JPH07100644B2 - Method for producing powder for cosmetics - Google Patents

Method for producing powder for cosmetics

Info

Publication number
JPH07100644B2
JPH07100644B2 JP62057602A JP5760287A JPH07100644B2 JP H07100644 B2 JPH07100644 B2 JP H07100644B2 JP 62057602 A JP62057602 A JP 62057602A JP 5760287 A JP5760287 A JP 5760287A JP H07100644 B2 JPH07100644 B2 JP H07100644B2
Authority
JP
Japan
Prior art keywords
gel
powder
cosmetic
cosmetics
present
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
JP62057602A
Other languages
Japanese (ja)
Other versions
JPS63225310A (en
Inventor
信之 山本
正典 小松
由加利 伊理
敏弘 陳野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lion Corp
Original Assignee
Lion Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lion Corp filed Critical Lion Corp
Priority to JP62057602A priority Critical patent/JPH07100644B2/en
Publication of JPS63225310A publication Critical patent/JPS63225310A/en
Publication of JPH07100644B2 publication Critical patent/JPH07100644B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、クリーム、ボディーパウダー、ローション、
ファウンデーション等の皮膚化粧料に配合できる化粧料
用粉体の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention relates to creams, body powders, lotions,
The present invention relates to a method for producing powder for cosmetics that can be incorporated into skin cosmetics such as foundations.

〔従来の技術〕[Conventional technology]

各種化粧料には、保湿剤、油分、殺菌剤等の薬用成分や
紫外線吸収剤などが配合されているが、これらの化粧料
を人体に施した場合、配合成分の効果の持続性が十分で
ないという問題がある。そこで、特定の成分の配合量を
多くして効果の持続性をもたせることが考えられるが、
配合量を多くするとべたついたり（保湿剤、油分）、皮
膚刺激性（殺菌剤、紫外線吸収剤）が顕著になるという
問題点が生じてしまう。Various cosmetics contain medicinal components such as moisturizers, oils, bactericides, and ultraviolet absorbers, but when these cosmetics are applied to the human body, the effects of the components are not long-lasting. There is a problem. Therefore, it is possible to increase the blending amount of specific ingredients to provide long-lasting effect.
If the blending amount is increased, problems such as stickiness (humectant, oil content) and skin irritation (bactericide, ultraviolet absorber) become remarkable occur.

そこで、配合量を多くする代わりにシリカ、タルク、酸
化チタン、炭酸カルシウム等無機粉体に配合成分を吸着
させて、効果の持続性を高める方法が種々提案されてい
る。例えば、スクアレン等の油状液を超微粉シリカ系粉
体に添加混合して該粉体に吸着させる方法（特開昭53−
38635号）、無水ケイ酸化合物などからつくられた中空
の多孔性粉体を配合する方法（特開昭60−100509号）及
び酸化アルミニウムの含量が0.35％である微粉状水和ケ
イ酸よりなるシリカ系担体を化粧料の担体として用いる
方法（特開昭60−226826号）などがあげられる。しかし
ながら、これらの方法は、いずれも化粧料成分を吸着す
る力が弱く、また担体として用いる無機粉体に化粧料成
分を吸着させているために粉体表面の化粧料成分濃度が
高く、十分な持続性が発揮されていない。Therefore, various methods have been proposed in which, instead of increasing the blending amount, the blending component is adsorbed to an inorganic powder such as silica, talc, titanium oxide, calcium carbonate, etc. to enhance the sustainability of the effect. For example, a method in which an oily liquid such as squalene is added to and mixed with ultrafine silica-based powder and adsorbed on the powder (Japanese Patent Laid-Open No. 53-
No. 38635), a method of blending a hollow porous powder made of silicic acid anhydride compound (JP-A-60-100509) and finely powdered hydrated silicic acid having an aluminum oxide content of 0.35%. Examples thereof include a method of using a silica-based carrier as a carrier for cosmetics (JP-A-60-226826). However, all of these methods have a weak ability to adsorb cosmetic ingredients, and since the cosmetic ingredients are adsorbed to the inorganic powder used as a carrier, the cosmetic ingredient concentration on the powder surface is high and sufficient. Sustainability is not demonstrated.

〔発明が解決しようとする問題点〕[Problems to be solved by the invention]

従って、本発明は、人体に施したときにべとつきや刺激
がなく、かつ化粧料成分を長期間継続して放出すること
ができる化粧料粉体の製造方法を提供することを目的と
する。Therefore, it is an object of the present invention to provide a method for producing a cosmetic powder which is free from stickiness and irritation when applied to a human body and which can continuously release a cosmetic component for a long period of time.

