JP2007223874A - Zinc oxide powder and its production method - Google Patents

Zinc oxide powder and its production method Download PDF

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JP2007223874A
JP2007223874A JP2006049951A JP2006049951A JP2007223874A JP 2007223874 A JP2007223874 A JP 2007223874A JP 2006049951 A JP2006049951 A JP 2006049951A JP 2006049951 A JP2006049951 A JP 2006049951A JP 2007223874 A JP2007223874 A JP 2007223874A
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zinc oxide
oxide powder
particles
plate
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JP4807569B2 (en
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Kazumichi Yanagisawa
和道 柳澤
Wuxing Zhang
五星 張
Yoshio Uchida
義男 内田
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Kyushu University NUC
Kochi University NUC
Sumitomo Chemical Co Ltd
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Kyushu University NUC
Kochi University NUC
Sumitomo Chemical Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide zinc oxide powders having high ultraviolet-screening performance without damaging the applicability when used as cosmetics, coating materials and the like. <P>SOLUTION: The zinc oxide powder comprises a platy particulate in which the primary particulates having the average particle size of ≥0.1 to ≤1 μm agglutinate in a plate-like form. The method for production of the zinc oxide powder comprising a platy particulate is characterized by: regulating the pH of the aqueous solution comprising zinc ions, chlorine ions and water to ≥5 to ≤6.5 to precipitate a zinc oxide precursor; hydrothermally treating the precursor-containing aqueous solution at a temperature of ≥170 to ≤250°C; lowering the temperature at a rate of ≥100 to ≤500°C/hr; and burning the dried hydrothermally-treated material at a temperature of ≥450 to ≤1,000°C. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、酸化亜鉛粉末およびその製造方法に関する。さらに詳しくは、板状粒子からなる酸化亜鉛粉末およびその製造方法に関する。   The present invention relates to zinc oxide powder and a method for producing the same. More specifically, the present invention relates to a zinc oxide powder comprising plate-like particles and a method for producing the same.

酸化亜鉛粉末は、紫外線遮蔽能を有し、化粧品、塗料、衣料品、包材品およびその他の紫外線遮蔽能を要する用途に用いられている。
従来の酸化亜鉛粉末として、亜鉛の塩類を含んだ酸性の水溶液から、酸性領域で水酸化亜鉛を析出し、８００℃の温度で加熱処理を行うことにより得られる六角板状の酸化亜鉛粉末が、特許文献１に具体的に記載されている。 Zinc oxide powder has an ultraviolet shielding ability and is used in cosmetics, paints, clothing, packaging materials, and other applications requiring ultraviolet shielding ability.
As a conventional zinc oxide powder, a hexagonal plate-shaped zinc oxide powder obtained by precipitating zinc hydroxide in an acidic region from an acidic aqueous solution containing zinc salts and performing a heat treatment at a temperature of 800 ° C., It is specifically described in Patent Document 1.

特開昭５３−８２６９８号公報JP-A-53-82698

しかしながら従来の酸化亜鉛粉末は、その紫外線遮蔽能が十分でなかった。本発明の目的は、化粧品、塗料等に用いたときの塗布性を損なうことなく、高い紫外線遮蔽能を有する酸化亜鉛粉末およびその製造方法を提供することにある。   However, the conventional zinc oxide powder has not had sufficient ultraviolet shielding ability. An object of the present invention is to provide a zinc oxide powder having a high ultraviolet shielding ability and a method for producing the same without impairing the applicability when used in cosmetics, paints and the like.

