JPH10194929A - Antimicrobial pigment for cosmetic, production of the pigment, and cosmetic composition containing the pigment - Google Patents

Antimicrobial pigment for cosmetic, production of the pigment, and cosmetic composition containing the pigment

Info

Publication number
JPH10194929A
JPH10194929A JP9015843A JP1584397A JPH10194929A JP H10194929 A JPH10194929 A JP H10194929A JP 9015843 A JP9015843 A JP 9015843A JP 1584397 A JP1584397 A JP 1584397A JP H10194929 A JPH10194929 A JP H10194929A
Authority
JP
Japan
Prior art keywords
antibacterial
cosmetics
particles
pigment
powder
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.)
Pending
Application number
JP9015843A
Other languages
Japanese (ja)
Inventor
Masaaki Horino
政章 堀野
Yoshikazu Nishizawa
美和 西澤
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.)
Miyoshi Kasei Inc
Original Assignee
Miyoshi Kasei Inc
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 Miyoshi Kasei Inc filed Critical Miyoshi Kasei Inc
Priority to JP9015843A priority Critical patent/JPH10194929A/en
Priority to FR9804668A priority patent/FR2777457B1/en
Publication of JPH10194929A publication Critical patent/JPH10194929A/en
Pending legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005—Antimicrobial preparations
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/06—Aluminium; Calcium; Magnesium; Compounds thereof
    • 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
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04—Antibacterial agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • 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
    • A61K2800/42—Colour properties
    • A61K2800/43—Pigments; Dyes
    • 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
    • A61Q1/02—Preparations containing skin colorants, e.g. pigments
    • 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
    • A61Q1/12—Face or body powders for grooming, adorning or absorbing
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases

Abstract

PROBLEM TO BE SOLVED: To obtain the subject pigment without damaging an antimicrobial activities, without causing transubstantiation of cosmetics and good in feeling in use by using antimicrobial fired particles obtained by firing magnesium oxide at a specific temperature, and further to obtain the subject composition. SOLUTION: This antimicrobial pigment for cosmetics includes antimicrobial fired particles comprising magnesium oxide obtained by firing one or more kinds of magnesium hydroxide and magnesium oxide at >=850 deg.C. The antimicrobial pigment also can include antimicrobial complex powder particles obtained by adhering powder particles for cosmetics to the antimicrobial fired particles obtained by the before way. The pigment provides no bad effect to a human body, thereby has no limit of a using amount imposed thereon, and does not affected by the pH of the cosmetics, or various coexisting components in the cosmetics when formulated in the cosmetics.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、化粧料用抗菌性顔
料（化粧料用抗菌性粉体顔料と化粧料用抗菌性複合粉体
顔料）、これらの顔料の製造方法及び、前記顔料のうち
の１種以上を含有する抗菌性化粧料組成物に関する。TECHNICAL FIELD The present invention relates to an antibacterial pigment for cosmetics (an antibacterial powder pigment for cosmetics and an antibacterial composite powder pigment for cosmetics), a process for producing these pigments, and The present invention relates to an antibacterial cosmetic composition containing at least one of the following.

【０００２】より詳細には、水酸化マグネシウム及び酸
化マグネシウムのうちの１種以上から成る抗菌性粒子を
高温で焼成することにより、吸湿性を防止し、経時安定
性が高く、化学的にも安定な抗菌性を有する、酸化マグ
ネシウムから成る抗菌性焼成粒子を含有する化粧料用抗
菌性顔料、前記化粧料用抗菌性顔料の製造方法及び前記
化粧料用抗菌性顔料を配合してなる化粧料組成物に関す
るものである。More specifically, antibacterial particles composed of one or more of magnesium hydroxide and magnesium oxide are calcined at a high temperature to prevent hygroscopicity, have high stability over time, and are chemically stable. Antibacterial pigment for cosmetics containing antibacterial baked particles composed of magnesium oxide having high antibacterial properties, a method for producing the antibacterial pigment for cosmetics, and a cosmetic composition comprising the antibacterial pigment for cosmetics It is about things.

【０００３】[0003]

【従来の技術】微生物は酒類や醗酵食品の生産を姶めと
して、各種の生理活性物質や抗生物質、環境浄化等の分
野や様々な分野で利用されており、化粧品分野でもその
有効利用が図られている。一方、微生物のもつこの様々
な能力が、逆に我々にとって望ましくない侵害という形
で現れることもある。化粧品が、微生物により汚染され
た場合には、製品の変色、異臭、混濁、酸敗、沈殿物や
浮遊物の発生、スライム生成など、我々が認知できる形
で現れることもあるが、このような形では表面化せず、
汚染を知らずに使用し続けるということも起こりうる。
一般的に、化粧品は無菌性を要求される製品ではない
が、本来、使用者に清潔さと美しさを提供するものであ
り、「微生物汚染」というトラブルがあってはならない
ものである。2. Description of the Related Art Microorganisms are used in various fields such as various physiologically active substances, antibiotics, environmental purification, etc. in the production of alcoholic beverages and fermented foods. Have been. On the other hand, the various abilities of microorganisms can manifest themselves in the form of infringements that are undesirable to us. If cosmetics are contaminated by microorganisms, they may appear in a form that we can recognize, such as discoloration of the product, off-flavor, turbidity, rancidity, generation of precipitates and suspended matter, and slime formation. Does not surface
Continued use without knowledge of contamination can also occur.
In general, cosmetics are not products that require sterility, but they are originally intended to provide users with cleanliness and beauty, and should not have the trouble of "microbial contamination".

【０００４】化粧品類はもともと微生物の増殖に好都合
な栄養分を含みまた、微生物汚染の高い天然物由来の原
料を使用する場合が多く、さらに安全性の問題から防腐
剤の種類や使用量に制限がある上に、多くの場合、最終
製品での滅菌も製品品質上ほとんど不可能に近く、より
厳密な無菌性を要求される医薬品や腐敗が起こりうるこ
とが一般的に認知されている食品とは異なった困難さを
抱えている。[0004] Cosmetics originally contain nutrients that are favorable for the growth of microorganisms, and in many cases use raw materials derived from natural products that are highly contaminated with microorganisms. In addition, the type and amount of preservatives are limited due to safety issues. In addition, in many cases, sterilization of the final product is almost impossible in terms of product quality.Pharmaceuticals that require stricter sterility and foods that are generally recognized as capable of causing spoilage are They have different difficulties.

【０００５】製品の微生物汚染は製造段階で起こる一次
汚染と、消費者の使用中に起こる二次汚染とに大別でき
る。一次汚染は、衛生的な製造設備や管理により、二次
汚染は適切な防腐剤の配合や、容器の材質や形態などの
工夫により防ぐことが基本とされている。微生物汚染
は、原料そのものから製品の腐敗や、作業者、製造工
程、環境、包装、保存、さらにこれらに付随する詳細な
項目があるが、これらを完全にまっとうするのは不可能
に近い。こうしたことから、化粧品に防腐殺菌剤を添加
する目的は、原料から製造設備、製造管理からくる一次
汚染と消費者の使用中に発生する二次汚染をより抑制
し、微生物による変質、変色、カビの発生等を防止する
ことにある。[0005] Microbial contamination of products can be broadly divided into primary contamination that occurs during the manufacturing stage and secondary contamination that occurs during consumer use. It is fundamental to prevent primary pollution by sanitary manufacturing equipment and management, and to prevent secondary pollution by mixing appropriate preservatives and devising the material and form of the container. Microbial contamination involves spoilage of products from raw materials themselves, workers, manufacturing processes, environment, packaging, preservation, and detailed items associated therewith, but it is almost impossible to completely eliminate them. For this reason, the purpose of adding preservatives and disinfectants to cosmetics is to further reduce primary pollution from raw materials, manufacturing equipment and manufacturing control, and secondary pollution that occurs during consumer use, and to prevent deterioration, discoloration, and mold by microorganisms. The purpose of the present invention is to prevent the occurrence of the problem.

【０００６】水銀性化合物は防腐殺菌効果をもっている
にもかかわらず、毒性が強いため、現在では厳格な法規
制により、化粧料における使用は禁止されている。一般
に細菌を含む微生物が増殖するためには水と栄養分と更
には増殖しやすい適度な温度、湿度を必要とする。化粧
品には、種々の原料が用いられているが、微生物はこの
ような原料の炭素源、あるいは窒素源を利用して増殖す
る。従って、水を含む製品ほど微生物の増殖が容易なた
め、そのリスクは大きく、非水系の製品ではそのリスク
は小さい。[0006] Although mercury compounds have a preservative and bactericidal effect, they are highly toxic. Therefore, strict laws and regulations have banned their use in cosmetics at present. Generally, in order for microorganisms including bacteria to proliferate, water, nutrients, and an appropriate temperature and humidity that facilitate growth are required. Various raw materials are used for cosmetics, and microorganisms grow by utilizing the carbon source or the nitrogen source of such raw materials. Therefore, the risk is greater for products containing water, since the growth of microorganisms is easier, and the risk is smaller for non-aqueous products.

【０００７】粉体メークアップ製品は油剤、界面活性
剤、粉体原料などにより構成され、通常、水を配合する
ケースは少ない。このために細菌、酵母は増殖しにくい
という処方上の特徴をもっている。しかし、カビについ
ては、製品のおかれる環境によっては、製品の表面に菌
系が伸張し、胞子形成まで至る。消費者は、化粧品の保
存場所にあまり気を使わないこともある。従って使用中
断後再使用する際カビが表面に発生したというケースも
多々ある。こうしたことを鑑みた時、製造時の一次汚染
防止を行うと同時に二次汚染防止のための適切な防腐殺
菌力を付与する必要がある。[0007] A powder make-up product is composed of an oil agent, a surfactant, a powder raw material and the like, and water is usually rarely mixed. For this reason, bacteria and yeast have the characteristic of formulation that they are difficult to grow. However, with regard to mold, depending on the environment in which the product is placed, the bacterial system extends to the surface of the product, leading to sporulation. Consumers may be less concerned about where cosmetics are stored. Therefore, there are many cases in which mold is generated on the surface when reusing after the use is interrupted. In view of the above, it is necessary to prevent primary contamination at the time of production and at the same time to impart appropriate antiseptic and sterilizing power for preventing secondary contamination.

【０００８】化粧品に用いられていた又は用いられてい
る防腐殺菌剤としては、パラオキシ安息香酸エステル、
サルチル酸、ヒノキチオール、フェノキシエタノール、
デヒドロ酢酸ナトリウム、安息香酸とその塩、アミノ酸
化第二水銀、ホウ砂、３−トリフルオロメチル−４，
４’ジクロルカルバニリド、Ｐ−フェノールスルフォン
酸亜鉛、ビオサルファ−Ｆ（ポリソルベート８０と沈降
イオウの混合物）、４−ヒドロキシ−２−オキシベンゾ
キサチオール、ヘキサクロロフェン、アルキルジメチル
ベンジルアンモニウムクロライド（塩化ベンザルコニウ
ム）、塩化ベンゼトニウム、クロルヘキシジンジグルコ
ネート２０％水溶液、２，４，４’−トリクロロ−２’
ハイドロキシジフェニルエーテル、塩化セチルピリジウ
ム、レゾルシン、ＤＭＤＭビダントインイソチアゾリン
オン、イミダゾリジニルウレア、等がある。The preservatives used or used in cosmetics include paraoxybenzoate,
Salicylic acid, hinokitiol, phenoxyethanol,
Sodium dehydroacetate, benzoic acid and its salts, amino acidated mercuric acid, borax, 3-trifluoromethyl-4,
4'-dichlorocarbanilide, zinc P-phenolsulfonate, biosulfur-F (a mixture of polysorbate 80 and precipitated sulfur), 4-hydroxy-2-oxybenzoxathiol, hexachlorophen, alkyldimethylbenzylammonium chloride (benza chloride chloride) Ruconium), benzethonium chloride, 20% aqueous solution of chlorhexidine digluconate, 2,4,4'-trichloro-2 '
Hydroxydiphenyl ether, cetylpyridinium chloride, resorcinol, DMDM bidantinisothiazolinone, imidazolidinyl urea, and the like.

【０００９】また、特開平７−１０８２１号公報には、
特定の抗菌性組成物を配合した化粧料が開示されてお
り、特開平８−４０８３０号公報には、特定の抗菌性化
粧料用顔料とその製造方法及び前記顔料を含有する化粧
料組成物が開示されている。[0009] Japanese Patent Application Laid-Open No. 7-10821 discloses that
JP-A-8-40830 discloses a cosmetic composition containing a specific antimicrobial composition, a specific antimicrobial cosmetic pigment, a method for producing the same, and a cosmetic composition containing the pigment. It has been disclosed.

【００１０】[0010]

【発明が解決しようとする課題】しかし、上述の防腐殺
菌剤は、それ自身が人体に及ぼす悪影響があり、安全性
の問題のために配合限度を定めて、使用量を規制し、表
示成分として取り扱われている物質が多い。However, the above-mentioned antiseptic disinfectant itself has an adverse effect on the human body. Therefore, in view of safety problems, the amount of the antiseptic disinfectant is set by limiting the amount of the antiseptic disinfectant and regulating the amount of use. Many substances are handled.

【００１１】例えば、サルチル酸は０．２％（重量％）
以下、パラオキシ安息香酸エステルは１．０％以下、デ
ヒドロ酢酸ナトリウムは０．５％以下、レゾルシンは
０．１％以下の規制がある。中には、３−トリフルオロ
メチル−４，４’ジクロルカルバニリドによるリール黒
皮症の原因物質の問題、ｐ−フェニルスルフォン酸亜鉛
によるアレルギー性の問題、ヘキサルクロフエンによる
神経毒性の問題等のように問題点を有する防腐殺菌剤も
あり、また、レゾルシンの様に染毛料に限定するなど化
粧品メーカーにより自主規制している防腐殺菌剤も少な
くない。For example, salicylic acid is 0.2% (% by weight)
Hereinafter, there are regulations of 1.0% or less for paraoxybenzoate, 0.5% or less for sodium dehydroacetate, and 0.1% or less for resorcin. Among them, 3-trifluoromethyl-4,4'-dichlorocarbanilide causes a problem of the melanosis of Lille, zinc p-phenylsulfonate has an allergic problem, and hexachloroclophen has a neurotoxicity problem. There are also preservatives and disinfectants which have problems such as, for example, and there are a number of preservatives and disinfectants which are voluntarily regulated by cosmetic manufacturers such as resorcinol, which is limited to hair dyes.

