JPH03153519A - Production of smectite - Google Patents
Production of smectiteInfo
- Publication number
- JPH03153519A JPH03153519A JP29522189A JP29522189A JPH03153519A JP H03153519 A JPH03153519 A JP H03153519A JP 29522189 A JP29522189 A JP 29522189A JP 29522189 A JP29522189 A JP 29522189A JP H03153519 A JPH03153519 A JP H03153519A
- Authority
- JP
- Japan
- Prior art keywords
- smectite
- colloidal silica
- mol
- urea
- synthesized
- 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
- 229910021647 smectite Inorganic materials 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008119 colloidal silica Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- -1 silicon alkoxide Chemical class 0.000 claims abstract description 9
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 7
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000002156 mixing Methods 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract 2
- 239000010703 silicon Substances 0.000 abstract 2
- 239000010419 fine particle Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 239000011686 zinc sulphate Substances 0.000 description 1
- 235000009529 zinc sulphate Nutrition 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は、最近、無機質フィルム、ビラードクレイ、ガ
スクロ分離材として注目を集めている膨潤性を有する層
状粘土鉱物の合成に関するもので、本発明により合成さ
れたスメクタイトは０．５μｍ以下と非常に粒径のそろ
った微粒子の結晶から構成されていることを特徴として
いるため、天然産のスメクタイトと異なり、さらに新し
い機能性を有した新規な材料としての利用が考えられる
。[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to the synthesis of layered clay minerals with swelling properties, which have recently attracted attention as inorganic films, billard clays, and gas chromatography separation materials. Synthesized smectite is characterized by being composed of fine particle crystals with a very uniform particle size of 0.5 μm or less, and therefore, unlike naturally occurring smectite, it can be used as a new material with new functionality. It is possible to use
〈従来の技術〉
これまでのＭｇスメクタイトは水熱合成法という、常圧
法に比較すれば非常に煩雑な方法で合成されてきた。
この方法は合成温度を１００℃以上に上げるために密閉
した容器が必要であり、連続生産には不適であった。常
圧下で合成する方法としては、ＮａＯＨやＫＯＨを用い
たＺｎ５Ｏ，と８１０２を主原料とするＺｎスメクタイ
トの合成方法があるが、この方法は単に試薬の混合によ
り得られるので、均一な組成でなかったり、粒径が均一
でなかったり、またＺｎＳＯ４のような特殊な元素を用
いなけらばならないという欠点もあった。<Prior Art> Until now, Mg smectite has been synthesized by a hydrothermal synthesis method, which is extremely complicated compared to the normal pressure method.
This method required a sealed container to raise the synthesis temperature to over 100°C, and was unsuitable for continuous production. As a method for synthesizing under normal pressure, there is a method for synthesizing Zn smectite using NaOH or KOH as the main raw materials and Zn5O and 8102, but this method is obtained simply by mixing reagents, so the composition is not uniform. It also has drawbacks such as non-uniform grain size, and the need to use special elements such as ZnSO4.
〈発明が解決しようとしている問題点〉本発明は、比較
的安価なマグネシウム塩を用い、常圧下で尿素を用いた
均一沈澱法により、コロイド化学的方法を用い、０．５
μｍ以下の微粒子のスメクタイトを合成し、層状の層間
に各種イオン、ポリカチオン、育機物或は酸化物等をイ
ンクカレートさせた新規な材料を得ることを目的とする
ものである。<Problems to be Solved by the Invention> The present invention uses a relatively inexpensive magnesium salt, a homogeneous precipitation method using urea under normal pressure, and a colloid chemical method.
The purpose is to synthesize smectite particles of micrometers or less, and to obtain a new material in which various ions, polycations, nucleators, oxides, etc. are ink-calated between the layers.
く問題点を解決するための手段〉
上記本発明の目的は次のごとき方法を採用することによ
り達成できる。即ち、シリカアルコキシドの０．０１ｉ
ｏｌから０．５ｉｏｌの水溶液をｐＨ２からｐＨ５の間
に調整し、７０″Ｃから９０℃に加温後、微粒コロイダ
ルシリカを生成させる。この微粒子は数ナノメータから
数十ナノメータの大きさを有する超微粒子のコロイダル
シリカである。 冷却後、０．０１■０１から０．５ｉ
ｏｌのマグネシウム塩、 ０．０５■Ｏ１から０．１
■０！の尿素を混合し、 再度７０℃から９０℃に加温
する。この際尿素の分解によりｐＨは３から９程度にま
で上昇するためマグネシウム塩は水酸化物に変化する。Means for Solving the Problems> The above object of the present invention can be achieved by employing the following method. That is, 0.01i of silica alkoxide
An aqueous solution of 0.5 iol to 0.5 iol is adjusted to pH 2 to 5 and heated from 70"C to 90°C to produce fine colloidal silica particles. These fine particles have a size of several nanometers to several tens of nanometers. It is colloidal silica of fine particles. After cooling, 0.01■01 to 0.5i
Magnesium salt of ol, 0.05■O1 to 0.1
■0! of urea and heated again from 70°C to 90°C. At this time, the pH increases from about 3 to about 9 due to the decomposition of urea, so the magnesium salt changes to hydroxide.
