JPS636113A - Production of inorganic fiber - Google Patents
Production of inorganic fiberInfo
- Publication number
- JPS636113A JPS636113A JP14670786A JP14670786A JPS636113A JP S636113 A JPS636113 A JP S636113A JP 14670786 A JP14670786 A JP 14670786A JP 14670786 A JP14670786 A JP 14670786A JP S636113 A JPS636113 A JP S636113A
- Authority
- JP
- Japan
- Prior art keywords
- polymer
- nozzle
- organic polymer
- organometallic
- fiber
- 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.)
- Pending
Links
- 239000012784 inorganic fiber Substances 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000000835 fiber Substances 0.000 claims abstract description 24
- 229920000620 organic polymer Polymers 0.000 claims abstract description 18
- 229920001795 coordination polymer Polymers 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 claims description 2
- 229920005594 polymer fiber Polymers 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 125000002524 organometallic group Chemical group 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 229920001709 polysilazane Polymers 0.000 description 5
- 238000004804 winding Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/589—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained from Si-containing polymer precursors or organosilicon monomers
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
Abstract
Description
【発明の詳細な説明】
本発明は無ＲＲ維の改良された製造方法にかかわり、更
に詳しくは、酸化又は加水分解され易い有機金属ポリマ
ーを熱分解して得られる無機繊維の製造方法の改良に関
する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improved method for producing RR-free fibers, and more particularly, to an improved method for producing inorganic fibers obtained by thermally decomposing organometallic polymers that are easily oxidized or hydrolyzed. .
有機金属ポリマーを熱分解して無機繊維を製造する方法
は，例えば
Ｈ３
ポリシラザン（（ｓ ｉ＋Ｎ＋，、、−３−４ｎ）を原
料ポリマーとする方法が知られており（特開昭５１−１
３０３２５号、特開昭５５−４６９９５号など）前者か
らは炭化ケイ素を主体とする無ｆ％ｔｔｔｉ維が、後者
からは窒化ケイ素を主体とする無機繊維が得られている
。しかしながら、これらの有機金属ポリマーを紡糸して
得られるブリカーサ−繊維（一般にグリーン繊維とも呼
ばれる）は強度が極めて小さく、通常の繊維製造工程で
行なわれる巻取り、巻返し等の操作が円滑に行なわれに
くいという問題点かあつた。又、ポリシラザンの場合は
空気中で容易に加水分解を受け、その結果、得られる煕
機繊 。As a method for producing inorganic fibers by thermally decomposing organometallic polymers, for example, a method is known in which H3 polysilazane ((s i + N +, , -3-4n) is used as a raw material polymer (Japanese Patent Laid-Open No. 51-1).
No. 30325, JP-A No. 55-46995, etc.) The former produces f%ttti-free fibers mainly composed of silicon carbide, and the latter produces inorganic fibers mainly composed of silicon nitride. However, the bricassor fibers (generally called green fibers) obtained by spinning these organometallic polymers have extremely low strength, and operations such as winding and unwinding that are performed in normal fiber manufacturing processes cannot be performed smoothly. The problem was that it was difficult. In addition, in the case of polysilazane, it easily undergoes hydrolysis in the air, resulting in the formation of sulfur fibers.
維の強度特性が損なわれるという問題があり、それを防
ぐには乾燥不活性ガス中で紡糸、巻取り等の操作を行う
必要があり、複雑な装置を必要とした。更に巻取り、巻
返し等の工程を経る際に繊維の外側に傷がつき易く、そ
の結果それをセラミック化して得られる無機繊維の強度
を著るしく損なうという問題点もあった。There is a problem that the strength characteristics of the fibers are impaired, and to prevent this, operations such as spinning and winding must be performed in a dry inert gas, which requires complicated equipment. Furthermore, there is a problem in that the outside of the fiber is easily damaged during winding, unwinding, and other steps, and as a result, the strength of the inorganic fiber obtained by ceramicizing it is significantly impaired.
本発明の目的は上記の如き問題点を解決すべく改良され
た、無機繊維の製造方法を提供することにある。An object of the present invention is to provide an improved method for producing inorganic fibers in order to solve the above-mentioned problems.