【００１２】ヒノキチオールは表示成分ではないが、光
安定性が悪いという欠点がある他、金属イオンと反応し
て錯イオンを形成し、例えば鉄イオンとの錯イオンは暗
赤色、マンガンとの錯イオンは淡褐色、銅イオンとの錯
イオンは緑色、アルミニウムイオンとの錯イオンは白色
に着色し、製品の外観を損なう欠点をもっている。Although hinokitiol is not a display component, it has the disadvantage of poor light stability and also reacts with metal ions to form complex ions. For example, complex ions with iron ions are dark red, complex ions with manganese Is colored light brown, complex ions with copper ions are colored green, and complex ions with aluminum ions are colored white, which impairs the appearance of the product.

【００１３】フェノキシエタノールは表示成分ではない
が通常配合される０．１〜０．２％程度の配合では防腐
殺菌効果が認められず、通常汎用される配合濃度ではそ
の効果が期待できず、好ましい防腐殺菌剤とは言い難
い。Although phenoxyethanol is not a labeling component, the antiseptic and bactericidal effect is not recognized when it is normally added at a concentration of about 0.1 to 0.2%, and the effect cannot be expected at the compounding concentration which is generally used. It is hard to say a fungicide.

【００１４】一方、化粧料に配合された防腐殺菌剤の防
腐殺菌効果に影響を与える因子としては、化粧料のｐ
Ｈ、防腐殺菌剤の溶解度（分配係数）、化粧料において
共存するノニオン活性剤、粉体、保湿剤、水溶性高分子
の各々の種類や容器の材質等がある。On the other hand, factors affecting the antiseptic and bactericidal effects of the antiseptic and germicide incorporated in the cosmetics include p
H, the solubility (partition coefficient) of the antiseptic disinfectant, the type of nonionic activator, powder, humectant, and water-soluble polymer coexisting in cosmetics, and the material of the container.

【００１５】例えば、パラオキシ安息香酸エステル（パ
ラベン）は、ｐＨがアルカリ側での加水分解安定性に課
題がある。通常のスキンケア商品は、ｐＨが８前後の商
品が多い。パラベン類は、ｐＨ８以上では、防腐殺菌効
果が弱く、ｐＨ８でのその必要量はｐＨ４の約２倍量必
要である。また、パラベン類は、低温での結晶の析出も
課題になっている。パラベン類は、多くの紫外線吸収剤
やイソプロピルミリステート、ひまし油、等の高極性油
に対しては、パラベンが取り込まれ防腐殺菌効果が低下
する。また、パラベン類は、高ＨＬＢの界面活性剤が共
存すると抗菌活性が著しく低下してしまうことがある。
これは、界面活性剤のミセルに可溶化され、界面活性剤
がパラベンとコンプレックスを形成し、不活性化すると
言われている。高分子化合物も、同様にパラベンと錯体
を形成し、防腐活性を著しく弱めるとされている。For example, paraoxybenzoic acid ester (paraben) has a problem in hydrolytic stability when the pH is on the alkaline side. There are many normal skin care products whose pH is around 8. Parabens have a weak preservative / sterilizing effect at pH 8 or higher, and their required amount at pH 8 is about twice that of pH 4. In addition, parabens also have a problem of crystal precipitation at low temperatures. Parabens are incorporated into many ultraviolet absorbers and highly polar oils such as isopropyl myristate, castor oil, etc., so that their antiseptic and sterilizing effects are reduced. Moreover, the antibacterial activity of parabens may be significantly reduced in the presence of a surfactant having a high HLB.
It is said that this is solubilized in the micelles of the surfactant, and the surfactant forms a complex with the paraben and inactivates it. It is said that a high molecular compound also forms a complex with paraben and significantly reduces preservative activity.

【００１６】粉体については有機樹脂粉末へのパラベン
の吸着により防腐殺菌効果が低下し、それら処方系への
有機樹脂粉末の配合は、微生物対策の面から配合量制限
を受けている。また、容器等の材質によっては、防腐剤
が吸着してしまい、期待した防腐効果が得られない場合
も多い。さらに化粧科において、有用物質としての生理
活性物質を配合する場合が多く、例えば、エリスリトー
ルやプラセンターエキスに見られるように、資化性のあ
る物質が多く、パラベンの防腐力の低下をまねく物質が
多く、抗菌力の低下の一翼になっている。The preservative sterilization effect of the powder is reduced by the adsorption of paraben to the organic resin powder, and the compounding amount of the organic resin powder in these formulation systems is limited in terms of microbial control. Further, depending on the material of the container or the like, the preservative may be adsorbed and the expected preservative effect may not be obtained in many cases. Furthermore, in cosmetics, there are many cases where a physiologically active substance is added as a useful substance.For example, as seen in erythritol and placenta extract, there are many assimilable substances, and substances that reduce the preservative power of paraben. Many, which is one of the factors that reduce antibacterial activity.

【００１７】防腐殺菌剤は、それ自体に刺激性があるた
め、表示成分のものが非常に多く、化粧品メーカーによ
っては、自主規制、あるいは、統制物質あるいは使用禁
止物質として取り扱っているものが少なくない。１９８
０年に薬事法の改正があり、防腐剤を含む成分表示が義
務付けられ、国内商品は、圧倒的にパラベンの表示が多
く見受けられるが、上述のように化粧料組成物のｐＨの
影響、非イオン界面活性剤の使用や水溶性高分子による
ミセル内への可溶性あるいは、錯体の形成による防腐力
の低下、生理活性物質配合による資化性物質の配合、使
用感の向上からくる極性油剤の多様化等により、パラベ
ンのみでは防腐殺菌効果の保持が難しく、他の防腐殺菌
剤との併用が余儀なくされ、化粧料の安定性は、もちろ
んのこと、安全性の確保に課題を残している。Since antiseptic disinfectants are irritating in themselves, there are very many of them with labeling components, and some cosmetics manufacturers treat them as self-regulated, controlled, or banned substances. . 198
Since the revision of the Pharmaceutical Affairs Law in 1998, labeling of ingredients including preservatives is mandatory, and in domestic products, parabens are overwhelmingly seen, but as described above, the effects of the pH of the cosmetic composition, Use of ionic surfactants, solubility in micelles by water-soluble polymers, or decrease in preservative power due to complex formation, blending of assimilable substances by blending bioactive substances, and improvement of usability As a result, parabens alone make it difficult to maintain the antiseptic and bactericidal effects, and must be used in combination with other antiseptic and bactericidal agents, leaving a problem not only in the stability of cosmetics but also in ensuring safety.

【００１８】一方、特開平７−１０８２１号公報には、
酸化亜鉛、酸化ジルコニウム、酸化チタン、酸化マグネ
シウム、酸化ケイ素、リン酸３カルシウム、ハイドロキ
シアパタイト、炭酸カルシウム、タルク、及び、ゼオラ
イトから選ばれた少なくとも一つのセラミックスに、
銀、銅及び亜鉛から選ばれた抗菌性金属を担持させた抗
菌性組成物を配合した化粧料が開示されている。また、
特開平８−４０８３０号公報には、化粧品用無機顔料の
表面にガラス質の無定形コーティング層を形成し、抗菌
性金属として、銀、銅、亜鉛を用いた抗菌性金属をコー
ティング層の結合格子内に固溶化させて、製造する抗菌
性化粧料用顔料とその製造方法及びこれを含有する化粧
料組成物が開示されている。On the other hand, JP-A-7-10821 discloses that
Zinc oxide, zirconium oxide, titanium oxide, magnesium oxide, silicon oxide, tricalcium phosphate, hydroxyapatite, calcium carbonate, talc, and at least one ceramic selected from zeolites,
A cosmetic composition containing an antibacterial composition carrying an antibacterial metal selected from silver, copper and zinc is disclosed. Also,
JP-A-8-40830 discloses that a glassy amorphous coating layer is formed on the surface of an inorganic pigment for cosmetics, and an antibacterial metal using silver, copper, or zinc is used as the antibacterial metal. Disclosed are an antimicrobial cosmetic pigment which is produced by being dissolved in a solution, a method for producing the pigment, and a cosmetic composition containing the same.

【００１９】しかし、このような抗菌性組成物及び抗菌
性化粧料顔料は、公知の銀、銅、亜鉛の金属あるいは、
それらのイオンによる抗菌を利用したものに過ぎない。
特に、銀や銅は、化粧料に関しては、安全性の課題か
ら、適用が禁止されている抗菌性金属であり、実用に供
しない。また、亜鉛に関しては、銀や銅と比較して抗菌
スペクトルが狭く、亜鉛を用いた抗菌剤のみでは防腐殺
菌剤としての強力な効果は望めない。However, such an antibacterial composition and an antibacterial cosmetic pigment are known silver, copper and zinc metals or
It is nothing but antibacterial effect by those ions.
In particular, silver and copper are antibacterial metals whose application is prohibited for cosmetics due to safety issues, and are not put to practical use. Further, zinc has a narrow antibacterial spectrum as compared with silver and copper, and a strong effect as an antiseptic and bactericide cannot be expected with only an antibacterial agent using zinc.

【００２０】なお、これらの抗菌性金属を担持させるた
めにゼオライト中の金属とイオン交換をさせた抗菌性粉
体も化粧品分野以外の市場に上市されている。しかし、
特に銀を用いた銀ゼオライトは変色しやすい。また、抗
菌性金属を担持した抗菌性ゼオライトは粒子が粗い。従
って、前記抗菌性ゼオライトを化粧料に含有させた場合
は、使用感が悪いほか、化粧料用油剤への酸化促進作用
があり化粧料を変質させる欠点をもっている。In addition, antibacterial powders obtained by ion-exchange with metals in zeolite in order to carry these antibacterial metals are also on the market outside the cosmetics field. But,
In particular, silver zeolite using silver is easily discolored. The antibacterial zeolite carrying the antibacterial metal has coarse particles. Therefore, when the antibacterial zeolite is contained in a cosmetic, the cosmetic has a disadvantage in that it has a poor feeling in use and has an effect of accelerating oxidation to an oil agent for cosmetics and deteriorates the cosmetic.

【００２１】本発明の目的は、上記従来の技術の問題点
を解消し、人体に対して悪影響がなく、使用量の制限を
受けることがなく、化粧料に配合した場合でも化粧料の
ｐＨ、化粧料の各種共存成分等により抗菌力を損なうこ
とがなく、化粧料を変質させることもなく、使用感が良
好な化粧料用抗菌性顔料、その製造方法及び抗菌性化粧
料組成物を提供することにある。[0021] An object of the present invention is to solve the above-mentioned problems of the prior art, to have no adverse effect on the human body, not to be restricted in the amount used, and to improve the pH, Provided is an antibacterial pigment for cosmetics which does not impair the antibacterial activity due to various coexisting components of the cosmetic, does not deteriorate the cosmetic, and has a good feeling in use, a method for producing the same, and an antibacterial cosmetic composition. It is in.

【００２２】また、本発明の他の目的は、微生物である
細菌やカビに対して抗菌力及び殺菌力に優れた新規な化
粧料用抗菌性顔料、その製造方法及び抗菌性化粧料組成
物を提供すること、化粧料に必要とされる防腐殺菌剤の
配合量をより低濃度に抑えた低濃度防腐殺菌剤配合化粧
料や無防腐殺菌剤（防腐殺菌剤フリー）の化粧料の開発
を可能にする化粧料用抗菌性顔料を提供すること、ま
た、既存製品に配合されている防腐殺菌剤による皮膚刺
激がなく、長期間に亘り、安定な防腐殺菌効果をもつ化
粧料組成物を提供することにある。Another object of the present invention is to provide a novel antibacterial pigment for cosmetics having excellent antibacterial activity and bactericidal activity against microorganisms such as bacteria and mold, a method for producing the same, and an antibacterial cosmetic composition. Providing low-concentration preservatives and disinfectants that contain less preservatives and disinfectants, and the development of non-preservatives (free of preservatives and disinfectants) To provide an antibacterial pigment for cosmetics, and to provide a cosmetic composition having a stable antiseptic and bactericidal effect for a long period of time without skin irritation caused by an antiseptic and germicide compounded in existing products. It is in.

【００２３】[0023]

【課題を解決するための手段】本発明者は、上記の従来
技術の問題点を解決すべく鋭意研究をした結果、水酸化
マグネシウム及び酸化マグネシウムはそれぞれ幅広い抗
菌スペクトルを有し、抗菌作用ないし殺菌作用があるこ
と、それにもかかわらず人体に対して悪影響がなく、使
用量の制限を受けることがなく、化粧料に配合した場合
でも化粧料のｐＨ、化粧料の各種共存成分等により抗菌
力を損なうことがなく、化粧料を変質させることもな
く、使用感が良好であるということを見出した。The present inventor has made intensive studies to solve the above-mentioned problems of the prior art, and as a result, magnesium hydroxide and magnesium oxide each have a broad antibacterial spectrum, and have an antibacterial action or sterilization. It has an action, nevertheless has no adverse effect on the human body, is not subject to restrictions on the amount of use, and even when blended in cosmetics, has an antibacterial effect due to the pH of the cosmetics, various coexisting components of the cosmetics, etc. It has been found that the feeling of use is good without impairing or deteriorating the cosmetic.

【００２４】しかしながら、通常、市販されている酸化
マグネシウムは、不安定なので抗菌力の持続性に問題が
あることが判った。例えば、酸化マグネシウムは、吸収
性があり、空気中の水分や炭酸ガスとの反応により、ヒ
ドロキシ炭酸マグネシウム（３ＭｇＣＯ3・Ｍｇ（Ｏ
Ｈ）2・３Ｈ2Ｏ）に変化したり、一般式で表すならば、
酸化マグネシウムがＸＭｇＣＯ3・ＹＭｇ（ＯＨ）2・Ｚ
Ｈ2Ｏになり、又、市販の酸化マグネシウムは水と反応
して水酸化マグネシウムに変化し、細菌類に対しての抗
菌力の低下が見られる。However, it has been found that commercially available magnesium oxide is generally unstable and has a problem in sustaining the antibacterial activity. For example, magnesium oxide is absorptive and reacts with moisture and carbon dioxide in the air to produce magnesium hydroxycarbonate (3MgCO 3 .Mg (O
H) 2・ 3H 2 O) or by a general formula:
Magnesium oxide is XMgCO 3 · YMg (OH) 2 · Z
It becomes H 2 O, and the commercially available magnesium oxide reacts with water to change to magnesium hydroxide, and a decrease in antibacterial activity against bacteria is observed.

