JP2019099411A - Keratin and hexagonal plate-like zinc oxide-containing granular complex - Google Patents
Keratin and hexagonal plate-like zinc oxide-containing granular complex Download PDFInfo
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- JP2019099411A JP2019099411A JP2017230999A JP2017230999A JP2019099411A JP 2019099411 A JP2019099411 A JP 2019099411A JP 2017230999 A JP2017230999 A JP 2017230999A JP 2017230999 A JP2017230999 A JP 2017230999A JP 2019099411 A JP2019099411 A JP 2019099411A
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- Japan
- Prior art keywords
- keratin
- zinc oxide
- hexagonal plate
- acid
- poe
- Prior art date
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- 108010076876 Keratins Proteins 0.000 title claims abstract description 126
- 102000011782 Keratins Human genes 0.000 title claims abstract description 126
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Abstract
Description
本発明は、ケラチン及び六角板状酸化亜鉛を含む粒状複合体等に関する。 The present invention relates to a particulate complex containing keratin and hexagonal plate-like zinc oxide.
太陽光は肌の老化の原因の一つとされている。太陽光は、様々な波長の光からなり、例えば、可視光線の他、紫外線や近赤外線等が含まれている。紫外線はそのエネルギーが比較的大きいことから、紫外線による肌へのダメージを軽減する方法が開発されてきている。一方で、近赤外線についてはそのエネルギーが比較的小さいことから、肌へ与えるダメージについての研究はあまり進んでいない。しかし、近年、紫外線は主に、皮膚表層で吸収され、深部には到達しない一方で、近赤外線は真皮から筋層にまで達し、深部にまで影響を及ぼすことが明らかになってきている。このため、太陽光による肌へのダメージを軽減するために、近赤外線を反射することが求められている。 Sunlight is considered to be one of the causes of skin aging. Sunlight is composed of light of various wavelengths, and includes, for example, ultraviolet rays and near infrared rays as well as visible light. Because the energy of ultraviolet light is relatively large, methods have been developed to reduce the damage to the skin due to ultraviolet light. On the other hand, because the energy of the near infrared rays is relatively small, studies on damage to the skin have not been advanced so much. However, in recent years, it has become clear that ultraviolet rays are mainly absorbed by the skin surface layer and do not reach the deep part, while near infrared rays reach from the dermis to the muscular layer and affect the deep part. For this reason, in order to reduce the damage to the skin by sunlight, it is required to reflect near infrared rays.
このために、外用組成物において、近赤外線を反射する能力を有する物質を配合することが研究されている。外用組成物は肌に適用するものであることから、適用時に肌の滑らかさ(高いスベスベ感)やザラツキの無さ(低いザラツキ感)が得られることも重要となる。よって、近赤外線を反射しながらも、高いスベスベ感及び低いザラツキ感が達成された外用組成物が求められる。 For this purpose, it has been studied to blend a substance having the ability to reflect near infrared rays in the composition for external use. Since the composition for external use is to be applied to the skin, it is also important to be able to obtain the smoothness of the skin (high slip feeling) and no roughness (low roughness) at the time of application. Therefore, there is a need for a composition for external use that achieves high smoothness and low roughness while reflecting near infrared rays.
本発明は、近赤外線を反射しながらも、高いスベスベ感及び低いザラツキ感が達成された外用組成物を提供可能な素材の開発を課題とする。 An object of the present invention is to develop a material capable of providing an external use composition in which high scanthiness and low roughness are achieved while reflecting near infrared light.
上記特許文献1には、特定の六角板状酸化亜鉛が記載されており、当該六角板状酸化亜鉛が赤外線(近赤外線波長領域含む)をある程度反射できることも記載されている。本発明者らは、六角板状酸化亜鉛にケラチン処理を施して得られる粒状複合体は、近赤外線を反射する能力は六角板状酸化亜鉛そのものとほぼ同等あるいはそれ以上であるうえ、当該粒状複合体は比較的低いMIU(平均摩擦係数)及び比較的低いMMD(摩擦係数の平均偏差)を示すことから、当該粒状複合体を配合した外用組成物は優れた滑らかさ及び低いザラツキ感を示し得ることを見出し、さらに検討を重ねて本発明を完成させるに至った。 Patent Document 1 describes a specific hexagonal plate-like zinc oxide, and also describes that the hexagonal plate-like zinc oxide can reflect infrared rays (including near infrared wavelength region) to some extent. The present inventors have found that a granular composite obtained by subjecting hexagonal plate-like zinc oxide to keratin treatment has an ability to reflect near-infrared rays that is almost equal to or higher than that of hexagonal plate-like zinc oxide itself, Since the body exhibits relatively low MIU (average coefficient of friction) and relatively low MMD (average deviation of coefficient of friction), the composition for external use containing the particulate composite may exhibit excellent smoothness and low roughness. The present invention has been completed after further investigations.
本発明は例えば以下の項に記載の主題を包含する。
項1.
ケラチン及び六角板状酸化亜鉛粒子を含む粒状複合体。
項2.
六角板状酸化亜鉛粒子表面にケラチンを備えた、項1に記載の粒状複合体。
項3.
ケラチンが、天然ケラチン、加水分解ケラチン、カチオン化加水分解ケラチン、及びシリル化加水分解ケラチンからなる群より選択される少なくとも1種である、項1又は2に記載の粒状複合体。
項4.
ケラチン含有量が0.05〜5質量%である、項1〜3のいずれかに記載の粒状複合体。
項5.
一次粒子径が0.1〜5μmである、項1〜4のいずれかに記載の粒状複合体。
項6.
請求項1〜5のいずれかに記載の粒状複合体を含む、外用組成物。
項7.
化粧品組成物、医薬部外品組成物、又は医薬品組成物である、項6に記載の外用組成物。
The present invention includes, for example, the subject matters described in the following sections.
Item 1.
A particulate complex comprising keratin and hexagonal plate-like zinc oxide particles.
Item 2.
The granular composite according to Item 1, wherein keratin is provided on the surface of hexagonal plate-like zinc oxide particles.
Item 3.
The particulate composite according to item 1 or 2, wherein the keratin is at least one selected from the group consisting of natural keratin, hydrolyzed keratin, cationized hydrolyzed keratin, and silylated hydrolyzed keratin.
Item 4.
The granular composite according to any one of Items 1 to 3, wherein the keratin content is 0.05 to 5% by mass.
Item 5.
The particulate composite according to any one of Items 1 to 4, wherein the primary particle size is 0.1 to 5 μm.
Item 6.
An external composition comprising the particulate composite according to any one of claims 1 to 5.
Item 7.
Item 7. The external composition according to item 6, which is a cosmetic composition, a quasi-drug composition, or a pharmaceutical composition.
本発明に係るケラチン及び六角板状酸化亜鉛粒子を含む粒状複合体は、六角板状酸化亜鉛粒子そのものに比べ、さらに優れた滑らかさ及び低いザラツキ感を奏する。さらに、六角板状酸化亜鉛そのものとほぼ同等あるいはそれ以上の近赤外線反射効果も奏し得る。このため、特に外用組成物への配合等に好ましく用いることができる。 The granular complex containing the keratin and the hexagonal plate-like zinc oxide particles according to the present invention exhibits more excellent smoothness and low roughness as compared with the hexagonal plate-like zinc oxide particles themselves. Furthermore, a near infrared reflection effect approximately equivalent to or more than that of the hexagonal plate-like zinc oxide itself can also be exhibited. For this reason, it can be preferably used particularly for blending into a composition for external use.
以下、本発明の各実施形態について、さらに詳細に説明する。 Hereinafter, each embodiment of the present invention will be described in more detail.
本発明に包含される粒状複合体はケラチン及び六角板状酸化亜鉛粒子を含む。 The particulate complex included in the present invention comprises keratin and hexagonal plate-like zinc oxide particles.
ケラチンとしては、特に制限はされないが、特に化粧品素材(例えば皮膚コンディショニング剤、ヘアコンディショニング剤等)として用いられる公知の各種ケラチンを用いることができる。このようなケラチンとしては、例えば天然ケラチン、加水分解ケラチン、カチオン化加水分解ケラチン、シリル化加水分解ケラチン等が挙げられる。加水分解ケラチンとしては、ケラチンタンパク質を、酸、アルカリ、又は酵素等により加水分解したものが挙げられる。また、加水分解ケラチンを変性剤等によりカチオン化若しくはシリル化させたり、あるいは予め変性させたカチオン化ケラチンタンパク質若しくはシリル化ケラチンタンパク質を加水分解させて、カチオン化加水分解ケラチン、シリル化加水分解ケラチンを調製することができる。カチオン化加水分解ケラチンとしては、例えばヒドロキシプロピルトリモニウム加水分解ケラチン、ステアルジモニウムヒドロキシプロピル加水分解ケラチン、ラウリルジモニウムヒドロキシプロピル加水分解ケラチン等が挙げられる。また、シリル化加水分解ケラチンとしては、例えば(ジヒドロキシメチルシリルプロポキシ)ヒドロキシプロピル加水分解ケラチン等が挙げられる。 The keratin is not particularly limited, and various known keratins used as cosmetic materials (for example, skin conditioning agents, hair conditioning agents, etc.) can be used. As such keratin, for example, natural keratin, hydrolyzed keratin, cationized hydrolyzed keratin, silylated hydrolyzed keratin and the like can be mentioned. As the hydrolyzed keratin, one obtained by hydrolyzing keratin protein with an acid, an alkali, an enzyme or the like can be mentioned. Also, cationized hydrolyzed keratin or silylated hydrolyzed keratin can be obtained by cationizing or silylation of hydrolyzed keratin with a modifier or by hydrolyzing cationized keratin protein or silylated keratin protein that has been previously modified. It can be prepared. Examples of the cationized hydrolyzed keratin include hydroxypropyltrimonium hydrolyzed keratin, stealdimonium hydroxypropyl hydrolyzed keratin, lauryldimonium hydroxypropyl hydrolyzed keratin and the like. In addition, examples of the silylated hydrolyzed keratin include (dihydroxymethylsilylpropoxy) hydroxypropyl hydrolyzed keratin and the like.
ケラチンの平均分子量としては、特に制限されないが、例えば100〜50000程度が好ましい。200〜40000程度がより好ましい。加水分解されて平均分子量が小さくなっているケラチンが好ましく、例えば300〜5000程度が好ましく、400〜3000程度がより好ましく、500〜2000程度がさらに好ましい。当該平均分子量は数平均分子量である。また、各化粧品素材メーカーからの市販品については数平均分子量値が提供されており、本発明におけるケラチンの平均分子量として、当該メーカー提供の数平均分子量値を好ましく用いることができる。 The average molecular weight of keratin is not particularly limited, but, for example, about 100 to 50,000 is preferable. About 200 to 40,000 are more preferable. The keratin which is hydrolyzed and an average molecular weight becomes small is preferable, for example, about 300-5000 are preferable, about 400-3000 are more preferable, and about 500-2000 are more preferable. The average molecular weight is a number average molecular weight. Moreover, the number average molecular weight value is provided about the commercial item from each cosmetic material maker, and the number average molecular weight value of the said maker provision can be preferably used as an average molecular weight of the keratin in this invention.
ケラチンの原料も特に制限されないが、化粧品素材として用いられる公知の各種ケラチンは例えば羊毛又は羽毛から調製されており、本発明においても羊毛又は羽毛から調製されたケラチンを好ましく用いることができる。 The raw material of keratin is not particularly limited, but various known keratins used as cosmetic materials are prepared, for example, from wool or feathers, and keratins prepared from wool or feathers can be preferably used in the present invention as well.
ケラチンは1種単独で又は2種以上を組み合わせて用いることができる。 Keratin can be used alone or in combination of two or more.
六角板状酸化亜鉛粒子としては、一次粒子径が0.1〜10μmであるものが好ましく、0.1〜5μmであるものがより好ましく、0.2〜4μmであるものがさらに好ましく、0.5〜3μmであるものがよりさらに好ましい。このような一次粒子径であると、高い滑らかさ、低いザラツキ感を有し、かつ、近赤外線反射効果により優れたものとなる。 The hexagonal plate-like zinc oxide particles preferably have a primary particle diameter of 0.1 to 10 μm, more preferably 0.1 to 5 μm, still more preferably 0.2 to 4 μm, and 0. Even more preferred is 5 to 3 μm. With such a primary particle diameter, it has high smoothness and low roughness, and is excellent due to the near infrared reflection effect.
なお、六角板状酸化亜鉛粒子の一次粒子径は、走査型電子顕微鏡(SEM)(例えばJSM−6510A:日本電子社製)で撮影した写真の2000〜50000倍の視野での対角線径(六角板状面の3本の対角線のうちの任意の1本の対角線の長さ)(μm)を粒子100個分について計測し、その累積分布の50%から求めた値である。 In addition, the primary particle diameter of hexagonal plate-like zinc oxide particles is a diagonal diameter (hexagonal plate in a field of 2000 to 50000 times of a photograph taken with a scanning electron microscope (SEM) (for example, JSM-6510A: manufactured by JEOL Ltd.) The length (μm) of one arbitrary one of the three diagonals of the flat surface (μm) is measured for 100 particles, and the value is obtained from 50% of the cumulative distribution.
