JPS6385115A - Preparation of stock solution for spinning alumina fiber - Google Patents
Preparation of stock solution for spinning alumina fiberInfo
- Publication number
- JPS6385115A JPS6385115A JP61232165A JP23216586A JPS6385115A JP S6385115 A JPS6385115 A JP S6385115A JP 61232165 A JP61232165 A JP 61232165A JP 23216586 A JP23216586 A JP 23216586A JP S6385115 A JPS6385115 A JP S6385115A
- Authority
- JP
- Japan
- Prior art keywords
- spinning
- silica sol
- aluminum chloride
- solution
- basic aluminum
- 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
- 238000009987 spinning Methods 0.000 title claims abstract description 42
- 239000000835 fiber Substances 0.000 title claims abstract description 31
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000011550 stock solution Substances 0.000 title abstract description 13
- 238000002360 preparation method Methods 0.000 title description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 44
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 32
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 19
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 abstract description 22
- 239000011259 mixed solution Substances 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 238000004079 fireproofing Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000004705 High-molecular-weight polyethylene Substances 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000003303 reheating Methods 0.000 description 2
- -1 silica compound Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- 229910020169 SiOa Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000013305 flexible fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はアルミナ繊維紡糸原液の調製方法に関し、殊に
塩基性塩化アルミニウムとシリカゾルを主原料とするア
ルミナ繊維に於て、耐火強度特性に優れたアルミナｍＭ
１を提供するためのアルミナ繊維紡糸原液の調製方法に
関する。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for preparing an alumina fiber spinning dope, and in particular, alumina fibers whose main raw materials are basic aluminum chloride and silica sol have excellent fire resistance and strength properties. alumina mm
1. The present invention relates to a method for preparing an alumina fiber spinning stock solution for providing an alumina fiber spinning dope.
（従来の技術）
アルミナ繊維は耐熱性に優れ、ま、た高強度、高弾性で
あることより従来から高温用断熱材、プラスチック、金
属等の強化材として利用検討されている。(Prior Art) Alumina fibers have excellent heat resistance, high strength, and high elasticity, and have thus far been considered for use as high-temperature insulation materials, reinforcing materials for plastics, metals, and the like.
しかし、この繊維は１５００℃以上の高温で使用すると
、α−ＡＩ２０３結晶が急激に成長し、結晶粒径が大き
くなり、また多くの空孔が発生し、４１維強度は急激に
低下し、長時間の使用では１５００℃が限界温度である
とされている。However, when this fiber is used at a high temperature of 1500°C or higher, the α-AI203 crystals grow rapidly, the crystal grain size increases, and many vacancies are generated, the strength of the 41 fiber decreases rapidly, and the length of the fiber increases. It is said that 1500° C. is the limit temperature for use for hours.
アルミナ繊維の粒成長を抑え、その結果、高温耐熱性を
改善するために、従来よりケイ素化合物をアルミナ繊維
中に導入する方法が知られており、シリカゾル等を紡糸
液と混合し、紡糸することが行われている。 また、塩
基性塩化アルミニウム溶液を濃縮して紡糸原液としたも
のは、曳糸性が不充分であり、紡糸原液が液滴下し易く
、シシットを多合したものしか得られないという欠点を
有するため、これを改善する方法としてポリビニルアル
コール、ポリビニルピロリドン、デンプン等の水溶性有
機高分子が使用される。In order to suppress the grain growth of alumina fibers and, as a result, improve their high-temperature heat resistance, it has been known to introduce silicon compounds into alumina fibers. is being carried out. In addition, the spinning stock solution obtained by concentrating the basic aluminum chloride solution has the disadvantage that the spinnability is insufficient, the spinning stock solution tends to drip, and only a mixture of shishite can be obtained. As a method to improve this, water-soluble organic polymers such as polyvinyl alcohol, polyvinylpyrrolidone, and starch are used.
