JP2880173B2 - Method for producing particles - Google Patents
Method for producing particlesInfo
- Publication number
- JP2880173B2 JP2880173B2 JP23634888A JP23634888A JP2880173B2 JP 2880173 B2 JP2880173 B2 JP 2880173B2 JP 23634888 A JP23634888 A JP 23634888A JP 23634888 A JP23634888 A JP 23634888A JP 2880173 B2 JP2880173 B2 JP 2880173B2
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- Japan
- Prior art keywords
- particles
- water
- organic compound
- added
- core
- Prior art date
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Description
【発明の詳細な説明】 ［発明の技術分野］ 本発明は、粒径が非常に良く揃いしかも単分散性の良
好な粒子の製造方法に関する。Description: TECHNICAL FIELD [0001] The present invention relates to a method for producing particles having a very uniform particle size and good monodispersity.
［発明の技術的背景並びにその問題点］ 従来、アルコキシシランなど加水分解可能な有機化合
物を、水、アンモニアおよびアルコールの反応液中にお
いて加水分解することにより、粒子を得る方法が知られ
ている。[Technical Background of the Invention and Problems Thereof] Conventionally, there has been known a method of obtaining particles by hydrolyzing a hydrolyzable organic compound such as an alkoxysilane in a reaction solution of water, ammonia, and an alcohol.
従来法は、加水分解可能な有機化合物、水、アンモニ
アおよびアルコールを反応母液に連続的に同時添加して
加水分解させて核粒子を生成させ、その核粒子の粒径を
成長させているが、このような反応系では、最初に生成
した核粒子表面に加水分解可能な有機化合物の分解生成
物が沈着して成長すると同時に、新たな核粒子が発生
し、この核粒子も先に存在した核粒子と同様に粒径の成
長が起こるため、最終的に得られる粒子の粒径分布が広
がった粒径の不揃いの粒子が製造されることになる。In the conventional method, a hydrolyzable organic compound, water, ammonia and alcohol are continuously and simultaneously added to the reaction mother liquor to hydrolyze to generate core particles and grow the particle size of the core particles. In such a reaction system, decomposition products of an organic compound that can be hydrolyzed are deposited and grown on the surface of the initially generated core particles, and at the same time, new core particles are generated. Since the growth of the particle size occurs as in the case of the particles, particles having irregular particle diameters in which the particle size distribution of the finally obtained particles is widened are produced.
新たな核粒子が発生するのは、有機化合物の加水分解
が核粒子の表面だけで起こるのではなく、反応溶液中で
も加水分解が起こり、分解生成物が核粒子表面に沈着さ
れずに、新たな核粒子として存在するようになるからで
ある。New core particles are generated not only because the hydrolysis of the organic compound occurs only on the surface of the core particles but also in the reaction solution, and the decomposition products are not deposited on the surface of the core particles. This is because they will be present as core particles.
［発明の目的］ 本発明は、上記のような従来技術に伴う問題点を解決
しようとするものであって、粒径が非常に良く揃いしか
も単分散性の良好な粒子の製造方法の提供を目的として
いる。[Object of the Invention] The present invention is intended to solve the problems associated with the prior art as described above, and provides a method for producing particles having a very good uniform particle size and good monodispersity. The purpose is.
［発明の概要］ 本発明に係る粒子の第一の製造方法は、核粒子が非水
溶媒中に分散している反応母液に、加水分解可能な有機
化合物を添加し、核粒子表面に形成されている水和層の
水（以下水和水という）で前記有機化合物を加水分解さ
せ、分解生成物を核粒子表面に沈着させて成長させるも
のである。さらに第二の製造方法は、第一の製造方法に
よる工程および該工程で得られた粒子の分散液に水を添
加して該粒子の表面に水和層を再形成させる工程を交互
に行って粒子を製造するものである。[Summary of the Invention] In the first method for producing particles according to the present invention, a hydrolyzable organic compound is added to a reaction mother liquor in which core particles are dispersed in a non-aqueous solvent, and the reaction mixture is formed on the surface of the core particles. The organic compound is hydrolyzed with the water of the hydration layer (hereinafter referred to as hydration water), and the decomposition products are deposited on the surface of the core particles to grow. Further, the second production method alternately performs the step of the first production method and the step of adding water to the dispersion liquid of the particles obtained in the step to re-form a hydrated layer on the surface of the particles. It is for producing particles.
