JP3876521B2 - Ultraviolet shielding fine powder composition and use thereof - Google Patents
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【０００１】
【発明の属する技術分野】
本発明は、紫外線遮蔽性微粉体組成物に関し、詳しくは、合成層状ポリケイ酸又はその塩の表面に無機酸化物微粒子を付着させ、複合化してなる紫外線遮蔽性微粉体組成物とその用途、特に、化粧料及び塗料に関する。
【０００２】
【従来の技術】
従来、化粧料には、着色の目的のほか、紫外線遮蔽を目的として、酸化チタン、酸化亜鉛、酸化ジルコニウム等、種々の無機酸化物微粒子が配合されている。しかし、従来、このように無機酸化物微粒子を配合した化粧料は、その無機微粒子の有する特性、特に、表面の物理的、化学的性状のほか、粒子径や形状等にも起因して、種々の問題を有している。例えば、酸化チタン微粒子を紫外線散乱剤として配合する場合、酸化チタン微粒子自体が一次粒子の凝集体であるので、例えば、パウダー状の化粧料中に均一に分散させることが困難であり、従って、その紫外線遮蔽効果を有効に発揮させることができない。他方、酸化亜鉛微粒子は、一般に、伸展性がよくなく、これを配合した化粧料も、伸展性が低下し、肌の上での伸びが悪い。
【０００３】
そこで、このような問題を解決するために、従来、薄片状の微粉基体にそのような無機酸化物微粒子を付着乃至担持させてなる紫外線遮蔽性微粉体組成物が種々提案されている。例えば、劈開セリサイトのような薄片状微粉基体と紫外線散乱剤である酸化チタン微粒子を乾式混合し、粉砕して、上記薄片状微粉基体に酸化チタン微粒子を吸着させてなる粉体化粧料が特開平６−９３３７号公報に記載されている。
【０００４】
他方、雲母、タルク、シリカ等からなる薄片状の微粉基体に酸化チタンを湿式法にて担持させてなる微粉体組成物が特開平９−１３２５１４号公報に記載されている。同様に、雲母等の薄片状の微粉基体と酸化亜鉛微粒子とを湿式処理し、微粉基体を酸化亜鉛微粒子で被覆してなる微粉体組成物からなる脂肪酸固化性微粉体も、特開平９−２２７７９２号公報に記載されている。
【０００５】
しかしながら、従来より知られている上述したような微粉体組成物、特に、酸化チタンや酸化亜鉛の微粒子を紫外線散乱剤として微粉基体に付着させてなる微粉体組成物によれば、実用的な紫外線遮蔽効果を得るには、多量の酸化チタンや酸化亜鉛の微粒子を基体に付着させる必要があるが、そのように多量の無機酸化物微粒子を微粉体基体に均一に付着させることは容易ではない。かくして、従来、多量の無機酸化物微粒子を微粉基体に付着させた微粉体組成物は、例えば、化粧料への分散性に劣る問題があり、更に、化粧料に配合した場合、透明性や伸展性が十分ではない問題がある。
【０００６】
【発明が解決しようとする課題】
本発明は、従来の紫外線遮蔽性微粉体組成物における上述したような問題を解決するためになされたものであって、薄片状微粉基体に無機微粒子が均一に付着しており、紫外線遮蔽効果にすぐれると共に、化粧料や塗料への分散性にもすぐれる紫外線遮蔽性微粉体組成物を提供することを目的とする。
【０００７】
【課題を解決するための手段】
本発明による紫外線遮蔽性微粉体組成物は、合成層状ポリケイ酸又はその塩からなる薄片状微粉基体の表面に無機酸化物微粒子を付着させてなることを特徴とする。
【０００８】
本発明による紫外線遮蔽性微粉体組成物においては、好ましくは、上記合成層状ポリケイ酸又はその塩からなる薄片状微粉基体は、一辺が１〜１０μｍの範囲にある四角形状を有する薄片であり、その表面に０．０１〜０．５μｍの範囲の粒子径を有する無機酸化物微粒子が１〜３０重量％の割合で付着されてなるものである。
【０００９】
【発明の実施の形態】