しかし、塩基性塩化アルミニウムとシリカゾルは種々な
面で相反する性質をイイし、塩基性塩化アルミニウムに
シリカ化合物を導入したものは、塩基性塩化アルミニウ
ムと相溶性の良い水溶性高分子とシリカ化合物との相互
作用を生じ、溶液が不均一となることより、４１維化し
た繊維中の組成が不均一となり、シリカ化合物の使用効
果が１）られない、 従って、通常水溶性高分子の内で
もシリカとの結合が比較的軽微なポリビニルアルコール
が使用されている。However, basic aluminum chloride and silica sol have contradictory properties in various aspects, and basic aluminum chloride with a silica compound has a water-soluble polymer and silica compound that are highly compatible with basic aluminum chloride. As a result of the interaction of Polyvinyl alcohol is used because it has a relatively weak bond with.
しかし、ポリビニルアルコールは本来曳糸性に優れず、
このため未だ紡糸液の曳糸性が充分でなく、従って限ら
れた高粘度範囲で使用され、紡糸方法もジェット紡糸、
遠心力紡糸等による方法に制限されているのが現状であ
り、ショットを多含する問題は依然として残されてい−
る。However, polyvinyl alcohol does not inherently have excellent spinnability,
For this reason, the spinnability of the spinning solution is still insufficient, so it is used in a limited high viscosity range, and the spinning methods are also jet spinning,
Currently, methods are limited to methods such as centrifugal spinning, and the problem of involving many shots still remains.
Ru.
（発明が解決しようとする問題点）
本発明者らはこの様な現状の中で、塩基性塩化アルミニ
ウムとシリカゾルを主原料とするアルミナｍ維の製造に
於て、強度、耐熱、耐火性の優れるアルミナｍ維を得る
ための紡糸原液を提供するために、その曳糸性を改善す
ること、並びにシリカゾルと水溶性高分子との相互作用
を生起させず、均一に紡糸液中にシリカゾルを分散させ
ることにより前記問題点を解決すべく、鋭意研究を進め
た。(Problems to be Solved by the Invention) Under the current circumstances, the present inventors have developed an approach to improve strength, heat resistance, and fire resistance in the production of alumina m-fiber whose main raw materials are basic aluminum chloride and silica sol. In order to provide a spinning stock solution for obtaining excellent alumina m-fibers, we need to improve its spinnability and uniformly disperse silica sol in the spinning solution without causing interaction between the silica sol and the water-soluble polymer. In order to solve the above problems by doing so, we have carried out intensive research.
（問題点を解決するための手段）
その結果、シリカゾル又はシリカゾルと塩基性塩化アル
ミニウムとの混合液を、予め低分子量のポリエチレング
リコールで前処理した後、次いで、高分子量のポリエチ
レンオキサイドを紡糸助剤として使用することにより、
前記問題が解決されることを見い出し、本発明を完成し
たものである。(Means for solving the problem) As a result, silica sol or a mixture of silica sol and basic aluminum chloride is pretreated with low molecular weight polyethylene glycol, and then high molecular weight polyethylene oxide is added as a spinning aid. By using it as
The present invention has been completed by discovering that the above problem can be solved.
即ち本発明は、塩基性塩化アルミニウムとシリカゾルを
主原料とするアルミナ４＆ｌ雑の製造に於・て、シリカ
ゾル又はシリカゾルと塩基性塩化アルミニウムとの混合
液を、分子量２０，０００以下のポリエチレングリコー
ルで前処理した後、次いで分子Ｆｉ３０ｏ、ｏｏｏ以上
のポリエチレンオキサイドを紡糸助剤として使用するこ
とを特徴とするアルミナ繊維紡糸原液の調製法に関する
。That is, in the production of alumina 4&l miscellaneous products whose main raw materials are basic aluminum chloride and silica sol, the present invention involves pre-preparing silica sol or a mixture of silica sol and basic aluminum chloride with polyethylene glycol having a molecular weight of 20,000 or less. The present invention relates to a method for preparing an alumina fiber spinning dope, which is characterized in that after the treatment, polyethylene oxide with a molecular Fi of 30o, ooo or more is used as a spinning aid.
