JP2820865B2 - Method for producing quartz glass foam - Google Patents
Method for producing quartz glass foamInfo
- Publication number
- JP2820865B2 JP2820865B2 JP16547293A JP16547293A JP2820865B2 JP 2820865 B2 JP2820865 B2 JP 2820865B2 JP 16547293 A JP16547293 A JP 16547293A JP 16547293 A JP16547293 A JP 16547293A JP 2820865 B2 JP2820865 B2 JP 2820865B2
- Authority
- JP
- Japan
- Prior art keywords
- silica
- powder
- quartz glass
- temperature
- surface area
- 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.)
- Expired - Fee Related
Links
Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【産業上の利用分野】本発明は、微細シリカ粉から石英
ガラス発泡体を製造する方法に関し、特に、取扱い困難
な微粉状シリカを原料として均質且つ発泡度のコントロ
−ルされた石英ガラス発泡体の効果的製造方法に関する
ものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a quartz glass foam from fine silica powder, and more particularly to a quartz glass foam having a uniform and controlled degree of foaming from finely divided silica which is difficult to handle. The present invention relates to an effective production method of
【０００２】[0002]
【従来の技術】合成石英ガラス発泡体の製造は、シリカ
ガラス粉体若しくはシリカガラス粉体の凝集体をアンモ
ニアガスを含む雰囲気中で加熱してシリカの表面にアン
モニア基を導入し、そのアンモニア化されたガラス粉体
又は凝集体を型に入れて、更に高い温度で加熱溶融さ
せ、粉体の融着とアンモニア基の分解，放出を同時に行
わせる発泡方法が一般に採用されている。この方法は、
例えば、ス−ト法で得られた多孔質シリカ母材（ス−ト
体）、あるいは微細な石英ガラス粉体をポリビニルアル
コ−ル等の樹脂で固めたような凝集体が一般に用いられ
る。2. Description of the Related Art In the production of a synthetic quartz glass foam, silica glass powder or an aggregate of silica glass powder is heated in an atmosphere containing ammonia gas to introduce ammonia groups onto the surface of silica, and the ammoniaation is carried out. A foaming method is generally employed in which the glass powder or the aggregate obtained is put into a mold, heated and melted at a higher temperature, and fusion of the powder and decomposition and release of the ammonia group are simultaneously performed. This method
For example, a porous silica base material (soot body) obtained by a soot method, or an aggregate obtained by hardening fine quartz glass powder with a resin such as polyvinyl alcohol is generally used.
【０００３】アンモニアを利用して均質なシリカガラス
の発泡体を得るには、シリカガラスに可及的均一にアン
モニアを結合させることが重要であり、そのためには、
シリカ粉体表面にアンモニアと化学的に結合すると思わ
れる反応基（一般にSiOH基と推定される）が多く存在す
ること、及びアンモニア化されるシリカ粉体が大きな表
面積を有する微細粉であることが望ましい。しかし、か
かる技術的概念にもかかわらず、処理される微細シリカ
粉の取扱いの困難さから、実際には、１g/cc以上のかさ
密度の比較的大きなシリカ粉体が用いられている。In order to obtain a homogeneous silica glass foam using ammonia, it is important to bond the ammonia to the silica glass as uniformly as possible.
There must be many reactive groups (generally presumed to be SiOH groups) on the surface of the silica powder that are considered to chemically bond with ammonia, and the silica powder to be ammoniated is a fine powder having a large surface area. desirable. However, despite such technical concept, silica powder having a bulk density of 1 g / cc or more is actually used due to the difficulty of handling the fine silica powder to be treated.
【０００４】他方、直接法やス−ト法による合成石英ガ
ラスの製造においては、合成石英ガラス体として固定で
きない多量のシリカ微粉体が生成するが、その取扱いの
困難さから廃棄処分されているのが実状である。そのよ
うな捨てられているシリカ微粉体は、例えば、かさ密度
が0.3 g/cc以下で粒径が 0.2〜数μｍ程度の微細粉であ
って、本来、アンモニア化するには望ましいが、ハンド
リングの困難さのために有効利用されることはなかっ
た。本発明者らは、かかる表面積の大きい極微細シリカ
粉をシリカガラス発泡体の製造に有効利用することに着
目した。[0004] On the other hand, in the production of synthetic quartz glass by the direct method or the soot method, a large amount of silica fine powder that cannot be fixed as a synthetic quartz glass body is generated, but is discarded due to difficulty in handling. Is the actual situation. Such discarded silica fine powder is, for example, a fine powder having a bulk density of 0.3 g / cc or less and a particle size of about 0.2 to several μm. It was not used effectively due to the difficulty. The present inventors have focused on effectively utilizing such ultrafine silica powder having a large surface area for producing a silica glass foam.