本発明者らは、鋭意研究を重ねた結果、本発明に至った。
すなわち、本発明は、下記の酸化亜鉛粉末およびその製造方法を提供するものである。
＜１＞平均粒子径が０．１μｍ以上１μｍ以下である一次粒子が板状に凝集してなる板状粒子からなる酸化亜鉛粉末。
＜２＞板状粒子の幅が５μｍ以上５００μｍ以下であり、板状粒子の厚みが一次粒子の平均粒子径より大きく５μｍ以下であり、前記幅を前記厚みで除した値が５以上１０００以下である前記＜１＞記載の酸化亜鉛粉末。
＜３＞亜鉛イオン、塩素イオンおよび水からなる水溶液をｐＨ５以上６．５以下に調整することにより、酸化亜鉛前駆体を析出し、該前駆体を含有する水溶液を１７０℃以上２５０℃以下の温度で水熱処理し、１００℃／時間以上５００℃／時間以下の速度で降温後、乾燥して得られる水熱処理品を４５０℃以上１０００℃以下の温度で焼成することを特徴とする板状粒子からなる酸化亜鉛粉末の製造方法。 As a result of intensive studies, the present inventors have reached the present invention.
That is, this invention provides the following zinc oxide powder and its manufacturing method.
<1> Zinc oxide powder comprising plate-like particles in which primary particles having an average particle diameter of 0.1 μm or more and 1 μm or less are aggregated in a plate shape.
<2> The width of the plate-like particles is 5 μm or more and 500 μm or less, the thickness of the plate-like particles is 5 μm or less larger than the average particle diameter of the primary particles, and the value obtained by dividing the width by the thickness is 5 or more and 1000 or less. The zinc oxide powder according to <1>.
<3> A zinc oxide precursor is precipitated by adjusting an aqueous solution comprising zinc ions, chlorine ions and water to a pH of 5 or more and 6.5 or less, and the aqueous solution containing the precursor is heated to a temperature of 170 ° C. or more and 250 ° C. or less. From the plate-like particles, characterized in that a hydrothermal treatment product obtained by hydrothermally treating at a rate of 100 ° C./hour to 500 ° C./hour and then drying is fired at a temperature of 450 ° C. to 1000 ° C. The manufacturing method of the zinc oxide powder which becomes.

本発明によれば、塗布性を損なうことなく、高い紫外線遮蔽能を有する酸化亜鉛粉末を提供することができ、該酸化亜鉛粉末は、化粧品、塗料、衣料品、包材品およびその他の紫外線遮蔽能を要する用途に適用でき、さらには該酸化亜鉛粉末を構成する一次粒子の平均粒子径の効果により、抗菌剤、脱臭剤、うわ薬、医薬、触媒等にも適用できることから、工業的に極めて有用である。   ADVANTAGE OF THE INVENTION According to this invention, the zinc oxide powder which has high ultraviolet-ray shielding ability can be provided, without impairing applicability | paintability, This zinc oxide powder is cosmetics, a coating material, clothing, packaging materials, and other ultraviolet-ray shielding. It can be applied to applications that require high performance, and it can also be applied to antibacterial agents, deodorants, glazes, pharmaceuticals, catalysts, etc. due to the effect of the average particle size of the primary particles constituting the zinc oxide powder. It is.

以下に本発明について詳しく説明する。
本発明の酸化亜鉛粒子は、平均粒子径が０．１μｍ以上１μｍ以下である一次粒子が凝集してなる板状粒子からなる。より、紫外線遮蔽能を高める意味では、平均粒子径は０．１μｍ以上０．５μｍ以下とすることが好ましい。ここで、一次粒子の平均粒子径は、一次粒子の走査型電子顕微鏡写真から測定される値であり、該写真に撮影されている、板状粒子を構成している一次粒子から任意に５０個抽出し、それぞれの粒子径を測定して得られる値の平均値である。 The present invention is described in detail below.
The zinc oxide particles of the present invention are composed of plate-like particles obtained by agglomerating primary particles having an average particle diameter of 0.1 μm or more and 1 μm or less. In order to improve the ultraviolet shielding ability, the average particle size is preferably 0.1 μm or more and 0.5 μm or less. Here, the average particle diameter of the primary particles is a value measured from a scanning electron micrograph of the primary particles, and 50 arbitrarily selected from the primary particles constituting the plate-like particles photographed in the photograph. The average value of the values obtained by extracting and measuring the respective particle diameters.

本発明における板状粒子について、その幅は５μｍ以上５００μｍ以下であることが好ましく、その厚みは、前記一次粒子の平均粒子径より大きく５μｍ以下であることが好ましい。また、前記幅を前記厚みで除した値が５以上１０００以下であることが好ましい。板状粒子の幅、厚みを前記の範囲とすることで、より塗布性に優れた酸化亜鉛粉末とすることができる。また、本発明における板状粒子は、前記の一次粒子が凝集してなることから、板状粒子の表面には凹凸が存在し、高い紫外線遮蔽能を有する酸化亜鉛粉末となるのである。   The width of the plate-like particles in the present invention is preferably 5 μm or more and 500 μm or less, and the thickness is preferably larger than the average particle diameter of the primary particles and 5 μm or less. Moreover, it is preferable that the value which remove | divided the said width | variety by the said thickness is 5 or more and 1000 or less. By setting the width and thickness of the plate-like particles within the above ranges, a zinc oxide powder with better coating properties can be obtained. Further, the plate-like particles in the present invention are formed by agglomeration of the primary particles, so that the surface of the plate-like particles has irregularities and becomes zinc oxide powder having high ultraviolet shielding ability.