【００２５】こうした事実から見ると、酸化マグネシウ
ムの吸湿性をいかに押さえ、耐湿性を保持できるかが問
題である。酸化マグネシウムの耐湿性改善のために特開
昭６１−９１２３２号公報では、酸化マグネシウムの表
面の疎水化、あるいは、樹脂との接合力を改善し、耐湿
性を向上させるために、酸化マグネシウムの表面にサラ
ンカップリング剤やチタネートカップリング剤を処理す
る方法が開示されている。特開昭６１−２８３６４８号
公報では、酸化マグネシウム粉末の表面をシリカで被覆
し、耐湿性に改善する方法が開示されている。特開平１
−１０８１５号公報では、酸化マグネシウム粉末にアル
ミナゾルを添加し、焼成することにより、酸化マグネシ
ウム粉末表面にスピネル酸を形成させ、耐湿性を改善す
る方法が開示されている。In view of these facts, the problem is how to suppress the hygroscopicity of magnesium oxide and maintain the moisture resistance. To improve the moisture resistance of magnesium oxide, Japanese Patent Application Laid-Open No. 61-91232 discloses that the surface of magnesium oxide is hydrophobized or the surface of magnesium oxide is improved in order to improve the bonding strength with resin and improve the moisture resistance. Discloses a method of treating a saran coupling agent or a titanate coupling agent. JP-A-61-283648 discloses a method of coating a surface of a magnesium oxide powder with silica to improve moisture resistance. JP 1
Japanese Patent Publication No. -10815 discloses a method in which alumina sol is added to magnesium oxide powder and baked, thereby forming spinel acid on the surface of the magnesium oxide powder to improve moisture resistance.

【００２６】しかし、上記の技術では、被覆層の機械的
強度や、酸化マグネシウム粉末の被覆が完全でなく十分
な耐湿性が得られず、酸化マグネシウムが経時変化によ
り、上記したようにヒドロキシ炭酸マグネシウムや、あ
るいは水酸化マグネシウムに変化するのは避けられない
ばかりか、酸化マグネシウムのもつ抗菌力ないし殺菌力
が消失するか、著しく低下するという欠点を有する。However, according to the above technique, the mechanical strength of the coating layer and the coating of the magnesium oxide powder are not complete and sufficient moisture resistance cannot be obtained. Not only is it inevitable to change to magnesium hydroxide or magnesium hydroxide, but also has the disadvantage that the antibacterial or bactericidal activity of magnesium oxide is lost or significantly reduced.

【００２７】そこで、本発明者は、酸化マグネシウムを
特定の温度で焼成することにより安定化させることがで
き、抗菌力ないし殺菌力を長期間持続させることができ
るということを見出し、本発明を完成するに至った。例
えば、特定温度の焼成により、吸湿性の高い酸化マグネ
シウムが空気中の水分と炭酸ガスの吸収によりＭｇＣＯ
3・ＭｇＯへ変化することを防止したり、水分の吸収に
よりＭｇ（ＯＨ）2（抗菌性を有するが抗菌性の持続性
に欠ける）へ構造変化することを防止して、経時安定性
が高く抗菌性ないし殺菌性が長期間持続する酸化マグネ
シウムを得ることができる。The present inventors have found that magnesium oxide can be stabilized by firing at a specific temperature, and that the antibacterial or bactericidal activity can be maintained for a long period of time. I came to. For example, when calcined at a specific temperature, highly hygroscopic magnesium oxide absorbs moisture and carbon dioxide in the air to form MgCO.
3. Prevents change to MgO and prevents structural change to Mg (OH) 2 (has antibacterial properties but lacks antibacterial continuity) due to absorption of moisture, resulting in high stability over time. It is possible to obtain magnesium oxide having a long-lasting antibacterial property or sterilizing property.

【００２８】即ち、本発明は、次の化粧料用抗菌性粉体
顔料、化粧料用抗菌性複合粉体顔料、前記各顔料の製造
方法及び抗菌性化粧料組成物により上記目的を達成する
ことができる。That is, the present invention achieves the above object by the following antibacterial powder pigment for cosmetics, antibacterial composite powder pigment for cosmetics, a method for producing each of the pigments, and an antibacterial cosmetic composition. Can be.

【００２９】(1)酸化マグネシウムから成る抗菌性焼成
粒子を含有する化粧料用抗菌性粉体顔料（請求項１）。 (2)酸化マグネシウムから成る抗菌性焼成粒子と化粧料
用粉体粒子が固着して成る抗菌性複合粉体粒子を含有す
る化粧料用抗菌性複合粉体顔料（請求項２）。前記抗菌
性焼成粒子は、安定しており、湿気、水分、炭酸ガス等
と容易に反応しないので、化粧料中に配合した場合でも
安定した状態で存在することができ、抗菌性ないし殺菌
性を長期間に亘り保持することができる。(1) An antibacterial powder pigment for cosmetics containing antibacterial baked particles composed of magnesium oxide (Claim 1). (2) An antibacterial composite powder pigment for cosmetics containing antibacterial baked particles composed of magnesium oxide and antibacterial composite powder particles in which powder particles for cosmetic are fixed (claim 2). The antibacterial baked particles are stable and do not easily react with moisture, moisture, carbon dioxide, etc., so that they can be present in a stable state even when incorporated into cosmetics, and exhibit antibacterial or bactericidal properties. It can be held for a long time.

【００３０】(3)水酸化マグネシウム及び酸化マグネシ
ウムのうちの１種以上から成る抗菌性粒子を８００℃以
上で焼成して抗菌性焼成粒子を得る焼成工程を含む化粧
料用抗菌性粉体顔料の製造方法（請求項３）。 (4)水酸化マグネシウム及び酸化マグネシウムのうちの
１種以上から成る抗菌性粒子を８００℃以上で焼成して
抗菌性焼成粒子を得る焼成工程と、前記焼成工程で得た
抗菌性焼成粒子と化粧料用粉体粒子を固着させて抗菌性
複合粉体粒子を得る複合化工程を含む化粧料用抗菌性複
合粉体顔料の製造方法（請求項４）。(3) An antibacterial powder pigment for cosmetics comprising a firing step of firing antibacterial particles comprising at least one of magnesium hydroxide and magnesium oxide at 800 ° C. or higher to obtain antibacterial fired particles. Manufacturing method (Claim 3). (4) a baking step of baking the antibacterial particles comprising at least one of magnesium hydroxide and magnesium oxide at 800 ° C. or higher to obtain baking particles having antibacterial properties; A method for producing an antibacterial composite powder pigment for cosmetics, comprising a compounding step of fixing the powder particles for cosmetics to obtain antibacterial composite powder particles (claim 4).

【００３１】(5)水酸化マグネシウム及び酸化マグネシ
ウムのうちの１種以上が付着する化粧料用粉体粒子を８
５０℃以上で焼成して、酸化マグネシウムから成る抗菌
性焼成粒子と化粧料用粉体粒子が固着して成る抗菌性複
合粉体粒子を得る焼成複合化工程を含む化粧料用抗菌性
複合粉体顔料の製造方法（請求項５）。 (6)請求項１の化粧料用抗菌性粉体顔料及び請求項２の
化粧料用抗菌性複合粉体顔料のうちの１種以上を含有す
る抗菌性化粧料組成物（請求項６）。なお、本発明にお
いて数値範囲の記載は、両端値のみならず、その中に含
まれる全ての任意の中間値を含むものとする。(5) Cosmetic powder particles to which one or more of magnesium hydroxide and magnesium oxide adhere
An antibacterial composite powder for cosmetics including a firing and complexing step of firing at 50 ° C. or more to obtain antibacterial composite powder particles comprising magnesium oxide and powder particles for cosmetics adhered to each other. A method for producing a pigment (Claim 5). (6) An antibacterial cosmetic composition containing one or more of the antibacterial powder pigment for cosmetics of claim 1 and the antibacterial composite powder pigment for cosmetics of claim 2 (claim 6). In the present invention, the description of the numerical range includes not only both end values, but also all arbitrary intermediate values included therein.

【００３２】[0032]

【発明の実施の形態】以下、本発明を更に説明する。 ［化粧料用抗菌性顔料］本発明の化粧料用抗菌性粉体顔
料は、酸化マグネシウムから成る抗菌性焼成粒子を含有
する。また、本発明の化粧料用抗菌性粉体顔料は、その
一部ないし全部を前記抗菌性焼成粒子にすることができ
る。即ち、本発明の化粧料用抗菌性粉体顔料は、前記抗
菌性焼成粒子以外の化粧料用顔料を含有することができ
る。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be further described. [Antibacterial pigment for cosmetics] The antibacterial powder pigment for cosmetics of the present invention contains antibacterial baked particles composed of magnesium oxide. In addition, the antibacterial powder pigment for cosmetics of the present invention can be partially or entirely made of the antibacterial baked particles. That is, the antibacterial powder pigment for cosmetics of the present invention can contain a pigment for cosmetics other than the above-mentioned antibacterial fired particles.

【００３３】本発明の化粧料用抗菌性複合粉体顔料は、
前記抗菌性焼成粒子と化粧料用粉体粒子が固着して成る
抗菌性複合粉体粒子を含有する。また、本発明の化粧料
用抗菌性複合粉体顔料は、その一部ないし全部を抗菌性
複合粉体粒子にすることができる。即ち、本発明の化粧
料用抗菌性複合粉体顔料は、前記抗菌性複合粉体粒子以
外の化粧料用顔料を含有することができる。The antibacterial composite powder pigment for cosmetics of the present invention comprises:
It contains antibacterial composite powder particles formed by fixing the antibacterial baked particles and the cosmetic powder particles. Further, the antibacterial composite powder pigment for cosmetics of the present invention can be partially or entirely made of antibacterial composite powder particles. That is, the antibacterial composite powder pigment for cosmetics of the present invention can contain a pigment for cosmetic other than the antibacterial composite powder particles.

【００３４】前記抗菌性複合粉体粒子にする第１の意味
は、複合化する事により、特に、化粧料用粉体粒子が有
機粉体粒子の場合、パラオキシ安息香酸エステル（パラ
ベン類）の吸着を抑制し、パラベンの防腐効果を維持、
発揮させる事ができると共に、防腐殺菌効果を実際に有
するパラベン類と本発明における抗菌性焼成粒子の併用
を可能にすることができる。即ち、化粧料に有機粉体粒
子とパラベン類を含有させる場合に、本発明における抗
菌性焼成粒子を化粧料用有機粉体粒子と固着させること
なくそのまま化粧料に含有させても、前記有機粉体粒子
はパラベン類を吸着してしまう。これに対して、抗菌性
焼成粒子と化粧料用有機粉体粒子が固着して成る抗菌性
複合粉体粒子とすることにより、化粧料用有機粉体粒子
がパラベン類を吸着することを防止することができる。The first meaning of the above-mentioned antibacterial composite powder particles is that, by forming a composite, especially when the cosmetic powder particles are organic powder particles, adsorption of paraoxybenzoate (parabens) is performed. And maintain the antiseptic effect of parabens,
In addition to being able to exert the effect, it is possible to use the antibacterial fired particles of the present invention together with parabens that actually have a preservative sterilization effect. That is, when organic powder particles and parabens are contained in the cosmetic, the antibacterial baked particles of the present invention may be contained in the cosmetic as they are without being fixed to the organic powder particles for the cosmetic. Body particles adsorb parabens. On the other hand, the antibacterial composite powder particles formed by fixing the antibacterial fired particles and the organic powder particles for cosmetics prevent the organic powder particles for cosmetics from adsorbing parabens. be able to.

【００３５】前記抗菌性複合粉体粒子にする第２の意味
は、複合化する事により、のびが軽く、肌に負担をかけ
ずに伸展性に優れ、肌へのつきの均一性に優れる利点が
発現するということであり、化粧料に配合する事は大変
有利に作用する特徴をもつ。The second meaning of the above-mentioned antibacterial composite powder particles is that, by forming a composite, there is an advantage that the spreadability is light, the extensibility is excellent without imposing a burden on the skin, and the uniformity of attachment to the skin is excellent. It has the feature that it is very advantageous to mix it with cosmetics.

【００３６】次に作用機序について考察してみる。一般
の抗菌剤の作用機構は、（１）生合成経路（蛋白質合
成、細胞膜合成、ＤＮＡ合成、ＲＮＡ合成など）の阻害
作用、（２）エネルギー系（呼吸、電子伝達系など）の
阻害作用、（３）変性作用（酵素蛋白、細胞膜、ＤＮ
Ａ、ＲＮＡなど）の生物学的性質が損なわれること、
（４）細胞膜の破壊作用等が考えられている。Next, the mechanism of action will be considered. The mechanism of action of general antibacterial agents includes (1) an inhibitory action on biosynthetic pathways (protein synthesis, cell membrane synthesis, DNA synthesis, RNA synthesis, etc.), (2) an inhibitory action on energy systems (respiration, electron transfer system, etc.), (3) Denaturing action (enzyme protein, cell membrane, DN
A, RNA, etc.)
(4) Destruction of cell membrane and the like are considered.

【００３７】通常の菌（カビを除く）は、ｐＨが１０以
上では生育できないといわれている。しかし、水酸化カ
ルシウムのｐＨが１１〜１２の範囲でも０．１％濃度で
は抗菌効果はない。０．２％濃度においても、緑膿菌に
対しては抗菌効果が見られない。このことから見るとカ
ルシウムは微生物の栄養源になることを考えても、水素
イオン濃度のみでは説明できない面がある。It is said that ordinary bacteria (excluding mold) cannot grow at a pH of 10 or more. However, even when the pH of calcium hydroxide is in the range of 11 to 12, there is no antibacterial effect at a concentration of 0.1%. Even at a concentration of 0.2%, no antibacterial effect is observed against Pseudomonas aeruginosa. In view of this, there are aspects that cannot be explained only by the hydrogen ion concentration, even if calcium is considered to be a nutrient source for microorganisms.

