JPS644979B2 - - Google Patents
Info
- Publication number
- JPS644979B2 JPS644979B2 JP59040520A JP4052084A JPS644979B2 JP S644979 B2 JPS644979 B2 JP S644979B2 JP 59040520 A JP59040520 A JP 59040520A JP 4052084 A JP4052084 A JP 4052084A JP S644979 B2 JPS644979 B2 JP S644979B2
- Authority
- JP
- Japan
- Prior art keywords
- fibers
- alginate
- solution
- alumina
- silica
- 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
Links
- 239000000835 fiber Substances 0.000 claims description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 235000010443 alginic acid Nutrition 0.000 claims description 15
- 229920000615 alginic acid Polymers 0.000 claims description 15
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 14
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 14
- 229940072056 alginate Drugs 0.000 claims description 14
- 239000000661 sodium alginate Substances 0.000 claims description 14
- 235000010413 sodium alginate Nutrition 0.000 claims description 14
- 229940005550 sodium alginate Drugs 0.000 claims description 14
- 239000000919 ceramic Substances 0.000 claims description 11
- 239000011651 chromium Substances 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000005342 ion exchange Methods 0.000 claims description 5
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 150000001844 chromium Chemical class 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 11
- 238000010304 firing Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 238000009987 spinning Methods 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Fibers (AREA)
Description
【発明の詳細な説明】
本発明はセラミツク繊維または膜の製造法、更
に詳しくはアルギン酸ナトリウムを用いてアルミ
ナ−シリカ系セラミツク繊維または膜を製造する
方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing ceramic fibers or membranes, and more particularly to a method for producing alumina-silica ceramic fibers or membranes using sodium alginate.
従来のセラミツク繊維の製造法としては、例え
ば、アルミナ−シリカ系繊維の製造においては、
アルミナとシリカを混合し、この混合物を溶融
し、圧さく空気あるいは遠心力によつて吹きとば
す方法が行われている。この方法で得られる繊維
は短繊維のみで長繊維及び膜状物は得られず、ま
た繊維径も不揃いで均一径の繊維が得られない欠
点があつた。 Conventional ceramic fiber manufacturing methods include, for example, alumina-silica fiber manufacturing methods.
The method used is to mix alumina and silica, melt the mixture, and blow it away using compressed air or centrifugal force. The fibers obtained by this method are only short fibers, not long fibers or membrane-like materials, and the fiber diameters are also irregular, making it impossible to obtain fibers with a uniform diameter.
本発明は従来法のセラミツク繊維の製造法にお
ける欠点を解消せんとするもので、その目的は長
繊維及び膜状物も容易に製造することができ、ま
た繊維の径及び膜状物の厚さも均一でかつ所望径
の高強度のアルミナ−シリカ系セラミツク製品を
容易に製造することができる方法を提供するにあ
る。 The present invention aims to solve the drawbacks of the conventional method for producing ceramic fibers, and its purpose is to easily produce long fibers and film-like products, and to reduce the diameter of the fibers and the thickness of the film-like products. The object of the present invention is to provide a method for easily manufacturing alumina-silica ceramic products that are uniform, have a desired diameter, and have high strength.
本発明はアルギン酸ナトリウムを用いて従来法
における欠点を解消し得たものである。 The present invention uses sodium alginate to overcome the drawbacks of conventional methods.
従来、アルギン酸ナトリウム溶液を金属塩溶液
中に紡糸してアルギン酸金属塩繊維を製造する方
法、またアルギン酸ナトリウム溶液を酸溶液中に
紡糸してアルギン酸繊維を作り、これを金属塩溶
液中に浸し、アルギン酸金属塩繊維を作ることは
知られている。 Conventionally, alginate metal salt fibers are produced by spinning a sodium alginate solution into a metal salt solution, and alginate fibers are produced by spinning a sodium alginate solution into an acid solution, and then immersed in a metal salt solution to produce alginate metal salt fibers. It is known to make metal salt fibers.