【０００５】[0005]
【発明が解決しようとする課題】従って、本発明の課題
は、ハンドリングが困難な極めて微細なシリカガラス粉
を有効に利用する工業的に望ましい技術を開発すること
にある。また、本発明の他の課題は、特に、従来合成石
英ガラスの製造において、バッグフィルタ−で捕集され
産業廃棄物として捨てられていた極めて微細なシリカガ
ラス粉を原料として、その大きな比表面積を利用して効
果的に且つ極めて均質な石英ガラス発泡体を製造する方
法を提供することにある。SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to develop an industrially desirable technique for effectively utilizing extremely fine silica glass powder which is difficult to handle. Another problem of the present invention is that, in the production of synthetic quartz glass, in particular, using a very fine silica glass powder, which has been collected by a bag filter and discarded as industrial waste, as a raw material, a large specific surface area is obtained. It is an object of the present invention to provide a method for producing a quartz glass foam which is effective and extremely homogeneous by utilizing the same.
【０００６】[0006]
【課題を解決するための手段】本発明者らは、比表面積
が大きいためアンモニアとの反応性としては望ましいも
のの、取扱いの困難な極微細なシリカ粉を出発原料とし
てシリカ発泡体を製造する方法について研究を重ねた結
果、該微細シリカ粉を水と接触させて、形成された水性
スラリ−からケ−キを形成させ、これを仮焼成して粉砕
した顆粒状の多孔質粉粒体が、実質的にその大きな表面
積が保持された取扱い容易なシリカ原料として極めて有
用であり望ましい材料であることを見出した。DISCLOSURE OF THE INVENTION The present inventors have proposed a method for producing a silica foam using ultrafine silica powder, which is desirable in terms of reactivity with ammonia due to its large specific surface area but difficult to handle, as a starting material. As a result of repeated studies, the fine silica powder was brought into contact with water to form a cake from the formed aqueous slurry, which was calcined and pulverized to obtain a granular porous powder. It has been found that the material is extremely useful and desirable as an easily handled silica raw material having substantially retained its large surface area.
【０００７】すなわち、本発明は、比表面積10ｍ2/ｇ〜
400 ｍ2/ｇを有するシリカ微粉末を水に分散させ、その
分散スラリ−を脱水，乾燥させて塊状の多孔質のシリカ
ケ−キを作り、該シリカケ−キを粉砕して得られた顆粒
状の多孔質シリカガラス粉粒体を 800〜1300℃の範囲内
の温度で加熱仮焼結させた後、又は該仮焼結時に同範囲
内の温度でアンモニア雰囲気中にてアンモニアと反応さ
せ、次いで、この仮焼結された粉粒体を型に入れて1400
℃以上の温度に加熱して発泡させることを特徴とする石
英ガラス発泡体の製造方法を要旨とするものでる。[0007] That is, the present invention provides a specific surface area of 10 m 2 / g or more.
A fine silica powder having a particle size of 400 m 2 / g is dispersed in water, and the dispersed slurry is dehydrated and dried to form a massive porous silica cake, and the granules obtained by pulverizing the silica cake are obtained. After preheating and sintering the porous silica glass powder at a temperature in the range of 800 to 1300 ° C., or during the presintering, reacting with ammonia in an ammonia atmosphere at a temperature in the same range, , Put the pre-sintered powder into a mold,
The present invention provides a method for producing a quartz glass foam, wherein the foam is formed by heating to a temperature of not less than ° C.