【００３８】一方、酸化マグネシウムのｐＨは９．３〜
１０．４程度で、通常、菌の生育は可能なｐＨの範囲で
ある。しかし、酸化マグネシウムには防腐殺菌作用があ
る。酸化マグネシウムの溶解度は、冷水では６．２×１
０-4ｇ／１００ｇ、３０℃で８×１０-3ｇ／１００ｇ程
度であるが、ｐＨが高い領域にある事と水素で解離した
酸化マグネシウムの塩基遊離（・ＯＨ）による細胞質で
の酸化作用と微生物中のＳＨ結合がＭｇイオンによりＳ
−Ｍｇ結合になり、吸収器系、電子伝達系の代謝機能障
害によるそれらの相乗作用で防腐殺菌作用が出ると思わ
れる。On the other hand, the pH of magnesium oxide is from 9.3 to
At about 10.4, the growth of bacteria is usually in the range of possible pH. However, magnesium oxide has an antiseptic and bactericidal action. The solubility of magnesium oxide is 6.2 × 1 in cold water
0 -4 g / 100 g, about 8 × 10 -3 g / 100 g at 30 ° C., but in the high pH region and oxidizing action in the cytoplasm due to base release (· OH) of magnesium oxide dissociated with hydrogen And SH binding in microorganisms
-It becomes Mg bond, and it seems that the antiseptic and bactericidal action is exerted by their synergistic action due to metabolic dysfunction of the absorber system and the electron transfer system.

【００３９】化粧料用粉体粒子に固着させない場合の抗
菌性焼成粒子の平均粒子径は０．０１〜１５μｍにする
ことができ、好ましい範囲は０．０１〜１０μｍであ
り、より好ましい範囲は０．０１〜５．０μｍであり、
更に好ましい範囲は０．０１〜２．５μｍである。The average particle size of the antibacterial baked particles when not fixed to the powder particles for cosmetics can be 0.01 to 15 μm, a preferred range is 0.01 to 10 μm, and a more preferred range is 0 to 10 μm. 0.01 to 5.0 μm,
A more preferred range is from 0.01 to 2.5 μm.

【００４０】抗菌性焼成粒子と化粧料用粉体粒子が固着
して成る抗菌性複合粉体粒子の好ましい平均粒子径は、
０．０３〜５０μｍであり、より好ましい範囲は０．１
〜２０μｍ、更に好ましくは０．２〜１５μｍの範囲で
ある。また、抗菌性複合粉体粒子において、抗菌性焼成
粒子の粒子径は、好ましくは化粧料用粉体粒子の粒子径
よりも小さくし、好ましい平均粒子径の範囲は０．０１
〜１５μｍであり、より好ましい範囲は０．０１〜１０
μｍであり、更に好ましい範囲は０．０１〜５．０μｍ
であり、最も好ましい範囲は０．０１〜２．５μｍであ
る。また、抗菌性複合粉体粒子における化粧料用粉体粒
子の粒子径は、好ましくは０．０２〜５０μｍであり、
より好ましい範囲は０．０２〜２０μｍであり、更に好
ましい範囲は０．０２〜５．０μｍである。特に、平均
粒子径が５０μｍ以下の場合は使用感上、肌に異和感を
感じないので好ましい。抗菌性複合粉体粒子における抗
菌性焼成粒子の粒径Ａと化粧料用粉体粒子の粒径Ｂの関
係については、Ａ／Ｂ≦０．５にすることができ、好ま
しくはＡ／Ｂ≦０．４にし、より好ましくは０．００１
≦Ａ／Ｂ≦０．３、更に好ましくは０．００５≦Ａ／Ｂ
≦０．２、最も好ましくは０．０１≦Ａ／Ｂ≦０．１に
する。The preferable average particle size of the antibacterial composite powder particles formed by fixing the antibacterial baked particles and the cosmetic powder particles is as follows:
0.03 to 50 μm, and a more preferred range is 0.1 to 50 μm.
To 20 μm, more preferably 0.2 to 15 μm. In the antibacterial composite powder particles, the particle size of the antibacterial baked particles is preferably smaller than the particle size of the cosmetic powder particles, and the preferable average particle size range is 0.01.
To 15 μm, more preferably 0.01 to 10 μm.
μm, and a more preferred range is 0.01 to 5.0 μm.
And the most preferable range is 0.01 to 2.5 μm. In addition, the particle diameter of the cosmetic powder particles in the antibacterial composite powder particles is preferably 0.02 to 50 μm,
A more preferred range is 0.02 to 20 μm, and a still more preferred range is 0.02 to 5.0 μm. In particular, when the average particle diameter is 50 μm or less, it is preferable because the skin does not feel uncomfortable in use. Regarding the relationship between the particle size A of the antibacterial fired particles and the particle size B of the cosmetic powder particles in the antibacterial composite powder particles, A / B ≦ 0.5, preferably A / B ≦. 0.4, more preferably 0.001
≦ A / B ≦ 0.3, more preferably 0.005 ≦ A / B
≦ 0.2, most preferably 0.01 ≦ A / B ≦ 0.1.

【００４１】抗菌性複合粉体粒子における化粧料用粉体
粒子としては、無機粉体、有機粉体、無機顔料及び有機
−無機複合粉体のそれぞれの粉体粒子がある。As the powder particles for cosmetics in the antibacterial composite powder particles, there are respective powder particles of inorganic powder, organic powder, inorganic pigment and organic-inorganic composite powder.

【００４２】無機粉体としては、カオリナイト、デッカ
イト、ナクライト、ハロイドサイト、アンチゴライト、
クリソタイル等のカオリン族、パイロフィライト、モン
モリロナイト、ノントロナイト、サポナイト、ヘクトラ
イト、ベントナイト等のスメクタイト族、セリサイト白
雲母、黒雲母、リチア雲母、合成雲母、合成セリサイト
等のイライト族、ハイデライト、ケイ酸マグネシウム、
ケイ酸カルシウム、ケイ酸アルミニウムマグネシウム等
のケイ酸塩、珪線石、藍晶石等のカルシウム化合物等の
シリマナイト族、リン酸３カルシウム、ハイドロキシア
パタイト、等のカルシウム化合物、タルク、蛇紋石等の
マグネシウムシリケート族、シリカ、アルミナ、等の単
一成分粉体、酸化チタン内包シリカ、酸化亜鉛内包シリ
カ、酸化鉄内包シリカ、酸化チタン内包ＰＭＭＡ（ポリ
メタクリル酸メチル）、酸化亜鉛内包ＰＭＭＡ、酸化セ
リウム内包ＰＭＭＡ、等の硬質カプセル、チタンマイ
カ、酸化チタン−硫酸バリウム、酸化チタン−タルク、
オキシ塩化ビスマス、オキシ塩化ビスマス−マイカ等の
パール顔料がある。As the inorganic powder, kaolinite, deckite, nacrite, haloid site, antigorite,
Helicites such as kaolins such as chrysotile, pyrophilites, montmorillonite, nontronites, saponites, hectorites, bentonites, etc .; serites muscovite, biotite; lithite mica; synthetic mica; Light, magnesium silicate,
Silicates such as calcium silicate and aluminum magnesium silicate; sillimanite family such as calcium compounds such as sillimanite and kyanite; calcium compounds such as tricalcium phosphate and hydroxyapatite; magnesium silicates such as talc and serpentine Single component powder such as group, silica, alumina, etc., titanium oxide-containing silica, zinc oxide-containing silica, iron oxide-containing silica, titanium oxide-containing PMMA (polymethyl methacrylate), zinc oxide-containing PMMA, cerium oxide-containing PMMA, Such as hard capsules, titanium mica, titanium oxide-barium sulfate, titanium oxide-talc,
There are pearl pigments such as bismuth oxychloride and bismuth oxychloride-mica.

【００４３】有機粉体としては、ナイロンパウダー、ポ
リエチレンパウダー、ポリプロピレンパウダー、酢酸ビ
ニルパウダー、ポリメタアクリル酸エステルパウダー、
ポリアクリルニトリルパウダー、ポリスチレンパウダ
ー、セルロースパウダー等がある。無機顔料としては、
酸化チタン、酸化亜鉛、酸化ジルコニウム、酸化セリウ
ム等の白色顔料と酸化鉄、水和酸化鉄、群青、紺青等の
有色顔料がある。有機−無機複合粉末は、上記の有機粉
体の粒子に無機粒子、好ましくはシリカ、アルミナ、酸
化チタン、酸化セリウム、酸化鉄のうちの１種以上の粒
子を固着して複合させた素材である。Examples of the organic powder include nylon powder, polyethylene powder, polypropylene powder, vinyl acetate powder, polymethacrylate ester powder,
Examples include polyacrylonitrile powder, polystyrene powder, and cellulose powder. As inorganic pigments,
There are white pigments such as titanium oxide, zinc oxide, zirconium oxide and cerium oxide, and colored pigments such as iron oxide, hydrated iron oxide, ultramarine and navy blue. The organic-inorganic composite powder is a material in which inorganic particles, preferably one or more particles of silica, alumina, titanium oxide, cerium oxide, and iron oxide, are fixed to the above-mentioned organic powder particles to form a composite. .

【００４４】［化粧料用抗菌性顔料の製造方法］本発明
の化粧料用抗菌性粉体顔料の製造方法及び本発明の化粧
料用抗菌性複合粉体顔料の製造方法における焼成工程
は、水酸化マグネシウム及び未焼成の酸化マグネシウム
のうちの１種以上から成る抗菌性粒子を８５０℃以上で
焼成して抗菌性焼成粒子（主として酸化マグネシウムか
ら成る抗菌性焼成粒子）を得る工程である。[Production method of antibacterial pigment for cosmetics] In the method of producing the antibacterial powder pigment for cosmetics of the present invention and the method of producing the antibacterial composite powder pigment for cosmetics of the present invention, the baking step is carried out by using water. In this step, antibacterial particles comprising at least one of magnesium oxide and unfired magnesium oxide are fired at 850 ° C. or higher to obtain antibacterial fired particles (antibacterial fired particles mainly composed of magnesium oxide).

【００４５】本発明の化粧料用抗菌性複合粉体顔料の製
造方法における複合化工程は、前記焼成工程で得た抗菌
性焼成粒子と化粧料用粉体粒子を固着させて抗菌性複合
粉体粒子を得る工程である。抗菌性焼成粒子と化粧料用
粉体粒子は、好ましくは、ボールミル等の機械的エネル
ギーを用いたメカノケミカル反応ないしメカノフュージ
ョン（ｍｅｃｈａｎｏｆｕｓｉｏｎ）により、あるいは
静電気により固着させることができる。The compounding step in the method for producing the antibacterial composite powder pigment for cosmetics of the present invention comprises the step of fixing the antibacterial baked particles obtained in the calcination step and the powder particles for cosmetics to form an antibacterial composite powder. This is the step of obtaining particles. The antibacterial baked particles and the powder particles for cosmetics can be preferably fixed by a mechanochemical reaction or mechanofusion using mechanical energy such as a ball mill, or by static electricity.

【００４６】メカノフュージョンとは、固体の表面が強
力な機械的エネルギーにより融解し、その融解した表面
に他の固体物質が固着し、固定化されることをいう。例
えば、ナイロンパウダーと酸化マグネシウム粒子とを混
合して強力なエネルギーを与えた場合、エネルギー的に
はプラズマ発生時のエネルギーが発生しナイロンパウダ
ーの表面が瞬間的に融解した状態になり、その状態にな
った表面に酸化マグネシウム粒子が固着すると考えられ
ている。Mechanofusion means that the surface of a solid is melted by strong mechanical energy, and another solid substance is fixed to the melted surface and fixed. For example, when nylon powder and magnesium oxide particles are mixed to give strong energy, energy is generated at the time of plasma generation and the surface of the nylon powder is instantaneously melted, and in this state, It is believed that the magnesium oxide particles adhere to the lost surface.

【００４７】本発明の化粧料用抗菌性複合粉体顔料の製
造方法における焼成複合化工程は、水酸化マグネシウム
及び未焼成の酸化マグネシウムのうちの１種以上が付着
する化粧料用粉体粒子を８５０℃以上で焼成して、酸化
マグネシウムから成る抗菌性焼成粒子と化粧料用粉体粒
子が固着して成る抗菌性複合粉体粒子を得る工程であ
る。好ましくは、水酸化マグネシウムを析出させること
のできる液体（溶液）と化粧料用粉体粒子を接触させて
前記粉体粒子に水酸化マグネシウムを析出させ８５０℃
以上で焼成する。このようにすると、前記水酸化マグネ
シウムは、酸化マグネシウムに変化しさらに酸化マグネ
シウム焼成粒子になると共に、この酸化マグネシウム焼
成粒子が化粧料用粉体粒子に固着した抗菌性複合粉体粒
子を得ることができる。The baking composite step in the method for producing the antibacterial composite powder pigment for cosmetics of the present invention comprises the step of removing powder particles for cosmetics to which at least one of magnesium hydroxide and unfired magnesium oxide adheres. This is a step of firing at 850 ° C. or higher to obtain antibacterial composite powder particles in which antibacterial fired particles made of magnesium oxide and powder particles for cosmetics are fixed. Preferably, a liquid (solution) capable of precipitating magnesium hydroxide and powder particles for cosmetics are brought into contact with each other to deposit magnesium hydroxide on the powder particles.
The above is fired. In this case, the magnesium hydroxide is changed to magnesium oxide, and further becomes magnesium oxide fired particles, and the antibacterial composite powder particles in which the magnesium oxide fired particles adhere to the cosmetic powder particles can be obtained. it can.

【００４８】例えば、硫酸マグネシウム６水和物の溶液
に化粧料用粉体を分散させ加温しながら水酸化ナトリウ
ム水溶液を滴下し、水酸化マグネシウム粒子と化粧料用
粉体粒子とを固着させ、さらに、８５０℃〜１２００℃
の温度で焼成する事により、酸化マグネシウムから成る
抗菌性焼成粒子と化粧料用粉体粒子が固着した抗菌性複
合粉体粒子を得ることができる。この方法を用いると微
粒子の抗菌性焼成粒子を化粧料用粉体粒子の表面に均一
に固着させる事が出来る。For example, a cosmetic powder is dispersed in a solution of magnesium sulfate hexahydrate, and an aqueous solution of sodium hydroxide is added dropwise while heating to fix the magnesium hydroxide particles and the cosmetic powder particles. Furthermore, 850 ° C to 1200 ° C
By baking at the above temperature, antibacterial composite powder particles in which antibacterial fired particles composed of magnesium oxide and powder particles for cosmetics are fixed can be obtained. By using this method, the antibacterial baked fine particles can be uniformly fixed to the surfaces of the powder particles for cosmetics.