また、六角板状酸化亜鉛粒子は、アスペクト比が2.5以上であることが好ましい。アスペクト比は、2.7以上であることがより好ましく、3.0以上であることがさらに好ましい。アスペクト比が2.5以上の板状であることで、形状に由来するより高い滑らかさや低いザラツキ感、より高い近赤外線反射効果を有するものとなる。 The hexagonal plate-like zinc oxide particles preferably have an aspect ratio of 2.5 or more. The aspect ratio is more preferably 2.7 or more, and still more preferably 3.0 or more. By having a plate shape having an aspect ratio of 2.5 or more, it is possible to have higher smoothness, lower roughness and higher near infrared reflection effect derived from the shape.
なお、当該アスペクト比は、走査型電子顕微鏡(SEM)(例えばJSM−6510A:日本電子社製)で六角板状酸化亜鉛粒子を撮影した写真の2000〜50000倍の視野において、六角板状表面が手前を向いている粒子についてその対角線径(六角板状酸化亜鉛粒子の場合、六角板状面の3本の対角線のうちの任意の1本の対角線の長さ)(μm)を粒子100個分計測した平均値をL、六角板状酸化亜鉛粒子の側面が手前を向いている粒子(長方形に見える粒子)についてその厚み(μm)(長方形の短い方の辺の長さ)を粒子100個分計測した平均値をTとしたとき、それらの値の比(L/T)として求めた値である。 The aspect ratio is a hexagonal plate-like surface in a field of 2000 to 50000 times that of a photograph of hexagonal plate-like zinc oxide particles taken with a scanning electron microscope (SEM) (for example, JSM-6510A: manufactured by JEOL Ltd.) For particles facing forward, the diameter of the diagonal (in the case of hexagonal plate-like zinc oxide particles, the length of any one of the three diagonals of the hexagonal plate-like surface) (μm) is divided by 100 particles The average of the measured values is L, and for particles in which the side faces of the hexagonal plate-like zinc oxide particles are facing forward (particles that appear to be rectangular), their thickness (μm) (length of shorter side of rectangle) is divided by 100 particles It is the value calculated | required as ratio (L / T) of those values, when the measured average value is set to T.
六角板状酸化亜鉛粒子は、例えば国際公開第2012/147886号、2015/118777号等に開示されており、例えば当該文献に記載の方法で製造することができる。より具体的には、例えば、微粒子酸化亜鉛を亜鉛塩水溶液中で熟成する工程を含む製造方法によって、得ることができる。以下、当該製造方法について詳述する。 The hexagonal plate-like zinc oxide particles are disclosed, for example, in WO 2012/147886, 2015/118777 and the like, and can be produced, for example, by the method described in the document. More specifically, it can be obtained, for example, by a production method including the step of aging particulate zinc oxide in an aqueous zinc salt solution. Hereinafter, the manufacturing method will be described in detail.
上記微粒子酸化亜鉛は、特に限定されるものではないが、粒子径が0.005μm以上、0.2μm以下である原料酸化亜鉛を使用することが好ましい。上記原料酸化亜鉛の粒子径は、BET法によって求められる比表面積と同一の表面積を有する球の直径に相当する。すなわち、粒子径は、BET法により測定して求めた比表面積:Sgと、酸化亜鉛の真比重:ρから、下記計算式により求めた値である。BET法による測定には、全自動BET比表面積測定装置(例えばMacsorb Model HM−1200(Mountech社製))を用いることができる。
粒子径(μm)=[6/(Sg×ρ)]
(Sg(m2/g):比表面積、ρ(g/cm3):粒子の真比重)
なお、当該計算において、粒子の真比重:ρは、酸化亜鉛の真比重の値である5.6を用いた。
上記原料酸化亜鉛としては特に限定されず、公知の方法によって製造された酸化亜鉛を使用することができる。市販のものとしては、例えば、堺化学工業社製FINEX−75、FINEX−50、FINEX−30、SF−15、微細酸化亜鉛等を挙げることができる。
六角板状酸化亜鉛粒子は、上記微粒子酸化亜鉛を亜鉛塩水溶液中で熟成させて得ることができる。すなわち、亜鉛塩水溶液中に上述した微粒子酸化亜鉛を分散させ、その状態で加熱し、結晶成長させることによって得ることができる。
The fine particle zinc oxide is not particularly limited, but it is preferable to use raw material zinc oxide having a particle diameter of 0.005 μm or more and 0.2 μm or less. The particle size of the raw material zinc oxide corresponds to the diameter of a sphere having the same surface area as the specific surface area determined by the BET method. That is, the particle diameter is a value determined by the following formula from the specific surface area: Sg determined by BET method and the true specific gravity of zinc oxide: ρ. For measurement by the BET method, a fully automatic BET specific surface area measuring device (for example, Macsorb Model HM-1200 (manufactured by Mountech)) can be used.
Particle size (μm) = [6 / (Sg × ρ)]
(Sg (m 2 / g): specific surface area, ρ (g / cm 3 ): true specific gravity of particles)
In addition, in the said calculation, 5.6 which is a value of true specific gravity of a zinc oxide was used for the true specific gravity of particle | grains (rho).
The raw material zinc oxide is not particularly limited, and zinc oxide produced by a known method can be used. Examples of commercially available products include FINEX-75, FINEX-50, FINEX-30, SF-15, fine zinc oxide and the like manufactured by Sakai Chemical Industry Co., Ltd.
Hexagonal plate-like zinc oxide particles can be obtained by maturing the above-mentioned fine particle zinc oxide in a zinc salt aqueous solution. That is, it can be obtained by dispersing the above-described particulate zinc oxide in a zinc salt aqueous solution and heating it in that state to grow crystals.
上記亜鉛塩水溶液における亜鉛塩は特に限定されず、例えば酢酸亜鉛、硝酸亜鉛、硫酸亜鉛、塩化亜鉛、ぎ酸亜鉛等の亜鉛塩化合物を挙げることができる。亜鉛塩水溶液のなかでも、特に酢酸亜鉛水溶液を使用した場合に好適に本発明の特定の六角板状酸化亜鉛粒子が得られる。 The zinc salt in the zinc salt aqueous solution is not particularly limited, and examples thereof include zinc salt compounds such as zinc acetate, zinc nitrate, zinc sulfate, zinc chloride and zinc formate. Among the zinc salt aqueous solutions, the particular hexagonal plate-shaped zinc oxide particles of the present invention are suitably obtained particularly when a zinc acetate aqueous solution is used.
また、これらの亜鉛塩水溶液は、酸化亜鉛と酸と水とを混合して酸化亜鉛を酸加水分解することで調製したものであってもよい。亜鉛塩水溶液を酸化亜鉛と酸と水で調製する際に使用する酸化亜鉛の粒子形状、粒子径は特に限定されないが、不純物をなるべく少なくするという観点から、酸化亜鉛のZn純度は95%以上であることが好ましい。また、酸としては、例えば酢酸、硝酸、硫酸、塩酸、ぎ酸、クエン酸、蓚酸、プロピオン酸、マロン酸、乳酸、酒石酸、グルコン酸、コハク酸等が挙げられる。特に酢酸を使用した場合に好適に本発明の特定の六角板状酸化亜鉛粒子が得られる。これらの亜鉛塩水溶液のうち、2種又はそれ以上を併用して使用してもよい。 Moreover, these zinc salt aqueous solutions may be prepared by mixing zinc oxide, an acid, and water, and acid-hydrolyzing zinc oxide. The particle shape and particle diameter of zinc oxide used when preparing a zinc salt aqueous solution with zinc oxide, acid and water are not particularly limited, but from the viewpoint of reducing impurities as much as possible, the zinc purity of zinc oxide is 95% or more Is preferred. Examples of the acid include acetic acid, nitric acid, sulfuric acid, hydrochloric acid, formic acid, citric acid, oxalic acid, propionic acid, malonic acid, lactic acid, tartaric acid, gluconic acid, succinic acid and the like. In particular, when using acetic acid, the specific hexagonal plate-like zinc oxide particles of the present invention can be obtained. Two or more of these aqueous zinc salt solutions may be used in combination.
亜鉛塩水溶液中の亜鉛塩濃度は0.1mol/lを超え、4.0mol/l以下であることが好ましく、特に、酢酸亜鉛水溶液を用いる場合、当該水溶液中の酢酸亜鉛濃度は、0.2mol/lを超え、2.0mol/l以下であることが好ましい。 The zinc salt concentration in the zinc salt aqueous solution is preferably more than 0.1 mol / l and 4.0 mol / l or less, and in particular, when using a zinc acetate aqueous solution, the zinc acetate concentration in the aqueous solution is 0.2 mol It is preferably more than 1 / l and not more than 2.0 mol / l.
上記亜鉛塩水溶液は、本発明の効果を損なわない範囲で、亜鉛塩、水以外の成分を少量含有してもよい。例えば、分散剤等を含有することもできる。 The zinc salt aqueous solution may contain a small amount of components other than the zinc salt and water, as long as the effects of the present invention are not impaired. For example, a dispersing agent etc. can also be contained.
亜鉛塩水溶液中に微粒子酸化亜鉛を添加してスラリーとする場合、スラリー全量に対して微粒子酸化亜鉛の濃度が10〜500g/lであることが好ましい。 When fine particle zinc oxide is added to a zinc salt aqueous solution to form a slurry, the concentration of the fine particle zinc oxide is preferably 10 to 500 g / l with respect to the total amount of the slurry.
上記熟成に際しては、本発明の効果を損なわない範囲で、微粒子酸化亜鉛、亜鉛塩、水以外の成分を少量添加してもよい。例えば、分散剤等を添加することもできる。
熟成は、45〜110℃において行うことが好ましい。熟成時間は0.5〜24時間を挙げることができる。熟成温度、熟成時間、原料酸化亜鉛濃度、亜鉛塩濃度等の条件によって粒子径の調整を図ることができるため、これらの条件については目的とする六角板状酸化亜鉛粒子に応じて適宜設定して行うことが好ましい。
In the above-mentioned ripening, fine particles of zinc oxide, zinc salts and components other than water may be added in small amounts, as long as the effects of the present invention are not impaired. For example, dispersants and the like can be added.
Aging is preferably performed at 45 to 110 ° C. Aging time can mention 0.5 to 24 hours. The particle diameter can be adjusted depending on conditions such as aging temperature, aging time, concentration of raw material zinc oxide, concentration of zinc salt, etc. Therefore, these conditions are appropriately set according to the target hexagonal plate-like zinc oxide particles. It is preferred to do.
このようにして得られた六角板状酸化亜鉛粒子は、必要に応じて、濾過、水洗、乾燥等の後処理を行ってもよい。
上記方法によって製造された六角板状酸化亜鉛粒子は、必要に応じて分級されてもよい。当該分級としては、例えば篩による分級を挙げることができる。篩による分級方法としては、例えば湿式分級、乾式分級を挙げることができる。また、湿式粉砕、乾式粉砕等の処理を行ってもよい。
The hexagonal plate-like zinc oxide particles thus obtained may be subjected to post treatments such as filtration, water washing, drying and the like, if necessary.
The hexagonal plate-like zinc oxide particles produced by the above method may be classified as required. As the said classification, classification by a sieve can be mentioned, for example. Examples of classification methods using a sieve include wet classification and dry classification. Further, processing such as wet grinding or dry grinding may be performed.
上述の製造方法は、焼成処理を行わずに六角板状酸化亜鉛粒子を得ることができるものであるが、上述した方法によって得られた六角板状酸化亜鉛粒子に焼成処理を施しても差し支えない。焼成に際しては、公知の任意の装置を利用した方法を挙げることができ、処理条件等も特に限定されない。 Although the above-mentioned manufacturing method can obtain hexagonal plate-like zinc oxide particles without performing the firing treatment, the hexagonal plate-like zinc oxide particles obtained by the above-mentioned method may be subjected to the firing treatment . In the case of baking, the method of utilizing the well-known arbitrary apparatus can be mentioned, Processing conditions etc. are not specifically limited.
なお、六角板状酸化亜鉛粒子としては、市販品を用いることもできる。例えば、六角板状酸化亜鉛XZシリーズ(堺化学工業社製)を好ましく用いることができ、なかでもXZ−1000F、XZ−2000F、及びXZ−3000F等をより好ましく用いることができる。なお、当該市販品の平均粒子径カタログ値はレーザー回折式粒度分布装置による測定値であるため、本発明における平均粒子径値とは異なる。 A commercial item can also be used as hexagonal plate-like zinc oxide particles. For example, hexagonal plate-like zinc oxide XZ series (manufactured by Sakai Chemical Industry Co., Ltd.) can be preferably used, and among them, XZ-1000F, XZ-2000F, XZ-3000F and the like can be more preferably used. In addition, since the average particle diameter catalog value of the said commercial item is a measured value by a laser diffraction type particle size distribution apparatus, it differs from the average particle diameter value in this invention.
六角板状酸化亜鉛粒子は1種単独で又は2種以上を組み合わせて用いることができる。 The hexagonal plate-like zinc oxide particles can be used singly or in combination of two or more.
本発明に係る粒状複合体は、ケラチン及び六角板状酸化亜鉛粒子を含むところ、ケラチンが六角板状酸化亜鉛粒子表面に備えられてることが好ましい。特に、六角板状酸化亜鉛粒子の板の表面にケラチンが存在することが好ましい。 The particulate composite according to the present invention preferably comprises keratin and zinc oxide particles in the form of keratin and zinc oxide particles. In particular, keratin is preferably present on the surface of a plate of hexagonal plate-like zinc oxide particles.
