JPS6296327A - Method of preparing sol - Google Patents
Method of preparing solInfo
- Publication number
- JPS6296327A JPS6296327A JP23556385A JP23556385A JPS6296327A JP S6296327 A JPS6296327 A JP S6296327A JP 23556385 A JP23556385 A JP 23556385A JP 23556385 A JP23556385 A JP 23556385A JP S6296327 A JPS6296327 A JP S6296327A
- Authority
- JP
- Japan
- Prior art keywords
- sol
- water
- silica
- stirring
- alkyl silicate
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、ゾル−ゲル法におけるゾルの調整方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for preparing a sol in a sol-gel method.
本発明は、ゾル−ゲル法におけるゾル調整において、微
粉末シリカを前もって水に分散させた後アルキルシリケ
ートを加え加水分解することにより、ゾルの粒度を落と
すに要する超音波照射の時間を短くシ、ゾル調整に要す
る時間を短縮したものである。In the sol preparation in the sol-gel method, the present invention shortens the ultrasonic irradiation time required to reduce the particle size of the sol by first dispersing finely powdered silica in water and then adding alkyl silicate for hydrolysis. This shortens the time required for sol adjustment.
アルキルシリケートおよび微粉末シリカを主原料として
用いるゾル−ゲル法による石英ガラス製造方法は、高品
質なガラスを安価に製造できるため、非常に注目されて
いる。A method for producing silica glass using a sol-gel method using alkyl silicate and finely powdered silica as main raw materials has attracted much attention because it can produce high-quality glass at low cost.
従来のゾル−ゲル法によるゾルの調整方法は、アルキル
シリケート、微粉末シリカ及び水を同時に混合し、攪拌
、超音波照射を行いながら加水分解を行い、加水分解終
了後もゾルの粒度がある一定の値に下がるまで攪拌及び
超音波照射’ｔａけた。The conventional method for preparing a sol using the sol-gel method is to simultaneously mix alkyl silicate, finely powdered silica, and water, and hydrolyze the mixture while stirring and irradiating it with ultrasonic waves. Stirring and ultrasound irradiation were continued until the value decreased to .
〔発明が解決しようとする問題点及び目的〕しかし、従
来のフルキルシリケート、微粉末シリカ及び水を同時に
混合して加水分解を行うという方法においては、次のよ
うな理由により、ゾルの粒度１！−落とすための攪拌、
超音波照射に要する時間が長くかかる。アルキルシリケ
ート及び水の溶液中に微粉末として混合された５１０７
粒子は、溶液に浸されると、溶液に８１０２粒子がなじ
む前に凝集してしまう。また、溶液にアルキルシリケー
トが含まれているために、アルキルシリケートの粘性に
より、ｓｌｏ、粒子が溶液中に分散されに＜＜１８１０
１粒子のかたまりも大きなものとなりやすい。また、８
１０．粒子が充分に分散される以前にアルキルシリケー
トの加水分解が行われ、加水分解によって生じた８ｌ−
ＯＨ分子は縮合全行い５１０１分子になる。この８１０
．分子線、最初から微粉末として加えられた８１０１粒
子を核にして成長していく。この時点で、超音波照射に
よる分散の効果は、Ｓｉｎ、粒子の成長によシうち消さ
れた状態になり、超音波照射のききめはあまシ見られ−
ない。その結果攪拌、超音波照射に要する時間が長くな
る。[Problems and objects to be solved by the invention] However, in the conventional method of simultaneously mixing furkyl silicate, finely powdered silica, and water for hydrolysis, the particle size of the sol ! - stirring to remove;
Ultrasonic irradiation takes a long time. 5107 mixed as a fine powder in a solution of alkyl silicate and water
When the particles are immersed in the solution, they aggregate before the 8102 particles are absorbed into the solution. In addition, since the solution contains alkyl silicate, the viscosity of the alkyl silicate prevents particles from being dispersed in the solution.
Even a single particle tends to become large. Also, 8
10. Hydrolysis of the alkyl silicate takes place before the particles are sufficiently dispersed, and the 8l-
The total condensation of OH molecules results in 5101 molecules. This 810
．． Molecular beams grow using 8101 particles, which were added as fine powder from the beginning, as cores. At this point, the dispersion effect caused by ultrasonic irradiation is canceled out by the growth of Sin and particles, and the fineness of ultrasonic irradiation is not observed.
do not have. As a result, the time required for stirring and ultrasonic irradiation becomes longer.
