JP2001058934A - Antisuntan cosmetic - Google Patents

Antisuntan cosmetic

Info

Publication number
JP2001058934A
JP2001058934A JP11232832A JP23283299A JP2001058934A JP 2001058934 A JP2001058934 A JP 2001058934A JP 11232832 A JP11232832 A JP 11232832A JP 23283299 A JP23283299 A JP 23283299A JP 2001058934 A JP2001058934 A JP 2001058934A
Authority
JP
Japan
Prior art keywords
weight
polyoxyalkylene
zinc oxide
fatty acid
less
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.)
Granted
Application number
JP11232832A
Other languages
Japanese (ja)
Other versions
JP4011799B2 (en
Inventor
Kyoko Shiroichi
京子 城市
Katsumoto Ogawa
克基 小川
Kazuhisa Ono
和久 大野
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.)
Shiseido Co Ltd
Original Assignee
Shiseido Co Ltd
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
Priority to JP23283299A priority Critical patent/JP4011799B2/en
Application filed by Shiseido Co Ltd filed Critical Shiseido Co Ltd
Priority to PCT/JP2000/005547 priority patent/WO2001013874A1/en
Priority to US09/807,750 priority patent/US6749838B1/en
Priority to EP00953503A priority patent/EP1123697A1/en
Priority to AU65961/00A priority patent/AU775971B2/en
Priority to KR1020017004871A priority patent/KR100849404B1/en
Priority to CNB008017425A priority patent/CN100369601C/en
Priority to TW089116871A priority patent/TWI231217B/en
Publication of JP2001058934A publication Critical patent/JP2001058934A/en
Application granted granted Critical
Publication of JP4011799B2 publication Critical patent/JP4011799B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Cosmetics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain an antisuntan cosmetic, good in dispersion and excellent in ultraviolet preventing effects, transparency of finish and stability in the system by formulating a complex powder prepared by carrying out a specific treatment of a particulate zinc oxide with a polyoxyalkylene-modified polysiloxane. SOLUTION: This antisuntan cosmetic is obtained by including (A) a complex powder prepared by coating a particulate zinc oxide having <=0.1 μm size with silicic acid anhydride at 5-30 wt.% coverage and carrying out a surface treatment of the coated zinc oxide with 3-12 wt.% of a silicone and (B) one or more kinds selected from polyoxyalkylene-modified polysiloxanes represented by formulae I to III (R is methyl or the like; R' is H or a 1-12C alkyl; p is 1-5; q is 2-3; x, m and n are each an average number and a numerical value so that the polyoxyalkylene-modified organopolysiloxanes are contained in an amount of 5-40 wt.% in the molecule and the molecular weight thereof is >=2,000). The ingredient A is preferably contained in an amount of 3-30 wt.% and the ingredient B is preferably contained in an amount of 0.5-7 wt.%.

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】本発明は微粒子酸化亜鉛を配
合した日焼け止め化粧料に関し、特にその安定性と紫外
線防止効果の改善に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sunscreen cosmetic containing finely divided zinc oxide, and more particularly to an improvement in its stability and an effect of preventing ultraviolet rays.

【0002】[0002]

【従来の技術】従来、日焼け止め化粧料には微粒子酸化
亜鉛が長波長紫外線を防止する目的に多量配合されてい
た。主にW/O乳化型日焼け止め化粧料に微粒子酸化亜
鉛を配合する場合には一般的には粉末の表面を疎水化処
理したものを用いていた。その疎水化処理としては例え
ばシリコーン、金属セッケン、脂肪酸、フッ素化合物等
が挙げられる。
2. Description of the Related Art Hitherto, a large amount of particulate zinc oxide has been incorporated into sunscreen cosmetics for the purpose of preventing long-wavelength ultraviolet rays. In the case of blending zinc oxide fine particles mainly in a W / O emulsified sunscreen cosmetic, a powder whose surface is subjected to a hydrophobic treatment is generally used. Examples of the hydrophobic treatment include silicone, metal soap, fatty acid, and fluorine compound.

【0003】[0003]

【発明が解決しようとする課題】しかしながら、このよ
うな表面処理微粒子酸化亜鉛を高度に分散することは非
常に難しく、思うようには紫外線防止効果が上がらず、
さらには系内の遊離脂肪酸と容易に反応することでゲル
化が起こり、安定性が経時で著しく悪くなるという欠点
を有していた。すなわち、本発明は微粒子酸化亜鉛の分
散が良好でSPF値やPFA値などの紫外線防止効果と
仕上りの透明性又は系内の安定性にも優れた日焼け止め
化粧料を提供するものである。
However, it is very difficult to highly disperse such surface-treated fine zinc oxide particles, and as expected, the effect of preventing ultraviolet rays does not increase.
Furthermore, it has a drawback that the gelation occurs by easily reacting with the free fatty acid in the system, and the stability is remarkably deteriorated with time. That is, the present invention provides a sunscreen cosmetic which has a good dispersion of fine-particle zinc oxide, an excellent effect of preventing ultraviolet rays such as SPF value and PFA value, and excellent transparency of finish or stability in the system.

【0004】[0004]

【課題を解決するための手段】本発明者らは、微粒子酸
化亜鉛を一次粒子に近い状態で無水ケイ酸の表面処理を
行った後にシリコーン処理を行った複合粉末は、ポリオ
キシアルキレン変性ポリシロキサンによって容易に高分
散することで、日焼け止め化粧料のSPF(SUN PROTEC
TION FACTOR)及びPFA(PROTECTION FACTOR OF UV
A)を効率的に向上することを見出した。しかも、粉末
の分散剤や表面処理剤として用いられている脂肪酸や脂
肪酸セッケンに起因する系内の遊離脂肪酸との反応(金
属セッケンの生成によるゲル化反応)が起こらず、常に
系内の粘度を安定的な状態に維持し、心地良い使用感触
を持続していることも見出した。
Means for Solving the Problems The present inventors have developed a composite powder obtained by subjecting a fine powder of zinc oxide to a surface treatment of silicic anhydride in a state close to primary particles and then carrying out a silicone treatment, thereby obtaining a polyoxyalkylene-modified polysiloxane. It is easy to disperse easily by using the sunscreen cosmetics SPF (SUN PROTEC
TION FACTOR) and PFA (PROTECTION FACTOR OF UV)
A) was found to improve efficiently. In addition, there is no reaction with free fatty acids in the system due to fatty acids or fatty acid soaps used as powder dispersing agents or surface treatment agents (gelation reaction due to the generation of metal soaps), and the viscosity in the system is always reduced. They also found that they maintained a stable state and maintained a comfortable use feel.

【0005】すなわち、本発明の日焼け止め化粧料は、
0.1μm以下の微粒子酸化亜鉛に無水ケイ酸を被覆率
5重量%以上30重量%以下で被覆し、さらにシリコー
ンを3重量%以上12重量%以下で表面処理した複合粉
末と、下記一般式[1][2]または[3]に示したポ
リオキシアルキレン変性ポリシロキサンから選ばれる1
種または2種以上とを配合することを特徴とする。
That is, the sunscreen cosmetics of the present invention
A composite powder obtained by coating fine particles of zinc oxide having a particle size of 0.1 μm or less with silicic anhydride at a coverage of 5% by weight or more and 30% by weight and further subjecting silicone to a surface treatment of 3% by weight or more and 12% by weight or less; 1] 1 selected from the polyoxyalkylene-modified polysiloxanes shown in [2] or [3]
It is characterized by blending with a seed or two or more kinds.