〔問題点を解決するための手段〕[Means for solving problems]

本発明は、特定のアルキルシリケートを加水分解、重縮
合反応させてゲルを形成させる際に少なくとも１種の化
粧料成分を存在させるか又はゲル形成後に化粧料成分を
添加してゲルに含浸させた後に、ゲルを乾燥すると、化
粧料成分が粉体の内部にまで十分含まれる形態のものが
得られ、これによれば化粧料成分を粉体内部から徐放す
るので上記問題点が極めて有効に解決できるとの知見に
基づいてなされたのである。According to the present invention, at least one cosmetic ingredient is present when a specific alkyl silicate is hydrolyzed and polycondensed to form a gel, or after the gel is formed, the cosmetic ingredient is added to impregnate the gel. After that, when the gel is dried, a form in which the cosmetic ingredient is sufficiently contained even inside the powder is obtained, and since the cosmetic ingredient is gradually released from the inside of the powder, the above problems are extremely effective. It was made based on the finding that it could be resolved.

すなわち、本発明は、 一般式〔Ｉ〕： （式中、R1〜R4は、水素又はCxH2x＋１（OC2H4）ｙ−
（但し、ｘは１〜５、ｙは０〜10の整数を示す。）で示
される基であるが、R1〜R4のすべてが水素であることは
ない。ｎは０〜20の整数である。） で表わされる少なくとも１種のアルキルシリケートの加
水分解、重縮合反応を化粧料成分の存在で行ってゲルを
形成させた後、又は該反応によりゲルを形成した後に化
粧料成分を該ゲルに含浸させた後、乾燥することを特徴
とする化粧料用粉体の製造方法を提供する。That is, the present invention provides a compound represented by the general formula [I]: (In the formula, R 1 to R 4 are hydrogen or CxH 2 x + 1 (OC 2 H 4 ) y−
(However, x is an integer of 1 to 5 and y is an integer of 0 to 10.) However, not all of R 1 to R 4 are hydrogen. n is an integer of 0-20. ) After the hydrolysis and polycondensation reaction of at least one alkyl silicate represented by the formula (1) is performed in the presence of the cosmetic ingredient to form a gel, or after the gel is formed by the reaction, the gel is impregnated with the cosmetic ingredient. A method for producing a powder for cosmetics is provided, which comprises drying after the treatment.

本発明では、上記一般式〔Ｉ〕で表わされるアルキルシ
リケートを原料として用いる。このうち、式中、R1〜R4
としてはCH3、C2H5、ｎ−C3H7、iso−C3H7、ｎ−C4H9、
−C2H4OCH3が好ましく、特に好ましくはR1〜R4が同一の
基である。又、ｘとしては１〜３が、ｙとしては０〜２
が好ましく、ｎは０〜10が好ましい。このうち、本発明
ではｎ＝０のものが特に好ましいが、ｎが１〜10の縮合
体も好ましい。一般式〔Ｉ〕で表わされるケイ酸エステ
ルを具体的に示すと、ケイ酸メチル、ケイ酸エチル、ケ
イ酸−プロピル、ケイ酸イソプロピル、ケイ酸ｎ−ブチ
ル、ケイ酸２−メトキシエチル、これらの２〜10量体等
があげられる。これらのうち、ケイ酸エチルSi（OC
2H5）４はエチルシリケート28、ケイ酸エチル平均５モ
ル縮合物： は、エチルシリケート40としてコルコート社より容易に
入手し得る。In the present invention, the alkyl silicate represented by the above general formula [I] is used as a raw material. Of these, in the formula, R 1 to R 4
The CH 3, C 2 H 5, n-C 3 H 7, iso-C 3 H 7, n-C 4 H 9,
—C 2 H 4 OCH 3 is preferable, and R 1 to R 4 are particularly preferably the same group. Further, x is 1 to 3 and y is 0 to 2
Is preferred, and n is preferably 0-10. Of these, in the present invention, n = 0 is particularly preferable, but a condensate in which n is 1 to 10 is also preferable. Specific examples of the silicate ester represented by the general formula [I] include methyl silicate, ethyl silicate, propyl silicate, isopropyl silicate, n-butyl silicate, 2-methoxyethyl silicate, and the like. 2-10 mer etc. are mentioned. Of these, ethyl silicate Si (OC
2 H 5 ) 4 is ethyl silicate 28, ethyl silicate average 5 mol condensate: Is readily available from Colcote as ethyl silicate 40.

上記ケイ酸エステル又はその縮合物は、水又は水／アル
コール溶媒、酸又はアルカリ触媒下で加水分解し、この
均一溶液を放置、又はpH調製後に放置してゲル化させ
る。この際強いゲルを得るには酸触媒下で加水分解する
のがよい。尚、上記反応において、加水分解と同時にケ
イ酸エステル間に重縮合反応が生じ、Si−Ｏ−Si結合が
３次元で生じ安定なゲルが生成する。The silicic acid ester or its condensate is hydrolyzed under water or a water / alcohol solvent, an acid or an alkali catalyst, and this homogeneous solution is left to stand or gelled after standing after pH adjustment. At this time, in order to obtain a strong gel, it is preferable to hydrolyze under an acid catalyst. In addition, in the above reaction, a polycondensation reaction occurs between the silicic acid esters simultaneously with the hydrolysis, and Si—O—Si bonds are three-dimensionally formed to form a stable gel.