本発明者はアルギン酸ナトリウムのこの特性を
利用して、アルミナ−シリカ系セラミツク繊維を
製造すべく鋭意研究の結果、(1)アルギン酸ナトリ
ウムのイオン交換反応によつて直接シリカを吸着
させることができないが、これに水ガラスを混合
すると、水ガラス中のSiO2の成分はアルギン酸
ポリマーに強固に結合され、この混合液を紡糸浴
中に紡糸して繊維を作り、これをアルミニウム塩
とクロム塩の混合溶液に浸した後焼成するとシリ
カ成分はアルミナと反応してアルミナ−シリカセ
ラミツク繊維が得られること。(2)紡糸浴として酸
にアルコールを添加した液を使用すると、ゲル化
反応が促進され、強固なケイ酸混合アルギン酸繊
維が得られること。(3)前記Alイオンと共に吸着
したCrイオンは焼成時のムライトの結晶成長に
よる強度劣化を抑制し得られること。(4)アルギン
酸金属塩を直接焼成すると空孔を生ずるが、その
前に減圧焼成すると空孔が生ずることなく高強度
のものが得られることを究明し、この知見に基い
て本発明を完成した。 The present inventor has conducted extensive research to utilize this property of sodium alginate to produce alumina-silica ceramic fibers, and has found that (1) silica cannot be directly adsorbed by the ion exchange reaction of sodium alginate; When water glass is mixed with this, the SiO 2 component in the water glass is firmly bound to the alginate polymer, and this mixture is spun into a spinning bath to make fibers, which are then mixed with aluminum salts and chromium salts. When calcined after soaking in a solution, the silica component reacts with alumina to obtain alumina-silica ceramic fibers. (2) When a solution prepared by adding alcohol to acid is used as a spinning bath, the gelation reaction is promoted and strong silicic acid-mixed alginate fibers can be obtained. (3) The Cr ions adsorbed together with the Al ions can suppress deterioration in strength due to crystal growth of mullite during firing. (4) It was discovered that when alginate metal salts are directly fired, pores are created, but if the alginate metal salts are fired under reduced pressure before that, high strength products can be obtained without the formation of pores, and based on this knowledge, the present invention was completed. .
本発明の要旨はアルギン酸ナトリウム溶液中に
水ガラスを混合した液を、酸にアルコールを混合
した液中に紡出してシリカ成分を含有するアルギ
ン酸繊維または膜を形成し、これをアルミニウム
塩とクロム塩の混合溶液に浸し、イオン交換反応
によつてAl、Crイオンを吸着せ、減圧下で焼成
した後、更に空気中で焼成することを特徴とする
アルミナ−シリカ系セラミツク繊維または膜の製
造法にある。 The gist of the present invention is to spin a solution of sodium alginate mixed with water glass into a solution of acid and alcohol to form alginate fibers or membranes containing silica components, and to form alginate fibers or membranes containing aluminum salts and chromium salts. A process for producing alumina-silica ceramic fibers or membranes, which is characterized by soaking the fibers in a mixed solution of the above, adsorbing Al and Cr ions through an ion-exchange reaction, firing them under reduced pressure, and then firing them in air. be.
原料のアルギン酸ナトリウム溶液の濃度は、３
〜５％（重量）であることが好ましい。これによ
り薄くなると紡糸して得られる繊維が柔く取扱い
にくくなり、他方濃くなると、有機成分が多くな
り、焼成後に気孔が多く残る欠点が生ずる。 The concentration of the raw material sodium alginate solution is 3
It is preferably 5% (by weight). As a result, when the fiber becomes thin, the resulting fiber becomes soft and difficult to handle, while when the fiber becomes thick, the organic component increases, resulting in the disadvantage that many pores remain after firing.
アルギン酸ナトリウム溶液に添加する水ガラス
量はアルギン酸ナトリウム／水ガラスが重量比で
約4.5の値になるように混合する。この量添加す
ると、水ガラス中のSiO2の量が約２％が多量の
水洗によつても残留し、強固にアルギン酸ポリマ
ーと均一に結合される。 The amount of water glass added to the sodium alginate solution is mixed so that the weight ratio of sodium alginate/water glass is about 4.5. When this amount is added, approximately 2% of SiO 2 in the water glass remains even after washing with a large amount of water, and is strongly and uniformly bonded to the alginate polymer.