然して、本発明の目的は、紡糸原液の曳糸性を改善する
ことにより、従来紡糸方法が制限されていたアルミナｕ
Ａ維前駆体の製造を容易ならしめ、繊維形態の向上とシ
ョットの低減を図ることにあり、更にはシリカゾルを紡
糸原液中に均一に分散させることにより、アルミナｍ維
の耐熱耐火強度特性を向上させることにある。However, the purpose of the present invention is to improve the spinnability of the spinning stock solution, thereby improving the spinnability of alumina U, which has been limited in the conventional spinning method.
The aim is to facilitate the production of A-fiber precursors, improve the fiber morphology and reduce shots, and further improve the heat and fire resistance properties of alumina M-fibers by uniformly dispersing silica sol in the spinning dope. It's about letting people know.
（作 用）
本発明について更に詳述すると、先ず本発明で使用する
塩基性塩化アルミニウムは、通常、塩基度が７０％以−
にのものでるり、これを下回ると本発明の効果を得るこ
とが困難となる。(Function) To explain the present invention in more detail, firstly, the basic aluminum chloride used in the present invention usually has a basicity of 70% or more.
Below this value, it becomes difficult to obtain the effects of the present invention.
またシリカゾルは、コロイド状態で無定形シリカ質から
なり、水溶液中で安定的にゾルを形成するものを使用す
る。The silica sol used is one that is made of amorphous silica in a colloidal state and forms a sol stably in an aqueous solution.
また、ポリエチレングリコールは分子量が２０，０００
以下のものとして、通常、２００〜２０，０００の範囲
のものを使用する。In addition, polyethylene glycol has a molecular weight of 20,000
As for the following, those in the range of 200 to 20,000 are usually used.
更に、ポリエチレンオキサイドは分子量が３００，００
０以上のものを使用する。Furthermore, polyethylene oxide has a molecular weight of 300,00
Use 0 or more.
即ち、これらポリエチレングリコール、ポリエチレンオ
キサイド以外の有機化合物、或いは分子量が前記の範囲
を逸脱するものを使用した場合には本発明の効果を得る
ことができない。That is, if an organic compound other than polyethylene glycol or polyethylene oxide is used, or if an organic compound having a molecular weight outside the above-mentioned range is used, the effects of the present invention cannot be obtained.
これらの原料を使用し、本発明のアルミナｍ雑紡糸原液
を調製する方法は、先ずシリカゾルを前記ポリエチレン
グリコールで前処理した後、ポリエチレンオキサイドを
加えるか、又はシリカゾルと塩基性塩化アルミニウムを
予め混合した液を、前記ポリエチレングリコールで前処
理した後、ポリエチレンオキサイド°を加える方法のい
ずれかの方法により行う。The method for preparing the alumina m-spun stock solution of the present invention using these raw materials is to first pre-treat silica sol with the polyethylene glycol and then add polyethylene oxide, or to pre-mix silica sol and basic aluminum chloride. The solution is pretreated with the polyethylene glycol and then polyethylene oxide is added thereto.
その際のこれら原料の使用割合についていえば、塩基性
塩化アルミニウムは、調製後の紡糸液中のＡｌ２Ｏ３換
算濃度が２８重量％以下となるような割合で使用し、シ
リカゾルは概ねこのＡｌｌ！０３１に対して１．０〜４
０．０′ｇＬ量％の範囲となるようにする。Regarding the proportions of these raw materials used in this case, basic aluminum chloride is used in such a proportion that the concentration in terms of Al2O3 in the spinning solution after preparation is 28% by weight or less, and silica sol is generally made of this All! 1.0-4 for 031
The amount should be within the range of 0.0'gL amount%.
また、ポリエチレングリコールについては、同様に塩基
性塩化アルミニウムのＡｌｅＯｓ呈に対して概ね１．０
重１％以上であり、使用する塩基性塩化アルミニウムの
塩基度が低い程、その使用量を増やすことが望ましい。Similarly, for polyethylene glycol, the AleOs expression of basic aluminum chloride is approximately 1.0.