【0006】[0006]

【化4】 Embedded image

【化5】 Embedded image

【化6】 (ただし、一般式[1][2][3]中、Rはメチル基
または一部がフェニル基、Rは水素または炭素数1〜1
2のアルキル基、pは1〜5の数、qは2〜3の数、
x、m、nは平均数でポリオキシアルキレン変性オルガ
ノポリシロキサンが分子中にポリオキシアルキレン基を
5〜40重量%含有し且つ該ポリオキシアルキレン変性
オルガノポリシロキサンの分子量が2000以上になるよう
な数値を表わす。)
Embedded image (However, in the general formulas [1], [2] and [3], R is a methyl group or a partially phenyl group, R is hydrogen or a carbon atom having 1 to 1 carbon atoms.
2 is an alkyl group, p is a number of 1 to 5, q is a number of 2 to 3,
x, m, and n are average numbers such that the polyoxyalkylene-modified organopolysiloxane contains 5 to 40% by weight of a polyoxyalkylene group in the molecule and the molecular weight of the polyoxyalkylene-modified organopolysiloxane becomes 2000 or more. Indicates a numerical value. )

【0007】また、本発明の日焼け止め化粧料において
は、無水ケイ酸とシリコーンで処理された微粒子酸化亜
鉛の複合粉末を3重量%以上30重量%以下配合し、ポ
リオキシアルキレン変性ポリシロキサンを0.5重量%
以上7重量%以下配合することが好適である。また、本
発明の日焼け止め化粧料においては、さらに脂肪酸及び
脂肪酸セッケン、脂肪酸エステルを0.1重量%以上配
合し、脂肪酸及び脂肪酸セッケン、脂肪酸エステルで表
面処理した粉末を1重量%以上配合することが好適であ
る。
Further, in the sunscreen cosmetic of the present invention, a composite powder of fine zinc oxide treated with silicic anhydride and silicone is blended in an amount of 3% by weight to 30% by weight, and the polyoxyalkylene-modified polysiloxane is added in an amount of 0 to 30% by weight. 0.5% by weight
It is preferable that the content is not less than 7% by weight. Further, in the sunscreen cosmetic of the present invention, a fatty acid, a fatty acid soap and a fatty acid ester are further blended in an amount of 0.1% by weight or more, and a powder surface-treated with the fatty acid, the fatty acid soap and the fatty acid ester is further blended in an amount of 1% by weight or more. Is preferred.

【0008】[0008]

【発明の実施の形態】本発明は0.1μm以下の微粒子
酸化亜鉛に無水ケイ酸で被覆率5重量%以上30重量%
以下で被覆し、さらにその表面にシリコーン処理を施し
た複合粉末とポリオキシアルキレン変性ポリシロキサン
とを組合わせることで、微粒子酸化亜鉛が従来にはなく
高く分散された状態となり、紫外線防止効果が向上する
ことを特徴とする日焼け止め化粧料である。
BEST MODE FOR CARRYING OUT THE INVENTION The present invention relates to a method of coating fine particles of zinc oxide having a particle size of 0.1 μm or less with silicic anhydride at a coverage of 5% by weight or more and 30% by weight.
By combining the composite powder coated below with a polyoxyalkylene-modified polysiloxane that has been subjected to a silicone treatment on its surface, the particulate zinc oxide is in a state of higher dispersion than ever before, and the UV protection effect is improved. It is a sunscreen cosmetic characterized by doing.

【0009】また、微粒子酸化亜鉛が無水ケイ酸で均一
に被覆されていることによって、系内への亜鉛イオンの
溶出が抑制され、遊離脂肪酸との反応による金属セッケ
ンの生成が起こらない。それによって、経時や温度によ
ってもゲル化しない為、系内の粘度を常に安定的な状態
に維持し、心地良い使用感触を持続していることを特徴
とする日焼け止め化粧料である。
In addition, since the fine zinc oxide is uniformly coated with silicic anhydride, elution of zinc ions into the system is suppressed, and generation of metal soap by reaction with free fatty acids does not occur. As a result, the composition does not gel even with the passage of time or temperature, so that the viscosity in the system is always maintained in a stable state, and the sunscreen cosmetic is characterized by maintaining a comfortable use feeling.

【0010】すなわち、本発明は微粒子酸化亜鉛の分散
が良好で安定性と紫外線防止効果に優れる日焼け止め化
粧料に関するものであり、さらに詳しくは微粒子酸化亜
鉛に無水ケイ酸とシリコーン処理を行うことで、ポリオ
キシアルキレン変性ポリシロキサンにより容易に高分散
することで紫外線防止効果に優れ、また、遊離脂肪酸と
の反応が起こらない安定性も良好な日焼け止め化粧料に
関するものである。
That is, the present invention relates to a sunscreen cosmetic having a good dispersion of fine zinc oxide and excellent stability and ultraviolet ray preventing effect. More specifically, the present invention relates to a fine zinc oxide treated with silicic anhydride and silicone. The present invention relates to a sunscreen cosmetic which is easily dispersed with a polyoxyalkylene-modified polysiloxane so as to have an excellent effect of preventing ultraviolet rays and has good stability not to react with free fatty acids.

【0011】本発明に用いられる微粒子酸化亜鉛は一般
的にフランス法やアメリカ法で得られる。市販の平均粒
子径が0.1μm以下の微粒子酸化亜鉛としてはFINEX-2
5,FINEX-50,FINEX-75(堺化学工業社製)、ZnO3
50(住友大阪セメント社製)、ZINCOX SUPER−10,ZI
NCOX SUPER−20R, ZINCOX SUPER−30(白水化学工業社
製)、Z-COTE(Sun Smart社製)などが挙げられる。
The particulate zinc oxide used in the present invention is generally obtained by a French method or an American method. As a commercially available fine particle zinc oxide having an average particle diameter of 0.1 μm or less, FINEX-2
5, FINEX-50, FINEX-75 (made by Sakai Chemical Industry Co., Ltd.), ZnO3
50 (Sumitomo Osaka Cement), ZINCOX SUPER-10, ZI
NCOX SUPER-20R, ZINCOX SUPER-30 (manufactured by Hakusui Chemical), Z-COTE (manufactured by Sun Smart) and the like.

【0012】次に本発明の複合粉体の製造法について説
明する。上記の微粒子酸化亜鉛を水溶液中でサンドグラ
インダーミル等を用いて高度の分散状態を保ったまま、
ケイ酸ソーダーを添加、中和して、無水ケイ酸を均一に
被覆する。または微粒子酸化亜鉛を有機溶媒中で高度に
分散した後、アルコキシシランを用いて無水ケイ酸を均
一に被覆する。他の製法にても製造可能で最終的に無水
ケイ酸で一定量被覆されていれば本発明に支障をきたさ
ない。無水ケイ酸を5重量%以上30重量%以下被覆す
ることが好ましい。特に10重量%以上23重量%以下
が特に好ましい。5重量%以下では酸化亜鉛の回りにを
均一に被覆することが難しく、亜鉛イオンの溶出により
安定性の悪化や紫外線防止効果の低下が見られれてく
る。また、30重量%以上では無水ケイ酸によるキシミ
感等の使用感触の悪化が見られてくる。その後、各種粉
末分散装置を用いてシリコーンを3重量%以上12重量
%以下の処理を施し、目的とする複合粉末を得る。
Next, a method for producing the composite powder of the present invention will be described. While maintaining a high dispersion state of the above fine particle zinc oxide in an aqueous solution using a sand grinder mill or the like,
Sodium silicate is added and neutralized to uniformly coat the silicic anhydride. Alternatively, after finely divided zinc oxide is highly dispersed in an organic solvent, silicic anhydride is uniformly coated with alkoxysilane. The present invention will not be hindered as long as it can be produced by other production methods and is finally coated with a certain amount of silicic anhydride. It is preferable to coat the silica with 5% by weight or more and 30% by weight or less. In particular, it is particularly preferably from 10% by weight to 23% by weight. If the content is less than 5% by weight, it is difficult to uniformly coat around the zinc oxide, and the elution of zinc ions leads to deterioration in stability and a decrease in the effect of preventing ultraviolet rays. Further, when the content is 30% by weight or more, the use sensation such as the tingling sensation due to the silicic anhydride is deteriorated. Thereafter, the silicone is subjected to a treatment of 3% by weight or more and 12% by weight or less using various kinds of powder dispersing apparatuses to obtain a target composite powder.