この時コロイダルシリカは負の電荷を有し、マグネシウ
ム水酸化物は正の電荷を有することと、さらに反応漕の
中でｐＨが均一に変化していくため、両者は反応清白で
均一にヘテロ凝集を起こす。その後、２日から７日間同
温度に保持することにより、結晶成長し板状の形態を存
するスメクタイトを製造することができる。さらに、同
上の方法に、アルミニウム塩、或はアルミニウムアルコ
キシドを添加することにより、より結晶塵のよいスメク
タイトを合成することができる。At this time, colloidal silica has a negative charge, magnesium hydroxide has a positive charge, and the pH changes uniformly in the reaction tank, so the reaction between the two is clear and uniformly hetero-coagulated. wake up Thereafter, by maintaining the temperature at the same temperature for 2 to 7 days, it is possible to produce smectite that undergoes crystal growth and has a plate-like form. Furthermore, by adding an aluminum salt or aluminum alkoxide to the above method, smectite with better crystal dust can be synthesized.
〈実施例〉 以下本発明の実施例を示す。<Example> Examples of the present invention will be shown below.
実施例Ｉ シリカアルコキシドとしてエチルシリケイトを用いた。Example I Ethyl silicate was used as the silica alkoxide.
０．１１０１のエチルシリケイトの溶液をｐＨ３に調
整し、 ３００ｃｃのメスフラスコに入れ、オイルバ
ス中で９０℃、１２時間保持した後、冷却した。この時
溶液は、わずかに半透明を示しており、微粒のコロイダ
ルシリカが生成していた。この溶液に０．１ｉｏｌの塩
化マグネシウムと尿素を添加した。再度オイルバス中で
９０℃に４日間保持した後、冷却し、生成物を遠心分離
して、合成物の同定をＸ線粉末回折装置、並びに透過型
電子顕微鏡にて合成物の形態観察を行った。Ｘ線粉末回
折パターンを図１ （Ａ）に示す。 この図より板状形
態を示すスメクタイトが合成されている事がわかる。
図１（Ｂ）に０．０３ｉｏｌにした場合のＸ線粉末回折
パターンを示すが、０．１膳０１の場合よりより結晶塵
の良いことがわかる。図２にＯ，１ｉｏｌの合成物の電
子顕微鏡写真を示す。図２（Ａ）に示すように板状の形
態を示すスメクタイトも認められるが、まだ、図２（Ｂ
）に示すように一部にコロイダルシリカの微粒子も認め
られることより、完全にスメクタイトには変化していな
い。A solution of 0.1101 ethyl silicate was adjusted to pH 3, placed in a 300 cc volumetric flask, kept at 90° C. for 12 hours in an oil bath, and then cooled. At this time, the solution was slightly translucent, and fine particles of colloidal silica were produced. To this solution was added 0.1 iol of magnesium chloride and urea. After keeping it at 90°C for 4 days in an oil bath again, it was cooled, the product was centrifuged, and the morphology of the compound was observed using an X-ray powder diffraction device and a transmission electron microscope to identify the compound. Ta. The X-ray powder diffraction pattern is shown in Figure 1 (A). This figure shows that smectite with a plate-like morphology is synthesized.
FIG. 1(B) shows the X-ray powder diffraction pattern when the concentration is 0.03 iol, and it can be seen that the crystal dust is better than when the concentration is 0.1 iol. FIG. 2 shows an electron micrograph of a composite of O, 1iol. As shown in Figure 2(A), smectite with a plate-like morphology is also observed, but it is still difficult to see in Figure 2(B).
) As shown in Fig. 2, fine particles of colloidal silica are also observed in some parts, so it has not completely changed to smectite.