本発明による紫外線遮蔽性微粉体組成物は、合成層状ポリケイ酸又はその塩からなる薄片状微粉基体の表面に無機酸化物微粒子を付着させてなる。合成層状ポリケイ酸塩は、「ゼオライト」第１３巻第３号第８９〜９６頁（１９９６年）に記載されているように、層格子がＳｉＯ４四面体のみからなり、代表例として、アイラアイトが知られている。
【００１０】
アイラアイトの合成方法は、例えば、特開平９−２２７１１６号公報に記載されている。例えば、水ガラスを水熱反応に付すことによって、ナトリウム型アイラアイト（層状ポリケイ酸塩）を得をことができ、これを塩酸で処理すれば、水素（Ｈ）型アイラアイト（層状ポリケイ酸）を得ることができる。
【００１１】
本発明によれば、このように、微粉基体として、合成層状ポリケイ酸又はその塩を用いる。ここに、塩としては、ナトリウム塩のほか、カルシウム塩やマグネシウム塩を例示することができる。しかし、本発明によれば、紫外線遮蔽性微粉体組成物を化粧料に配合する場合には、微粉基体としては、Ｈ型アイラアイトを用いることが好ましい。
【００１２】
本発明によれば、合成層状ポリケイ酸又はその塩からなる薄片状微粉基体は、一辺が１〜１０μｍの範囲にある四角形状を有する薄片であるのが好ましい。厚みは、通常、０．００５〜０．１μｍの範囲である。本発明によれば、微粉基体として、このように、合成層状ポリケイ酸又はその塩は、合成品である故に、純度、大きさ等の揃ったものを用いることができ、かくして、微粉基体に単層に、しかも、均一に付着させることができる。
【００１３】
本発明において、無機酸化物微粒子としては、紫外線を散乱し、又は吸収する等によって、紫外線を遮蔽する性質を有するものであれば、特に、限定されるものではないが、好ましくは、酸化亜鉛、酸化チタン、酸化第二鉄、酸化セリウム、二酸化ケイ素、酸化ジルコニウム、酸化タングステン及び酸化スズから選ばれる少なくとも１種が用いられる。これらのなかでは、特に、酸化亜鉛又は酸化チタンの微粒子が好ましく用いられる。本発明においては、これら無機酸化物微粒子は、通常、０．０１〜０．５μｍの範囲の粒子径を有しており、好ましくは、０．０１〜０．２μｍの範囲の粒子径を有する。
【００１４】
本発明によれば、薄片状微粉基体への上記無機酸化物微粒子の付着量は、１〜３０重量％の範囲であり、好ましくは、３〜２０重量％の範囲であり、特に好ましくは、５〜１５重量％の範囲である。
【００１５】
本発明による紫外線遮蔽性微粉体組成物は、薄片状微粉基体と無機微粒子とを強力な攪拌装置を用いて混合攪拌することによって得ることができるが、好ましくは、薄片状微粉基体と無機微粒子との混合物に瞬間的に同時に大きい圧縮力と剪断力を繰り返して与える所謂機械的複合化処理することによって得ることができる。このような機械的複合化処理自体は、例えば、特開平９−５９０１５号公報に記載されているように、既に知られており、一般に、粒子複合化装置として知られている装置を用いることによって行なうことができる。そのような装置として、例えば、メカノフュージョンシステム（ホソカワミクロン株式会社製）、シータ・コンポーザ（株式会社徳寿工作所製）等を挙げることができる。
【００１６】
必要ならば、透明性を改善することを目的として、得られた微粉体組成物を空気のような酸化性雰囲気中、３００〜６００℃、好ましくは、３００〜５００℃以下の温度で焼成してもよい。
【００１７】
本発明による微粉体組成物は、以上のように、合成層状ポリケイ酸又はその塩からなる薄片状微粉基体と無機酸化物微粒子との混合物に瞬間的に同時に大きい圧縮力と剪断力を繰り返して与える所謂機械的複合化処理することによって、基体の表面に実質的に単層に且つ均一に無機酸化物微粒子を付着させてなるものであり、従って、薄片状微粉基体に対して、多量の無機微粒子を配合せずとも、高い紫外線遮蔽効果を有する。
【００１８】
しかも、本発明による紫外線遮蔽性微粉体組成物は、粉体組成物における分散性にすぐれるのみならず、伸展性、透明性にもすぐれるので、化粧料における紫外線遮蔽剤として有用である。
【００１９】
