JPS62297237A - Spinning dope - Google Patents
Spinning dopeInfo
- Publication number
- JPS62297237A JPS62297237A JP13924486A JP13924486A JPS62297237A JP S62297237 A JPS62297237 A JP S62297237A JP 13924486 A JP13924486 A JP 13924486A JP 13924486 A JP13924486 A JP 13924486A JP S62297237 A JPS62297237 A JP S62297237A
- Authority
- JP
- Japan
- Prior art keywords
- silica sol
- compound
- group
- spinning
- spinning solution
- 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 29
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000001875 compounds Chemical class 0.000 claims abstract description 23
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 12
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 5
- 125000003118 aryl group Chemical group 0.000 claims abstract description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 10
- 238000006116 polymerization reaction Methods 0.000 abstract description 9
- 238000001879 gelation Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000003763 carbonization Methods 0.000 abstract description 3
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000002845 discoloration Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000003377 acid catalyst Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- XQMTUIZTZJXUFM-UHFFFAOYSA-N tetraethoxy silicate Chemical compound CCOO[Si](OOCC)(OOCC)OOCC XQMTUIZTZJXUFM-UHFFFAOYSA-N 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 description 1
- -1 A11yl group Chemical group 0.000 description 1
- 241000880298 Baculum Species 0.000 description 1
- 101100203596 Caenorhabditis elegans sol-1 gene Proteins 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/011—Manufacture of glass fibres or filaments starting from a liquid phase reaction process, e.g. through a gel phase
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
- Inorganic Fibers (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
Description
【発明の詳細な説明】
３、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よってシリカファイバーを製造す
るために用いられる紡糸液に関するものである。Detailed Description of the Invention 3. Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a spinning solution used for producing silica fibers by a sol-gel method.
［従来の技術］
シリカファイア＜−（ＳｉＱ２ファイバー）をゾルゲル
法で製造することが近時知られるようになった。このた
めに用いられるシリカゾルを主体とする紡糸液は、テト
ラメトキシシリケート、テトラエトキシシリケートのよ
うなＳｉアルコキシドを塩酸のような酸触媒の存在下に
アルコール中で加水分解、縮合を行ない、適当な濃度迄
ｃｉｌｉｉすることによって好適に製造することができ
る。[Prior Art] It has recently become known to produce silica fire <- (SiQ2 fiber) by a sol-gel method. The spinning solution mainly composed of silica sol used for this purpose is produced by hydrolyzing and condensing Si alkoxides such as tetramethoxysilicate and tetraethoxysilicate in alcohol in the presence of an acid catalyst such as hydrochloric acid to obtain an appropriate concentration. It can be suitably produced by carrying out the following steps.
シリカゾルは常温で放置すると加水分解、重合が進行し
、重合度とともに粘度が次第に増加する傾向を有する。When silica sol is left at room temperature, hydrolysis and polymerization progress, and the viscosity tends to gradually increase with the degree of polymerization.
紡糸液に曳糸性を生じさせるためには、シリカゾルの濃
度をＳ ｉ０２として３５〜５０ｗｔ％程度とする必要
があるが、このような濃度においては、粘度の増大、ゲ
ル化速度の急激な増大により、長時間安定した紡糸を行
なうことが困難となり、又シリカファイバーの太さを一
定に保ち、或は細いシリカファイバーを製造することが
困難である。In order to produce stringiness in the spinning solution, the concentration of silica sol needs to be approximately 35 to 50 wt% as Si02, but at such a concentration, the viscosity increases and the gelation rate rapidly increases. This makes it difficult to perform stable spinning over a long period of time, and it is also difficult to maintain a constant thickness of silica fibers or to produce thin silica fibers.
さらに、従来の紡糸液を用いた場合、乾燥性が悪く、こ
のため紡糸装置に用いられるチムニ−の温度を大とした
り、紡糸用ノズルと捲取機の距離を大とする必要がある
。或いは又、紡糸によって得られたシリカゲルよりなる
ファイバーを焼成してシリカファイバーとする際、炭化
によって黒化を生じ易い欠点がある。Furthermore, when conventional spinning solutions are used, drying properties are poor, and therefore it is necessary to increase the temperature of the chimney used in the spinning device or to increase the distance between the spinning nozzle and the winding machine. Alternatively, when fibers made of silica gel obtained by spinning are fired to produce silica fibers, there is a drawback that blackening is likely to occur due to carbonization.
［発明の解決しようとする問題点］
本発明は、従来技術が有していた前述の欠点を解消する
ことを目的とするものである。[Problems to be Solved by the Invention] The present invention aims to eliminate the above-mentioned drawbacks of the prior art.