また、Ｓｉｎ、粒子が分散されにくい点から、最終的に
８１０．が分散されず°粘径が完全に浩ちない場合が生
じてくる。その結果、アルキルシリケート、微粉末シリ
カ等の原料の無駄が生じる。In addition, since the particles of Sin are difficult to disperse, the final value is 810. There may be cases where the viscosity is not completely increased because the viscosity is not dispersed. As a result, raw materials such as alkyl silicate and finely powdered silica are wasted.
本発明は、このよりな問題点を解決するもので、その目
的とするところは、常に同じ状態のゾルを量産性良く得
るところにある。The present invention is intended to solve this further problem, and its purpose is to obtain a sol that is always in the same state with good mass production.
本発明のゾル調整方法は、微粉末シリカを前もって必要
量の水に分散させた後、アルキルシリケートを加え加水
分解をすることを特徴とする。The sol preparation method of the present invention is characterized in that finely powdered silica is previously dispersed in a required amount of water, and then an alkyl silicate is added and hydrolyzed.
ゾルの調整において、アルキルシリケート、微粉末シリ
カ及び水を同時に混合し、攪拌、超音波照射を行いなが
ら加水分解をして、その後も攪拌超音波照射を続けてゾ
ルを得る方法においては、微粒子である５１０３粒子は
ｓ Ｉ＠ｙに浸されると凝集しやすく、ましてアルキル
シリケートにより粘度が高まって分散されにくくなる。When preparing a sol, alkyl silicate, finely powdered silica, and water are mixed simultaneously, hydrolyzed while stirring and irradiated with ultrasonic waves, and then stirring and irradiation with ultrasonic waves are continued to obtain a sol. Certain 5103 particles tend to aggregate when immersed in s I@y, and moreover, the alkyl silicate increases the viscosity and makes it difficult to disperse.
その結果。the result.
５１０８粒子の分散に要する時間は長く要求され、時に
は分散されずに終わってしまう場合も生じ兼ねない。It takes a long time to disperse the 5108 particles, and sometimes the particles may not be dispersed.
本発明では、このような問題を避けるために、あらかじ
めＳｉｎ、粒子を必要量の水に分散させておく。日１０
１粒子は、水に浸されると最初は従来の方法と同様凝集
し、粒径は大きくなる。しかし８１０、粒子は水になじ
みやすく、また水の粘性がそれほど嵩くないために、攪
拌、超音波照射により分散が容易に行なわれる。こうし
て得られた分散液とアルキルシリケートヲ混合し、塩＃
１を触媒に加水分解を行いゾルを得る。加水分解が行な
われる前、Ｓｉｎ、粒子の粒径は分散液におけるＳｉｎ
。In the present invention, in order to avoid such problems, Sin and particles are dispersed in a necessary amount of water in advance. day 10
When one particle is immersed in water, it initially aggregates as in the conventional method, and the particle size increases. However, since the particles 810 are easily compatible with water and the viscosity of water is not so bulky, dispersion is easily performed by stirring and ultrasonic irradiation. The thus obtained dispersion and alkyl silicate were mixed, and salt #
1 is hydrolyzed using a catalyst to obtain a sol. Before hydrolysis, the particle size of the particles is the same as the Sin in the dispersion.
.
粒子の粒径であり、加水分解が行われ、 Ｓｉｎ、分子
の縮合が起こっても、本来の８１０．粒子の粒径が小さ
いために、全体の粒径もそれほど大きくならず１短時間
の攪拌、超音波照射によシ、望みの粒径のゾルが得られ
る。また、分散液の時点での粒径にゾルの粒径が必ず落
ちる保証があるため、分散液の段階で望みの粒径にまで
分散させれば容易にゾルが得られる。゛また、万が一１
分散液の段階で粒径が落ちず、望みの分散液が得られな
かったとしても、その損失は最小限に押さえることが可
能となる。Even if hydrolysis occurs and condensation of Sin and molecules occurs, the original 810. Since the particle size of the particles is small, the overall particle size does not become too large, and a sol with a desired particle size can be obtained by stirring for a short time and irradiating with ultrasonic waves. Furthermore, since there is a guarantee that the particle size of the sol will always fall to the particle size at the time of dispersion, a sol can be easily obtained by dispersing to the desired particle size at the stage of dispersion.゛Also, just in case
Even if the desired dispersion cannot be obtained because the particle size does not decrease at the dispersion stage, the loss can be kept to a minimum.