ケラチンを六角板状酸化亜鉛粒子表面に備えさせる方法(換言すれば、六角板状酸化亜鉛粒子表面のケラチン処理方法)としては、例えば、六角板状酸化亜鉛粒子及びケラチンを含有するスラリーを乾燥させる工程を有する方法が挙げられる。より詳細には、例えば六角板状酸化亜鉛及び水を混合してスラリーを調製し、当該スラリーを撹拌しながらケラチンを特定量(例えば、酸化亜鉛及びケラチン合計量に対してケラチンの添加量が0.5〜10質量%又は1〜8質量%程度となるよう)添加し、特定時間(例えば30〜120分程度)熟成させ、必要に応じて濾過及び水洗を行い、さらに乾燥(例えば30〜50℃で12〜24時間程度)させることで、ケラチンを六角板状酸化亜鉛粒子表面に備えた粒状複合体を調製することができる。 As a method of providing keratin on the surface of hexagonal plate-like zinc oxide particles (in other words, a method of keratin treatment of the surface of hexagonal plate-like zinc oxide particles), for example, a slurry containing hexagonal plate-like zinc oxide particles and keratin is dried. The method which has a process is mentioned. More specifically, for example, a hexagonal plate-like zinc oxide and water are mixed to prepare a slurry, and while the slurry is stirred, a specific amount of keratin (for example, the amount of keratin added relative to the total amount of zinc oxide and keratin is 0) 0.5 to 10% by mass or 1 to 8% by mass), and aging for a specific time (for example, about 30 to 120 minutes), filtering and washing as necessary, and further drying (for example, 30 to 50) By conducting the reaction at 12 ° C. for about 12 to 24 hours, a granular composite having keratin on the surface of hexagonal plate-like zinc oxide particles can be prepared.
本発明に係る粒状複合体のケラチン含有量は、0.05〜5質量%であることが好ましく、0.8〜4質量%であることがより好ましく、0.1〜3質量%であることがさらに好ましい。このような割合でケラチンを含むことにより、滑らかさ、ザラツキ感、赤外線反射性においてより優れた効果を得ることができる。なお、当該粒状複合体のケラチン含有量は次のようにして求める値である。すなわち、粒状複合体及び、その原料の六角板状酸化亜鉛粒子を、それぞれ2gずつ坩堝に入れ、電気炉中500℃で1時間加熱し、加熱後の重量を測定する。そして、粒状複合体に含まれるケラチンは全て消失しており、且つ、原料である六角状酸化亜鉛粒子の減少率はいずれであっても同じであるとして、粒状複合体中のケラチン含有率(質量%)を算出する。 The keratin content of the particulate complex according to the present invention is preferably 0.05 to 5% by mass, more preferably 0.8 to 4% by mass, and 0.1 to 3% by mass. Is more preferred. By including keratin in such a ratio, more excellent effects can be obtained in smoothness, roughness and infrared reflectivity. The keratin content of the particulate complex is a value determined as follows. That is, 2 g of each of the granular composite and the hexagonal plate-like zinc oxide particles as the raw material is put in a crucible, and heated in an electric furnace at 500 ° C. for 1 hour, and the weight after heating is measured. Then, all keratins contained in the particulate complex have disappeared, and the keratin content rate (mass) in the particulate complex is assumed to be the same regardless of the rate of reduction of the hexagonal zinc oxide particles as the raw material. Calculate%).
なお、本発明に係る粒状複合体は、表面にケラチンを備えることが好ましい。また、当該粒状複合体は、六角板状酸化亜鉛粒子及びケラチンのみからなるものであってもよいし、本発明の効果を損なわない範囲で、これら以外の成分を含むものであってもよい。ただし、複合体の表面の一部又は全部に、ケラチンが存在していることが好ましい。また、当該粒状複合体自体が六角板状の形状であることが好ましい。また例えば、六角板状酸化亜鉛粒子及びケラチンが積層体を形成しているものが好ましい。また、六角板状酸化亜鉛粒子の板の表面にケラチンが処理されて固定化されたものが好ましい。限定的な解釈を望むものではないが、複合体自体が六角板状である場合、当該複合体が面状に敷き詰められた際には、大きな隙間なく面を敷き詰めることが可能となると考えられる。さらには当該複合体のケラチンが処理された表面が表になるよう敷き詰めることによって、敷き詰めた面の表にはケラチン処理面が形成されると考えられ、好ましい。 In addition, it is preferable that the granular complex which concerns on this invention equips the surface with keratin. Moreover, the said granular composite may consist only of hexagonal plate-like zinc oxide particle and keratin, and may contain components other than these in the range which does not impair the effect of this invention. However, it is preferable that keratin is present on part or all of the surface of the complex. Moreover, it is preferable that the said granular composite body itself is a hexagonal plate-like shape. Further, for example, it is preferable that hexagonal plate-like zinc oxide particles and keratin form a laminate. Further, it is preferable that keratin is treated and immobilized on the surface of a plate of hexagonal plate-like zinc oxide particles. Although not wanting a limited interpretation, it is considered that when the composite itself is in the form of a hexagonal plate, when the composite is spread in a plane, it becomes possible to spread the surface without a large gap. Furthermore, it is considered that a keratin-treated surface is formed on the surface of the spread surface by laying the surface of the complex on which the keratin has been treated to be a surface, which is preferable.
なお、当該粒状複合体において、六角板状酸化亜鉛粒子及びケラチン以外の成分が含まれる場合には、六角板状酸化亜鉛粒子及びケラチンの間に存在することが好ましい。例えば、他成分により表面処理された六角板状酸化亜鉛粒子にケラチン処理を施して当該粒状複合体を調製した場合、六角板状酸化亜鉛粒子及びケラチンの間にその他成分(予め六角板状酸化亜鉛粒子表面になされていた表面処理に用いた成分)が存在することになる。 In addition, when components other than hexagonal plate-shaped zinc oxide particles and keratin are contained in the said granular composite, it is preferable to exist between hexagonal plate-shaped zinc oxide particles and keratin. For example, when a hexagonal plate-like zinc oxide particle surface-treated with another component is subjected to keratin treatment to prepare the granular composite, another component (a hexagonal plate-like zinc oxide in advance is prepared between the hexagonal plate-like zinc oxide particle and keratin The components used for surface treatment that have been applied to the particle surface will be present.
なお、本明細書において、六角板状酸化亜鉛粒子表面にケラチンを備えた粒状複合体は、六角板状酸化亜鉛粒子及びケラチンの間にその他成分が含まれる粒状複合体をも包含する概念である。言い換えれば、六角板状酸化亜鉛粒子表面にケラチンを備えた粒状複合体は、粒状複合体の表面にケラチンを備えていれば、ケラチンは六角板状酸化亜鉛粒子表面と接して備えられていてもよいし、ケラチンと六角板状酸化亜鉛粒子表面との間にその他成分が備えられていてもよい。 In addition, in the present specification, a particulate complex having keratin on the surface of hexagonal plate-like zinc oxide particles is a concept including also a particulate complex in which other components are contained between hexagonal plate-like zinc oxide particles and keratin. . In other words, if the granular composite having keratin on the surface of hexagonal plate-like zinc oxide particles has keratin on the surface of the granular composite, keratin may be provided in contact with the surface of hexagonal plate-like zinc oxide particles Other components may be provided between the keratin and the surface of the hexagonal plate-like zinc oxide particles.
この、予め六角板状酸化亜鉛粒子表面に施されていてもよい表面処理としては、特に限定されず、例えばケイ素酸化物、ケイ素酸化物の水和物、アルミニウムの酸化物及びアルミニウムの水酸化物からなる群から選択される少なくとも1種の化合物による皮膜を形成させる表面処理、撥水性有機化合物による表面処理、シランカップリング剤、チタンカップリング剤等のカップリング剤による表面処理等を挙げることができる。これらの2種以上の表面処理を組み合わせて行うものであってもよい。 The surface treatment which may be applied to the surface of the hexagonal plate-like zinc oxide particles in advance is not particularly limited. For example, silicon oxide, hydrate of silicon oxide, oxide of aluminum and hydroxide of aluminum Surface treatment with at least one compound selected from the group consisting of: surface treatment with a water repellent organic compound; surface treatment with a coupling agent such as a silane coupling agent or a titanium coupling agent; it can. These two or more surface treatments may be performed in combination.
上記ケイ素酸化物、ケイ素酸化物の水和物、アルミニウムの酸化物及びアルミニウムの水酸化物からなる群から選択される少なくとも1種の化合物による皮膜の形成は、Si源化合物及び/又はAl源化合物を、加水分解や加熱分解などにより粉体表面に析出させる等の方法で行うことができる。上記Si源化合物及び/又はAl源化合物としては、テトラアルコキシシランやその加水分解縮合物、ケイ酸ナトリウム、ケイ酸カリウム、アルミニウムアルコキシドやその加水分解縮合物、アルミン酸ナトリウム等、容易にSiO2やAl(OH)3、Al2O3に変換する化合物等を使用することができる。 The formation of a film by at least one compound selected from the group consisting of the above silicon oxides, hydrates of silicon oxides, oxides of aluminum and hydroxides of aluminum is a Si source compound and / or an Al source compound. Can be deposited on the surface of the powder by hydrolysis, thermal decomposition or the like. As the Si source compound and / or the Al source compound, tetraalkoxysilane or its hydrolytic condensate, sodium silicate, potassium silicate, aluminum alkoxide or its hydrolytic condensate, sodium aluminate etc., SiO 2 or the like easily A compound etc. which convert to Al (OH) 3 and Al 2 O 3 can be used.
上記加水分解としては特に限定されないが、硫酸、塩酸、酢酸、硝酸などの酸を使用した方法が挙げられる。この水分散体を用いたシリカの処理方法における中和方法は、六角板状酸化亜鉛粒子を含有する分散体に酸を入れてからSi源化合物及び/又はAl源化合物を添加する方法、分散体にSi源化合物及び/又はAl源化合物を入れてから酸を添加する方法、分散体にSi源化合物及び/又はAl源化合物と酸を同時に添加する方法のいずれでもよい。 The hydrolysis is not particularly limited, and examples thereof include a method using an acid such as sulfuric acid, hydrochloric acid, acetic acid or nitric acid. In the method of treating silica using this aqueous dispersion, the method of adding an acid to a dispersion containing hexagonal plate-like zinc oxide particles, and then adding a Si source compound and / or an Al source compound, a dispersion The method may be any of a method of adding an Si source compound and / or an Al source compound and then adding an acid, and a method of simultaneously adding a Si source compound and / or an Al source compound and an acid to the dispersion.
上記撥水性有機化合物による処理としては、特に限定されるものではないが、例えば、シリコーンオイル、アルキルシラン、アルキルチタネート、アルキルアルミネート、ポリオレフィン、ポリエステル、金属石鹸、アミノ酸、アミノ酸塩などが挙げられる。なかでも、化学的な安定性からシリコーンオイルが好ましい。このシリコーンオイルの具体例としては、ジメチルポリシロキサン(例えば、信越化学工業製KF−96A−100cs、旭化成ワッカーシリコーン製DM10)、メチルハイドロジェンポリシロキサン(例えば、信越化学工業製KF−99P、東レ・ダウコーニング製SH1107C)、(ジメチコン/メチコン)コポリマー(例えば、信越化学工業製KF−9901)、メチルフェニルシリコーン(例えば、信越化学工業製KF−50−100cs)、アミノ変性シリコーン(例えば、信越化学工業製KF−8015、東レ・ダウコーニング製JP−8500 Conditioning Agent、旭化成ワッカーシリコーン製ADM6060)、トリエトキシシリルエチルポリジメチルシロキシエチルジメチコン(例えば、信越化学工業製KF−9908)、トリエトキシシリルエチルポリジメチルシロキシエチルヘキシルジメチコン(例えば、信越化学工業製KF−9909)による処理等を挙げることができる。 The treatment with the water repellent organic compound is not particularly limited, and examples thereof include silicone oil, alkylsilane, alkyl titanate, alkyl aluminate, polyolefin, polyester, metal soap, amino acid, amino acid salt and the like. Among them, silicone oil is preferable in view of chemical stability. Specific examples of this silicone oil include dimethylpolysiloxane (for example, Shin-Etsu Chemical KF-96A-100cs, Asahi Kasei Wacker Silicone DM10), methylhydrogenpolysiloxane (for example Shin-Etsu Chemical KF-99P, Toray. Dow Corning SH1107C, (dimethicone / methicone) copolymer (eg, Shin-Etsu Chemical KF-9901), methylphenyl silicone (eg, Shin-Etsu Chemical KF-50-100 cs), amino-modified silicone (eg, Shin-Etsu Chemical) KF-8015, Toray Dow Corning JP-8500 Conditioning Agent, Asahi Kasei Wacker Silicone ADM 6060), triethoxysilylethyl polydimethylsiloxyethyl dimethicone (for example, Shinetsu Manabu Kogyo KF-9908), triethoxysilyl ethyl polydimethylsiloxy hexyl dimethicone (for example, a treatment by Shin-Etsu Chemical KF-9909).