【０００８】本発明は、従来、合成石英ガラス製造にお
いて生ずる工業的に利用できなかった大きな比表面積を
有する、換言すれば、見かけ比重の極めて小さいハンド
リング困難なシリカ微粉を、そのハンドリングを容易に
すると共に、大きな比表面積を利用して好都合にアンモ
ニア化を行い、更に、これを加熱溶融と発泡を連続し
て、あるいは同時に行わせて所望の均質な石英ガラス発
泡体を効果的に製造することができるという技術的発見
に新規性と進歩性を主張するものである。[0008] The present invention facilitates the handling of silica fine powder having a large specific surface area, which is conventionally not industrially available in the production of synthetic quartz glass and has a very small apparent specific gravity, which is difficult to handle. At the same time, it is possible to carry out ammonia conveniently using a large specific surface area, and furthermore, to carry out the heating melting and foaming continuously or simultaneously to effectively produce a desired homogeneous quartz glass foam. It asserts novelty and inventive step in the technological discovery that it can be done.
【０００９】本発明の方法に用いられる出発原料は、10
ｍ2/ｇ〜400 ｍ2/ｇの比表面積を有する極微細なシリカ
粉であり、揮発性珪素化合物を酸水素炎で加水分解して
得られるシリカ超微粉体や合成石英ガラスの製造の際に
ダクトを経てバッグフィルタ−に捕集される極めて軽量
なシリカ微粉体やシリカを粉砕する時などに形成される
取扱い困難な極微細な粉体であって、例えば、粒径が
0.2〜２μｍで比表面積が30ｍ2/ｇ以上を有する微粉状
シリカ類が包含される。The starting material used in the process of the present invention is 10
m 2 / g~400 m 2 / g is a very fine silica powder having a specific surface area of, the production of ultrafine silica fine powder and a synthetic quartz glass obtained by a volatile silicon compound is hydrolyzed in an oxyhydrogen flame At this time, very light silica fine powder collected in a bag filter through a duct or an extremely fine powder that is difficult to handle and formed when crushing silica, for example, having a particle size of
Finely divided silicas having a specific surface area of 0.2 m to 2 m and a specific surface area of 30 m2 / g or more are included.
【００１０】このような極微細状シリカ粉は、まず水に
接触させ懸濁させてスラリ−に形成される。次いで、こ
のシリカスラリ−は媒体水を分離除去してケ−キに形成
されるが、懸濁シリカ粒子は極めて微細なため、通常の
濾過分離は困難であり、例えば、５kgf/cm2 の加圧濾過
を施しても、濾布が直ぐに目詰まりを生じて実質的に濾
過が停止し、濾過によるケ−キの形成はできないし、た
とえ時間をかけて濾過したとしてしても水洗浄は不可能
である。従って、このスラリ−は、好ましくは遠心分離
等によってある程度水を分離し、次いで、通常、放置乾
燥、あるいは多少加熱して乾燥，凝固させることにより
適度の硬さのシリカケ−キにすることができる。[0010] Such ultrafine silica powder is first contacted with water and suspended to form a slurry. Next, this silica slurry is formed into a cake by separating and removing the medium water. However, since the suspended silica particles are extremely fine, ordinary filtration and separation are difficult. For example, a pressure of 5 kgf / cm 2 is applied. Even if filtration is performed, the filter cloth is immediately clogged and the filtration is substantially stopped, so that the cake cannot be formed by the filtration. It is. Therefore, the slurry can be separated into water to some extent, preferably by centrifugation, and then usually dried by standing, or slightly heated to be dried and solidified to obtain a silica cake having an appropriate hardness. .
