JP2023147613A - Aqueous dispersion and cosmetic - Google Patents
Aqueous dispersion and cosmetic Download PDFInfo
- Publication number
- JP2023147613A JP2023147613A JP2022055208A JP2022055208A JP2023147613A JP 2023147613 A JP2023147613 A JP 2023147613A JP 2022055208 A JP2022055208 A JP 2022055208A JP 2022055208 A JP2022055208 A JP 2022055208A JP 2023147613 A JP2023147613 A JP 2023147613A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- aqueous dispersion
- oxide particles
- coated zinc
- coating film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000006185 dispersion Substances 0.000 title claims abstract description 111
- 239000002537 cosmetic Substances 0.000 title claims description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 244
- 239000002245 particle Substances 0.000 claims abstract description 129
- 239000011787 zinc oxide Substances 0.000 claims abstract description 121
- 239000011248 coating agent Substances 0.000 claims abstract description 66
- 238000000576 coating method Methods 0.000 claims abstract description 66
- 238000002834 transmittance Methods 0.000 claims abstract description 42
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 24
- 239000011164 primary particle Substances 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 18
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 12
- 238000003917 TEM image Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-DYCDLGHISA-N deuterium hydrogen oxide Chemical compound [2H]O XLYOFNOQVPJJNP-DYCDLGHISA-N 0.000 claims abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 13
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Abstract
Description
本発明は、水系分散体及び化粧料に関する。 The present invention relates to an aqueous dispersion and a cosmetic.
微粒子酸化亜鉛は紫外線遮蔽性や透明性が高いため、紫外線散乱剤として日焼け止め化粧料などに用いられてきた。このような紫外線散乱剤として、粒子サイズ100nm以下の酸化亜鉛が多く用いられるが、表面活性の抑制やきしみ緩和、凝集防止を目的として粒子表面に撥水処理等の表面処理をして利用することが多い。 Particulate zinc oxide has high UV-shielding properties and transparency, so it has been used as a UV-scattering agent in sunscreen cosmetics and the like. Zinc oxide with a particle size of 100 nm or less is often used as such a UV scattering agent, but it can also be used after surface treatment such as water-repellent treatment is applied to the particle surface for the purpose of suppressing surface activity, alleviating squeaks, and preventing agglomeration. There are many.
しかしながら、このような表面処理微粒子酸化亜鉛も少なからず凝集しており、分散体を製造する際には何らかの分散処理を施す、または、分散剤を併用する等の対応をしなければ、粒子本来の持っている性能を発揮することができなかった(例えば、特許文献1及び2参照)。
また、微粒子分散体は、製剤への配合のしやすさや製剤の感触向上といった点から、高濃度かつ低粘度で、分散剤量の少ない分散体が望ましい。しかし、微粒子酸化亜鉛は比表面積が高いことから、少量の分散剤で粉体濃度を高めることが困難であった。
However, these surface-treated fine particles of zinc oxide also aggregate to some extent, and unless some kind of dispersion treatment is performed or a dispersant is used together when producing a dispersion, the original particle size will be lost. It was not possible to demonstrate the performance that it has (for example, see Patent Documents 1 and 2).
Further, the fine particle dispersion is desirably a dispersion with high concentration, low viscosity, and a small amount of dispersant from the viewpoint of ease of blending into the formulation and improvement of the feel of the formulation. However, since particulate zinc oxide has a high specific surface area, it has been difficult to increase the powder concentration with a small amount of dispersant.
本発明は、低粘度かつ高濃度で、従来よりも分散剤量が少ない有機ケイ素表面被覆酸化亜鉛粒子の水系分散体を提供することを目的とするものである。 An object of the present invention is to provide an aqueous dispersion of organosilicon surface-coated zinc oxide particles that has a low viscosity, a high concentration, and a smaller amount of dispersant than conventional dispersants.
本発明は、有機ケイ素表面被覆酸化亜鉛粒子(A)、非イオン性界面活性剤(B)、多価アルコール(C)、及び、水(D)を含む水系分散体であって、
上記有機ケイ素表面被覆酸化亜鉛粒子(A)は、透過型電子顕微鏡写真から測定した一次粒子径が0.1μm以下であり、
上記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量は、水系分散体全量に対して60質量%以上であり、
波長600nmの(乾燥後塗膜の平行光透過率)/(塗布直後塗膜の平行光透過率)の比が0.8以上であり、
上記乾燥後塗膜は、前記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%の水系分散体を室温にて塗布した後に50℃で2時間乾燥させたものであり、
上記塗布直後塗膜は、前記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%の水系分散体を室温にて塗布後5分以内のものである
ことを特徴とする水系分散体に関する。
The present invention is an aqueous dispersion comprising organosilicon surface-coated zinc oxide particles (A), a nonionic surfactant (B), a polyhydric alcohol (C), and water (D),
The organosilicon surface-coated zinc oxide particles (A) have a primary particle diameter of 0.1 μm or less as measured from a transmission electron micrograph,
The content of the organosilicon surface-coated zinc oxide particles (A) is 60% by mass or more based on the total amount of the aqueous dispersion,
The ratio of (parallel light transmittance of the coating film after drying) / (parallel light transmittance of the coating film immediately after application) at a wavelength of 600 nm is 0.8 or more,
The dried coating film is obtained by applying an aqueous dispersion containing 60% by mass of the organosilicon surface-coated zinc oxide particles (A) at room temperature and then drying it at 50°C for 2 hours,
The freshly applied coating film is an aqueous dispersion that is obtained within 5 minutes after application of the aqueous dispersion containing 60% by mass of the organosilicon surface-coated zinc oxide particles (A) at room temperature. Regarding.
上記有機ケイ素表面被覆酸化亜鉛粒子(A)は、イソプロピルアルコール中に入れ、超音波ホモジナイザーで定格出力600W、振動振幅100%の超音波を常温で30秒間照射して分散した分散液のレーザー回折散乱法での体積基準におけるメジアン径が0.15μm以下であることが好ましい。
上記非イオン性界面活性剤(B)の含有量は、有機ケイ素表面被覆酸化亜鉛粒子(A)100質量%に対して8.5質量%以下であることが好ましい。
上記有機ケイ素表面被覆酸化亜鉛粒子(A)は、水系分散体中におけるメジアン径が0.15μm以下であることが好ましい。
上記水系分散体は、25℃における粘度が4,000mPa・s以下であることが好ましい。
上記乾燥後塗膜を干渉顕微鏡で観察した際に、100μm×100μm視野中に2μm以上の凝集物が30個以下であり、かつ、光沢(20°グロス)が80以上となることが好ましい。
The above organosilicon surface-coated zinc oxide particles (A) are dispersed by laser diffraction scattering of a dispersion liquid that is dispersed by placing it in isopropyl alcohol and irradiating it with ultrasonic waves with a rated output of 600 W and a vibration amplitude of 100% for 30 seconds at room temperature using an ultrasonic homogenizer. It is preferable that the median diameter on a volume basis in the method is 0.15 μm or less.
The content of the nonionic surfactant (B) is preferably 8.5% by mass or less based on 100% by mass of the organosilicon surface-coated zinc oxide particles (A).
The organosilicon surface-coated zinc oxide particles (A) preferably have a median diameter of 0.15 μm or less in the aqueous dispersion.
The aqueous dispersion preferably has a viscosity of 4,000 mPa·s or less at 25°C.
When the dried coating film is observed with an interference microscope, it is preferable that there are no more than 30 aggregates of 2 μm or more in a 100 μm×100 μm field of view, and the gloss (20° gloss) is 80 or more.
上記非イオン性界面活性剤(B)は、オルガノポリシロキサン系の非イオン活性剤であることが好ましい。
上記多価アルコール(C)は、プロピレングリコール、ブチレングリコール、ペンタンジオール、ジプロピレングリコール、ヘキサンジオール、ヘプタンジオール及びグリセリンからなる群より選ばれる1種又は2種以上の多価アルコールであることが好ましい。
本発明は、上述の水系分散体を含有することを特徴とする化粧料でもある。
The nonionic surfactant (B) is preferably an organopolysiloxane-based nonionic surfactant.
The polyhydric alcohol (C) is preferably one or more polyhydric alcohols selected from the group consisting of propylene glycol, butylene glycol, pentanediol, dipropylene glycol, hexanediol, heptanediol, and glycerin. .
The present invention also provides a cosmetic containing the above-mentioned aqueous dispersion.
本発明により、分散剤量を低減した微粒子酸化亜鉛の水系分散体を得ることができる。さらに、本発明の水系分散体は低粘度かつ高濃度であるため、化粧料、放熱性組成物等に好適に配合することができる。 According to the present invention, it is possible to obtain an aqueous dispersion of particulate zinc oxide with a reduced amount of dispersant. Furthermore, since the aqueous dispersion of the present invention has low viscosity and high concentration, it can be suitably blended into cosmetics, heat dissipating compositions, and the like.
以下に、本発明を詳細に説明する。
本発明の水系分散体は、易分散性に優れた有機ケイ素表面被覆酸化亜鉛粒子(A)を含有するものである。すなわち、非常に高い分散性を有する有機ケイ素表面被覆酸化亜鉛粒子(A)を使用するため、分散剤が少量であっても、微粒子酸化亜鉛が高濃度で安定に分散した水系分散体を得ることができるものである。
このような水系分散体は、少量で所望量の微粒子酸化亜鉛を配合できるため、製剤への配合が容易である点からも好ましい。
The present invention will be explained in detail below.
The aqueous dispersion of the present invention contains organosilicon surface-coated zinc oxide particles (A) with excellent easy dispersibility. That is, since the organosilicon surface-coated zinc oxide particles (A) having extremely high dispersibility are used, even if the amount of dispersant is small, an aqueous dispersion in which fine particulate zinc oxide is stably dispersed at a high concentration can be obtained. It is something that can be done.
Such an aqueous dispersion is preferable from the viewpoint that it is easy to incorporate a desired amount of fine particulate zinc oxide into a preparation in a small amount.
上記有機ケイ素表面被覆酸化亜鉛粒子(A)は、易分散性に優れ、溶媒中で一次粒子に近い状態まで分散すると考えられる。
このような有機ケイ素表面被覆酸化亜鉛粒子(A)は、透過型電子顕微鏡写真から測定した一次粒子径が0.1μm以下となるものである。
It is thought that the organosilicon surface-coated zinc oxide particles (A) have excellent dispersibility and are dispersed in a solvent to a state close to that of primary particles.
Such organosilicon surface-coated zinc oxide particles (A) have a primary particle diameter of 0.1 μm or less as measured from a transmission electron micrograph.
本発明における一次粒子径は、具体的には、透過型電子顕微鏡JEM-1200EX II(日本電子社製)で撮影した写真の2000~50000倍の視野での定方向径(粒子を挟む一定方向の二本の平行線の間隔;画像上のどのような形状の粒子についても、一定方向で測定した)で定義される粒子径(μm)であって、TEM写真内の一次粒子250個の定方向径を計測し、その累積分布の平均値を求めたものである。
上記一次粒子径の測定方法については、図1を添付した。
上記一次粒子径は、0.005μm以上0.08μm未満であることがより好ましい。
Specifically, the primary particle diameter in the present invention is defined as the diameter in a fixed direction (in a fixed direction sandwiching the particle) in a field of view 2000 to 50000 times larger than a photograph taken with a transmission electron microscope JEM-1200EX II (manufactured by JEOL Ltd.). Particle diameter (μm) defined as the distance between two parallel lines (measured in a fixed direction for particles of any shape on the image), which is defined as the fixed direction of 250 primary particles in the TEM photograph. The diameter was measured and the average value of the cumulative distribution was calculated.
Figure 1 is attached for the method for measuring the primary particle diameter.
The primary particle diameter is more preferably 0.005 μm or more and less than 0.08 μm.
本発明の水系分散体は、有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%の水系分散体における波長600nmの(乾燥後塗膜の平行光透過率)/(塗布直後塗膜の平行光透過率)の比が0.8以上である。このような値を満たすものは、乾燥凝集が抑制されていることから、本発明の水系分散体において酸化亜鉛粒子が良好に分散されている。
以下、当該パラメータにおける平行光透過率について、詳述する。
The aqueous dispersion of the present invention has a wavelength of 600 nm in an aqueous dispersion in which the content of organosilicon surface-coated zinc oxide particles (A) is 60% by mass. (parallel light transmittance) is 0.8 or more. In the aqueous dispersion of the present invention, the zinc oxide particles are well dispersed in the aqueous dispersion of the present invention because dry aggregation is suppressed in the dispersion satisfying such values.
The parallel light transmittance in this parameter will be explained in detail below.
(平行光透過率)
上記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%の水系分散体を室温にて塗布し、塗布直後(本発明においては、塗布後5分以内とする)を塗膜1、塗膜1を50℃で2時間乾燥させたものを塗膜2として、それぞれの波長600nmにおける平行光線透過率1(%)、平行光線透過率2(%)を測定した。
上記塗膜の作成、乾燥条件、平行光透過率の測定等については、実施例に記載の方法により行うことができる。有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%を超える水系分散体については、水系分散体の一部を取り出し、有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%となるよう水で希釈してから塗膜の作成に用いる。希釈時の攪拌手段は特に限定されず、攪拌羽やホモディスパーなど一般的に使用される攪拌機で作成することができる。
(Parallel light transmittance)
The aqueous dispersion having a content of 60% by mass of the organosilicon surface-coated zinc oxide particles (A) was applied at room temperature, and immediately after application (in the present invention, within 5 minutes after application) was applied as coating film 1. Coating film 1 was dried at 50° C. for 2 hours to form coating film 2, and parallel light transmittance 1 (%) and parallel light transmittance 2 (%) at a wavelength of 600 nm were measured.
The preparation of the coating film, drying conditions, measurement of parallel light transmittance, etc. can be carried out by the methods described in Examples. For an aqueous dispersion in which the content of organosilicon surface-coated zinc oxide particles (A) exceeds 60% by mass, a part of the aqueous dispersion is taken out and the content of organosilicon surface-coated zinc oxide particles (A) is 60% by mass. % with water and then use it to create a coating film. The stirring means used during dilution is not particularly limited, and a commonly used stirrer such as a stirring blade or a homodisper can be used.
