JPS58239A - Production of gelatinous porous body - Google Patents
Production of gelatinous porous bodyInfo
- Publication number
- JPS58239A JPS58239A JP9669681A JP9669681A JPS58239A JP S58239 A JPS58239 A JP S58239A JP 9669681 A JP9669681 A JP 9669681A JP 9669681 A JP9669681 A JP 9669681A JP S58239 A JPS58239 A JP S58239A
- Authority
- JP
- Japan
- Prior art keywords
- gel
- raw material
- vessel
- soln
- container
- 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
Links
- 238000004519 manufacturing process Methods 0.000 title description 4
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 9
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000013307 optical fiber Substances 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 30
- 239000011240 wet gel Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/016—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by a liquid phase reaction process, e.g. through a gel phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Glass Compositions (AREA)
- Colloid Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、柱状多孔質体、臀に柱状シリカ物体の製造方
法に関し、さらに特に多孔質シリカゲルの製造方法に関
する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a columnar porous body, a columnar silica body, and more particularly to a method for producing a porous silica gel.
金属アルコキシド（例えば８ｇ（ＯＣＨｓｈ）を加水分
解して得らｎるゲル状物体を乾燥、焼結し、無孔のブロ
ック体（例えばシリカガラスロンド）を作成する方法（
以下ゾル、ゲル法と呼ぶ）が提案さｔている。A method of drying and sintering a gel-like substance obtained by hydrolyzing a metal alkoxide (e.g. 8 g (OCHsh)) to create a non-porous block body (e.g. silica glass iron) (
A method (hereinafter referred to as sol or gel method) has been proposed.
ゾル、ゲル法のプロセスの概要を述べると、例えば、Ｓ
’ （ＯＣＲＩＩ）４ を原料とし、ＣＨ，ＯＨ，お
よび蒸留水を混合かくはんして原料溶液となし、こｎ全
所定形状の容器、九とえは第１図（ａ）に示した１うな
円筒状の容器１に充填し、ゲル化させる。このゲル２を
以下ウェットゲルと呼ぶ。つぎにこのウェットゲル２ｔ
−徐々に乾燥せしめるとゲルｒＸする程度収縮して第１
図（ｂ）に示すように円筒容器と相似形の円柱状多孔質
ゲル３を得る。以下このゲル３をドライゲルと呼ぶ。し
かるのち約１０００ｔｌ’以上で焼結ガラス化してガラ
ス体たとえばガラスロッド會得る。To give an overview of the sol/gel process, for example, S
' (OCRII) 4 is used as a raw material, and CH, OH, and distilled water are mixed and stirred to obtain a raw material solution. The mixture is filled into a shaped container 1 and allowed to gel. This gel 2 is hereinafter referred to as wet gel. Next, this wet gel 2t
- When gradually dried, it shrinks to the extent of gel rX and the first
As shown in Figure (b), a cylindrical porous gel 3 having a similar shape to the cylindrical container is obtained. Hereinafter, this gel 3 will be referred to as a dry gel. Thereafter, it is sintered and vitrified at about 1000 tl' or more to obtain a glass body, such as a glass rod.
このようにして得らｆＬタガラスに光学部品、光ファイ
バその他に用いらｎるが、焼結前のドライゲルは当然そ
の原料となるものであり、また、ドライゲルそのものも
透光性の吸着剤その他に用いらｎる。The fL tag glass obtained in this way is used for optical parts, optical fibers, etc., but the dry gel before sintering is naturally the raw material for it, and the dry gel itself can also be used as a translucent adsorbent or other material. Not used.
上記ゾル、ゲル法で得らｎるドライゲルは作成条件にも
依存するが、第１図（Ｃ）で示した工うに円柱状ゲルが
乾燥の過程で曲がる場合がある。この傾向に仕上リゲル
が直径に対して長いほど強く表わｎる。このように曲っ
たゲルに１その後の焼結原料に用いるにしても、筐た、
ゲルそのものとして利用するにしても不都合な場合が多
い。Although the dry gel obtained by the above-mentioned sol-gel method depends on the preparation conditions, the cylindrical gel shown in FIG. 1(C) may be bent during the drying process. This tendency becomes more pronounced as the finished rig is longer relative to its diameter. Even if the bent gel is used as a raw material for subsequent sintering,
Even if it is used as a gel itself, it is often inconvenient.