また板状粒子の幅および厚みは後述の方法により制御することができ、用途に応じて、その幅、厚みは異なる場合がある。例えば化粧品用では、幅は５μｍ以上２０μｍ以下であり、厚みは０．１μｍ以上２μｍ以下である場合が好ましく、塗料用では、幅は５μｍ以上１０μｍであり、厚みは０．１μｍ以上１μｍ以下である場合が好ましい。   The width and thickness of the plate-like particles can be controlled by the method described later, and the width and thickness may vary depending on the application. For example, for cosmetics, the width is preferably 5 μm to 20 μm and the thickness is preferably 0.1 μm to 2 μm. For paints, the width is 5 μm to 10 μm, and the thickness is 0.1 μm to 1 μm. The case is preferred.

次に、本発明の酸化亜鉛粉末の製造方法について説明する。
本発明の酸化亜鉛粉末は、次のようにして製造することができる。すなわち原料として、亜鉛イオン、塩素イオンおよび水からなる水溶液を用い、該水溶液をｐＨ５以上６．５以下に調整することにより、酸化亜鉛前駆体を析出し、該前駆体を含有する水溶液を１７０℃以上２５０℃以下の温度で水熱処理し、１００℃／時間以上５００℃／時間以下の速度で降温後、乾燥して得られる水熱処理品を４５０℃以上１０００℃以下の温度で焼成して、製造することができる。 Next, the manufacturing method of the zinc oxide powder of this invention is demonstrated.
The zinc oxide powder of the present invention can be produced as follows. That is, an aqueous solution comprising zinc ions, chlorine ions and water is used as a raw material, and the aqueous solution is adjusted to pH 5 or more and 6.5 or less to precipitate a zinc oxide precursor, and an aqueous solution containing the precursor is 170 ° C. Hydrothermal treatment is performed at a temperature of 250 ° C. or less, and after cooling at a rate of 100 ° C./hour or more and 500 ° C./hour or less, a hydrothermal treatment product obtained by drying is fired at a temperature of 450 ° C. or more and 1000 ° C. or less to produce can do.

亜鉛イオン、塩素イオンおよび水からなる水溶液は、塩化亜鉛を水に溶解させることにより得ることができる。また、塩化亜鉛の代わりに硫酸亜鉛、硝酸亜鉛、酢酸亜鉛を用いてさらに塩酸（または塩化水素）を混合することによっても、水溶液を得ることができるが、このときは、本発明の板状粒子からなる酸化亜鉛粉末とならない場合があり、水溶液中の塩素イオン濃度とその他のイオン（硫酸イオン、硝酸イオン、酢酸イオン）の濃度とのバランスについて注意が必要である。また、水溶液中の亜鉛イオンの濃度は、０．３Ｍ以上３Ｍ以下であり、この範囲内においては、前記濃度が大きくなると、板状粒子の幅が大きくなる傾向にある。   An aqueous solution composed of zinc ions, chloride ions and water can be obtained by dissolving zinc chloride in water. In addition, an aqueous solution can be obtained by further mixing hydrochloric acid (or hydrogen chloride) using zinc sulfate, zinc nitrate, and zinc acetate instead of zinc chloride. Zinc oxide powder may not be formed, and attention must be paid to the balance between the chlorine ion concentration in the aqueous solution and the concentration of other ions (sulfate ion, nitrate ion, acetate ion). Further, the concentration of zinc ions in the aqueous solution is 0.3 M or more and 3 M or less. Within this range, the width of the plate-like particles tends to increase as the concentration increases.

上記のようにして、亜鉛イオン、塩素イオンおよび水からなる水溶液を得て、該水溶液と水酸化ナトリウム水溶液またはアンモニア水とを混合することにより、ｐＨを５以上６．５以下に調整する。このｐＨの範囲内においてはｐＨが大きくなると板状粒子の厚みが大きくなる傾向にある。このｐＨ調整工程において、該水溶液中に酸化亜鉛前駆体が析出する。また、ここでｐＨが６．５を超えると、本発明における酸化亜鉛粒子は板状とはならない傾向にあり、塗布性の点で好ましくない。   As described above, an aqueous solution composed of zinc ions, chlorine ions and water is obtained, and the aqueous solution is mixed with a sodium hydroxide aqueous solution or aqueous ammonia to adjust the pH to 5 or more and 6.5 or less. Within this pH range, the thickness of the plate-like particles tends to increase as the pH increases. In this pH adjustment step, a zinc oxide precursor is precipitated in the aqueous solution. Moreover, when pH exceeds 6.5 here, the zinc oxide particle in this invention exists in the tendency which does not become plate shape, and is unpreferable at the point of applicability | paintability.