【００４９】他の方法としては、通常の中和法で常温に
て塩化マグネシウム６水和物の水溶液に化粧料用粉体粒
子を分散させたのち、水酸化ナトリウム水溶液を滴下す
ることによって、化粧料用粉体粒子表面にかなり含水率
の高い水酸化マグネシウム粒子を固着させ、８５０〜１
２００℃の温度で焼成する方法があり、この方法により
酸化マグネシウム焼成粒子と化粧料用粉体粒子が固着し
た抗菌性複合粉体粒子を得る事が出来る。Another method is to disperse powder particles for cosmetics in an aqueous solution of magnesium chloride hexahydrate at room temperature by a normal neutralization method, and then add an aqueous solution of sodium hydroxide dropwise. Magnesium hydroxide particles having a considerably high water content on the surface of
There is a method of firing at a temperature of 200 ° C., and by this method, antibacterial composite powder particles in which fired magnesium oxide particles and powder particles for cosmetics are fixed can be obtained.

【００５０】酸化マグネシウムは、（ａ）金属マグネシ
ウムを空気中で熱して得ることができ、また、（ｂ）炭
酸マグネシウム、ヒドロキシ炭酸マグネシウム、水酸化
マグネシウムのいずれか１種以上を熱分解して得ること
ができる。従って、金属マグネシウム粒子を空気中で熱
して酸化マグネシウム粒子得て、引き続き酸化マグネシ
ウム粒子から酸化マグネシウム焼成粒子を得る工程を１
回の熱処理で行うことができる。また、同様に炭酸マグ
ネシウム、ヒドロキシ炭酸マグネシウム、水酸化マグネ
シウムのいずれか１種以上の粒子を熱分解して酸化マグ
ネシウム粒子を得て、引き続き酸化マグネシウム粒子か
ら酸化マグネシウム焼成粒子を得る工程を１回の熱処理
で行うことができる。なお、酸化マグネシウムは、通
常、市販されている。Magnesium oxide can be obtained by heating (a) metallic magnesium in the air, and (b) by thermally decomposing at least one of magnesium carbonate, magnesium hydroxycarbonate and magnesium hydroxide. be able to. Therefore, the steps of heating magnesium metal particles in the air to obtain magnesium oxide particles, and subsequently obtaining magnesium oxide fired particles from the magnesium oxide particles are as follows.
The heat treatment can be performed twice. Similarly, a step of thermally decomposing at least one kind of particles of magnesium carbonate, magnesium hydroxycarbonate, and magnesium hydroxide to obtain magnesium oxide particles, and subsequently obtaining magnesium oxide fired particles from the magnesium oxide particles is performed once. It can be performed by heat treatment. Note that magnesium oxide is usually commercially available.

【００５１】水酸化マグネシウム及び未焼成の酸化マグ
ネシウムのうちの１種以上から成る抗菌性粒子を焼成し
て酸化マグネシウムから成る抗菌性焼成粒子を得る際に
適用される焼成温度は、８５０℃以上であり、好ましく
は８５０〜１１００℃の範囲にし、より好ましくは１０
００〜１１００℃の範囲である。焼成温度が８５０℃未
満、特に８００℃以下で焼成した場合の酸化マグネシウ
ムは大気中の水分の吸湿性がきわめて大きく、酸化マグ
ネシウムが水酸化マグネシウムに構造変化したり、ある
いは大気中の水分及び炭酸ガスと反応し、ヒドロキシ炭
酸マグネシウムに構造が変化し、本来もつ酸化マグネシ
ウムの防腐殺菌効果が低下したり、場合によっては消失
してしまう。The firing temperature applied when firing antibacterial particles composed of one or more of magnesium hydroxide and unfired magnesium oxide to obtain antibacterial fired particles composed of magnesium oxide is 850 ° C. or higher. And preferably in the range of 850 to 1100 ° C., more preferably 10 to 100 ° C.
It is in the range of 00 to 1100 ° C. Magnesium oxide when calcined at a temperature of less than 850 ° C., particularly 800 ° C. or less, has a very large hygroscopic property of moisture in the atmosphere, and the structure of magnesium oxide changes to magnesium hydroxide, or moisture and carbon dioxide in the atmosphere are reduced. And the structure is changed to magnesium hydroxycarbonate, and the preservative and bactericidal effect of the inherent magnesium oxide is reduced or disappears in some cases.

【００５２】安定な酸化マグネシウムの構造を有し、長
期間の防腐殺菌効果を維持できる抗菌性焼成粒子を得る
ための焼成温度は、１０００〜１１００℃である。この
温度範囲が好適である理由としては、不明な点が多い
が、酸化マグネシウムの多孔質性が消滅し、多孔質部分
の活性部分が消失したり、粒子表面の一部或いは粒子が
融解したりして、結晶構造がより緻密化されているのも
一つの要因と推測している。The sintering temperature for obtaining antibacterial sintering particles having a stable structure of magnesium oxide and capable of maintaining a long-term antiseptic and sterilizing effect is 1000 to 1100 ° C. There are many unknown reasons why this temperature range is suitable. However, the porosity of magnesium oxide disappears, the active portion of the porous portion disappears, or a part of the particle surface or the particles are melted. Therefore, it is speculated that one of the factors is that the crystal structure is further densified.

【００５３】酸化マグネシウム（ＭｇＯ）の焼成温度と
吸湿度（重量の増加分を重量％で示す）の関係（焼成温
度ごとの吸湿度の経時変化）について次の表１に示す。
なお、表１には、ＭｇＯ（未焼成の試薬）とＭｇ（Ｏ
Ｈ）2（未焼成の試薬）についての吸湿度の経時変化及
び、吸湿度測定時の温度（℃）及び湿度（％）について
も示す。The relationship between the sintering temperature of magnesium oxide (MgO) and the hygroscopicity (the increase in weight is indicated by weight%) (time-dependent change in the hygroscopicity at each sintering temperature) is shown in Table 1 below.
Table 1 shows that MgO (unfired reagent) and Mg (O
H) The time-dependent change in the moisture absorption of the (unfired reagent) 2 and the temperature (° C.) and humidity (%) at the time of the moisture absorption measurement are also shown.

【００５４】[0054]

【表１】 [Table 1]

【００５５】酸化マグネシウムの焼成時の雰囲気は、酸
化雰囲気、不活性雰囲気、還元雰囲気のいずれでも良
い。焼成時間は１〜２４時間にすることができる。望ま
しくは２〜１２時間、更には４〜８時間である。焼成時
間は、ろ体の大きさや雰囲気、ろ体の温度分布幅にもよ
るが、より短時間で焼成するのが経済的でもあるし、ま
た、必要以上の時間を費やしても経済的にも望ましくな
い。The atmosphere for firing magnesium oxide may be any of an oxidizing atmosphere, an inert atmosphere, and a reducing atmosphere. The firing time can be from 1 to 24 hours. Desirably, it is 2 to 12 hours, more preferably 4 to 8 hours. The firing time depends on the size and atmosphere of the filter, the temperature distribution width of the filter, but it is economical to fire in a shorter time, and it is also economical to spend more time than necessary. Not desirable.

【００５６】［抗菌性化粧料組成物］本発明の化粧料用
抗菌性粉体顔料及び本発明の化粧料用抗菌性複合粉体顔
料のうちの１種以上は、一般的な無機粉体や無機顔料、
有機粉末及び、有機−無機複合粉末等の化粧料用粉体を
含有または、配合できるすべての化粧料組成物に適用す
ることができる。本発明の抗菌性化粧料組成物は、前記
化粧料用粉体を含有させることができ、前記化粧料用粉
体の粒子（抗菌性焼成粒子と固着していない化粧料用粉
体粒子）の平均粒子径は好ましくは０．０１〜５０μｍ
にすることができ、より好ましい範囲は０．０１〜２０
μｍ、更に好ましい範囲は０．０１〜５μｍである。特
に、平均粒子径が５０μｍ以下の場合は使用感上、肌に
異和感を感じないので好ましい。[Antibacterial Cosmetic Composition] At least one of the antibacterial powder pigment for cosmetics of the present invention and the antibacterial composite powder pigment for cosmetics of the present invention comprises general inorganic powder or Inorganic pigments,
The present invention can be applied to all cosmetic compositions containing or blending cosmetic powders such as organic powders and organic-inorganic composite powders. The antibacterial cosmetic composition of the present invention may contain the cosmetic powder, and the particles of the cosmetic powder (cosmetic powder particles that are not fixed to the antibacterial baked particles). Average particle diameter is preferably 0.01 to 50 μm
And a more preferred range is 0.01 to 20.
μm, and a more preferred range is 0.01 to 5 μm. In particular, when the average particle diameter is 50 μm or less, it is preferable because the skin does not feel uncomfortable in use.

【００５７】一般的な無機顔料や無機粉体、および有機
粉末を用いることのできる化粧料としては、パウダーフ
ァンデーション、コンパクトパウダー、ツーウェイケー
キ、フェイスパウダー、制汗スプレーの白粉類とアイシ
ャドー、パウダーブラッシャー、マスカラ、リップステ
ィック、アイブロウペンシル、アイライナー等のポイン
トメーク化粧料、乳化型ファンデーション、メークアッ
プベース等の乳化製品類、粉末パック、クレンジングパ
ック、サンスクリーンクリーム、ローション化粧水等の
一部基礎化粧品類とベビーパウダー、ボディパウダー、
フレグランスパウダー等の全身用製品類などがある。Examples of cosmetics which can use general inorganic pigments, inorganic powders, and organic powders include powder foundation, compact powder, two-way cake, face powder, antiperspirant spray white powder and eye shadow, powder brusher. , Mascara, lipstick, eyebrow pencil, eyeliner, etc., point makeup cosmetics, emulsified products such as emulsified foundation, makeup base, powdered packs, cleansing packs, sunscreen creams, lotion lotions, etc. Kind and baby powder, body powder,
There are products for whole body such as fragrance powder.

【００５８】本発明の抗菌性焼成粒子及び抗菌性複合粉
体粒子（抗菌性焼成粒子と化粧料用粉体粒子が固着して
成る抗菌性複合粉体粒子）のうちの１種以上は、０．１
重量％（抗菌性複合粉体粒子を含有する場合は、化粧料
用粉体粒子を除く抗菌性焼成粒子のみの配合率に換算、
以下同様）程度の配合で十分な抗菌効果をもつが、望ま
しい配合率は０．１５〜０．２重量％程度である。ま
た、白粉では４０重量％以上の配合はできるがこの場
合、抗菌効果を発揮する側面からは、非経済的である。
従って、化粧料組成物中における抗菌性焼成粒子及び抗
菌性複合粉体粒子（抗菌性焼成粒子と化粧料用粉体粒子
が固着して成る抗菌性複合粉体粒子）のうちの１種以上
の配合量は０．０５〜４０重量％にすることができ、好
ましくは、０．１〜３０重量％、更に好ましくは０．１
〜２０重量％である。At least one of the fired antibacterial particles and the antibacterial composite powder particles of the present invention (antibacterial composite powder particles obtained by adhering antibacterial fired particles and cosmetic powder particles) is 0%. .1
% By weight (in the case of containing antibacterial composite powder particles, conversion to the blending ratio of only antibacterial baked particles excluding cosmetic powder particles,
The same is applied in the following), but a sufficient antibacterial effect is obtained, but a desirable compounding ratio is about 0.15 to 0.2% by weight. In addition, white powder can be blended in an amount of 40% by weight or more, but in this case, it is uneconomical from the aspect of exhibiting an antibacterial effect.
Therefore, at least one of the baked antibacterial particles and the antibacterial composite powder particles (the antibacterial composite powder particles formed by fixing the baked antibacterial particles and the powder particles for cosmetics) in the cosmetic composition. The compounding amount can be 0.05 to 40% by weight, preferably 0.1 to 30% by weight, more preferably 0.1 to 30% by weight.
-20% by weight.

【００５９】本発明の化粧料組成物に適用される無機粉
体は、例えば、セリサイト、白雲母、黒雲母、リチア雲
母、合成雲母、合成セリサイト等のイライト族、カオリ
オナイト、ナクライト、デッカイト、ハロサイト等のカ
オリン族、珪線石、藍晶石等のシリマナイト族、タル
ク、蛇蚊石等のマグネシウムシリケートとシリカとそれ
らの着色粉体、炭酸マグネシウム、炭酸カルシウム等の
炭酸塩化化合物、ケイ酸マグネシウム、ケイ酸カルシウ
ム、リン酸カルシウム、ハイドロキシアパタイト等の複
合化合物、チタンマイカ、チタン−硫酸バリウム、チタ
ン−タルク、オキシ塩化ビスマス−マイカ等のパール類
料およぴ着色した着色パール顔料と硫酸バリウム、ゼオ
ライト、アルミナ等である。The inorganic powders applicable to the cosmetic composition of the present invention include, for example, illite family such as sericite, muscovite, biotite, lithia mica, synthetic mica, synthetic sericite, kaorionite, nacrite, deckite, and the like. Kaolin group such as halosite, sillimanite group such as sillimanite and kyanite, magnesium silicate and silica such as talc and serpentine stone and their colored powders, carbonated compounds such as magnesium carbonate and calcium carbonate, magnesium silicate , Calcium silicate, calcium phosphate, complex compounds such as hydroxyapatite, titanium mica, titanium-barium sulfate, titanium-talc, bismuth oxychloride-mica and other pearl materials and colored pearl pigments and barium sulfate, zeolite, Alumina and the like.