本発明では上記ゲルを形成させるための加水分解、重縮
合反応を化粧料成分の存在下に行わせるか、又はゲル形
成後に化粧料成分をゲルに含浸させることを特徴とす
る。ここで使用できる化粧料成分としては、化粧料に配
合される成分であって、水又はアルコールに可溶若しく
は、界面活性剤により水中に乳化又は分散可能なもので
あればいかなる成分であってもよい。具体的には、グリ
セリン、ソルビトール、ピロリドンカルボン酸ソーダ、
グルコサミン、ペプタイドなどの保湿剤、スクアラン、
スワアレン、流動パラフィン、脂肪酸、高級アルコール
などの油分、塩化ベンザルコニウム、クロルヘキシジ
ン、トリクロサンなどの殺菌剤、Ｐ−アミノ安息香酸、
サリチル酸フェニル、２−ヒドロキシ−４−メトキシベ
ンゾフェノン、サリチル酸ホモメンチルなどの紫外線吸
収剤などの１種又は２種以上の混合物が例示される。The present invention is characterized in that the hydrolysis or polycondensation reaction for forming the gel is carried out in the presence of the cosmetic ingredient, or that the gel is impregnated with the cosmetic ingredient after the gel is formed. The cosmetic ingredient that can be used here is any ingredient that is blended into a cosmetic and that is soluble in water or alcohol or that can be emulsified or dispersed in water by a surfactant. Good. Specifically, glycerin, sorbitol, sodium pyrrolidone carboxylic acid,
Glucosamine, moisturizer such as peptide, squalane,
Oils such as swarene, liquid paraffin, fatty acids and higher alcohols, bactericides such as benzalkonium chloride, chlorhexidine and triclosan, P-aminobenzoic acid,
Examples include one or a mixture of two or more UV absorbers such as phenyl salicylate, 2-hydroxy-4-methoxybenzophenone, and homomenthyl salicylate.

これらの化粧料成分は任意の量で用いることができる
が、通常ケイ酸エステルに対して0.1〜30重量％（以
下、％と略称する）、好ましくは0.2〜20％添加するの
がよく、化粧料成分が水又はアルコール可溶の場合には
そのまま又は１〜50％濃度となるように水やアルコール
に溶解して加えるのがよく、溶解しない場合には、界面
活性剤等で水に乳化又は分散して添加するのがよい。
尚、化粧料成分は酸性下で変質するものが多いので中性
付近にpH調整後添加するのが好ましい。Although these cosmetic ingredients can be used in any amount, they are usually added in an amount of 0.1 to 30% by weight (hereinafter abbreviated as%), preferably 0.2 to 20%, based on silicic acid ester. When the ingredient is soluble in water or alcohol, it is preferable to add it as it is or to dissolve it in water or alcohol so as to have a concentration of 1 to 50%, and if it does not dissolve, emulsify it in water with a surfactant or the like. It is better to add it dispersedly.
Since many cosmetic ingredients change in quality under acidic conditions, it is preferable to add them after adjusting the pH to around neutral.

本発明においてアルキルシリケートの重縮合時に化粧料
成分を存在させると、３次元化したSi−Ｏ−Si結合に化
粧料成分がからみあった状態でゲル化する。また、ゲル
化直はSi−Ｏ−Si結合がゆるく、この状態のゲルに化粧
料成分を含浸させても、ゲル奥深くため化粧料成分が浸
透し、反応中に化粧料成分を添加した場合と同様の状態
となるのである。In the present invention, when the cosmetic ingredient is present during the polycondensation of the alkyl silicate, the three-dimensional Si—O—Si bond is gelled with the cosmetic ingredient entangled. In addition, since the Si-O-Si bond is loose immediately after gelation, even if the gel in this state is impregnated with the cosmetic ingredient, the deeper gel penetrates the cosmetic ingredient, and the cosmetic ingredient is added during the reaction. It will be in the same state.