不発明の目的に上記ゾル、ゲル法の欠点である柱状多孔
質ゲルの曲がり全防止する方法を提供することＫある。It is an object of the invention to provide a method for completely preventing the bending of columnar porous gels, which is a drawback of the above-mentioned sol-gel methods.
本発明に工れば、上記ゾル、ゲル法において、円柱状ゲ
ル全作成する場合に円筒状の容器として、核答器の開口
端を筒状部工り大きい直径の容器を用い、原料溶液を直
径の大きくなった部分まで満たし、かつ、容器を笑質的
に鉛直に支持しながら乾燥させることにより、上記目的
が達成できる。According to the present invention, in the above-mentioned sol/gel method, when a cylindrical gel is entirely produced, a cylindrical container with a large diameter is used by cutting the open end of the nuclear reactor into a cylindrical part, and the raw material solution is poured into a cylindrical container. The above objective can be achieved by filling the container up to its increased diameter and drying while supporting the container vertically.
以下実施例にエリ詳細に説明する。This will be explained in detail in Examples below.
実施例
原料としてＳｉ（ＯＣＨｉ）４ｔ−ｔｓ２ｇ％ＣＨａ
ＯＨ’１１８０ｃｃ、お工びＩ）Ｈｔ−１０，６に調製
した希釈ア／モニ≠’４７２ｃｃｍえて混合し原料液と
し友。Si(OCHi)4t-ts2g%CHa as an example raw material
OH'1180cc, 1) Diluted a/moni prepared to Ht-10,6≠'472ccm and mix to make a raw material liquid.
ｎた。ついでウェットゲル６を容器中で鉛直に支持しな
がら、７０″Ｃで徐々に乾燥させたところ、第２図（ｂ
）で示す工うなドライゲル７が得らｎた。It was. Next, while supporting the wet gel 6 vertically in the container, it was gradually dried at 70"C, as shown in Fig. 2 (b).
) was obtained.
ドライゲル７の真直度に従来法に比較していちじるしく
改善さｒしていた。The straightness of Dry Gel 7 was significantly improved compared to the conventional method.
以上の実施例では開口部の内径Ｄ１ と円筒部の内径
り、の比ＤＩ ／Ｄｔを１．７に選んだか、この比にゲ
ルの乾燥に伴なう収縮率から求めることができる。すな
わち、ある製造条件に対してウェットゲルの外径をｄｌ
、ドライゲルの外径がｄ、であったとすｎば、同じ条件
で製造する限り％Ｄ１／Ｄ、比’ｔｄｔ ／ｄｔ比より
も大きくしておけばよい。In the above embodiment, the ratio DI/Dt between the inner diameter D1 of the opening and the inner diameter of the cylindrical portion was selected to be 1.7, or it can be determined from this ratio and the shrinkage rate as the gel dries. In other words, the outer diameter of the wet gel is dl for certain manufacturing conditions.
If the outer diameter of the dry gel is d, then the ratio %D1/D should be larger than the ratio 'tdt/dt as long as the dry gel is manufactured under the same conditions.
上記の実施例でに円柱状のゲル作製を目的としたもので
あるが、任意断面形状の柱状ゲルの製造に対しても同様
な容器音用いることができる。また、上記実施例では純
シリカヲ収分とするゲルを作成するものであるが、ガラ
スマ穴ホゲルの屈折率を調整するための金属アルコキシ
ドを添加した原料または任意の金属アルコキシドを原料
とじて使用することができる。Although the purpose of the above embodiment was to produce a cylindrical gel, a similar container sound can be used for producing a cylindrical gel having an arbitrary cross-sectional shape. In addition, in the above example, a gel is made from pure silica, but a raw material to which metal alkoxide is added to adjust the refractive index of the glass porcelain gel, or any metal alkoxide may be used as the raw material. I can do it.