［問題点を解決するための手段］
本発明は、前述の問題点を解決すべくなされたものであ
り、シリカゾルに一般式Ｙｌ （Ｙ２ ） （Ｙ３ ）
ＳｉＸで表わされるＳｉ化合物を添加したことを特徴と
する紡糸液を提供するものである。[Means for Solving the Problems] The present invention has been made to solve the above-mentioned problems.
The present invention provides a spinning solution characterized by adding a Si compound represented by SiX.
ここに、Ｙｌ 、Ｙ２ 、Ｙ３ ：アルキル（Ａｌｋｙ
ｌ）基、アリル（Ａｌｌｙｌ）基又はア
リール（Ａｒ７１）基。Here, Yl, Y2, Y3: Alkyl
l) group, allyl group or aryl (Ar71) group.
Ｘ ： Ｈ，ＣＩ、Ｏｒ、Ｉ、ＯＨ基又は０Ｒ（Ｒ
は炭素数１−１０のアルキル基）
である。X: H, CI, Or, I, OH group or 0R (R
is an alkyl group having 1 to 10 carbon atoms).
次に本発明を更に具体的に説明する。Next, the present invention will be explained in more detail.
本発明に使用するシリカゾルの製法に特に限定はなく、
テトラメトキシシリケート、テトラエトキシシリケート
のようなＳｉアルコキシドを常法に従い、塩酸のような
酸触媒の存在下に、メチルアルコール、エチルアルコー
ルのような低級アルコール中で加水分解、縮合を行ない
、適当な濃度迄濃縮することによって製造したものを用
いるのが適ちである。There is no particular limitation on the manufacturing method of the silica sol used in the present invention,
A Si alkoxide such as tetramethoxysilicate or tetraethoxysilicate is hydrolyzed and condensed in a lower alcohol such as methyl alcohol or ethyl alcohol in the presence of an acid catalyst such as hydrochloric acid according to a conventional method to obtain an appropriate concentration. It is appropriate to use a product produced by concentrating to a certain extent.
シリカゾル中に一般式Ｙｌ （Ｙ２ ） （Ｙ３ ）Ｓ
ｉＸで表わされる１ ３個の有機官能基Ｙｌ ｌＹ２
、Ｙ３と１個の加水分解基Ｘとを有するＳｉ化合物（
以下本Ｓｉ化合物という）を添加する。General formula Yl (Y2) (Y3)S in silica sol
1 3 organic functional groups Yl lY2 represented by iX
, a Si compound having Y3 and one hydrolyzable group X (
(hereinafter referred to as the present Si compound) is added.
Ｙｌ 、Ｙ２ 、Ｙ３ トＬ テはＣＨ３−、Ｃ２Ｈ５
−、Ｃ３Ｈ７−。Yl , Y2 , Y3 te is CH3-, C2H5
-, C3H7-.
Ｃ８Ｈ１７−等のアルキル（Ａｌｋｙｌ）基、Ｃ２Ｈａ
−等のアリル（Ａｌｌｙｌ）基、
等のアリール（Ａｒｙｌ）基を用いることができる。Alkyl groups such as C8H17-, C2Ha
Allyl groups such as - and Aryl groups such as these can be used.
Ａｌｋｙｌ基、Ａ１１ｙｌ基、 Ａｒｙｌ基はこれらの
誘導体も含むものである。なお、ｙ＋ 、Ｙ２．Ｙ３は
互いに異なる基であってもよく、或いはそのうち２っ又
は３つが同一の基であってもよい。又、Ｙｌ。The Alkyl group, A11yl group, and Aryl group also include derivatives thereof. Note that y+, Y2. Y3 may be different groups, or two or three of them may be the same group. Also, Yl.
Ｙ２＋Ｙ３ として炭素数１〜４のＡｌｋｙｌ基、或い
はＰｈｅｎｙ ｌ基を用いた場合特に好適な結果をうる
ことができる。 ＹＩ、 Ｙ２． Ｙ３の有する炭素数
は２０以下とするのが適当である。 Ａｌｋｙｌ基、
Ａ１１ｙ１基としては側鎖を有するもの、或いは環式化
合物も使用できる。Particularly favorable results can be obtained when an Alkyl group having 1 to 4 carbon atoms or a Phenyl group is used as Y2+Y3. YI, Y2. It is appropriate that Y3 has 20 or less carbon atoms. Alkyl group,
As the A11y1 group, one having a side chain or a cyclic compound can also be used.