かくして、本発明による微粉体組成物を通常の化粧料に配合することによって、紫外線遮蔽性にすぐれる化粧料を得ることができる。本発明による微粉体組成物は、粉体組成物におけるすぐれた分散性を利用して、粉末状化粧料に有利に配合することができるが、しかし、ケーキ状、ペンシル状、スティック状、液状、乳液状、クリーム状等、任意の形態の化粧料に配合してもよい。
【００２０】
また、本発明による紫外線遮蔽性微粉体組成物は、水性、油性いずれの塗料においても、分散性と安定性にすぐれており、従って、紫外線遮蔽性塗料における紫外線遮蔽剤として有用であり、本発明による微粉体組成物を配合した塗料は、紫外線遮蔽効果を有するものとして有用である。
【００２１】
【発明の効果】
以上のように、本発明による紫外線遮蔽性微粉体組成物は、合成層状ポリケイ酸又はその塩からなる薄片状微粉基体に酸化チタンや酸化亜鉛等の無機酸化物微粒子を単層に均一に付着させ、複合化してなり、紫外線遮蔽効果にすぐれるのみならず、分散性、伸展性、透明性にもすぐれ、化粧料や塗料における紫外線遮蔽剤として有用である。
【００２２】
【実施例】
以下に実施例を挙げて本発明を説明するが、本発明はこれら実施例により何ら限定されるものではない。
【００２３】
参考例１
ＳｉＯ２が２３．３重量％、Ｎａ２Ｏが６．２重量％（ＮａＯＨ／ＳｉＯ２モル比＝０．５１／１．０）からなる水ガラス（４号ケイ酸ナトリウム）７００ｇを１Ｌ容量オートクレーブ中、１０７℃の水熱条件下に２８０時間処理した。反応終了後、濾別し、固相を分離し、水洗し、８０℃で一昼夜乾燥させて、ナトリウム型アイラアイト（層状ポリケイ酸塩）を得た。得られた反応生成物がナトリウム型アイラアイト（層状ポリケイ酸塩）であることは、Ｘ線回折パターンにて確認した。
【００２４】
このナトリウム型アイラアイトを塩酸処理して、ナトリウムが０．３％以下であるＨ型アイラアイト（層状ポリケイ酸）を得た。このＨ型アイラアイトを試料１とし、図１に透過型電子顕微鏡写真を示し、図２にそのＸ線回折パターンを示す。
【００２５】
実施例１
参考例１で得られたＨ型アイラアイト（平均で縦３μｍ、横３．５μｍ、厚み０．０５μｍ）９４重量部と平均粒子径０．０２μｍの酸化亜鉛微粒子（堺化学工業株式会社製ＦＩＮＥＸ−５０）６重量部とをシータ・コンポーザ（株式会社徳寿工作所製）に仕込み、乾式混合して、Ｈ型アイラアイトの表面に酸化亜鉛微粒子を付着させ、複合化してなる酸化亜鉛付着量６重量％の微粉体組成物を得た。この微粉体組成物を試料２とし、その走査型電子顕微鏡写真を図３に示す。
【００２６】
また、上記微粉体組成物を空気中、５００℃で２時間、焼成した。これを試料４とする。
【００２７】
実施例２
実施例１において、酸化亜鉛付着量を８重量％とした以外は、同様にして、微粉体組成物を得た。これを試料３とし、その走査型電子顕微鏡写真を図４に示す。これを空気中、５００℃で２時間、焼成したものを試料５とする。
【００２８】
以上の試料２〜５のそれぞれ０．６０重量部と白色ワセリン（小堺製薬株式会社製）２．４０重量部とを樹脂板上で木へらを用いて混練してペーストを調製した。このペーストを２枚の石英ガラスの間に厚み２８μｍとなるように挟み、日本分光株式会社製Ｖ−５５０型分光光度計で光透過率を測定した。また、実施例１及び２において、微粉体組成物を調製するために用いた酸化亜鉛微粒子自体を試料６とし、その０．０５重量部と白色ワセリン２．９５重量部とを同様に混練し、ペーストとして、光透過率を測定した。結果を図５及び図６に示す。
【００２９】
酸化亜鉛微粒子を８重量％配合した微粉体組成物、試料３は、ペースト中の酸化亜鉛濃度は、試料６（酸化亜鉛微粒子のみ）と同じであるが、中紫外線（２９０〜３２０ｎｍ、Ｂ領域）と近紫外線（３２０〜４００ｎｍ、Ａ領域）領域において、試料６よりも、紫外線遮蔽効果が高く、ペースト中における酸化亜鉛微粒子が分散性にすぐれることが示される。しかも、可視光領域（４００〜８００ｎｍ）においては、試料３は、試料６よりも、光透過率が高く、透明性にすぐれることが示される。試料の焼成品である試料５についても、同様である。
【００３０】
