JPH0859238A - Surface-treated zinc oxide powder - Google Patents
Surface-treated zinc oxide powderInfo
- Publication number
- JPH0859238A JPH0859238A JP19919894A JP19919894A JPH0859238A JP H0859238 A JPH0859238 A JP H0859238A JP 19919894 A JP19919894 A JP 19919894A JP 19919894 A JP19919894 A JP 19919894A JP H0859238 A JPH0859238 A JP H0859238A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- aluminum
- fine powder
- treated
- cyclic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、酸化亜鉛微粉末の表面
処理されたものに関する。尚、本明細書において、”表
面処理”とは、以下に詳述するように、”微粒子粉末の
光触媒活性を抑制するために、微粒子表面に金属化合物
被膜層を形成する表面処理”を意味する。TECHNICAL FIELD The present invention relates to a surface-treated fine zinc oxide powder. In the present specification, "surface treatment" means "surface treatment for forming a metal compound coating layer on the surface of fine particles in order to suppress photocatalytic activity of fine particle powder", as described in detail below. .
【０００２】[0002]
【従来の技術】従来から酸化チタン粒子に対しては、光
触媒活性を抑制する目的で粒子表面を金属化合物の被覆
層を形成する表面処理が行なわれてきた（”酸化チタ
ン”清野学著、技報堂、1991年発行、２９〜３３頁参
照）が、酸化亜鉛粒子については、ほとんど行なわれて
いない。その理由としては、酸化亜鉛粒子は、酸化チタ
ン粒子に比べて光触媒活性が低く、例えば、樹脂に練り
込んで使用する場合に樹脂の劣化を促進するという問題
が生じないと考えられているためである。2. Description of the Related Art Titanium oxide particles have been conventionally subjected to a surface treatment for forming a coating layer of a metal compound on the surface of the particles for the purpose of suppressing photocatalytic activity ("Titanium oxide", written by Manabu Seino, Gihodo). , 1991, pp. 29-33), but little has been done with zinc oxide particles. The reason is that the zinc oxide particles have a lower photocatalytic activity than the titanium oxide particles, and for example, it is considered that there is no problem of promoting deterioration of the resin when kneaded into the resin. is there.
【０００３】然し乍ら、酸化亜鉛粒子の粒径が、０．１
μｍ以下と小さくした場合に、微粉末において、その表
面の占める割合が大きくなるため、光触媒活性が大きく
なり、樹脂に練り込んだり油脂と混合して使用する場合
に、これらの有機物を劣化、変質する恐れが生じてき
た。However, the particle size of zinc oxide particles is 0.1.
When the particle size is reduced to less than μm, the proportion of the surface of the fine powder increases, so the photocatalytic activity increases, and when these are kneaded into a resin or mixed with fats and oils, these organic substances are deteriorated or deteriorated. There is a fear of
【０００４】[0004]
【発明が解決しようとする課題】そこで、本発明者等
は、酸化チタン粒子で通常実施されている、光触媒活性
を低減する目的で行なっている表面処理方法を、０．１
μｍ以下の微粒子酸化亜鉛粒子に適用したところ、微粒
子酸化亜鉛の性状を著しく損なうため、同様の処理方法
が適用できないことが分かった。Therefore, the present inventors have conducted a surface treatment method, which is usually carried out with titanium oxide particles, for the purpose of reducing photocatalytic activity.
It was found that the same treatment method cannot be applied to the fine zinc oxide particles having a particle size of μm or less because the properties of the fine zinc oxide particles are significantly impaired.
【０００５】その原因として、酸化チタン粒子の表面処
理では、所定量のＡｌ、Ｓｉ、Ｔｉ、Ｚｒ、Ｓｂ、Ｓ
ｎ、Ｚｎ等の塩基水溶液を加え、これを中和するアルカ
リ又は酸を加えて生成する含水酸化物で酸化チタン粒子
表面を被覆する方法が行なわれるが、ｐＨ１１以上及び
ｐＨ４以下では、酸化亜鉛粒子は溶解してしまうこと、
また、たとえｐＨを４〜１１の範囲内に保持したとして
も液相処理後、乾燥する際に、酸化亜鉛粒子の凝集が著
しく、粉末の分散性が損なわれることを挙げることがで
きる。The reason for this is that in the surface treatment of titanium oxide particles, a predetermined amount of Al, Si, Ti, Zr, Sb, S is used.
A method of coating a titanium oxide particle surface with a hydrous oxide produced by adding an aqueous base solution of n, Zn or the like and adding an alkali or an acid to neutralize the same is used. Will dissolve,
Further, even if the pH is kept within the range of 4 to 11, it can be mentioned that the zinc oxide particles are remarkably aggregated during the drying after the liquid phase treatment and the dispersibility of the powder is impaired.