It is 1% or more by weight, and the lower the basicity of the basic aluminum chloride used, the more desirably the amount used is increased.
更に、紡糸助剤として使用するポリエチレンオキサイド
については、紡糸の手段によっても異なるが、Ａｌ２Ｏ
３量に対して概ね０．１〜５．（ｌ量％の範囲である。Furthermore, polyethylene oxide used as a spinning aid varies depending on the spinning method, but Al2O
Approximately 0.1 to 5. (The range is 1%.
本発明に於て殊に重要な点は、ポリエチレングリコー
ルのみ、又はポリエチレンオキサイドのみの使用、或い
はポリエチレングリコール、ポリエチレンオキサイドの
分子量が前記範囲外のものでは、本発明の効果を得るこ
とができず、必ず、分子量２０，０００以下のポリエチ
レングリコールで処理した後に、分子１３００，０００
以上のポリエチレンオキサイドを加えることである。そ
れぞれの有機化合物の添加後は、適度な攪はんを行ない
、有機化合物が均一に溶解すればよい。A particularly important point in the present invention is that the effects of the present invention cannot be obtained if only polyethylene glycol or polyethylene oxide is used, or if the molecular weight of polyethylene glycol or polyethylene oxide is outside the above range. Be sure to treat with polyethylene glycol with a molecular weight of 20,000 or less before
The above is to add polyethylene oxide. After adding each organic compound, appropriate stirring may be performed to uniformly dissolve the organic compound.
前掲の従来技術に記載した如く、通常、紡糸助剤として
使用される高分子量のポリエチレンオキサイドの添加に
より、シリカとポリエチレンオキサイドどの相互作用で
紡糸原液は不均一なものとなり、多くの場合ガム状沈澱
を生成するが、本発明の方法によればポリエチレンオキ
サイドの添加後も紡糸原液は極めて均−且つ安定であり
、紡糸後の繊維強度の向上に寄与し、また紡糸液の曳糸
性に優れたものとなる。As described in the above-mentioned prior art, the addition of high molecular weight polyethylene oxide, which is usually used as a spinning aid, causes the spinning stock solution to become non-uniform due to the interaction between silica and polyethylene oxide, and in many cases results in gummy precipitates. However, according to the method of the present invention, even after the addition of polyethylene oxide, the spinning stock solution is extremely uniform and stable, contributing to improving the fiber strength after spinning, and also improving the spinnability of the spinning solution. Become something.
（実施例）
以下に本発明の実施例をあげて更に説明を行うが、本発
明はこれらに限定されるものではない。(Example) The present invention will be further explained below with reference to Examples, but the present invention is not limited thereto.
また、％は特にことわらない限り全て１ｉｆｔ％を示す
。Moreover, all percentages indicate 1if% unless otherwise specified.
実施例１
１Ｌ容のビーカーに、塩基性塩化アルミニウム（Ａ１２
０３２３．５％、塩基度８１％） ６００ｇを投入し、
次いでこれにシリカゾル（ＳｉＯａ２０．５％、触媒化
成（株）製、商品名「カタロイビ３ＭＪ ）１０３．２
ｇを攪拌下添加した。Example 1 Basic aluminum chloride (A12
0323.5%, basicity 81%) 600g was added,
Next, silica sol (SiOa 20.5%, manufactured by Catalyst Kasei Co., Ltd., trade name "Kataroibi 3MJ") 103.2
g was added under stirring.
この混合液は若干のチンダル光を放つ透明安定液であっ
た。この混合溶液に、ポリエチレングリコール（分子量
２０．Ｇｏｏ、日本油！ｉ？（株）製）４５ｇを添加溶
解した。This mixture was a transparent stable liquid that emitted some Tyndall light. To this mixed solution, 45 g of polyethylene glycol (molecular weight 20.Goo, manufactured by Nippon Oil!i? Co., Ltd.) was added and dissolved.