試料２の微粉体組成物中の酸化亜鉛微粒子量は６重量％であり、紫外線領域における光透過率は、試料６とほぼ同等であるが、試料６よりも可視光領域における透明性が高い。
【００３１】
また、焼成品は、焼成前に比べて、可視光領域での光透過率が改善されており、透明性がより高いことが示される。
【００３２】
実施例３
参考例１で得られたＨ型アイラアイト（平均で縦３μｍ、横３．５μｍ、厚み０．０５μｍ）９０重量部と平均粒子径０．０３μｍの酸化チタン微粒子（堺化学工業株式会社製ＳＴＲ−４０Ａ）１０重量部とをシータ・コンポーザ（株式会社徳寿工作所製）に仕込み、乾式混合して、Ｈ型アイラアイトの表面に酸化チタン微粒子を付着させ、複合化してなる酸化チタン付着量１０重量％の微粉体組成物を得た。この微粉体組成物を試料７とし、その走査型電子顕微鏡写真を図７に示す。
【００３３】
試料７の０．６０重量部と白色ワセリン（小堺製薬株式会社製）２．４０重量部とを樹脂板上で木へらを用いて混練してペーストを調製した。このペーストを２枚の石英ガラスの間に厚み２８μｍとなるように挟み、日本分光株式会社製Ｖ−５５０型分光光度計で光透過率を測定した。また、微粉体組成物を調製するために用いた酸化チタン微粒子自体を試料８とし、その０．０６重量部と白色ワセリン２．９４重量部とを同様に混練し、ペーストとして、光透過率を測定した。結果を図８に示す。
【００３４】
酸化チタン微粒子を１０重量％配合した微粉体組成物、試料７は、ペースト中の酸化チタン濃度は、試料８（酸化チタン微粒子のみ）と同じであるが、紫外領域において、試料８よりも、紫外線遮蔽効果が高く、ペースト中における酸化チタン微粒子が分散性にすぐれることが示される。しかも、可視光領域（４００〜８００ｎｍ）においては、試料７は、試料８よりも、光透過率が高く、透明性にすぐれることが示される。
【図面の簡単な説明】
【図１】は、本発明による微粉体組成物の調製に用いたＨ型アイラアイト（合成層状ポリケイ酸）の透過型電子顕微鏡写真（倍率１００００倍）である。
【図２】は、本発明による微粉体組成物の調製に用いたＨ型アイラアイト（合成層状ポリケイ酸）のＸ線回折パターンである。
【図３】は、酸化亜鉛微粒子をＨ型アイラアイトに付着させた本発明による微粉体組成物（酸化亜鉛微粒子６重量％）の一例の走査型電子顕微鏡写真（倍率２００００倍）である。
【図４】は、酸化亜鉛微粒子をＨ型アイラアイトに付着させた本発明による微粉体組成物（酸化亜鉛微粒子８重量％）の一例の走査型電子顕微鏡写真（倍率２００００倍）である。
【図５】は、本発明による微粉体組成物（酸化亜鉛微粒子６重量％）及びその焼成品の紫外及び可視光領域の光透過率を酸化亜鉛微粒子の光透過率と共に示すグラフである。
【図６】は、本発明による微粉体組成物（酸化亜鉛微粒子８重量％）及びその焼成品の紫外及び可視光領域の光透過率を酸化亜鉛微粒子の光透過率と共に示すグラフである。
【図７】は、酸化チタン微粒子をＨ型アイラアイトに付着させた本発明による微粉体組成物（酸化チタン微粒子１０重量％）の一例の走査型電子顕微鏡写真（倍率２００００倍）である。
【図８】は、本発明による微粉体組成物（酸化チタン微粒子１０重量％）の紫外及び可視光領域の光透過率を酸化チタン微粒子の光透過率と共に示すグラフである。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an ultraviolet shielding fine powder composition, and more specifically, an ultraviolet shielding fine powder composition obtained by adhering inorganic oxide fine particles to the surface of a synthetic layered polysilicic acid or a salt thereof and combining them, and its use, in particular. , Cosmetics and paints.