【００１１】このケ−キの硬さは、スラリ−中のシリカ
粉体と媒体水の割合と乾燥速度に大きく影響され、例え
ば、水の量が多いほど、また乾燥速度が遅いほど硬いケ
−キが形成される。それ故、シリカ微粉の水懸濁スラリ
−の形成においては、得ようとする乾燥ケ−キの所望硬
さに応じて、その懸濁用水の量が選択使用される。水の
量があまり多すぎては脱水乾燥に時間を要するので不利
であり、また、少なすぎては取扱いやケ−キの硬さをコ
ントロ−ルすることが困難となるので好ましくない。実
用的には、例えば、シリカ微粉の重量に対して１〜２重
量倍程度の範囲量のスラリ−用水が使用される。乾燥速
度は、乾燥温度によって調整することができるが、通
常、乾燥温度は 100℃前後が工業的に有利に採用され
る。The hardness of the cake is greatly affected by the ratio of the silica powder in the slurry to the medium water and the drying speed. For example, the harder the amount of water and the slower the drying speed, the harder the cake. A key is formed. Therefore, in forming a water suspension slurry of fine silica powder, the amount of water for suspension is selected and used depending on the desired hardness of the dried cake to be obtained. If the amount of water is too large, it takes a long time for dehydration and drying, which is disadvantageous. On the other hand, if the amount is too small, it becomes difficult to handle and control the hardness of the cake. Practically, for example, slurry water is used in an amount of about 1 to 2 times the weight of the silica fine powder. The drying speed can be adjusted by the drying temperature, but usually, the drying temperature of about 100 ° C. is industrially advantageously employed.
【００１２】このようにして形成された硬い多孔質体の
ケ−キは、これを粉砕して、望ましくは、粒径が10μｍ
〜１mm程度の範囲の顆粒状の多孔質シリカ粉体に調整さ
れ、アンモニア化処理に供される。その分級は、用途や
目的によって更に狭い粒度範囲に調整することができ
る。粉砕はどのような手段を用いてもよいが、ボ−ルミ
ルが実用的である。また使用するボ−ルは、アルミナボ
−ルミルでは混入するアルミナの除去が非常に困難なた
め、例えば、ポリエチレンやテフロン等が好都合に使用
できるが、石英ガラス製のボ−ルが極めて有利である。
それらのボ−ル類は、通常、ケ−キの硬さによって適切
なものが選択使用される。更に、この粉砕は、上記のよ
うな粒径範囲の顆粒状粉粒体に調整されることが好まし
い。The hard porous cake thus formed is pulverized, preferably to a particle size of 10 μm.
It is adjusted to a granular porous silica powder having a size of about 1 mm and is subjected to an ammonia treatment. The classification can be adjusted to a narrower particle size range depending on the application and purpose. Although any means may be used for the pulverization, a ball mill is practical. As for the ball to be used, it is very difficult to remove alumina mixed with an alumina ball mill. For example, polyethylene or Teflon can be conveniently used, but a ball made of quartz glass is extremely advantageous.
These balls are usually selected appropriately depending on the hardness of the cake. Further, this pulverization is preferably adjusted to a granular powder having a particle size range as described above.
【００１３】形成された顆粒状のシリカ粉粒体は、原料
超微粉粒子の凝集体であって、径が大幅に増大した取扱
いの容易な粉粒体である。この粉粒体は、原料シリカ微
粉に比べてその非表面積が僅かに低減する程度の優れた
多孔性を有する多孔質体であり、シリカガラスの変性に
極めて好都合に利用することができる。本発明方法にお
いては、このように粉砕し調整された顆粒状シリカ粉粒
体は 800〜1300℃の範囲内の温度に加熱して仮焼結れ
る。得られた仮焼結体も高い多孔性を保持するので、こ
れをアンモニア雰囲気中で加熱することにより、極めて
効果的にアンモニアと反応させることができる。The formed granular silica powder is an agglomerate of raw material ultrafine powder particles, and has a greatly increased diameter and is easy to handle. This powder is a porous material having excellent porosity such that its non-surface area is slightly reduced as compared with the raw material silica fine powder, and can be used very advantageously for modifying silica glass. In the method of the present invention, the granular silica powder thus pulverized and adjusted is preliminarily sintered by heating to a temperature in the range of 800 to 1300 ° C. Since the obtained pre-sintered body also retains high porosity, it can be reacted with ammonia very effectively by heating it in an ammonia atmosphere.