液が完全に透明となるまで攪拌した後、次いでこれにポ
リエチレンオキサイド（分子ｉ３，５００．Ｇｏｏ、製
鉄化学（株）製ＰＥ０−１５）を１．４１ｇ添加した。After the liquid was stirred until it became completely transparent, 1.41 g of polyethylene oxide (molecule i3,500.Goo, PE0-15 manufactured by Tetsu Seikagaku Co., Ltd.) was added thereto.
ポリエチレンオキサイドは完全に均一溶解し、何等濁り
、沈澱も生じず、透明安定な本発明の紡糸原液を得た。The polyethylene oxide was completely and uniformly dissolved, and no turbidity or precipitation occurred, yielding a transparent and stable spinning solution of the present invention.
この紡糸液の粘度は８６０ＰＳと低いにもかかわらず、
曳糸性は８２ｃｍと非常に優れていた。（曳糸性測定法
：紡糸液温度２５℃、測定棒ＳＯ３（断面積２．８ｃｍ
”）で、棒の底部を紡糸液面と接触し、棒引上げ速度１
．５ｍ／ｆｆ１ｉｎで引上げた際の曳糸長を測定）また
、この紡糸原液を濃縮操作を行わずに原液のまま遠心方
法紡糸器を用いて紡糸したところ、非常に優れた紡糸性
を示し、ショットの生成が殆ど見られない美しいウール
状の嵩高い前駆体繊維を得た。この前駆体繊維を２００
℃ハｒの昇温速度で１０００°Ｃまで昇温焼成し、更に
４００９Ｃ／ｈｒで１２５０°Ｃまで昇温した後、この
温度で３０分間保持焼成を行った。Although the viscosity of this spinning solution is as low as 860PS,
The stringability was very excellent at 82 cm. (Measurement method for stringability: spinning solution temperature 25°C, measuring rod SO3 (cross-sectional area 2.8 cm)
”), the bottom of the rod is brought into contact with the surface of the spinning solution, and the rod is pulled up at a speed of 1.
．． (Measuring the string length when pulled up at 5m/ff1in) Furthermore, when this spinning stock solution was spun using a centrifugal spinner without performing any concentration operation, it showed very excellent spinnability, and shot A beautiful wool-like bulky precursor fiber with almost no visible formation was obtained. 200% of this precursor fiber
The temperature was raised to 1000°C at a rate of 100°C/hour, and then the temperature was raised to 1250°C at a rate of 4009°C/hr, followed by holding firing at this temperature for 30 minutes.
電気炉中で自然放冷した後、取り出した繊維は、平均直
径３μｍ、＋ｎ維長数ｃｍ以上の透明感のある強靭かっ
可撓性のある繊維であった。またＸ線的にはＡｌ−３ｉ
スピネル構造を有し、紡糸液中のＡｌ２Ｏ３，５１０２
成づ♂ａ≠→動粱＃吻＝を市；が証明された。After being left to cool naturally in an electric furnace, the fibers taken out were transparent, tough, and flexible fibers with an average diameter of 3 μm and a +n fiber length of several cm or more. Also, in X-rays, Al-3i
Al2O3,5102 in the spinning solution has a spinel structure
It has been proven that the result is ♂a≠→motion 粱#吻=を市;.
更に、繊維中のショット含有率は０％であり、１６００
’０２４時間での再加熱収縮率は０．４％以下であるこ
とがら、本発明の紡糸液の使用により、高温断熱材用等
として優れた性質を有するアルミナ繊維を得ることがで
きる。Furthermore, the shot content in the fiber is 0% and 1600
Since the reheating shrinkage rate after 24 hours is 0.4% or less, by using the spinning solution of the present invention, alumina fibers having excellent properties for use in high-temperature insulation materials, etc. can be obtained.
尚、上記ショット含有率の測定はＪ Ｉ Ｓ Ｒ−３３
１１（セラミックブランケット）（５，４ショット含有
率試験法）に基づき行ない、また再加熱数１ｉ１′４ｔ
、の測定は、同Ｒ−３３１１（５，５加熱線収縮率試験
法）に基づき行なった。In addition, the measurement of the above-mentioned shot content rate was carried out in accordance with JIS R-33.