[0002]
[Prior art]
Conventionally, various inorganic oxide fine particles such as titanium oxide, zinc oxide and zirconium oxide are blended in cosmetics for the purpose of shielding ultraviolet rays in addition to the purpose of coloring. However, conventionally, cosmetics containing inorganic oxide fine particles in this manner are various due to the characteristics of the inorganic fine particles, particularly the physical and chemical properties of the surface, as well as the particle diameter and shape. Have problems. For example, when titanium oxide fine particles are blended as an ultraviolet scattering agent, since the titanium oxide fine particles themselves are aggregates of primary particles, for example, it is difficult to uniformly disperse them in a powdery cosmetic. The ultraviolet shielding effect cannot be exhibited effectively. On the other hand, zinc oxide fine particles generally do not have good extensibility, and cosmetics containing the fine zinc oxide have low extensibility and poor elongation on the skin.
[0003]
In order to solve such problems, various ultraviolet shielding fine powder compositions in which such inorganic oxide fine particles are adhered or supported on a flaky fine powder substrate have been proposed. For example, a powder cosmetic comprising a flaky fine powder substrate such as cleaved sericite and titanium oxide fine particles, which are ultraviolet scattering agents, is dry-mixed and pulverized to adsorb the titanium oxide fine particles to the flaky fine powder substrate. It is described in Kaihei 6-9337.
[0004]
On the other hand, Japanese Patent Application Laid-Open No. 9-132514 discloses a fine powder composition in which titanium oxide is supported on a flaky fine powder base composed of mica, talc, silica and the like by a wet method. Similarly, a fatty acid-solidifying fine powder comprising a fine powder composition obtained by wet-treating a flaky fine powder substrate such as mica and zinc oxide fine particles and coating the fine powder substrate with zinc oxide fine particles is also disclosed in JP-A-9-227792. It is described in the gazette.
[0005]
However, the above-mentioned fine powder composition as described above, in particular, a fine powder composition in which fine particles of titanium oxide or zinc oxide are adhered to a fine powder substrate as an ultraviolet scattering agent, can be used for practical ultraviolet radiation. In order to obtain a shielding effect, it is necessary to attach a large amount of fine particles of titanium oxide or zinc oxide to the substrate. However, it is not easy to uniformly attach a large amount of inorganic oxide fine particles to the fine powder substrate. Thus, conventionally, a fine powder composition in which a large amount of inorganic oxide fine particles are adhered to a fine powder substrate has, for example, a problem inferior in dispersibility in cosmetics. There is a problem that sex is not enough.
[0006]
[Problems to be solved by the invention]
The present invention has been made in order to solve the above-mentioned problems in the conventional ultraviolet shielding fine powder composition, and the inorganic fine particles are uniformly attached to the flaky fine powder substrate, and the ultraviolet shielding effect is thus improved. An object of the present invention is to provide an ultraviolet shielding fine powder composition having excellent dispersibility in cosmetics and paints.
[0007]
[Means for Solving the Problems]
The ultraviolet shielding fine powder composition according to the present invention is characterized in that inorganic oxide fine particles are adhered to the surface of a flaky fine powder substrate made of synthetic layered polysilicic acid or a salt thereof.
[0008]
In the ultraviolet shielding fine powder composition according to the present invention, preferably, the flaky fine powder substrate made of the synthetic layered polysilicic acid or a salt thereof is a thin piece having a quadrangular shape with one side in a range of 1 to 10 μm, Inorganic oxide fine particles having a particle diameter in the range of 0.01 to 0.5 μm are adhered to the surface in a proportion of 1 to 30% by weight.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
The ultraviolet shielding fine powder composition according to the present invention comprises inorganic oxide fine particles adhered to the surface of a flaky fine powder base composed of synthetic layered polysilicic acid or a salt thereof. As described in “Zeolite” Vol. 13, No. 3, pp. 89-96 (1996), the synthetic layered polysilicate is composed of only a SiO 4 tetrahedron. Are known.