【００１４】上記仮焼結温度とアンモニア化反応温度
は、その温度領域がほゞ同じであるから仮焼結と、これ
に続くアンモニア化反応を連続して行うことができる
が、共通温度領域を利用して仮焼結をアンモニア雰囲気
中で行うことにより、仮焼結と同時にアンモニア化反応
を行わせることができるので、この同時処理は工業的に
極めて望ましい。仮焼結されアンモニア化された多孔質
シリカ粉粒体は、次いで、所望の成形型に入れ、1400℃
以上の温度に加熱溶融することにより、シリカ粉粒体を
相互に融着一体化すると共にアンモニア基の分解，ガス
化発泡により、成形型の形状の石英ガラス発泡体成形物
を効率良く製造することができる。Since the temperature range of the preliminary sintering temperature and the ammoniating reaction temperature is almost the same, the preliminary sintering and the subsequent ammoniating reaction can be continuously performed. By performing the preliminary sintering in an ammonia atmosphere by utilizing the same, the ammoniating reaction can be performed simultaneously with the preliminary sintering, so that this simultaneous treatment is industrially extremely desirable. The pre-sintered and ammoniated porous silica powder is then placed in a desired mold, at 1400 ° C.
By heating and melting at the above temperature, the silica powder particles are fused and integrated with each other, and the ammonia group is decomposed and gasified and foamed to efficiently produce a quartz glass foam molded article in the shape of a mold. Can be.
【００１５】上記のアンモニア化処理された仮焼結粉粒
体の発泡化処理においては、そのアンモニア化粉粒体に
他のアンモニア化処理を施さないシリカ微粉末を加えて
発泡体の発泡度をコントロ−ルすることができる。その
場合、好ましくは、例えば、粒径が 100〜700 μｍの範
囲のアンモニア化された多孔質シリカ粉粒体に、その10
0重量部に対し、10ｍ2/ｇ〜400 ｍ2/ｇの比表面積を有
するアンモニア化処理されていないシリカ微粉末 0.5〜
50重量部を混合することにより、より低い所望密度の発
泡体を得ることができる。[0015] In the foaming treatment of the above-mentioned ammoniated pre-sintered granules, the fine particles of silica which are not subjected to other ammonium treatment are added to the ammoniated granules to reduce the foaming degree of the foam. It can be controlled. In that case, preferably, for example, the ammoniated porous silica powder having a particle size in the range of 100 to 700 μm has
To 0 parts by weight of silica fine powder 0.5 not treated ammoniated having a specific surface area of 10m 2 / g~400 m 2 / g
By mixing 50 parts by weight, a foam having a lower desired density can be obtained.
【００１６】[0016]
【作用】本発明の石英ガラス発泡体の製造方法は、廃棄
処分されていた超微細合成シリカ粉を原料に用いて、容
易なハンドリングで所望発泡度の石英ガラス発泡体を効
率良く製造することができる。According to the method for producing a quartz glass foam of the present invention, it is possible to efficiently produce a quartz glass foam having a desired degree of foaming by easy handling by using a discarded ultrafine synthetic silica powder as a raw material. it can.
【００１７】[0017]
【実施例】次に、本発明を具体例により、更に詳細に説
明する。 実施例 １ 四塩化珪素を酸水素バ−ナ−火炎中に導入し、微細シリ
カ粉を基体上に堆積させてス−ト体を形成させると共
に、堆積されずにダクトを経て排出される極微細なシリ
カ粉をフィルタ−で捕集した。得られた微細なシリカ粉
の粒径は 0.1〜３μｍで、ＢＥＴ法によって測定された
比表面積は約50ｍ2/ｇの極めて軽いものであった。この
微粉体１kgを純水1.5 kg中に入れて良く混合し均一なス
ラリ−を形成させ、次いで、このスラリ−を遠心分離機
である程度の水を分離させ、得られた比較的粘度の高い
どろどろした濃縮スラリ−をバットにあけて全体に広
げ、80℃の温度で24時間乾燥してシリカケ−キを形成さ
せた。Now, the present invention will be described in further detail with reference to specific examples. Example 1 Silicon tetrachloride was introduced into an oxyhydrogen burner flame, and fine silica powder was deposited on a substrate to form a soot body. Silica powder was collected with a filter. The particle size of the obtained fine silica powder was 0.1 to 3 μm, and the specific surface area measured by the BET method was very light, about 50 m 2 / g. 1 kg of this fine powder is put into 1.5 kg of pure water and mixed well to form a uniform slurry, and then this slurry is separated to a certain extent by a centrifuge to obtain a relatively thick muddy mud. The concentrated slurry was spread in a vat and spread over the whole, and dried at a temperature of 80 ° C. for 24 hours to form a silica cake.