11 (ceramic blanket) (5,4 shot content test method), and reheating number 1i1'4t
, was measured based on R-3311 (5,5 heating linear shrinkage rate test method).
比較例１
実施例１と同様に、ＩＬ容ビーカーに塩基性塩化アルミ
ニウム６０９ｇを入れ、更にシリカゾル１０３．２［を
攪拌下に添加分ｔｔｔさゼた。この混合溶液にポリエチ
レンオキサイド（前記ＰＥ０−１５）を１４１ＪＦ添加
し、攪拌溶解を行なった。Comparative Example 1 In the same manner as in Example 1, 609 g of basic aluminum chloride was placed in an IL-capacity beaker, and 103.2 g of silica sol was added thereto while stirring. To this mixed solution, 141 JF of polyethylene oxide (PE0-15) was added and dissolved with stirring.
しかし、この溶液はポリエチレンオキサイド添加直後よ
り濁り始め、１０分後にはガノ、状沈澱を生成し、完全
に固液分離状態となった。またその化学分析の結果では
、沈澱物はシリカとポリエチレンオキサイドが主体であ
り、溶液はアルミ分が主体で、溶液中にシリカ分は殆ど
定量されず、シリカゾルとポリエチレンオキサイドとの
反応性の高さが実証された。However, this solution began to become cloudy immediately after the addition of polyethylene oxide, and after 10 minutes, a gunk-like precipitate was formed, resulting in complete solid-liquid separation. In addition, the chemical analysis results showed that the precipitate was mainly composed of silica and polyethylene oxide, the solution was mainly aluminum, and the silica content was hardly quantified in the solution, indicating the high reactivity between silica sol and polyethylene oxide. has been proven.
当然ながら、上記紡糸液からは均一組成の繊維は製造出
来なかった。Naturally, fibers of uniform composition could not be produced from the above spinning solution.
実施例２
１Ｌ容ビーカーに塩基性塩化アルミニウム（＾１ ｅｏ
ｓ２３．５％、塩基度８１％） ９００ｇを投入し、次
いでこれにシリカゾル（ＳｉＯｅ２０．５％、日産化学
工業（株）製。Example 2 Basic aluminum chloride (^1 eo
s23.5%, basicity 81%), and then added 900 g of silica sol (SiOe20.5%, manufactured by Nissan Chemical Industries, Ltd.).
商品名「スノーテックス−０Ｊ）１５４．８ｇを攪拌下
に添加した。154.8 g of "Snowtex-0J" (trade name) was added under stirring.
この混合液を１００履ｌ容ビーカーに各々１００ｇづつ
分取し、第１表に示した分子量の異なるポリエチレング
リコールを所定量添加、溶解させた後、ポリエチレンオ
キサイド（分子量２，０００，０００、製鉄化学（株）
製ＰＥ０−８）を０．２ｇ添加し、その溶液状態を観察
した。結果を第１表に示した。100 g each of this mixed solution was placed in a 100-l capacity beaker, and after adding and dissolving a predetermined amount of polyethylene glycol with different molecular weights shown in Table 1, polyethylene oxide (molecular weight 2,000,000, (KK)
0.2 g of PE0-8) was added, and the state of the solution was observed. The results are shown in Table 1.
第１表の結果から、分子量２０，０００以下のポリエチ
レングリコールの使用により、シリカゾルとポ第１表
リエチレンオキサイドとの反応が抑止されることが明ら
かである。From the results in Table 1, it is clear that the reaction between silica sol and polyethylene oxide in Table 1 is suppressed by using polyethylene glycol having a molecular weight of 20,000 or less.
次いで、第１表の試料Ｎｏ、４．６．１３．１０と同一
組成液を更に５００ｇづつ調製し、これを実施例１と同
様に紡糸、焼成を行った。その結果を第２表に示した。Next, 500 g of a solution having the same composition as Sample No. 4.6.13.10 in Table 1 was prepared, and the same solution was spun and fired in the same manner as in Example 1. The results are shown in Table 2.