平行光線透過率1(%)、平行光線透過率2(%)の値が大きい程、可視光透明性が高いことを意味し、平行光透過率1に対する平行光透過率2の割合が高いほど、乾燥凝集が少なく白浮きが抑制されていることを意味する。
上記平行光線透過率1(%)は、35%以上であることが好ましく、45%以上であることがより好ましい。
また、上記平行光線透過率2(%)は、30%以上であることが好ましく、40%以上であることがより好ましい。
The larger the values of parallel light transmittance 1 (%) and parallel light transmittance 2 (%), the higher the visible light transparency, and the higher the ratio of parallel light transmittance 2 to parallel light transmittance 1. This means that there is little dry agglomeration and white cast is suppressed.
The parallel light transmittance 1 (%) is preferably 35% or more, more preferably 45% or more.
Further, the parallel light transmittance 2 (%) is preferably 30% or more, more preferably 40% or more.
本発明において、平行光透過率1に対する平行光透過率2の割合、すなわち、(塗膜2の平行光線透過率2)/(塗膜1の平行光線透過率1)は、0.8以上である。上述の割合が0.8以上であると、充分に白浮きが抑制されていることを意味する。上記(塗膜2の平行光線透過率2)/(塗膜1の平行光線透過率1)は、0.9以上であることが好ましい。 In the present invention, the ratio of parallel light transmittance 2 to parallel light transmittance 1, that is, (parallel light transmittance 2 of coating film 2)/(parallel light transmittance 1 of coating film 1) is 0.8 or more. be. When the above-mentioned ratio is 0.8 or more, it means that whitening is sufficiently suppressed. The above (parallel light transmittance 2 of coating film 2)/(parallel light transmittance 1 of coating film 1) is preferably 0.9 or more.
本発明の水系分散体は、更に、塗膜1,2を形成した場合に当該塗膜が以下のような性質を有するものであることが好ましい。 When the aqueous dispersion of the present invention forms coating films 1 and 2, it is preferable that the coating films have the following properties.
(塗膜凹凸)
上記塗膜2の表面を干渉顕微鏡で観察し、100μm×100μm内に観察された2μm以上の凝集物は、30個以下であることが好ましく、20個以下であることがより好ましい。上記凝集物が30個以下であると、微粒子酸化亜鉛の乾燥凝集が発生しにくく、凹凸が少ないことを意味するため好ましい。
上記凝集物は、実施例に記載の方法により観察することができる。
(paint film unevenness)
When the surface of the coating film 2 is observed with an interference microscope, the number of aggregates of 2 μm or more observed within 100 μm×100 μm is preferably 30 or less, more preferably 20 or less. It is preferable that the number of aggregates is 30 or less because it means that dry aggregation of fine zinc oxide particles is difficult to occur and there are few irregularities.
The above-mentioned aggregates can be observed by the method described in the Examples.
(光沢(20°グロス))
上記塗膜2の光沢は、80以上であることが好ましい。光沢(20°グロス)の値が大きいほど、作成した塗膜内部における微粒子酸化亜鉛の分散性が高いことで乾燥凝集も起こりにくく、塗膜表面の凹凸が少ないことを意味する。上記光沢は、100以上であることがより好ましい。
上記光沢(20°グロス)は、実施例に記載の方法で測定することができる。
(Gloss (20° gloss))
The gloss of the coating film 2 is preferably 80 or higher. The larger the value of gloss (20° gloss), the higher the dispersibility of fine zinc oxide particles within the created coating film, which means that dry aggregation is less likely to occur and the coating film surface has fewer irregularities. The gloss is more preferably 100 or more.
The above gloss (20° gloss) can be measured by the method described in Examples.
本発明において使用する有機ケイ素表面被覆酸化亜鉛粒子は、酸化亜鉛粒子を有機ケイ素化合物によって表面処理したものである。
上記有機ケイ素化合物としては加水分解によりシラノール性水酸基を生成する化合物であれば特に限定されず、例えば、メチルトリエトキシシラン、メチルトリメトキシシラン、メチルトリクロロシラン、ジメチルジエトキシシラン、ジメチルジメトキシシラン、ジメチルジクロロシラン、フェニルトリエトキシシラン、フェニルトリメトキシシラン、フェニルトリクロロシラン、ヘキシルトリエトキシシラン、ヘキシルトリメトキシシラン、ヘキシルトリクロロシラン、オクチルトリエトキシシラン、オクチルトリメトキシシラン、オクチルトリクロロシラン、デシルトリエトキシシラン、デシルトリメトキシシラン、デシルトリクロロシラン、テトラエトキシシラン、トリメチルクロロシラン、ヘキサメチルジシラザン、ヘキサメチルジシロキサンおよびパーフルオロアルキルトリメトキシシラン、さらに、メチルハイドロジェンポリシロキサンやジメチルポリシロキサン等のオルガノポリシロキサンや、トリエトキシビニルシランやジフェニルジメトキシシラン等のシランカップリング剤を挙げることができる。上記有機ケイ素化合物としては、一種又は二種以上を併用してもよい。
The organosilicon surface-coated zinc oxide particles used in the present invention are zinc oxide particles surface-treated with an organosilicon compound.
The above-mentioned organosilicon compound is not particularly limited as long as it is a compound that generates a silanol hydroxyl group by hydrolysis, and examples thereof include methyltriethoxysilane, methyltrimethoxysilane, methyltrichlorosilane, dimethyldiethoxysilane, dimethyldimethoxysilane, and dimethyl Dichlorosilane, phenyltriethoxysilane, phenyltrimethoxysilane, phenyltrichlorosilane, hexyltriethoxysilane, hexyltrimethoxysilane, hexyltrichlorosilane, octyltriethoxysilane, octyltrimethoxysilane, octyltrichlorosilane, decyltriethoxysilane, Decyltrimethoxysilane, decyltrichlorosilane, tetraethoxysilane, trimethylchlorosilane, hexamethyldisilazane, hexamethyldisiloxane and perfluoroalkyltrimethoxysilane, as well as organopolysiloxanes such as methylhydrogenpolysiloxane and dimethylpolysiloxane. , silane coupling agents such as triethoxyvinylsilane and diphenyldimethoxysilane. The above organosilicon compounds may be used alone or in combination of two or more.
有機ケイ素被覆量は、ケイ素換算で、0.1質量%以上、0.6質量%以下であることが好ましい。0.1質量%未満であると、充分な撥水効果を発揮できないおそれがある。0.6質量%より多いと、酸化亜鉛の純分が下がり性能が低下するおそれがある。 The amount of organic silicon coating is preferably 0.1% by mass or more and 0.6% by mass or less in terms of silicon. If it is less than 0.1% by mass, there is a risk that a sufficient water repellent effect may not be exhibited. If it is more than 0.6% by mass, the purity of zinc oxide may decrease and the performance may deteriorate.
上記有機ケイ素被覆量は、プレス機にて成形した有機ケイ素表面被覆酸化亜鉛粒子を、蛍光X線分析装置(リガク社製 PRIMUS II)にてFP法による半定量分析で測定したケイ素の値である。
なお、本発明において、上述の測定方法により得られるケイ素の値は、酸化亜鉛粒子の表面に被覆した有機ケイ素化合物中のケイ素と、被覆していないフリーの有機ケイ素化合物中のケイ素とを含んだ値である。しかしながら、被覆していないフリーの有機ケイ素化合物は洗浄や加熱などの工程があれば流れ出ることがほとんどであり、被覆していないフリーの有機ケイ素化合物中のケイ素は微量であると考えられるため、上述の測定方法により得られる値が、酸化亜鉛粒子に被覆している有機ケイ素化合物中のケイ素とほぼ同量であると考えて問題はない。
The above organosilicon coating amount is the silicon value measured by semi-quantitative analysis using the FP method using a fluorescent X-ray analyzer (PRIMUS II manufactured by Rigaku Corporation) on organosilicon surface-coated zinc oxide particles molded using a press machine. .
In addition, in the present invention, the silicon value obtained by the above-mentioned measurement method includes silicon in the organosilicon compound coated on the surface of the zinc oxide particles and silicon in the free organosilicon compound that is not coated. It is a value. However, in most cases, uncoated free organosilicon compounds flow out during processes such as washing or heating, and the amount of silicon in uncoated free organosilicon compounds is thought to be small. There is no problem in considering that the value obtained by the measurement method is approximately the same amount of silicon in the organosilicon compound coating the zinc oxide particles.
上述したような上記「波長600nmの(乾燥後塗膜の平行光透過率)/(塗布直後塗膜の平行光透過率)の比」を有する分散体は、特に分散性に優れ、透過型電子顕微鏡写真から測定した一次粒子径が0.1μm以下となる有機ケイ素表面処理被覆酸化亜鉛粒子を原料として使用することによって得ることができる。 The dispersion having the above-mentioned "ratio of (parallel light transmittance of the coating film after drying)/(parallel light transmittance of the coating film immediately after application)" at a wavelength of 600 nm has particularly excellent dispersibility and is suitable for transmission electron transmission. It can be obtained by using as a raw material organosilicon surface-treated coated zinc oxide particles having a primary particle diameter of 0.1 μm or less as measured from a microscopic photograph.
分散体の原料とするうえで好ましい性質を有する有機ケイ素表面被覆酸化亜鉛粒子(A)として、より具体的には、例えば、以下のような性質を有するものを挙げることができる。 More specifically, examples of the organosilicon surface-coated zinc oxide particles (A) having desirable properties for use as a raw material for a dispersion include those having the following properties.
分散体製造の原料として使用される上記有機ケイ素表面被覆酸化亜鉛粒子(A)は、以下の方法で測定して求めたメジアン径が0.15μm以下であることが好ましい。なお、ここでのメジアン径は、後述のメジアン径2にあたる。
上記有機ケイ素表面被覆酸化亜鉛粒子0.4gを、イソプロピルアルコール200mlに入れ、超音波ホモジナイザーUS-600E(日本精機製作所製 定格出力600W)を用いて、常温で振動振幅100%の超音波を30秒間照射してスラリーを調製し、レーザー回折/散乱式粒度分布測定装置LA-960S(堀場製作所社製)を用いて体積基準におけるメジアン径を測定した。
また、上記有機ケイ素表面被覆酸化亜鉛粒子(A)は非常に高い分散性を有するため、超音波による弱い衝撃を加えるだけで充分に分散する、という点も特徴の一つである。
上記メジアン径は、0.13μm以下であることがより好ましい。
It is preferable that the organosilicon surface-coated zinc oxide particles (A) used as a raw material for producing a dispersion have a median diameter of 0.15 μm or less as measured by the following method. Note that the median diameter here corresponds to median diameter 2, which will be described later.
Add 0.4 g of the above organosilicon surface-coated zinc oxide particles to 200 ml of isopropyl alcohol, and use an ultrasonic homogenizer US-600E (manufactured by Nippon Seiki Seisakusho, rated output 600 W) to apply ultrasonic waves at 100% vibration amplitude for 30 seconds at room temperature. A slurry was prepared by irradiation, and the median diameter on a volume basis was measured using a laser diffraction/scattering particle size distribution analyzer LA-960S (manufactured by Horiba, Ltd.).
Furthermore, since the organosilicon surface-coated zinc oxide particles (A) have extremely high dispersibility, one of their characteristics is that they can be sufficiently dispersed simply by applying a weak impact with ultrasonic waves.
The median diameter is more preferably 0.13 μm or less.
分散体製造の原料として使用される上記有機ケイ素表面被覆酸化亜鉛粒子において、上記メジアン径と一次粒子径との比(メジアン径/一次粒子径)は、4以下であることが好ましい。上記メジアン径と一次粒子径との比は、粉末を構成する一次粒子の独立性の高さの指標となる値であり、この値が1に近いほど、一次粒子が凝集粒子ではなく独立して存在していることを意味する。上記メジアン径と一次粒子径との比は、3以下がより好ましい。なお、ここでのメジアン径は、後述のメジアン径2にあたる。 In the organosilicon surface-coated zinc oxide particles used as a raw material for producing a dispersion, the ratio between the median diameter and the primary particle diameter (median diameter/primary particle diameter) is preferably 4 or less. The ratio of the above median diameter to the primary particle diameter is a value that is an index of the degree of independence of the primary particles that make up the powder, and the closer this value is to 1, the more independent the primary particles are rather than aggregated particles. means existing. The ratio of the median diameter to the primary particle diameter is more preferably 3 or less. Note that the median diameter here corresponds to median diameter 2, which will be described later.
分散体製造の原料として使用される上記有機ケイ素表面被覆酸化亜鉛粒子は易分散性を有するものであるが、分散処理をしない場合には、適度に凝集した状態で存在するものであることが好ましい。具体的には、当該粉体をイソプロピルアルコール中に入れ、ホモディスパーで500rpm、5秒間攪拌したスラリーのレーザー回折散乱法での体積基準におけるメジアン径が10μm以上であることが好ましい。すなわち、撹拌機や超音波等で分散処理をしない限りは緩い凝集粒子を形成し、衝撃を与えると、凝集状態が解けて一次粒子に近い状態まで分散するものである。より好ましくは、13μm以上である。
本明細書において、上述のホモディスパーで500rpm、5秒間攪拌した状態のメジアン径をメジアン径1、上述の30秒間超音波分散した状態のメジアン径をメジアン径2と表す。
The organosilicon surface-coated zinc oxide particles used as a raw material for producing a dispersion are easily dispersible, but if no dispersion treatment is performed, they are preferably present in a moderately agglomerated state. . Specifically, it is preferable that the volume-based median diameter of a slurry obtained by placing the powder in isopropyl alcohol and stirring with a homodisper at 500 rpm for 5 seconds is 10 μm or more using a laser diffraction scattering method. That is, unless dispersion treatment is performed using a stirrer, ultrasonic waves, etc., loosely aggregated particles are formed, and when an impact is applied, the agglomerated state is dissolved and the particles are dispersed to a state close to that of primary particles. More preferably, it is 13 μm or more.
In this specification, the median diameter after stirring at 500 rpm for 5 seconds with the above-mentioned homodisper is referred to as median diameter 1, and the median diameter after ultrasonic dispersion for 30 seconds as described above is referred to as median diameter 2.