【０００６】即ち、本発明は、前記の課題を解決するた
めに成されたもので、酸化亜鉛粒子の光触媒活性を抑制
し、そして、同時に、微粉末の分散性を付与することを
目的とする。That is, the present invention has been made to solve the above-mentioned problems, and an object thereof is to suppress the photocatalytic activity of zinc oxide particles and, at the same time, to impart the dispersibility of fine powder. .
【０００７】[0007]
【課題を解決するための手段】本発明は、上記の技術的
な課題の解決のために、酸化亜鉛微粉末において、その
粒子表面がアルミニウムキレート化合物又は環状アルミ
ニウムオリゴマーにより表面処理がされていることを特
徴とする。また、更に、必要によりアルミニウムキレー
ト化合物又は環状アルミニウムオリゴマーの分解温度以
上で焼成することにより表面処理した酸化亜鉛微粉末で
ある。In order to solve the above technical problems, the present invention provides that zinc oxide fine powder is surface-treated with an aluminum chelate compound or a cyclic aluminum oligomer. Is characterized by. Further, it is a zinc oxide fine powder which is surface-treated by firing at a temperature not lower than the decomposition temperature of the aluminum chelate compound or the cyclic aluminum oligomer, if necessary.
【０００８】更に、アルミニウムキレート化合物又はア
ルミニウムオリゴマーの表面処理層の内部又は外部にＳ
ｉＯ2 被膜が更に形成されている酸化亜鉛微粉末を提供
する。Further, S is formed inside or outside the surface-treated layer of aluminum chelate compound or aluminum oligomer.
Provided is a zinc oxide fine powder further formed with an iO 2 coating.
【０００９】以下、本発明を詳しく説明する。本発明
は、酸化亜鉛微粉末の光触媒活性を抑制し、分散性を付
与することを目的とする表面処理に関する。The present invention will be described in detail below. The present invention relates to a surface treatment for the purpose of suppressing the photocatalytic activity of zinc oxide fine powder and imparting dispersibility.
【００１０】従って、本発明に用いる表面処理剤は、酸
化亜鉛粒子表面との親和性にすぐれ、凝集した粒子間隙
に浸透し、個々の粒子表面に均一に付着し、安定な被膜
を形成するものでなければならない。そして、その被膜
は、酸化亜鉛微粉末の光触媒反応を抑制するものでなけ
ればならない。Therefore, the surface-treating agent used in the present invention has a good affinity with the surface of zinc oxide particles, penetrates into the interstices of agglomerated particles, and uniformly adheres to the surface of each particle to form a stable film. Must. And the coating film must suppress the photocatalytic reaction of the zinc oxide fine powder.
【００１１】本発明者は、以上の観点から表面処理剤を
種々検討した結果、アルミニウムキレート化合物又はア
ルミニウムオリゴマーが適していることを見出し、本発
明に至ったものである。As a result of various investigations on the surface treatment agent from the above viewpoints, the present inventor has found that an aluminum chelate compound or an aluminum oligomer is suitable, and arrived at the present invention.
【００１２】本発明で用いられるアルミニウムキレート
化合物は、１乃至３のβ−ジケトン配位子又はβ−ケト
エステル配位子を有するアルミニウムキレート化合物
で、配位子として、アセチルアセトン、トリフルオロア
セチルアセトン、ベンゾイルアセトン、ヘキサフルオロ
アセトン、ベンゾイルトリフルオロアセトン、ジベンゾ
イルメタン、アセト酢酸メチルエステル、アセト酢酸エ
チルエステル、アセト酢酸ブチルエステル等を挙げるこ
とができる。これらの中で、特にアセチルアセトンを用
いることが好適である。The aluminum chelate compound used in the present invention is an aluminum chelate compound having 1 to 3 β-diketone ligands or β-ketoester ligands, and the ligands are acetylacetone, trifluoroacetylacetone and benzoylacetone. , Hexafluoroacetone, benzoyltrifluoroacetone, dibenzoylmethane, acetoacetic acid methyl ester, acetoacetic acid ethyl ester, acetoacetic acid butyl ester and the like. Among these, it is particularly preferable to use acetylacetone.
【００１３】アセチルアセトンキレート化合物として
は、エチルアセトアセテートアルミニウムジイソプロピ
レート、アルミニウムトリス（エチルアセトアセテー
ト）、オクチルアセトアセテートアルミニウムジイソプ
ロプレート、ステアリルアセトアルミニウムジイソプロ
ピレート、アルミニウムモノアセチルアセトネートビス
（エチルアセトアセテート）、アルミニウムトリス（ア
セチルアセトネート）等を例示することができる。Examples of the acetylacetone chelate compound include ethyl acetoacetate aluminum diisopropylate, aluminum tris (ethylacetoacetate), octylacetoacetate aluminum diisopropylate, stearylacetoaluminum diisopropylate, aluminum monoacetylacetonate bis (ethylacetoacetate). ), Aluminum tris (acetylacetonate), and the like.