また開口部の面積が大きい場合、乾燥過程で割ｎが生じ
やすくなるが、この種の割ｎを防止するためには、開口
部をしぼっておくか、または適当なキャップヶし、乾燥
速度を低めて適正にすればＬい。Also, if the area of the opening is large, cracks are likely to occur during the drying process, but in order to prevent this type of crack, it is necessary to close the opening, cap it appropriately, or slow down the drying speed. If you do it properly, it will be L.
第１図（ａ）、 （ｂＬ （ｃ）ｒｃ従来のゲル乾燥方
法を示す概略断面図、第２図（ａ）、（ｂ）は本発明の
一実施例におけるゲル乾燥工程金示す概略断面図である
。
１．１’ 、１“・・・ゲル作成容器、２・・・ウェッ
トゲル、３．４・・・ドライゲル、５．５’・・・ゲル
作成容器、６・・・ウェットゲル、７・・・ドライゲル
。
代理人 弁理士 薄田利
′ＪＩＪ１ 図
゛（α） ＜ｂノ
（Ｃ２り第 ２ 図
（Ｌ） （ｂ）
第１頁の続き
０発 明 者 佐藤信
国分寺市東恋ケ窪１丁目２８０番
地株式会社日立製作所中央研究
所内
０発 明 者 菅沼庸雄
国分寺市東恋ケ窪１丁目２８０番
地株式会社日立製作所中央研究
所内Figures 1 (a) and (c) rc are schematic cross-sectional views showing a conventional gel drying method, and Figures 2 (a) and (b) are schematic cross-sectional views showing a gel drying process in an embodiment of the present invention. 1.1', 1"... Gel preparation container, 2... Wet gel, 3.4... Dry gel, 5.5'... Gel preparation container, 6... Wet gel, 7... Dreigel. Agent Patent Attorney Toshi Usuda'JIJ1 Figure ゛(α) <bノ
(C2 Figure 2 (L) (b)
Continued from page 1 0 Author: Shinobu Sato Inside the Central Research Laboratory, Hitachi, Ltd., 1-280 Higashi-Koigakubo, Kokubunji City. 0 Author: Tsuneo Suganuma. Inside the Central Research Laboratory, Hitachi, Ltd., 1-280 Higashi-Koigakubo, Kokubunji City.
Claims (1)
容器中で加水分解して得らｎるゲルを乾燥せしめ、ゲル
状多孔質体を得る方法において、該容器がその開口部に
おいて筒状部よりも大きい幅の拡大部分を有し、該原料
液を該拡大部分まで充填し、かつ該容萎ヲ実質的に鉛直
に支持しつつ乾燥せしめることｔ−Ｗ徴とするゲル状多
孔質体の製造方法。1. In a method for obtaining a gel-like porous body by drying a gel obtained by hydrolyzing a raw material solution containing a metal alkoxide and water in a predetermined cylindrical container, the container has a cylindrical shape at its opening. A gel-like porous material having an enlarged portion having a width larger than the shaped portion, and having a t-W characteristic in which the raw material liquid is filled up to the enlarged portion and is dried while supporting the volume substantially vertically. How the body is manufactured.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9669681A JPS58239A (en) | 1981-06-24 | 1981-06-24 | Production of gelatinous porous body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9669681A JPS58239A (en) | 1981-06-24 | 1981-06-24 | Production of gelatinous porous body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS58239A true JPS58239A (en) | 1983-01-05 |
Family
ID=14171926
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9669681A Pending JPS58239A (en) | 1981-06-24 | 1981-06-24 | Production of gelatinous porous body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58239A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59145036A (en) * | 1983-02-09 | 1984-08-20 | Asahi Chem Ind Co Ltd | Hard hydrogel |
-
1981
- 1981-06-24 JP JP9669681A patent/JPS58239A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59145036A (en) * | 1983-02-09 | 1984-08-20 | Asahi Chem Ind Co Ltd | Hard hydrogel |
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