【0013】本発明で行われるシリコーン処理剤として
は、メチルハイドロジェンポリシロキサン、ジメチルポ
リシロキサン、メチルフェニルポリシロキサンなどの各
種のシリコーンオイル、メチルトリメトキシシラン、エ
チルトリメトキシシラン、ヘキシルトリメトキシシラ
ン、オクチルトリメトキシシランなどの各種のアルキル
シラン、トリフルオロメチルエチルトリメトキシシラ
ン、ヘプタデカフルオロデシルトリメトキシシランなど
の各種のフルオロアルキルシランなどが挙げら、これら
を単独、または二種以上を混合して用いることができ
る。
Examples of the silicone treating agent used in the present invention include various silicone oils such as methyl hydrogen polysiloxane, dimethyl polysiloxane and methyl phenyl polysiloxane, methyltrimethoxysilane, ethyltrimethoxysilane, hexyltrimethoxysilane, Various alkylsilanes such as octyltrimethoxysilane, trifluoromethylethyltrimethoxysilane, various fluoroalkylsilanes such as heptadecafluorodecyltrimethoxysilane and the like, and these can be used alone or in combination of two or more. Can be used.

【0014】本発明で用いられる複合粉末を日焼け止め
化粧料に3重量%以上配合し、30重量%以下配合する
ことが好ましい。特に好ましいのは10重量%以上配合
し、23重量%以下が紫外線防止効果と透明性、使用感
触的にバランスが良い。反対に3重量%以下では紫外線
防止効果は得られず、30重量%以上では透明性や使用
感触が極端に悪化してくる。
The composite powder used in the present invention is blended in the sunscreen cosmetic at 3% by weight or more, preferably at 30% by weight or less. Particularly preferred is 10% by weight or more, and 23% by weight or less has a good balance between the ultraviolet ray preventing effect and the transparency and feel when used. Conversely, if the amount is less than 3% by weight, the effect of preventing ultraviolet rays cannot be obtained.

【0015】本発明に使用されるポリオキシアルキレン
変性ポリシロキサンとしては下記一般式[1]、[2]
又は[3]で示される。
The polyoxyalkylene-modified polysiloxane used in the present invention includes the following general formulas [1] and [2].
Or [3].

【化7】 Embedded image

【化8】 Embedded image

【化9】 一般式[1][2][3]中、Rはメチル基または一部
がフェニル基、Rは水素または炭素数1〜12のアルキ
ル基、pは1〜5の数、qは2〜3の数、x、m、nは
平均数でポリオキシアルキレン変性オルガノポリシロキ
サンが分子中にポリオキシアルキレン基を5〜40重量
%含有し且つ該ポリオキシアルキレン変性オルガノポリ
シロキサンの分子量が2000以上になるような数値を表わ
す。本発明には該ポリオキシアルキレン変性オルガノポ
リシロキサンを少なくても1種または2種以上を配合す
ることを特徴とする。
Embedded image In the general formulas [1], [2] and [3], R is a methyl group or a partially phenyl group, R is hydrogen or an alkyl group having 1 to 12 carbon atoms, p is a number of 1 to 5, and q is 2 to 3 The numbers x, m, and n are the average numbers of the polyoxyalkylene-modified organopolysiloxane containing 5 to 40% by weight of a polyoxyalkylene group in the molecule and the molecular weight of the polyoxyalkylene-modified organopolysiloxane is 2,000 or more. Represents a numerical value such as The present invention is characterized in that at least one or more of the polyoxyalkylene-modified organopolysiloxanes are blended.

【0016】本発明に使用されるポリオキシアルキレン
変性ポリシロキサンを日焼け止め化粧料に0.5重量%
以上7重量%以下配合して用いることが出来る。0.5
重量%より少ないと粉末の分散が不充分となることがあ
り、凝集ブツ等が見られることがある。一方で、7重量
%を超えて配合すると肌上では残留油分として働き、べ
たつき等が見られ使用感触が極端に悪くなる。
The polyoxyalkylene-modified polysiloxane used in the present invention is added to the sunscreen cosmetic in an amount of 0.5% by weight.
More than 7% by weight can be used. 0.5
If the amount is less than the weight percentage, the dispersion of the powder may be insufficient, and cohesion or the like may be observed. On the other hand, if the content exceeds 7% by weight, it acts as a residual oil component on the skin, stickiness and the like are observed, and the feeling of use becomes extremely poor.

【0017】本発明に使用される粉末の分散剤及び表面
処理剤としての脂肪酸及び脂肪酸セッケン、脂肪酸エス
テルとしてはパルミチン酸、イソステアリン酸、ステア
リン酸、ラウリン酸、ミリスチン酸、ベヘニン酸、オレ
イン酸、ロジン酸、12―ヒドロキシステアリン酸等の
脂肪酸及びステアリン酸アルミニウム、ステアリン酸カ
ルシウム、12―ヒドロキシステアリン酸アルミニウム
等の脂肪酸セッケン及びデキストリン脂肪酸エステル、
コレステロール脂肪酸エステル、ショ糖脂肪酸エステ
ル、デンプン脂肪酸エステル等が挙げられ、これらを単
独、または二種以上を用いることができる。分散剤とし
ての効果を得るためには0.1重量%以上の配合が好ま
しい。
Fatty acids and fatty acid soaps as dispersants and surface treating agents for the powder used in the present invention, and palmitic acid, isostearic acid, stearic acid, lauric acid, myristic acid, behenic acid, oleic acid, rosin as fatty acid esters Acid, fatty acid such as 12-hydroxystearic acid and aluminum stearate, calcium stearate, fatty acid soap and dextrin fatty acid ester such as aluminum 12-hydroxystearate,
Cholesterol fatty acid esters, sucrose fatty acid esters, starch fatty acid esters and the like can be mentioned, and these can be used alone or in combination of two or more. In order to obtain the effect as a dispersant, the content is preferably 0.1% by weight or more.

【0018】本発明の日焼け止め化粧料には、酸化チタ
ン、酸化亜鉛、ベンガラ、黄酸化鉄、黒酸化鉄、群青、
酸化セリウム、タルク、マイカ、セリサイト、カオリ
ン、ベントナイト、クレー、ケイ酸、無水ケイ酸、ケイ
酸マグネシウム、ステアリン酸亜鉛、含フッ素金雲母、
合成タルク、硫酸バリウム、硫酸マグネシウム、硫酸カ
ルシウム、チッ化ホウ素、オキシ塩化ビスマス、アルミ
ナ、酸化ジルコニウム、酸化マグネシウム、酸化クロ
ム、カラミン、炭酸マグネシウムおよびこれらの複合体
等の無機粉末;シリコーン粉末、シリコーン弾性粉末、
ポリウレタン粉末、セルロース粉末、ナイロン粉末、P
MMA粉末、スターチ、ポリエチレン粉末等及びこれら
の複合体等の有機粉末を用いることができ、これらの1
種以上を含有せしめる。これら粉末は前記脂肪酸及び脂
肪酸セッケン、脂肪酸エステルで表面処理されているこ
とが好ましく、配合量としては1重量%以上が日焼け止
め効果が高まるので好ましい。この粉末を配合する場
合、前記脂肪酸及び脂肪酸セッケン、脂肪酸エステルが
配合されていることが紫外線防止効果上、系内の安定性
上好ましい。
The sunscreen cosmetics of the present invention include titanium oxide, zinc oxide, red iron oxide, yellow iron oxide, black iron oxide, ultramarine,
Cerium oxide, talc, mica, sericite, kaolin, bentonite, clay, silicic acid, silicic anhydride, magnesium silicate, zinc stearate, fluorophlogopite,
Inorganic powders such as synthetic talc, barium sulfate, magnesium sulfate, calcium sulfate, boron nitride, bismuth oxychloride, alumina, zirconium oxide, magnesium oxide, chromium oxide, calamine, magnesium carbonate and composites thereof; silicone powder, silicone elasticity Powder,
Polyurethane powder, cellulose powder, nylon powder, P
Organic powders such as MMA powder, starch, polyethylene powder and composites thereof can be used.
Contains more than species. These powders are preferably surface-treated with the above-mentioned fatty acids, fatty acid soaps and fatty acid esters, and a blending amount of 1% by weight or more is preferable because the sunscreen effect is enhanced. When this powder is blended, it is preferable to blend the fatty acid, the fatty acid soap and the fatty acid ester from the viewpoint of the ultraviolet ray preventing effect and the stability in the system.