ＸとしてはＨ、Ｃｌ、Ｂｒ、Ｉ、ＯＨ基又は０Ｒ（Ｒは
炭素数１−１０のＡｌｋｙｌ基）が使用できる。Ｒは側
鎖を有するものであってもよく、具体的にはＣＨ３−、
Ｃ２Ｈ５−、Ｃ３Ｈｚ−、ＣａＨｑ−、ＣａＨ＋ ７−
等を挙げることができ、特に炭素数１〜６のものが好ま
しい、シリカゾル中に本Ｓｉ化合物を添加する。添加方
法としては、Ｓｉアルコキシドを加水分解縮合させ、所
望の粘度（重合度）に達した時に溶剤アセトン、トルエ
ン、ヘキサン、エチルアルコール又はメチルアルコール
に溶解させたＳｉ化合物（Ｃ度：４０〜９０ｗｔ％）を
添加する方法や、直接Ｓｉ化合物を添加し攪拌する等の
方法をとることができる。As X, H, Cl, Br, I, an OH group or 0R (R is an Alkyl group having 1 to 10 carbon atoms) can be used. R may have a side chain, specifically CH3-,
C2H5-, C3Hz-, CaHq-, CaH+ 7-
The present Si compound is added to a silica sol, which is particularly preferably a silica sol having 1 to 6 carbon atoms. The addition method is to hydrolyze and condense Si alkoxide, and when the desired viscosity (degree of polymerization) is reached, add a Si compound (C degree: 40 to 90 wt%) dissolved in a solvent such as acetone, toluene, hexane, ethyl alcohol, or methyl alcohol. ), or directly adding a Si compound and stirring.
本Ｓｉ化合物の添加量は、本Ｓｉ化合物中に含まれるＳ
ｉの量とシリカゾル中に含まれるＳｉのモル比が０８０
１〜２．５、好ましくは０．０５〜０．８の範囲となる
よう定めるのが適当である０本Ｓｉ化合物の添加量があ
まり小さいと効果が充分でなく、又添加量があまり大き
いと紡糸後のゲル化が生じ難しくなる傾向を有する他、
下記の問題点を考慮し、上述の範囲を定めた。The amount of addition of the present Si compound is the amount of S contained in the present Si compound.
The amount of i and the molar ratio of Si contained in the silica sol are 080
It is appropriate to set it in the range of 1 to 2.5, preferably 0.05 to 0.8. If the amount of Si compound added is too small, the effect will not be sufficient, and if the amount added is too large, the effect will not be sufficient. In addition to the tendency for gelation to occur after spinning,
The above scope was determined by considering the following issues.
本Ｓｉ化合物を添加することにより、シリカゾルの重合
速度が小となり、粘度の増大速度、ゲル化速度が小とな
る。このため安定した紡糸作業が可能となり、得られる
繊維径のバラツキも小となるが、同時に曳糸性を生じさ
せるのに必要な重合度に到達するのに要する時間も大と
なる。又本Ｓｉ化合物の添加量が大となる程ポットライ
フも大となるので、所望のポットライフが得られるよう
、本Ｓｉ化合物の添加量を定め、又シリカゾルの貯蔵期
間、本Ｓｉ化合物の添加量等を考慮し、本Ｓｉ化合物を
添加すべきシリカゾルの重合度を定める。例えば添加量
が大きい場合にはシリカゾルの重合度を大とし、又添加
量が小さく、使用化の貯蔵時間の大きいときは重合度の
小さいシリカゾルに本Ｓｉ化合物を添加し。By adding the present Si compound, the polymerization rate of the silica sol decreases, and the viscosity increase rate and gelation rate decrease. This makes it possible to perform a stable spinning operation and reduce the variation in the diameter of the obtained fibers, but at the same time the time required to reach the degree of polymerization required to produce stringiness becomes long. Also, the larger the amount of the Si compound added, the longer the pot life will be, so the amount of the Si compound added is determined to obtain the desired pot life, and the storage period of the silica sol and the amount of the Si compound added are determined. Taking these into consideration, the degree of polymerization of the silica sol to which the present Si compound is to be added is determined. For example, when the amount added is large, the degree of polymerization of the silica sol is increased, and when the amount added is small and the storage time before use is long, the present Si compound is added to the silica sol with a low degree of polymerization.
貯蔵期間中にシリカゾルを所望の程度迄重合させること
ができ、これらの条件は実験的に容易に定めることがで
きる。なお紡糸方法は特に限定はなく、従来の紡糸法を
採用できる。The silica sol can be polymerized to the desired extent during storage, and these conditions can be easily determined experimentally. Note that the spinning method is not particularly limited, and conventional spinning methods can be employed.