［発明の具体的説明］ 本発明に係る非水溶媒を分散媒とする核粒子分散液に
ついて、まず説明する。[Specific description of the invention] First, a nuclear particle dispersion using a non-aqueous solvent according to the present invention as a dispersion medium will be described.
本発明に係る非水溶媒とは、加水分解可能な有機化合
物を溶解することができ、しかも水と均一に混合できる
ものであれば特に制限しない。例えば、メタノール、エ
タノール、ｎ−プロパノール、ｉ−プロパノール、ｎ−
ブタノール、ｉ−ブタノール、sec−ブタノール、tert
−ブタノール、エチレングリコール、プロピレングリコ
ール等のアルコール類、エチレングリコールモノメチル
エーテル、エチレングリコールモノエチルエーテル、エ
チレングリコールモノブチルエーテル等のエーテル類、
ジメチルホルムアミド、Ｎ−メチル−２−ピロリドンな
どが単独あるいは組合せて用いられる。また前記の非水
溶媒に疎水性有機溶媒を混合しても良い。The non-aqueous solvent according to the present invention is not particularly limited as long as it can dissolve a hydrolyzable organic compound and can be uniformly mixed with water. For example, methanol, ethanol, n-propanol, i-propanol, n-propanol
Butanol, i-butanol, sec-butanol, tert
Alcohols such as butanol, ethylene glycol and propylene glycol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethers such as ethylene glycol monobutyl ether,
Dimethylformamide, N-methyl-2-pyrrolidone and the like are used alone or in combination. Further, a hydrophobic organic solvent may be mixed with the non-aqueous solvent.
本発明に用いられる核粒子は、前記非水溶媒中に単分
散しており、水和層をその表面に有している粒子であれ
ば、粒子を構成する元素、形状、大きさは特に限定しな
いが、特に水和層をその表面に有するシリカゾルが好ま
しい。The core particles used in the present invention are monodispersed in the non-aqueous solvent, and as long as the particles have a hydration layer on the surface, the elements constituting the particles, the shape, and the size are particularly limited. However, a silica sol having a hydrated layer on its surface is particularly preferred.
本発明に係る加水分解可能な有機化合物は、M(OR)4ま
たはMR′n(OR)n-4（ｎは１または２）で表わされる金属
アルコキシドで、その一種または二種以上の混合物が好
ましく使用される。ＲまたはＲ′は、メチル基、エチル
基、プロピル基、ブチル基等の低級アルキル基が好適で
ある。Ｍはアルコキシドを形成する金属、例えば、Be、
Ｂ、Al、Si、Ｐ、Sc、Ti、Ｖ、Cr、Fe、Ni、Zn、Ga、G
e、As、Se、Ｙ、Zr、Nb、In、Sn、Sb、Te、Hf、Ta、
Ｗ、Pb、Biが使用できる。添加する加水分解可能な有機
化合物の金属元素は、核粒子を構成する金属元素と同一
のものでも、異種のものでもかまわない。従って同一の
ものを添加した場合には、単一元素の化合物からなる粒
子が得られ、異種のものを添加した場合には、異種元素
の化合物が表面に沈着した二層構造を有する粒子が得ら
れる。さらに加水分解可能な有機化合物は、同一のもの
を供給し続けてもよいし、粒子成長の途中で異種のもの
に変えてもよい。途中で異種のものに変更した場合に
は、多層構造を有する粒子が得られる。Hydrolyzable organic compounds according to the present invention, M (OR) 4 or MR 'n (OR) n- 4 (n is 1 or 2) with a metal alkoxide represented by the one or a mixture of two or more is It is preferably used. R or R 'is preferably a lower alkyl group such as a methyl group, an ethyl group, a propyl group, and a butyl group. M is a metal forming an alkoxide, for example, Be,
B, Al, Si, P, Sc, Ti, V, Cr, Fe, Ni, Zn, Ga, G
e, As, Se, Y, Zr, Nb, In, Sn, Sb, Te, Hf, Ta,
W, Pb, Bi can be used. The metal element of the hydrolyzable organic compound to be added may be the same as or different from the metal element constituting the core particles. Therefore, when the same compound is added, particles composed of a single element compound are obtained, and when different compounds are added, particles having a two-layer structure in which a compound of a different element is deposited on the surface are obtained. Can be Further, the same hydrolyzable organic compound may be continuously supplied, or may be changed to a different one during the grain growth. If a different type is used in the course, particles having a multilayer structure can be obtained.