【００１４】また、環状アルミニウムオリゴマーは、式
（Ｉ）に示す化学構造式の化合物であり、環状アルミニ
ウムオキサイドオクチレート、環状アルミニウムオキサ
イドステアレート、環状アルミニウムオキサイドイソプ
ロピレート等を例示することができる。The cyclic aluminum oligomer is a compound having the chemical structural formula shown in formula (I), and examples thereof include cyclic aluminum oxide octylate, cyclic aluminum oxide stearate, and cyclic aluminum oxide isopropylate.
【００１５】[0015]
【化１】 （但し、Ｘは、Ｒ又はＯＲである。Ｒは、Ｃ2 〜Ｃ13の
アルキル基を表示する）Embedded image (Wherein, X is R or OR .R displays an alkyl group of C 2 -C 13)
【００１６】前記の処理剤の添加量は、酸化亜鉛粒子重
量に対して、１重量％から１５重量％とすることが好適
である。更に好ましくは、１．５重量％から１２重量％
の範囲が、より好適である。処理剤が１重量％未満で
は、光触媒活性の抑制効果が低く、１５重量％を超える
と、処理に時間がかかり、また、処理剤の使用量が多く
なり、コスト的に不利である。The amount of the treatment agent added is preferably 1% by weight to 15% by weight based on the weight of the zinc oxide particles. More preferably from 1.5% to 12% by weight
Is more preferable. If the amount of the treating agent is less than 1% by weight, the effect of suppressing the photocatalytic activity is low, and if it exceeds 15% by weight, the treatment takes a long time, and the amount of the treating agent used increases, which is disadvantageous in terms of cost.
【００１７】表面処理方法としては、酸化亜鉛微粉末に
直接、処理剤を添加する乾式法又は溶媒に酸化亜鉛微粉
末を分散して処理剤を添加する湿式法が採用できる。As the surface treatment method, a dry method in which the treating agent is added directly to the zinc oxide fine powder or a wet method in which the treating agent is added by dispersing the zinc oxide fine powder in a solvent can be employed.
【００１８】乾式法では、ヘンシェルミキサー、スーパ
ーミキサー、レーデイゲミキサー、Ｖ型ブレンダーを用
いて、酸化亜鉛微粉末を良く撹拌し、処理剤の原液又は
希釈剤を添加し、十分均一になるまで分散することによ
り行なう。このときに、同時に加熱することにより、処
理剤の揮発成分を除去するとともに、酸化亜鉛粒子表面
への吸着力を大きくすることができる。In the dry method, a Henschel mixer, a super mixer, a Reedige mixer, and a V-type blender are used to stir the zinc oxide fine powder well, and a stock solution or a diluent of the treating agent is added until it becomes sufficiently uniform. This is done by dispersing. At this time, by heating at the same time, the volatile components of the treatment agent can be removed and the adsorption power to the surface of the zinc oxide particles can be increased.
【００１９】また、湿式法では、ボールミル、サンドミ
ル、ホジナイザー等を用いて、酸化亜鉛微粉末を非水溶
媒中に分散し、この分散液に処理剤を添加し、次いで、
濾過又は蒸留すること等により溶媒を除去することによ
り行なう。用いる溶媒としては、表面処理剤を溶解する
ことの外に、表面張力の小さいものが望ましく、ｎ−ヘ
キサン、トルエン、キシレン、イソプロパノール、トリ
クレン、ミネラルスピリット、パークレン等を用いるこ
とが好適である。In the wet method, the zinc oxide fine powder is dispersed in a non-aqueous solvent by using a ball mill, a sand mill, a homogenizer, etc., a treating agent is added to this dispersion, and then,
It is carried out by removing the solvent by filtration or distillation. As the solvent to be used, it is desirable to use one having a small surface tension in addition to dissolving the surface treatment agent, and it is preferable to use n-hexane, toluene, xylene, isopropanol, trichlene, mineral spirit, perklene or the like.
【００２０】分散溶媒としては、水を用いることは表面
張力が大きく、水分除去するときに、酸化亜鉛微粉末が
凝集するために好ましくない。また、湿式法は、乾式法
に比べ、粒子をより細かく分散することができ、均一な
表面処理が可能となる。然し乍ら、溶媒を除去する工程
が必要となり、コスト的には不利になる。It is not preferable to use water as the dispersion solvent because the surface tension is large and the zinc oxide fine powder aggregates when removing water. In addition, the wet method can disperse the particles more finely than the dry method, and enables uniform surface treatment. However, a step of removing the solvent is required, which is disadvantageous in cost.