微粉末シリカ２５１ｆと水５６９ ｔ、さらに布板のエ
チルシリケー） （５ｉ（００，Ｈ，）、 ８００＋ｄ
、１５Ｎの塩Ｈｓａｃｃを用い、次の二連シの方法で平
均粒径（Ｌ１５μｍのゾルを得た。251f of finely powdered silica, 569t of water, and ethyl silica on a cloth plate) (5i(00,H,), 800+d
, 15N salt Hsacc was used to obtain a sol with an average particle size (L of 15 μm) using the following two-part method.
（１）微粉末シリカ２３１２を水５６９ｆに流し込み、
攪拌、超音波照射′ｔ−続けて平均粒径Ｑ、１５μｍの
分散［−得た。これにエチルシリケート（ｓｌ（００，
）Ｉ、 ）、 ） ８００−と（ＬＯ５Ｎ壇ｆｆｉ、５
０ｃｃｆ加え、加水分Ｍ’ｔ−行い、加水分解後、攪拌
、超音波照射を繰り返し行い平均粒径α１５μｍのゾル
を得た。(1) Pour fine powder silica 2312 into water 569f,
Stirring and ultrasonic irradiation were followed to obtain a dispersion with an average particle size Q of 15 μm. To this, ethyl silicate (sl(00,
)I, ), ) 800- and (LO5Ndanffi, 5
0 ccf was added, hydrolysis M't- was carried out, and after hydrolysis, stirring and ultrasonic irradiation were repeated to obtain a sol with an average particle size α of 15 μm.
（２１微粉末シリカ２５１？と水５６９２、さらにエチ
ルシリケート（ｓｌ（ｏｃ、 Ｈ，）４ ） ８００ｄ
ｔ”同時に混合し、これに００５Ｎ塩酸３ｏｃｃ″ｆ！
：加え、攪拌、超音波照射を行いながら加水分解を行い
、加水分解後も攪拌、超音波照射を行い、平均粒径α１
５μｍのゾルを得た。(21 fine powder silica 251? and water 5692, further ethyl silicate (sl(oc, H,)4) 800d
t" Mix at the same time, add 3 occ of 005N hydrochloric acid"f!
: Addition, hydrolysis while stirring and ultrasonic irradiation, stirring and ultrasonic irradiation after hydrolysis, average particle size α1
A 5 μm sol was obtained.
（１）の方法においては、微粉末シリカと水の混合５分
、分散液の超音波照射５０分、エチルシリケート添加３
分、加水分解４０分、加水分解後の攪拌、超音波照射６
０分を要した。この手順の間の８１０！粒子の粒径は、
第１図に示すような変化を示し、全工程１５８分で望み
の粒径１１５μｍのゾルを得た。In method (1), fine powder silica and water were mixed for 5 minutes, the dispersion was irradiated with ultrasonic waves for 50 minutes, and ethyl silicate was added for 3 minutes.
minutes, hydrolysis 40 minutes, stirring after hydrolysis, ultrasonic irradiation 6
It took 0 minutes. 810 during this procedure! The particle size of the particles is
The changes were as shown in FIG. 1, and a sol with the desired particle size of 115 μm was obtained in a total process of 158 minutes.
（２１０方法においては、微粉末シリカと水、エチルシ
リケートの混合８分、加水分解４０分、加水分解後の攪
拌、超音波照射２１０分を要した。またこの間の８１０
１粒子の粒径は、第２図に示すような変化を示し、全工
程２５８分で望みの粒径Ｑ、１５μｍのゾルを得た。(The 210 method required 8 minutes of mixing fine powder silica, water, and ethyl silicate, 40 minutes of hydrolysis, stirring after hydrolysis, and 210 minutes of ultrasonic irradiation.
The particle size of each particle showed a change as shown in FIG. 2, and a sol with a desired particle size Q of 15 μm was obtained in the entire process of 258 minutes.