本発明は溶融状態の有機金属ポリマーを、紡糸口金の中
心部に開口する第１ノズルから吐出させると同時に、第
１ノズルを同心円状に囲む様に開口する第２ノズルから
溶融状態の疎水性でかつ熱分解残炎の少ない有機ポリマ
ーを吐出、引取ること；二より外側が有機ポリマーで被
覆された有機金属ポリマーの複合繊維を得、次いでこの
複合繊維を不活性雰囲気中、高温度で熱処理することに
より外側の有機ポリマー屑を分解、揮散せしめると共に
有機金属ポリマー繊維を熱分解して無機化させることを
特徴とする無機繊維を製造する方法である。In the present invention, a molten organometallic polymer is discharged from a first nozzle that opens at the center of a spinneret, and at the same time, a molten hydrophobic polymer is discharged from a second nozzle that opens concentrically surrounding the first nozzle. Discharging and collecting an organic polymer with less pyrolysis afterflame; obtaining a composite fiber of an organometallic polymer whose outer side is coated with an organic polymer, and then heat-treating the composite fiber at a high temperature in an inert atmosphere. This is a method for producing inorganic fibers, which is characterized by decomposing and volatilizing outer organic polymer debris and thermally decomposing organic metal polymer fibers to inorganicize them.
本発明によれば溶融状態の有機金属ポリマーが直接空気
に触れないため、その加水分解又は酸化が防止され、空
気中での紡糸が可能となり、且つ、外側の有機ポリマー
の補強効果により、通常の巻取り装置で支障なく巻取る
ことが出来る。芯（コア）がグリーン繊維であるこの複
合繊維は、不活性雰囲気中で徐々に昇温することにより
、まず外側の有機ポリマーが熱分解してぞ１敗し、つい
でコアのグリーン繊維が熱分解して目的の無機繊維とな
る。According to the present invention, since the organometallic polymer in the molten state does not come into direct contact with air, its hydrolysis or oxidation is prevented, and spinning in the air becomes possible. It can be wound up without any problem using the winding device. This composite fiber, whose core is a green fiber, is heated gradually in an inert atmosphere so that the organic polymer on the outside is first thermally decomposed, and then the green fiber in the core is thermally decomposed. and becomes the desired inorganic fiber.
ここで外側に使用する有機ポリマーとしては・疎水性で
熱分解残炎が少なく、融点が有機金属ポリマーの融点に
近いものを撰択して使用すればよいが、この様なポリマ
ーの代表的なものとしてポリオレフィン類、特に好適な
ものとしてポリエチレン・ポリプロピレン等をあげるこ
とが出来る。The organic polymer to be used on the outside may be one that is hydrophobic, has little thermal decomposition afterflame, and has a melting point close to that of the organometallic polymer. Among them, polyolefins are particularly preferred, such as polyethylene and polypropylene.
本発明の製造方法を効果的に適用できる、加水分解又は
酸化し易い、或はグリーン繊維の強度の小さい有機金属
ポリマーとしてはポリカーボンラン類、ボリンラザン類
、ポリシラン類などが代表的なものとしてあげることが
できる。Typical organometallic polymers that are easily hydrolyzed or oxidized or have low green fiber strength to which the production method of the present invention can be effectively applied include polycarbonlans, borinrazanes, and polysilanes. be able to.
例えば本発明名らの出願に係る特願昭６０−１３７２８
９号に記載されているＳｉＣ／ａとＣＨ３ＮＨ２の反応
により得られるＳ ｉ （ＮＨＣＨ３） ４の熱重合に
よって得られるポリシラザンは重合度により１２０〜２
００℃の融点をもっているが、この場合は、高密度ポリ
エチレン又はポリプロピレンの融点と近いので・これら
を外側の有機ポリマーとして使用すればよい。更にポリ
オレフィン類は官能基が殆んどなく、不活性でポリシラ
ザンとも反応せず、ポリシラザンを保護する被覆として
適したものである。For example, patent application No. 60-13728 filed by the inventors of the present invention.
The polysilazane obtained by thermal polymerization of Si (NHCH3) 4 obtained by the reaction of SiC/a and CH3NH2 described in No. 9 has a polymerization degree of 120 to 2
It has a melting point of 00°C, but in this case, it is close to the melting point of high-density polyethylene or polypropylene, so these can be used as the outer organic polymer. Furthermore, polyolefins have almost no functional groups, are inert and do not react with polysilazane, and are suitable as a coating for protecting polysilazane.
この様にして得られた複合ＦＱ維化したグリーン繊維は
その強度が大きくなっているので、巻取り作業における
高速、高引き落しも可能となり、又内部グリーン繊維の
表面に傷がつくのが防げるため・得られる無機繊維の強
度も向上する。The strength of the composite FQ fibrous green fiber obtained in this way is high, so high speed and high drawdown is possible during winding work, and damage to the surface of the internal green fiber can be prevented. The strength of the resulting inorganic fibers is also improved.