【００６０】無機顔料は、好ましくは、酸化鉄、水和酸
化鉄、群青、紺青、酸化チタン、酸化亜鉛、酸化ジルコ
ニウム、酸化セリウム等である。有機粉末は、ナイロン
パウダー、ポリエチレンパウダー、ポリプロピレンパウ
ダー、ポリメタクリル酸エステルパウダー、ポリスチレ
ンパウダー、ポリアクリルニトリルパウダー、セルロー
スパウダー等である。有機−無機複合粉末は、上記の有
機粉末に、好ましくはシリカ、アルミナ、酸化チタン、
酸化セリウム、酸化鉄のうちの１種以上の粒子を固着し
て複合させた素材である。The inorganic pigment is preferably iron oxide, hydrated iron oxide, ultramarine, navy blue, titanium oxide, zinc oxide, zirconium oxide, cerium oxide, or the like. Organic powders include nylon powder, polyethylene powder, polypropylene powder, polymethacrylate ester powder, polystyrene powder, polyacrylonitrile powder, cellulose powder and the like. Organic-inorganic composite powder, the above organic powder, preferably silica, alumina, titanium oxide,
It is a material in which one or more particles of cerium oxide and iron oxide are fixed and combined.

【００６１】[0061]

【実施例】以下本発明を実施例と比較例を挙げて詳細に
説明する。 ［実施例（１）］市販の酸化マグネシウム（和光純薬
製）を酸化雰囲気中にて１１００℃、６時間焼成して、
抗菌性化粧品顔料の焼成酸化マグネシウムを得た。The present invention will be described in detail below with reference to examples and comparative examples. [Example (1)] A commercially available magnesium oxide (manufactured by Wako Pure Chemical Industries, Ltd.) was calcined in an oxidizing atmosphere at 1100 ° C for 6 hours.
A calcined magnesium oxide antibacterial cosmetic pigment was obtained.

【００６２】試験概要；任意濃度に検体を添加した液体
培地に大腸菌、緑膿菌、黄色ぶどう球菌、カンジダ、黒
コウジカビの菌液をそれぞれの添加後、振とう培養し、
菌の発育の有無を確認した。Outline of test: Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Candida and Aspergillus fungi were added to a liquid medium to which a sample was added at an arbitrary concentration, and the mixture was shake-cultured.
The presence or absence of bacterial growth was confirmed.

【００６３】試験方法 （１）試験菌 細菌：Escherichia coli IFO 3972（大腸菌）Pseudomonas aeruginosa IFO 13275（緑膿菌）Staphylococcus aureus IFO 13276（黄色ブドウ球菌） 酵母：Candida albicans IFO 1594（カンジダ） カビ：Aspergillus niger IFO 4407（黒コウジカビ）Test method (1) Test bacteria Bacteria: Escherichia coli IFO 3972 (Escherichia coli) Pseudomonas aeruginosa IFO 13275 (Pseudomonas aeruginosa) Staphylococcus aureus IFO 13276 (Staphylococcus aureus) Yeast: Candida albicans IFO 1594 (Candida) Mold: Aspergillus niger IFO 4407 (Black Aspergillus)

【００６４】（２）試験用培養地 細菌：Ｍｕｅｌｌｅｒ Ｈｉｎｔｏｎ Ｂｒｏｔｈ（Ｄ
ｉｆｃｏ） 酵母およびカビ：ブドウ糖ペプトン培地（日水製薬
(株)） （３）接種用菌液の調製 細菌：継代培養した各試験菌を試験用培地に接種し、３
５℃で１８〜２０時間培養後、菌数が１０4／ｍｌにな
るように試験用培地で希釈し、接種用菌液とした。 酵母：継代培養した試験菌を各種試験用培地に接種し、
２５℃で４８時間培養後、菌数が約１０4／ｍｌになる
ように試験用培地で希釈し、接種用菌液とした。(2) Test culture area Bacteria: Mueller Hinton Broth (D
ifco) Yeast and mold: glucose peptone medium (Nissui Pharmaceutical)
(3) Preparation of Bacterial Solution for Inoculation Bacteria: Each subcultured test strain was inoculated into a test medium,
After culturing at 5 ° C. for 18 to 20 hours, the mixture was diluted with a test medium so that the number of bacteria became 10 4 / ml, and used as a bacterial solution for inoculation. Yeast: Subcultured test bacteria are inoculated into various test media,
After culturing at 25 ° C. for 48 hours, the cells were diluted with a test medium so that the number of bacteria was about 10 4 / ml, and used as a bacterial solution for inoculation.

【００６５】カビ：継代培養した試験菌をポテトデキス
トロース寒天培地［栄研科学(株)］に接種し、２５℃で
７日間培養後、形成された胞子（分生子）を、ポリソル
ベート８０を０．０５％添加した滅菌生理食塩水に浮遊
させ、胞子数が約１０4／ｍｌになるように調製し、接
種用菌液とした。Mold: The subcultured test bacteria were inoculated on a potato dextrose agar medium [Eiken Kagaku Co., Ltd.], cultured at 25 ° C. for 7 days, and the formed spores (conidia) were dissolved in polysorbate 80 with 0%. The suspension was suspended in sterile physiological saline to which 0.05% was added, and was prepared so that the number of spores became about 10 4 / ml.

【００６６】（４）感受性測定用培地の作成 検体を乾熱滅菌（１２１℃、３０分）後、これを試験用
培地にそれぞれ０．１、０．２、０．５、２．５、５．
０、１０、１５％添加し、感受性測定用培地とした。(4) Preparation of culture medium for sensitivity measurement After the specimen was dry-heat sterilized (121 ° C., 30 minutes), this was added to the culture medium for test at 0.1, 0.2, 0.5, 2.5 and 5, respectively. .
0, 10, and 15% were added to obtain a sensitivity measurement medium.

【００６７】（５）培養 感受性測定用培地に接種用菌液０．１ｍｌを添加し、細
菌は３５℃で１８〜２４時間、酵母及びカビは２５℃で
５日間振とう培養した （６）判定 培養後、肉眼観察又は顕微鏡及び、生菌数により試験菌
の発育の有無を判定した。(5) Culture 0.1 ml of the inoculum was added to the culture medium for sensitivity measurement, and the bacteria were shake-cultured at 35 ° C. for 18 to 24 hours, and the yeast and mold were shake-cultured at 25 ° C. for 5 days. After the cultivation, the presence or absence of the growth of the test bacteria was determined by visual observation or microscopy and the viable cell count.

【００６８】[0068]

【表２】 [Table 2]

【００６９】表２に示すように、実施例（１）の抗菌性
顔料（焼成酸化マグネシウム）は、細菌類である大腸
菌、黄色ブドウ球菌と酵母、黒コウジカビに対して、
０．１重量％で菌の成長抑制効果が現れ、接種した緑膿
菌に対しては、０．２重量％で菌の抑制効果が認められ
た。これに対して、化粧品配合に際し、表示成分である
メチルパラベンは０．１重量％では酵母、黒コウジカビ
に対しては菌の抑制効果が認められたが、細菌に対して
はその効果は認められず、０．２重量％で本発明の抗菌
性顔料と同様に菌の抑制効果が認められた。表示成分で
ない防腐殺菌剤のフェノキシエタノールは０．１〜０．
２重量％では、菌の抑制効果が認められない結果であっ
た。以上の結果から、本発明の抗菌性顔料がより低濃度
で成長抑制効果があることが判明した。なお、表２に
は、参考として、水酸化マグネシウム（未焼成）であっ
て経時変化していないものについての結果も併せて示
す。As shown in Table 2, the antibacterial pigment (calcined magnesium oxide) of Example (1) was effective against bacteria Escherichia coli, Staphylococcus aureus and yeast, and Aspergillus niger.
At 0.1% by weight, the effect of inhibiting the growth of the bacteria appeared, and with respect to the inoculated Pseudomonas aeruginosa, the effect of inhibiting the bacteria was observed at 0.2% by weight. On the other hand, in the case of formulating cosmetics, 0.1% by weight of methyl paraben, a labeling component, showed an inhibitory effect on yeasts and Aspergillus fungi, but no effect on bacteria. , 0.2% by weight, an effect of suppressing bacteria was recognized as in the case of the antibacterial pigment of the present invention. The preservative bactericide phenoxyethanol, which is not a labeling component, is 0.1 to 0.1.
At 2% by weight, no effect of inhibiting the bacteria was observed. From the above results, it was found that the antibacterial pigment of the present invention had a growth inhibiting effect at a lower concentration. Table 2 also shows, for reference, the results of magnesium hydroxide (unfired) that has not changed over time.

【００７０】酸化マグネシウムのＭＢＣ（最小殺菌濃
度）を測定した結果、細菌類の大腸菌と黄色ブドウ球菌
に対して０．５重量％で、緑膿菌に対しては０．４重量
％で殺菌効果が認められた。メチルパラベンのＭＢＣ測
定は水に対する溶解度が０．２％以上では不溶になるた
めに測定はできないが酸化マグネシウムのＭＩＣ（最小
発育阻止濃度）とＭＢＣの関係からメチルパラベンのＭ
ＩＣの関係から推測すると、パラベン類のＭＢＣは酸化
マグネシウムより高い濃度になると思われる。As a result of measuring the MBC (minimum bactericidal concentration) of magnesium oxide, the bactericidal effect was 0.5% by weight for bacteria Escherichia coli and Staphylococcus aureus and 0.4% by weight for Pseudomonas aeruginosa. Was observed. Methyl paraben MBC cannot be measured because its solubility in water is insoluble when the solubility in water is 0.2% or more, but it cannot be determined from the relationship between MIC (minimum inhibitory concentration) of magnesium oxide and MBC.
Inferred from the relationship of IC, it is considered that MBC of parabens has a higher concentration than magnesium oxide.

【００７１】［実施例（２）］ナイロンパウダーＳＰ５
００（東レ製）２００ｇに対し、１１００℃焼成酸化マ
グネシウム８０ｇを均一混合した後、ボールミル処理を
１２時間行った。その結果ナイロンパウダーＳＰ５００
の表面に均一に焼成酸化マグネシウムが固着していた。
そこでナイロンＳＰ５００と本発明のハイブリッドパウ
ダ（抗菌性複合粉体粒子）であるナイロン−ＭｇＯにつ
いてパラベンの吸着量を測定した。[Example (2)] Nylon powder SP5
After 200 g of 00 (manufactured by Toray Industries, Inc.) and 80 g of magnesium oxide fired at 1100 ° C. were uniformly mixed, a ball mill treatment was performed for 12 hours. As a result, nylon powder SP500
The calcined magnesium oxide was uniformly adhered to the surface of.
Then, the adsorption amount of paraben was measured for nylon SP500 and nylon-MgO which is the hybrid powder (antibacterial composite powder particles) of the present invention.

【００７２】セリサイト５０ｇとナイロンパウダー５０
ｇに対しメチルパラベン０．２ｇを精秤し、高速混合機
で５分間混合した後、試料１ｇを正確に精秤し、精製水
１０ｇ中に分散させ、超音波で５分間処理する。その処
理物を２時間、２０℃で静置後、上澄液を液体クロマト
グラフィー用フィルターを用いて濾過し、そのろ液から
液体クロマトグラフィーを用いて残留パラベン量を求め
た。50 g of sericite and 50 of nylon powder
After 0.2 g of methyl paraben is precisely weighed and mixed with a high-speed mixer for 5 minutes, 1 g of the sample is precisely weighed, dispersed in 10 g of purified water, and treated with ultrasonic waves for 5 minutes. After the treated product was allowed to stand at 20 ° C. for 2 hours, the supernatant was filtered using a liquid chromatography filter, and the amount of residual paraben was determined from the filtrate using liquid chromatography.

【００７３】その結果、ナイロンＳＰ５００に対するメ
チルパラベンの吸着量は８５．６％であるのに対し、本
発明の抗菌性複合粉体粒子（ハイブリッドパウダー）へ
の吸着量は０．９％であった。この結果により、パラベ
ンがナイロンパウダーへの吸着により資化されてしまい
防腐殺菌効果が殆どないのに対し、ハイブリッドパウダ
ーヘのパラベンの吸着量が極めて少なく、本発明の抗菌
性複合粉体粒子にパラベンを併用しても、パラベンの効
果が維持できることがわかった。As a result, the adsorption amount of methyl paraben to nylon SP500 was 85.6%, while the adsorption amount to the antibacterial composite powder particles (hybrid powder) of the present invention was 0.9%. According to this result, paraben was assimilated by adsorption to nylon powder and had almost no preservative / sterilizing effect. On the other hand, the amount of paraben adsorbed to the hybrid powder was extremely small, and paraben was added to the antibacterial composite powder particles of the present invention. It was found that the effect of paraben could be maintained even when the combination was used.

【００７４】［実施例（３）］硝酸カルシウム４水和物
２３．６６１ｇを精製水１５０ｍｌに溶解させｐＨ４に
合わせた液と、リン酸二水素アンモニウム７．９２３ｇ
を精製水１５０ｍｌに溶解させた液を、１０００ｍｌ冷
却管付二口フラスコの中で混合して得られた液を１００
℃に昇温した後、この液に、１７Ｎのアンモニア水６ｍ
ｌを６００ｍｌの精製水に希釈した液を５ｍｌ／分の速
度で滴下させた。滴下終了後１５時間そのままの温度で
成熟後、ろ別、水洗後４０℃、２０時間減圧乾燥し、１
０ｇのハイドロキシアパタイトを得た。Example (3) A solution prepared by dissolving 23.661 g of calcium nitrate tetrahydrate in 150 ml of purified water and adjusting the pH to 4, and 7.923 g of ammonium dihydrogen phosphate
Was dissolved in 150 ml of purified water and mixed in a 1000 ml two-necked flask equipped with a cooling tube.
After the temperature was raised to 6 ° C., the solution was added with 6 m of 17N ammonia water.
1 was diluted with 600 ml of purified water and dropped at a rate of 5 ml / min. After completion of the dropping, the mixture was matured at the same temperature for 15 hours, filtered, washed with water, dried at 40 ° C. for 20 hours under reduced pressure, and dried.
0 g of hydroxyapatite was obtained.