実施例２
０、ｌ■ｏｌのエチルシリケイトと ０．０２園０１の
アルミニウムブトキシドの混合溶液をｐＨ４に調整し、
３００ＣＣのメスフラスコに入れ、オイルバス中で８０
℃、１２時間保持した後、冷却した。この時溶液は、実
施例１と同様にわずかに半透明を示しており、微粒のコ
ロイダルシリカが生成していた。この溶液に０．１１■
０１の塩化マグネシウムと０．１ｉｏｌの尿素を添加し
た。再度オイルバス中で８０℃に６日間保持した後、冷
却し、遠心分離して、生成物の同定をＸ線粉末回折装置
、並びに透過型電子顕微鏡にて観察を行った。Ｘ線粉末
回折パターンを図３に示す。この図より板状形態を示す
スメクタイトが合成されている事がわかる。実施例１の
場合より、かなり結晶塵の良いことがわかる。図４に０
．１ｉｏｌの合成物の電子顕微鏡写真を示す。図４（Ａ
）、（Ｂ）に示すように板状の形態を示すスメクタイト
が多く認められ、はとんどコロイダルシリカの微粒子は
認められなかった。Example 2 A mixed solution of 0.1 mol of ethyl silicate and 0.02 mol of aluminum butoxide was adjusted to pH 4,
Place in a 300CC volumetric flask and heat in an oil bath for 80
℃ for 12 hours, and then cooled. At this time, the solution was slightly translucent as in Example 1, and fine particles of colloidal silica were produced. 0.11μ in this solution
01 of magnesium chloride and 0.1 iol of urea were added. After being kept at 80° C. for 6 days in an oil bath again, it was cooled, centrifuged, and the product was identified using an X-ray powder diffractometer and a transmission electron microscope. The X-ray powder diffraction pattern is shown in FIG. This figure shows that smectite with a plate-like morphology is synthesized. It can be seen that the crystal dust is considerably better than in Example 1. 0 in Figure 4
．． An electron micrograph of 1 iol of the compound is shown. Figure 4 (A
), (B), many smectites with a plate-like morphology were observed, and almost no colloidal silica particles were observed.
（発明の効果）
以上述べてきたごとく、本発明方法は、初期に超微粒の
負の電荷を有するコロイダルシリカを生成させ、マグネ
シウム塩とアルミニウム塩、或はアルミニウムアルコキ
シドとを混合後、さらに尿素を添加し加温することによ
り、正の電荷を有するマグネシウム水酸化物のコロイド
粒子を生成させ、両コロイド粒子を均一にヘテロ凝集さ
せながら結晶成長させる新規な合成方法であるため、新
しい多（の用途に利用できるものである。(Effects of the Invention) As described above, in the method of the present invention, ultrafine particles of negatively charged colloidal silica are initially produced, and after mixing magnesium salt and aluminum salt or aluminum alkoxide, urea is further added. This is a novel synthesis method that generates positively charged colloidal particles of magnesium hydroxide by adding and heating the colloidal particles, and grows crystals while uniformly heteroagglomerating both colloidal particles. It can be used for
第１図（Ａ）、 （Ｂ）は、実施例１の製造方法で合成
されたスメクタイトのＸ線粉末回折パターンである。２
θで２０° と３５゛近傍に非対称なピークプロファイ
ルが認められるが、これらのピークは単純な非晶質のプ
ロファイルとは異なりスメクタイトの生成していること
を示している。第２図はスメクタイトの形状を示す透過
型電子顕微鏡の写真である。第２図（Ａ）は微粒ではあ
るが、板状の形態を示すスメクタイトが合成されている
ことを示している。第２図（Ｂ）は合成物の中に、まだ
未反応のコロイダルシリカが残存していることを示して
いる。第３図は実施例２の方法で合成されたスメクタイ
トのＸ線粉末回折パターンを示している。実施例１の場
合より、２θで５゛近傍に（００１）反射の認められる
ことより、かなり結晶底の良いスメクタイトであること
を示している。第４図（＾）、（Ｂ）はスメクタイトの
形状を示す透過型電子顕微鏡の写真を示す。０．１μｍ
から０．５μｍの大きさを有する結晶底の良い薄板状の
スメクタイトである。
第
図
（ハラ
（Ｂ〕
２１１（Ｃｕにα）
２１１（Ｃｕにα）FIGS. 1(A) and 1(B) are X-ray powder diffraction patterns of smectite synthesized by the manufacturing method of Example 1. 2
Asymmetrical peak profiles are observed near 20° and 35°, but these peaks differ from simple amorphous profiles and indicate the formation of smectite. FIG. 2 is a transmission electron microscope photograph showing the shape of smectite. FIG. 2(A) shows that smectite having a plate-like form is synthesized, although it is fine particles. FIG. 2(B) shows that unreacted colloidal silica still remains in the composite. FIG. 3 shows an X-ray powder diffraction pattern of smectite synthesized by the method of Example 2. Compared to the case of Example 1, the fact that (001) reflection was observed in the vicinity of 5° at 2θ indicates that it is a smectite with a fairly good crystal base. Figures 4 (^) and (B) show transmission electron microscope photographs showing the shape of smectite. 0.1μm
It is a thin plate-like smectite with a good crystal bottom and a size of 0.5 μm. Diagram (Hara (B)) 211 (α to Cu) 211 (α to Cu)
Claims (1)
ｏｌの水溶液をｐＨ２からｐＨ５の間に調整し、７０℃
から９０℃に加温後、微粒コロイダルシリカを生成させ
、冷却後、０．０１ｍｏｌから０．５ｍｏｌのマグネシ
ウム塩、０．０５ｍｏｌから０．５ｍｏｌの尿素を混合
し、再度７０℃から９０℃に加温後、２日から７日間同
温度に保持することを特徴とするスメクタイトの製造方
法。 ２、同上の方法に、さらにアルミニウム塩、或いはアル
ミニウムアルコキシドを添加して合成することを特徴と
するスメクタイトの製造方法。[Claims] 1. 0.01 mol to 0.5 m of silica alkoxide
An aqueous solution of ol was adjusted to between pH 2 and pH 5 and heated to 70°C.