非水溶媒を分散媒とする核粒子分散液は、核粒子の表
面の水和層により、分散媒中で粒子同士が結合せずに単
分散状態を保っている。本発明では、この水和層を形成
する水、つまり水和水によって加水分解可能な有機化合
物を加水分解させ、その分解生成物を核粒子表面に沈着
させ粒子成長を行わせる。従って表面の水和水がすべて
消費されると、もはや粒子成長は行われない。そこで、
さらに粒経の大きな粒子を得る場合は、粒子表面に新た
な水和層を形成するのに必要な量の水を反応母液に供給
する。このとき反応母液中には水和水以外の水の存在が
できるだけ少なくなるように供給する。反応母液中に水
が存在すると、その後供給される加水分解可能な有機化
合物がこの水で加水分解され、分解生成物が粒子表面に
沈着せずに新たな核粒子が発生し、粒径が不揃いになる
原因となる。The core particle dispersion liquid containing a non-aqueous solvent as a dispersion medium maintains a monodispersed state in the dispersion medium without the particles being bonded to each other due to the hydration layer on the surface of the core particles. In the present invention, water forming the hydration layer, that is, the hydrolyzable organic compound is hydrolyzed by the hydration water, and the decomposition product is deposited on the surface of the core particle to grow the particle. Therefore, when all the water of hydration on the surface has been consumed, particle growth no longer occurs. Therefore,
When particles having a larger particle diameter are to be obtained, an amount of water necessary to form a new hydration layer on the particle surface is supplied to the reaction mother liquor. At this time, the reaction mother liquor is supplied such that the presence of water other than water of hydration is minimized. When water is present in the reaction mother liquor, the hydrolyzable organic compound supplied thereafter is hydrolyzed by the water, and decomposition products are not deposited on the particle surface, new core particles are generated, and the particle size becomes irregular. Cause
加水分解により水和水の全部が消費されたとしても、
粒子の表面はアルコキシ基によって覆われているため、
粒子の単分散状態は保たれている。Even if all the water of hydration is consumed by hydrolysis,
Because the surface of the particles is covered with alkoxy groups,
The monodispersed state of the particles is maintained.
本発明では、消費された量に見合う水が反応母液に添
加されると、粒子表面のアルコキシ基と水が反応して、
水酸基とアルコールが生成され、さらに粒子表面が水和
層で覆われるようになることがある。In the present invention, when water corresponding to the consumed amount is added to the reaction mother liquor, the alkoxy group on the particle surface reacts with water,
Hydroxyl groups and alcohol are generated, and the particle surface may become covered with a hydrated layer.
（−OR＋H2O → −OH＋ROH） 加水分解時の反応温度は特に限定しないが、水または
非水溶媒の沸点以上で行う場合は、反応母液内の液層を
保持できるように加圧することが好ましい。(−OR + H 2 O → −OH + ROH) The reaction temperature during the hydrolysis is not particularly limited. However, when the reaction is carried out at a temperature higher than the boiling point of water or a non-aqueous solvent, it is preferable to apply pressure so that the liquid layer in the reaction mother liquor can be maintained. .
［発明の効果］ 本発明においては、核粒子が非水溶媒中に分散してい
る反応母液に、加水分解可能な有機化合物を添加し、核
粒子表面の水和水で前記有機化合物を加水分解させ、分
解生成物を核粒子表面に沈着させて粒子成長を行わせる
ことにより、粒子を製造しているので、粒径が非常に良
く揃いしかも単分散性の良好な粒子が得られる。[Effect of the Invention] In the present invention, a hydrolyzable organic compound is added to a reaction mother liquor in which core particles are dispersed in a non-aqueous solvent, and the organic compound is hydrolyzed with water of hydration on the surface of the core particles. The particles are produced by depositing the decomposition products on the surface of the core particles and growing the particles, whereby particles having a very uniform particle size and good monodispersity can be obtained.
また添加する加水分解可能な有機化合物の金属元素
が、核粒子を構成する金属元素と同一のものを添加した
場合には、単一金属化合物の粒子が得られ、異種のもの
を添加した場合には、二層構造を有する粒子が得られ
る。さらに加水分解可能な有機化合物を、粒子成長の途
中で異種のものに変更した場合には、多層構造を有する
粒子が得られるという効果がある。In addition, when the metal element of the hydrolyzable organic compound to be added is the same as the metal element constituting the core particles, a single metal compound particle is obtained. Yields particles having a two-layer structure. Further, when the hydrolyzable organic compound is changed to a different one during the growth of the particles, there is an effect that particles having a multilayer structure can be obtained.