【0019】また、本発明の化粧料における油性成分と
しては、流動パラフィン、スクワラン、エステル油、ジ
グリセライド、トリグリセライド、パーフルオロポリエ
ーテル、ワセリン、ラノリン、セレシン、カルナバロ
ウ、固型パラフィン、脂肪酸、多価アルコール、シリコ
ーン樹脂、フッ素樹脂、アクリル樹脂、ビニルピロリド
等を組合わせて、油性成分として1種以上含有せしめ
る。本発明の化粧料には、更に、色素、pH調整剤、保
質剤、増粘剤、界面活性剤、分散在、安定化剤、着色
剤、防腐剤、酸化防止剤、紫外線吸収剤、香料等も本発
明の目的を達する範囲内で適宜配合することが出来る。
The oily components in the cosmetic of the present invention include liquid paraffin, squalane, ester oil, diglyceride, triglyceride, perfluoropolyether, petrolatum, lanolin, ceresin, carnauba wax, solid paraffin, fatty acid, and polyhydric alcohol. , A silicone resin, a fluororesin, an acrylic resin, vinyl pyrrolide, etc., in combination to contain at least one oily component. The cosmetic of the present invention further includes a pigment, a pH adjuster, a preservative, a thickener, a surfactant, a dispersant, a stabilizer, a coloring agent, a preservative, an antioxidant, an ultraviolet absorber, and a fragrance. And the like can be appropriately compounded within a range that achieves the object of the present invention.

【0020】[0020]

【実施例】以下、実施例によって本発明を更に詳細に説
明する。なお、実用特性の評価については後述の通りで
ある。紫外線防止効果は特開平7−167781記載の
我々が以前開発し、高い精度でSPF値とPFA値が測
定出来るin vitro SPF測定システムを用いた。また、製
剤の透明性については人工皮革に一定量(2.0mg/
cm)塗布し、未塗布部分と共にCM-1000R(ミノルタ
社製)で測色した後、色差(ΔE)を算出した。(ΔE
の値が低い程透明性が高くなる。)製剤の安定性につい
ては経時(50℃、1ヶ月)での粘度を25℃に戻した
後に測定し、官能で確認した。
The present invention will be described in more detail with reference to the following examples. The evaluation of the practical characteristics is as described later. For the effect of preventing ultraviolet rays, an in vitro SPF measurement system described in Japanese Patent Application Laid-Open No. 7-167781, which was previously developed and can measure SPF and PFA values with high accuracy, was used. Also, regarding the transparency of the preparation, a certain amount (2.0 mg /
cm 2 ), and the color difference (ΔE) was calculated after measuring the color with CM-1000R (manufactured by Minolta) together with the uncoated portion. (ΔE
The lower the value, the higher the transparency. ) The stability of the preparation was measured after returning the viscosity over time (50 ° C, 1 month) to 25 ° C and confirmed by sensory evaluation.

【0021】実用特性評価 20名の女性パネラーに試料を塗布し、使用感触及び仕
上りの透明性について評価した。 <評価> 17名以上が良いと回答 ◎ 12〜16名が良いと回答 ○ 9〜11名が良いと回答 △ 5〜8名が良いと回答 × 4名以下が良いと回答 ××
[0021]Evaluation of practical characteristics  Apply the sample to 20 female panelists, feel and use
The climbing transparency was evaluated. <Evaluation> 17 or more respondents are good ◎ 12 to 16 respondents are good ○ 9 to 11 respondents are good △ 5 to 8 respondents are good × 4 or less are good ××

【0022】粉末の表面処理 まず、本発明者らは微粒子酸化亜鉛の表面処理について
検討を行った。本発明にかかる無水ケイ酸で被覆しシリ
コーン処理を施した本発明にかかる実施例1、シリコー
ン処理のみを施した比較例1及びミリスチン酸処理のみ
を施した比較例2の日焼け止め化粧料(W/O型乳化組
成物)を下記表の組成に基づいて調製し、各試験及び評
価を行った。結果を下記表に示す。
[0022]Surface treatment of powder  First, the present inventors described the surface treatment of particulate zinc oxide.
Study was carried out. The silica coated with the silicic acid anhydride according to the present invention
Example 1 according to the present invention subjected to corn treatment, silicon
Comparative Example 1 with only myristic acid treatment and only myristic acid treatment
Sunscreen cosmetic (W / O type emulsified composition)
Product) was prepared based on the composition shown in the table below.
Value. The results are shown in the table below.

【0023】[0023]

【表1】 実施例1 比較例1 比較例2 シクロメチコン 38 38 38 ジメチコン 3 3 3 オクチルメトキシシンナメート 5 5 5 ポリオキシアルキレン変性ポリシロキサン 3 3 3 (ホ゜リオキシアルキレン基15%、平均分子量6000) シリコーンレジン 2 2 2 ベントナイト 1 1 1 抗酸化剤 適量 適量 適量 ジメチコーン処理無水ケイ酸被覆微粒子酸化亜鉛 15 ― ― (シ゛メチコーン3重量%、無水ケイ酸20重量%、微粒子酸化亜鉛平均粒子径0.03μm) ジメチコーン処理微粒子酸化亜鉛 ― 15 ― (シ゛メチコーン7重量%、微粒子酸化亜鉛平均粒子径0.03μm) ミリスチン酸処理微粒子酸化亜鉛 ― ― 15 (ミリスチン酸12重量%、微粒子酸化亜鉛平均粒子径0.03μm) ステアリン酸アルミ処理微粒子酸化チタン 4 4 4 ナイロンパウダー 5 5 5 イオン交感水 to 100 to 100 to 100 グリセリン 5 5 5 ジプロピレングリコール 5 5 5 防腐剤 適量 適量 適量 安定化剤 適量 適量 適量 香料 適量 適量 適量 in vitro SPF値 38.3 28.7 29.2 in vitro PFA値 9.8 6.4 7.2 透明性(ΔE) 3.2 5.8 6.6 使用感触 ◎ △ ○ 仕上りの透明性 ○ △ × 粘度(50℃)初期値 4800 5200 4500 1ヶ月 4900 7400 7700 安定性(50℃、1ヶ月) ◎ △ △ [Table 1]  Example 1 Comparative Example 1 Comparative Example 2  Cyclomethicone 38 38 38 Dimethicone 33 33 Octyl methoxycinnamate 55 55 Polyoxyalkylene-modified polysiloxane 33 33 (polyoxyalkylene group 15%, average molecular weight 6000) Silicone resin 2 2 2 Bentonite 1 1 1 Antioxidant Appropriate amount Appropriate amount Appropriate amount Dimethicone-treated silica-coated fine particle zinc oxide 15 ― ― (Dimethicone 3% by weight, Silicic anhydride 20% by weight, fine particle zinc oxide average particle size 0.03μm) Dimethicone-treated fine particle zinc oxide -15 ― (Dimethicone 7% by weight, Fine particle zinc oxide average particle diameter 0.03 μm) Myristic acid-treated fine particle zinc oxide ― ― 15 (12% by weight of myristic acid, fine particle zinc oxide average particle diameter 0.03 μm) Aluminum stearate-treated fine particle titanium oxide 4 4 4 Nylon powder 5 5 5 ion Sympathetic water to 100 to 100 to 10 0 Glycerin 5 5 5 Dipropylene glycol 5 5 5 Preservatives proper amount proper amount proper amount Stabilizer proper amount proper amount proper amount perfume proper amount proper amount proper amount  in vitro SPF value 38.3 28.7 29.2 in vitro PFA value 9.8 6.4 7.2 Transparency (ΔE) 3.2 5.8 6.6 Tactile feel ◎ △ ○ Finished transparency ○ △ × Viscosity (50 ° C) Initial value 4800 5200 4500 1 month 4900 7400 7700 Stable (50 ° C, 1 month) ◎ △ △