次に、析出された酸化亜鉛前駆体を含む水溶液を、１７０℃以上２５０℃以下の温度、好ましくは２００℃以上２３０℃以下の温度で水熱処理し、１００℃／時間以上５００℃／時間以下の速度で降温後、乾燥することにより、水熱処理品を得る。この水熱処理品は、式Ｚｎ5（ＯＨ）8Ｃｌ2・２Ｈ2Ｏで表される化合物からなる場合がある。また、水熱処理の温度は、好ましくは０．５時間以上５時間以下、さらに好ましくは１時間以上２時間以下である。前記ｐＨ調整工程後に、前記の水熱処理を行わなければ、本発明の酸化亜鉛粉末とはならない。また、乾燥は、通常、乾燥機を用いて、６０℃以上１２０℃以下の温度範囲で保持して行う。 Next, the aqueous solution containing the precipitated zinc oxide precursor is hydrothermally treated at a temperature of 170 ° C. or more and 250 ° C. or less, preferably 200 ° C. or more and 230 ° C. or less, and 100 ° C./hour or more and 500 ° C./hour or less. A hydrothermally treated product is obtained by drying after cooling at a speed. This hydrothermally treated product may be composed of a compound represented by the formula Zn 5 (OH) 8 Cl 2 .2H 2 O. The temperature of the hydrothermal treatment is preferably 0.5 hours or more and 5 hours or less, more preferably 1 hour or more and 2 hours or less. If the hydrothermal treatment is not performed after the pH adjustment step, the zinc oxide powder of the present invention is not obtained. In addition, drying is usually performed by using a dryer and holding in a temperature range of 60 ° C. or higher and 120 ° C. or lower.

次に、上記の水熱処理品を４５０℃以上１０００℃以下の温度で焼成して、本発明の酸化亜鉛粉末を得る。この焼成温度の範囲において、焼成温度が高くなると一次粒子の平均粒子径が大きくなる傾向にある。焼成時の雰囲気は、通常、酸素または空気であるが、紫外線遮蔽能をより高くする意味では、酸素が好ましい。また、焼成時間は、通常１０分以上１０時間以下、好ましくは１時間以上３時間以下である。   Next, the hydrothermally treated product is fired at a temperature of 450 ° C. or higher and 1000 ° C. or lower to obtain the zinc oxide powder of the present invention. In this firing temperature range, the average particle size of the primary particles tends to increase as the firing temperature increases. The atmosphere at the time of firing is usually oxygen or air, but oxygen is preferable in the sense of increasing the ultraviolet shielding ability. The firing time is usually 10 minutes or longer and 10 hours or shorter, preferably 1 hour or longer and 3 hours or shorter.

次に、本発明を実施例によりさらに詳しく説明する。   Next, the present invention will be described in more detail with reference to examples.

実施例１
１Ｍの塩化亜鉛水溶液の水酸化ナトリウム水溶液添加によりｐＨを５．４に調製して、酸化亜鉛前駆体を析出させ、オートクレーブに入れ、２２０℃，１時間の水熱処理を行い、３００℃／時間の速度で室温まで降温させ、水熱処理品を得た。得られた水熱処理品は、式Ｚｎ5（ＯＨ）8Ｃｌ2・２Ｈ2Ｏで表される化合物からなる板状粒子からなった。該水熱処理品の走査型電子顕微鏡写真を図１に示す。該水熱処理品を酸素雰囲気で５００℃の温度で焼成すると、板状粒子からなる酸化亜鉛粉末が得られた。該酸化亜鉛粉末の走査型電子顕微鏡写真を図２、図３に示す。図２は板状粒子からなる粉末の写真であり、図３は板状粒子の表面を撮影した写真である。図２、図３から、該板状粒子の厚みは約１μｍ、大きさは約５０μｍであることがわかり、また板状粒子は、平均粒子径が約０．５μｍの一次粒子が凝集してなることがわかった。 Example 1
The pH is adjusted to 5.4 by adding 1M zinc chloride aqueous solution to sodium hydroxide solution, the zinc oxide precursor is precipitated, put into an autoclave, subjected to hydrothermal treatment at 220 ° C. for 1 hour, and 300 ° C./hour. The temperature was lowered to room temperature at a rate to obtain a hydrothermally treated product. The obtained hydrothermally treated product was composed of plate-like particles made of a compound represented by the formula Zn 5 (OH) 8 Cl 2 .2H 2 O. A scanning electron micrograph of the hydrothermally treated product is shown in FIG. When the hydrothermally treated product was fired at a temperature of 500 ° C. in an oxygen atmosphere, zinc oxide powder composed of plate-like particles was obtained. Scanning electron micrographs of the zinc oxide powder are shown in FIGS. FIG. 2 is a photograph of powder composed of plate-like particles, and FIG. 3 is a photograph of the surface of the plate-like particles. 2 and 3, it can be seen that the plate-like particles have a thickness of about 1 μm and a size of about 50 μm, and the plate-like particles are formed by aggregation of primary particles having an average particle diameter of about 0.5 μm. I understood it.

