JPH0196027A - Production of glass - Google Patents

Abstract

PURPOSE:To improve yield in a transferring process and to drastically rationalize man-hour by drying wet gel on the partition plate of a vertically-type charging vessel and producing glass by a sol-gel method while using metal alkoxide as a raw material. CONSTITUTION:In production of glass by a sol-gel method in which metal alkoxide is used as a starting raw material, wet gel is dried on the partition plate of a vertical-type charging vessel. In this production of glass, wet gel is dried on the partition plate without transferring it and thereby as preparation of drying, wet gel is drawn out from the vertical-type charging vessel at every partition plates and only set in a drying vessel. Further more, since wet gel is always protected with the partition plates, a crack due to carelessness at the time of transferring, can be drastically reduced.

Description

[Detailed description of the invention] [Industrial application field] The present invention relates to a method for manufacturing glass.

[Summary of the invention]

In the production of glass by the sol-gel method using a metal alkoxide as a starting material, the present invention is directed to a wet gel made by charging II (as shown in FIG. 2) into a container.
On the partition plate of the vertical preparation container as shown in Figure 3,
This is a method of manufacturing glass that involves drying it in the shape shown in the figure. For drying in the conventional vertical feeding method, the wet gel made by pouring the sol into a vertical feeding container cannot be dried as it is, so it is pulled out from the vertical feeding container, transferred to a polypropylene or Teflon container, and dried. was.

However, with this method, the extremely fragile wet gel had to be transferred to a drying container, requiring great care. Therefore, it took a lot of man-hours, and the yield at the time of transfer was also poor. Therefore, in the present invention, it was decided to dry on the partition plate without transferring. As a result, preparation for drying can be accomplished by simply pulling out the wet gel along with the partition plate from the vertical container and setting it in the drying container. In addition, since the wet gel is always protected by the temporary partition, it is possible to significantly reduce the chance of cracking due to carelessness during transfer.

[Conventional technology]

For drying in the conventional vertical filtration method, the wet gel made by filling the sol in a vertical filtration container cannot be dried as it is, so it is pulled out from the vertical filtration container and the wet gel is transferred alone to a container made of polypropylene or Teflon. It was changed and dried. However, with this method, the extremely fragile wet gel had to be transferred to a drying container, requiring great care. Therefore, it took a lot of man-hours, and the yield at the time of transfer was also poor.

[Problem that the invention seeks to solve]

However, in the above-mentioned prior art, the very fragile wet gel had to be transferred to a drying container, which required great care. Therefore, it takes a lot of man-hours, and
There is also a problem in that the transfer yield is poor. Therefore, in the present invention, by using a method of drying on a partition plate without transferring the gel, preparation for drying is as simple as pulling out the wet gel with the partition from the vertical container and setting it in the drying container. It's getting better. In addition, since the wet gel is always protected by the partition plate, it is possible to significantly reduce the chance of cracking due to carelessness during transfer. Therefore, the purpose is to improve the yield and significantly streamline the man-hours in the transfer process.

[Means for solving problems]

The method for producing glass of the present invention includes producing glass by a sol-gel method using a metal alkoxide as a starting material.
It is characterized by drying the wet gel prepared by charging it into a vertical storage container on the partition plate of the vertical storage container.

[Effect]

According to the above-mentioned configuration of the present invention, it is possible to improve the yield in the transfer process and to significantly rationalize the number of man-hours.

〔Example〕

Example 1 Tetraethoxysilane 17.91 and O,Of normal hydrochloric acid aqueous solution 23.51 and silica fine particles (Aerosil 0X-
50 (manufactured by Degussa, West Germany) were mixed and vigorously stirred for 1 hour to obtain a hydrolyzed solution. The obtained sol was irradiated with ultrasonic waves (26 kHz, 1200 W) for 4 hours to crush and disperse coarse particles. The sol obtained by ultrasonic irradiation was then loaded onto a centrifuge Km, and centrifugal force was applied at 1500 G for 15 minutes to remove remaining coarse particles and foreign matter. Next, the obtained sol' is 10μms 7μm% 3μm%
After passing through a 1 μm pre-filter, it was passed through a Membrane 5 μm filter.

The pH value of the obtained homogeneous sol was raised from 2.2 to 4.0 using 0.01N aqueous ammonia. Furthermore, the obtained sol was taken into the centrifuge again and 1500G was
After applying the voltage for 5 minutes, the mixture was passed through a Membrane 5 μm filter again and charged into the vertical container shown in FIG. This vertical container is made to be able to obtain 12 sheets of wet gel measuring 25 cm x 25 cm x 1.80 cm.