以下実施例により本発明を説明するが、本発明はこれ
ら実施例に限定されるものではない。Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited to these examples.
実施例１ メタノールに分散したシリカゾル（SiO2 30重量％
平均粒径80mμ）100gとエタノール650gと28％アンモニ
ア水3gとを充分混合し、核粒子分散液を調製した。この
シリカ粒子の全水和層の水は、2.15gであり、水和層の
厚さは、20であった。この液を撹拌し35℃に保持しなが
ら、エチルシリケート−28（SiO2に換算して28重量％）
12.44gとエタノール18gを添加した。その後15分間撹拌
を続けた。さらに28％アンモニア水3gを添加したのち、
５分間撹拌を続けた。Example 1 Silica sol dispersed in methanol (SiO 2 30% by weight)
100 g of an average particle size (80 μm), 650 g of ethanol and 3 g of 28% aqueous ammonia were sufficiently mixed to prepare a core particle dispersion. The water in the entire hydration layer of the silica particles was 2.15 g, and the thickness of the hydration layer was 20. Ethyl silicate-28 (28% by weight in terms of SiO 2 ) while stirring this solution and keeping it at 35 ° C.
12.44 g and 18 g of ethanol were added. Thereafter, stirring was continued for 15 minutes. After adding 3g of 28% ammonia water,
Stirring was continued for 5 minutes.
以下この操作を、エチルシリケート−28の全添加量が
5542g、エチルアルコールの全添加量が8155g及び28％ア
ンモニア水の全添加量が1370gになるまで繰返し、その
後２時間撹拌を続けた。Hereinafter, this operation is repeated until the total amount of ethyl silicate-28 added is reduced.
This was repeated until 5542 g, the total addition amount of ethyl alcohol became 8155 g, and the total addition amount of 28% aqueous ammonia became 1370 g, and then stirring was continued for 2 hours.
実施例２ エタノールに分散したシリカゾル（SiO2 30重量％
平均粒径300mμ）100gとエタノール650gと28％アンモニ
ア水0.8gとを充分混合し、核粒子分散液を調製した。こ
の粒子の全水和層の水は、0.55gであり、水和層の厚さ
は、20であった。この液を撹拌し35℃に保持しながら、
エチルシリケート−28 3.18gとエタノール4.57gを添加
した。その後15分間撹拌を続けた。さらに28％アンモニ
ア水0.8gを添加した後、５分間撹拌を続けた。Example 2 Silica sol dispersed in ethanol (SiO 2 30% by weight)
100 g of an average particle diameter of 300 mμ), 650 g of ethanol and 0.8 g of 28% aqueous ammonia were sufficiently mixed to prepare a core particle dispersion. The water in the entire hydration layer of the particles was 0.55 g, and the thickness of the hydration layer was 20. While stirring this liquid and keeping it at 35 ° C,
3.18 g of ethyl silicate-28 and 4.57 g of ethanol were added. Thereafter, stirring was continued for 15 minutes. Further, after adding 0.8 g of 28% aqueous ammonia, stirring was continued for 5 minutes.
以下この操作を、エチルシリケート−28の全添加量が
3786g、エチルアルコールの全添加量が5445g及び28％ア
ンモニア水の全添加量が918gになるまで繰返し、その後
２時間撹拌を続けた。Hereinafter, this operation is repeated until the total amount of ethyl silicate-28 added is reduced.
The process was repeated until 3786 g, the total amount of ethyl alcohol added reached 5445 g, and the total amount of 28% aqueous ammonia became 918 g, and then stirring was continued for 2 hours.
実施例３ エタノールに分散したシリカゾル（SiO2 10重量％
平均粒径1000mμ）400gとエタノール400gと28％アンモ
ニア水0.67gとを充分混合し、核粒子分散液を調製し
た。この粒子の全水和層の水は、0.22gであり、水和層
の厚さは、20であった。この液を撹拌し35℃に保持しな
がら、エチルシリケート−28 1.27gとエタノール1.69g
を添加した。その後15分間撹拌を続けた。さらに28％ア
ンモニア水0.31gを添加したのち、５分間撹拌を続け
た。Example 3 Silica sol dispersed in ethanol (SiO 2 10% by weight)
400 g of average particle diameter (1000 mμ), 400 g of ethanol and 0.67 g of 28% ammonia water were sufficiently mixed to prepare a core particle dispersion. The water in the entire hydration layer of the particles was 0.22 g, and the thickness of the hydration layer was 20. While stirring this solution and keeping it at 35 ° C, ethyl silicate -28 1.27 g and ethanol 1.69 g
Was added. Thereafter, stirring was continued for 15 minutes. Further, after adding 0.31 g of 28% aqueous ammonia, stirring was continued for 5 minutes.