分散体製造の原料として使用される上記有機ケイ素表面被覆酸化亜鉛粒子は、BET比表面積が25m2/g以下であることが好ましい。BET比表面積が25m2/gを超えると、粒子サイズが小さくなるため凝集が起こりやすくなる。
上記BET比表面積は、実施例に記載の方法により測定することができる。
The organosilicon surface-coated zinc oxide particles used as a raw material for producing the dispersion preferably have a BET specific surface area of 25 m 2 /g or less. When the BET specific surface area exceeds 25 m 2 /g, agglomeration tends to occur because the particle size becomes small.
The above BET specific surface area can be measured by the method described in Examples.
上記有機ケイ素表面被覆酸化亜鉛粒子(A)は、その製造方法を特に限定されるものではないが、例えば、原体である酸化亜鉛粒子を水と有機溶剤とを含む溶媒中にリパルプしてスラリーを調製する工程(1)、有機ケイ素化合物を水と有機溶剤とを含む溶媒中で加水分解する工程(2)、及び、前記加水分解後のシラン化合物で酸化亜鉛粒子を表面処理する工程(3)を有する有機ケイ素表面被覆酸化亜鉛粒子の製造方法等を挙げることができる。 The method for manufacturing the organosilicon surface-coated zinc oxide particles (A) is not particularly limited, but for example, the raw material zinc oxide particles are repulped into a solvent containing water and an organic solvent to form a slurry. (1), a step (2) of hydrolyzing an organosilicon compound in a solvent containing water and an organic solvent, and a step (3) of surface-treating zinc oxide particles with the silane compound after the hydrolysis. ), etc. can be mentioned.
上記工程(1)は、原体である酸化亜鉛粒子を水と有機溶剤とを含む溶媒中にリパルプしてスラリーを調製する工程である。本発明の製造方法において、工程(1)で酸化亜鉛粒子のスラリーを調製することは重要な工程である。すなわち、上記酸化亜鉛粒子が凝集した乾燥状態ではなく、分散したスラリー状態で有機ケイ素被覆を形成することを特徴としたものである。 The above step (1) is a step of preparing a slurry by repulping zinc oxide particles as a raw material into a solvent containing water and an organic solvent. In the production method of the present invention, preparing a slurry of zinc oxide particles in step (1) is an important step. That is, the organosilicon coating is formed not in a dry state in which the zinc oxide particles are aggregated, but in a dispersed slurry state.
ここで、工程(1)において原料として使用する酸化亜鉛粒子は、水性媒体中で合成反応を行ったものについて、乾燥工程を経ることなく、そのまま、スラリーを調製するものであることが好ましい。すなわち、粒子の製造工程から、有機ケイ素被覆処理の工程に至るまでの間に、粒子を乾燥させる工程を有さないことが好ましい。このようにすることで、粒子間の凝集を抑制し、凝集した粒子に対して表面処理を行うことがなくなるため、上述したような優れた分散性能を得ることができる。 Here, the zinc oxide particles used as a raw material in step (1) are preferably those subjected to a synthesis reaction in an aqueous medium and then prepared as a slurry without undergoing a drying step. That is, it is preferable that there is no step of drying the particles between the step of manufacturing the particles and the step of coating with organosilicon. By doing so, agglomeration between particles is suppressed and surface treatment is not performed on aggregated particles, so that the excellent dispersion performance as described above can be obtained.
この工程(1)により、酸化亜鉛粒子の一つ一つが表面処理されることになるため、有機ケイ素被覆量を過剰にする必要なく、効率的に撥水性を付与することができる。
上記工程(1)において、酸化亜鉛粒子のスラリーは限定されるものではないが、例えば、酸化亜鉛粒子を10~1000g/Lの範囲で含むことが好ましい。
Through this step (1), each zinc oxide particle is surface-treated, so that water repellency can be efficiently imparted without the need for an excessive amount of organosilicon coating.
In the above step (1), the slurry of zinc oxide particles is not limited, but preferably contains zinc oxide particles in a range of 10 to 1000 g/L, for example.
スラリーの調製方法は特に限定されず、例えば、酸化亜鉛粒子の製造工程によって得られた酸化亜鉛粒子を濾過した後、乾燥させることなく水に添加し、5~30℃で10~30分間、分散させることによって、酸化亜鉛粒子の濃度が10~1000g/Lの均一なスラリーとすることができる。 The method for preparing the slurry is not particularly limited. For example, after filtering the zinc oxide particles obtained in the zinc oxide particle manufacturing process, the slurry is added to water without drying, and dispersed at 5 to 30°C for 10 to 30 minutes. By doing so, a uniform slurry with a zinc oxide particle concentration of 10 to 1000 g/L can be obtained.
上記有機溶剤としては特に限定されないが、後述のものを使用することができる。 The above-mentioned organic solvent is not particularly limited, but those described below can be used.
上記工程(2)は、有機ケイ素化合物を水と有機溶剤とを含む溶媒中で加水分解する工程(2)である。 The above step (2) is a step (2) of hydrolyzing the organosilicon compound in a solvent containing water and an organic solvent.
工程(2)に用いる有機溶剤は、有機ケイ素化合物を加水分解させることができる限り特に制限されないが、メタノール、エタノール及びプロパノールからなる群より選択される少なくとも一種を用いることが好ましい。このような低級アルコールを用いることで加水分解が進みやすくなる。より好ましくは、エタノールである。 The organic solvent used in step (2) is not particularly limited as long as it can hydrolyze the organosilicon compound, but it is preferable to use at least one selected from the group consisting of methanol, ethanol, and propanol. By using such a lower alcohol, hydrolysis progresses more easily. More preferred is ethanol.
上記工程(2)は、pHが3.5~4.5の条件で行われることが好ましい。pHが3.5~4.5の条件で行うことで、有機ケイ素化合物の加水分解を短時間で進行させることができる上、加水分解で得られたシラン化合物の自己縮合を効果的に抑制することができる。pHは、より好ましくは3.8~4.2である。pHは、酸やアルカリを用いて適宜調整すればよい。 The above step (2) is preferably carried out at a pH of 3.5 to 4.5. By carrying out the process at a pH of 3.5 to 4.5, the hydrolysis of the organosilicon compound can proceed in a short time, and the self-condensation of the silane compound obtained by hydrolysis can be effectively suppressed. be able to. The pH is more preferably 3.8 to 4.2. The pH may be adjusted appropriately using an acid or an alkali.
上記工程(2)は、攪拌して行われることが好ましい。攪拌することで、有機ケイ素化合物をより充分に加水分解させることができる。
加水分解工程を行う時間は特に制限されないが、30分以上であることが好ましい。また、加水分解を行う温度は特に限定されないが、40℃以上であることが好ましい。このような条件とすることで、有機ケイ素化合物の加水分解を充分に進めつつ、シラン化合物の自己縮合を抑制することができる。
The above step (2) is preferably performed with stirring. By stirring, the organosilicon compound can be more fully hydrolyzed.
Although the time for performing the hydrolysis step is not particularly limited, it is preferably 30 minutes or more. Moreover, the temperature at which hydrolysis is performed is not particularly limited, but is preferably 40° C. or higher. Under such conditions, self-condensation of the silane compound can be suppressed while sufficiently promoting hydrolysis of the organosilicon compound.
上記工程(2)における攪拌手段は、特に限定されないが、撹拌羽根による撹拌、振とう攪拌、ミキサーによる撹拌、スターラーによる撹拌等が挙げられる。 The stirring means in step (2) above is not particularly limited, and examples thereof include stirring using a stirring blade, shaking stirring, stirring using a mixer, stirring using a stirrer, and the like.
上記工程(3)は、加水分解後のシラン化合物で酸化亜鉛粒子を表面処理する工程である。
表面処理工程では、加水分解後のシラン化合物を工程(1)で得られた酸化亜鉛粒子のスラリーに添加した後、攪拌することが好ましい。攪拌することで加水分解したシラン化合物のシラノール基の反応を充分に進めて、表面処理をより効率的に行うことができる。
攪拌する時間は特に制限されないが、60分以上であることが好ましい。攪拌する手段としては、ブレンダー、ビーズミルなどが挙げられる。
表面処理工程を行う温度は特に制限されないが、30~100℃で行うことが好ましい。
The above step (3) is a step of surface-treating the zinc oxide particles with a hydrolyzed silane compound.
In the surface treatment step, it is preferable to add the hydrolyzed silane compound to the slurry of zinc oxide particles obtained in step (1) and then stir it. By stirring, the reaction of the silanol groups of the hydrolyzed silane compound can proceed sufficiently, and the surface treatment can be performed more efficiently.
The stirring time is not particularly limited, but is preferably 60 minutes or longer. Examples of stirring means include a blender and a bead mill.
The temperature at which the surface treatment step is carried out is not particularly limited, but it is preferably carried out at 30 to 100°C.
上記工程(3)は、加水分解後のシラン化合物溶液を添加する工程であるが、シラン化合物の仕込み量が酸化亜鉛粒子に対して1.0質量%以上になるように添加することが好ましい。上記仕込み量が1.0質量%未満であると、撥水性が不足するおそれがある。より好ましくは1.5質量%以上である。また、上記仕込み量は、10質量%以下が好ましい。上記仕込み量が10質量%を超えると、酸化亜鉛の純度が低くなりUV遮蔽性等の性能が低下するおそれがある。より好ましくは8質量%以下である。 The above step (3) is a step of adding the silane compound solution after hydrolysis, and it is preferable to add the silane compound in an amount of 1.0% by mass or more based on the zinc oxide particles. If the amount added is less than 1.0% by mass, water repellency may be insufficient. More preferably, it is 1.5% by mass or more. Moreover, the amount of the above-mentioned preparation is preferably 10% by mass or less. If the above-mentioned amount exceeds 10% by mass, the purity of zinc oxide may decrease and performance such as UV shielding properties may deteriorate. More preferably, it is 8% by mass or less.
このようにして、上記表面処理工程を行った後、攪拌を続けながら、得られたスラリーを0.5時間乃至数時間、熟成して、酸化亜鉛粒子の表面に有機ケイ素被覆を形成させる。
上記熟成に際しては、本発明の効果を損なわない範囲で、他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。
After performing the above surface treatment step in this way, the resulting slurry is aged for 0.5 to several hours while stirring to form an organosilicon coating on the surface of the zinc oxide particles.
During the above-mentioned ripening, other components may be added in small amounts to the extent that the effects of the present invention are not impaired. For example, a dispersant or the like may be added.
熟成は、45~110℃において行うことが好ましい。特に、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、微粒子酸化亜鉛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。 Aging is preferably carried out at 45 to 110°C. In particular, the aging time can be 0.5 to 24 hours. Since the particle size can be adjusted by adjusting the conditions such as aging temperature, aging time, and concentration of fine zinc oxide particles, it is preferable to set these conditions as appropriate depending on the target zinc oxide particles.
このようにして得られた有機ケイ素表面被覆酸化亜鉛粒子は、必要に応じて、濾過、水洗、乾燥等の後処理を行ってもよい。
例えば、有機ケイ素被覆酸化亜鉛粒子のスラリーを濾過して、有機ケイ素表面被覆酸化亜鉛粒子を分離し、水洗した後、通常、80~150℃の範囲の温度に加熱して乾燥し、有機ケイ素表面被覆酸化亜鉛粒子を乾燥粉体として得ることができる。なお、上記有機ケイ素表面被覆酸化亜鉛粒子は、表面被覆後に300℃以上で加熱するような焼成工程を経ないものであることが好ましい。このようなものとすることで、上述したような本発明の効果を特に好適に得ることができる。
The organosilicon surface-coated zinc oxide particles thus obtained may be subjected to post-treatments such as filtration, water washing, and drying, if necessary.
For example, a slurry of organosilicon-coated zinc oxide particles is filtered to separate organosilicon-surface-coated zinc oxide particles, washed with water, and then dried by heating to a temperature usually in the range of 80 to 150°C. Coated zinc oxide particles can be obtained as a dry powder. Note that it is preferable that the organosilicon surface-coated zinc oxide particles do not undergo a firing process such as heating at 300° C. or higher after surface coating. With this configuration, the effects of the present invention as described above can be particularly preferably obtained.
上記原体となる酸化亜鉛粒子としては特に限定されないが、それ自体の分散性が高いものを使用したほうが、得られる有機ケイ素表面被覆酸化亜鉛粒子の分散性も高まるため好ましい。例えば、一次粒子径が0.1μm未満であるものが好ましく、アスペクト比が2.5未満であるものが好ましく、吸油量/BET比表面積が1.5ml/100m2以下であるもの等が好ましい。吸油量/BET比表面積(ml/100m2)は、吸油量(ml/100g)の値を、BET比表面積(m2/g)の値で除した値であり、この値が小さい程、粒子表面の単位面積当りの吸油量が低いことを意味し、粒子同士の凝集が少なく、粒子の独立性、分散性が高いことを意味する。このような原体酸化亜鉛粒子としては、例えば、一次粒子径が0.005μm以上、0.05μm以下の微粒子酸化亜鉛を、亜鉛塩を溶解した水中で熟成する工程を含む製造方法によって得られたもの等を挙げることができる。具体的には、例えば、国際公開2012/147888に開示された酸化亜鉛粒子等を使用することが好ましい。 The zinc oxide particles that serve as the raw material are not particularly limited, but it is preferable to use particles that have high dispersibility themselves because the dispersibility of the resulting organosilicon surface-coated zinc oxide particles will also increase. For example, the primary particle diameter is preferably less than 0.1 μm, the aspect ratio is preferably less than 2.5, and the oil absorption/BET specific surface area is preferably 1.5 ml/100 m 2 or less. Oil absorption/BET specific surface area (ml/100m 2 ) is the value obtained by dividing the oil absorption (ml/100g) by the BET specific surface area (m 2 /g). This means that the amount of oil absorbed per unit area of the surface is low, there is little aggregation of particles, and the independence and dispersibility of particles are high. Such raw zinc oxide particles may be obtained by a manufacturing method that includes a step of aging fine particulate zinc oxide having a primary particle diameter of 0.005 μm or more and 0.05 μm or less in water in which zinc salt is dissolved. I can list things, etc. Specifically, it is preferable to use, for example, zinc oxide particles disclosed in International Publication No. 2012/147888.