【0024】表1の結果に示されるように、本発明にか
かる無水ケイ酸被覆処理を施し、シリコーン表面処理を
行った微粒子酸化亜鉛を用いた実施例1は、かかる処理
を施さない微粒子酸化亜鉛を用いた比較例1及び比較例
2と比較して、SPF値が高く、紫外線防止効果に優れ
ていることがわかる。また、同様に実施例1はPFA値
が高く、紫外線の中でも特に日焼け止め効果に影響を与
えるUVA(320〜400nm)を防止する効果に優
れていることがわかる。また、本発明にかかる実施例1
は紫外線防止効果に優れるだけでなくΔEが低いことか
ら透明性が高く、仕上がりの透明性にも優れ、使用感触
も良好であることがわかる。また、本発明にかかる実施
例1の日焼け止め化粧料は粘度の経時変化が少なく安定
性に優れていることもわかる。したがって、従来技術に
かかる比較例1、2の微粒子酸化亜鉛の複合表面処理で
は系内の安定性や紫外線防止効果に劣ることがわかる。
As shown in the results of Table 1, Example 1 using the fine particle zinc oxide which had been subjected to the silicic acid anhydride coating treatment according to the present invention and which had been subjected to the silicone surface treatment was the same as the fine particle zinc oxide which was not subjected to such treatment. It can be seen that the SPF value is higher than that of Comparative Example 1 and Comparative Example 2 using No. and the ultraviolet ray preventing effect is excellent. Similarly, it can be seen that Example 1 has a high PFA value and is excellent in the effect of preventing UVA (320 to 400 nm) which particularly affects the sunscreen effect among ultraviolet rays. Example 1 of the present invention
Shows that not only the UV protection effect is excellent but also the ΔE is low, so that the transparency is high, the transparency of the finish is excellent, and the feel in use is good. In addition, it can also be seen that the sunscreen cosmetic of Example 1 according to the present invention has little change with time in viscosity and is excellent in stability. Therefore, it can be seen that the composite surface treatment of the particulate zinc oxide of Comparative Examples 1 and 2 according to the prior art is inferior in the stability in the system and the effect of preventing ultraviolet rays.

【0025】ポリオキシアルキレン変性ポリシロキサン
の特定 つぎに、本発明者らはポリオキシアルキレン変性ポリシ
ロキサンについて検討を行った。本発明にかかる特定の
ポリオキシアルキレン変性ポリシロキサンを配合した実
施例2、ポリオキシアルキレン変性ポリシロキサンのポ
リオキシアルキレン基の割合が低い比較例2、ポリオキ
シアルキレン変性ポリシロキサンの平均分子量が低い比
較例4の日焼け止め化粧料(W/O型乳化組成物)を下
記表の組成に基づいて調製し、各試験及び評価を行っ
た。結果を下記表に示す。
[0025]Polyoxyalkylene-modified polysiloxane
Identification  Next, the present inventors studied the polyoxyalkylene-modified policy.
Loxane was studied. Certain of the present invention
Fruit containing polyoxyalkylene-modified polysiloxane
Example 2, polyoxyalkylene-modified polysiloxane polysiloxane
Comparative Example 2 in which the ratio of a lioxyalkylene group is low,
Low average molecular weight ratio of silalkylene-modified polysiloxane
Under the sunscreen cosmetic (W / O type emulsified composition) of Comparative Example 4
Prepared based on the composition in the table, perform each test and evaluation
Was. The results are shown in the table below.

【0026】[0026]

【表2】 実施例2 比較例3 比較例4 シクロメチコン 30 30 30 ジメチコン 2 2 2 ポリオキシアルキレン変性ポリシロキサン 5 ― ― (ホ゜リオキシアルキレン基20%、平均分子量6200) ポリオキシアルキレン変性ポリシロキサン ― 5 ― (ホ゜リオキシアルキレン基5%、平均分子量3000) ポリオキシアルキレン変性ポリシロキサン ― ― 5 (ホ゜リオキシアルキレン基15%、平均分子量500) シリコーンレジン 1 1 1 抗酸化剤 適量 適量 適量 オクチルメトキシシンナメート 3 3 3 4-tertブチル-4‘-メトキシベンゾイルメタン 1 1 1 イソステアリン酸 1 1 1 シリコーン処理硫酸バリウム 3 3 3 カチオン変性ベントナイト 2 2 2 ジメチコーン処理無水ケイ酸被覆微粒子酸化亜鉛 18 18 18 (シ゛メチコーン3重量%、無水ケイ酸22重量%、微粒子酸化亜鉛平均粒子径0.025μm) タルク 5 5 5 PMMA球状樹脂粉末 5 5 5 イオン交感水 to 100 to 100 to 100 グリセリン 4 4 4 ポリエチレングリコール 1 1 1 防腐剤 適量 適量 適量 安定化剤 適量 適量 適量 香料 適量 適量 適量 in vitro SPF値 27.4 21.4 22.2 in vitro PFA値 8.1 7.2 7.3 透明性(ΔE) 1.8 4.6 4.9 使用感触 ◎ ○ ○ 仕上りの透明性 ◎ △ △ 粘度(50℃)初期値 5600 5200 4700 1ヶ月 5900 5900 5400 安定性(50℃、1ヶ月) ◎ × × [Table 2]  Example 2 Comparative Example 3 Comparative Example 4  Cyclomethicone 30 30 30 Dimethicone 22 2 Polyoxyalkylene-modified polysiloxane 5--(polyoxyalkylene group 20%, average molecular weight 6200) Polyoxyalkylene-modified polysiloxane-5--(polyoxyalkylene group 5%, average molecular weight 3000) ) Polyoxyalkylene-modified polysiloxane--5 (polyoxyalkylene group 15%, average molecular weight 500) Silicone resin 111 Antioxidant appropriate amount appropriate amount appropriate amount octyl methoxycinnamate 33 33 4-tertbutyl-4'-methoxybenzoyl Methane 1 1 1 1 Isostearic acid 1 1 1 1 Silicone treated barium sulfate 3 3 3 Cationic modified bentonite 2 2 2 Dimethicone treated silicic anhydride coated fine particle zinc oxide 18 18 18 (3% by weight dimethicone, 22% by weight silicic anhydride, fine particle zinc oxide Average particle diameter 0.025 .mu.m) Talc 5 5 5 PMMA spherical resin powder 5 5 5 Ion sympathetic water to 100 to 100 to 100 Glycerin 4 4 4 Polyethylene glycol 1 1 1 Preservative qs qs qs stabilizers qs qs qs Perfume qs qs qs  in vitro SPF value 27.4 21.4 22.2 in vitro PFA value 8.1 7.2 7.3 Transparency (ΔE) 1.8 4.6 4.9 Feeling of use ◎ ○ ○ Finished transparency ◎ △ △ Viscosity (50 ° C) Initial value 5600 5200 4700 1 month 5900 5900 5400 Stable (50 ° C, 1 month) ◎ × ×

