of FIG. A scanning electron micrograph of amorphous calcium phosphate-coated sericite particles of Production Example 5. The enlarged photograph of FIG. The powder X-ray-diffraction chart of an amorphous calcium phosphate and crystalline calcium phosphate.

Explanation of symbols

A Amorphous calcium phosphate-coated sericite particles B Spherical amorphous calcium phosphate C Rod-shaped amorphous calcium phosphate D Substrate exposed portion E Large particles

Claims (3)

Amorphous calcium phosphate-coated sericite particles obtained by coating sericite particles with amorphous calcium phosphate are blended in an amount of 0.1 to 50% by mass, and the amorphous calcium phosphate-coated sericite particles are (1) sericite particles and pH1. An acid treatment step of washing the surface of the sericite particles with an acid having a pH of 1.5 or less by mixing with an acid of .5 or less;
(2) Sericite particles treated in the acid treatment step so that the pH of a suspension in which sericite particles are dispersed in water at a solid content concentration of 0.1 to 50% by mass is 2.0 or more. Cleaning process to wash,
(3) An alkaline process for preparing an alkaline suspension in which the sericite particles washed by the washing process and calcium hydroxide are mixed;
(4) A calcium phosphate coating step of coating the surface of sericite particles with amorphous calcium phosphate by adding phosphoric acid to the alkaline suspension prepared in the alkaline step,
Cosmetics produced by carrying out the above.   The cosmetic according to claim 1, wherein phosphoric acid is used as an acid in the acid treatment step.   Either hydrochloric acid, nitric acid, sulfuric acid or citric acid is used as the acid in the acid treatment step, and sericite particles are dispersed in water at a solid content concentration of 0.1 to 50% by weight as the washing in the washing step. The cosmetic according to claim 1, wherein the suspension is washed so that the pH of the suspension becomes 6.0 or more.