上記シランカップリング剤による処理としては、ビニルトリス(2−メトキシエトキシ)シラン、ビニルトリクロルシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、2−(3,4エポキシシクロヘキシル)エチルトリメトキシシラン、3−グリシドキシプロピルトリメトキシシラン、3−グリシドキシプロピルメチルジエトキシシラン、3−グリシドキシプロピルトリエトキシシラン、p−スチリルトリメトキシシラン、3−メタクリロキシプロピルメチルジメトキシシラン、3−メタクリロキシプロピルトリメトキシシラン、3−メタクリロキシプロピルメチルジエトキシシラン、3−メタクリロキシプロピルトリエトキシシラン、3−アクリロキシプロピルトリメトキシシラン、N−2(アミノエチル)3−アミノプロピルメチルジメトキシシラン、N−2(アミノエチル)3−アミノプロピルトリメトキシシラン、N−2(アミノエチル)3−アミノプロピルトリエトキシシラン、3−アミノトリエトキシシラン、3−トリエトキシシリル−N−(1,3−ジメチル−ブチリデン)プロピルアミン、N−フェニル−3−アミノプロピルトリメトキシシラン、N−(ビニルベンジル)−2−アミノエチル−3−アミノプロピルトリメトキシシラン塩酸塩、3−ウレイドプロピルトリエトキシシラン、3−クロロプロピルトリメトキシシラン、3−メルカプトプロピルメチルジメトキシシラン、3−メルカプトプロピルトリメトキシシラン、ビス(トリエトキシシリルプロピル)テトラスルフィド、3−イソシアネートプロピルトリエトキシシラン、テトラメトキシシラン、テトラエトキシシラン、メチルトリメトキシシラン、メチルトリエトキシシラン、フェニルトリエトキシシラン、ヘキサメチルジシラザン、ヘキシルトリメトキシシラン、デシルトリメトキシシランを挙げることができる。 As the treatment with the above-mentioned silane coupling agent, vinyltris (2-methoxyethoxy) silane, vinyltrichlorosilane, vinyltrimethoxysilane, vinyltriethoxysilane, 2- (3,4 epoxycyclohexyl) ethyltrimethoxysilane, 3-glycone Cidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 3-glycidoxypropyltriethoxysilane, p-styryltrimethoxysilane, 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethylsilane Methoxysilane, 3-methacryloxypropylmethyldiethoxysilane, 3-methacryloxypropyltriethoxysilane, 3-acryloxypropyltrimethoxysilane, N-2 (aminoethyl) 3-aminopropyl Methyldimethoxysilane, N-2 (aminoethyl) 3-aminopropyltrimethoxysilane, N-2 (aminoethyl) 3-aminopropyltriethoxysilane, 3-aminotriethoxysilane, 3-triethoxysilyl-N- (1,3-dimethyl-butylidene) propylamine, N-phenyl-3-aminopropyltrimethoxysilane, N- (vinylbenzyl) -2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride, 3-ureidopropyl Triethoxysilane, 3-chloropropyltrimethoxysilane, 3-mercaptopropylmethyldimethoxysilane, 3-mercaptopropyltrimethoxysilane, bis (triethoxysilylpropyl) tetrasulfide, 3-isocyanatopropyltriethoxysilane, tetramethosilane Shishiran, tetraethoxysilane, methyl trimethoxysilane, methyl triethoxysilane, phenyl triethoxy silane, hexamethyldisilazane, hexyltrimethoxysilane and decyltrimethoxysilane.
上記チタンカップリング剤による処理としては、テトライソプロピルチタネート、テトラノルマルブチルチタネート、ブチルチタネートダイマー、テトラ(2−エチルヘキシル)チタネート、テトラメチルチタネート、チタンアセチルアセトネート、チタンテトラアセチルアセトネート、チタンエチルアセトアセテート、チタンオクタンジオレート、チタンラクテート、チタントリエタノールアミネート、ポリヒドロキシチタンステアレートを挙げることができる。 As treatment with the above-mentioned titanium coupling agent, tetraisopropyl titanate, tetranormal butyl titanate, butyl titanate dimer, tetra (2-ethylhexyl) titanate, tetramethyl titanate, titanium acetylacetonate, titanium tetraacetylacetonate, titanium ethyl acetoacetate And titanium octanediolate, titanium lactate, titanium triethanolaminate, and polyhydroxy titanium stearate.
上記表面処理(ケラチン処理前に、予め六角板状酸化亜鉛粒子表面になされる表面処理)を行う場合は、表面処理は、処理後の粉体の全量に対して0.1〜30重量%となる割合で行うことが好ましい。当該範囲内のものとすることで、滑り性が向上し、かつ耐湿性が向上し、樹脂への分散性が向上するという点で好ましい。 In the case of performing the above surface treatment (surface treatment to be applied to the surface of the hexagonal plate-like zinc oxide particles in advance before keratin treatment), the surface treatment is 0.1 to 30% by weight with respect to the total amount of powder after treatment. It is preferable to carry out in the following ratio. By setting it as the thing within the said range, it is preferable at the point that slipperiness improves, and moisture resistance improves and the dispersibility to resin improves.
本発明に係る粒状複合体の一次粒子径としては、上述した六角板状酸化亜鉛粒子の一次粒子径と同等のものが好ましく、なかでも0.1〜5μmであるものが好ましく、0.2〜4μmであるものがより好ましく、0.5〜3μmであるものがさらに好ましい。このような一次粒子径であると、より高い滑らかさ、低いザラツキ感を有し、かつ、近赤外線反射効果により優れたものとなる。 The primary particle diameter of the particulate composite according to the present invention is preferably equivalent to the primary particle diameter of the hexagonal plate-like zinc oxide particles described above, and in particular, the particle diameter is preferably 0.1 to 5 μm, 0.2 to 0.2 The thickness is more preferably 4 μm, and still more preferably 0.5 to 3 μm. With such a primary particle diameter, it has higher smoothness, low roughness, and is more excellent due to the near infrared reflection effect.
なお、粒状複合体の一次粒子径は、走査型電子顕微鏡(SEM)(例えばJSM−6510A:日本電子社製)で撮影した写真の2000〜50000倍の視野での対角線径(特に粒状複合体が六角板状の形状である場合、六角板状面の3本の対角線のうちの任意の1本の対角線の長さ)(μm)を粒子100個分について計測し、その累積分布の50%から求めた値である。 In addition, the primary particle diameter of the granular composite is a diagonal diameter (in particular, the granular composite) in a field of 2000 to 50000 times of a photograph taken with a scanning electron microscope (SEM) (for example, JSM-6510A: manufactured by Nippon Denshi Co., Ltd.) In the case of a hexagonal plate shape, the length of any one of the three diagonals of the hexagonal plate surface) (μm) is measured for 100 particles, and 50% of its cumulative distribution It is the calculated value.
また、本発明に係る粒状複合体は、アスペクト比が2.5以上であることが好ましい。アスペクト比は、2.7以上であることがより好ましく、3.0以上であることがさらに好ましい。アスペクト比が2.5以上の板状であることで、形状に由来するより高い滑らかさや低いザラツキ感、より高い近赤外線反射効果を有するものとなる。 The granular composite according to the present invention preferably has an aspect ratio of 2.5 or more. The aspect ratio is more preferably 2.7 or more, and still more preferably 3.0 or more. By having a plate shape having an aspect ratio of 2.5 or more, it is possible to have higher smoothness, lower roughness and higher near infrared reflection effect derived from the shape.
なお、粒状複合体が六角板状の形状である場合には、当該アスペクト比は、走査型電子顕微鏡(SEM)で六角板状粒状複合体を撮影した写真の2000〜50000倍の視野において、六角板状の粒状複合体の表面が手前を向いている粒子についてその対角線径(六角板状面の3本の対角線のうちの任意の1本の対角線の長さ)(μm)を粒子100個分計測した平均値をL、六角板状の粒状複合体の側面が手前を向いている粒子(長方形に見える粒子)についてその厚み(μm)(長方形の短い方の辺の長さ)を粒子100個分計測した平均値をTとしたとき、それらの値の比(L/T)として求めた値である。 In the case where the granular composite has a hexagonal plate shape, the aspect ratio is hexagonal in a field of 2000 to 50000 times that of a photograph of the hexagonal plate-like granular composite taken with a scanning electron microscope (SEM). For particles in which the surface of the plate-like granular composite faces the front, 100 diagonal particles (the length of any one of the three diagonals of the hexagonal plate surface) (μm) The measured average value is L, and for particles in which the side face of the hexagonal plate-like granular composite faces the front (particles that appear to be rectangular), the thickness (μm) (length of the shorter side of the rectangle) is 100 particles When an average value obtained by minute measurement is T, it is a value obtained as a ratio (L / T) of those values.
本発明に係る粒状複合体は、例えば外用組成物に配合する等して用いた場合、優れた滑らかさ及び低いザラツキ感を奏し得る。具体的には、本発明に係る粒状複合体(粉体)は、小さいMIU(平均摩擦係数)及び小さいMMD(摩擦係数の平均偏差)を示す。MIU(平均摩擦係数)の値が小さい程、滑り性が良く滑り易いことを意味する。また、MMD(摩擦係数の平均偏差)の値が小さい程、ザラツキ感が少ないことを意味する。なお、ここでの比較対象は、粒状複合体の原料として用いた六角板状酸化亜鉛粒子そのものである。より具体的に述べれば、本発明に係る粒状複合体(粉体)は、当該粒状複合体の原料として用いた六角板状酸化亜鉛粒子(粉体)に比べて、小さいMIU(平均摩擦係数)及びMMD(摩擦係数の平均偏差)を示す、ということである。 The granular composite according to the present invention can exhibit excellent smoothness and low roughness, for example, when it is used by being blended in a composition for external use. Specifically, the particulate composite (powder) according to the present invention exhibits a small MIU (mean friction coefficient) and a small MMD (mean deviation of the friction coefficient). The smaller the value of the MIU (mean friction coefficient), the better the slipperiness, which means that it is slippery. Also, the smaller the value of MMD (average deviation of the coefficient of friction), the less the rough feeling. In addition, the comparison object here is the hexagonal plate-like zinc oxide particle itself used as a raw material of the granular composite. More specifically, the granular composite (powder) according to the present invention has a smaller MIU (average coefficient of friction) than the hexagonal plate-like zinc oxide particles (powder) used as the raw material of the granular composite. And MMD (mean deviation of the coefficient of friction).
例えば、特に制限されないが、例えば本発明に係る粒状複合体(粉体)は、MIUが1.15以下であることが好ましく、1.1以下であることがより好ましく、1.05以下であることがさらに好ましい。また、MMDが0.05以下であることが好ましい。MMDは、0.04以下、又は0.03以下であるとより好ましい。これらのMIU値及びMMD値をともに満たすものが中でも好ましい。 For example, although not particularly limited, for example, in the particulate composite (powder) according to the present invention, the MIU is preferably 1.15 or less, more preferably 1.1 or less, and 1.05 or less Is more preferred. Moreover, it is preferable that MMD is 0.05 or less. The MMD is more preferably 0.04 or less, or 0.03 or less. Among these, those satisfying both the MIU value and the MMD value are preferable.
MIU値及びMMD値は、次のようにして測定した値である。すなわち、摩擦感テスター(例えばKES−SE摩擦感テスター(カトーテック社製))を用いて、両面テープ上に伸ばした粒状複合体(粉体)に対し、摩擦測定荷重25gf、表面測定試料移動速度1mm/sec、測定距離範囲20mmの条件で、MIU及びMMDを測定して得られた値である。 The MIU value and the MMD value are values measured as follows. That is, using a friction tester (for example, KES-SE friction tester (manufactured by Kato Tech)), for a granular composite (powder) stretched on a double-sided tape, the friction measurement load 25 gf, surface measurement sample moving speed It is a value obtained by measuring MIU and MMD under conditions of 1 mm / sec and a measuring distance range of 20 mm.
本発明に係る粒状複合体は、その他の成分と混合して、例えば外用組成物(例えば医薬品、医薬部外品、及び化粧品)、インキ、塗料、プラスチック等に配合することもできる。特に、上述の特性を有しているため、滑り性が良くざらつきも少ないという優れた粉体感触を持つ外用組成物を得ることができる点で好ましいものである。中でも、化粧品に配合して用いるのに好適である。 The particulate composite according to the present invention can be mixed with other components and incorporated, for example, into a composition for external use (for example, pharmaceuticals, quasi-drugs and cosmetics), ink, paint, plastics and the like. In particular, since it has the above-mentioned characteristics, it is preferable in that it can obtain an external use composition having an excellent powder feel that it has good slipperiness and less roughness. Above all, they are suitable for use in cosmetics.
上記化粧品としては特に限定されず、このような粉体に、必要に応じて化粧品原料を混合することによって、サンスクリーン剤等の紫外線防御用化粧品;ファンデーション等のベースメイク化粧品;口紅等のポイントメイク化粧品;、化粧水、クリーム等のスキンケア化粧品、トリートメント、スタイリング剤等のヘアケア化粧品等を得ることができる。また、本発明の六角板状酸化亜鉛粒子は上述した優れた粉体感触に加え、紫外線吸収能も持ち合わせていることから、化粧品に使用した場合に優れた性能を有するものである。
上記化粧品は、油性化粧品、水性化粧品、O/W型化粧品、W/O型化粧品等の任意の形態とすることができる。
The above cosmetic is not particularly limited, and by mixing cosmetic powder with such powder, if necessary, UV protective cosmetic such as sunscreen agent; base makeup cosmetic such as foundation; point makeup such as lipstick Cosmetics, skin care cosmetics such as lotions and creams, hair care cosmetics such as treatments and styling agents, etc. can be obtained. In addition to the excellent powder feel mentioned above, the hexagonal plate-like zinc oxide particles of the present invention also have ultraviolet absorbing ability, and therefore have excellent performance when used in cosmetics.
The cosmetic may be in any form such as oily cosmetic, aqueous cosmetic, O / W cosmetic, W / O cosmetic and the like.