【0027】表2の結果に示されるように、本発明にか
かる特定のポリオキシアルキレン変性ポリシロキサンを
用いた実施例2は、特定外のポリオキシアルキレン変性
ポリシロキサンを用いた比較例3及び比較例4と比較し
て、SPF値が高く、紫外線防止効果に優れていること
がわかる。また、同様に実施例2はPFA値が高く、紫
外線の中でも特に日焼け止め効果に影響を与えるUVA
(320〜400nm)を防止する効果に優れているこ
とがわかる。また、本発明にかかる実施例2は紫外線防
止効果に優れるだけでなくΔEが低いことから透明性が
高く、仕上がりの透明性にも優れ、使用感触も良好であ
ることがわかる。また、本発明にかかる実施例2の日焼
け止め化粧料は粘度の経時変化が少なく安定性に優れて
いることもわかる。したがって、比較例3、4からポリ
オキシアルキレン変性ポリシロキサンのポリオキシレン
基と分子量によって分散不良や乳化安定性が悪化するこ
とがわかる。
As shown in the results of Table 2, Example 2 using the specific polyoxyalkylene-modified polysiloxane according to the present invention was compared with Comparative Example 3 using a non-specific polyoxyalkylene-modified polysiloxane. Compared with Example 4, it is understood that the SPF value is higher and the ultraviolet ray preventing effect is excellent. Similarly, Example 2 has a high PFA value, and UVA which particularly affects the sunscreen effect among ultraviolet rays.
(320 to 400 nm). In addition, it can be seen that Example 2 according to the present invention is not only excellent in the effect of preventing ultraviolet rays but also has a low ΔE, so that the transparency is high, the finished transparency is excellent, and the use feeling is good. In addition, it can also be seen that the sunscreen cosmetic of Example 2 according to the present invention has little change in viscosity over time and is excellent in stability. Therefore, it can be seen from Comparative Examples 3 and 4 that poor dispersion and poor emulsion stability are caused by the polyoxylene group and the molecular weight of the polyoxyalkylene-modified polysiloxane.

【0028】界面活性剤の検討 つぎに、本発明者らは無水ケイ酸を被覆しシリコーン処
理をした微粒子酸化亜鉛を分散させる界面活性剤につい
てポリオキシアルキレン変性ポリシロキサン以外のもの
で検討を行った。本発明にかかる特定のポリオキシアル
キレン変性ポリシロキサンを配合した実施例3、グリセ
ルモノステアリン酸を配合した比較例5、ソルビタンジ
ステアリン酸エステルを配合した比較例6の日焼け止め
化粧料(W/O型乳化組成物)を下記表の組成に基づい
て調製し、各試験及び評価を行った。結果を下記表に示
す。
[0028]Examination of surfactant  Next, we coated the silicic anhydride and treated it with silicone.
Surfactants that disperse treated zinc oxide
Other than polyoxyalkylene-modified polysiloxane
Was examined. Specific polyoxyal according to the present invention
Example 3 in which a kilen-modified polysiloxane was blended,
Comparative Example 5 containing Lumonostearic acid, sorbitandi
Sunscreen of Comparative Example 6 containing stearic acid ester
Cosmetics (W / O type emulsified composition) based on the composition in the table below
Each test and evaluation were performed. The results are shown in the table below
You.

【0029】[0029]

【表3】 実施例3 比較例5 比較例6 シクロメチコン 30 30 30 ジメチコン 5 5 5 ポリオキシアルキレン変性ポリシロキサン 4 ― ― (ホ゜リオキシアルキレン基20%、平均分子量6200) グリセルモノステアリン酸エステル ― 4 ― (ホ゜リオキシエチレン25モル) ソルビタンジステアリン酸エステル ― ― 4 シリコーンレジン 1 1 1 抗酸化剤 適量 適量 適量 オクチルメトキシシンナメート 3 3 3 モノオレイン酸エステル 1.5 1.5 1.5 カチオン変性ベントナイト 2 2 2 ジメチコーン処理無水ケイ酸被覆微粒子酸化亜鉛 17 17 17 (シ゛メチコーン5重量%、無水ケイ酸10重量%、微粒子酸化亜鉛平均粒子径0.02μm) ミリスチン酸カルシウム処理タルク 5 5 5 PMMA球状樹脂粉末 5 5 5 イオン交感水 to 100 to 100 to 100 グリセリン 4 4 4 ポリエチレングリコール 1 1 1 防腐剤 適量 適量 適量 安定化剤 適量 適量 適量 香料 適量 適量 適量 in vitro SPF値 29.2 17.9 18.1 in vitro PFA値 7.2 5.4 4.9 透明性(ΔE) 2.0 4.2 4.5 使用感触 ◎ △ △ 仕上りの透明性 ◎ △ △ 粘度(50℃)初期値 5700 4900 5100 1ヶ月 5900 5100 5500 安定性(50℃、1ヶ月) ◎ △ △ [Table 3]  Example 3 Comparative Example 5 Comparative Example 6  Cyclomethicone 30 30 30 Dimethicone 55 5 5 Polyoxyalkylene-modified polysiloxane 4---(polyoxyalkylene group 20%, average molecular weight 6200) Glyceryl monostearate-4-(Polyoxyethylene 25 mol) Sorbitan distearate- -4 Silicone resin 1 1 1 1 Antioxidant appropriate amount appropriate amount appropriate amount octyl methoxycinnamate 3 3 3 monooleate 1.5 1.5 1.5 1.5 cation-modified bentonite 2 2 2 Dimethicone-treated silica-coated microparticles zinc oxide 17 17 17 (dimethicone 5% by weight, silicic acid anhydride 10% by weight, fine zinc oxide average particle diameter 0.02 μm) Calcium myristate-treated talc 5 5 5 PMMA spherical resin powder 5 5 5 Ion-interactive water to 100 to 100 to 100 4 poly Ethylene glycol 1 1 1 Preservative proper amount proper amount proper amount stabilizer proper amount proper amount proper amount perfume proper amount proper amount proper amount  in vitro SPF value 29.2 17.9 18.1 in vitro PFA value 7.2 5.4 4.9 Transparency (ΔE) 2.0 4.2 4.5 Usage feel ◎ △ △ Finished transparency ◎ △ △ Viscosity (50 ° C) Initial value 5700 4900 5100 1 month 5900 5100 5500 Stable (50 ° C, 1 month) ◎ △ △

【0030】表3の結果に示されるように、本発明にか
かる特定のポリオキシアルキレン変性ポリシロキサンを
用いた実施例3は、他の界面活性剤を用いた比較例5及
び比較例6と比較して、粉末の分散性が良好となるため
SPF値が高く、紫外線防止効果に優れていることがわ
かる。また、同様に実施例2はPFA値が高く、紫外線
の中でも特に日焼け止め効果に影響を与えるUVA(3
20〜400nm)を防止する効果に優れていることが
わかる。また、本発明にかかる実施例3は紫外線防止効
果に優れるだけでなくΔEが低いことから透明性が高
く、仕上がりの透明性にも優れ、使用感触も良好である
ことがわかる。また、本発明にかかる実施例3の日焼け
止め化粧料は粘度の経時変化が少なく安定性に優れてい
ることもわかる。したがって、従来技術にかかる比較例
5、6からポリオキシアルキレン変性ポリシロキサン以
外の界面活性剤との組合せでは粉末の分散性が悪く紫外
線効果や透明性の点で劣ることがわかる。
As shown in the results in Table 3, Example 3 using the specific polyoxyalkylene-modified polysiloxane according to the present invention was compared with Comparative Examples 5 and 6 using other surfactants. As a result, the dispersibility of the powder becomes good, so that the SPF value is high, and it can be seen that the ultraviolet ray prevention effect is excellent. Similarly, Example 2 has a high PFA value, and UVA (3) which particularly affects the sunscreen effect among ultraviolet rays.
20 to 400 nm). In addition, it can be seen that Example 3 according to the present invention is not only excellent in the effect of preventing ultraviolet rays, but also has a low ΔE, and thus has high transparency, excellent finish transparency, and good use feeling. In addition, it can also be seen that the sunscreen cosmetic of Example 3 according to the present invention has little change over time in viscosity and is excellent in stability. Therefore, it can be seen from Comparative Examples 5 and 6 according to the prior art that the combination with a surfactant other than the polyoxyalkylene-modified polysiloxane results in poor powder dispersibility and poor ultraviolet light effect and transparency.