上記ゲルの調整において、加水分解は低pHの方がはや
く、加水分解した液をゲル化させるのには、pHが高い方
がはやい。従って、効率的なゲル化は、低pH、例えばpH
0.5〜3.0で加水分解後、中性付近、つまりpH4.0〜8.0に
pH調整するのがよい。この際、液のpHを酸性にするに
は、塩酸、硝酸、硫酸等の鉱酸及び酢酸、クエン酸、乳
酸等の有機酸を用いるがよく、その後pHを中性付近に上
昇させるには、アンミニア水、水酸化ナトリウム、水酸
化カリウム、モノエタノールアミン、ジエタノールアミ
ン、トリエタノールアミン、などを用いるのがよい。In the preparation of the above gel, hydrolysis is faster at a low pH and gelation of the hydrolyzed liquid is faster at a higher pH. Thus, efficient gelation requires low pH, such as pH.
After being hydrolyzed at 0.5 to 3.0, the pH is adjusted to near neutral, that is, pH 4.0 to 8.0.
It is better to adjust the pH. At this time, in order to make the pH of the liquid acidic, it is preferable to use mineral acids such as hydrochloric acid, nitric acid, sulfuric acid and organic acids such as acetic acid, citric acid and lactic acid, and thereafter to raise the pH to around neutral, Ammonia water, sodium hydroxide, potassium hydroxide, monoethanolamine, diethanolamine, triethanolamine, etc. are preferably used.

又、反応系の水の量は、加水分解に必要な最低量あれば
よく、希釈されてゲル化しなくなるまで添加可能である
が、通常反応溶液中に0.5〜95％、好ましくは１〜70％
含有されるように用いるのがよい。尚、化粧料成分が親
水性ならば水の量を多くするのが好ましい。Further, the amount of water in the reaction system may be the minimum amount necessary for hydrolysis and can be added until it is diluted and does not gel, but it is usually 0.5 to 95% in the reaction solution, preferably 1 to 70%.
It is good to use so that it may be contained. If the cosmetic ingredient is hydrophilic, it is preferable to increase the amount of water.

本発明では、上記ケイ酸エステルの加水分解によりアル
コールが生成するので、別にアルコールを添加する必要
はないが、アルコールはゲル中の化粧料成分の分布を均
一にし、かつ化粧料成分を可溶化するので、反応溶液中
に0.1〜95％含まれるようにするのがよい。尚、化粧料
成分がアルコール可溶の場合は、アルコール量が多い方
が好ましい。この際、別に添加するアルコールとして
は、ケイ酸エステルの加水分解により生じるアルコール
と同種のものが好ましいが、別の種類のものでもよい。In the present invention, since alcohol is produced by the hydrolysis of the silicate ester, it is not necessary to add alcohol separately, but alcohol makes the distribution of the cosmetic ingredients in the gel uniform and solubilizes the cosmetic ingredients. Therefore, it is preferable that 0.1 to 95% is contained in the reaction solution. When the cosmetic ingredient is soluble in alcohol, it is preferable that the amount of alcohol is large. At this time, the alcohol added separately is preferably the same as the alcohol produced by the hydrolysis of the silicate ester, but may be another type.

本発明では上記ゲル化反応を０〜80℃で行った後、化粧
料成分を含有したゲルを常法により乾燥して乾燥ゲルを
製造し、これを粉砕して化粧料を含有する粉体を得る
が、乾燥前にゲルを球状に成形し、これを乾燥して球状
物を得るのが好ましい。In the present invention, after the gelation reaction is performed at 0 to 80 ° C., the gel containing the cosmetic ingredients is dried by a conventional method to produce a dry gel, which is crushed to obtain a powder containing the cosmetic. It is preferable that the gel is formed into a spherical shape before drying, and the spherical shape is obtained by drying the gel.

この際ゲルの乾燥方法としては、ゲルを常圧又は減圧
下、０〜100℃、好ましくは15〜60℃でゲル重量が変化
しなくなるまで乾燥する。この乾燥工程で重縮合反応は
さらにすすみ、化粧料成分をとじこめたままゲルはしだ
いに堅くなる。次に、乾燥ゲルを粉砕するが、ゲルを粉
砕したのち乾燥してもよい。At this time, as a method for drying the gel, the gel is dried under normal pressure or reduced pressure at 0 to 100 ° C, preferably 15 to 60 ° C until the weight of the gel does not change. In this drying step, the polycondensation reaction proceeds further, and the gel gradually hardens while the cosmetic ingredients are confined. Next, the dried gel is ground, but the gel may be ground and then dried.

尚、一般に化粧料用粉体は、肌ざわりの良さから滑りの
よい球状（0.01〜50μ）であることが好ましい。そこ
で、特開昭60−180923号などの方法により球状のゲルを
形成し、これを乾燥して球状粉体とするのがよい。In general, the powder for cosmetics is preferably spherical (0.01 to 50 μm) with good slipperiness because of its good texture. Therefore, it is preferable to form a spherical gel by a method such as that disclosed in JP-A-60-180923 and dry it to obtain spherical powder.