国際公開2012/147888は、微粒子酸化亜鉛を、亜鉛塩を溶解した水中で熟成する工程を含む製造方法によって、分散性に優れた酸化亜鉛粒子を得る方法が開示されている。このような方法によって水中で酸化亜鉛粒子を製造した後、濾過を行い、乾燥させることなく、上述したような方法での表面処理を行うことが好ましい。これによって、凝集が少ない状態の酸化亜鉛粒子に対して表面処理を行うことができ、本発明の目的を好適に達成することができる。 International Publication No. 2012/147888 discloses a method for obtaining zinc oxide particles with excellent dispersibility by a production method including a step of aging fine particulate zinc oxide in water in which a zinc salt is dissolved. After producing zinc oxide particles in water by such a method, it is preferable to perform filtration and surface treatment by the method described above without drying. Thereby, the surface treatment can be performed on the zinc oxide particles with little agglomeration, and the object of the present invention can be suitably achieved.
国際公開2012/147888の製造方法によって一次粒子径が0.1μm未満であり、アスペクト比が2.5未満であり、吸油量/BET比表面積が1.5ml/100m2以下であることを特徴とする酸化亜鉛粒子を得ることができる。このような酸化亜鉛粒子を原料とすることが特に好ましい。 The primary particle diameter is less than 0.1 μm, the aspect ratio is less than 2.5, and the oil absorption/BET specific surface area is 1.5 ml/100 m 2 or less according to the production method of International Publication 2012/147888. Zinc oxide particles can be obtained. It is particularly preferable to use such zinc oxide particles as a raw material.
本発明の水系分散体は、上記有機ケイ素表面被覆酸化亜鉛粒子(A)を高濃度で含有するものであるが、その含有量は水系分散体全量に対して60質量%以上であり、70質量%以上であることが好ましい。上限は特に限定されないが、75質量%であることが好ましい。 The aqueous dispersion of the present invention contains the organosilicon surface-coated zinc oxide particles (A) at a high concentration, and the content is 60% by mass or more based on the total amount of the aqueous dispersion, and 70% by mass. % or more. Although the upper limit is not particularly limited, it is preferably 75% by mass.
さらに、本発明の水系分散体は分散剤である非イオン性界面活性剤(B)を含有するものであるが、上記有機ケイ素表面被覆酸化亜鉛粒子(A)が易分散性に優れたものであるため、非イオン性界面活性剤(B)の含有量を上記有機ケイ素表面被覆酸化亜鉛粒子(A)に対して10質量%以下とすることができる。上記非イオン性界面活性剤(B)の含有量が従来のものより少量であるため、良好な感触を有する水系分散体を得ることができる。
上記非イオン性界面活性剤界面活性剤(B)の含有量は、上記有機ケイ素表面被覆酸化亜鉛粒子(A)に対して8.5質量%以下であることがより好ましい。下限は特に限定されないが、5質量%であることが好ましい。
Furthermore, the aqueous dispersion of the present invention contains a nonionic surfactant (B) as a dispersant, and the organosilicon surface-coated zinc oxide particles (A) have excellent dispersibility. Therefore, the content of the nonionic surfactant (B) can be 10% by mass or less based on the organosilicon surface-coated zinc oxide particles (A). Since the content of the nonionic surfactant (B) is smaller than conventional ones, an aqueous dispersion with a good feel can be obtained.
The content of the nonionic surfactant surfactant (B) is more preferably 8.5% by mass or less based on the organosilicon surface-coated zinc oxide particles (A). Although the lower limit is not particularly limited, it is preferably 5% by mass.
上記非イオン性界面活性剤(B)としては、分散剤として作用するものであれば特に限定されないが、例えば、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレン脂肪酸エステル、ポリオキシアルキレンソルビタン脂肪酸エステル、ポリオキシアルキレンヒマシ油、ポリオキシアルキレン硬化ヒマシ油、ポリオキシアルキレンソルビトールテトラ脂肪酸エステル、グリセリン脂肪酸エステル、ソルビタン脂肪酸エステル、ポリグリセリン脂肪酸エステル、ショ糖脂肪酸エステル、ポリオキシアルキレン基を有するオルガノポリシロキサン、ポリグリセリン基を有するオルガノポリシロキサン、糖鎖を有するオルガノポリシロキサン等が挙げられる。
上記非イオン性界面活性剤(B)は、1種のみの使用であってもよいし、2種以上を組みあわせて使用してもよい。
The nonionic surfactant (B) is not particularly limited as long as it acts as a dispersant, but examples include polyoxyalkylene alkyl ether, polyoxyalkylene fatty acid ester, polyoxyalkylene sorbitan fatty acid ester, polyoxyalkylene alkyl ether, polyoxyalkylene fatty acid ester, polyoxyalkylene sorbitan fatty acid ester, Alkylene castor oil, polyoxyalkylene hydrogenated castor oil, polyoxyalkylene sorbitol tetra fatty acid ester, glycerin fatty acid ester, sorbitan fatty acid ester, polyglycerin fatty acid ester, sucrose fatty acid ester, organopolysiloxane with polyoxyalkylene group, polyglycerin group and organopolysiloxanes having sugar chains.
The nonionic surfactant (B) may be used alone or in combination of two or more.
なかでも、ポリオキシアルキレン脂肪酸エステル、ポリオキシアルキレンソルビタン脂肪酸エステル、ポリオキシアルキレン基を有するオルガノポリシロキサンを非イオン性界面活性剤(B)として使用することが好ましい。 Among these, it is preferable to use polyoxyalkylene fatty acid ester, polyoxyalkylene sorbitan fatty acid ester, and organopolysiloxane having a polyoxyalkylene group as the nonionic surfactant (B).
さらには、上述したようなオルガノポリシロキサン系の非イオン性界面活性剤が最も好ましく、オルガノポリシロキサン系の非イオン性界面活性剤を使用した場合、水系分散体の安定性、化粧料において使用したときの使用感等において、特に優れた効果を得ることができる。 Furthermore, the above-mentioned organopolysiloxane-based nonionic surfactants are most preferred, and when organopolysiloxane-based nonionic surfactants are used, the stability of the aqueous dispersion, the stability of the cosmetics used, etc. Particularly excellent effects can be obtained in terms of the feeling of use and the like.
このような界面活性剤のHLBとしては、6-12であることが望ましい。HLBが12を超える非イオン性界面活性剤だけを使用して分散させた水系分散体は、O/W製剤へ配合した場合、非イオン性界面活性剤の水への溶解性が高過ぎるため粉への吸着性が悪くなり、製剤の粘度上昇を起こしやすく、耐水性が悪くなりやすい。また非イオン性界面活性剤のHLBが6未満の場合は水分散体を作成することが難しくなる。なお、本明細書においてHLBは、W.C.Grifinnによって定義された次式によって求める。
NHLB=(E+P)/5
(NHLB:HLB値、E:ポリオキシエチレン部の分散剤分子全体に対する質量%、
P:多価アルコール部の分散剤分子全体に対する質量%)
The HLB of such a surfactant is preferably 6-12. When an aqueous dispersion made using only a nonionic surfactant with an HLB of over 12 is mixed into an O/W formulation, the solubility of the nonionic surfactant in water is too high, so it cannot be used as a powder. The adsorption properties of the formulation are likely to deteriorate, the viscosity of the formulation tends to increase, and the water resistance tends to deteriorate. Furthermore, if the HLB of the nonionic surfactant is less than 6, it becomes difficult to create an aqueous dispersion. In addition, in this specification, HLB is W. C. It is determined by the following equation defined by Griffin.
N HLB = (E+P)/5
( NHLB : HLB value, E: mass % of polyoxyethylene moiety relative to the entire dispersant molecule,
P: mass % of polyhydric alcohol moiety based on the entire dispersant molecule)
本発明の水系分散体は、さらに、多価アルコール(C)を含有するものである。多価アルコール(C)としては、プロピレングリコール、ブチレングリコール、ペンタンジオール、ジプロピレングリコール、ヘキサンジオール、ヘプタンジオール、グリセリンから選ばれる1種又は2種以上であることが好ましく、特にブチレングリコール、ペンタンジオール、ジプロピレングリコール、ヘキサンジオールが好ましい。この多価アルコール(C)は、水系分散体中に5~25質量%含有することが好ましい。このような多価アルコール(C)を配合することによって、非イオン性界面活性剤(B)が粉体表面により均一に配向でき、分散体が安定するものと考えられる。より好ましくは8~20質量%である。 The aqueous dispersion of the present invention further contains a polyhydric alcohol (C). The polyhydric alcohol (C) is preferably one or more selected from propylene glycol, butylene glycol, pentanediol, dipropylene glycol, hexanediol, heptanediol, and glycerin, particularly butylene glycol and pentanediol. , dipropylene glycol and hexanediol are preferred. This polyhydric alcohol (C) is preferably contained in an amount of 5 to 25% by mass in the aqueous dispersion. It is believed that by blending such a polyhydric alcohol (C), the nonionic surfactant (B) can be more uniformly oriented on the powder surface, thereby stabilizing the dispersion. More preferably, it is 8 to 20% by mass.
本発明の水系分散体は、水を含有するものであるが、水の含有量は、組成物全量に対して、20~30質量%であることが好ましい。このような範囲内のものとすることで、上述した効果を好適に得ることができる。 The aqueous dispersion of the present invention contains water, and the water content is preferably 20 to 30% by mass based on the total amount of the composition. By setting it within such a range, the above-mentioned effects can be suitably obtained.
本発明の水系分散体を得るための製造方法としては特に限定されず、上述した成分を混合することにより作製すればよい。混合方法も限定されず、均一に分散させることができる通常の手法を採用すればよい。例えば、ビーズミル、ジェットミル、高圧ホモジナイザー
等の分散機・装置を用いてもよいが、本発明の水系分散体はこれらの高価な分散機・装置
を使用しなくても簡易な攪拌機で容易に作製することができるため、ビーズミル等の高価
な分散機が不要になるという利点も有する。
The method for producing the aqueous dispersion of the present invention is not particularly limited, and may be produced by mixing the above-mentioned components. The mixing method is not limited either, and any conventional method that can achieve uniform dispersion may be used. For example, a dispersing machine or device such as a bead mill, jet mill, or high-pressure homogenizer may be used, but the aqueous dispersion of the present invention can be easily produced using a simple stirrer without using these expensive dispersing machines or devices. This also has the advantage of eliminating the need for an expensive dispersion machine such as a bead mill.
本発明の水系分散体には、分散体の性能を損なわない範囲で必要に応じて、パラオキシ安息香酸アルキルエステル、安息香酸、安息香酸ナトリウム、ソルビン酸、ソルビン酸カリウム、フェノキシエタノール、サリチル酸、石炭酸、ソルビン酸、パラクロルメタクレゾール、ヘキサクロロフェン、塩化ベンザルコニウム、塩化クロルヘキシジン、感光素、フェノキシエタノール等の防菌防腐剤や抗菌剤等を添加することができる。 The aqueous dispersion of the present invention may contain paraoxybenzoic acid alkyl ester, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, phenoxyethanol, salicylic acid, carbolic acid, sorbic acid, etc., as necessary to the extent that the performance of the dispersion is not impaired. Antibacterial preservatives and antibacterial agents such as acids, parachlormetacresol, hexachlorophene, benzalkonium chloride, chlorhexidine chloride, photosensors, and phenoxyethanol can be added.
このようにして得られた水系分散体は、紫外線遮断効果を有する化粧料を作成するための成分として有用である。この場合、本発明の水系分散体のみを紫外線遮断成分としても良いが、微粒子無機粉体の油系分散体や有機紫外線吸収剤等を併用しても良い。 The aqueous dispersion thus obtained is useful as a component for preparing cosmetics having an ultraviolet blocking effect. In this case, only the aqueous dispersion of the present invention may be used as the ultraviolet blocking component, but an oil-based dispersion of fine particle inorganic powder, an organic ultraviolet absorber, etc. may also be used in combination.
次に、本発明の水系分散体の物性について詳述する。
(粘度)
本発明の水系分散体は、高濃度で微粒子酸化亜鉛を含有するものであるが、分散性に優れる有機ケイ素表面被覆酸化亜鉛粒子(A)を含有するため低粘度を示すものである。具体的には、25℃における粘度が4,000mPa.s以下であることが好ましく、1000mPa.s以下であることがより好ましく、100mPa.s以下であることが特に好ましい。粘度が4,000m.Pa.s以下であると、製剤への配合が容易である点で好ましい。上記粘度は、実施例に記載の方法により測定することができる。
Next, the physical properties of the aqueous dispersion of the present invention will be explained in detail.
(viscosity)
The aqueous dispersion of the present invention contains particulate zinc oxide at a high concentration, but exhibits low viscosity because it contains organosilicon surface-coated zinc oxide particles (A) that have excellent dispersibility. Specifically, the viscosity at 25° C. is 4,000 mPa. s or less, preferably 1000 mPa.s or less. s or less, more preferably 100 mPa.s or less. It is particularly preferable that it is less than or equal to s. Viscosity is 4,000m. Pa. It is preferable that it is less than or equal to s because it can be easily incorporated into a preparation. The above viscosity can be measured by the method described in Examples.
(メジアン径)
上記水系分散体中の有機ケイ素表面被覆酸化亜鉛粒子(A)のメジアン径は、0.15μm以下であることが好ましく、0.12μm以下であることがより好ましく、0.01μm以上であることが好ましい。上記メジアン径が0.15μm以下であることは、可視光透明性が高く、かつ紫外線遮蔽領域が好適なものである点で好ましい。本明細書において、水分散体中における有機ケイ素表面被覆酸化亜鉛粒子(A)のメジアン径をメジアン径3と表す。上記メジアン径3は、実施例に記載の方法により測定することができる。
(median diameter)
The median diameter of the organosilicon surface-coated zinc oxide particles (A) in the aqueous dispersion is preferably 0.15 μm or less, more preferably 0.12 μm or less, and preferably 0.01 μm or more. preferable. It is preferable that the median diameter is 0.15 μm or less because visible light transparency is high and the ultraviolet shielding region is suitable. In this specification, the median diameter of the organosilicon surface-coated zinc oxide particles (A) in the aqueous dispersion is expressed as median diameter 3. The above median diameter 3 can be measured by the method described in Examples.