上記化粧品は、化粧品分野において使用することができる任意の水性成分、油性成分を併用するものであってもよい。上記水性成分及び油性成分としては特に限定されず、例えば、油剤、界面活性剤、保湿剤、高級アルコール、金属イオン封鎖剤、天然及び合成高分子、水溶性及び油溶性高分子、紫外線遮蔽剤、各種抽出液、有機染料等の色剤、防腐剤、酸化防止剤、色素、増粘剤、pH調整剤、香料、冷感剤、制汗剤、殺菌剤、皮膚賦活剤、各種粉体等の成分を含有するものであってもよい。 The cosmetic may be used in combination with any aqueous component or oil component that can be used in the cosmetic field. The aqueous component and the oily component are not particularly limited, and examples thereof include oils, surfactants, moisturizers, higher alcohols, sequestering agents, natural and synthetic polymers, water-soluble and oil-soluble polymers, ultraviolet screening agents, Extracts, coloring agents such as organic dyes, preservatives, antioxidants, dyes, thickeners, pH adjusters, perfumes, cooling agents, antiperspirants, bactericides, skin activators, various powders, etc. It may contain ingredients.
上記油剤は特に限定はないが、例えば、天然動植物油脂(例えば、オリーブ油、ミンク油、ヒマシ油、パーム油、牛脂、月見草油、ヤシ油、ヒマシ油、カカオ油、マカデミアナッツ油等);蝋(例えば、ホホバ油、ミツロウ、ラノリン、カルナウバロウ、キャンデリラロウ等);高級アルコール(例えば、ラウリルアルコール、ステアリルアルコール、セチルアルコール、オレイルアルコール等);高級脂肪酸(例えば、ラウリン酸、パルミチン酸、ステアリン酸、オレイン酸、ベヘニン酸、ラノリン脂肪酸等;高級脂肪族炭化水素(例えば、流動パラフィン、固形パラフィン、スクワラン、ワセリン、セレシン、マイクロクリスタリンワックス等);合成エステル油(例えば、ブチルステアレート、ヘキシルラウレート、ジイソプロピルアジペート、ジイソプロピルセバケート、ミリスチン酸オクチルドデシル、イソプロピルミリステート、イソプロピルパルミテートイソプロピルミリステート、セチルイソオクタノエート、ジカプリン酸ネオペンチルグリコール);シリコーン誘導体(例えば、メチルシリコーン、メチルフェニルシリコーン等のシリコーン油)などが例示できる。さらに、油溶性のビタミン、防腐剤、美白剤などを配合することもできる。 The above oil agent is not particularly limited, but, for example, natural animal and vegetable fats and oils (eg, olive oil, mink oil, castor oil, palm oil, beef tallow, evening primrose oil, coconut oil, castor oil, castor oil, cocoa oil, macadamia nut oil etc.); , Jojoba oil, beeswax, lanolin, carnauba wax, candelilla wax, etc .; higher alcohols (eg, lauryl alcohol, stearyl alcohol, cetyl alcohol, oleyl alcohol, etc.); higher fatty acids (eg, lauric acid, palmitic acid, stearic acid, olein) Acids, behenic acid, lanolin fatty acids, etc .; higher aliphatic hydrocarbons (eg, liquid paraffin, solid paraffin, squalane, vaseline, ceresin, microcrystalline wax, etc.); synthetic ester oils (eg, butyl stearate, hexyl laurate, diisopropyl ester) A PETE, diisopropyl sebacate, octyldodecyl myristate, isopropyl myristate, isopropyl palmitate isopropyl myristate, cetyl isooctanoate, neopentyl glycol dicaprate, silicone derivatives (eg, methyl silicone, methyl phenyl silicone, etc.) Furthermore, oil-soluble vitamins, preservatives, whitening agents, etc. can also be blended.
上記界面活性剤としては、親油性非イオン界面活性剤、親水性非イオン界面活性剤等を挙げることができる。上記親油性非イオン界面活性剤としては特に限定されず、例えば、ソルビタンモノオレエート、ソルビタンモノイソステアレート、ソルビタンモノラウレート、ソルビタンモノパルミテート、ソルビタンモノステアレート、ソルビタンセスキオレエート、ソルビタントリオレエート、ペンタ−2−エチルヘキシル酸ジグリセロールソルビタン、テトラ−2−エチルヘキシル酸ジグリセロールソルビタン等のソルビタン脂肪酸エステル類、モノ綿実油脂肪酸グリセリン、モノエルカ酸グリセリン、セスキオレイン酸グリセリン、モノステアリン酸グリセリン、α,α’−オレイン酸ピログルタミン酸グリセリン、モノステアリン酸グリセリンリンゴ酸等のグリセリンポリグリセリン脂肪酸類、モノステアリン酸プロピレングリコール等のプロピレングリコール脂肪酸エステル類、硬化ヒマシ油誘導体、グリセリンアルキルエーテル等を挙げることができる。 Examples of the surfactant include lipophilic nonionic surfactants and hydrophilic nonionic surfactants. The above-mentioned lipophilic nonionic surfactant is not particularly limited. For example, sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan sesquioleate, sorbitan triole Sorbitan fatty acid esters such as alate, diglycerol sorbitan penta-2-ethylhexyl acid, diglycerol sorbitan tetra-2-ethylhexyl acid, mono cotton seed oil fatty acid glycerin, glycerol monoerucate glycerine sesquioleate, glycerin monostearate α, α '-Proline of glycerin polyglycerin fatty acids such as pyroglutamate oleic acid pyroglutamate, glycerin monostearic acid malic acid, propylene glycol monostearate etc. Examples thereof include glycol fatty acid esters, hydrogenated castor oil derivatives, glycerin alkyl ether and the like.
親水性非イオン界面活性剤としては特に限定されず、例えば、POEソルビタンモノオレエート、POEソルビタンモノステアレート、POEソルビタンテトラオレエート等のPOEソルビタン脂肪酸エステル類、POEソルビットモノラウレート、POEソルビットモノオレエート、POEソルビットペンタオレエート、POEソルビットモノステアレート等のPOEソルビット脂肪酸エステル類、POEグリセリンモノステアレート、POEグリセリンモノイソステアレート、POEグリセリントリイソステアレート等のPOEグリセリン脂肪酸エステル類、POEモノオレエート、POEジステアレート、POEジオレエート、システアリン酸エチレングリコール等のPOE脂肪酸エステル類、POEラウリルエーテル、POEオレイルエーテル、POEステアリルエーテル、POEベヘニルエーテル、POE2−オクチルドデシルエーテル、POEコレスタノールエーテル等のPOEアルキルエーテル類、POEオクチルフェニルエーテル、POEノニルフェニルエーテル、POEジノニルフェニルエーテル等のPOEアルキルフェニルエーテル類、ブルロニック等のプルアロニック型類、POE・POPセチルエーテル、POE・POP2−デシルテトラデシルエーテル、POE・POPモノブチルエーテル、POE・POP水添ラノリン、POE・POPグリセリンエーテル等のPOE・POPアルキルエーテル類、テトロニック等のテトラPOE・テトラPOPエチレンジアミン縮合物類、POEヒマシ油、POE硬化ヒマシ油、POE硬化ヒマシ油モノイソステアレート、POE硬化ヒマシ油トリイソステアレート、POE硬化ヒマシ油モノピログルタミン酸モノイソステアリン酸ジエステル、POE硬化ヒマシ油マレイン酸等のPOEヒマシ油硬化ヒマシ油誘導体、POEソルビットミツロウ等のPOEミツロウ・ラノリン誘導体、ヤシ油脂肪酸ジエタノールアミド、ラウリン酸モノエタノールアミド、脂肪酸イソプロパノールアミド等のアルカノールアミド、POEプロピレングリコール脂肪酸エステル、POEアルキルアミン、POE脂肪酸アミド、ショ糖脂肪酸エステル、POEノニルフェニルホルムアルデヒド縮合物、アルキルエトキシジメチルアミンオキシド、トリオレイルリン酸等を挙げることができる。 The hydrophilic non-ionic surfactant is not particularly limited. For example, POE sorbitan monooleate, POE sorbitan monostearate, POE sorbitan fatty acid esters such as POE sorbitan tetraoleate, POE sorbit monolaurate, POE sorbit mono POE sorbite fatty acid esters such as oleate, POE sorbite pentaoleate, POE sorbite monostearate POE glycerin monostearate POE glycerin mono isostearate POE glycerin fatty acid esters such as POE glycerin triisostearate POE POE fatty acid esters such as mono oleate, POE distearate, POE dioleate, ethylene glycol distearate, POE lauryl ether, POE oley POE alkyl ethers such as ether, POE stearyl ether, POE behenyl ether, POE 2-octyldodecyl ether, POE cholestanol ether, POE alkyl phenyl ethers such as POE octyl phenyl ether, POE nonyl phenyl ether, POE dinonyl phenyl ether, Pluronic types such as bluronics, POE · POP cetyl ether, POE · POP 2-decyl tetradecyl ether, POE · POP monobutyl ether, POE · POP hydrogenated lanolin, POE · POP alkyl ethers such as POE · glycerin glycerin ether, tee Toronika et al. Tetra POE · tetra POP ethylene diamine condensates, POE castor oil, POE hydrogenated castor oil, POE hydrogenated castor oil mono isosteare POE castor oil-cured castor oil derivatives such as POE-cured castor oil triisostearate, POE-cured castor oil monopyroglutamic acid monoisostearate diester POE-cured castor oil maleic acid POE beeswax lanolin derivatives such as POE sorbite beeswax , Coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, alkanolamide such as fatty acid isopropanolamide, POE propylene glycol fatty acid ester, POE alkylamine, POE fatty acid amide, sucrose fatty acid ester, POE nonylphenylformaldehyde condensate, alkylethoxydimethyl Amine oxide, trioleyl phosphate and the like can be mentioned.
その他の界面活性剤としては、例えば、脂肪酸セッケン、高級アルキル硫酸エステル塩、POEラウリル硫酸トリエタノールアミン、アルキルエーテル硫酸エステル塩等のアニオン界面活性剤、アルキルトリメチルアンモニウム塩、アルキルピリジニウム塩、アルキル四級アンモニウム塩、アルキルジメチルベンジルアンモニウム塩、POEアルキルアミン、アルキルアミン塩、ポリアミン脂肪酸誘導体等のカチオン界面活性剤、及び、イミダゾリン系両性界面活性剤、ベタイン系界面活性剤等の両性界面活性剤を安定性及び皮膚刺激性に問題のない範囲で配合してもよい。 Other surfactants include, for example, anionic surfactants such as fatty acid soap, higher alkyl sulfate ester salt, POE lauryl sulfate triethanolamine, alkyl ether sulfate ester salt, alkyl trimethyl ammonium salt, alkyl pyridinium salt, alkyl quaternary Stability of cationic surfactants such as ammonium salts, alkyldimethylbenzyl ammonium salts, POE alkylamines, alkylamine salts and polyamine fatty acid derivatives, and amphoteric surfactants such as imidazoline based amphoteric surfactants and betaine based surfactants And you may mix | blend in the range which has no problem in skin irritation.
上記保湿剤としては特に限定されず、例えば、キシリトール、ソルビトール、マルチトール、コンドロイチン硫酸、ヒアルロン酸、ムコイチン硫酸、カロニン酸、アテロコラーゲン、コレステリル−12−ヒドロキシステアレート、乳酸ナトリウム、胆汁酸塩、dl−ピロリドンカルボン酸塩、短鎖可溶性コラーゲン、ジグリセリン(EO)PO付加物、イザヨイバラ抽出物、セイヨウノコギリソウ抽出物、メリロート抽出物等を挙げることができる。 The above-mentioned humectant is not particularly limited, and examples thereof include xylitol, sorbitol, maltitol, chondroitin sulfate, hyaluronic acid, mucotin sulfate, caronic acid, atelocollagen, cholesteryl-12-hydroxystearate, sodium lactate, bile salt, dl- There may be mentioned pyrrolidone carboxylate, short chain soluble collagen, diglycerin (EO) PO adduct, Izayoira extract, Yarrow extract, Meriloto extract and the like.
上記高級アルコールとしては特に限定されず、例えば、ラウリルアルコール、セチルアルコール、ステアリルアルコール、ベヘニルアルコール、ミリスチルアルコール、オレイルアルコール、セトステアリルアルコール等の直鎖アルコール、モノステアリルグリセリンエーテル(バチルアルコール)、2−デシルテトラデシノール、ラノリンアルコール、コレステロール、フィトステロール、ヘキシルドデカノール、イソステアリルアルコール、オクチルドデカノール等の分枝鎖アルコール等を挙げることができる。 The above-mentioned higher alcohol is not particularly limited, and examples thereof include linear alcohols such as lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, monostearyl glycerin ether (batyl alcohol), 2-decyl Examples include branched alcohols such as tetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyldodecanol, isostearyl alcohol, octyldodecanol and the like.
金属イオン封鎖剤としては特に限定されず、例えば、1−ヒドロキシエタン−1,1−ジフォスホン酸、1−ヒドロキシエタン−1,1−ジフォスホン酸四ナトリウム塩、クエン酸ナトリウム、ポリリン酸ナトリウム、メタリン酸ナトリウム、グルコン酸、リン酸、クエン酸、アスコルビン酸、コハク酸、エデト酸等を挙げることができる。 The sequestering agent is not particularly limited. For example, 1-hydroxyethane-1,1-diphosphonic acid, 1-hydroxyethane-1,1-diphosphonic acid tetrasodium salt, sodium citrate, sodium polyphosphate, metaphosphoric acid Sodium, gluconic acid, phosphoric acid, citric acid, ascorbic acid, succinic acid, edetic acid and the like can be mentioned.