実施例２
水溶液の塩化亜鉛濃度を２Ｍとした以外は、実施例１と同様にして、水熱処理品を得た。得られた水熱処理品は、式Ｚｎ5（ＯＨ）8Ｃｌ2・２Ｈ2Ｏで表される化合物からなる板状粒子からなった。該水熱処理品の走査型電子顕微鏡写真を図４に示す。該水熱処理品を酸素雰囲気で５００℃の温度で焼成すると、板状粒子からなる酸化亜鉛粉末が得られた。 Example 2
A hydrothermally treated product was obtained in the same manner as in Example 1 except that the concentration of zinc chloride in the aqueous solution was 2M. The obtained hydrothermally treated product was composed of plate-like particles made of a compound represented by the formula Zn 5 (OH) 8 Cl 2 .2H 2 O. A scanning electron micrograph of the hydrothermally treated product is shown in FIG. When the hydrothermally treated product was fired at a temperature of 500 ° C. in an oxygen atmosphere, zinc oxide powder composed of plate-like particles was obtained.

比較例１
水酸化ナトリウム水溶液添加によりｐＨを８に調整した以外は、実施例１と同様にして、酸化亜鉛粉末を得た。得られた酸化亜鉛粉末は板状ではなかった。 Comparative Example 1
A zinc oxide powder was obtained in the same manner as in Example 1 except that the pH was adjusted to 8 by adding an aqueous sodium hydroxide solution. The obtained zinc oxide powder was not plate-shaped.

実施例１における水熱処理品を示す図。The figure which shows the hydrothermal treatment goods in Example 1. FIG. 実施例１における酸化亜鉛粉末を示す図。The figure which shows the zinc oxide powder in Example 1. FIG. 実施例１における酸化亜鉛粉末を構成する板状粒子の表面を拡大した図。The figure which expanded the surface of the plate-shaped particle which comprises the zinc oxide powder in Example 1. FIG. 実施例２における水熱処理品を示す図。The figure which shows the hydrothermal treatment goods in Example 2. FIG.

Claims (3)

平均粒子径が０．１μｍ以上１μｍ以下である一次粒子が板状に凝集してなる板状粒子からなる酸化亜鉛粉末。   A zinc oxide powder comprising plate-like particles obtained by agglomerating primary particles having an average particle diameter of 0.1 µm or more and 1 µm or less into a plate shape. 板状粒子の幅が５μｍ以上５００μｍ以下であり、板状粒子の厚みが一次粒子の平均粒子径より大きく５μｍ以下であり、前記幅を前記厚みで除した値が５以上１０００以下である請求項１記載の酸化亜鉛粉末。   The width of the plate-like particles is 5 μm or more and 500 μm or less, the thickness of the plate-like particles is larger than the average particle diameter of the primary particles and 5 μm or less, and the value obtained by dividing the width by the thickness is 5 or more and 1000 or less. The zinc oxide powder according to 1. 亜鉛イオン、塩素イオンおよび水からなる水溶液をｐＨ５以上６．５以下に調整することにより、酸化亜鉛前駆体を析出し、該前駆体を含有する水溶液を１７０℃以上２５０℃以下の温度で水熱処理し、１００℃／時間以上５００℃／時間以下の速度で降温後、乾燥して得られる水熱処理品を４５０℃以上１０００℃以下の温度で焼成することを特徴とする板状粒子からなる酸化亜鉛粉末の製造方法。   A zinc oxide precursor is precipitated by adjusting an aqueous solution comprising zinc ions, chlorine ions and water to a pH of 5 or more and 6.5 or less, and the aqueous solution containing the precursor is hydrothermally treated at a temperature of 170 ° C. or more and 250 ° C. or less. Zinc oxide comprising plate-like particles, characterized in that a hydrothermal treatment product obtained by drying after drying at a rate of 100 ° C./hour to 500 ° C./hour is fired at a temperature of 450 ° C. to 1000 ° C. Powder manufacturing method.
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JP2015038014A (en) * 2013-07-19 2015-02-26 パナソニック株式会社 Flaky powder, production method of flaky powder, and flaky powder-containing cosmetic
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JP7088773B2 (en) 2018-07-30 2022-06-21 株式会社ファンケル Plate-shaped zinc oxide powder and cosmetics containing it

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