When the container was left sealed for one day and night, the sol gelatinized and a wet gel was obtained. The obtained wet gel was placed in a drying container in the form shown in FIG. There were no cracks in the 12 wet gels during transfer. Also, the time required to transfer 12 sheets was 4 minutes.

It was replaced with a lid with holes having an open area ratio of 0.3%, placed in a dryer, and dried at 60° C. for one week to obtain a dry gel. The drying yield at this time was 100% with no cracks among the 12 sheets.

The obtained dry gel was further dried at 200° C. to completely remove remaining water. Put this in an atmospheric furnace and Dr.
Sintering was performed at 1000°C in a y-Air atmosphere. Next, it was placed in a vacuum furnace and sintered at 1400° C. in a vacuum to obtain quartz glass.

Comparative Example 1 Twelve sheets of wet gel prepared in the same manner as in Example 1 were transferred to a dry container in the state shown in FIG. 4. 1
Three out of two sheets were broken, and the transfer yield at this time was 7.
It was 5%. Further, the time required for transfer was 11 minutes. It was replaced with a lid with holes with an opening ratio of 0.3%, placed in a dryer, and dried at 60°C for one week to obtain a dry gel.

The obtained dried gel was sintered under the same conditions as in Example 1 to obtain quartz glass.

Example 2 Eta/-Lua, 200 mb 2,000 ml of water and 240 ml of aqueous ammonia were stirred to form a homogeneous system, and 74,980 ml of tetraethoxysila was added with stirring. When the mixture was slowly stirred and left for 3 hours, fine silica particles were generated.

The resulting silica dispersion was concentrated to a concentration of 31 using a rotary evaporator. This is called liquid A. This operation was repeated 5 times to obtain 151 liquid A.

Next, 11,280ml of tetraethoxysilane and 0.0
3,200 ml of 2N hydrochloric acid was mixed and stirred vigorously for 1 hour to obtain a hydrolyzed solution of tetraethoxysilane. This is B
Make it into a liquid.

The AfiQPH value was adjusted to 4.5 using 2N hydrochloric acid, mixed with Solution B, and thoroughly stirred. 40μ of the obtained sol
The mixture was passed through a filter with a diameter of 15 μm and charged into a vertical container shown in FIG. This vertical preparation container is 30cmX
30CIX 12 wet gels of 1.6cm size
It is designed so that you can get one.

When the container was left sealed for one day and night, the sol gelatinized and a wet gel was obtained. The obtained wet gel was placed in a drying container in the form shown in FIG. There were no cracks in the 12 wet gels during transfer. Also, the time required to transfer 12 sheets was 5 minutes.

It was replaced with a lid with holes with an opening ratio of 0.3%, placed in a dryer, and dried at 60°C for one week to obtain a dry gel. At this time, the drying yield was 100% with no cracks among the 12 sheets.

The resulting dry gel was further dried at 200°C to completely remove remaining water. This was further dried at 400°C to remove remaining ammonia chloride. Next, it was placed in an atmospheric furnace and heated for 80 minutes in a Dry-Air atmosphere.
Sintered at 0°C. Next, put it in a vacuum furnace and vacuum it for 18 hours.
When sintered at 00°C, quartz glass was obtained.

Comparative Example 2 Twelve sheets of wet gel prepared in the same manner as in Example 2 were transferred to a dry container in the state shown in FIG. 4. 1
5 out of 2 sheets were broken, and the transfer yield at this time was 4.
It was 1.7%. Also, the time required for transfer was 18
It was a minute. Instead of a lid with holes with an opening ratio of 0.3%,
The gel was placed in a dryer and dried at 60° C. for one week to obtain a dry gel.

The obtained dried gel was sintered under the same conditions as in Example 2 to obtain quartz glass.

〔Effect of the invention〕

As described above, the present invention significantly improves the transfer yield and rationalizes the transfer man-hours by drying on the partition plate of the vertical preparation container in the IA type live-in.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing the drying state on the partition plate. 120...Vent hole 121...Wet gel 122... Polypropylene drying container 123... Lid 124...Partition plate FIG. 2 is a diagram showing an outline of a vertical preparation container. 11... Vertical preparation container 12...Partition plate 13...Wet gel FIG. 3 is a diagram showing an outline of the partition plate. 101... Pull-out hole 102...Partition plate 103...Spacer FIG. 4 is a diagram showing a normal dry state. 130...Vent hole 131...lid 133...Wet gel 134...Polypropylene drying container and above Applicant: Seiko Epson Corporation

Claims (1)

[Claims] A method for producing glass, which comprises drying a wet gel produced by filling a vertical charging container on a partition plate of the vertical charging container, in the manufacturing of glass by the sol-gel method using metal alkoxide as a starting material. .