【００７５】このハイドロキシアパタイト１０ｇを精製
水２００ｍｌに分散させた溶液に別に水酸化ナトリウム
２．４８ｇを５０ｍｌの精製水に溶解させておいた溶液
を加え、均一に混合した後、攪拌しながら塩化マグネシ
ウム６水和物６．３ｇを溶解させた溶液を滴下し、ハイ
ドロキシアパタイトの表面に水酸化マグネシウムを固着
させ、濾過し、飽和水酸化マグネシウム溶液で、洗浄し
た後、エタノール洗浄をし、６０℃で乾燥する。その後
取り出し、１０００℃で１２時間焼成後、カルシウムア
パタイト−酸化マグネシウム複合粉体顔料を得た。この
複合粉体顔料における酸化マグネシウムは、抗菌性焼成
粒子である。Separately, a solution prepared by dissolving 2.48 g of sodium hydroxide in 50 ml of purified water was added to a solution of 10 g of hydroxyapatite dispersed in 200 ml of purified water. A solution in which 6.3 g of hexahydrate was dissolved was added dropwise, and magnesium hydroxide was fixed on the surface of hydroxyapatite, filtered, washed with a saturated magnesium hydroxide solution, washed with ethanol, and heated at 60 ° C. dry. Thereafter, it was taken out and calcined at 1000 ° C. for 12 hours to obtain a calcium apatite-magnesium oxide composite powder pigment. Magnesium oxide in the composite powder pigment is an antibacterial fired particle.

【００７６】［実施例（４）］精製水１０００ｍｌ中に
セリサイト（三信鉱工社製）８０ｇを攪拌分散させた
後、塩化アルミニウム６水和物５３ｇと塩化マグネシウ
ム４４．４ｇを加え溶解させる。別に水酸化ナトリウム
４１．１ｇを３００ｍｌの精製水に溶解させた溶液を前
記セリサイトが分散する液に滴下し、セリサイトの表面
に水酸化アルミニウムと水酸化マグネシウムを固着す
る。この固着した試料を濾過した後、飽和水酸化マグネ
シウム溶液で、洗浄し、６０℃で乾燥する。乾燥した試
料を９５０℃にて１０時間以上焼成し、セリサイト−酸
化アルミニウム−酸化マグネシウムの複合粉体顔料を得
た。この複合粉体顔料における酸化マグネシウムは、抗
菌性焼成粒子である。Example (4) 80 g of sericite (manufactured by Sanshin Mining Co., Ltd.) was stirred and dispersed in 1000 ml of purified water, and then 53 g of aluminum chloride hexahydrate and 44.4 g of magnesium chloride were added and dissolved. Separately, a solution prepared by dissolving 41.1 g of sodium hydroxide in 300 ml of purified water is dropped into the liquid in which the sericite is dispersed, and aluminum hydroxide and magnesium hydroxide are fixed on the surface of the sericite. After the fixed sample is filtered, it is washed with a saturated magnesium hydroxide solution and dried at 60 ° C. The dried sample was calcined at 950 ° C. for 10 hours or more to obtain a composite powder pigment of sericite-aluminum oxide-magnesium oxide. Magnesium oxide in the composite powder pigment is an antibacterial fired particle.

【００７７】［実施例（５）］精製水１０００ｍｌ中に
チタンマイカであるチミロンスーパーシーンＭＰ１００
１（メルク社製）８０ｇを攪拌分散させた後、塩化マグ
ネシウム１００．９ｇを溶解させる。この溶液に精製水
３００ｍｌ中に水酸化ナトリウム３９．７ｇを溶解させ
た溶液を滴下し、チミロンスーパーシーンＭＰ１００１
の表面に水酸化マグネシウムを固着化させる。次いで濾
過した後、飽和水酸化マグネシウム溶液で洗浄をくり返
す。濾過した後、８０℃で乾燥し、９００℃にて２０時
間焼成し、チタンマイカ−酸化マグネシウムの複合粉体
顔料を得た。この複合粉体顔料における酸化マグネシウ
ムは、抗菌性焼成粒子である。[Example (5)] Timilon supercene MP100 which is titanium mica in 1000 ml of purified water
After stirring and dispersing 80 g of 1 (Merck), 100.9 g of magnesium chloride is dissolved. A solution obtained by dissolving 39.7 g of sodium hydroxide in 300 ml of purified water was added dropwise to this solution, and the solution was added to Timilon Supercene MP1001.
To fix magnesium hydroxide on the surface of. Then, after filtration, the washing is repeated with a saturated magnesium hydroxide solution. After filtration, the resultant was dried at 80 ° C. and calcined at 900 ° C. for 20 hours to obtain a titanium mica-magnesium oxide composite powder pigment. Magnesium oxide in the composite powder pigment is an antibacterial fired particle.

【００７８】［実施例（６）］ハイブリタリゼーション
システム（奈良機械製作所）を用いて、ポリメタクリル
酸メチル（略称、ＰＭＭＡ）と酸化亜鉛と焼成酸化マグ
ネシウムの複合粉体顔料を製造した。ＰＭＭＡ（積水化
成工業社製）１０ｋｇの母粒子と子粒子の酸化亜鉛（堺
化学社製）を、８５０℃で焼成した酸化マグネシウム３
ｋｇに投入し、Ｏ．Ｍ．タイザー（前記ハイブリタリゼ
ーションシステムの中の一部分に当たるオーダードミク
スチャータイザーのことであり、粉体を混合分散させ母
粒子の表面に小粒子をまぶすもの）の混合分散作用で母
粒子の表面に子粒子をまぶしたオーダードミックスチャ
ーを形成させる。オーダードミックスチャーを計量器で
一定量計量し、ハイブリタイザーにかける。ハイブリタ
イザーにかけ、粒子を気相中に分散させながら、衝撃力
を主体とする機械的エネルギーを粒子に与え、完全にＰ
ＭＭＡの表面に粒子（酸化亜鉛粒子と焼成酸化マグネシ
ウム粒子）をメカノフュージョンにより固着化させた。Example (6) A composite powder pigment of polymethyl methacrylate (abbreviation: PMMA), zinc oxide and calcined magnesium oxide was produced using a hybridization system (Nara Machinery Co., Ltd.). PMMA (manufactured by Sekisui Chemical Co., Ltd.) 10 kg of zinc oxide (manufactured by Sakai Chemical Co., Ltd.) of base particles and child particles was calcined at 850 ° C. to obtain magnesium oxide 3.
kg. M. Tyzer (ordered mixture typer that corresponds to a part of the above-mentioned hybridization system, which mixes and disperses powder and scatters small particles on the surface of mother particles). To form an ordered mixture. A fixed amount of the ordered mixture is weighed with a measuring device, and the mixture is applied to a hybridizer. Applying mechanical energy mainly by impact force to the particles while dispersing the particles in the gas phase with a hybridizer,
Particles (zinc oxide particles and calcined magnesium oxide particles) were fixed on the surface of the MMA by mechanofusion.

【００７９】実施例（２）、実施例（３）、実施例
（４）、実施例（５）、実施例（６）で得た化粧料用抗
菌性有機複合粉体顔料、無機複合粉体顔料の微生物に対
するＭＩＣ（最小発育阻止濃度）を調べ、抗菌効果を測
定した。その結果を表３、表４で示す。なお、表３〜４
における実施（２）、実施（３）、実施（４）、実施
（５）、実施（６）は、それぞれ、実施例（２）、実施
例（３）、実施例（４）、実施例（５）、実施例（６）
を示す。The antibacterial organic composite powder pigment and inorganic composite powder for cosmetics obtained in Example (2), Example (3), Example (4), Example (5), and Example (6) The MIC (minimum inhibitory concentration) of the pigment on microorganisms was examined, and the antibacterial effect was measured. The results are shown in Tables 3 and 4. Tables 3 and 4
(2), (3), (4), (5), and (6) in Example 2 are the examples (2), (3), (4), and ( 5), Example (6)
Is shown.

【００８０】[0080]

【表３】 [Table 3]

【００８１】[0081]

【表４】 [Table 4]

【００８２】表３、表４から判るように、本発明の化粧
料用抗菌性粉体顔料及び複合粉体顔料は、抗菌、防腐効
果を示した。As can be seen from Tables 3 and 4, the antibacterial powder pigment for cosmetics and the composite powder pigment of the present invention exhibited antibacterial and antiseptic effects.

【００８３】［実施例（７）及び比較例（１）と比較例
（２）の評価］表５の組成にしたがって、８０℃に加温
した油相を溶解し、減圧した後、８０℃に加温した水相
を徐々に添加し、５００ｒｐｍで１０分間乳化し、冷却
した後取り出し、クリームを得た。[Evaluation of Example (7) and Comparative Examples (1) and (2)] According to the composition shown in Table 5, the oil phase heated to 80 ° C. was dissolved, and the pressure was reduced. The warmed aqueous phase was gradually added, emulsified at 500 rpm for 10 minutes, cooled, and taken out to obtain a cream.

【００８４】[0084]

【表５】 [Table 5]

【００８５】［実施例（８）及び比較例（３）と比較例
（４）の評価］表６の組成にしたがって８５℃に加温
し、溶解、分散させた油相を減圧し、この油相に、８５
℃に加温し、分散させた水相を徐々に添加し、１０分間
乳化する。その後３０℃まで冷却した後取り出し、クリ
ームファンデーションを得た。[Evaluation of Example (8), Comparative Example (3) and Comparative Example (4)] According to the composition shown in Table 6, the oil phase dissolved and dispersed was depressurized by heating at 85 ° C. 85
C., and the dispersed aqueous phase is gradually added and emulsified for 10 minutes. Thereafter, the mixture was cooled to 30 ° C. and taken out to obtain a cream foundation.

【００８６】[0086]

【表６】 [Table 6]

【００８７】［実施例（９）及び比較例（５）と比較例
（６）の評価］表７の組成にしたがって、粉体をヘンジ
ェルミキサーで混合した後、粉砕機で粉砕、分散させ
る。この粉砕物に油剤を注入し、５分間攪拌混合した
後、取り出し、粉砕機で解砕し、中皿に充填してパウダ
ーファンデーションを得た。[Evaluation of Example (9) and Comparative Examples (5) and (6)] According to the composition shown in Table 7, the powder was mixed with a Hängel mixer, and then ground and dispersed with a crusher. An oil solution was poured into the pulverized product, and the mixture was stirred and mixed for 5 minutes, taken out, crushed by a pulverizer, and filled in a middle plate to obtain a powder foundation.

【００８８】[0088]

【表７】 [Table 7]

【００８９】［製品防腐試験］各製品５０ｇを製品容器
に入れ、大腸菌、黄色ブドウ球菌、緑膿菌は寒天培地に
３７℃で２４時間培養した後、滅菌食塩水に懸濁させて
使用し、カンジタ、黒コウジカビはポテトデキストロー
ス寒天に３０℃で各々４８時間と４日間培養した後に、
滅菌食塩水に懸濁させたものを１０6ｃｅｌｌｓ／ｇに
接種し、時間経過にともなう菌数を測定した。その結果
を表８に示す。[Product Preservative Test] 50 g of each product was placed in a product container, and Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa were cultured on an agar medium at 37 ° C. for 24 hours, and used by suspending in sterile saline. Candida and Aspergillus niger were cultured on potato dextrose agar at 30 ° C. for 48 hours and 4 days, respectively.
The suspension in sterile saline was inoculated at 10 6 cells / g, and the number of bacteria over time was measured. Table 8 shows the results.

【００９０】[0090]

【表８】 [Table 8]

【００９１】上記以外の化粧料にも本発明の化粧料用抗
菌性粉体顔料及び複合粉体顔料は、カーマインローショ
ン、整肌化粧水、ツーウェイケーキ、ケーキアイシャド
ウ、コンパクトパウダー、制汗スプレー、フェイスパウ
ダー、ボディパウダー、フェースブラッシュ、ベビーパ
ウダー、クリームルージュ、リップスティック、リップ
グロス、アイライナー、マスカラ、アイブロウペンシ
ル、アンダーメークアップベースに配合したときも、同
様に優れた抗菌効果を示した。In addition to the above-mentioned cosmetics, the antibacterial powder pigment and the composite powder pigment for cosmetics of the present invention include carmine lotion, skin lotion, two-way cake, cake eyeshadow, compact powder, antiperspirant spray, When used in face powder, body powder, face brush, baby powder, cream rouge, lipstick, lip gloss, eyeliner, mascara, eyebrow pencil, and under makeup base, the same antibacterial effect was exhibited.

【００９２】以上のように、発明の化粧料用抗菌性粉体
顔料及び複合粉体顔料は、優れた抗菌効果を示し、これ
を配合した化粧品業界で汎用されている表示成分である
パラベン類やフェノキシエタノールやヒノキチオール等
の無表示成分の防腐剤を配合した化粧料よりも接種した
微生物に対する抗菌効果が優れているばかりでなく、よ
り低濃度で抗菌作用があり、長期間に亘る持続的効果を
有すると共に優れた安定性を示した。従って、本発明の
抗菌性素材を配合した化粧料は、市場にある防腐剤を使
用する事なく、又、その配合量に法的規制もなく、更に
は防腐剤フリーとしての化粧料の開発に役立つ。As described above, the antibacterial powder pigments for cosmetics and the composite powder pigments of the present invention exhibit excellent antibacterial effects, and include parabens, which are display components commonly used in the cosmetics industry, containing the same. It has better antibacterial effect against inoculated microorganisms than cosmetics containing preservatives of non-labeled components such as phenoxyethanol and hinokitiol, as well as antibacterial activity at lower concentrations and has a long-lasting effect. And showed excellent stability. Therefore, the cosmetics containing the antibacterial material of the present invention can be used without the use of preservatives on the market, without any legal restrictions on the amount of the preservatives, and in the development of preservative-free cosmetics. Useful.

【００９３】[0093]

【発明の効果】請求項１の化粧料用抗菌性粉体顔料及び
請求項２の化粧料用抗菌性複合粉体顔料は、酸化マグネ
シウムから成る抗菌性焼成粒子を有するので、次の効果
を奏することができる。The antibacterial powder pigment for cosmetics according to claim 1 and the antibacterial composite powder pigment for cosmetics according to claim 2 have antibacterial baked particles composed of magnesium oxide, and therefore have the following effects. be able to.