上記天然の水溶性高分子としては特に限定されず、例えば、アラアビアガム、トラガカントガム、ガラクタン、グアガム、キャロブガム、カラヤガム、カラギーナン、ペクチン、カンテン、クインスシード(マルメロ)、アルゲコロイド(カッソウエキス)、デンプン(コメ、トウモロコシ、バレイショ、コムギ)、グリチルリチン酸等の植物系高分子、キサンタンガム、デキストラン、サクシノグルカン、プルラン等の微生物系高分子、コラーゲン、カゼイン、アルブミン、ゼラチン等の動物系高分子を挙げることができる。
半合成の水溶性高分子としては特に限定されず、例えば、カルボキシメチルデンプン、メチルヒドロキシプロピルデンプン等のデンプン系高分子、メチルセルロース、ニトロセルロース、エチルセルロース、メチルヒドロキシプロピルセルロース、ヒドロキシエチルセルロース、セルロース硫酸ナトリウム、ヒドロキシプロピルセルロース、カルボキシメチルセルロースナトリウム(CMC)、結晶セルロース、セルロース末等のセルロース系高分子、アルギン酸ナトリウム、アルギン酸プロピレングリコールエステル等のアルギン酸系高分子等を挙げることができる。
The above-mentioned naturally-occurring water-soluble polymer is not particularly limited. For example, arabia gum, tragacanth gum, galactan, guar gum, carob gum, caraya gum, carrageenan, pectin, agarten, quince seed (marello), arge colloid (kaso extract), starch (rice, Plant polymers such as corn, potato, wheat), glycyrrhizinic acid, microbial polymers such as xanthan gum, dextran, succinoglucan, pullulan, and animal polymers such as collagen, casein, albumin, gelatin, etc. .
The semi-synthetic water-soluble polymer is not particularly limited, and examples thereof include starch-based polymers such as carboxymethyl starch and methyl hydroxypropyl starch, methyl cellulose, nitrocellulose, ethyl cellulose, methyl hydroxypropyl cellulose, hydroxyethyl cellulose, cellulose sodium sulfate, Examples thereof include cellulose polymers such as hydroxypropyl cellulose, sodium carboxymethyl cellulose (CMC), crystalline cellulose and cellulose powder, and alginic acid polymers such as sodium alginate and alginic acid propylene glycol ester.
合成の水溶性高分子としては特に限定されず、例えば、ポリビニルアルコール、ポリビニルメチルエーテル、ポリビニルピロリドン等のビニル系高分子、ポリエチレングリコール20,000、40,000、60,000等のポリオキシエチレン系高分子、ポリオキシエチレンポリオキシプロピレン共重合体共重合系高分子、ポリアクリル酸ナトリウム、ポリエチルアクリレート、ポリアクリルアミド等のアクリル系高分子、ポリグリセリン、ポリエチレンイミン、カチオンポリマー、カルボキシビニルポリマー、アルキル変性カルボキシビニルポリマー、(アクリル酸ヒドロキシエチル/アクリロイルジメチルタウリンNa)コポリマー、(アクリル酸Na/アクリロイルジメチルタウリンNa)コポリマー、(アクリロイルジメチルタウリンアンモニウム/ビニルピロリドン)コポリマー、(アクリロイルジメチルタウリンアンモニウムメタクリル酸ベヘネス−25)クロスポリマー等を挙げることができる。 The synthetic water-soluble polymer is not particularly limited, and examples thereof include vinyl polymers such as polyvinyl alcohol, polyvinyl methyl ether, and polyvinyl pyrrolidone, and polyoxyethylene polymers such as polyethylene glycol 20,000, 40,000, and 60,000. Polymer, polyoxyethylene-polyoxypropylene copolymer copolymer, sodium polyacrylate, polyethyl acrylate, acrylic polymer such as polyacrylamide, polyglycerin, polyethyleneimine, cationic polymer, carboxyvinyl polymer, alkyl Modified carboxyvinyl polymer, (Hydroxyethyl acrylate / Acryloyldimethyltaurine Na) copolymer, (Na-acrylate / Acryloyldimethyltaurine Na) copolymer, (Acryloyldimethylta) Phosphorus ammonium / vinylpyrrolidone) copolymer, and (ammonium acryloyldimethyltaurate methacrylate Beheneth-25) cross-polymer.
無機の水溶性高分子としては特に限定されず、例えば、ベントナイト、ケイ酸AlMg(ビーガム)、ラポナイト、ヘクトライト、無水ケイ酸等を挙げることができる。
紫外線遮蔽剤としては特に限定されず、例えば、パラアミノ安息香酸(以下PABAと略す)、PABAモノグリセリンエステル、N,N−ジプロポキシPABAエチルエステル、N,N−ジエトキシPABAエチルエステル、N,N−ジメチルPABAエチルエステル、N,N−ジメチルPABAブチルエステル等の安息香酸系紫外線遮蔽剤;ホモメンチル−N−アセチルアントラニレート等のアントラニル酸系紫外線遮蔽剤;アミルサリシレート、メンチルサリシレート、ホモメンチルサリシレート、オクチルサリシレート、フェニルサリシレート、ベンジルサリシレート、p−イソプロパノールフェニルサリシレート等のサリチル酸系紫外線遮蔽剤;オクチルシンナメート、エチル−4−イソプロピルシンナメート、メチル−2,5−ジイソプロピルシンナメート、エチル−2,4−ジイソプロピルシンナメート、メチル−2,4−ジイソプロピルシンナメート、プロピル−p−メトキシシンナメート、イソプロピル−p−メトキシシンナメート、イソアミル−p−メトキシシンナメート、2−エトキシエチル−p−メトキシシンナメート、シクロヘキシル−p−メトキシシンナメート、エチル−α−シアノ−β−フェニルシンナメート、2−エチルヘキシル−α−シアノ−β−フェニルシンナメート、グリセリルモノ−2−エチルヘキサノイル−ジパラメトキシシンナメート等のケイ皮酸系紫外線遮蔽剤;2,4−ジヒドロキシベンゾフェノン、2,2’−ジヒドロキシ−4−メトキシベンゾフェノン、2,2’−ジヒドロキシ−4,4’−ジメトキシベンゾフェノン、2,2’,4,4’−テトラヒドロキシベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン、2−ヒドロキシ−4−メトキシ−4’−メチルベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン−5−スルホン酸塩、4−フェニルベンゾフェノン、2−エチルヘキシル−4’−フェニル−ベンゾフェノン−2−カルボキシレート、2−ヒドロキシ−4−n−オクトキシベンゾフェノン、4−ヒドロキシ−3−カルボキシベンゾフェノン等のベンゾフェノン系紫外線遮蔽剤;3−(4’−メチルベンジリデン)−d,l−カンファー、3−ベンジリデン−d,l−カンファー、ウロカニン酸、ウロカニン酸エチルエステル、2−フェニル−5−メチルベンゾキサゾール、2,2’−ヒドロキシ−5−メチルフェニルベンゾトリアゾール、2−(2’−ヒドロキシ−5’−t−オクチルフェニル)ベンゾトリアゾール、2−(2’−ヒドロキシ−5’−メチルフェニルベンゾトリアゾール、ジベンザラジン、ジアニソイルメタン、4−メトキシ−4’−t−ブチルジベンゾイルメタン、5−(3,3−ジメチル−2−ノルボルニリデン)−3−ペンタン−2−オン等を挙げることができる。
The inorganic water-soluble polymer is not particularly limited, and examples thereof include bentonite, AlMg silicate (bee gum), laponite, hectorite, and silicic acid anhydride.
The UV screening agent is not particularly limited. For example, paraaminobenzoic acid (hereinafter abbreviated as PABA), PABA monoglycerin ester, N, N-dipropoxy PABA ethyl ester, N, N-diethoxy PABA ethyl ester, N, N-dimethyl ester Benzoic acid type ultraviolet screening agents such as PABA ethyl ester, N, N-dimethyl PABA butyl ester; anthranilic acid type ultraviolet screening agents such as homomentyl-N-acetyl anthranilate; amyl salicylate, menthyl salicylate, homomentyl salicylate, octyl salicylate Salicylic acid based ultraviolet screening agents such as phenyl salicylate, benzyl salicylate, p-isopropanol phenyl salicylate and the like; octyl cinnamate, ethyl-4-isopropyl cinnamate, methyl-2,5- Isopropylcinnamate, ethyl-2,4-diisopropylcinnamate, methyl-2,4-diisopropylcinnamate, propyl-p-methoxycinnamate, isopropyl-p-methoxycinnamate, isoamyl-p-methoxycinnamate, 2- Ethoxyethyl-p-methoxycinnamate, cyclohexyl-p-methoxycinnamate, ethyl-α-cyano-β-phenylcinnamate, 2-ethylhexyl-α-cyano-β-phenylcinnamate, glyceryl mono-2-ethylhexanoate UV-screening agents based on cinnamic acid such as noyl-diparamethoxycinnamate; 2,4-dihydroxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone , 2, 2 ', 4,4'-Tetrahydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4'-methylbenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonate, 4-phenylbenzophenone Benzophenone-based ultraviolet screening agents such as 2-ethylhexyl-4'-phenyl-benzophenone-2-carboxylate, 2-hydroxy-4-n-octoxybenzophenone, 4-hydroxy-3-carboxybenzophenone and the like; 3- (4 ') -Methylbenzylidene) -d, l-camphor, 3-benzylidene-d, l-camphor, urocanic acid, urocanic acid ethyl ester, 2-phenyl-5-methylbenzoxazole, 2,2'-hydroxy-5-methyl Phenyl benzotriazole, 2 (2′-hydroxy-5′-t-octylphenyl) benzotriazole, 2- (2′-hydroxy-5′-methylphenylbenzotriazole, dibenzalazine, dianisoylmethane, 4-methoxy-4′-t-butyldi Examples include benzoylmethane, 5- (3,3-dimethyl-2-norbornylidene) -3-pentan-2-one and the like.
その他薬剤成分としては特に限定されず、例えば、ビタミンA油、レチノール、パルミチン酸レチノール、イノシット、塩酸ピリドキシン、ニコチン酸ベンジル、ニコチン酸アミド、ニコチン酸DL−α−トコフェロール、アルコルビン酸リン酸マグネシウム、2−O−α−D−グルコピラノシル−L−アスコルビン酸、ビタミンD2(エルゴカシフェロール)、dl−α−トコフェロール、酢酸dl−α−トコフェロール、パントテン酸、ビオチン等のビタミン類;エストラジオール、エチニルエストラジオール等のホルモン;アルギニン、アスパラギン酸、シスチン、システイン、メチオニン、セリン、ロイシン、トリプトファン等のアミノ酸;アラントイン、アズレン等の抗炎症剤、アルブチン等の美白剤、;タンニン酸等の収斂剤;L−メントール、カンフル等の清涼剤やイオウ、塩化リゾチーム、塩化ピリドキシン等を挙げることができる。 Other pharmaceutical ingredients are not particularly limited. For example, vitamin A oil, retinol, retinol palmitate, inositol, pyridoxine hydrochloride, benzyl nicotinate, nicotinic acid amide, nicotinic acid DL-α-tocopherol, magnesium ascorbate phosphate, 2 -O-α-D-glucopyranosyl-L-ascorbic acid, vitamin D2 (ergocasiferol), dl-α-tocopherol, dl-α-tocopherol acetate, pantothenic acid, vitamins such as biotin; estradiol, ethynyl estradiol etc. Hormones; amino acids such as arginine, aspartic acid, cystine, cysteine, methionine, serine, leucine and tryptophan; anti-inflammatory agents such as allantoin and azulene; whitening agents such as arbutin; astringents such as tannic acid; Menthol, cooling agents and sulfur camphor such as, lysozyme chloride, can be mentioned pyridoxine chloride, and the like.
各種の抽出液としては特に限定されず、例えば、ドクダミエキス、オウバクエキス、メリロートエキス、オドリコソウエキス、カンゾウエキス、シャクヤクエキス、サボンソウエキス、ヘチマエキス、キナエキス、ユキノシタエキス、クララエキス、コウホネエキス、ウイキョウエキス、サクラソウエキス、バラエキス、ジオウエキス、レモンエキス、シコンエキス、アロエエキス、ショウブ根エキス、ユーカリエキス、スギナエキス、セージエキス、タイムエキス、茶エキス、海藻エキス、キューカンバーエキス、チョウジエキス、キイチゴエキス、メリッサエキス、ニンジンエキス、マロニエエキス、モモエキス、桃葉エキス、クワエキス、ヤグルマギクエキス、ハマメリスエキス、プラセンタエキス、胸腺抽出物、シルク抽出液、甘草エキス等を挙げることができる。 The various extract solutions are not particularly limited, and, for example, Dokudami extract, Ginseng extract, Meriloto extract, Odorikoso extract, licorice extract, Licorice extract, Paeonysia extract, Sabong extract, Hechima extract, Kina extract, Yukinoshita extract, Clara extract, Koho Neon extract, English extract Extract, primrose extract, rose extract, diower extract, lemon extract, shone extract, aloe extract, shrub root extract, eucalyptus extract, sugina extract, sage extract, thyme extract, tea extract, seaweed extract, cucumber extract, clove extract, raspberry extract, melissa extract , Carrot extract, Maronie extract, peach extract, peach leaf extract, mulberry extract, cornflower extract, hamamelis extract, placenta extract, thymus extract, silk extract, licorice Mention may be made of the kiss and the like.