【００１８】この硬い多孔質シリカケ−キをネット間隙
約１mmのトロンメルふるいに入れ、石英ガラスビ−ズを
用いて50rpm の速度で回転させながら粉砕と予備分級を
行った。このふるいを通過した粉砕シリカ粉を 700μｍ
にかけ、このふるい目を通ったものについて更に 100μ
ｍのふるいにかけ、これを通った微細粒子を除外して10
0〜700 μｍの粒径範囲の多孔質シリカ粉を調製した。
得られた顆粒状シリカ粉粒体は、約600ｇで、ＢＥＴ法
によるその比表面積値は35m2/gであった。これを石英ガ
ラス製ボ−トに入れ、横型の石英ガラス製炉芯管を載置
した電気炉内でアンモニアガスと窒素ガスの１：１容量
割合の混合ガスを毎分10リットルの速度で雰囲気中に流
しながら、1100℃の温度条件下に５時間アンモニア化処
理を行った。This hard porous silica cake was placed in a trommel sieve having a net gap of about 1 mm, and crushed and pre-classified while rotating at a speed of 50 rpm using a quartz glass bead. 700 μm of ground silica powder passed through this sieve
And further pass through this sieve for another 100μ
m, excluding fine particles that have passed through
Porous silica powder having a particle size range of 0 to 700 μm was prepared.
The obtained granular silica powder weighed about 600 g, and had a specific surface area of 35 m 2 / g by the BET method. This was placed in a quartz glass boat, and a mixed gas of ammonia gas and nitrogen gas at a volume ratio of 1: 1 at an atmosphere of 10 liters per minute was placed in an electric furnace equipped with a horizontal quartz glass furnace tube. Ammonia treatment was carried out for 5 hours at a temperature of 1100 ° C. while flowing the solution.
【００１９】アンモニア処理を行った顆粒状石英ガラス
粉 ｇを、グラファイト製の内容が15cm×15cm×20cmの
型に入れ、真空炉内で1650℃の温度に１時間加熱溶融処
理した。冷却後、型から15cm×15cm×６cmの発泡体が取
出された。その多孔質直方体状発泡体の密度は、0.4g／
ccであった。The granulated silica glass powder g subjected to the ammonia treatment was placed in a mold having a content of graphite of 15 cm × 15 cm × 20 cm, and was heated and melted at a temperature of 1650 ° C. for 1 hour in a vacuum furnace. After cooling, a 15 cm × 15 cm × 6 cm foam was removed from the mold. The density of the porous rectangular foam is 0.4 g /
It was cc.
【００２０】実施例 ２ 四塩化珪素を酸水素バ−ナ−火炎中に導入し、生成する
微細シリカ粉をバッグフィルタ−で捕集した。得られた
微細なシリカ粉の粒径は 0.1〜３μｍで、ＢＥＴ法によ
って測定された比表面積は約50ｍ2/ｇであった。この微
粉体１kgを純水1.5 kg中に入れて良く混合し均一なスラ
リ−を形成させ、次いで、このスラリ−を遠心分離機で
ある程度の水を分離した後、得られた比較的粘度の高い
どろどろした濃縮スラリ−をバットにあけて全体に広
げ、80℃の温度で24時間乾燥してシリカケ−キを形成得
た。Example 2 Silicon tetrachloride was introduced into an oxyhydrogen burner flame, and the resulting fine silica powder was collected by a bag filter. The particle size of the obtained fine silica powder was 0.1 to 3 μm, and the specific surface area measured by the BET method was about 50 m 2 / g. 1 kg of this fine powder is put into 1.5 kg of pure water and mixed well to form a uniform slurry. Then, the slurry is separated into a certain amount of water by a centrifugal separator. The thick slurry was poured into a vat, spread over the whole, and dried at a temperature of 80 ° C. for 24 hours to form a silica cake.