以下この操作を、エチルシリケート−28の全添加量が
330g、エチルアルコールの全添加量が439g及び28％アン
モニア水の全添加量が83gになるまで繰返し、その後２
時間撹拌を続けた。Hereinafter, this operation is repeated until the total amount of ethyl silicate-28 added is reduced.
Repeat until 330g, total addition of ethyl alcohol is 439g and total addition of 28% ammonia water is 83g, then 2
Stirring was continued for hours.
実施例４ エタノールに分散したシリカゾル（SiO2 10重量％
平均粒径1500mμ）500gとエタノール500gと28％アンモ
ニア水0.25gとを充分混合し、核粒子分散液を調製し
た。この粒子の全水和層の水は、0.18gであり、水和層
の厚さは、20であった。この液を撹拌し35℃に保持しな
がら、エチルシリケート−28 1.05gとエタノール1.04g
を添加した。その後15分間撹拌を続けた。さらに28％ア
ンモニア水0.25gを添加したのち、５分間撹拌を続け
た。Example 4 Silica sol dispersed in ethanol (SiO 2 10% by weight)
500 g of an average particle diameter of 1500 mμ), 500 g of ethanol, and 0.25 g of 28% aqueous ammonia were sufficiently mixed to prepare a core particle dispersion. The water in the entire hydration layer of the particles was 0.18 g, and the thickness of the hydration layer was 20. While stirring this solution and keeping it at 35 ° C., 1.05 g of ethyl silicate-28 and 1.04 g of ethanol
Was added. Thereafter, stirring was continued for 15 minutes. Furthermore, after adding 0.25 g of 28% ammonia water, stirring was continued for 5 minutes.
以下この操作を、エチルシリケート−28の全添加量が
245g、エチルアルコールの全添加量が243g及び28％アン
モニア水の全添加量が60gになるまで繰返し、その後２
時間撹拌を続けた。Hereinafter, this operation is repeated until the total amount of ethyl silicate-28 added is reduced.
Repeat until 245g, total addition of ethyl alcohol is 243g and total addition of 28% ammonia water is 60g, then 2
Stirring was continued for hours.
実施例５ エチルシリケート−28の代わりにTiO2として28重量％
のテトライソプロポキシチタンを使用した以外は、実施
例１と同様にした。Example 5 28% by weight as TiO 2 instead of ethyl silicate-28
The procedure was the same as in Example 1, except that tetraisopropoxytitanium was used.
実施例６ エチルシリケート−28の代わりにZrO2として28重量％
のテトラブトキシジルコニウムを使用し、エタノールの
代わりにｎ−ブタノール／イソプロパノール（重量比1/
1）の混合溶剤を使用した以外は、実施例１と同様にし
た。Example 6 28% by weight as ZrO 2 instead of ethyl silicate-28
Of tetrabutoxyzirconium, and n-butanol / isopropanol (weight ratio 1 /
Example 1 was repeated except that the mixed solvent of 1) was used.
比較例１ メタノールに分散したシリカゾルの代わりに、水に分
散したシリカゾル（SiO2 30重量％ 平均粒径80mμ）10
0gを使用した以外は、実施例１と同様にした。Comparative Example 1 Instead of silica sol dispersed in methanol, silica sol dispersed in water (SiO 2 30% by weight, average particle size 80 mμ) 10
Same as Example 1 except that 0 g was used.
得られた粒子に対して、以下の評価を行った。 The following evaluation was performed on the obtained particles.
1.平均粒径を走査形電子顕微鏡（SEM）と、光透過式粒
度測定器（商品名CAPA-500 掘場製作所製）により測定
した。1. The average particle size was measured with a scanning electron microscope (SEM) and a light transmission type particle size measuring device (trade name: CAPA-500, manufactured by Digyard).
2.次式により均一係数を求めた。2. The uniformity coefficient was determined by the following equation.
均一係数（Cv）＝（D2−D1）／（2Dp） D1:重量累計16％のときの粒径 D2:重量累計84％のときの粒径 Dp:重量累計50％のときの粒径 なお、D1、D2、DpはCAPA-500による測定値である。Uniformity coefficient (Cv) = (D2-D1) / (2Dp) D1: Particle size when the total weight is 16% D2: Particle size when the total weight is 84% Dp: Particle size when the total weight is 50% D1, D2, and Dp are values measured by CAPA-500.