［作用］
本Ｓｉ化合物は１個の加水分解基と３個の有機官能基を
有しているので、シリカゾルを構成するＳｉ骨格の末端
と本Ｓｉ化合物が反応し、該末端が３個の有機官能基を
有するＳｉで封鎖され、反応性を失う０本Ｓｉ化合物に
含まれるＳｉの量とシリカゾル中に含まれるＳｉの量の
モル比が０．０１〜２．５好ましくは０．０５〜０．８
の範囲に定められているため、Ｓｉ骨格の末端はその一
部のみが封鎖される。このためシリカゾルの反応性が抑
えられるが紡糸後のゲル化性が失われることはない。[Function] Since the present Si compound has one hydrolyzable group and three organic functional groups, the terminal of the Si skeleton constituting the silica sol reacts with the present Si compound, and the terminal reacts with the three organic functional groups. The molar ratio between the amount of Si contained in the Si compound and the amount of Si contained in the silica sol is 0.01 to 2.5, preferably 0.05 to 0. .8
Therefore, only a portion of the terminal end of the Si skeleton is blocked. Therefore, the reactivity of the silica sol is suppressed, but the gelation property after spinning is not lost.
［実施例］
５ｉ（Ｃ２Ｈ５０）ａ ４７．４重量部を０２Ｈ５０Ｈ
４９，５重量部、ＭＣＩ ０．３重量部、 Ｈ２Ｏ８重
量部よりなる液中に攪拌しつつ加え、７０℃で２日間攪
拌を続けた。ついでロータリーバキュラムエバポレータ
ーで５℃に保ち、上記組成液を４０重量部となる迄濃縮
した。所要時間は２時間で、得られたシリカゾル（以下
原シリカゾルという）の数平均分子量はポリスチレン換
算でおよそ１０，０００であった。原シリカゾルに本Ｓ
ｉ化合物を直接添加することによって加え、第１図に示
す５０〜１０００個のノズルを有する紡糸装置で紡糸し
た結果を第１表に示す、なお捲取速度は１５０ｍ／ｓｉ
ｎ、、加圧ガスの圧力は元圧で３５ｋｇ／ｃｒｎ’、ノ
ズルの内径は０．１ｍｉ＋である。[Example] 47.4 parts by weight of 5i(C2H50)a was converted into 02H50H
The mixture was added with stirring to a liquid consisting of 49.5 parts by weight, 0.3 parts by weight of MCI, and 8 parts by weight of H2O, and stirring was continued at 70° C. for 2 days. The composition was then concentrated using a rotary baculum evaporator at 5° C. to a total volume of 40 parts by weight. The required time was 2 hours, and the number average molecular weight of the obtained silica sol (hereinafter referred to as raw silica sol) was approximately 10,000 in terms of polystyrene. Book S on raw silica sol
Table 1 shows the results obtained by adding Compound i directly and spinning using a spinning device having 50 to 1000 nozzles as shown in FIG. 1, with a winding speed of 150 m/si.
n,, the pressure of the pressurized gas is 35 kg/crn' at the original pressure, and the inner diameter of the nozzle is 0.1 mi+.
第１表中液の安定性は７０°Ｃの温度におけるゲル化す
る迄の峙間で示し、数字の大きい程安定性は大きい。The stability of the liquid in Table 1 is shown by the time taken to gel at a temperature of 70°C, and the larger the number, the greater the stability.
又紡糸性は糸径の安定性、乾燥性、糸切れ等紡糸作業の
安定性で判定した。その際■は極めて良好なもの、Ｏは
良好なもの、Δはやや不良なもの、×は不良なものを示
す。The spinnability was evaluated based on the stability of the spinning operation, such as stability of yarn diameter, drying performance, and yarn breakage. In this case, ■ indicates extremely good, O indicates good, Δ indicates slightly poor, and × indicates poor.
紡糸したシリカゲル繊維を２５０℃でｌ ｈｒ。The spun silica gel fibers were heated at 250°C for 1 hour.
８００℃テ２ｈｒ焼成し、モノフィラメントの強度をイ
ンストロン引張試験機によってゲージレングス２５ａ＋
ｍ、引玉速度０．５＋ｓｍ／ｗｉｎ、の条件で測定した
。After firing at 800℃ for 2 hours, the strength of the monofilament was measured using an Instron tensile tester with a gauge length of 25a+.
The measurement was carried out under the following conditions: m, ball pulling speed 0.5+sm/win.
又黒化は肉眼によって判定した。■は純白、Ｏは白色、
Δはやや茶色に着色、Ｘはかなり茶色に着色である。Darkening was also determined visually. ■ is pure white, O is white,
Δ is colored slightly brown, and X is colored considerably brown.