[0010]
A method for synthesizing Iraite is described, for example, in JP-A-9-227116. For example, by applying water glass to a hydrothermal reaction, it is possible to obtain a sodium type Iraite (layered polysilicate), and if this is treated with hydrochloric acid, a hydrogen (H) type Iraite (layered polysilicate) is obtained. be able to.
[0011]
According to the present invention, synthetic layered polysilicic acid or a salt thereof is thus used as the fine powder base. Examples of the salt include a calcium salt and a magnesium salt in addition to a sodium salt. However, according to the present invention, when the ultraviolet shielding fine powder composition is blended in cosmetics, it is preferable to use H-type eyesight as the fine powder base.
[0012]
According to the present invention, the flaky fine powder substrate made of synthetic layered polysilicic acid or a salt thereof is preferably a flaky piece having a square shape with one side in the range of 1 to 10 μm. The thickness is usually in the range of 0.005 to 0.1 μm. According to the present invention, since the synthetic layered polysilicic acid or a salt thereof is a synthetic product as described above, it is possible to use those having a uniform purity, size, etc. It can be deposited uniformly on the layer.
[0013]
In the present invention, the inorganic oxide fine particles are not particularly limited as long as they have a property of shielding ultraviolet rays by scattering or absorbing ultraviolet rays, but preferably zinc oxide, At least one selected from titanium oxide, ferric oxide, cerium oxide, silicon dioxide, zirconium oxide, tungsten oxide and tin oxide is used. Of these, fine particles of zinc oxide or titanium oxide are particularly preferably used. In the present invention, these inorganic oxide fine particles usually have a particle size in the range of 0.01 to 0.5 μm, and preferably have a particle size in the range of 0.01 to 0.2 μm.
[0014]
According to the present invention, the amount of the inorganic oxide fine particles attached to the flaky fine powder substrate is in the range of 1 to 30% by weight, preferably in the range of 3 to 20% by weight, and particularly preferably 5%. It is in the range of ˜15% by weight.
[0015]
The ultraviolet shielding fine powder composition according to the present invention can be obtained by mixing and stirring the flaky fine powder substrate and the inorganic fine particles using a powerful stirring device, but preferably the flaky fine powder substrate and the inorganic fine particles. It can be obtained by a so-called mechanical compounding treatment in which a large compression force and shearing force are repeatedly and instantaneously simultaneously applied to the mixture. Such a mechanical complexing process itself is already known, for example, as described in JP-A-9-59015, and generally by using an apparatus known as a particle complexing apparatus. Can be done. As such an apparatus, for example, a mechano-fusion system (manufactured by Hosokawa Micron Co., Ltd.), theta composer (manufactured by Tokuju Kogakusho Co., Ltd.) and the like can be mentioned.
[0016]
If necessary, the obtained fine powder composition is calcined in an oxidizing atmosphere such as air at a temperature of 300 to 600 ° C., preferably 300 to 500 ° C. or less for the purpose of improving transparency. Also good.
[0017]
As described above, the fine powder composition according to the present invention repeatedly applies a large compressive force and shear force instantaneously and simultaneously to a mixture of a flaky fine powder substrate composed of a synthetic layered polysilicic acid or a salt thereof and inorganic oxide fine particles. By so-called mechanical complexing treatment, inorganic oxide fine particles are adhered to the surface of the substrate substantially in a single layer and uniformly. Therefore, a large amount of inorganic fine particles are formed on the flaky fine powder substrate. Even without blending, it has a high ultraviolet shielding effect.
[0018]
Moreover, the ultraviolet shielding fine powder composition according to the present invention is not only excellent in dispersibility in the powder composition but also excellent in extensibility and transparency, and thus is useful as an ultraviolet shielding agent in cosmetics.
[0019]
Thus, by blending the fine powder composition according to the present invention into a normal cosmetic, a cosmetic having excellent ultraviolet shielding properties can be obtained. The fine powder composition according to the present invention can be advantageously blended into a powdery cosmetic composition by utilizing the excellent dispersibility in the powder composition, however, it is cake-like, pencil-like, stick-like, liquid, You may mix | blend with cosmetics of arbitrary forms, such as emulsion and cream form.