上記各種粉体としては、ベンガラ、黄酸化鉄、黒酸化鉄、雲母チタン、酸化鉄被覆雲母チタン、酸化チタン被覆ガラスフレーク等の光輝性着色顔料、マイカ、タルク、カオリン、セリサイト、二酸化チタン、シリカ等の無機粉末やポリエチレン末、ナイロン末、架橋ポリスチレン、セルロースパウダー、シリコーン末等の有機粉末等を挙げることができる。好ましくは、官能特性向上、化粧持続性向上のため、粉末成分の一部又は全部をシリコーン類、フッ素化合物、金属石鹸、油剤、アシルグルタミン酸塩等の物質にて、公知の方法で疎水化処理して使用される。また、本発明に該当しない他の複合粉体を混合して使用するものであってもよい。 As the above various powders, bright color pigments such as bengara, yellow iron oxide, black iron oxide, mica titanium, iron oxide coated mica titanium, titanium oxide coated glass flakes, mica, talc, kaolin, sericite, titanium dioxide, Examples thereof include inorganic powders such as silica and organic powders such as polyethylene powder, nylon powder, crosslinked polystyrene, cellulose powder and silicone powder. Preferably, part or all of the powder component is treated with a substance such as silicones, a fluorine compound, a metal soap, an oil agent, an acyl glutamate salt and the like by a known method to improve sensory characteristics and cosmetic persistence. Used. In addition, other composite powders not falling under the present invention may be mixed and used.
本発明に係る粒状複合体をインキへの添加成分として使用する場合は、酸化チタン、ベンガラ、アンチモンレッド、カドミウムイエロー、コバルトブルー、紺青、群青、カーボンブラック、黒鉛などの有色顔料、及び、炭酸カルシウム、カオリン、クレー、硫酸バリウム、水酸化アルミニウム、タルク等の体質顔料を挙げることができる。さらに有機顔料としては、溶性アゾ顔料、不溶性アゾ顔料、アゾレーキ顔料、縮合アゾ顔料、銅フタロシアニン顔料、縮合多環顔料等の顔料成分;シェラック樹脂、アクリル樹脂、スチレン−アクリル樹脂、スチレン−マレイン酸樹脂、スチレン−アクリル−マレイン酸樹脂、ポリウレタン樹脂、ポリエステル樹脂、ポリアミド樹脂等のバインダー樹脂;水混和性有機溶剤等と併用して使用することができる。 When the particulate composite according to the present invention is used as an additive component to the ink, titanium oxide, red iron oxide, antimony red, cadmium yellow, cobalt blue, bitumen, ultramarine, carbon black, colored pigments such as graphite, calcium carbonate And extender pigments such as kaolin, clay, barium sulfate, aluminum hydroxide and talc. Furthermore, as organic pigments, pigment components such as soluble azo pigments, insoluble azo pigments, azo lake pigments, condensed azo pigments, copper phthalocyanine pigments, condensed polycyclic pigments, etc .; shellac resin, acrylic resin, styrene-acrylic resin, styrene-maleic acid resin Binder resins such as styrene-acrylic-maleic acid resin, polyurethane resin, polyester resin, polyamide resin; water-miscible organic solvents etc. can be used in combination.
本発明に係る粒状複合体を塗料組成物への添加成分として使用する場合は、アクリル樹脂、ポリエステル樹脂、エポキシ樹脂等の塗膜形成樹脂;着色顔料、体質顔料、光輝性顔料等の各種顔料;硬化触媒、表面調整剤、消泡剤、顔料分散剤、可塑剤、造膜助剤、紫外線吸収剤、酸化防止剤等と併用して使用することができる。また、塗料中の樹脂は、硬化性を有するものであっても、硬化性を有さないものであってもよい。 When the particulate composite according to the present invention is used as an additive component to a coating composition, coating film-forming resins such as acrylic resin, polyester resin, epoxy resin, etc .; various pigments such as coloring pigment, extender pigment, glitter pigment; It can be used in combination with a curing catalyst, a surface control agent, an antifoaming agent, a pigment dispersant, a plasticizer, a film forming aid, an ultraviolet light absorber, an antioxidant and the like. In addition, the resin in the paint may be curable or non-curable.
本発明は、上述した本発明に係る粒状複合体を含有する樹脂組成物も包含する。このような樹脂組成物は、当該粒状複合体が放熱性フィラーとして作用することによって、優れた放熱性を有するものとなる。更に、赤外線(特に近赤外線)反射能において優れたものであるから、これらの性能を有する樹脂組成物として使用することもできる。 The present invention also encompasses a resin composition containing the above-described particulate composite according to the present invention. Such a resin composition has excellent heat dissipation properties by the particulate composite acting as a heat dissipation filler. Furthermore, since it is excellent in infrared (especially near infrared) reflective power, it can also be used as a resin composition which has these performances.
本発明の六角板状酸化亜鉛粒子は、上述したように、赤外線(特に近赤外線)反射性能を有するものであるから、種々の分野における赤外線(特に近赤外線)遮蔽材として使用することもできる。 The hexagonal plate-like zinc oxide particles of the present invention, as described above, have infrared (especially near infrared) reflection performance, and can also be used as an infrared (especially near infrared) shielding material in various fields.
なお、本明細書において「含む」とは、「本質的にからなる」と、「からなる」をも包含する(The term "comprising" includes "consisting essentially of” and "consisting of.")。 In the present specification, the term "comprising" also includes "consisting essentially of" and "consisting of" (The term "comprising" includes "consisting essentially of" and "consisting of.").
以下、本発明をより具体的に説明するが、本発明は下記の例に限定されるものではない。 Hereinafter, the present invention will be described more specifically, but the present invention is not limited to the following examples.
(実施例1):XZ−1000Fへのカチオン化加水分解ケラチン処理(5質量%)
粒子径0.66μmの六角板状酸化亜鉛(XZ−1000F、堺化学工業社製)150gを水750gに添加し、十分に撹拌することにより酸化亜鉛濃度193g/Lの水性スラリーを得た。続いて、スラリーを撹搾しながら、酸化亜鉛95質量%に対してケラチンの添加量が5質量%となるように、純度15%のカチオン化加水分解ケラチン水溶液(ステアルジモニウムヒドロキシプロピル加水分解ケラチン:promois WK−SAQ、成和化成社製)52.6gを添加した。そのまま60分間熟成した後、濾過、水洗を行い、40℃で16時間乾燥させることにより、一次粒子径0.67μmのケラチン及び酸化亜鉛粒子含有粒状複合体を得た。得られた粒状複合体のサイズ及び形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
(Example 1): Cationized hydrolytic keratin treatment to XZ-1000F (5% by mass)
150 g of hexagonal plate-like zinc oxide (XZ-1000F, manufactured by Sakai Chemical Industry Co., Ltd.) having a particle diameter of 0.66 μm was added to 750 g of water and sufficiently stirred to obtain an aqueous slurry with a zinc oxide concentration of 193 g / L. Subsequently, while stirring the slurry, an aqueous solution of cationized hydrolyzed keratin (stealdimonium hydroxypropyl hydrolyzed keratin) having a purity of 15% such that the amount of keratin added is 5% by mass with respect to 95% by mass of zinc oxide : 52.6 g of promois WK-SAQ, manufactured by Sariwa Kasei Co., Ltd. were added. After aging for 60 minutes as it is, filtration, washing with water, and drying at 40 ° C. for 16 hours, a granular composite containing keratin and zinc oxide particles having a primary particle diameter of 0.67 μm was obtained. The size and form of the obtained granular composite were observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
(実施例2):XZ−1000Fへのシリル化加水分解ケラチン処理(5質量%)
粒子径0.66μmの六角板状酸化亜鉛(XZ−1000F、堺化学工業社製)150gを水750gに添加し、十分に撹枠することにより酸化亜鉛濃度193g/Lの水性スラリーを得た。続いて、スラリーを撹拌しながら、酸化亜鉛95質量%に対してケラチンの添加量が5質量%となるように、純度25%のシリル化加水分解ケラチン水溶液((ジヒドロキシメチルシリルプロポキシ)ヒドロキシプロピル加水分解ケラチン:promois WK−HSIGF、成和化成社製)31.6gを添加した。そのまま60分間熟成した後、濾過、水洗を行い、40℃で16時間乾燥させることにより、一次粒子径0.64μmのケラチン及び酸化亜鉛粒子含有粒状複合体を得た。得られた粒状複合体のサイズ及び形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
(Example 2): Silylation hydrolytic keratin treatment to XZ-1000F (5% by mass)
150 g of hexagonal plate-like zinc oxide (XZ-1000F, manufactured by Sakai Chemical Industry Co., Ltd.) having a particle diameter of 0.66 μm was added to 750 g of water and sufficiently stirred to obtain an aqueous slurry with a zinc oxide concentration of 193 g / L. Subsequently, while stirring the slurry, a 25% pure aqueous solution of silylated hydrolyzed keratin ((dihydroxymethylsilylpropoxy) hydroxypropyl hydrolized so that the amount of keratin added is 5% by mass with respect to 95% by mass of zinc oxide Degraded keratin: 31.6 g of promois WK-HSIGF (manufactured by Seiwa Kasei) was added. After aging for 60 minutes as it is, filtration, washing with water, and drying at 40 ° C. for 16 hours, a granular composite containing keratin and zinc oxide particles having a primary particle diameter of 0.64 μm was obtained. The size and form of the obtained granular composite were observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
(実施例3):XZ−1000Fへの加水分解ケラチン処理(5質量%)
粒子径0.66μmの六角板状酸化亜鉛(XZ−1000F、堺化学工業社製)150gを水750gに添加し、十分に撹枠することにより酸化亜鉛濃度193g/Lの水性スラリーを得た。続いて、スラリーを撹拌しながら、酸化亜鉛95質量%に対してケラチンの添加量が5質量%となるように、加水分解ケラチン粉体(成和化成社製)7.9gを添加した。そのまま60分間熟成した後、濾過、水洗を行い、40℃で16時間乾燥させることにより、一次粒子径0.63μmのケラチン及び酸化亜鉛粒子含有粒状複合体を得た。得られた粒状複合体のサイズ及び形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
(Example 3): Hydrolysis keratin treatment to XZ-1000F (5 mass%)
150 g of hexagonal plate-like zinc oxide (XZ-1000F, manufactured by Sakai Chemical Industry Co., Ltd.) having a particle diameter of 0.66 μm was added to 750 g of water and sufficiently stirred to obtain an aqueous slurry with a zinc oxide concentration of 193 g / L. Subsequently, while the slurry was stirred, 7.9 g of a hydrolyzed keratin powder (manufactured by Seiwa Kasei Co., Ltd.) was added such that the amount of keratin added was 5% by mass with respect to 95% by mass of zinc oxide. After aging for 60 minutes as it is, filtration, washing with water, and drying at 40 ° C. for 16 hours, a granular composite containing keratin and zinc oxide particles having a primary particle diameter of 0.63 μm was obtained. The size and form of the obtained granular composite were observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
(実施例4):XZ−1000Fへの天然ケラチン処理(5質量%)
粒子径0.66μmの六角板状酸化亜鉛(XZ−1000F、堺化学工業社製)150gを水750gに添加し、十分に撹枠することにより酸化亜鉛濃度193g/Lの水性スラリーを得た。続いて、スラリーを撹拌しながら、酸化亜鉛95質量%に対してケラチンの添加量が5質量%となるように、純度5%の天然ケラチン水溶液(成和化成社製)158.0gを添加した。そのまま60分間熟成した後、濾過、水洗を行い、40℃で16時間乾燥させることにより、一次粒子径0.66μmのケラチン及び酸化亜鉛粒子含有粒状複合体を得た。得られた粒状複合体のサイズ及び形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
(Example 4): Natural keratin treatment to XZ-1000F (5% by mass)
150 g of hexagonal plate-like zinc oxide (XZ-1000F, manufactured by Sakai Chemical Industry Co., Ltd.) having a particle diameter of 0.66 μm was added to 750 g of water and sufficiently stirred to obtain an aqueous slurry with a zinc oxide concentration of 193 g / L. Subsequently, while stirring the slurry, 158.0 g of a natural keratin aqueous solution (manufactured by Siwa Chemical Co., Ltd.) having a purity of 5% was added so that the amount of keratin added was 5% by mass with respect to 95% by mass of zinc oxide . After aging for 60 minutes as it is, filtration, washing with water and drying at 40 ° C. for 16 hours were carried out to obtain a granular composite containing keratin and zinc oxide particles having a primary particle diameter of 0.66 μm. The size and form of the obtained granular composite were observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
(実施例5):XZ−1000Fへのカチオン化加水分解ケラチン処理(1質量%)
粒子径0.66μmの六角板状酸化亜鉛(XZ−1000F、堺化学工業社製)150gを水750gに添加し、十分に撹拌することにより酸化亜鉛濃度193g/Lの水性スラリーを得た。続いて、スラリーを撹拌しながら、酸化亜鉛99質量%に対してケラチンの添加量が1質量%となるように、純度15%のカチオン化加水分解ケラチン水溶液(ステアルジモニウムヒドロキシプロピル加水分解ケラチン:promois WK−SAQ、成和化成社製)10.1gを添加した。そのまま60分間熟成した後、濾過、水洗を行い、40℃で16時間乾燥させることにより、一次粒子径0.70μmのケラチン及び酸化亜鉛粒子含有粒状複合体を得た。得られた粒状複合体のサイズ及び形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
(Example 5): Cationized hydrolytic keratin treatment to XZ-1000F (1% by mass)
150 g of hexagonal plate-like zinc oxide (XZ-1000F, manufactured by Sakai Chemical Industry Co., Ltd.) having a particle diameter of 0.66 μm was added to 750 g of water and sufficiently stirred to obtain an aqueous slurry with a zinc oxide concentration of 193 g / L. Subsequently, while stirring the slurry, an aqueous solution of cationized hydrolyzed keratin (stealdimonium hydroxypropyl hydrolyzed keratin: purity 15% so that the amount of keratin added is 1% by mass with respect to 99% by mass of zinc oxide 10.1 g of promois WK-SAQ, manufactured by Sariwa Kasei Co., Ltd. were added. After aging for 60 minutes as it was, filtration, washing with water and drying at 40 ° C. for 16 hours were carried out to obtain a granular composite containing keratin and zinc oxide particles having a primary particle diameter of 0.70 μm. The size and form of the obtained granular composite were observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
(実施例6)XZ−1000Fへのカチオン化加水分解ケラチン処理(10質量%)
ケラチンの添加量について、酸化亜鉛90質量%に対するケラチンの添加量が10質量%となるよう変更したした以外は、実施例1及び5と同様にして、ケラチン及び酸化亜鉛粒子含有粒状複合体を得、形態観察及び物性評価を行った。
(Example 6) Cationized hydrolytic keratin treatment (10% by mass) to XZ-1000F
A keratin and zinc oxide particle-containing particulate composite is obtained in the same manner as in Examples 1 and 5 except that the addition amount of keratin is changed so that the addition amount of keratin to 90% by mass of zinc oxide is 10% by mass. , Form observation and physical property evaluation.