After heating from 70°C to 90°C, fine colloidal silica was generated, and after cooling, 0.01 mol to 0.5 mol of magnesium salt and 0.05 mol to 0.5 mol of urea were mixed, and the mixture was heated again from 70°C to 90°C. A method for producing smectite, which comprises heating and then maintaining the same temperature for 2 to 7 days. 2. A method for producing smectite, which is characterized in that it is synthesized by adding an aluminum salt or an aluminum alkoxide to the same method as above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1295221A JPH0613404B2 (en) | 1989-11-13 | 1989-11-13 | Method for producing smectite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1295221A JPH0613404B2 (en) | 1989-11-13 | 1989-11-13 | Method for producing smectite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03153519A true JPH03153519A (en) | 1991-07-01 |
| JPH0613404B2 JPH0613404B2 (en) | 1994-02-23 |
Family
ID=17817775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1295221A Expired - Lifetime JPH0613404B2 (en) | 1989-11-13 | 1989-11-13 | Method for producing smectite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0613404B2 (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996007613A1 (en) * | 1994-09-02 | 1996-03-14 | Akzo Nobel N.V. | Synthetic swelling clay minerals |
| JP2003517988A (en) * | 1999-12-22 | 2003-06-03 | アクゾ ノーベル ナムローゼ フェンノートシャップ | Method for producing synthetic clay minerals |
| KR100598160B1 (en) * | 2004-09-09 | 2006-07-10 | 한국지질자원연구원 | Synthesis of beidellite from agalatomitedickite |
| JP2008087971A (en) * | 2006-09-06 | 2008-04-17 | National Institute For Materials Science | Manufacturing method of synthetic layered silicate containing metal ion |
| JP2009107907A (en) * | 2007-10-31 | 2009-05-21 | Hitachi Chem Co Ltd | Synthetic smectite and dispersion liquid containing this, clay film, waterproof film, and method of producing synthetic smectite and waterproof film |
| JP2011057486A (en) * | 2009-09-08 | 2011-03-24 | Hitachi Chem Co Ltd | Synthetic smectite, method for manufacturing the same, and composite film |
| JP2014024711A (en) * | 2012-07-26 | 2014-02-06 | Shinshu Univ | Smectite-coated silica particles and method for manufacturing the same |
| KR200481474Y1 (en) * | 2015-12-02 | 2016-10-05 | 정은화 | Pants with outer clothes |
-
1989
- 1989-11-13 JP JP1295221A patent/JPH0613404B2/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996007613A1 (en) * | 1994-09-02 | 1996-03-14 | Akzo Nobel N.V. | Synthetic swelling clay minerals |
| NL9401433A (en) * | 1994-09-02 | 1996-04-01 | Univ Utrecht | Synthetic swellable clay minerals. |
| AU718224B2 (en) * | 1994-09-02 | 2000-04-13 | Albemarle Netherlands B.V. | Synthetic swelling clay minerals |
| JP2003517988A (en) * | 1999-12-22 | 2003-06-03 | アクゾ ノーベル ナムローゼ フェンノートシャップ | Method for producing synthetic clay minerals |
| KR100598160B1 (en) * | 2004-09-09 | 2006-07-10 | 한국지질자원연구원 | Synthesis of beidellite from agalatomitedickite |
| JP2008087971A (en) * | 2006-09-06 | 2008-04-17 | National Institute For Materials Science | Manufacturing method of synthetic layered silicate containing metal ion |
| JP2009107907A (en) * | 2007-10-31 | 2009-05-21 | Hitachi Chem Co Ltd | Synthetic smectite and dispersion liquid containing this, clay film, waterproof film, and method of producing synthetic smectite and waterproof film |
| JP2011057486A (en) * | 2009-09-08 | 2011-03-24 | Hitachi Chem Co Ltd | Synthetic smectite, method for manufacturing the same, and composite film |
| JP2014024711A (en) * | 2012-07-26 | 2014-02-06 | Shinshu Univ | Smectite-coated silica particles and method for manufacturing the same |
| KR200481474Y1 (en) * | 2015-12-02 | 2016-10-05 | 정은화 | Pants with outer clothes |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0613404B2 (en) | 1994-02-23 |
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