【0031】微粒子酸化亜鉛に無水ケイ酸を被覆しシリ
コーン表面処理した複合粉末の配合量 つぎに微粒子酸化亜鉛に無水ケイ酸を被覆しシリコーン
表面処理した複合粉末の配合量について検討した。実施
例3の組成のうち、微粒子酸化亜鉛に無水ケイ酸を被覆
しシリコーン表面処理した複合粉末の配合量を変化させ
た下記表の組成の日焼け止め化粧料を調製し、紫外線防
止効果、使用感触、仕上りの透明性及び安定性について
評価を行った。試験及び評価は前記の通りであるが、紫
外線防止効果については、下記の評価基準にしたがっ
た。
[0031]Silicic acid is coated on fine zinc oxide
Compounding amount of composite powder treated with corn surface  Next, silica oxide is coated on fine zinc oxide
The mixing amount of the surface-treated composite powder was examined. Implementation
In the composition of Example 3, fine zinc oxide was coated with silicic anhydride.
The amount of the composite powder treated with silicone
A sunscreen cosmetic having the composition shown in the following table was prepared and
About stopping effect, feeling of use, transparency and stability of finish
An evaluation was performed. Tests and evaluations are as described above, but purple
For the effect of preventing outside lines, follow the evaluation criteria below.
Was.

【0032】<紫外線防止効果>微粒子酸化亜鉛に無水
ケイ酸を被覆しシリコーン表面処理した複合粉末を配合
しない組成物を調製し、試験例の組成物とin vitro S
PF値、in vitro PFA値の比較を行った。評価基準
は下記の通りである。 in vitro SPF値が8以上、in vitro PFA値が5以上の上昇が認められた ◎ in vitro SPF値が4以上、in vitro PFA値が2以上の上昇が認められた ○ in vitro SPF値が1以上〜4未満、in vitro PFA値が1以上2未満の上昇が認め られた △ in vitro SPF値、in vitro PFA値の上昇が全く認められなかった ×
<Ultraviolet ray preventive effect> A composition was prepared in which a composite powder obtained by coating fine particle zinc oxide with silicic acid anhydride and treating it with a silicone surface was not blended.
The PF value and the in vitro PFA value were compared. The evaluation criteria are as follows. Increase of in vitro SPF value of 8 or more and increase of in vitro PFA value of 5 or more were observed. ◎ Increase of in vitro SPF value of 4 or more and increase of in vitro PFA value of 2 or more were observed. ○ In vitro SPF value of 1 No less than 4 and less than 4, an increase in in vitro PFA value of 1 or more and less than 2 was observed △ No increase in in vitro SPF value or in vitro PFA value was observed ×

【0033】[0033]

【表4】 試験例 試験例 試験例 試験例 1 2 3 4 シクロメチコン 30 30 30 30 ジメチコン 5 5 5 5 ポリオキシアルキレン変性ポリシロキサン 4 4 4 4 (ホ゜リオキシアルキレン基20%、平均分子量6200) シリコーンレジン 1 1 1 1 抗酸化剤 適量 適量 適量 適量 オクチルメトキシシンナメート 3 3 3 3 モノオレイン酸エステル 1.5 1.5 1.5 1.5 カチオン変性ベントナイト 2 2 2 2シ゛メチコーン 処理無水ケイ酸被覆微粒子酸化亜鉛 3 10 23 30 (シ゛メチコーン5重量%、無水ケイ酸10重量%、微粒子酸化亜鉛平均粒子径0.02μm) ミリスチン酸カルシウム処理タルク 5 5 5 5 PMMA球状樹脂粉末 5 5 5 5 イオン交感水 to 100 to 100 to 100 to 100 グリセリン 4 4 4 4 ポリエチレングリコール 1 1 1 1 防腐剤 適量 適量 適量 適量 安定化剤 適量 適量 適量 適量 香料 適量 適量 適量 適量 紫外線防止効果 △ ○ ◎ ◎ 使用感触 ◎ ◎ ○ △ 仕上りの透明性 ◎ ◎ ○ △ 安定性 (1ヶ月) ◎ ◎ ◎ ○ [Table 4]  Test example Test example Test example Test example 1 2 3 4  Cyclomethicone 30 30 30 30 Dimethicone 5.5 5 5 Polyoxyalkylene-modified polysiloxane 4 4 4 4 (polyoxyalkylene group 20%, average molecular weight 6200) Silicone resin 11 1 1 Antioxidant proper amount proper amount proper amount octyl methoxycinnamate 3 3 3 3 Monooleate 1.5 1.5 1.5 1.5 1.5 Cation-modified bentonite 222 2 Dimethicone Treated silicic acid-coated fine particle zinc oxide 3 10 23 30 (Dimethicone 5% by weight, Silicic anhydride 10 Weight%, fine zinc oxide average particle diameter 0.02 μm) Calcium myristate-treated talc 5.55 5 PMMA spherical resin powder 5 5 5 5 ionized water to 100 to 100 to 100 to 100 glycerin 4 4 4 4 polyethylene glycol 11 1 1 1 Preservatives Appropriate amount Appropriate amount Appropriate amount Appropriate amount Stabilizer Appropriate amount Appropriate Amount Appropriate amount Appropriate amount Fragrance Appropriate amount Appropriate amount Appropriate amount Appropriate amount  UV protection effect △ ○ ◎ ◎ Feeling in use ◎ ◎ ○ △ Finish transparency ◎ ◎ ○ △ Stability (1 month) ◎ ◎ ◎ ○

【0034】表4の結果より、本発明にかかる微粒子酸
化亜鉛に無水ケイ酸を5重量%以上30重量%以下で被
覆し、さらにシリコーンを3重量%以上12重量%以下
で表面処理した複合粉末の配合量は3〜30重量%で好
適に用いられることがわかる。
From the results shown in Table 4, the composite powder obtained by coating the fine particle zinc oxide according to the present invention with silicic acid in an amount of 5% by weight to 30% by weight and further surface-treating silicone with 3% by weight to 12% by weight. It can be understood that the compounding amount of 3 to 30% by weight is suitably used.

【0035】特定ポリオキシアルキレン変性ポリシロキ
サンの配合量 つぎに特定ポリオキシアルキレン変性ポリシロキサンの
配合量について検討した。実施例1の組成のうち、特定
ポリオキシアルキレン変性ポリシロキサンの配合量を変
化させた下記表の組成の日焼け止め化粧料を調製し、紫
外線防止効果、使用感触、仕上りの透明性及び安定性に
ついて評価を行った。試験及び評価は前記の通りであ
る。
[0035]Specific polyoxyalkylene-modified polysiloxane
Sun content  Next, the specific polyoxyalkylene-modified polysiloxane
The mixing amount was examined. Specific of the composition of Example 1
Change the amount of polyoxyalkylene-modified polysiloxane
Prepared sunscreen cosmetics of the composition shown in the following table,
Outer line prevention effect, feeling of use, transparency and stability of finish
About it. The tests and evaluations are as described above.
You.

【0036】[0036]

【表5】 試験例5 試験例6 試験例7 シクロメチコン 38 38 38 ジメチコン 3 3 3 オクチルメトキシシンナメート 5 5 5 ポリオキシアルキレン変性ポリシロキサン 0.5 3 7 (ホ゜リオキシアルキレン基15%、平均分子量6000) シリコーンレジン 2 2 2 ベントナイト 1 1 1 抗酸化剤 適量 適量 適量 ジメチコーン処理無水ケイ酸被覆微粒子酸化亜鉛 3 10 30 (シ゛メチコーン3重量%、無水ケイ酸20重量%、微粒子酸化亜鉛平均粒子径0.03μm) ステアリン酸アルミ処理微粒子酸化チタン 4 4 4 ナイロンパウダー 5 5 5 イオン交感水 to 100 to 100 to 100 グリセリン 5 5 5 ジプロピレングリコール 5 5 5 防腐剤 適量 適量 適量 安定化剤 適量 適量 適量 香料 適量 適量 適量 紫外線防止効果 ○ ◎ ◎ 使用感触 ◎ ◎ ○ 仕上りの透明性 ○ ◎ ◎ 安定性(1ヶ月) ○ ◎ ◎ [Table 5]  Test Example 5 Test Example 6 Test Example 7  Cyclomethicone 38 38 38 Dimethicone 33 33 Octylmethoxycinnamate 55 55 Polyoxyalkylene-modified polysiloxane 0.537 (polyoxyalkylene group 15%, average molecular weight 6000) Silicone resin 2 2 2 Bentonite 1 1 1 1 Antioxidation Agent Suitable amount Suitable amount Suitable amount Dimethicone-treated silica-coated fine particle zinc oxide 3 10 30 (dimethicone 3% by weight, silicic anhydride 20% by weight, fine particle zinc oxide average particle size 0.03 μm) Aluminum stearate-treated fine particle titanium oxide 4 4 4 Nylon powder 55 5 5 Ion-sympathetic water to 100 to 100 to 100 Glycerin 5 5 5 Dipropylene glycol 5 5 5  UV protection effect ○ ◎ ◎ Feeling of use ◎ ◎ ○ Transparency of finish ○ ◎ ◎ Stability (1 month) ○ ◎ ◎