第２表の結果からも、分子量２０，０００以下のポリエ
チレングリコールを使用する紡糸液がアルミナ繊維とし
て優れた性能を供与することが明らかである。It is clear from the results in Table 2 that spinning solutions using polyethylene glycol with a molecular weight of 20,000 or less provide excellent performance as alumina fibers.
第２表
ゝ＼１、
実施例２と同様に調製した塩基性塩化アルミニウムーシ
リカゾル混合液１００ｇに、ポリエチレングリコール（
分子１１２０，０００）５ｇと、ポリエチレンオキサイ
ド（前記ＰＥ０−８）０．２ｇを同時に添加溶解させた
ところ、混合液は沈澱を生成した。Table 2 ＼1, Polyethylene glycol (
When 5 g of polyethylene oxide (PE0-8) and 0.2 g of polyethylene oxide (PE0-8) were simultaneously added and dissolved, a precipitate was formed in the mixture.
比較例３
実施例２と同様に調製した塩基性塩化アルミニウムーシ
リカゾル混合液ＩＱＯｇに、ポリエチレンオキサイド（
前記ＰＥ０−１３）０．２ｇを添加、溶解させたが、液
は白色沈澱を生じた。２時間の攪拌の後、ポリエチレン
グリコール（分子ｉ２０．Ｇｏｏ）５ｇを添加溶解させ
たが、白色沈澱に変化は生じなかった。Comparative Example 3 Polyethylene oxide (
0.2 g of PE0-13) was added and dissolved, but a white precipitate formed in the liquid. After stirring for 2 hours, 5 g of polyethylene glycol (molecule i20.Goo) was added and dissolved, but no change occurred in the white precipitate.
Claims (1)
アルミナ繊維の製造に於て、シリカゾル又はシリカゾル
と塩基性塩化アルミニウムとの混合液を、分子量２０，
０００以下のポリエチレングリコールで前処理した後、
次いで分子量３００，０００以上のポリエチレンオキサ
イドを紡糸助剤として使用することを特徴とするアルミ
ナ繊維紡糸原液の調製法。In the production of alumina fibers whose main raw materials are basic aluminum chloride and silica sol, silica sol or a mixture of silica sol and basic aluminum chloride is mixed with a molecular weight of 20,
After pretreatment with polyethylene glycol below 000,
Next, a method for preparing an alumina fiber spinning dope, characterized in that polyethylene oxide having a molecular weight of 300,000 or more is used as a spinning aid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61232165A JPS6385115A (en) | 1986-09-29 | 1986-09-29 | Preparation of stock solution for spinning alumina fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61232165A JPS6385115A (en) | 1986-09-29 | 1986-09-29 | Preparation of stock solution for spinning alumina fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6385115A true JPS6385115A (en) | 1988-04-15 |
| JPH0143046B2 JPH0143046B2 (en) | 1989-09-18 |
Family
ID=16935013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61232165A Granted JPS6385115A (en) | 1986-09-29 | 1986-09-29 | Preparation of stock solution for spinning alumina fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6385115A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1182006A (en) * | 1997-09-12 | 1999-03-26 | Denki Kagaku Kogyo Kk | Heat insulative sealant and its use |
| JP2005344257A (en) * | 2004-06-07 | 2005-12-15 | Denki Kagaku Kogyo Kk | Aluminous fiber, method for producing the same and use |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6335827A (en) * | 1986-07-24 | 1988-02-16 | Taki Chem Co Ltd | Production of spinning solution for alumina fiber |
-
1986
- 1986-09-29 JP JP61232165A patent/JPS6385115A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6335827A (en) * | 1986-07-24 | 1988-02-16 | Taki Chem Co Ltd | Production of spinning solution for alumina fiber |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1182006A (en) * | 1997-09-12 | 1999-03-26 | Denki Kagaku Kogyo Kk | Heat insulative sealant and its use |
| JP2005344257A (en) * | 2004-06-07 | 2005-12-15 | Denki Kagaku Kogyo Kk | Aluminous fiber, method for producing the same and use |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0143046B2 (en) | 1989-09-18 |
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