【００２１】その光触媒活性の抑制効果は、処理剤の吸
着量に概ね比例している。従って、一回の表面処理量に
制限がある場合には、何回かに分けて行なうことが必要
である。光触媒活性の表面抑制効果を高くする必要があ
る場合には、必要に応じて、複数回に分けて表面処理す
ることができる。The effect of suppressing the photocatalytic activity is approximately proportional to the amount of the treatment agent adsorbed. Therefore, when the surface treatment amount is limited, it is necessary to divide into several times. When it is necessary to enhance the effect of suppressing the surface of the photocatalytic activity, the surface treatment can be carried out in plural times if necessary.
【００２２】本発明により、アルミニウムキレート化合
物又は環状アルミニウムオリゴマーにより処理された酸
化亜鉛粒子は、表面が親油性となり、有機物に対する分
散性にすぐれたものとなる。According to the present invention, the zinc oxide particles treated with the aluminum chelate compound or the cyclic aluminum oligomer have a lipophilic surface and have excellent dispersibility in organic substances.
【００２３】また、光触媒反応により生成する酸素ラジ
カルは、処理剤被膜内で消費されることとなるため、本
発明により表面処理された酸化亜鉛粒子は、光触媒活性
が抑制されている。Further, the oxygen radicals generated by the photocatalytic reaction are consumed in the treatment agent film, so that the zinc oxide particles surface-treated according to the present invention have suppressed photocatalytic activity.
【００２４】本発明の表面処理酸化亜鉛微粉末において
は、アルミニウムキレート化合物又は環状アルミニウム
オリゴマーの分解温度以上で焼成することにより、表面
処理された酸化亜鉛微粉末を親水性にすることができ、
水中への分散が容易となる。この場合、表面処理被膜
は、無機質となり、酸素ラジカルの捕促をより効果的に
行なうことができることとなる。これは、被膜がより緻
密になることによるためと推定される。In the surface-treated zinc oxide fine powder of the present invention, the surface-treated zinc oxide fine powder can be made hydrophilic by firing at a temperature above the decomposition temperature of the aluminum chelate compound or cyclic aluminum oligomer,
Dispersion in water becomes easy. In this case, the surface-treated coating becomes inorganic, and oxygen radicals can be more effectively trapped. It is presumed that this is because the coating becomes more dense.
【００２５】本発明は、更に、他の表面処理と組み合わ
せることも可能である。特に本発明の表面処理におい
て、その表面処理され形成された被膜の内部又は外部
に、ＳｉＯ2 被膜の処理形成を施すことにより、更に、
大きな光触媒活性低減効果を得ることができる。The present invention can also be combined with other surface treatments. In particular, in the surface treatment of the present invention, by performing the treatment formation of the SiO 2 coating on the inside or outside of the coating formed by the surface treatment,
A large effect of reducing the photocatalytic activity can be obtained.
【００２６】ＳｉＯ2 の表面処理は、使用材料、処理
量、処理方法等においては、既知の方法と同様に行なう
ことが望ましい。例えば、テトラエトキシシラン、テト
ラメトキシシラン、メチルトリエトキシシラン、ビニル
トリエトキシシラン等のシラン化合物による表面処理を
例示することができる。The surface treatment of SiO 2 is preferably performed in the same manner as the known method in terms of materials used, treatment amount, treatment method and the like. For example, surface treatment with a silane compound such as tetraethoxysilane, tetramethoxysilane, methyltriethoxysilane, and vinyltriethoxysilane can be exemplified.
【００２７】本発明によれば、光触媒活性を抑制するこ
とができ、酸化亜鉛粒子の凝集がなく、粉末分散性のす
ぐれた酸化亜鉛微粉末を得ることができる。According to the present invention, it is possible to obtain a zinc oxide fine powder which can suppress photocatalytic activity, do not aggregate zinc oxide particles, and have excellent powder dispersibility.
【００２８】本発明は、粒径０．１μｍ以下の微粒子酸
化亜鉛粒子に用いることが望ましいが、０．１μｍを超
える酸化亜鉛粒子に適用することも、一向に差し仕えな
い。The present invention is preferably used for fine zinc oxide particles having a particle size of 0.1 μm or less, but it can be applied to zinc oxide particles having a particle size of more than 0.1 μm.
【００２９】本発明による表面処理された酸化亜鉛微粉
末は、以上のように、光触媒活性を低減されていると同
時に、微粉末凝集が少なく、粉末の分散性が保持された
ものとして、得られる。As described above, the surface-treated zinc oxide fine powder according to the present invention has a reduced photocatalytic activity and, at the same time, is obtained as a fine powder with less aggregation and maintaining the dispersibility of the powder. .