(実施例7)XZ−1000Fへのカチオン化加水分解ケラチン処理(20質量%)
ケラチンの添加量について、酸化亜鉛80質量%に対するケラチンの添加量を20質量%となるよう変更した以外は、実施例1及び5と同様にして、ケラチン及び酸化亜鉛粒子含有粒状複合体を得、形態観察及び物性評価を行った。
(Example 7) Cationized hydrolytic keratin treatment (20% by mass) to XZ-1000F
The keratin and zinc oxide particle-containing granular composite is obtained in the same manner as in Examples 1 and 5 except that the addition amount of keratin relative to 80% by mass of zinc oxide is changed to 20% by mass. Morphological observation and physical property evaluation were performed.
(実施例8):XZ−3000Fへのカチオン化加水分解ケラチン処理(5質量%)
粒子径2.08μmの六角板状酸化亜鉛(XZ−3000F、堺化学工業社製)150gを水750gに添加し、十分に撹拌することにより酸化亜鉛濃度193g/Lの水性スラリーを得た。続いて、スラリーを撹拌しながら、酸化亜鉛95質量%に対してケラチンの添加量が5質量%となるように、純度15%のカチオン化加水分解ケラチン水溶液(ステアルジモニウムヒドロキシプロピル加水分解ケラチン:promois WK−SAQ、成和化成社製)52.6gを添加した。そのまま60分間熟成した後、濾過、水洗を行い、40℃で16時間乾燥させることにより、一次粒子径2.15μmのケラチン及び酸化亜鉛粒子含有粒状複合体を得た。得られた粒状複合体のサイズ及び形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
(Example 8): Cationic hydrolytic keratin treatment to XZ-3000F (5% by mass)
150 g of hexagonal plate-like zinc oxide (XZ-3000F, manufactured by Sakai Chemical Industry Co., Ltd.) having a particle diameter of 2.08 μm was added to 750 g of water and sufficiently stirred to obtain an aqueous slurry with a zinc oxide concentration of 193 g / L. Subsequently, while stirring the slurry, an aqueous solution of cationized hydrolyzed keratin (stealdimonium hydroxypropyl hydrolyzed keratin: purity 15% so that the amount of keratin added is 5% by mass with respect to 95% by mass of zinc oxide 52.6 g of promois WK-SAQ, manufactured by Sariwa Kasei Co., Ltd. was added. After aging for 60 minutes as it is, filtration, washing with water and drying at 40 ° C. for 16 hours were carried out to obtain a granular composite containing keratin and zinc oxide particles having a primary particle diameter of 2.15 μm. The size and form of the obtained granular composite were observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
(比較例1):処理なしXZ−1000F
六角板状酸化亜鉛(XZ−1000F、堺化学工業社製)を比較対象の粒子とした。一次粒子径は0.66μmであった。粒子の形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。なお、上記の内容から明らかな通り、当該粒子は実施例l、2、3、4及び5で得られたケラチン及び酸化亜鉛粒子含有粒状複合体の母体となる酸化亜鉛粒子である。
(Comparative Example 1): No treatment XZ-1000F
Hexagonal plate-like zinc oxide (XZ-1000F, manufactured by Sakai Chemical Industry Co., Ltd.) was used as particles for comparison. The primary particle size was 0.66 μm. The morphology of the particles was observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.). In addition, as is clear from the above contents, the particles are zinc oxide particles serving as a matrix of the keratin- and zinc oxide particle-containing particulate composites obtained in Examples 1, 2, 3, 4 and 5.
(比較例2):処理なしXZ−3000F
六角板状酸化亜鉛(XZ−3000F、堺化学工業社製)を比較対象の粒子とした。一次粒子径は2.08μmであった。粒子の形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。なお、当該粒子は実施例6で得られたケラチン及び酸化亜鉛粒子含有粒状複合体の母体となる酸化亜鉛粒子である。
(Comparative Example 2): No treatment XZ-3000F
Hexagonal plate-like zinc oxide (XZ-3000F, manufactured by Sakai Chemical Industry Co., Ltd.) was used as particles for comparison. The primary particle size was 2.08 μm. The morphology of the particles was observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.). In addition, the said particle | grain is a zinc oxide particle used as the base of the keratin and the zinc oxide particle containing granular composite body obtained in Example 6. FIG.
(比較例3):不定形酸化亜鉛粒子
不定形酸化亜鉛(酸化亜鉛1種:JIS規格、堺化学工業社製)を比較対象の粒子とした。一次粒子径は0.48μmであった。粒子の形態を走査型電子顕微鏡JSM−6510A(日本電子社製)で観察した。
Comparative Example 3 Amorphous Zinc Oxide Particles Amorphous zinc oxide (type 1 zinc oxide: JIS standard, manufactured by Sakai Chemical Industry Co., Ltd.) was used as particles to be compared. The primary particle size was 0.48 μm. The morphology of the particles was observed with a scanning electron microscope JSM-6510A (manufactured by Nippon Denshi Co., Ltd.).
MIU(平均摩擦係数)の測定
MIU(平均摩擦係数)は、ケラチン及び六角状酸化亜鉛粒子を含む粒状複合体を、KES−SE摩擦感テスター(カトーテック社製)で測定した。具体的には、スライドガラスに25mm幅の両面テープを貼り、当該粒状複合体(粉体)を載せ、化粧用パフで伸ばし、KES−SE摩擦感テスター(カトーテック社製)によりMIU(平均摩擦係数)を測定した。摩擦測定荷重25gf、表面測定試料移動速度1mm/sec、測定距離範囲20mmの条件で測定を行った。センサーとしては、シリコーン接触子(人間の指を想定した凹凸が施されたシリコーンゴム製の摩擦子)を用いた。
Measurement of MIU (average friction coefficient) MIU (average friction coefficient) was measured with a KES-SE friction tester (manufactured by Kato Tech Co., Ltd.) for a granular composite containing keratin and hexagonal zinc oxide particles. Specifically, a double-sided tape with a width of 25 mm is attached to a slide glass, the granular composite (powder) is placed, stretched with a cosmetic puff, and MIU (average friction) is measured by a KES-SE friction tester (manufactured by Kato Tech). Coefficient) was measured. The measurement was performed under the conditions of a friction measurement load of 25 gf, a surface measurement sample moving speed of 1 mm / sec, and a measurement distance range of 20 mm. As a sensor, a silicone contactor (frictional element made of silicone rubber with irregularities assumed to be a human finger) was used.
MMD(摩擦係数の平均偏差)の測定
MMD(摩擦係数の平均偏差)は、ケラチン及び六角状酸化亜鉛粒子を含む粒状複合体を、KES−SE摩擦感テスター(カトーテック社製)で測定した。具体的には、スライドガラスに25mm幅の両面テープを貼り、当該粒状複合体(粉体)を載せ、化粧用パフで伸ばし、KES−SE摩擦感テスター(カトーテック社製)によりMMD(摩擦係数の平均偏差)を測定した。摩擦測定荷重25gf、表面測定試料移動速度1mm/sec、測定距離範囲20mmの条件で測定を行った。センサーとしては、シリコーン接触子(人間の指を想定した凹凸が施されたシリコーンゴム製の摩擦子)を用いた。
Measurement of MMD ( Average Deviation of Friction Coefficient) MMD ( average deviation of friction coefficient) was measured for a granular composite containing keratin and hexagonal zinc oxide particles with a KES-SE friction tester (manufactured by Kato Tech). Specifically, a double-sided tape with a width of 25 mm is attached to a slide glass, the granular composite (powder) is placed, stretched with a cosmetic puff, and the MMD (coefficient of friction) is measured by a KES-SE friction tester (manufactured by Kato Tech). The average deviation of The measurement was performed under the conditions of a friction measurement load of 25 gf, a surface measurement sample moving speed of 1 mm / sec, and a measurement distance range of 20 mm. As a sensor, a silicone contactor (frictional element made of silicone rubber with irregularities assumed to be a human finger) was used.
一次粒子径の測定
六角状酸化亜鉛粒子及び粒状複合体の一次粒子径は、走査型電子顕微鏡(SEM)(JSM−6510A:日本電子社製)で撮影した写真の2000〜50000倍の視野での対角線径(六角状酸化亜鉛粒子又は粒状複合体が六角板状の形状である場合、六角板状面の3本の対角線のうちの任意の1本の対角線の長さ)(μm)を粒子100個分について計測し、その累積分布の50%から求めた値である。
不定形粒子の一次粒子径は、走査型電子顕微鏡(SEM)(JSM−6510A:日本電子社製)で当該粒子を撮影した写真の2000〜50000倍の視野におけるXY軸平均径(粒子を挟むX軸方向及びY軸方向、それぞれ二本の平行線の間隔を平均した長さ)で定義される粒子径(μm)を粒子100個分について測定し、その累積分布の50%から求めた値である。
Measurement of Primary Particle Size The primary particle size of the hexagonal zinc oxide particles and the particulate complex is 2000 to 50000 times the photograph taken with a scanning electron microscope (SEM) (JSM-6510A: manufactured by Nippon Denshi Co., Ltd.) Diameter in the field of view (if the hexagonal zinc oxide particles or granular composite is in the form of a hexagonal plate, the length of any one of the three diagonals of the hexagonal plate surface) (μm ) Was measured for 100 particles, and the value was obtained from 50% of the cumulative distribution.
The primary particle diameter of the irregularly shaped particles is the average XY axis diameter (X sandwiching the particles in a field of 2000 to 50000 times of the photograph of the particles taken with a scanning electron microscope (SEM) (JSM-6510A: made by Nippon Denshi Co.) The particle diameter (μm) defined by the axial direction and the Y-axis direction, the length obtained by averaging the distance between two parallel lines) is measured for 100 particles, and the value determined from 50% of the cumulative distribution is there.
粒状複合体中のケラチン含有率の測定
粒状複合体及び、その原料の六角状酸化亜鉛粒子を、それぞれ2gずつ坩堝に入れ、電気炉中500℃で1時間加熱した。それぞれ、加熱後の重量を測定した。粒状複合体に含まれるケラチンは全て消失しており、且つ、原料である六角状酸化亜鉛粒子の減少率はいずれであっても同じであるとして、粒状複合体中のケラチン含有率(質量%)を算出した。
Measurement of Keratin Content in Particulate Composite The particulate composite and the hexagonal zinc oxide particles as a raw material thereof were placed in a crucible of 2 g each and heated in an electric furnace at 500 ° C. for 1 hour. Each weight was measured after heating. The keratin content (% by mass) in the particulate composite is assumed to be all keratin in the particulate composite has disappeared, and the reduction rate of the hexagonal zinc oxide particles as the raw material is the same regardless of which Was calculated.
分光反射率の測定
分光反射率は、分光光度計(日本分光製V−570型)により測定した。より具体的には、各実施例及び各比較例で得られた粒状複合体又は粒子を専用セルに入れ、分光光度計に装着し、各波長における分光反射率を測定した。反射率=100−吸収率となるため、吸収がある程、反射率は下がることとなり、好ましい。
Measurement of spectral reflectance The spectral reflectance was measured by a spectrophotometer (V-570, manufactured by JASCO Corporation). More specifically, the particulate composite or particles obtained in each Example and each Comparative Example were placed in a dedicated cell, mounted on a spectrophotometer, and the spectral reflectance at each wavelength was measured. Since the reflectance = 100−absorptivity, the more the absorption, the lower the reflectance, which is preferable.
以上の検討結果は下記表に示した。また、得られた粒子の物性の評価結果も下記表に示した。さらに、用いた各ケラチンの数平均分子量も下記表に示した。なお、分光反射率測定結果は、図1〜図2に示す。 The above examination results are shown in the following table. Further, the evaluation results of the physical properties of the obtained particles are also shown in the following table. Furthermore, the number average molecular weight of each keratin used is also shown in the following table. The spectral reflectance measurement results are shown in FIGS. 1 and 2.
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