この混合液を紡出する液はアルギン酸ナトリウ
ムを凝固させる酸、例えば塩酸、酢酸、硫酸が挙
げられるが、塩酸が好ましい。これにアルコー
ル、例えばエタノールを0.5％添加すると、ゲル
化反応が促進され、取扱い易い強度を持つたケイ
酸混合アルギン酸繊維が得られる。紡糸浴の温度
は10〜40℃、好ましくは20〜30℃である。40℃を
超えると繊維が膨潤して切れ易くなり、10℃以下
となるとイオン交換反応に時間がかかるので、前
記の温度範囲が適当である。 The liquid used to spin this mixture may be an acid that coagulates sodium alginate, such as hydrochloric acid, acetic acid, or sulfuric acid, but hydrochloric acid is preferred. When 0.5% of alcohol, for example ethanol, is added to this, the gelation reaction is promoted and silicic acid-mixed alginate fibers with strength that are easy to handle are obtained. The temperature of the spinning bath is 10-40°C, preferably 20-30°C. If the temperature exceeds 40°C, the fibers will swell and break easily, and if the temperature falls below 10°C, the ion exchange reaction will take time, so the above temperature range is appropriate.
紡糸して得られたシリカ成分を含有したアルギ
ン酸繊維をアルミニウム塩例えばAl（NO3）3とク
ロム塩例えばCr（NO3）3の混合溶液に浸し、イオ
ン交換反応によつてAl、Crイオンを吸着させる
が、ムライトの結晶成長の抑制に有効なCr量は
Cr2O3として約４％であつた。得られた繊維を減
圧下例えば0.1〜１mmHg圧の下で800〜900℃で約
２時間焼成する。これによりアルギン酸は燃焼さ
れると同時にSiO2とAl2O3が反応してアルミナ−
シリカ系セラミツクが生成される。この焼成を減
圧下で行うとCrイオンの存在によつて、焼成時
にムライトの結晶成長が抑制され、更に減圧焼成
は有機物の焼燃による空孔の除去に役立ち空孔が
なく高強度の繊維が得られる。 Alginate fibers containing silica components obtained by spinning are immersed in a mixed solution of aluminum salts such as Al(NO 3 ) 3 and chromium salts such as Cr(NO 3 ) 3 to remove Al and Cr ions through an ion exchange reaction. The amount of Cr that is effective in suppressing mullite crystal growth is
It was approximately 4% as Cr 2 O 3 . The resulting fibers are fired at 800-900° C. for about 2 hours under reduced pressure, e.g., 0.1-1 mmHg. As a result, alginic acid is burned and at the same time SiO 2 and Al 2 O 3 react to form alumina.
Silica-based ceramic is produced. When this firing is performed under reduced pressure, the presence of Cr ions suppresses the crystal growth of mullite during firing, and furthermore, reduced pressure firing helps to remove pores caused by combustion of organic matter and produces high-strength fibers without pores. can get.
次に空気中で800〜900℃で約30分間焼成するこ
とにより、有機物の燃焼によつて表面にできてい
るカーボンを除去する。 Next, carbon formed on the surface due to combustion of organic matter is removed by firing in air at 800-900°C for about 30 minutes.
以上繊維の製造法について記載したが、紡糸に
代え膜状物とすることにより同様にして膜が得ら
れる。 Although the method for producing fibers has been described above, a membrane can be obtained in the same manner by forming a membrane material instead of spinning.