[0020]
Further, the ultraviolet shielding fine powder composition according to the present invention is excellent in dispersibility and stability in both aqueous and oil-based paints, and is therefore useful as an ultraviolet shielding agent in ultraviolet shielding paints. The coating material containing the fine powder composition is useful as an ultraviolet shielding effect.
[0021]
【The invention's effect】
As described above, the ultraviolet shielding fine powder composition according to the present invention allows inorganic oxide fine particles such as titanium oxide and zinc oxide to uniformly adhere to a single layer on a flaky fine powder base composed of synthetic layered polysilicic acid or a salt thereof. In addition to being excellent in ultraviolet shielding effect, it is excellent in dispersibility, extensibility, and transparency, and is useful as an ultraviolet shielding agent in cosmetics and paints.
[0022]
【Example】
EXAMPLES The present invention will be described below with reference to examples, but the present invention is not limited to these examples.
[0023]
Reference example 1
1 L capacity autoclave of 700 g of water glass (No. 4 sodium silicate) composed of 23.3 wt% SiO 2 and 6.2 wt% Na 2 O (NaOH / SiO 2 molar ratio = 0.51 / 1.0) The solution was treated under hydrothermal conditions at 107 ° C. for 280 hours. After completion of the reaction, the mixture was separated by filtration, the solid phase was separated, washed with water, and dried at 80 ° C. for a whole day and night to obtain sodium-type ilaite (layered polysilicate). It was confirmed by an X-ray diffraction pattern that the obtained reaction product was sodium type Iraite (layered polysilicate).
[0024]
This sodium-type Iraite was treated with hydrochloric acid to obtain H-type Iraite (layered polysilicic acid) having a sodium content of 0.3% or less. This H-type eyesight is taken as sample 1, FIG. 1 shows a transmission electron micrograph, and FIG. 2 shows its X-ray diffraction pattern.
[0025]
Example 1
94 parts by weight of H-type eyeraite (average 3 μm, width 3.5 μm, thickness 0.05 μm) obtained in Reference Example 1 and zinc oxide fine particles having an average particle size of 0.02 μm (FINEX-50 manufactured by Sakai Chemical Industry Co., Ltd.) ) 6 parts by weight is charged into theta composer (manufactured by Tokuju Kogakusho Co., Ltd.), dry-mixed, and the zinc oxide fine particles are adhered to the surface of the H-type Iraite. A fine powder composition was obtained. This fine powder composition was used as
[0026]
The fine powder composition was fired in air at 500 ° C. for 2 hours. This is designated as
[0027]
Example 2
A fine powder composition was obtained in the same manner as in Example 1, except that the amount of zinc oxide deposited was 8% by weight. This is designated as Sample 3, and a scanning electron micrograph thereof is shown in FIG. This was fired in air at 500 ° C. for 2 hours to give sample 5.
[0028]
A paste was prepared by kneading 0.60 parts by weight of each of the
[0029]
A fine powder composition containing 8% by weight of zinc oxide fine particles, sample 3 has the same zinc oxide concentration in the paste as sample 6 (only zinc oxide fine particles), but medium ultraviolet (290 to 320 nm, B region). In the near ultraviolet (320 to 400 nm, A region) region, the ultraviolet shielding effect is higher than that of the
[0030]
The amount of zinc oxide fine particles in the fine powder composition of
[0031]
In addition, the fired product has improved light transmittance in the visible light region and higher transparency than before firing.
[0032]
Example 3
90 parts by weight of H type Iraite (average 3 μm, width 3.5 μm, thickness 0.05 μm) obtained in Reference Example 1 and titanium oxide fine particles having an average particle diameter of 0.03 μm (STR-40A manufactured by Sakai Chemical Industry Co., Ltd.) ) 10 parts by weight is charged into theta composer (manufactured by Tokuju Kogakusho Co., Ltd.), dry-mixed, and the fine particles of titanium oxide are deposited on the surface of the H-type Iraite. A fine powder composition was obtained. This fine powder composition was used as Sample 7, and a scanning electron micrograph thereof is shown in FIG.