本発明の水系分散体は、その用途を特に限定されるものではないが、例えば、化粧料、塗料等の用途において好適に使用することができる。このような化粧料も本発明の一つである。 The aqueous dispersion of the present invention is not particularly limited in its use, but can be suitably used, for example, in cosmetics, paints, and the like. Such cosmetics are also part of the present invention.
本発明の水系分散体を含有する化粧料は、分散性及び安定性に優れ、良好な取り扱い性も有するものである。 Cosmetics containing the aqueous dispersion of the present invention have excellent dispersibility and stability, and also have good handling properties.
本発明の化粧料としては、ファンデーション、化粧下地、アイシャドウ、頬紅、マスカラ、口紅、サンスクリーン剤、スキンケア製品、頭髪製品等を挙げることができる。なかでも、サンスクリーン剤において特に好適に使用することができる。
また、本発明の化粧料は、油性化粧料、水性化粧料、O/W型化粧料、W/O型化粧料の任意の形態とすることができるが、O/W型化粧料が特に好ましい。
また、製品の形態についても特に限定はないが、液状、乳液状、クリーム状、固形状、ペースト状、ゲル状、多層状、ムース状、スプレー状等に適用が可能である。
Cosmetics of the present invention include foundations, makeup bases, eye shadows, blushers, mascaras, lipsticks, sunscreens, skin care products, hair products, and the like. Among these, it can be particularly suitably used in sunscreen agents.
Furthermore, the cosmetic of the present invention can be in any form including oil-based cosmetics, water-based cosmetics, O/W type cosmetics, and W/O type cosmetics, but O/W type cosmetics are particularly preferred. .
Further, there is no particular limitation on the form of the product, but it can be applied in liquid, emulsion, cream, solid, paste, gel, multilayer, mousse, spray, etc.
本発明の化粧料は、上記混合物を構成する成分以外に、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、油分、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、無機及び有機顔料、無機及び有機粘土鉱物や金属石鹸処理又はシリコーンで処理された無機及び有機顔料等の各種粉体、有機染料等の色剤、防腐剤、酸化防止剤、色素、pH調整剤、香料、冷感剤、制汗剤、殺菌剤、皮膚賦活剤等の成分を含有するものであってもよい。具体的には、以下に列挙した配合成分の1種又は2種以上を任意に配合して常法により目的の化粧料を製造することが可能である。これらの配合成分の配合量は、本発明の効果を損なわない範囲であれば特に限定されない。 In addition to the components constituting the above-mentioned mixture, the cosmetic of the present invention may contain any aqueous component or oil component that can be used in the cosmetics field. The above-mentioned aqueous components and oil-based components are not particularly limited, and include, for example, oils, surfactants, humectants, higher alcohols, sequestering agents, natural and synthetic polymers, water-soluble and oil-soluble polymers, ultraviolet shielding agents, Various extracts, inorganic and organic pigments, various powders such as inorganic and organic clay minerals, inorganic and organic pigments treated with metal soap or silicone, colorants such as organic dyes, preservatives, antioxidants, pigments, It may contain components such as pH adjusters, fragrances, cooling agents, antiperspirants, disinfectants, and skin activators. Specifically, it is possible to manufacture the desired cosmetic by a conventional method by arbitrarily blending one or more of the ingredients listed below. The amounts of these ingredients are not particularly limited as long as they do not impair the effects of the present invention.
上記油分としては特に限定されず、例えば、アボガド油、ツバキ油、タートル油、マカデミアナッツ油、トウモロコシ油、ミンク油、オリーブ油、ナタネ油、卵黄油、ゴマ油、パーシック油、小麦胚芽油、サザンカ油、ヒマシ油、アマニ油、サフラワー油、綿実油、エノ油、大豆油、落花生油、茶実油、カヤ油、コメヌカ油、シナギリ油、日本キリ油、ホホバ油、胚芽油、トリグリセリン、トリオクタン酸グリセリン、トリイソパルミチン酸グリセリン、カカオ脂、ヤシ油、馬脂、硬化ヤシ油、パーム油、牛脂、羊脂、硬化牛脂、パーム核油、豚脂、牛骨脂、モクロウ核油、硬化油、牛脚脂、モクロウ、硬化ヒマシ油、ミツロウ、カンデリラロウ、綿ロウ、カルナウバロウ、ベイベリーロウ、イボタロウ、鯨ロウ、モンタンロウ、ヌカロウ、ラノリン、カポックロウ、酢酸ラノリン、液状ラノリン、サトウキビロウ、ラノリン脂肪酸イソプロピル、ラウリン酸ヘキシル、還元ラノリン、ジョジョバロウ、硬質ラノリン、セラックロウ、POEラノリンアルコールエーテル、POEラノリンアルコールアセテート、POEコレステロールエーテル、ラノリン脂肪酸ポリエチレングリコール、POE水素添加ラノリンアルコールエーテル、流動パラフィン、オゾケライト、プリスタン、パラフィン、セレシン、スクワレン、ワセリン、マイクロクリスタリンワックス等を挙げることができる。 The above-mentioned oils are not particularly limited, and include, for example, avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, sasanquat oil, and castor oil. Oil, linseed oil, safflower oil, cottonseed oil, eno oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, chinese oil, Japanese tung oil, jojoba oil, germ oil, triglycerin, glycerin trioctanoate, Glycerin triisopalmitate, cocoa butter, coconut oil, horse tallow, hydrogenated coconut oil, palm oil, beef tallow, mutton tallow, hydrogenated beef tallow, palm kernel oil, pork fat, beef bone fat, Japanese oak kernel oil, hydrogenated oil, beef leg Fat, Japanese wax, hydrogenated castor oil, beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, privet wax, spermaceti wax, Montan wax, bran wax, lanolin, kapok wax, acetic acid lanolin, liquid lanolin, sugar cane wax, lanolin fatty acid isopropyl, hexyl laurate, reduction Lanolin, Jojoba wax, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether, liquid paraffin, ozokerite, pristane, paraffin, ceresin, squalene, petrolatum , microcrystalline wax, and the like.
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。 The lipophilic nonionic surfactant is not particularly limited, and examples include sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan sesquioleate, and sorbitan trioleate. ate, diglycerol pent-2-ethylhexylate, diglycerol sorbitan tetra-2-ethylhexylate, sorbitan fatty acid esters such as diglycerol sorbitan tetra-2-ethylhexylate, monocottonseed oil fatty acid glycerin, monoerucic acid glycerin, sesquioleate glycerin, monostearate glycerin, α, α Examples include glycerol polyglycerol fatty acids such as glyceryl oleate, glyceryl monostearate and malic acid, propylene glycol fatty acid esters such as propylene glycol monostearate, hydrogenated castor oil derivatives, and glycerin alkyl ethers.
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ソルビタンモノステアレート、POEソルビタンモノオレエート、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モノジオレエート、ジ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 nonionic surfactant is not particularly limited, and includes, for example, POE sorbitan fatty acid esters such as POE sorbitan monostearate, POE sorbitan monooleate, POE sorbitan tetraoleate, POE sorbitan monolaurate, and POE sorbitan monolaurate. POE sorbit fatty acid esters such as oleate, POE sorbit pentaoleate, POE sorbit monostearate, POE glycerin fatty acid esters such as POE glycerin monostearate, POE glycerin monoisostearate, POE glycerin triisostearate, POE POE fatty acid esters such as monooleate, POE distearate, POE monodioleate, and ethylene glycol distearate; POE alkyl ethers such as POE lauryl ether, POE oleyl ether, POE stearyl ether, POE behenyl ether, POE 2-octyl dodecyl ether, and POE cholestanol ether; , POE alkylphenyl ethers such as POE octyl phenyl ether, POE nonylphenyl ether, POE dinonylphenyl ether, pluronic types such as Bluronic, POE/POP cetyl ether, POE/POP 2-decyltetradecyl ether, POE/POP monobutyl ether , POE/POP hydrogenated lanolin, POE/POP alkyl ethers such as POE/POP glycerin ether, tetra-POE/tetra-POP ethylenediamine condensates such as Tetronic, POE castor oil, POE hydrogenated castor oil, POE hydrogenated castor oil mono POE castor oil hydrogenated castor oil derivatives such as isostearate, POE hydrogenated castor oil triisostearate, POE hydrogenated castor oil monopyroglutamic acid monoisostearate diester, POE hydrogenated castor oil maleic acid, POE beeswax and lanolin such as POE sorbit beeswax. Derivatives, alkanolamides such as coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide, POE propylene glycol fatty acid ester, POE alkylamine, POE fatty acid amide, sucrose fatty acid ester, POE nonylphenyl formaldehyde condensate, alkyl ethoxy Dimethylamine oxide, trioleyl phosphoric acid, etc. 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。 Examples of other surfactants include fatty acid soaps, higher alkyl sulfate salts, POE lauryl sulfate triethanolamine, anionic surfactants such as alkyl ether sulfate salts, alkyltrimethylammonium salts, alkylpyridinium salts, alkyl quaternary Stabilizes cationic surfactants such as ammonium salts, alkyldimethylbenzyl ammonium salts, POE alkylamines, alkylamine salts, polyamine fatty acid derivatives, and amphoteric surfactants such as imidazoline-based amphoteric surfactants and betaine-based surfactants. It may also be blended within a range that does not cause problems with 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、イサイヨバラ抽出物、セイヨウノキギリソウ抽出物、メリロート抽出物等を挙げることができる。 The moisturizers mentioned above are not particularly limited, and include, for example, xylitol, sorbitol, maltitol, chondroitin sulfate, hyaluronic acid, mucoitin sulfate, caronic acid, atelocollagen, cholesteryl-12-hydroxystearate, sodium lactate, bile salts, dl- Examples include pyrrolidone carboxylate, short chain soluble collagen, diglycerin (EO) PO adduct, Isaiyo rosea extract, St. John's rose extract, Melilot 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 alcohols are not particularly limited, and include, for example, linear alcohols such as lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, and cetostearyl alcohol, monostearyl glycerin ether (batyl alcohol), and 2-decyl alcohol. Examples include branched chain alcohols such as tetradecinol, lanolin alcohol, cholesterol, phytosterols, hexyldodecanol, isostearyl alcohol, and octyldodecanol.
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 metal ion sequestering agent is not particularly limited and includes, for example, 1-hydroxyethane-1,1-diphosphonic acid, 1-hydroxyethane-1,1-diphosphonic acid tetrasodium salt, sodium citrate, sodium polyphosphate, metaphosphoric acid. Examples include sodium, gluconic acid, phosphoric acid, citric acid, ascorbic acid, succinic acid, and edetic acid.
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。 The natural water-soluble polymers mentioned above are not particularly limited, and include, for example, gum aravia, gum tragacanth, galactan, guar gum, carob gum, gum karaya, carrageenan, pectin, agar, quince seed (quince), algae colloid (cassou extract), starch (rice, Plant polymers such as corn, potato, wheat), glycyrrhizic acid, microbial polymers such as xanthan gum, dextran, succinoglucan, pullulan, and animal polymers such as collagen, casein, albumin, and gelatin. .
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。 Semi-synthetic water-soluble polymers are not particularly limited, and include, for example, starch-based polymers such as carboxymethyl starch and methylhydroxypropyl starch, methylcellulose, nitrocellulose, ethylcellulose, methylhydroxypropylcellulose, hydroxyethylcellulose, sodium cellulose sulfate, Examples 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 propylene glycol alginate 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、ポリエチレンイミン、カチオン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 includes, for example, vinyl-based polymers such as polyvinyl alcohol, polyvinyl methyl ether, and polyvinylpyrrolidone, and polyoxyethylene-based polymers such as polyethylene glycol 20,000, 40,000, and 60,000. Examples include polymers, polyoxyethylene polyoxypropylene copolymer polymers, acrylic polymers such as sodium polyacrylate, polyethyl acrylate, and polyacrylamide, polyethyleneimine, and cationic polymers.
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A1Mg(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。 The inorganic water-soluble polymer is not particularly limited, and examples thereof include bentonite, A1Mg silicate (veegum), laponite, hectorite, and silicic anhydride.
油溶性高分子としては特に限定されず、例えば、ジステアルジモニウムヘクトライト、パルミチン酸デキストリン、ミリスチン酸デキストリン、(パルミチン酸/エチルヘキサン酸)デキストリン、(パルミチン酸/ヘキシルデカン酸)デキストリン、ステアリン酸イヌリン等を挙げることができる。 The oil-soluble polymer is not particularly limited, and includes, for example, disteardimonium hectorite, dextrin palmitate, dextrin myristate, (palmitate/ethylhexanoate) dextrin, (palmitate/hexyldecanoate) dextrin, and inulin stearate. etc. can be mentioned.