【００２１】得られたシリカケ−キを石英ガラスビ−ズ
入りトロンメルふるいに入れ、50rpm の速度で回転させ
ながら扮し予備分級を行った。得られた分級粉を 100μ
ｍ目のふるい及び 700μｍ目のふるいで 100〜700 μｍ
の粒径範囲の顆粒状多孔質シリカ粉に調製した。ＢＥＴ
法によって測定された比表面積値35m2/gの顆粒状シリカ
粉粒体約600ｇが得られた。これを石英ガラス製ボ−ト
に入れ、横型の石英ガラス製炉芯管を載置した電気炉内
でアンモニアガスと窒素ガスの１：１容量割合の混合ガ
スを毎分10リットルの速度で雰囲気中に流しながら、11
00℃の温度条件下に５時間アンモニア処理を行った。The obtained silica cake was put into a trommel sieve containing quartz glass beads, and preliminarily classified while rotating at a speed of 50 rpm. 100μ of the obtained classified powder
100-700 μm with m-th sieve and 700 μm sieve
Was prepared into a granular porous silica powder having a particle size range of BET
About 600 g of granular silica powder having a specific surface area of 35 m 2 / g measured by the method was obtained. This was placed in a quartz glass boat, and a mixed gas of ammonia gas and nitrogen gas at a volume ratio of 1: 1 at an atmosphere of 10 liters per minute was placed in an electric furnace equipped with a horizontal quartz glass furnace tube. 11
Ammonia treatment was performed at a temperature of 00 ° C. for 5 hours.
【００２２】アンモニア化処理された顆粒状石英ガラス
多孔質体300gと四塩化珪素を酸水素バ−ナ−火炎中に導
入して作製したＢＥＴ法による比表面積値50m2/gの微細
シリカ粉100gを混合し、実施例１で用いた同じグラファ
イト製型内に入れて同様の条件で発泡体を作製した。得
られた発泡体は、密度が0.27g/ccの比較的低密度の多孔
質直方体（15cm×15cm×10cm）であった。この発泡体
は、低密度であるにもかかわらず極めて均一な泡分布が
認められた。100 g of fine silica powder having a specific surface area of 50 m 2 / g by the BET method, prepared by introducing 300 g of the ammoniated granular porous silica glass and silicon tetrachloride into a oxyhydrogen burner flame. Were mixed and placed in the same graphite mold used in Example 1 to produce a foam under the same conditions. The obtained foam was a relatively low-density porous rectangular parallelepiped (15 cm × 15 cm × 10 cm) having a density of 0.27 g / cc. The foam had a very uniform foam distribution despite its low density.
【００２３】[0023]
【発明の効果】本発明の方法によれば、これまで合成石
英ガラス製造時に不可避的に形成されている取扱いが困
難で廃棄処理されていた極微細なシリカ粉から極めて高
純度の石英ガラス発泡体を効率良く製造することができ
るので、本発明は、産業上の絶大な有利性を有するのみ
ならず、環境衛生上の見地からも優れた実用的価値を有
する。According to the method of the present invention, a very high-purity quartz glass foam is produced from ultrafine silica powder which has been inevitably formed during the production of synthetic quartz glass and which has been difficult to handle and has been discarded. Since the present invention can be produced efficiently, the present invention has not only a great industrial advantage, but also an excellent practical value from the viewpoint of environmental health.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 木村 博至 福井県武生市北府２丁目13番60号 信越 石英株式会社 武生工場内 (56)参考文献 特開 平１−308846（ＪＰ，Ａ) 特開 平５−279083（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) C03B 20/00 C03C 11/00 C03C 3/00────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hiroshi Kimura 2-13-60 Kitafu, Takefu-shi, Fukui Prefecture Shin-Etsu Quartz Co., Ltd. Inside the Takefu Plant (56) References JP-A-1-308846 (JP, A) Kaihei 5-2799083 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) C03B 20/00 C03C 11/00 C03C 3/00
Claims (3)
リカ微粉末を水に分散させ、その分散スラリ−を脱水，
乾燥させて塊状の多孔質のシリカケ−キを作り、該シリ
カケ−キを粉砕して得られた顆粒状の多孔質シリカガラ
ス粉粒体を 800〜1300℃の範囲内の温度で加熱仮焼結さ
せた後、又は該仮焼結時に同範囲内の温度でアンモニア
雰囲気中にてアンモニアと反応させ、次いで、この仮焼
結された粉粒体を型に入れて1400℃以上の温度に加熱し
て発泡させることを特徴とする石英ガラス発泡体の製造
方法。1. A fine silica powder having a specific surface area of 10m 2 / g~400 m 2 / g were dispersed in water, the dispersion slurry - dehydration,
It is dried to form a massive porous silica cake, and the granular porous silica glass powder obtained by pulverizing the silica cake is heated and pre-sintered at a temperature in the range of 800 to 1300 ° C. After that, or during the preliminary sintering, react with ammonia in an ammonia atmosphere at a temperature within the same range, and then place the temporarily sintered powder in a mold and heat it to a temperature of 1400 ° C. or more. A method for producing a quartz glass foam, wherein the quartz glass foam is foamed.