本発明においては、上記製造工程において、所望により
種々の成分を添加することができる。例えば得られる化
粧料粉体の表面特性を変えるためにアルキルシリケート
溶液にAl、Ti、Zr等の金属アルコキシド、ポリビニルア
ルコール、ポリビニルピロリドン、ポリエチレングリコ
ール、ポリアクリルアミド、ポリアクリル酸、ポリアク
リル酸エステル、ポリ酢酸ビニル、グァーガム、カラギ
ーナン、ヒドロキシエチルセルロース、ヒドロキシプロ
ピルセルロースなどの高分子や化粧料用無機粉体を添加
することができる。In the present invention, various components can be added, if desired, in the above manufacturing process. For example, in order to change the surface characteristics of the obtained cosmetic powder, Al, Ti, metal alkoxides such as Zr, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, polyacrylamide, polyacrylic acid, polyacrylic acid ester, polyalkyl silicate solution, etc. Polymers such as vinyl acetate, guar gum, carrageenan, hydroxyethyl cellulose, hydroxypropyl cellulose and inorganic powders for cosmetics can be added.

〔発明の効果〕〔The invention's effect〕

本発明によれば人体に施したときにべとつきや刺激性が
なく、かつ化粧料成分を長期間継続して放出できる化粧
料粉体が提供される。According to the present invention, there is provided a cosmetic powder having no stickiness or irritation when applied to a human body and capable of continuously releasing a cosmetic component for a long period of time.

従って本発明により製造した化粧料用粉体は、スキンク
リーム、粉白粉、パウダーファンデーション、ボディパ
ウダー、乳化ファンデーション（クレジングクリーム、
バニシングクリーム）、制汗剤、日やけ止め、日やけ用
化粧品等に広く配合できる。Therefore, the cosmetic powder produced by the present invention is a skin cream, a white powder, a powder foundation, a body powder, an emulsification foundation (creasing cream,
Vanishing cream), antiperspirant, sunscreen, sunscreen cosmetics, etc.

次に実施例により本発明を説明するが本発明はこれらに
限定されるものではない。Next, the present invention will be described with reference to examples, but the present invention is not limited thereto.

〔実施例〕〔Example〕

実施例１ Si（OC2H5）452.1g（0.25モル）に28mmol/の塩酸水54
gを加え、室温で攪拌して１時間後に均一溶液を得た。
この溶液を1/2規定のアンモニア水でpH5.0に調整した
後、これにトリクロサン（殺菌剤）の20％エタノール溶
液27gを添加した。攪拌して均一溶液としたのち45℃で
１夜静置したところゲル化した。このゲルを45℃で１週
間乾燥させたところ、乾燥重量24.8gの乾燥ゲルを得
た。この乾燥ゲルを粉砕してトリクロサンを21.8％含む
化粧料用粉体Ａを得た。Example 1 52.1 g (0.25 mol) of Si (OC 2 H 5 ) 4 28 mmol / hydrochloric acid water 54
g was added and the mixture was stirred at room temperature for 1 hour to obtain a uniform solution.
After adjusting the pH of this solution to 5.0 with 1/2 normal ammonia water, 27 g of 20% ethanol solution of triclosan (bactericide) was added thereto. After stirring to make a uniform solution, the mixture was allowed to stand at 45 ° C. overnight and gelled. When this gel was dried at 45 ° C. for 1 week, a dry gel having a dry weight of 24.8 g was obtained. The dried gel was crushed to obtain a powder A for cosmetics containing 21.8% of triclosan.

この粉体Ａを用いてボディパウダーを調製し、その防臭
効果及び効果の持続性について下記の評価方法により評
価した。その結果を表−１に示す。A body powder was prepared using this powder A, and its deodorizing effect and the sustainability of the effect were evaluated by the following evaluation methods. The results are shown in Table-1.

評価方法 （１） 防臭効果試験 腋臭が強いと判定されたパネラー男15名、女15名の計30
名で下記の試験を行った。Evaluation method (1) Deodorant effect test A total of 30 male and female 15 panelists judged to have strong axillary odor
The following tests were conducted by name.

入浴後、パネラーの一方の腋下に試料を塗布し、他方を
コントロールとした。塗布24時間を経過した後、腋下に
綿パッドを当て、10分後に採取し、パッドの臭気を専門
判定員によりコントロールと比較した。コントロールよ
りも明らかに臭気強度が強い場合を体臭防止効果が良好
であるとした。数値はパネラー30名中の効果を認めた人
数で表わした。After bathing, the sample was applied to one armpit of the panelist, and the other was used as a control. After 24 hours from the application, a cotton pad was applied to the armpit, and 10 minutes later, the odor of the pad was compared with the control by a specialist judge. When the odor intensity was obviously stronger than that of the control, the body odor prevention effect was considered good. The numerical value is represented by the number of persons who recognized the effect among 30 panelists.