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 UV screening agent is not particularly limited, and includes, for example, para-aminobenzoic acid (hereinafter abbreviated as PABA), PABA monoglycerin ester, N,N-dipropoxy PABA ethyl ester, N,N-diethoxy PABA ethyl ester, N,N-dimethyl Benzoic acid-based UV screening agents such as PABA ethyl ester and N,N-dimethyl PABA butyl ester; Anthranilic acid-based UV screening agents such as homomenthyl-N-acetylanthranilate; amyl salicylate, menthyl salicylate, homomentyl salicylate, octyl salicylate , phenyl salicylate, benzyl salicylate, p-isopropanol phenyl salicylate, etc.; octyl cinnamate, ethyl-4-isopropyl cinnamate, methyl-2,5-diisopropyl cinnamate, ethyl-2,4-diisopropyl cinnamate mate, methyl-2,4-diisopropylcinnamate, propyl-p-methoxycinnamate, isopropyl-p-methoxycinnamate, isoamyl-p-methoxycinnamate, 2-ethoxyethyl-p-methoxycinnamate, cyclohexyl-p - Cinnamic acids such as methoxycinnamate, ethyl-α-cyano-β-phenylcinnamate, 2-ethylhexyl-α-cyano-β-phenylcinnamate, glyceryl mono-2-ethylhexanoyl-diparamethoxycinnamate UV screening agent: 2,4-dihydroxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, 2,2',4,4'-tetra Hydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4'-methylbenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonate, 4-phenylbenzophenone, 2-ethylhexyl- Benzophenone UV screening agents such as 4'-phenyl-benzophenone-2-carboxylate, 2-hydroxy-4-n-octoxybenzophenone, 4-hydroxy-3-carboxybenzophenone; 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-methylphenylbenzotriazole, 2 -(2'-hydroxy-5'-t-octylphenyl)benzotriazole, 2-(2'-hydroxy-5'-methylphenylbenzotriazole, dibenzalazine, dianisoylmethane, 4-methoxy-4'-t-butyl) Examples include dibenzoylmethane, 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 drug ingredients are not particularly limited, and include, for example, vitamin A oil, retinol, retinol palmitate, inosit, pyridoxine hydrochloride, benzyl nicotinate, nicotinamide, DL-α-tocopherol nicotinate, magnesium ascorbate phosphate, 2 -O-α-D-glucopyranosyl-L-ascorbic acid, vitamin D2 (ergocasiferol), dl-α-tocopherol, dl-α-tocopherol acetate, pantothenic acid, biotin, and other vitamins; estradiol, ethinylestradiol, etc. Hormones; Amino acids such as arginine, aspartic acid, cystine, cysteine, methionine, serine, leucine, tryptophan; Anti-inflammatory agents such as allantoin and azulene; Whitening agents such as arbutin; Astringents such as tannic acid; L-menthol, camphor Examples include cooling agents such as sulfur, lysozyme chloride, pyridoxine chloride, etc.
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、ヤグリマギクエキス、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 extracts are not particularly limited, and include, for example, Heutyami extract, Lavatica extract, Melilot extract, Dead Licorice extract, Licorice extract, Peony extract, Soapwort extract, Loofah extract, Cinchona extract, Saxifrage extract, Clara extract, Kouhone extract, Fennel extract. Extract, primrose extract, rose extract, rhododendron extract, lemon extract, rhubarb extract, aloe extract, calamus root extract, eucalyptus extract, horsetail extract, sage extract, thyme extract, tea extract, seaweed extract, cucumber extract, clove extract, rubus extract, melissa extract , carrot extract, horse chestnut extract, peach extract, peach leaf extract, mulberry extract, cornflower extract, hamamelis extract, placenta extract, thymus extract, silk extract, licorice extract, etc.
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酸化亜鉛粒子を混合して使用するものであってもよい。 The various powders mentioned above include bright colored pigments such as red iron oxide, yellow iron oxide, black iron oxide, titanium mica, titanium mica coated with iron oxide, and glass flakes coated with titanium oxide, mica, talc, kaolin, sericite, titanium dioxide, Examples include inorganic powders such as silica, and organic powders such as polyethylene powder, nylon powder, crosslinked polystyrene, cellulose powder, and silicone powder. Preferably, in order to improve organoleptic properties and make-up durability, part or all of the powder components are hydrophobized using a substance such as silicone, fluorine compound, metal soap, oil agent, acyl glutamate, etc. by a known method. used. Further, other zinc oxide particles not applicable to the present invention may be mixed and used.
本発明の水系分散体は、上述した化粧料の他に、放熱性組成物、ゴムの加硫促進剤、塗料・インキ用顔料、フェライトやバリスタ等の電子部品、医薬品等の分野においても使用することができる。 In addition to the above-mentioned cosmetics, the aqueous dispersion of the present invention can also be used in fields such as heat dissipating compositions, rubber vulcanization accelerators, pigments for paints and inks, electronic components such as ferrite and varistors, and pharmaceuticals. be able to.
以下に、実施例を挙げて本発明を説明するが、本発明はこれらの実施例によって何ら限定されるものではない。実施例中、配合割合において「%」とあるのは特に言及がない限り「質量%」を意味する。 The present invention will be described below with reference to Examples, but the present invention is not limited to these Examples in any way. In the examples, "%" in the compounding ratio means "% by mass" unless otherwise specified.
(原体酸化亜鉛ケーキの製造例)
FINEX-50(堺化学工業社製 一次粒子径0.020μm)80gを、酢酸亜鉛としての濃度が0.135mol/lの酢酸亜鉛水溶液1200mlにリパルプしスラリーとした。続いて、そのスラリーを攪拌しながら42分間で70℃ に昇温し、攪拌しながら70℃で2時間熟成した。熟成後、ろ過、水洗した。続いて、得られた固形物を水3リットルにリパルプしてスラリーとし、攪拌しながら95℃に昇温し、攪拌しながら95℃で60分間加熱洗浄した。加熱洗浄後、ろ過、水洗し、酸化亜鉛ケーキを得た。
(Production example of bulk zinc oxide cake)
80 g of FINEX-50 (manufactured by Sakai Chemical Industry Co., Ltd., primary particle size 0.020 μm) was repulped into 1200 ml of an aqueous zinc acetate solution having a concentration of 0.135 mol/l as a zinc acetate to form a slurry. Subsequently, the slurry was heated to 70°C for 42 minutes while stirring, and aged at 70°C for 2 hours while stirring. After aging, it was filtered and washed with water. Subsequently, the obtained solid material was repulped into 3 liters of water to form a slurry, heated to 95° C. with stirring, and heated and washed at 95° C. for 60 minutes while stirring. After heating and washing, it was filtered and washed with water to obtain a zinc oxide cake.
(製造例1)
製造例で得られたケーキをエタノール濃度が44%となるようにエタノール200mlと純水65mlを混合したエタノール水溶液にリパルプし、44%エタノール水溶液スラリーとした。44%エタノール水溶液20mlを酢酸でpH4に調整し、オクチルトリエトキシシラン(信越化学製KBE-3083)を2.0g(酸化亜鉛に対して2.5%)添加し、80℃で2時間攪拌することで得たオクチルトリエトキシシラン加水分解液を得た。44%エタノール水溶液スラリーを50℃に昇温し、オクチルトリエトキシシラン加水分解液を添加し、50℃を保持したまま2時間熟成した。熟成後、ろ過、水洗し、120℃で16時間乾燥することにより、一次粒子径が0.061μmのオクチルトリエトキシシラン被覆酸化亜鉛粒子を得た。
(Manufacturing example 1)
The cake obtained in the production example was repulped into an ethanol aqueous solution in which 200 ml of ethanol and 65 ml of pure water were mixed so that the ethanol concentration was 44% to obtain a 44% ethanol aqueous slurry. Adjust 20 ml of 44% ethanol aqueous solution to pH 4 with acetic acid, add 2.0 g (2.5% based on zinc oxide) of octyltriethoxysilane (KBE-3083, manufactured by Shin-Etsu Chemical), and stir at 80°C for 2 hours. An octyltriethoxysilane hydrolyzate was obtained. The 44% ethanol aqueous slurry was heated to 50°C, the octyltriethoxysilane hydrolyzate was added, and the mixture was aged for 2 hours while maintaining the temperature at 50°C. After aging, the mixture was filtered, washed with water, and dried at 120° C. for 16 hours to obtain octyltriethoxysilane-coated zinc oxide particles having a primary particle size of 0.061 μm.
(製造例2)
製造例1と同様に加熱洗浄、ろ過、水洗まで実施し、得られた固形物を乾燥機にて120℃で16時間乾燥して酸化亜鉛乾燥物を得た。得られた乾燥物をコーヒーミルにて粉砕し、酸化亜鉛粉体を得た。得られた酸化亜鉛粉体をポリ袋に入れ、オクチルトリエトキシシラン2.4g(酸化亜鉛に対して3%)を添加して混合し、乾燥機にて120℃で16時間熱処理することで、オクチルトリエトキシシラン被覆酸化亜鉛粒子を得た。
(Manufacturing example 2)
Heat washing, filtration, and water washing were carried out in the same manner as in Production Example 1, and the obtained solid was dried in a drier at 120° C. for 16 hours to obtain a dried zinc oxide product. The obtained dried product was ground in a coffee mill to obtain zinc oxide powder. The obtained zinc oxide powder was placed in a plastic bag, 2.4 g of octyltriethoxysilane (3% based on zinc oxide) was added, mixed, and heat treated in a dryer at 120 ° C. for 16 hours. Octyltriethoxysilane coated zinc oxide particles were obtained.
製造例1、製造例2で得られたオクチルトリエトキシシラン被覆酸化亜鉛粒子及び有機ケイ素表面被覆酸化亜鉛粒子A~Cのサイズ・形態を透過型電子顕微鏡(TEM、JEM-1200EX II、日本電子社製)で観察した。得られた粒子の物性を表1に示す。 The sizes and shapes of the octyltriethoxysilane-coated zinc oxide particles and organosilicon surface-coated zinc oxide particles A to C obtained in Production Examples 1 and 2 were examined using a transmission electron microscope (TEM, JEM-1200EX II, JEOL Ltd.). (manufactured by). Table 1 shows the physical properties of the obtained particles.
(実施例1~3)
表2に示す組成の水系分散体を、下記の製造方法により調製した。得られた水系分散体の物性、及び、塗膜の物性について評価を行い、結果を表2に示した。
なお、表2中で使用した原料は、下記の通りである。
PEG-9ジメチコン:KF-6013(信越化学社製)
PEG-10ジメチコン:KF-6943(信越化学社製)
(Examples 1 to 3)
An aqueous dispersion having the composition shown in Table 2 was prepared by the following manufacturing method. The physical properties of the obtained aqueous dispersion and the coating film were evaluated, and the results are shown in Table 2.
The raw materials used in Table 2 are as follows.
PEG-9 dimethicone: KF-6013 (manufactured by Shin-Etsu Chemical)
PEG-10 dimethicone: KF-6943 (manufactured by Shin-Etsu Chemical)
(製造方法)
成分6,7、成分8,9、成分1~5、成分10の順でビーカーに投入する度に金ヘラを用いて馴染ませ、攪拌機にて500rpmで15分間混合することにより、有機ケイ素化合物表面処理微粒子酸化亜鉛水分散体を得た。
(Production method)
Each time components 6 and 7, components 8 and 9, components 1 to 5, and component 10 are added to a beaker in that order, they are mixed using a metal spatula, and mixed for 15 minutes at 500 rpm with a stirrer to form the surface of the organosilicon compound. A treated fine particle zinc oxide aqueous dispersion was obtained.
(比較例1)
成分(A)を製造例2で得られた有機ケイ素表面被覆酸化亜鉛粒子に変更したこと以外は、実施例1と同様に水系分散体を製造した。
(Comparative example 1)
An aqueous dispersion was produced in the same manner as in Example 1, except that component (A) was changed to the organosilicon surface-coated zinc oxide particles obtained in Production Example 2.
(比較例2)
成分(A)を有機ケイ素表面被覆酸化亜鉛粒子Aに変更したこと以外は、実施例1と同様に水系分散体を製造した。
(Comparative example 2)
An aqueous dispersion was produced in the same manner as in Example 1, except that component (A) was changed to organosilicon surface-coated zinc oxide particles A.
(比較例3)
成分(A)を有機ケイ素表面被覆酸化亜鉛粒子Bに変更したこと以外は、実施例1と同様に水系分散体を製造した。
(Comparative example 3)
An aqueous dispersion was produced in the same manner as in Example 1, except that component (A) was changed to organosilicon surface-coated zinc oxide particles B.
(比較例4)
成分(A)を有機ケイ素表面被覆酸化亜鉛粒子Cに変更したこと以外は、実施例1と同様に水系分散体を製造した。
(Comparative example 4)
An aqueous dispersion was produced in the same manner as in Example 1, except that component (A) was changed to organosilicon surface-coated zinc oxide particles C.
成分(A)の物性を以下の方法により測定した。
(評価方法1)一次粒子径
成分(A)の粒子について、透過型電子顕微鏡JEM-1200EX II(日本電子社製 定格出力600W)で撮影した写真の2000~50000倍の視野での定方向径(粒子を挟む一定方向の二本の平行線の間隔;画像上のどのような形状の粒子についても、一定方向で測定した)で定義される粒子径(μm)であって、TEM写真内の一次粒子250個の定方向径を計測し、その累積分布の平均値を求めた。
The physical properties of component (A) were measured by the following method.
(Evaluation method 1) Regarding the particles of primary particle size component (A), the diameter in a fixed direction ( Particle diameter (μm) defined as the distance between two parallel lines in a fixed direction that sandwich a particle; particles of any shape on the image are measured in a fixed direction), and is the primary diameter in a TEM photograph. The directional diameters of 250 particles were measured, and the average value of the cumulative distribution was determined.
(評価方法2)BET比表面積
BET比表面積(m2/g)は、全自動BET比表面積測定装置MacsorbModel HM-1200(Mountech社製)により測定した。
(Evaluation method 2) BET specific surface area The BET specific surface area (m 2 /g) was measured using a fully automatic BET specific surface area measuring device Macsorb Model HM-1200 (manufactured by Mountech).
(評価方法3)ケイ素含有量
プレス機にて成形した粉体を、蛍光X線分析装置(リガク社製 PRIMUSII)にてFP法による半定量分析で測定した。
(Evaluation method 3) Silicon content The powder molded using a press was measured by semi-quantitative analysis using the FP method using a fluorescent X-ray analyzer (PRIMUSII manufactured by Rigaku Corporation).