［発明の効果］
本発明によれば、紡糸液の安定性が増大し、糸径を小に
且つバラツキを少なくすることができる。なお得られた
糸の強度が増大し、焼成時の炭化による着色も生ずるこ
とがない。[Effects of the Invention] According to the present invention, the stability of the spinning solution is increased, and the yarn diameter can be reduced and variation can be reduced. Furthermore, the strength of the obtained yarn is increased, and coloration due to carbonization during firing does not occur.
第１図は紡糸装置の説明図である。 ｌ−−一紡糸液タンク ２−−一加圧ガス用バルブ ３−ｍ−フイルター ４−一一空気送風孔 ５−−一紡糸ノズル ６−ｍ−チムニー ７−ｍ−空気排出孔 ８−ｍ−ゲルファイバー ９−−一捲取機 FIG. 1 is an explanatory diagram of a spinning device. l--One spinning solution tank 2--1 Pressurized gas valve 3-m-filter 4-11 Air ventilation hole 5--One spinning nozzle 6-m-chimney 7-m-Air exhaust hole 8-m-gel fiber 9--One winder
Claims (4)
ＳｉＸで表わされるＳｉ化合物を添加したことを特徴と
する紡糸液。 ここに、 Ｙ＿１、Ｙ＿２、Ｙ＿３：アルキル基、アリル基又はア
リール基、 Ｘ：Ｈ、Ｃｌ、Ｂｒ、Ｉ、ＯＨ基又はＯＲ（Ｒは炭素数
１〜１０のアルキル基）(1) General formula Y_1 (Y_2) (Y_3) in silica sol
A spinning solution characterized by adding a Si compound represented by SiX. Here, Y_1, Y_2, Y_3: alkyl group, allyl group or aryl group, X: H, Cl, Br, I, OH group or OR (R is an alkyl group having 1 to 10 carbon atoms)
ル基または炭素数１〜４のアルキル基であることを 特徴とする特許請求の範囲第１項記載の紡 糸液。(2) The spinning solution according to claim 1, wherein Y_1, Y_2, and Y_3 are phenyl groups, vinyl groups, or alkyl groups having 1 to 4 carbon atoms.
であることを特徴とする特許請求の範囲第１項記載の紡
糸液。(3) The spinning solution according to claim 1, wherein the silica sol is a hydrolysis product of Si alkoxide.
中に含まれるＳｉの量に対するモル比が０．０１〜２．
５であることを特徴とする特許請求の範囲第１項記載の
紡糸液。(4) The molar ratio of the amount of Si contained in the Si compound to the amount of Si contained in the silica sol is 0.01 to 2.
5. The spinning solution according to claim 1, wherein the spinning solution is
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13924486A JPH0667770B2 (en) | 1986-06-17 | 1986-06-17 | Spinning liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13924486A JPH0667770B2 (en) | 1986-06-17 | 1986-06-17 | Spinning liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62297237A true JPS62297237A (en) | 1987-12-24 |
| JPH0667770B2 JPH0667770B2 (en) | 1994-08-31 |
Family
ID=15240810
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13924486A Expired - Lifetime JPH0667770B2 (en) | 1986-06-17 | 1986-06-17 | Spinning liquid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0667770B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01221536A (en) * | 1988-02-26 | 1989-09-05 | Asahi Fiber Glass Co Ltd | Bulky yarn and production thereof |
| US4919871A (en) * | 1989-01-04 | 1990-04-24 | Ppg Industries, Inc. | Forming glass fibers from sol-gel compositions |
| JPH02221417A (en) * | 1989-01-04 | 1990-09-04 | Ppg Ind Inc | Method and apparatus for preparing inorganic oxide fiber from sol-gel composition |
| US5089188A (en) * | 1989-01-04 | 1992-02-18 | Ppg Industries, Inc. | Spinning of sol gel siliceous-containing fibers with wet coagulation |
-
1986
- 1986-06-17 JP JP13924486A patent/JPH0667770B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01221536A (en) * | 1988-02-26 | 1989-09-05 | Asahi Fiber Glass Co Ltd | Bulky yarn and production thereof |
| US4919871A (en) * | 1989-01-04 | 1990-04-24 | Ppg Industries, Inc. | Forming glass fibers from sol-gel compositions |
| JPH02221417A (en) * | 1989-01-04 | 1990-09-04 | Ppg Ind Inc | Method and apparatus for preparing inorganic oxide fiber from sol-gel composition |
| US5089188A (en) * | 1989-01-04 | 1992-02-18 | Ppg Industries, Inc. | Spinning of sol gel siliceous-containing fibers with wet coagulation |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0667770B2 (en) | 1994-08-31 |
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