（２） 防臭効果持続試験 上記パネラー10名（男５名、女５名）で下記の試験を行
った。上記と同様にパネラーの腋下に試料を塗布し、他
方をコントロールとして、試料塗布後、２日間入浴せず
に３日目に臭気を上記と同様に判定した。コントロール
よりも明らかに臭気強度が弱い場合を防臭効果の持続性
が良好であるとした。数値はパネラー10名中の持続効果
を認めた人数で表わした。(2) Deodorant effect duration test The following test was conducted by 10 panelists (5 males and 5 females). The sample was applied to the axilla of the panel in the same manner as above, and the other side was used as a control, and after application of the sample, the odor was determined in the same manner as above on the 3rd day without bathing for 2 days. When the odor intensity was clearly weaker than that of the control, the deodorizing effect was lasting longer. The numerical value was expressed by the number of 10 panelists who confirmed the sustained effect.

〔ボディパウダー組成〕[Body powder composition]

本発明品 粉体A: 2.3％ （本発明品中にトリクロサンとして0.5％を含有） タルク： 87.9 炭酸マグネシウム： 5.0 ステアリン酸マグネシウム： 3.0 香 料 適 量 比較例 タルク： 91.5％ トリクロサン： 0.5 炭酸マグネシウム： 5.0 ステアリン酸マグネシウム： 3.0 香 料 適 量 表−１により本発明品は防臭効果が良好であり、比較例
に比べ防臭持続効果が特に優れていることがわかる。Product of the present invention Powder A: 2.3% (containing 0.5% of triclosan in the product of the present invention) Talc: 87.9 Magnesium carbonate: 5.0 Magnesium stearate: 3.0 Fragrance suitable amount Comparative example Talc: 91.5% Triclosan: 0.5 Magnesium carbonate: 5.0 Magnesium stearate: 3.0 Fragrance Suitable amount From Table 1, it can be seen that the product of the present invention has a good deodorizing effect and is particularly excellent in the deodorizing sustaining effect as compared with the comparative example.

実施例２ トリクロサンの２％のエタノール溶液6.75gを用いた以
外には実施例１と同様にしてトリクロサンを0.5％含有
する化粧料用粉体Ｂを得た。Example 2 A cosmetic powder B containing 0.5% triclosan was obtained in the same manner as in Example 1 except that 6.75 g of a 2% ethanol solution of triclosan was used.

このＢ粉体を用いて下記のエアゾールを調製し、その防
臭効果及びその効果の持続性について実施例１と同様に
評価した。結果を表−２に示す。The following aerosol was prepared using this B powder, and the deodorizing effect and the sustainability of the effect were evaluated in the same manner as in Example 1. The results are shown in Table-2.

〔エアゾール組成〕[Aerosol composition]

本発明品 粉体B: 3.0％ （本発明品中にトリクロサンとして0.015％含有） イソプロピルミリステート 0.5 香 料 適量 フロン12/フロン11（30/70） バランス 比較例 タルク： 3.0％ トリクロサン 0.015％ イソプロピルミリステート 0.5％ 香 料 適量 フロン12/フロン11（30/70） バランス 表−２より、明らかに本発明品は防臭効果が良好であ
り、比較例に比べ防臭持続性に特に優れていることがわ
かる。Product of the present invention Powder B: 3.0% (0.015% as triclosan in the product of the present invention) Isopropyl myristate 0.5 Fragrance Freon 12 / Freon 11 (30/70) Balance Comparative Example Talc: 3.0% Triclosan 0.015% Isopropyl milli State 0.5% Fragrance Suitable amount CFC12 / CFC11 (30/70) Balance From Table 2, it is apparent that the product of the present invention has a good deodorizing effect and is particularly excellent in deodorizing durability as compared with Comparative Examples.

実施例３ Si（OCH3）445.6g（0.3モル）に28mmol/の塩酸水54g
を加え、室温で１時間攪拌した後、1/2規定のアンモニ
ア水でpH5.0に調整した。油分として流動パラフィン3.7
5gとパルミチ酸イソプロピル3.75gを用い、これを水21.
6gに乳化した液を加えて前記アルキルシリケート溶液に
攪拌して乳濁液を得た。45℃で１夜静置したところゲル
化した。このゲルを粉砕したのち室温で減圧乾燥させ乾
燥重量30gの化粧料用粉体Ｃを得た。この粉体を用いて
油性ファンデーションを調製し、皮膚への付着性、付着
の持続性、べたつきのなさについて評価した。Example 3 54 mmol of 28 mmol / hydrochloric acid in 45.6 g (0.3 mol) of Si (OCH 3 ) 4
Was added, and the mixture was stirred at room temperature for 1 hour, and then adjusted to pH 5.0 with 1 / 2N ammonia water. Liquid paraffin as oil 3.7
5 g and isopropyl palmitate 3.75 g were used, and this was water 21.
The emulsified liquid was added to 6 g, and the mixture was stirred in the alkyl silicate solution to obtain an emulsion. When it was allowed to stand at 45 ° C overnight, it gelled. The gel was crushed and then dried under reduced pressure at room temperature to obtain a powder C for cosmetics having a dry weight of 30 g. An oily foundation was prepared using this powder, and the adhesion to the skin, the persistence of the adhesion, and the non-stickiness were evaluated.