3.凝集状態をSEMにより観察した。3. The state of aggregation was observed by SEM.
4.全水和層の水量を測定し、水和層の厚さを算出した。4. The amount of water in all the hydrated layers was measured, and the thickness of the hydrated layers was calculated.
結果を表−１に示す。 The results are shown in Table 1.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｃ０９Ｃ 3/08 Ｃ０９Ｃ 3/08 (56)参考文献 特開 昭62−151469（ＪＰ，Ａ) 特開 昭63−113080（ＪＰ，Ａ) 特開 平２−1307（ＪＰ，Ａ) 特開 昭62−275005（ＪＰ，Ａ) 特開 昭61−220726（ＪＰ，Ａ) 特開 平１−275667（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) B01J 2/00 C01B 13/14 C01B 33/18 C01G 23/053 C01G 25/00 C09C 3/08 B01J 19/00 ────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification symbol FI C09C 3/08 C09C 3/08 (56) References JP-A-62-151469 (JP, A) JP-A-63-113080 (JP) JP-A-2-1307 (JP, A) JP-A-62-275005 (JP, A) JP-A-61-220726 (JP, A) JP-A-1-275667 (JP, A) (58) Field surveyed (Int.Cl. 6 , DB name) B01J 2/00 C01B 13/14 C01B 33/18 C01G 23/053 C01G 25/00 C09C 3/08 B01J 19/00
Claims (2)
有する核粒子分散液に、加水分解可能な有機化合物を添
加して、該有機化合物を前記核粒子表面の水和層の水に
よって加水分解させ、その分解生成物を核粒子の表面に
沈着させて成長させることを特徴とする粒子の製造方
法。1. A hydrolyzable organic compound is added to a core particle dispersion having a non-aqueous solvent as a dispersion medium and a hydration layer on the surface, and the organic compound is added to the hydration layer on the core particle surface. A method for producing particles, wherein the particles are hydrolyzed with water, and the decomposition products are deposited and grown on the surface of the core particles.
特徴とする粒子の製造方法。 非水溶媒を分散媒としかつ水和層を表面に有する核粒
子分散液に加水分解可能な有機化合物を添加して、該有
機化合物を核粒子表面の水和層の水によって加水分解さ
せ、その分解生成物を核粒子の表面に沈着させて該粒子
を成長させる工程。 前記工程で得られた粒子の分散液に水を添加して該粒
子の表面に水和層を再形成する工程。2. A method for producing particles, wherein the following steps are alternately performed. A non-aqueous solvent is used as a dispersion medium, and a hydrolyzable organic compound is added to the core particle dispersion having a hydration layer on the surface, and the organic compound is hydrolyzed with water of the hydration layer on the core particle surface. Depositing the decomposition products on the surface of the core particles and growing the particles. A step of adding water to the dispersion liquid of the particles obtained in the above step to re-form a hydrated layer on the surface of the particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23634888A JP2880173B2 (en) | 1988-09-22 | 1988-09-22 | Method for producing particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23634888A JP2880173B2 (en) | 1988-09-22 | 1988-09-22 | Method for producing particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0286823A JPH0286823A (en) | 1990-03-27 |
| JP2880173B2 true JP2880173B2 (en) | 1999-04-05 |
Family
ID=16999478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23634888A Expired - Lifetime JP2880173B2 (en) | 1988-09-22 | 1988-09-22 | Method for producing particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2880173B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7988947B2 (en) | 2004-11-23 | 2011-08-02 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of titanium |
| US7601327B2 (en) | 2004-11-23 | 2009-10-13 | E.I. Du Pont De Nemours And Company | Mesoporous oxide of hafnium |
| US20060263291A1 (en) | 2004-11-23 | 2006-11-23 | Carmine Torardi | Mesoporous amorphous oxide of titanium |
| US7601326B2 (en) | 2004-11-23 | 2009-10-13 | E. I. Du Pont De Nemours And Company | Mesoporous oxide of zirconium |
| US7858066B2 (en) | 2007-05-08 | 2010-12-28 | E.I. Du Pont De Nemours And Company | Method of making titanium dioxide particles |
-
1988
- 1988-09-22 JP JP23634888A patent/JP2880173B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0286823A (en) | 1990-03-27 |
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