水素火炎で加水分解して得られる比表面積が15〜80ｍ2/
ｇの合成石英ガラス微粉末である請求項１に記載の石英
ガラス発泡体の製造方法。Wherein the silica fine powder, the specific surface area obtained by a volatile silicon compound is hydrolyzed with oxyhydrogen flame 15～80M 2 /
The method for producing a quartz glass foam according to claim 1, which is a synthetic quartz glass fine powder of g.
リカ微粉末を水に分散させ、形成されたスラリ−を脱
水，乾燥させて塊状の多孔質のシリカケ−キを作り、該
シリカケ−キを粉砕して得られた顆粒状の多孔質シリカ
ガラスの粉粒体を 800〜1300℃の範囲内の温度で加熱仮
焼結させた後、又は該仮焼結時に同範囲内の温度でアン
モニア雰囲気中にてアンモニアと反応させ、その多孔質
シリカ粉粒体を分級して得られた粒径が 100〜700 μｍ
の範囲の該粉粒体に、10ｍ2/ｇ〜400 ｍ2/ｇの比表面積
を有するアンモニア化されていないシリカ微粉体を前記
仮焼結された多孔質シリカ粉粒体 100重量部に対し 0.5
〜50重量部の範囲割合で混合し、次いで、この混合物を
型に入れて1400℃以上の温度に加熱して発泡させること
を特徴とする石英ガラス発泡体の製造方法。3. A fine silica powder having a specific surface area of 10m 2 / g~400 m 2 / g was dispersed in water, the formed slurry - dehydrated and dried to a porous bulk Shirikake - make key, After the powdery granules of the porous silica glass obtained by pulverizing the silica cake are heated and pre-sintered at a temperature within the range of 800 to 1300 ° C., or within the same range during the pre-sintering. At a temperature of ammonia in an ammonia atmosphere and classify the porous silica particles to a particle size of 100-700 μm.
The powder or granular material ranging in respect 10m 2 / g~400 m 2 / porous silica powder granules 100 parts by weight of silica fine powder which has not been ammoniated is the preliminary sintering has a specific surface area of g 0.5
A method for producing a quartz glass foam, comprising mixing the mixture in a proportion of about 50 parts by weight, and then placing the mixture in a mold and heating to a temperature of 1400 ° C. or more to foam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16547293A JP2820865B2 (en) | 1993-07-05 | 1993-07-05 | Method for producing quartz glass foam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16547293A JP2820865B2 (en) | 1993-07-05 | 1993-07-05 | Method for producing quartz glass foam |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0717731A JPH0717731A (en) | 1995-01-20 |
| JP2820865B2 true JP2820865B2 (en) | 1998-11-05 |
Family
ID=15813064
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16547293A Expired - Fee Related JP2820865B2 (en) | 1993-07-05 | 1993-07-05 | Method for producing quartz glass foam |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2820865B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4297578B2 (en) * | 1999-12-22 | 2009-07-15 | 信越石英株式会社 | Method for producing opaque quartz glass |
| RU2634321C1 (en) * | 2016-08-04 | 2017-10-25 | Акционерное общество "Научно-исследовательский и технологический институт оптического материаловедения Всероссийского научного центра "Государственный оптический институт им. С.И. Вавилова" (АО "НИТИОМ ВНЦ "ГОИ им. С.И. Вавилова") | Method of producing optical quartz glass |
-
1993
- 1993-07-05 JP JP16547293A patent/JP2820865B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0717731A (en) | 1995-01-20 |
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