【００３０】次に、本発明により表面処理された酸化亜
鉛微粉末を具体的な実施例により、説明するが、本発明
はそれらによって限定されるものではない。Next, the zinc oxide fine powder surface-treated according to the present invention will be explained with reference to specific examples, but the present invention is not limited thereto.
【００３１】尚、実施例１、２、３では、本発明による
Ａｌ2Ｏ3被膜形成処理のみの酸化亜鉛微粉末を例とした
が、実施例４では、本発明によるＡｌ2Ｏ3被膜形成の内
部にＳｉＯ2 被膜を形成した場合を例とした。更に、本
発明による表面処理を行なわない酸化亜鉛微粉末の特性
を測定したものを、参考例とした。In Examples 1, 2 and 3, the zinc oxide fine powder only by the Al 2 O 3 film forming treatment according to the present invention was taken as an example, but in Example 4, the Al 2 O 3 film forming according to the present invention was performed. An example is the case where a SiO 2 coating is formed inside. Further, the characteristics of the zinc oxide fine powder not subjected to the surface treatment according to the present invention were measured and used as a reference example.
【００３２】[0032]
【実施例１】平均粒径０．０２５μｍの微粒子酸化亜鉛
粉末５ｋｇにアルキルアセトアセテートアルミニウムジ
イソプロピレート（川研ファインケミカル株式会社製、
商品名アルミキレートＭ）０．９ｋｇを添加し、ヘンシ
ェルミキサーで１０００ｒｐｍの撹拌回転数で、１０分
間行ない、次いで、回転数を２０００ｒｐｍに上げ、１
３０℃に加熱して、２０分間撹拌した。その後、撹拌処
理された酸化亜鉛微粉末を取り出し、空気流通下で、５
００℃で１時間焼成した。この焼成処理により、約１．
５重量％のＡｌ2Ｏ3で被覆された酸化亜鉛微粉末が得ら
れた。Example 1 Alkyl acetoacetate aluminum diisopropylate (manufactured by Kawaken Fine Chemical Co., Ltd., was added to 5 kg of fine zinc oxide powder having an average particle diameter of 0.025 μm,
0.9 kg of trade name aluminum chelate M) was added, and the mixture was stirred for 10 minutes at 1000 rpm with a Henschel mixer, then the rotation speed was increased to 2000 rpm, and 1
Heat to 30 ° C. and stir for 20 minutes. Then, the zinc oxide fine powder subjected to the stirring treatment is taken out, and is put under an air flow for 5
It was baked at 00 ° C. for 1 hour. By this firing treatment, about 1.
A zinc oxide fine powder coated with 5% by weight of Al 2 O 3 was obtained.
【００３３】このようにして表面処理された酸化亜鉛粉
末について、光触媒活性を、以下の方法により測定し
た。即ち、表面処理された酸化亜鉛粉末１０重量部とワ
セリン９０重量部を良く混合し、４００Ｗ水銀ランプを
１時間照射した。照射の前後のワセリンの明度を、カラ
ーアナライザー（東京電色株式会社製、ＴＣ−１０００
−ＭＫII）により、１０度視野で反射光を、波長３８０
〜７８０μｍで、測定し、R.HunterのＬａｂ表色系にお
けるＬ（明度）を測定し、その変化ΔＬ（明度の差）に
より、光触媒活性を評価した。その測定結果を表１に示
す。The photocatalytic activity of the zinc oxide powder surface-treated in this manner was measured by the following method. That is, 10 parts by weight of the surface-treated zinc oxide powder and 90 parts by weight of petrolatum were thoroughly mixed and irradiated with a 400 W mercury lamp for 1 hour. The brightness of petrolatum before and after irradiation was measured with a color analyzer (TC-1000 manufactured by Tokyo Denshoku Co., Ltd.).
-MKII), reflected light in a 10 degree field of view with a wavelength of 380
At 780 μm, L (lightness) in R. Hunter's Lab color system was measured, and the change ΔL (difference in lightness) was used to evaluate photocatalytic activity. The measurement results are shown in Table 1.
【００３４】更に、以下の方法により、水に対する分散
性を評価した。表面処理された酸化亜鉛粉末１０重量部
を純水９０重量部中に懸濁し、超音波により、１０分間
分散させた。この液を試験管に入れ、２４時間静置し、
酸化亜鉛微粉末と水との分離状態を観察した。その観察
の結果を表１に示す。Further, the dispersibility in water was evaluated by the following method. 10 parts by weight of the surface-treated zinc oxide powder was suspended in 90 parts by weight of pure water and dispersed by ultrasonic waves for 10 minutes. Put this solution in a test tube and let stand for 24 hours.