評価方法 20℃、50％RHの条件の部屋において、調製した試料を乾
いた肌に塗布して皮膚への付着性、べたつきのなさ及び
８時間後の皮膚への付着の持続性について次の基準で官
能評価した。結果を表−３に示す。Evaluation method In a room at 20 ° C and 50% RH, apply the prepared sample to dry skin, and then adhere to the skin, non-greasiness and persistence of adherence to the skin after 8 hours It was sensory evaluated. The results are shown in Table-3.

皮膚への付着性及びその持続性 ◎非常にある ○ある △ややある ×ほとんどない べたつきのなさ ◎べたつきが全くない ○ない △ややある ×べたつく 本発明品 粉体Ｃ 40％ （本発明品中に流動パラフィンとして５％、パルミチン
酸イソプロピル５％含有） 流動パラフィン 15 パルミチン酸イソプロピル 10 ラノリン 5 マイクロクリスタリンワックス 7 オゾケライト 8 酸化チタン 10 カオリン 5 香 料 適量 比較例 流動パラフィン 20％ パルミチン酸イソプロピル 15 ラノリン 5 マイクロクリスタリンワックス 7 オゾケライト 8 酸化チタン 20 カオリン 20 タルク 5 香 料 適量 実施例４ エチルシリケート40を45g、エタノール54gに100mmol/
の塩酸水54gを加え、室温で１時間攪拌した。この溶液
を1/2規定のアンモニア水でpH5.0に調製したのち、Ｐ−
アミノ安息香酸（紫外線吸収剤）の20％エタノール溶液
10gを添加した。これを攪拌して均一溶液を得たのち45
℃で１夜静置してゲル化させた。生成したゲルを45℃で
１週間乾燥させて乾燥重量25gの乾燥ゲルを得た。この
乾燥ゲルを粉砕してＰ−アミノ安息香酸８％を含有する
化粧料用粉体Ｄを得た。Adhesion to the skin and its persistence ◎ Very good ○ Some △ Somewhat × Almost no stickiness ◎ No stickiness ○ No △ Somewhat sticky × Product of the present invention Powder C 40% (in the product of the present invention Liquid paraffin contains 5% and isopropyl palmitate 5%) Liquid paraffin 15 Isopropyl palmitate 10 Lanolin 5 Microcrystalline wax 7 Ozokerite 8 Titanium oxide 10 Kaolin 5 Fragrance Suitable amount Comparative example Liquid paraffin 20% Isopropyl palmitate 15 Lanolin 5 Microcrystalline Wax 7 Ozokerite 8 Titanium oxide 20 Kaolin 20 Talc 5 Fragrance Example 4 45 mmol of ethyl silicate 40 and 100 mmol / in 54 g of ethanol
54 g of hydrochloric acid water was added, and the mixture was stirred at room temperature for 1 hour. The pH of this solution was adjusted to 5.0 with 1/2 normal ammonia water, and then P-
20% ethanol solution of aminobenzoic acid (UV absorber)
10 g was added. After stirring this to obtain a uniform solution, 45
The mixture was left to stand overnight at 0 ° C. for gelation. The produced gel was dried at 45 ° C. for 1 week to obtain a dry gel having a dry weight of 25 g. The dried gel was pulverized to obtain a cosmetic powder D containing 8% of P-aminobenzoic acid.

この粉体を用いてサンタンローションを調製したとこ
ろ、このローションは日やけ止め効果に優れ、かつ皮膚
に対する刺激性が認められないというすぐれた効果を有
することがわかった。When a suntan lotion was prepared using this powder, it was found that this lotion had an excellent sunscreen effect and an excellent effect that no irritation to the skin was observed.

サンタンローション 粉体 20 ％ PEG＃600 5 ％ ポリアクリル酸ソーダ（カーボポール＃940） 1.5％ ジイソプロパノールアミン 適量 香 料 適量 精製水 バランス 実施例５ Si（OC2H5）462.5g（0.3モル）に28mmol/の塩酸水27g
を加え、室温で１時間攪拌して均一溶液を得た。この液
を45℃で１夜静置してゲル化させた。このゲルを10％グ
リセリン水溶液54gに浸漬し、24時間静置後そのまま、4
5℃の乾燥器で１週間乾燥させた。乾燥重量は31gであり
粉砕して、グリセリン（保湿剤）を17.4％、水分を22％
含む化粧料用粉体を得た。Suntan lotion Powder 20% PEG # 600 5% Sodium polyacrylate (Carbopol # 940) 1.5% Diisopropanolamine Appropriate amount Fragrance Appropriate amount Purified water balance Example 5 Si (OC 2 H 5 ) 4 62.5 g (0.3 mol) 28 mmol / hydrochloric acid water 27 g
Was added and stirred at room temperature for 1 hour to obtain a uniform solution. This solution was allowed to stand at 45 ° C. overnight for gelation. Immerse this gel in 54 g of 10% glycerin aqueous solution, leave it for 24 hours, and then
It was dried in a dryer at 5 ° C for 1 week. The dry weight is 31g, and it is pulverized to 17.4% glycerin (moisturizer) and 22% water.
A cosmetic powder containing it was obtained.