(評価方法4)メジアン径1、メジアン径2
メジアン径1、メジアン径2は、レーザー回折/散乱式粒度分布測定装置LA-960S(堀場製作所社製)によって測定した。実施例、比較例の酸化亜鉛粒子0.4gを、イソプロピルアルコール200mlに入れ、メジアン径1は薬さじで馴染ませたスラリーを測定し、メジアン径2はスラリーを超音波ホモジナイザーUS-600E(日本精機製作所製)を用いて30秒間超音波分散したスラリーを測定した。実施例及び比較例の酸化亜鉛の屈折率を2.00、イソプロピルアルコールの屈折率を1.378とし、体積基準で測定した。メジアン径1は有姿の粒子の大きさを表し、メジアン径2は弱分散時の粒子の大きさを表す。
(Evaluation method 4) Median diameter 1, median diameter 2
Median diameter 1 and median diameter 2 were measured using a laser diffraction/scattering particle size distribution analyzer LA-960S (manufactured by Horiba, Ltd.). 0.4 g of zinc oxide particles of Examples and Comparative Examples were placed in 200 ml of isopropyl alcohol, and the median diameter of 1 was measured using a spoon.The median diameter of 2 was measured using an ultrasonic homogenizer US-600E (Nippon Seiki). The slurry that had been ultrasonically dispersed for 30 seconds was measured using a 30-second ultrasonically dispersed slurry (manufactured by Seisakusho). In Examples and Comparative Examples, the refractive index of zinc oxide was 2.00, and the refractive index of isopropyl alcohol was 1.378, and measurements were made on a volume basis. The median diameter 1 represents the size of particles in the form of particles, and the median diameter 2 represents the size of particles during weak dispersion.
(注2)FINEX-50-OTS(堺化学工業社製)
(注3)MZX-508OTS(テイカ株式会社製)
(Note 2) FINEX-50-OTS (manufactured by Sakai Chemical Industry Co., Ltd.)
(Note 3) MZX-508OTS (manufactured by Teika Co., Ltd.)
得られた水系分散体の物性、及び、塗膜の物性について、以下の方法で評価を行った。
(評価方法5)初期粘度
分散後、9mlのスクリュー瓶に分散体を入れ、B型粘度計(東京計器製)でローターNo.4を使用し、12rpmで回転開始から60秒後の粘度(25℃)を測定した。
The physical properties of the obtained aqueous dispersion and the physical properties of the coating film were evaluated by the following methods.
(Evaluation method 5) After initial viscosity dispersion, put the dispersion into a 9 ml screw bottle, and measure the rotor No. with a B-type viscometer (manufactured by Tokyo Keiki). 4, the viscosity (25° C.) was measured 60 seconds after the start of rotation at 12 rpm.
(評価方法6)40℃経時粘度
9mlのスクリュー瓶に分散体を入れ、40℃恒温槽にて7日間保管し、B型粘度計(東京計器製)でローターNo.4を使用し、12rpmで回転開始から60秒後の粘度を測定した。
(Evaluation method 6) Viscosity over time at 40°C: Put the dispersion in a 9ml screw bottle, store it in a constant temperature bath at 40°C for 7 days, and measure the rotor No. with a B-type viscometer (manufactured by Tokyo Keiki). 4, and the viscosity was measured 60 seconds after the start of rotation at 12 rpm.
(評価方法7)メジアン径3
得られた水系分散体を水で希釈後、レーザー回折/散乱式粒度分布測定装置LA-960S(堀場製作所社製)を用いて体積基準におけるメジアン径D50を測定した。
(Evaluation method 7) Median diameter 3
After diluting the obtained aqueous dispersion with water, the volume-based median diameter D50 was measured using a laser diffraction/scattering particle size distribution analyzer LA-960S (manufactured by Horiba, Ltd.).
(塗膜の作成)
水系分散体を、室温でスライドガラス(縦・横・厚み=76mm・26mm・0.8~1.0mm 松浪硝子工業社製)の上に少量滴下し、バーコーター(No.579 ROD No.10 安田精機製作所社製)でwet膜厚22.90μmの塗膜1を作成した。
また、塗膜1を50℃で2時間乾燥させ、塗膜2を得た。作成した塗膜1を平行光透過率1の測定に、塗膜2を平行光透過率2、白浮き、凹凸、光沢(20°グロス)の測定に用いた。
(Creation of coating film)
A small amount of the aqueous dispersion was dropped onto a slide glass (length/width/thickness = 76 mm, 26 mm, 0.8 to 1.0 mm, manufactured by Matsunami Glass Industry Co., Ltd.) at room temperature, and coated with a bar coater (No. 579 ROD No. 10). (manufactured by Yasuda Seiki Seisakusho Co., Ltd.) to form a coating film 1 with a wet film thickness of 22.90 μm.
Further, Coating Film 1 was dried at 50° C. for 2 hours to obtain Coating Film 2. The prepared coating film 1 was used to measure the parallel light transmittance 1, and the coating film 2 was used to measure the parallel light transmittance 2, white float, unevenness, and gloss (20° gloss).
(評価方法8)平行光透過率
平行光線透過率1(%)、平行光線透過率2(%)は、作成した塗膜1,2を分光光度計V-770(日本分光社製)で測定した値である。なお、平行光線透過率1(%)、平行光線透過率2(%)の値は波長600nmにおける平行光線透過率の値である。平行光線透過率1(%)、平行光線透過率2(%)の値が大きい程、可視光透明性が高いことを意味し、平行光透過率1に対する平行光透過率2の割合が高いほど、乾燥凝集が少なく白浮きが抑制されていることを意味する。
(Evaluation method 8) Parallel light transmittance Parallel light transmittance 1 (%) and parallel light transmittance 2 (%) are measured using a spectrophotometer V-770 (manufactured by JASCO Corporation) for the prepared coating films 1 and 2. This is the value. Note that the values of parallel light transmittance 1 (%) and parallel light transmittance 2 (%) are values of parallel light transmittance at a wavelength of 600 nm. The larger the values of parallel light transmittance 1 (%) and parallel light transmittance 2 (%), the higher the visible light transparency, and the higher the ratio of parallel light transmittance 2 to parallel light transmittance 1. This means that there is little dry agglomeration and white cast is suppressed.
(評価方法9)白浮き
塗膜1と塗膜2の白さの変化を目視にて観察した際に、下記の基準に従って評価した。
〇:塗膜1が塗膜2よりも白い、または塗膜1と塗膜2がほぼ同じ白さ
△:塗膜2が塗膜1よりもわずかに白い
×:塗膜2が塗膜1よりも白い
(Evaluation method 9) When the change in whiteness of white floating coating film 1 and coating film 2 was visually observed, evaluation was made according to the following criteria.
〇: Coating film 1 is whiter than coating film 2, or coating film 1 and coating film 2 are almost the same whiteness. △: Coating film 2 is slightly whiter than coating film 1. ×: Coating film 2 is slightly whiter than coating film 1. Also white
(評価方法10)乾燥後塗膜凹凸
塗膜2を工業用顕微鏡 ECLIPSE LV100ND(ニコン社製)で観察した際に、100μm×100μm内に観察された2μm以上の凝集物を下記の基準に従って評価した。
〇:30個以下
×:30個より多い
(Evaluation method 10) When the uneven coating film 2 after drying was observed using an industrial microscope ECLIPSE LV100ND (manufactured by Nikon Corporation), aggregates of 2 μm or more observed within 100 μm x 100 μm were evaluated according to the following criteria. .
〇: Less than 30 pieces ×: More than 30 pieces
(評価方法11)光沢(20°グロス)
本明細書において、塗膜の光沢(20°グロス)は、塗膜2をGLOSS METER VG7000(村上色彩技術研究所社製)により測定した値であり、入射角20°における光沢の値である。光沢(20°グロス)の値が大きいほど、作成した塗膜内部における酸化亜鉛粒子の凝集が少なく分散性が高いことで、乾燥凝集しにくく凹凸が少ないことを意味する。
(Evaluation method 11) Gloss (20° gloss)
In this specification, the gloss of the coating film (20° gloss) is a value measured by measuring the coating film 2 using GLOSS METER VG7000 (manufactured by Murakami Color Research Institute), and is the gloss value at an incident angle of 20°. The larger the value of gloss (20° gloss), the less agglomeration of zinc oxide particles inside the created coating film and the higher the dispersibility, which means that it is less likely to aggregate during drying and has fewer irregularities.
実施例の水系分散体は、高濃度、かつ低粘度で、40℃1週間保管後も粘度の大きな変化は見られず、安定性に優れた分散体であることが示された。また、平行光透過率1に対する平行光透過率2の割合も比較例に比べて大きく、白浮きが抑制されていることが示された。
乾燥後塗膜の凹凸、及び、光沢も良好で、乾燥後凝集が抑制されていることは明らかである。
The aqueous dispersion of the example had high concentration and low viscosity, and no major change in viscosity was observed even after storage at 40° C. for one week, indicating that it was a dispersion with excellent stability. Furthermore, the ratio of parallel light transmittance 2 to parallel light transmittance 1 was also larger than that of the comparative example, indicating that whitening was suppressed.
The unevenness and gloss of the coating film after drying were good, and it is clear that agglomeration after drying was suppressed.
(実施例4、比較例5,6,7)
得られた実施例1、比較例1,2,3の酸化亜鉛水分散体を用いて、以下に示す組成の実施例4および比較例5,6,7の日焼け止めO/Wクリームを調整し、その品質を評価した。
(Example 4, Comparative Examples 5, 6, 7)
Using the obtained zinc oxide aqueous dispersions of Example 1 and Comparative Examples 1, 2, and 3, sunscreen O/W creams of Example 4 and Comparative Examples 5, 6, and 7 having the compositions shown below were prepared. , evaluated its quality.
(注5)植物由来セルロース:RHEOCRYSTA C-2SP(第一工業製薬株式会社製)
(Note 5) Plant-derived cellulose: RHEOCRYSTA C-2SP (manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.)
(製造方法)
A:成分1~6を混合し、加熱する。
B:成分7~12を混合、溶解し均一にする。
C:BにAを添加して乳化し、冷却後に成分13を添加してそれぞれの日焼け止めO/Wクリーム(実施例4、比較例5~7)を得た。
(Production method)
A: Mix ingredients 1 to 6 and heat.
B: Mix and dissolve components 7 to 12 to make them uniform.
C: A was added to B and emulsified, and after cooling, component 13 was added to obtain each sunscreen O/W cream (Example 4, Comparative Examples 5 to 7).
(評価方法)
(in vitro SPF・in vitroUVAPF)
各サンプルをスライドガラス(縦・横・厚み=76mm・26mm・0.8~1.0mm 松浪硝子工業社製)にバーコーター(No.579 ROD No.6 安田精機製作所社製)で塗布し、分光光度計V-770(日本分光社製)で透過率を測定し、in vitro SPF値・in vitro UVAPF値を得た。
(Evaluation method)
(in vitro SPF・in vitroUVAPF)
Each sample was coated on a slide glass (length, width, thickness = 76 mm, 26 mm, 0.8-1.0 mm, manufactured by Matsunami Glass Industry Co., Ltd.) using a bar coater (No. 579 ROD No. 6, manufactured by Yasuda Seiki Seisakusho Co., Ltd.). Transmittance was measured using a spectrophotometer V-770 (manufactured by JASCO Corporation) to obtain in vitro SPF values and in vitro UVAPF values.
(べたつき)
専門評価パネル20名による使用テストを行い、実施例の水中油型乳化日焼け止め化粧料を皮膚上に塗付し、べたつきのなさを評価した。評価を以下の基準に基づいて行った。
[評 価 基 準 ]
非常に良好 :5点
良好 :4点
普通 :3点
やや不良 :2点
不良 :1点
[判 定 ]
平均点4.5以上 :◎
平均点3.5点以上4.5点未満:○
平均点2.5点以上3.5点未満:△
平均点2.5点未満 :×
(sticky)
A use test was conducted by 20 expert evaluation panels, in which the oil-in-water emulsion sunscreen cosmetics of Examples were applied onto the skin and the lack of stickiness was evaluated. Evaluation was performed based on the following criteria.
[Evaluation criteria ]
Very good: 5 points Good: 4 points Average: 3 points Slightly poor: 2 points Poor: 1 point
[judgement ]
Average score 4.5 or higher: ◎
Average score: 3.5 points or more but less than 4.5 points: ○
Average score 2.5 points or more but less than 3.5 points: △
Average score less than 2.5 points: ×
(きしみ)
専門評価パネル20名による使用テストを行い、実施例の水中油型乳化日焼け止め化粧料を皮膚上に塗付し、きしみのなさを評価した。評価を以下の基準に基づいて行った。
[評 価 基 準 ]
非常に良好 :5点
良好 :4点
普通 :3点
やや不良 :2点
不良 :1点
[判 定 ]
平均点4.5以上 :◎
平均点3.5点以上4.5点未満:○
平均点2.5点以上3.5点未満:△
平均点2.5点未満 :×
(squeak)
A usage test was conducted by 20 expert evaluation panels, in which the oil-in-water emulsion sunscreen cosmetics of the examples were applied onto the skin and the lack of squeakiness was evaluated. Evaluation was performed based on the following criteria.
[Evaluation criteria ]
Very good: 5 points Good: 4 points Average: 3 points Slightly poor: 2 points Poor: 1 point
[judgement ]
Average score 4.5 or higher: ◎
Average score: 3.5 points or more but less than 4.5 points: ○
Average score 2.5 points or more but less than 3.5 points: △
Average score less than 2.5 points: ×
実施例4で得られたO/Wクリームは経時変化を起こさず安定で、白浮きもなく、また、使用感に関しても、比較例5~6に比べて塗布時の肌へののび広がりが軽く滑らかで、比較例7に比べて塗布時の粉のきしみ感を感じない、感触の優れたO/Wクリームであった。
さらに、実施例4で得られたO/Wクリームは、比較例よりも優れたin vitroSPF値及びin vitroUVAPF値を示した。
The O/W cream obtained in Example 4 did not change over time, was stable, did not have a white cast, and in terms of feeling of use, it spread easily on the skin when applied compared to Comparative Examples 5 and 6. It was an O/W cream that was smooth and had an excellent feel, with no powdery feeling when applied compared to Comparative Example 7.
Furthermore, the O/W cream obtained in Example 4 showed superior in vitro SPF values and in vitro UV APF values than the comparative example.
実施例5(日焼け止めO/Wクリーム)
下記表5に示す成分を用い、以下の製造方法にて日焼け止めO/Wクリームを得た。
(製造方法)
A:成分1~6を均一に混合し、加温溶解する。
B:成分7~15を均一に混合し、加温する。
C:BにAを添加して乳化し、冷却して日焼け止めO/Wクリームを得た。
Example 5 (Sunscreen O/W cream)
A sunscreen O/W cream was obtained by the following manufacturing method using the ingredients shown in Table 5 below.