The separated state of zinc oxide fine powder and water was observed. The results of the observation are shown in Table 1.
【００３５】[0035]
【実施例２】平均粒径０．０２５μｍの微粒子の酸化亜
鉛粉末５ｋｇにアルミニウムトリス（エチルアセトアセ
テート）（川研ファインケミカル株式会社製、商品名Ａ
ＬＣＨ−ＴＲ）１ｋｇを添加し、実施例１と同様な方法
により処理した。この表面処理により、約１．８重量％
のＡｌ2Ｏ3で被覆された酸化亜鉛粉末が得られた。Example 2 Aluminum tris (ethyl acetoacetate) (manufactured by Kawaken Fine Chemicals Co., Ltd., trade name A) was added to 5 kg of fine zinc oxide powder having an average particle size of 0.025 μm.
LCH-TR) 1 kg was added and treated in the same manner as in Example 1. By this surface treatment, about 1.8% by weight
An Al 2 O 3 -coated zinc oxide powder was obtained.
【００３６】得られた酸化亜鉛粉末の光触媒活性及び分
散性を実施例１と同様の方法により、測定した。その測
定結果は、表１に示される。The photocatalytic activity and dispersibility of the obtained zinc oxide powder were measured by the same method as in Example 1. The measurement results are shown in Table 1.
【００３７】[0037]
【実施例３】平均粒径０．０２５μｍの微粒子の酸化亜
鉛粉末５ｋｇに環状アルミニウムオキサイドイソプロピ
レート）（川研ファインケミカル株式会社製、商品名ア
ルゴマー７）１ｋｇを添加し、実施例１と同様な方法に
より表面処理した。この表面処理により、約３．４重量
％のＡｌ2Ｏ3で被覆された酸化亜鉛微粉末が得られた。Example 3 1 kg of cyclic aluminum oxide isopropyl) (Kawaken Fine Chemicals Co., Ltd., trade name Algomer 7) was added to 5 kg of fine zinc oxide powder having an average particle size of 0.025 μm, and the same method as in Example 1 was performed. Was surface-treated. This surface treatment resulted in zinc oxide fine powder coated with about 3.4% by weight of Al 2 O 3 .
【００３８】得られた酸化亜鉛微粉末の光触媒活性及び
分散性を実施例１と同様な方法により測定した。その測
定結果を表１に示す。The photocatalytic activity and dispersibility of the obtained zinc oxide fine powder were measured in the same manner as in Example 1. The measurement results are shown in Table 1.
【００３９】[0039]
【実施例４】平均粒径０．０２５μｍの微粒子の酸化亜
鉛粉末５ｋｇにメチルトリエトキシシラン０．５ｋｇを
添加し、ヘンシェルミキサーにより１０００ｒｐｍの撹
拌回転数で１０分間撹拌し、混合した。その後、容器を
１８０℃に加熱し、撹拌回転数を２０００ｒｐｍに上
げ、２０分間撹拌した。次に、容器温度を常温に戻し、
環状アルミニウムオキサイドジイソプロピレート０．５
ｋｇを添加し、１０００ｒｐｍの撹拌回転数で、１０分
間、混合し、次いで、容器を１３０℃に加熱し、回転数
を２０００ｒｐｍに上げ、２０分間、撹拌した。Example 4 0.5 kg of methyltriethoxysilane was added to 5 kg of fine zinc oxide powder having an average particle diameter of 0.025 μm, and the mixture was stirred by a Henschel mixer at a stirring rotation speed of 1000 rpm for 10 minutes and mixed. Then, the container was heated to 180 ° C., the stirring rotation speed was increased to 2000 rpm, and stirring was performed for 20 minutes. Next, return the container temperature to room temperature,
Cyclic aluminum oxide diisopropylate 0.5
kg was added and mixed at a stirring rotation speed of 1000 rpm for 10 minutes, then the container was heated to 130 ° C., the rotation speed was increased to 2000 rpm, and stirring was performed for 20 minutes.
【００４０】次に、混合撹拌した酸化亜鉛粉末を取り出
し、空気流通下で、５００℃で１時間焼成した。この表
面処理により、約３．４重量％のＳｉＯ2 及び約１．７
重量％のＡｌ2Ｏ3で被覆された酸化亜鉛微粉末が得られ
た。Next, the zinc oxide powder mixed and stirred was taken out and fired at 500 ° C. for 1 hour under air flow. This surface treatment resulted in about 3.4% by weight of SiO 2 and about 1.7.
A zinc oxide fine powder coated with wt% Al 2 O 3 was obtained.