この粉体を30％RH湿度下に25℃で24時間保存をしても17
％の水分を乾しており、優れた保温性能を示した。Even if this powder is stored for 24 hours at 25 ° C under 30% RH humidity, 17
% Of water was dried and showed excellent heat retention performance.

実施例６ Si（OC2H5）462.5g（0.3モル）に28mmol/の塩酸水54g
を加え、室温で１時間攪拌後20％塩化ベンジルコニウム
水溶液を27g加えた。この溶液を1/2規定のアンモニア水
でpH5に調整後、すぐにシクロヘキサン1000ml、ソルビ
タンモノステアレート10gのはいった液中へ室温で攪拌
しながらゆっくりと滴下した。滴下終了後液温を50℃に
あげ２時間攪拌した。その後攪拌を停止すると滴下した
液は微小球状にゲル化して沈降した。このゲルをろ過で
取り出し、減圧乾燥させた。この乾燥ゲルは殺菌剤とし
て塩化ベンザルコニウムを含有し、平均粒径10μの球状
粉体であり、市販の気相法シリカ、湿式法シリカ、実施
例１〜５の粉砕した粉体よりも滑性に優れていた。Example 6 Si (OC 2 H 5 ) 4 62.5 g (0.3 mol) and 28 mmol / hydrochloric acid water 54 g
Was added, and the mixture was stirred at room temperature for 1 hour, and 27 g of a 20% aqueous benzirconium chloride solution was added. This solution was adjusted to pH 5 with 1/2 N ammonia water, and immediately thereafter, it was slowly added dropwise to a liquid containing 1000 ml of cyclohexane and 10 g of sorbitan monostearate at room temperature while stirring. After completion of dropping, the liquid temperature was raised to 50 ° C. and the mixture was stirred for 2 hours. After that, when stirring was stopped, the dropped liquid gelled into a fine spherical shape and settled. This gel was taken out by filtration and dried under reduced pressure. This dry gel contains benzalkonium chloride as a bactericide and is a spherical powder having an average particle size of 10 μ. It was excellent.

Claims (2)

【特許請求の範囲】[Claims] 【請求項１】一般式〔Ｉ〕： （式中、R1〜R4は、水素又はCxH2x＋１（OC2H4）ｙ−
（但し、ｘは１〜５、ｙは０〜10の整数を示す。）で示
される基であるが、R1〜R4のすべてが水素であることは
ない。ｎは０〜20の整数である。） で表わされる少なくとも１種のアルキルシリケートの加
水分解、重縮合反応を化粧料成分の存在で行ってゲルを
形成させた後、又は該反応によりゲルを形成した後に化
粧料成分を該ゲルに含浸させた後、乾燥することを特徴
とする化粧料用粉体の製造方法。1. A general formula [I]: (In the formula, R 1 to R 4 are hydrogen or CxH 2 x + 1 (OC 2 H 4 ) y−
(However, x is an integer of 1 to 5 and y is an integer of 0 to 10.) However, not all of R 1 to R 4 are hydrogen. n is an integer of 0-20. ) After the hydrolysis and polycondensation reaction of at least one alkyl silicate represented by the formula (1) is performed in the presence of the cosmetic ingredient to form a gel, or after the gel is formed by the reaction, the gel is impregnated with the cosmetic ingredient. A method for producing a powder for cosmetics, which comprises drying after the drying. 【請求項２】ゲルを球状に成形した後に乾燥する特許請
求の範囲第１項記載の方法。2. The method according to claim 1, wherein the gel is formed into a spherical shape and then dried.
JP62057602A 1987-03-12 1987-03-12 Method for producing powder for cosmetics Expired - Lifetime JPH07100644B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62057602A JPH07100644B2 (en) 1987-03-12 1987-03-12 Method for producing powder for cosmetics

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62057602A JPH07100644B2 (en) 1987-03-12 1987-03-12 Method for producing powder for cosmetics

Publications (2)

Publication Number Publication Date
JPS63225310A JPS63225310A (en) 1988-09-20
JPH07100644B2 true JPH07100644B2 (en) 1995-11-01

Family

ID=13060402

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62057602A Expired - Lifetime JPH07100644B2 (en) 1987-03-12 1987-03-12 Method for producing powder for cosmetics

Country Status (1)

Country Link
JP (1) JPH07100644B2 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0812546A (en) * 1994-06-30 1996-01-16 Toray Dow Corning Silicone Co Ltd Anti-suntan cosmetic

Also Published As

Publication number Publication date
JPS63225310A (en) 1988-09-20

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