実施例 １
５％アルギン酸ナトリウム溶液に水ガラスをア
ルギン酸ナトリウム／水ガラスが4.5重量％に混
合し、この混合液を4NHClにエチルアルコール
５％添加した液中に紡糸してゲル状ケイ酸混合ア
ルギン酸繊維を作つた。この繊維を水洗後、室温
で２時間乾燥し、0.2N、Al（NO3）3と1N、Cr
（NO3）3の混合液中に20分間浸した。これを水洗
して室温で乾燥し、１mmHgの減圧下で900℃で２
時間焼成した後、900℃で30分間空気中で焼成し
た。アルミナ−シリカ系セラミツク繊維が得られ
た。Example 1 Water glass was mixed in a 5% sodium alginate solution at a concentration of 4.5% by weight of sodium alginate/water glass, and this mixed solution was spun into a solution containing 4NHCl and 5% ethyl alcohol to produce gelled silicic acid mixed alginate fibers. I made it. After washing this fiber with water, it was dried at room temperature for 2 hours, and 0.2N, Al(NO 3 ) 3 and 1N, Cr
(NO 3 ) 3 for 20 minutes. This was washed with water, dried at room temperature, and heated to 900°C under a reduced pressure of 1 mmHg for 2 hours.
After baking for an hour, it was baked in air at 900°C for 30 minutes. Alumina-silica ceramic fibers were obtained.
以上のように、本発明の方法によると、従来法
では得られなかつた長繊維及び膜も容易に得ら
れ、また少量のCrの添加により焼成に際してム
ライトの結晶の生長を抑制し、及び減圧焼成によ
る空孔の除去を行い得られるため、極めて高強度
のアルミナ−シリカ系繊維及び膜を製造すること
ができる優れた効果を奏し得られる。 As described above, according to the method of the present invention, long fibers and films that could not be obtained by conventional methods can be easily obtained, and the addition of a small amount of Cr suppresses the growth of mullite crystals during firing, and Since the pores can be removed by removing the pores, it is possible to produce extremely high-strength alumina-silica fibers and membranes, which is an excellent effect.
Claims (1)
した液を、酸にアルコールを混合した液中に紡出
してシリカ成分を含有するアルギン酸繊維または
膜を形成し、これをアルミニウム塩とクロム塩の
混合液に浸し、更にイオン交換反応によつてAl、
Crイオンを吸着させ、減圧下で焼成した後、更
に空気中で焼成することを特徴とするアルミナ−
シリカ系セラミツク繊維または膜の製造法。1 Spun a mixture of sodium alginate solution and water glass into a mixture of acid and alcohol to form alginate fibers or membranes containing silica components, and then soak this in a mixture of aluminum salts and chromium salts. , further by ion exchange reaction, Al,
Alumina that adsorbs Cr ions, is fired under reduced pressure, and then fired in air.
A method for producing silica-based ceramic fibers or membranes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59040520A JPS60186459A (en) | 1984-03-05 | 1984-03-05 | Manufacture of alumina-silica ceramic fiber or film using sodium alginate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59040520A JPS60186459A (en) | 1984-03-05 | 1984-03-05 | Manufacture of alumina-silica ceramic fiber or film using sodium alginate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60186459A JPS60186459A (en) | 1985-09-21 |
| JPS644979B2 true JPS644979B2 (en) | 1989-01-27 |
Family
ID=12582784
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59040520A Granted JPS60186459A (en) | 1984-03-05 | 1984-03-05 | Manufacture of alumina-silica ceramic fiber or film using sodium alginate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60186459A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH062930U (en) * | 1992-06-04 | 1994-01-14 | 三井石化エンジニアリング株式会社 | Support for electrical wiring protection tube |
| US11605079B2 (en) * | 2019-03-29 | 2023-03-14 | VocaLink Limited | Method, apparatus and computer program for transaction destination verification |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04243958A (en) * | 1991-01-31 | 1992-09-01 | Sekisui Plastics Co Ltd | Production of self-supporting alumina film |
| JP4252054B2 (en) * | 2005-09-06 | 2009-04-08 | 蛯名 堅悟 | Method for forming superconducting ceramic thin film |
-
1984
- 1984-03-05 JP JP59040520A patent/JPS60186459A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH062930U (en) * | 1992-06-04 | 1994-01-14 | 三井石化エンジニアリング株式会社 | Support for electrical wiring protection tube |
| US11605079B2 (en) * | 2019-03-29 | 2023-03-14 | VocaLink Limited | Method, apparatus and computer program for transaction destination verification |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60186459A (en) | 1985-09-21 |
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