【００４１】得られた酸化亜鉛微粉末の光触媒活性と分
散性を、実施例１と同様の方法により測定した。その測
定結果を表１に示す。The photocatalytic activity and dispersibility of the obtained zinc oxide fine powder were measured in the same manner as in Example 1. The measurement results are shown in Table 1.
【００４２】[0042]
【比較例】表面処理を施していない酸化亜鉛微粉末の光
触媒活性と実施例１と同様な方法により測定した。その
測定結果も、上記の実施例の結果と同様に、表１に示
す。Comparative Example The photocatalytic activity of zinc oxide fine powder not subjected to surface treatment and the same method as in Example 1 were measured. The measurement results are also shown in Table 1 in the same manner as the results of the above examples.
【００４３】[0043]
【表１】 [Table 1]
【００４４】表１から、本発明により表面処理された酸
化亜鉛微粉末は、光触媒活性が低減されており、樹脂に
練り込んだり油脂と混合して使用した場合にも、これら
有機物を劣化、変質することが少なく、それと同時に、
微粒子の分散性が良く保持されており、超音波で分散さ
れ、２４時間静置された後も、上澄みが生じなくて、安
定した分散性を有することが分かる。From Table 1, the zinc oxide fine powder surface-treated according to the present invention has a reduced photocatalytic activity, and even when it is used by being kneaded into a resin or mixed with a fat or oil, these organic substances are deteriorated or deteriorated. Less often and at the same time
It can be seen that the dispersibility of the fine particles is well maintained, the particles are dispersed by ultrasonic waves, and no supernatant is generated even after standing for 24 hours, and the particles have stable dispersibility.
【００４５】[0045]
【発明の効果】以上説明したように、本発明の表面処理
酸化亜鉛微粉末により、次のような顕著な技術的効果が
得られた。即ち、以上のように、アルミニウムキレート
化合物又はアルミニウムオリゴマーにより表面処理され
た酸化亜鉛粉末は、光触媒活性が大幅に抑制されてい
る。また、改善された分散性が保持されている。As described above, the surface-treated zinc oxide fine powder of the present invention has the following remarkable technical effects. That is, as described above, the photocatalytic activity of the zinc oxide powder surface-treated with the aluminum chelate compound or the aluminum oligomer is significantly suppressed. Also, the improved dispersibility is retained.
Claims (3)
又は環状アルミニウムオリゴマーにより表面処理した酸
化亜鉛微粉末。1. A zinc oxide fine powder whose surface is treated with an aluminum chelate compound or a cyclic aluminum oligomer.
状アルミニウムオリゴマーにより酸化亜鉛微粉末を表面
処理し、更に、 該アルミニウムキレート化合物及び環状アルミニウムオ
リゴマーの分解温度以上で焼成したことを特徴とする請
求項１に記載の表面処理した酸化亜鉛微粉末。2. The zinc oxide fine powder is surface-treated with the aluminum chelate compound or cyclic aluminum oligomer, and is further calcined at a decomposition temperature of the aluminum chelate compound or cyclic aluminum oligomer or higher. The surface-treated zinc oxide fine powder described.
ニウムオリゴマーの表面処理層の内部又は外部に、表面
処理によりＳｉＯ2 被膜が形成されていることを特徴と
する請求項１或いは２に記載の表面処理した酸化亜鉛微
粉末。3. The surface-treated oxidation according to claim 1 or 2, wherein a SiO 2 coating is formed inside or outside the surface-treated layer of the aluminum chelate compound or aluminum oligomer by surface treatment. Fine zinc powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19919894A JP3491983B2 (en) | 1994-08-24 | 1994-08-24 | Surface treated zinc oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19919894A JP3491983B2 (en) | 1994-08-24 | 1994-08-24 | Surface treated zinc oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0859238A true JPH0859238A (en) | 1996-03-05 |
| JP3491983B2 JP3491983B2 (en) | 2004-02-03 |
Family
ID=16403778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19919894A Expired - Lifetime JP3491983B2 (en) | 1994-08-24 | 1994-08-24 | Surface treated zinc oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3491983B2 (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998017730A1 (en) * | 1996-10-23 | 1998-04-30 | Kanebo, Ltd. | Zinc oxide powder with suppressed activity and cosmetic preparation |
| WO1998026011A1 (en) * | 1996-12-10 | 1998-06-18 | Catalysts & Chemicals Industries Co., Ltd. | Pigments coated with inorganic compounds and cosmetics |
| JP2000016841A (en) * | 1998-07-03 | 2000-01-18 | Nippon Shokubai Co Ltd | Laminated glass and intermediate film used therefor |
| JP2006036854A (en) * | 2004-07-23 | 2006-02-09 | Jsr Corp | Dispersion of metal oxide particle and method for producing the same |