(Production method)
A: Components 1 to 6 are mixed uniformly and dissolved by heating.
B: Mix components 7 to 15 uniformly and heat.
C: A was added to B, emulsified, and cooled to obtain a sunscreen O/W cream.
(注7)(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:SIMULGEL NS(SEPPIC社製)
(注8)アクリル酸アルキルコポリマー:DERMACRYL AQF(ヌーリオン・ジャパン社製)
(注9)撥水性微粒子酸化チタン水分散体:DIS-AB-10W(堺化学工業社製)
(Note 7) (Hydroxyethyl acrylate/Na acryloyldimethyltaurine) copolymer: SIMULGEL NS (manufactured by SEPPIC)
(Note 8) Alkyl acrylate copolymer: DERMACRYL AQF (manufactured by Nourion Japan)
(Note 9) Water-repellent microparticle titanium oxide water dispersion: DIS-AB-10W (manufactured by Sakai Chemical Industry Co., Ltd.)
以上のようにして得られた実施例5の日焼け止めO/Wクリームは、酸化亜鉛と酸化チタンが混合分散した系にも関わらず経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで、後肌のべたつき感もきしみ感もなく、透明性が高く、白浮きがない、日焼け止め効果の持続性にも優れた有機紫外線吸収剤フリーの日焼け止めO/Wクリームであった。 The sunscreen O/W cream of Example 5 obtained as described above is stable without causing any change over time despite being a mixed and dispersed system of zinc oxide and titanium oxide, and also has a good feel when applied. An organic ultraviolet absorber-free sunscreen that spreads smoothly onto the skin, does not leave a sticky or greasy feeling, is highly transparent, does not leave a white cast, and has excellent long-lasting sunscreen effects. It was an O/W cream.
実施例6(日焼け止めO/Wクリーム)
下記表6に示す成分を用い、以下の製造方法にて日焼け止めO/Wクリームを得た。
(製造方法)
A:成分1~7を均一に混合し、加温溶解する。
B:成分8~16を均一に混合し、加温する。
C:Bに上記Aを添加して乳化し、冷却して日焼け止めO/Wクリームを得た。
Example 6 (Sunscreen O/W cream)
A sunscreen O/W cream was obtained by the following manufacturing method using the ingredients shown in Table 6 below.
(Production method)
A: Components 1 to 7 are mixed uniformly and dissolved by heating.
B: Mix components 8 to 16 uniformly and heat.
C: The above A was added to B, emulsified, and cooled to obtain a sunscreen O/W cream.
以上のようにして得られた実施例6の日焼け止めO/Wクリームは、経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで、後肌のべたつき感もきしみ感もなく、透明性が高く、白浮きがない、日焼け止め効果の持続性にも優れた有機紫外線吸収剤フリーの日焼け止めO/Wクリームであった。 The sunscreen O/W cream of Example 6 obtained as described above is stable without causing any change over time, and in terms of feeling of use, it spreads well on the skin when applied, is smooth, and has a smooth texture after application. It was an organic ultraviolet absorber-free sunscreen O/W cream with no sticky or squeaky feeling, high transparency, no white cast, and excellent long-lasting sunscreen effect.
実施例7(日焼け止めO/Wクリーム)
下記表7に示す成分を用い、以下の製造方法にて日焼け止めO/Wクリームを得た。
(製造方法)
A:成分1~8を均一に混合し、加温溶解する。
B:成分9~16を均一に混合し、加温する。
C:BにAを添加して乳化し、冷却して日焼け止めO/Wクリームを得た。
Example 7 (Sunscreen O/W cream)
A sunscreen O/W cream was obtained by the following manufacturing method using the ingredients shown in Table 7 below.
(Production method)
A: Mix components 1 to 8 uniformly and dissolve by heating.
B: Mix components 9 to 16 uniformly and heat.
C: A was added to B, emulsified, and cooled to obtain a sunscreen O/W cream.
以上のようにして得られた実施例7の日焼け止めO/Wクリームは、経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで、後肌のべたつき感もきしみ感もなく、透明性が高く、白浮きがない、日焼け止め効果の持続性、耐水性にも優れた日焼け止めO/Wクリームであった。 The sunscreen O/W cream of Example 7 obtained as described above is stable without causing any change over time, and in terms of feeling of use, it spreads well on the skin when applied, is smooth, and has a smooth texture after application. It was a sunscreen O/W cream with no sticky or squeaky feeling, high transparency, no white cast, long-lasting sunscreen effect, and excellent water resistance.
実施例8(O/Wリキッドファンデーション)
下記表8に示す成分を用い、以下の製造方法にてO/Wリキッドファンデーションを得た。
(製造方法)
A:成分1~8を均一に混合して、加温溶解する。
B:成分14~17を成分19の一部に均一に混合する。
C:成分9~12,18,19の残部を均一に混合し、加温する。
D:CにAを添加して乳化し、冷却後にBと13を添加して均一に混合し、O/Wリキッドファンデーションを得た。
Example 8 (O/W liquid foundation)
An O/W liquid foundation was obtained by the following manufacturing method using the components shown in Table 8 below.
(Production method)
A: Components 1 to 8 are mixed uniformly and dissolved by heating.
B: Components 14 to 17 are uniformly mixed into a portion of component 19.
C: The remaining components 9 to 12, 18, and 19 are mixed uniformly and heated.
D: A was added to C and emulsified, and after cooling, B and 13 were added and mixed uniformly to obtain an O/W liquid foundation.
(注13)撥水性酸化チタン液状分散体:DIP-T1(N)(堺化学工業社製)
(注14)撥水性酸化鉄(黄)液状分散体:DIP-Y1(N)(堺化学工業社製)
(注15)撥水性酸化鉄(赤)液状分散体:DIP-R1(N)(堺化学工業社製)
(注16)撥水性酸化鉄(黒)液状分散体:DIP-K1(N)(堺化学工業社製)
(注17)板状硫酸バリウム:H-LFM (堺化学工業社製)
(Note 13) Water-repellent titanium oxide liquid dispersion: DIP-T1 (N) (manufactured by Sakai Chemical Industry Co., Ltd.)
(Note 14) Water-repellent iron oxide (yellow) liquid dispersion: DIP-Y1 (N) (manufactured by Sakai Chemical Industry Co., Ltd.)
(Note 15) Water-repellent iron oxide (red) liquid dispersion: DIP-R1 (N) (manufactured by Sakai Chemical Industry Co., Ltd.)
(Note 16) Water-repellent iron oxide (black) liquid dispersion: DIP-K1 (N) (manufactured by Sakai Chemical Industry Co., Ltd.)
(Note 17) Plate barium sulfate: H-LFM (manufactured by Sakai Chemical Industry Co., Ltd.)
以上のようにして得られた実施例8のO/Wリキッドファンデーションは、経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで止まりも良く、後肌のべたつき感もきしみ感もなく、紫外線防御効果のある非常に化粧持ちに優れたO/Wリキッドファンデーションであった。 The O/W liquid foundation of Example 8 obtained as described above is stable without causing any change over time, and in terms of feeling of use, it spreads smoothly and stays on the skin well when applied, and has a good aftertaste. It was an O/W liquid foundation that did not make the skin feel sticky or squeaky, and had a UV protection effect and had excellent makeup longevity.
実施例9(日焼け止め W/Oミルク)
下記表9に示す成分を用い、以下の製造方法にて日焼け止めW/Oミルクを得た。
(製造方法)
A:成分1~9を均一に混合する。
B:成分10~14を均一に混合する。
C:AにBを添加して乳化し、日焼け止めW/Oミルクを得た。
Example 9 (Sunscreen W/O Milk)
A sunscreen W/O milk was obtained by the following manufacturing method using the ingredients shown in Table 9 below.
(Production method)
A: Mix components 1 to 9 uniformly.
B: Components 10 to 14 are mixed uniformly.
C: B was added to A and emulsified to obtain sunscreen W/O milk.
(注19)酸化チタンシリコーン分散体:DIS-11A(堺化学工業社製)
(注20)硫酸Ba:ばりまる(堺化学工業社製)
(Note 19) Titanium oxide silicone dispersion: DIS-11A (manufactured by Sakai Chemical Industry Co., Ltd.)
(Note 20) Ba sulfate: Barimaru (manufactured by Sakai Chemical Industry Co., Ltd.)
以上のようにして得られた実施例9の日焼け止めW/Oミルクは、経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで、後肌のべたつき感もきしみ感もなく、白浮きせずにソフトフォーカス効果があり、日焼け止め効果の持続性、耐水性にも優れた日焼け止めW/Oミルクであった。 The sunscreen W/O milk of Example 9 obtained as described above is stable without causing any change over time, and in terms of feeling of use, it spreads smoothly on the skin when applied, and has a smooth texture after application. It was a sunscreen W/O milk that was neither sticky nor squeaky, had a soft focus effect without leaving a white cast, and had excellent long-lasting sunscreen effect and water resistance.
実施例10(日焼け止め W/Oミルク)
下記表10に示す成分を用い、以下の製造方法にて日焼け止めW/Oミルクを得た。
(製造方法)
A:成分1~10を均一に混合する。
B:成分11~15を均一に混合する。
C:AにBを加えて乳化し、日焼け止めW/Oミルクを得た。
Example 10 (Sunscreen W/O Milk)
Sunscreen W/O milk was obtained using the ingredients shown in Table 10 below and by the following manufacturing method.
(Production method)
A: Mix components 1 to 10 uniformly.
B: Components 11 to 15 are mixed uniformly.
C: B was added to A and emulsified to obtain sunscreen W/O milk.
(注22)炭酸Ca:かるまるSMS-M5 (堺化学工業株式会社製)
(Note 22) Ca carbonate: Karumaru SMS-M5 (manufactured by Sakai Chemical Industry Co., Ltd.)
以上のようにして得られた実施例10の日焼け止めW/Oミルクは、経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで、後肌のべたつき感もきしみ感もなく、透明性が高く、白浮きがない、日焼け止め効果の持続性、耐水性にも優れた日焼け止めW/Oミルクであった。 The sunscreen W/O milk of Example 10 obtained as described above is stable without causing any change over time, and in terms of feeling of use, it spreads smoothly on the skin when applied, and has a smooth texture after application. It was a sunscreen W/O milk with no sticky or squeaky feeling, high transparency, no white cast, long-lasting sunscreen effect, and excellent water resistance.
実施例11(W/Oリキッドファンデーション)
下記表11に示す成分を用い、以下の製造方法にてW/Oリキッドファンデーションを得た。
(製造方法)
A:成分1~11を均一に混合する。
B:成分15~18を成分20の一部に均一に混合する。
C:成分12~14,19,20及びBを均一に混合する。
D:AにCを加えて乳化し、W/Oリキッドファンデーションを得た。
Example 11 (W/O liquid foundation)
A W/O liquid foundation was obtained by the following manufacturing method using the components shown in Table 11 below.
(Production method)
A: Mix components 1 to 11 uniformly.
B: Components 15 to 18 are uniformly mixed into a portion of component 20.
C: Components 12 to 14, 19, 20 and B are mixed uniformly.
D: C was added to A and emulsified to obtain a W/O liquid foundation.
以上のようにして得られた実施例11のW/Oリキッドファンデーションは、経時変化を起こさず安定で、また使用感に関しても、塗布時の肌へののび広がりが良くなめらかで止まりも良く、後肌のべたつき感もきしみ感もなく、皮脂吸着効果をもち、化粧持ち効果、耐水性に優れたW/Oリキッドファンデーションであった。 The W/O liquid foundation of Example 11 obtained as described above is stable without causing any change over time, and also has a feeling of use: it spreads well on the skin when applied, is smooth, stays on well, and has a good aftertaste. It was a W/O liquid foundation that did not make the skin feel sticky or squeaky, had a sebum adsorption effect, had a makeup-wearing effect, and was excellent in water resistance.
本発明の水系分散体は、化粧料の成分として好適に使用することができる。 The aqueous dispersion of the present invention can be suitably used as a component of cosmetics.
Claims (9)
前記有機ケイ素表面被覆酸化亜鉛粒子(A)は、透過型電子顕微鏡写真から測定した一次粒子径が0.1μm以下であり、
前記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量は、水系分散体全量に対して60質量%以上であり
波長600nmの(乾燥後塗膜の平行光透過率)/(塗布直後塗膜の平行光透過率)の比が0.8以上であり、
前記乾燥後塗膜は、前記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%の水系分散体を室温にて塗布した後に50℃で2時間乾燥させたものであり、
前記塗布直後塗膜は、前記有機ケイ素表面被覆酸化亜鉛粒子(A)の含有量が60質量%の水系分散体を室温にて塗布後5分以内のものである
ことを特徴とする水系分散体。 An aqueous dispersion containing organosilicon surface-coated zinc oxide particles (A), a nonionic surfactant (B), a polyhydric alcohol (C), and water (D),
The organosilicon surface-coated zinc oxide particles (A) have a primary particle diameter of 0.1 μm or less as measured from a transmission electron micrograph,
The content of the organosilicon surface-coated zinc oxide particles (A) is 60% by mass or more based on the total amount of the aqueous dispersion, and the content is (parallel light transmittance of the coating film after drying)/(parallel light transmittance of the coating film immediately after application) at a wavelength of 600 nm. parallel light transmittance) is 0.8 or more,
The dried coating film is obtained by applying an aqueous dispersion containing 60% by mass of the organosilicon surface-coated zinc oxide particles (A) at room temperature and then drying it at 50° C. for 2 hours,
The freshly applied coating film is an aqueous dispersion characterized in that the aqueous dispersion having a content of 60% by mass of the organosilicon surface-coated zinc oxide particles (A) is applied within 5 minutes at room temperature. .
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CN117298665A (en) * | 2023-11-29 | 2023-12-29 | 江苏赛欧信越消泡剂有限公司 | Polyether modified organosilicon defoamer and preparation method thereof |
CN117298665B (en) * | 2023-11-29 | 2024-02-09 | 江苏赛欧信越消泡剂有限公司 | Polyether modified organosilicon defoamer and preparation method thereof |
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