[0033]
A paste was prepared by kneading 0.60 parts by weight of Sample 7 and 2.40 parts by weight of white petrolatum (manufactured by Kosuge Pharmaceutical Co., Ltd.) using a wooden spatula on a resin plate. This paste was sandwiched between two quartz glasses so as to have a thickness of 28 μm, and light transmittance was measured with a V-550 spectrophotometer manufactured by JASCO Corporation. Further, the titanium oxide fine particles themselves used for preparing the fine powder composition were used as
[0034]
A fine powder composition containing 10% by weight of titanium oxide fine particles, sample 7, the titanium oxide concentration in the paste is the same as that of sample 8 (only titanium oxide fine particles), but in the ultraviolet region, it is more ultraviolet than
[Brief description of the drawings]
FIG. 1 is a transmission electron micrograph (magnification 10,000 times) of H-type Iraite (synthetic layered polysilicic acid) used for the preparation of a fine powder composition according to the present invention.
FIG. 2 is an X-ray diffraction pattern of H-type Iraite (synthetic layered polysilicic acid) used for preparing the fine powder composition according to the present invention.
FIG. 3 is a scanning electron micrograph (magnification 20000 times) of an example of a fine powder composition (6 wt% of zinc oxide fine particles) according to the present invention in which zinc oxide fine particles are adhered to H-type eyelets.
FIG. 4 is a scanning electron micrograph (magnification 20000 times) of an example of a fine powder composition (8% by weight of zinc oxide fine particles) according to the present invention in which zinc oxide fine particles are adhered to H-type eyelets.
FIG. 5 is a graph showing the light transmittance in the ultraviolet and visible light regions of the fine powder composition (6% by weight of zinc oxide fine particles) according to the present invention and the fired product together with the light transmittance of zinc oxide fine particles.
FIG. 6 is a graph showing the light transmittance in the ultraviolet and visible light regions of the fine powder composition (8% by weight of zinc oxide fine particles) according to the present invention and the fired product together with the light transmittance of zinc oxide fine particles.
FIG. 7 is a scanning electron micrograph (magnification 20000 times) of an example of the fine powder composition (titanium oxide
FIG. 8 is a graph showing the light transmittance in the ultraviolet and visible light regions of the fine powder composition (titanium oxide
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08015198A JP3876521B2 (en) | 1998-02-20 | 1998-02-20 | Ultraviolet shielding fine powder composition and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08015198A JP3876521B2 (en) | 1998-02-20 | 1998-02-20 | Ultraviolet shielding fine powder composition and use thereof |
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| Publication Number | Publication Date |
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| JPH11236515A JPH11236515A (en) | 1999-08-31 |
| JP3876521B2 true JP3876521B2 (en) | 2007-01-31 |
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| JP08015198A Expired - Fee Related JP3876521B2 (en) | 1998-02-20 | 1998-02-20 | Ultraviolet shielding fine powder composition and use thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012051759A (en) * | 2010-09-01 | 2012-03-15 | Osaka Prefecture Univ | Method of manufacturing layer silicate compound |
| JP2013040066A (en) * | 2011-08-12 | 2013-02-28 | Osaka Prefecture Univ | Method for manufacturing lamellar silicate compound |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002535430A (en) * | 1999-01-20 | 2002-10-22 | キャボット コーポレイション | Aggregates with attached polymer groups and polymer foam |
| JP5576055B2 (en) * | 2009-04-09 | 2014-08-20 | 岩瀬コスファ株式会社 | Surface treatment powder |
| WO2011016140A1 (en) * | 2009-08-04 | 2011-02-10 | L'oreal | Composite pigment and method for preparation thereof |
| JP6012339B2 (en) * | 2012-08-28 | 2016-10-25 | 大東化成工業株式会社 | Method for producing composite powder |
| CN104151868B (en) * | 2014-07-10 | 2015-10-28 | 池州市英派科技有限公司 | Modified nano-titanium dioxide that a kind of photocatalysis effect strengthens and preparation method thereof |
-
1998
- 1998-02-20 JP JP08015198A patent/JP3876521B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012051759A (en) * | 2010-09-01 | 2012-03-15 | Osaka Prefecture Univ | Method of manufacturing layer silicate compound |
| JP2013040066A (en) * | 2011-08-12 | 2013-02-28 | Osaka Prefecture Univ | Method for manufacturing lamellar silicate compound |
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| Publication number | Publication date |
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| JPH11236515A (en) | 1999-08-31 |
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