| WO2014171322A1 (en) * | 2013-04-19 | 2014-10-23 | 住友大阪セメント株式会社 | Silicon-oxide-coated zinc oxide and method for manufacturing same, silicon-oxide-coated-zinc-oxide-containing composition, and cosmetic |
| JP2015006976A (en) * | 2013-04-19 | 2015-01-15 | 住友大阪セメント株式会社 | Silicon oxide-coated zinc oxide, production method thereof, silicon oxide-coated zinc oxide-containing composition, and cosmetic |
| JP2015110503A (en) * | 2013-04-19 | 2015-06-18 | 住友大阪セメント株式会社 | Silicon oxide-coated zinc oxide and production method of the same, silicon oxide-coated zinc oxide-containing composition, and cosmetic |
| JP2018115098A (en) * | 2017-01-20 | 2018-07-26 | 堺化学工業株式会社 | Surface treated zinc oxide powder and usage thereof |
| US10238589B2 (en) | 2014-03-31 | 2019-03-26 | Sumitomo Osaka Cement Co., Ltd. | Silicon oxide-coated zinc oxide, method for producing same, and composition and cosmetic including silicon oxide-coated zinc oxide |
| KR20210009953A (en) * | 2019-07-18 | 2021-01-27 | 주식회사 엘지화학 | Method for preparing positive electrode active material for lithium secondary battery and positive electrode active material thereby |
-
1994
- 1994-08-24 JP JP19919894A patent/JP3491983B2/en not_active Expired - Lifetime
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998017730A1 (en) * | 1996-10-23 | 1998-04-30 | Kanebo, Ltd. | Zinc oxide powder with suppressed activity and cosmetic preparation |
| EP0953610A4 (en) * | 1996-12-10 | 2008-06-25 | Catalysts & Chem Ind Co | Pigments coated with inorganic compounds and cosmetics |
| WO1998026011A1 (en) * | 1996-12-10 | 1998-06-18 | Catalysts & Chemicals Industries Co., Ltd. | Pigments coated with inorganic compounds and cosmetics |
| EP0953610A1 (en) * | 1996-12-10 | 1999-11-03 | Catalysts & Chemicals Industries Co., Ltd. | Pigments coated with inorganic compounds and cosmetics |
| US6355260B1 (en) | 1996-12-10 | 2002-03-12 | Catalysts & Chemicals Industries Co., Ltd. | Inorganic compound-coated pigments and cosmetics using the same |
| JP2000016841A (en) * | 1998-07-03 | 2000-01-18 | Nippon Shokubai Co Ltd | Laminated glass and intermediate film used therefor |
| JP2006036854A (en) * | 2004-07-23 | 2006-02-09 | Jsr Corp | Dispersion of metal oxide particle and method for producing the same |
| WO2014171322A1 (en) * | 2013-04-19 | 2014-10-23 | 住友大阪セメント株式会社 | Silicon-oxide-coated zinc oxide and method for manufacturing same, silicon-oxide-coated-zinc-oxide-containing composition, and cosmetic |
| JP2015006976A (en) * | 2013-04-19 | 2015-01-15 | 住友大阪セメント株式会社 | Silicon oxide-coated zinc oxide, production method thereof, silicon oxide-coated zinc oxide-containing composition, and cosmetic |
| JP2015110503A (en) * | 2013-04-19 | 2015-06-18 | 住友大阪セメント株式会社 | Silicon oxide-coated zinc oxide and production method of the same, silicon oxide-coated zinc oxide-containing composition, and cosmetic |
| KR20150144748A (en) * | 2013-04-19 | 2015-12-28 | 스미토모 오사카 세멘토 가부시키가이샤 | Silicon oxide-coated zinc oxide and method for manufacturing same, silicon oxide-coated zinc oxide containing composition, and cosmetic |
| US9642785B2 (en) | 2013-04-19 | 2017-05-09 | Sumitomo Osaka Cement Co., Ltd. | Silicon-oxide-coated zinc oxide and method for manufacturing same, silicon-oxide-coated-zinc-oxide-containing composition, and cosmetic |
| US10238589B2 (en) | 2014-03-31 | 2019-03-26 | Sumitomo Osaka Cement Co., Ltd. | Silicon oxide-coated zinc oxide, method for producing same, and composition and cosmetic including silicon oxide-coated zinc oxide |
| JP2018115098A (en) * | 2017-01-20 | 2018-07-26 | 堺化学工業株式会社 | Surface treated zinc oxide powder and usage thereof |
| KR20210009953A (en) * | 2019-07-18 | 2021-01-27 | 주식회사 엘지화학 | Method for preparing positive electrode active material for lithium secondary battery and positive electrode active material thereby |
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