次に本発明の製造方法の主要部分をなＴ６合図は本発明
の方法（二於ける、複合グリーン繊維を製造する際に使
用する紡糸口金の１例の縦断面図であり、無機繊維の原
料となる有は金Ｊ戊ポリマーは有機金属ポリマー融液用
溜り１を硅て口金の中心部に位置する第１ノズル２から
押出され、同時に有機ポリマーは有機ポリマー触液用溜
り３を経て、＄１ノズルを囲む様開口したｒ“ＰＪ２ノ
ズル４から押出されｓ ’４１１ノズルかう押出された
有機金属ポリマーのグリーン繊維の外τ１りを被覆して
複合グリーン繊維が得られる。Next, the main part of the production method of the present invention, T6, is a longitudinal sectional view of an example of a spinneret used in the production of composite green fibers in the method of the present invention (2), and is a raw material for inorganic fibers. The polymer passes through the organometallic polymer melt reservoir 1 and is extruded from the first nozzle 2 located at the center of the nozzle, and at the same time, the organic polymer passes through the organic polymer molten reservoir 3 and is extruded from the first nozzle 2. Composite green fibers are obtained by covering the outside of the organic metal polymer green fibers extruded from r'PJ2 nozzle 4, which is opened so as to surround one nozzle, and then extruded through s'411 nozzle.
図は本発明の方法を実施する際に用いる紡糸口金の一実
施例を示す縦断面図である。
１・・・・・・・・・・・・有機金属ポリマー融液用溜
り２・・・・・・・・・・・・第１ノズル３・・・・・
・・・・・・・有機ポリマー融液用溜り４・・・・・・
・・・・・・第２ノズル５・・・・・・・・・・・・ヒ
ーター
以上
特許出願人 チ ッ ソ 株 式 会 社代理人 弁
理士 佐々井 彌太部
同 上 野中克彦
図The figure is a longitudinal cross-sectional view showing one embodiment of a spinneret used in carrying out the method of the present invention. 1...Reservoir for organometallic polymer melt 2...First nozzle 3...
・・・・・・Reservoir for organic polymer melt 4・・・・・・
・・・・・・Second nozzle 5・・・・・・・・・・・・Heater and above Patent applicant Chisso Co., Ltd. Company representative Patent attorney Yatabe Sasai Same as above Katsuhiko Nonaka
Claims (1)
口する第１ノズルから吐出させると同時に、第１ノズル
を同心円状に囲む様に開口する第２ノズルから溶融状態
の、疎水性でかつ熱分解残査の少ない有機ポリマーを吐
出、引取ることにより外側が有機ポリマーで被覆された
有機金属ポリマーの複合繊維を得、次いでこの複合繊維
を不活性雰囲気中、高温度で熱処理することにより、外
側の有機ポリマー層を分解、揮散せしめると共に有機金
属ポリマー繊維を熱分解して無機化させることを特徴と
する無機繊維の製造方法。A molten organometallic polymer is discharged from a first nozzle opening at the center of the spinneret, and at the same time a molten hydrophobic and thermal polymer is discharged from a second nozzle concentrically surrounding the first nozzle. By discharging and collecting the organic polymer with little decomposition residue, we obtain a composite fiber of organometallic polymer whose outside is coated with an organic polymer.Then, by heat-treating this composite fiber at high temperature in an inert atmosphere, the outside is coated with an organic polymer. 1. A method for producing inorganic fibers, which comprises decomposing and volatilizing an organic polymer layer, and pyrolyzing and inorganicizing an organic metal polymer fiber.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14670786A JPS636113A (en) | 1986-06-23 | 1986-06-23 | Production of inorganic fiber |
| FR8708733A FR2600346A1 (en) | 1986-06-23 | 1987-06-22 | Process for the production of inorganic fibres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14670786A JPS636113A (en) | 1986-06-23 | 1986-06-23 | Production of inorganic fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS636113A true JPS636113A (en) | 1988-01-12 |
Family
ID=15413724
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14670786A Pending JPS636113A (en) | 1986-06-23 | 1986-06-23 | Production of inorganic fiber |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JPS636113A (en) |
| FR (1) | FR2600346A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007007410A1 (en) * | 2007-02-12 | 2008-08-14 | Sgl Carbon Ag | Process for producing a fiber-reinforced carbide ceramic component and a carbide ceramic component |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL301748A (en) * | 1962-12-22 | |||
| US4312970A (en) * | 1981-02-20 | 1982-01-26 | Dow Corning Corporation | Silazane polymers from {R'3 Si}2 NH and organochlorosilanes |
| JPS59168121A (en) * | 1983-03-10 | 1984-09-21 | Nippon Ester Co Ltd | Conjugated yarn |
-
1986
- 1986-06-23 JP JP14670786A patent/JPS636113A/en active Pending
-
1987
- 1987-06-22 FR FR8708733A patent/FR2600346A1/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| FR2600346A1 (en) | 1987-12-24 |
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