【0037】表5の結果より、本発明にかかる特定ポリ
オキシアルキレン変性ポリシロキサンの配合量は0.5
〜7重量%で好適に用いられることがわかる。
From the results shown in Table 5, the amount of the specific polyoxyalkylene-modified polysiloxane according to the present invention was 0.5%.
It can be seen that it is suitably used at 77% by weight.

【0038】[0038]

【発明の効果】以上記載のごとく、本発明にかかる日焼
け止め化粧料は0.1μm以下の微粒子酸化亜鉛に無水
ケイ酸を被覆率5重量%以上30重量%以下で被覆し、
さらにシリコーンを3重量%以上12重量%以下で表面
処理した複合粉末と特定のポリオキシアルキレン変性ポ
リシロキサンから選ばれる1種または2種以上とを配合
したので、SPF値やPFA値などの紫外線防止効果と
仕上りの透明性又は系内の安定性にも優れたものとする
ことができる。
As described above, the sunscreen cosmetic according to the present invention is obtained by coating fine particle zinc oxide of 0.1 μm or less with silicic anhydride at a coverage of 5% by weight or more and 30% by weight or less,
Furthermore, since a composite powder obtained by surface-treating silicone at 3% by weight or more and 12% by weight or less and one or more kinds selected from specific polyoxyalkylene-modified polysiloxanes are blended, ultraviolet rays such as SPF value and PFA value are prevented. The effect and the transparency of the finish or the stability in the system can be excellent.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 大野 和久 神奈川県横浜市港北区新羽町1050番地 株 式会社資生堂第一リサーチセンター内 Fターム(参考) 4C083 AB052 AB171 AB211 AB212 AB442 AC122 AC241 AC342 AC351 AC352 AD072 AD151 AD152 AD161 AD162 AD172 CC19 EE17  ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Kazuhisa Ohno 1050 Nippa-cho, Kohoku-ku, Yokohama-shi, Kanagawa Prefecture F-term in Shiseido Daiichi Research Center 4C083 AB052 AB171 AB211 AB212 AB442 AC122 AC241 AC342 AC351 AC352 AD072 AD151 AD152 AD161 AD162 AD172 CC19 EE17

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 0.1μm以下の微粒子酸化亜鉛に無水
ケイ酸を被覆率5重量%以上30重量%以下で被覆し、
さらにシリコーンを3重量%以上12重量%以下で表面
処理した複合粉末と、 下記一般式[1][2]または[3]に示したポリオキ
シアルキレン変性ポリシロキサンから選ばれる1種また
は2種以上とを配合することを特徴とする日焼け止め化
粧料。 【化1】 【化2】 【化3】 (ただし、一般式[1][2][3]中、Rはメチル基
または一部がフェニル基、Rは水素または炭素数1〜1
2のアルキル基、pは1〜5の数、qは2〜3の数、
x、m、nは平均数でポリオキシアルキレン変性オルガ
ノポリシロキサンが分子中にポリオキシアルキレン基を
5〜40重量%含有し且つ該ポリオキシアルキレン変性
オルガノポリシロキサンの分子量が2000以上になるよう
な数値を表わす。)
Claims: 1. A fine particle zinc oxide having a particle size of 0.1 μm or less is coated with silicic anhydride at a coverage of 5% by weight or more and 30% by weight or less,
Further, a composite powder obtained by surface-treating silicone at 3% by weight or more and 12% by weight or less, and one or more kinds selected from polyoxyalkylene-modified polysiloxanes represented by the following general formula [1] [2] or [3] A sunscreen cosmetic characterized by containing Embedded image Embedded image Embedded image (However, in the general formulas [1], [2] and [3], R is a methyl group or a partially phenyl group, R is hydrogen or a carbon atom having 1 to 1 carbon atoms.
2 is an alkyl group, p is a number of 1 to 5, q is a number of 2 to 3,
x, m, and n are average numbers such that the polyoxyalkylene-modified organopolysiloxane contains 5 to 40% by weight of a polyoxyalkylene group in the molecule and the molecular weight of the polyoxyalkylene-modified organopolysiloxane becomes 2000 or more. Indicates a numerical value. )
【請求項2】 請求項1記載の化粧料において、無水ケ
イ酸とシリコーンで処理された微粒子酸化亜鉛の複合粉
末を3重量%以上30重量%以下配合し、ポリオキシア
ルキレン変性ポリシロキサンを0.5重量%以上7重量
%以下配合することを特徴とする日焼け止め化粧料。
2. The cosmetic according to claim 1, wherein a composite powder of finely divided zinc oxide treated with silicic anhydride and silicone is mixed in an amount of 3% by weight or more and 30% by weight or less, and the polyoxyalkylene-modified polysiloxane is added in an amount of 0.1% by weight or less. A sunscreen cosmetic comprising 5% by weight or more and 7% by weight or less.
【請求項3】 請求項1または2に記載の化粧料におい
て、さらに脂肪酸及び脂肪酸セッケン、脂肪酸エステル
を0.1重量%以上配合し、脂肪酸及び脂肪酸セッケ
ン、脂肪酸エステルで表面処理した粉末を1重量%以上
配合することを特徴とする日焼け止め化粧料。
3. The cosmetic according to claim 1, further comprising 0.1% by weight or more of a fatty acid, a fatty acid soap and a fatty acid ester, and 1% by weight of a powder surface-treated with the fatty acid, the fatty acid soap and the fatty acid ester. % Sunscreen cosmetic.
JP23283299A 1999-08-19 1999-08-19 Sunscreen cosmetics Expired - Lifetime JP4011799B2 (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
JP23283299A JP4011799B2 (en) 1999-08-19 1999-08-19 Sunscreen cosmetics
US09/807,750 US6749838B1 (en) 1999-08-19 2000-08-18 Cosmetic sunscreen preparation
EP00953503A EP1123697A1 (en) 1999-08-19 2000-08-18 Cosmetic sunscreen preparation
AU65961/00A AU775971B2 (en) 1999-08-19 2000-08-18 Cosmetic sunscreen preparation
PCT/JP2000/005547 WO2001013874A1 (en) 1999-08-19 2000-08-18 Cosmetic sunscreen preparation
KR1020017004871A KR100849404B1 (en) 1999-08-19 2000-08-18 Cosmetic sunscreen preparation
CNB008017425A CN100369601C (en) 1999-08-19 2000-08-18 Cosmetic sunscreen prpearation
TW089116871A TWI231217B (en) 1999-08-19 2000-08-19 Sun screen cosmetic comprising micro particle zinc oxide

Applications Claiming Priority (1)

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US8728503B2 (en) 2009-11-06 2014-05-20 Kao Corporation Emulsion cosmetic
EP2918260A1 (en) 2009-11-06 2015-09-16 Kao Corporation UV screening emulsifiedcomposition comprising surface treated zinc oxide
JP2012240995A (en) * 2011-05-24 2012-12-10 Sakai Chem Ind Co Ltd Zinc oxide dispersion and cosmetic
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