【００９４】微生物である細菌やカビに対して良好な抗
菌性ないし殺菌性を有するにもかかわらず、人体に対し
て悪影響がなく、使用量の制限を受けることがなく、化
粧料に配合した場合でも化粧料のｐＨ、化粧料の各種共
存成分等により抗菌力を損なうことがなく、化粧料を変
質させることもなく、使用感が良好である。また、化粧
料に必要とされる防腐殺菌剤の配合量をより低濃度に抑
えた低濃度防腐殺菌剤配合化粧料や無防腐殺菌剤（防腐
殺菌剤フリー）の化粧料の開発を可能にすることができ
る。さらに、微生物である細菌やカビに対して良好な抗
菌性ないし殺菌性を長期間に亘って持続することができ
る。Despite having good antibacterial or bactericidal properties against microorganisms such as bacteria and fungi, it has no adverse effect on the human body, is not restricted in the amount used, and is incorporated in cosmetics. However, the antimicrobial activity is not impaired by the pH of the cosmetic, various coexisting components of the cosmetic, and the like, and the cosmetic does not deteriorate, and the feeling of use is good. In addition, it enables the development of low-concentration antiseptic-bleeding cosmetics and cosmetics with no preservatives (antiseptic-free), in which the amount of preservatives and sterilizing agents required for cosmetics is reduced to a lower level. be able to. Further, good antibacterial property or bactericidal property can be maintained for a long period of time against microorganisms such as bacteria and mold.

【００９５】前記抗菌性焼成粒子又は、前記抗菌性焼成
粒子と化粧料用粉体粒子が固着して成る抗菌性複合粉体
粒子のいずれかを化粧料組成物に配合した場合、前記抗
菌性焼成粒子と前記抗菌性複合粉体粒子は、いずれも、
水や炭酸ガスの影響、ｐＨの影響や高極性油に対する影
響を受けず、又、非イオン活性剤とコンプレックスを形
成せず、不活性化することもなく、水溶性高分子への吸
着或いは錯体形成による防腐活性低下の問題も起こさず
に、しかも安全性が高いので、長期間安定で高い抗菌力
を有する化粧料組成物を提供することができる。更に、
前記抗菌性焼成粒子と前記抗菌性複合粉体粒子は、いず
れも、製造段階で生じる微生物の一次汚染や消費者の使
用中に発生する微生物の二次汚染に対しても優れた防腐
効果を付与するので、既存の化粧料組成物の微生物汚染
に関する課題を解決することができる。When the antibacterial baked particles or the antibacterial composite powder particles obtained by fixing the baked antibacterial particles and the powder particles for cosmetics are blended in a cosmetic composition, Both the particles and the antibacterial composite powder particles,
It is not affected by water or carbon dioxide gas, pH or highly polar oils, does not form a complex with nonionic surfactants, does not deactivate, and adsorbs or complexes with water-soluble polymers. Since there is no problem of a decrease in preservative activity due to the formation and high safety, a cosmetic composition having long-term stability and high antibacterial activity can be provided. Furthermore,
Both the antibacterial baked particles and the antibacterial composite powder particles impart an excellent antiseptic effect to primary contamination of microorganisms generated during the production stage and secondary contamination of microorganisms generated during use by consumers. Therefore, the problem relating to microbial contamination of the existing cosmetic composition can be solved.

【００９６】請求項３の化粧料用抗菌性粉体顔料の製造
方法は、水酸化マグネシウム及び酸化マグネシウムのう
ちの１種以上から成る抗菌性粒子を８５０℃以上で焼成
して抗菌性焼成粒子を得る焼成工程を含むので、請求項
１の化粧料用抗菌性粉体顔料を製造することができる。The method for producing an antibacterial powder pigment for cosmetics according to claim 3 is characterized in that the antibacterial particles comprising at least one of magnesium hydroxide and magnesium oxide are fired at 850 ° C. or higher to obtain the fired antibacterial particles. Since the calcination step is included, the antibacterial powder pigment for cosmetics of claim 1 can be produced.

【００９７】請求項４の化粧料用抗菌性複合粉体顔料の
製造方法は、前記焼成工程と、前記焼成工程で得た抗菌
性焼成粒子と化粧料用粉体粒子を固着させて抗菌性複合
粉体粒子を得る複合化工程を含むので、請求項２の化粧
料用抗菌性複合粉体顔料を製造することができる。請求
項５の化粧料用抗菌性複合粉体顔料の製造方法は、水酸
化マグネシウム及び酸化マグネシウムのうちの１種以上
が付着する化粧料用粉体粒子を８５０℃以上で焼成し
て、酸化マグネシウムから成る抗菌性焼成粒子と化粧料
用粉体粒子が固着して成る抗菌性複合粉体粒子を得る焼
成複合化工程を含むので、請求項２の化粧料用抗菌性複
合粉体顔料を製造することができる。The method for producing an antibacterial composite powder pigment for cosmetics according to claim 4 is characterized in that the calcination step and the baked antibacterial particles obtained in the calcination step and the powder particles for cosmetics are fixed. Since the method includes a compounding step of obtaining powder particles, the antibacterial composite powder pigment for cosmetics according to claim 2 can be manufactured. The method for producing an antibacterial composite powder pigment for cosmetics according to claim 5, wherein the powdery cosmetic powder to which at least one of magnesium hydroxide and magnesium oxide adheres is calcined at 850 ° C or higher to obtain magnesium oxide. The present invention includes the step of baking and compounding to obtain antibacterial composite powder particles obtained by fixing the antibacterial baked particles composed of and the powder particles for cosmetics, thereby producing the antibacterial composite powder pigment for cosmetics according to claim 2. be able to.

【００９８】請求項６の抗菌性化粧料組成物は、請求項
１の化粧料用抗菌性粉体顔料及び請求項２の化粧料用抗
菌性複合粉体顔料のうちの１種以上を含有するので、次
の効果を奏することができる。The antibacterial cosmetic composition of claim 6 contains at least one of the antibacterial powder pigment for cosmetics of claim 1 and the antibacterial composite powder pigment for cosmetics of claim 2. Therefore, the following effects can be obtained.

【００９９】化粧品原料基準に収載されている防腐剤や
化粧品以外に使用されている銀化合物、銅化合物、亜鉛
化合物を含有しない場合でも、微生物である細菌やカビ
に対して良好な抗菌性ないし殺菌性を有することができ
る。また、微生物である細菌やカビに対して良好な抗菌
性ないし殺菌性を有するにもかかわらず、化粧料に必要
とされる防腐殺菌剤の配合量をより低濃度に抑えたり、
あるいは無防腐殺菌剤（防腐殺菌剤フリー）にすること
ができる。さらに、微生物である細菌やカビに対して良
好な抗菌性ないし殺菌性を長期間に亘って持続すること
ができる。従って、防腐殺菌剤による皮膚刺激がなく、
長期間に亘り、安定な防腐殺菌効果を有することができ
る。Good antibacterial or bactericidal properties against microbes such as bacteria and fungi even when they do not contain preservatives listed in the standard for cosmetic raw materials or silver compounds, copper compounds and zinc compounds used other than cosmetics. Property. In addition, despite having good antibacterial or fungicidal properties against microorganisms such as bacteria and mold, the amount of antiseptic disinfectant required for cosmetics can be suppressed to a lower concentration,
Alternatively, an antiseptic disinfectant (preservative-free disinfectant free) can be used. Further, good antibacterial property or bactericidal property can be maintained for a long period of time against microorganisms such as bacteria and mold. Therefore, there is no skin irritation due to the preservative disinfectant,
It can have a stable antiseptic effect over a long period of time.

Claims (6)

【特許請求の範囲】[Claims] 【請求項１】酸化マグネシウムから成る抗菌性焼成粒子
を含有することを特徴とする化粧料用抗菌性粉体顔料。An antibacterial powder pigment for cosmetics, characterized by containing antibacterial baked particles composed of magnesium oxide. 【請求項２】酸化マグネシウムから成る抗菌性焼成粒子
と化粧料用粉体粒子が固着して成る抗菌性複合粉体粒子
を含有することを特徴とする化粧料用抗菌性複合粉体顔
料。2. An antibacterial composite powder pigment for cosmetics, comprising antibacterial baked particles composed of magnesium oxide and antibacterial composite powder particles formed by fixing powder particles for cosmetic. 【請求項３】水酸化マグネシウム及び酸化マグネシウム
のうちの１種以上から成る抗菌性粒子を８５０℃以上で
焼成して抗菌性焼成粒子を得る焼成工程を含むことを特
徴とする化粧料用抗菌性粉体顔料の製造方法。3. An antibacterial property for cosmetics comprising a firing step of firing antibacterial particles comprising at least one of magnesium hydroxide and magnesium oxide at 850 ° C. or higher to obtain antibacterial fired particles. A method for producing a powder pigment. 【請求項４】水酸化マグネシウム及び酸化マグネシウム
のうちの１種以上から成る抗菌性粒子を８５０℃以上で
焼成して抗菌性焼成粒子を得る焼成工程と、 前記焼成工程で得た抗菌性焼成粒子と化粧料用粉体粒子
を固着させて抗菌性複合粉体粒子を得る複合化工程を含
むことを特徴とする化粧料用抗菌性複合粉体顔料の製造
方法。4. A sintering step of sintering antibacterial particles composed of at least one of magnesium hydroxide and magnesium oxide at 850 ° C. or higher to obtain sinterable antibacterial particles; A method for producing an antibacterial composite powder pigment for cosmetics, comprising a composite step of fixing the powder particles and cosmetic powder particles to obtain antibacterial composite powder particles. 【請求項５】水酸化マグネシウム及び酸化マグネシウム
のうちの１種以上が付着する化粧料用粉体粒子を８５０
℃以上で焼成して、酸化マグネシウムから成る抗菌性焼
成粒子と化粧料用粉体粒子が固着して成る抗菌性複合粉
体粒子を得る焼成複合化工程を含むことを特徴とする化
粧料用抗菌性複合粉体顔料の製造方法。5. Cosmetic powder particles to which at least one of magnesium hydroxide and magnesium oxide adheres are 850.
And baking at a temperature of not less than ℃ to obtain antibacterial composite powder particles comprising magnesium oxide and antibacterial composite powder particles obtained by fixing cosmetic powder particles. Production method of functional composite powder pigment. 【請求項６】請求項１の化粧料用抗菌性粉体顔料及び請
求項２の化粧料用抗菌性複合粉体顔料のうちの１種以上
を含有することを特徴とする抗菌性化粧料組成物。6. An antibacterial cosmetic composition comprising at least one of the antibacterial powdery pigment for cosmetics according to claim 1 and the antibacterial composite powdery pigment for cosmetics according to claim 2. Stuff.
JP9015843A 1997-01-13 1997-01-13 Antimicrobial pigment for cosmetic, production of the pigment, and cosmetic composition containing the pigment Pending JPH10194929A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP9015843A JPH10194929A (en) 1997-01-13 1997-01-13 Antimicrobial pigment for cosmetic, production of the pigment, and cosmetic composition containing the pigment
FR9804668A FR2777457B1 (en) 1997-01-13 1998-04-15 ANTIBACTERIAL COSMETIC PRODUCTS, ANTIBACTERIAL SPRAY PIGMENT FOR SUCH PRODUCTS, AND PROCESS FOR THE PRODUCTION THEREOF

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP9015843A JPH10194929A (en) 1997-01-13 1997-01-13 Antimicrobial pigment for cosmetic, production of the pigment, and cosmetic composition containing the pigment
FR9804668A FR2777457B1 (en) 1997-01-13 1998-04-15 ANTIBACTERIAL COSMETIC PRODUCTS, ANTIBACTERIAL SPRAY PIGMENT FOR SUCH PRODUCTS, AND PROCESS FOR THE PRODUCTION THEREOF

Publications (1)

Publication Number Publication Date
JPH10194929A true JPH10194929A (en) 1998-07-28

Family

ID=26234265

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9015843A Pending JPH10194929A (en) 1997-01-13 1997-01-13 Antimicrobial pigment for cosmetic, production of the pigment, and cosmetic composition containing the pigment

Country Status (2)

Country Link
JP (1) JPH10194929A (en)
FR (1) FR2777457B1 (en)

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WO2002030365A1 (en) * 2000-10-06 2002-04-18 Kabushiki Kaisha Sangi Antibacterial resin
JP2003335631A (en) * 2002-05-17 2003-11-25 Shiseido Co Ltd Method for reducing skin irritation of composition for external use
JP2011051913A (en) * 2009-08-31 2011-03-17 Miyoshi Kasei Inc Composition for cosmetic preparation having ultraviolet-shielding effect and sebum solidifying ability
JP2015182958A (en) * 2014-03-20 2015-10-22 ポーラ化成工業株式会社 base makeup cosmetics
JP2016526530A (en) * 2013-07-09 2016-09-05 ロレアル Long-lasting cosmetic composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10065271A1 (en) * 2000-12-29 2002-07-18 Univ Hannover Process for combating fire blight and bacterial fire
JP5987672B2 (en) * 2011-12-28 2016-09-07 宇部マテリアルズ株式会社 Plant disease control agent and plant disease control method using the same

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Publication number Priority date Publication date Assignee Title
KR970000745B1 (en) * 1993-11-19 1997-01-18 주식회사 엘지화학 Coloring material for antibiotic cosmetics, method for their preparation and cosmetic compositions containing coloring material
JPH0930917A (en) * 1995-07-20 1997-02-04 Miyoshi Kasei:Kk Inorganic metal oxide-clay mineral-coated powder and cosmetic compounded with the coated powder
JPH09272815A (en) * 1996-04-02 1997-10-21 Merck Japan Kk Composite metal oxide fine particle and production of the same

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002030365A1 (en) * 2000-10-06 2002-04-18 Kabushiki Kaisha Sangi Antibacterial resin
JPWO2002030365A1 (en) * 2000-10-06 2004-02-19 株式会社サンギ Antibacterial resin
JP2003335631A (en) * 2002-05-17 2003-11-25 Shiseido Co Ltd Method for reducing skin irritation of composition for external use
JP2011051913A (en) * 2009-08-31 2011-03-17 Miyoshi Kasei Inc Composition for cosmetic preparation having ultraviolet-shielding effect and sebum solidifying ability
JP2016526530A (en) * 2013-07-09 2016-09-05 ロレアル Long-lasting cosmetic composition
JP2015182958A (en) * 2014-03-20 2015-10-22 ポーラ化成工業株式会社 base makeup cosmetics

Also Published As

Publication number Publication date
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FR2777457A1 (en) 1999-10-22

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