以上述べたように、本発明によるゾル調整の手順にてゾ
ルの調整を行うことによｐ、Ｓ１ａ、粒子が水に分散さ
れやすく、目的の粒径の分散ｇｔ容易に得ることができ
、また、そのため加水分解後の粒径も大きくならず短時
間の攪拌、超音波照射により容易に目的のゾルが得られ
る。したがって、この方法によシ均質のゾルがｉｋ産性
良く得ることが可能となる。またこのような均質なゾル
により得られるガラスも均質なガラスとなり、ゾル−ゲ
ル法によるガラス型造の均質化、１を産性を改善したも
のと言える。こうしてできたガラスは、一般的に広く匣
われているガラス器具はもちろんのこと、高純度、高精
度を必要とする光フアイバー用ジャケット管としても応
用できる。As described above, by adjusting the sol using the sol preparation procedure according to the present invention, particles p, S1a, and particles can be easily dispersed in water, and a dispersion gt of the desired particle size can be easily obtained. Therefore, the particle size after hydrolysis does not increase, and the desired sol can be easily obtained by short-time stirring and ultrasonic irradiation. Therefore, this method makes it possible to obtain a homogeneous sol with good yield. Moreover, the glass obtained by such a homogeneous sol also becomes a homogeneous glass, and it can be said that the glass mold formation by the sol-gel method is homogenized and the productivity is improved. The glass made in this way can be used not only in commonly used glass appliances, but also as jacket tubes for optical fibers, which require high purity and precision.
第１図に実施例に述べた（１１の方法（本発明の方法）
にてゾル調整を行った時の粒度の経時変化図を示す、第
２図に実施例のは）の方法（従来の方法）にてゾル調整
を行った時の粒度の経時変化図を示す。
以上FIG. 1 shows 11 methods (methods of the present invention) described in the Examples.
FIG. 2 shows a graph of the change in particle size over time when the sol was adjusted using the method of Example 1 (conventional method). that's all
Claims (1)
いるゾル−ゲル法におけるゾル調整において、微粉末シ
リカを前もつて水に分散させた後アルキルシリケートを
加え加水分解することを特徴とするゾルの調整方法。A method for preparing a sol in a sol-gel method using an alkyl silicate and finely powdered silica as main raw materials, which comprises dispersing finely powdered silica in water in advance, then adding an alkylsilicate and hydrolyzing it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23556385A JPS6296327A (en) | 1985-10-22 | 1985-10-22 | Method of preparing sol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23556385A JPS6296327A (en) | 1985-10-22 | 1985-10-22 | Method of preparing sol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6296327A true JPS6296327A (en) | 1987-05-02 |
Family
ID=16987841
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23556385A Pending JPS6296327A (en) | 1985-10-22 | 1985-10-22 | Method of preparing sol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6296327A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990007390A1 (en) * | 1988-12-27 | 1990-07-12 | Symetrix Corporation | Methods and apparatus for material deposition |
| US5138520A (en) * | 1988-12-27 | 1992-08-11 | Symetrix Corporation | Methods and apparatus for material deposition |
| US5614252A (en) * | 1988-12-27 | 1997-03-25 | Symetrix Corporation | Method of fabricating barium strontium titanate |
| US5962085A (en) * | 1991-02-25 | 1999-10-05 | Symetrix Corporation | Misted precursor deposition apparatus and method with improved mist and mist flow |
| US7059153B2 (en) | 2000-06-05 | 2006-06-13 | Murata Manufacturing Co., Ltd. | Method for producing glass powders |
| JP2011527278A (en) * | 2008-07-09 | 2011-10-27 | エボニック デグサ ゲーエムベーハー | Unsintered compact based on silicon |
-
1985
- 1985-10-22 JP JP23556385A patent/JPS6296327A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990007390A1 (en) * | 1988-12-27 | 1990-07-12 | Symetrix Corporation | Methods and apparatus for material deposition |
| US5138520A (en) * | 1988-12-27 | 1992-08-11 | Symetrix Corporation | Methods and apparatus for material deposition |
| US5614252A (en) * | 1988-12-27 | 1997-03-25 | Symetrix Corporation | Method of fabricating barium strontium titanate |
| US5962085A (en) * | 1991-02-25 | 1999-10-05 | Symetrix Corporation | Misted precursor deposition apparatus and method with improved mist and mist flow |
| US7059153B2 (en) | 2000-06-05 | 2006-06-13 | Murata Manufacturing Co., Ltd. | Method for producing glass powders |
| JP2011527278A (en) * | 2008-07-09 | 2011-10-27 | エボニック デグサ ゲーエムベーハー | Unsintered compact based on silicon |
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