FR2600346A1 - Process for the production of inorganic fibres - Google Patents

Process for the production of inorganic fibres Download PDF

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Publication number
FR2600346A1
FR2600346A1 FR8708733A FR8708733A FR2600346A1 FR 2600346 A1 FR2600346 A1 FR 2600346A1 FR 8708733 A FR8708733 A FR 8708733A FR 8708733 A FR8708733 A FR 8708733A FR 2600346 A1 FR2600346 A1 FR 2600346A1
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Prior art keywords
polymer
nozzle
organic polymer
fibers
organometallic
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FR8708733A
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French (fr)
Inventor
Serita Tamio
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JNC Corp
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Chisso Corp
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    • 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

Process for the production of inorganic fibres, characterised in that an organometallic polymer is extruded in the molten state from a first nozzle 2 which emerges outside at a central part of a die and a hydrophobic organic polymer is simultaneously extruded in the molten state, containing little pyrolysis residue, from a second nozzle 4 which emerges outside surrounding the first nozzle concentrically in order to obtain, by drawing, composite fibres of the organometallic polymer which are coated externally with the organic polymer, and in that the composite fibres obtained are then subjected to heat treatment at a sufficiently elevated temperature in an inert gas atmosphere to decompose and volatilise the layer of organic polymer and simultaneously to cause the pyrolysis of the fibres of the organometallic polymer and to convert them into the inorganic state.

Description

La présente invention est relative à un procédé perfectionné de production de fibres inorganiques. La présente invention se rapporte plus particulièrement à un procédé perfectionné de production de fibres inorganiques obtenues par pyrolyse de polymères organométalliques qui sont susceptibles d'être décomposés par oxydation ou par hydrolyse. The present invention relates to an improved process for producing inorganic fibers. The present invention relates more particularly to an improved process for producing inorganic fibers obtained by pyrolysis of organometallic polymers which are capable of being broken down by oxidation or by hydrolysis.

Parmi les procédés de production de fibres inorganiques par pyrolyse de polymères organométalliques, on connaît notamment un procédé dans lequel on utilise des polycarbosilanes

Figure img00010001

(demande de brevet japonais non examinée (Takukai) 130325/1976) et un autre dans lequel on utilise des polysilaz anes
Figure img00010002

(demande de brevet japonais non examinée (Tokukai) 46995/1980) et analogues.Among the processes for producing inorganic fibers by pyrolysis of organometallic polymers, a process is known in which polycarbosilanes are used
Figure img00010001

(Japanese patent application unexamined (Takukai) 130325/1976) and another in which polysilaz anes are used
Figure img00010002

(Japanese patent application unexamined (Tokukai) 46995/1980) and the like.

Dans le premier procédé, on obtient des fibres inorganiques riches en carbure de silicium et dans le deuxième procédé, on obtient des fibres inorganiques riches en nitrure de silicium. Toutefois, les précurseurs de fibres (également désignés par fibres brutes), obtenus en filant ces polymères organométalliques, ont une résistance très faible et ceci entraine un problème consistant en ce que des opérations telles que le bobinage, le débobinage ou analogues, qui sont mises en oeuvre dans des étapes classiques pour la préparation de fibres, ne sont pas effectuées de manière régulière.En outre, dans le cas des polysilazanes, on rencontre un problème consistant en ce que les fibres obtenues perdent leur propriété de résistance dans la mesure où elles sont très sensibles à l'hydrolyse dans l'air, et des opérations telles que le filage, le bobinage ou analogues, doivent être effectuées dans un gaz inerte anhydre afin de surmonter le problème précité, et des dispositifs compliqués sont nécessaires. On rencontre par ailleurs un problème consistant en ce que les fibres sont susceptibles d'être dégradées au niveau de leur surface extérieure pendant l'opération de bobinage, de débobinage, etc., et en conséquence, la résistance des fibres inorganiques obtenues par transformation en céramique, est fortement dégradée. In the first method, inorganic fibers rich in silicon carbide are obtained and in the second method, inorganic fibers rich in silicon nitride are obtained. However, the fiber precursors (also known as crude fibers), obtained by spinning these organometallic polymers, have a very low resistance and this causes a problem consisting in that operations such as winding, unwinding or the like, which are carried out. used in conventional steps for the preparation of fibers, are not carried out regularly. In addition, in the case of polysilazanes, there is a problem consisting in that the fibers obtained lose their strength property insofar as they are very sensitive to hydrolysis in air, and operations such as spinning, winding or the like, must be performed in an anhydrous inert gas in order to overcome the above problem, and complicated devices are required. There is also a problem that the fibers are liable to be degraded at their outer surface during the winding, unwinding, etc. operation, and consequently, the resistance of the inorganic fibers obtained by transformation into ceramic, is strongly degraded.

Le but de la présente invention est de fournir un procédé de production de fibres inorganiques permettant de surmonter les divers problèmes mentionnés ci-dessus des fibres inorganiques de l'art antérieur. The object of the present invention is to provide a process for producing inorganic fibers which overcomes the various problems mentioned above of the inorganic fibers of the prior art.

Le but précité peut être atteint par le procédé de la présente invention. The above object can be achieved by the method of the present invention.

La présente invention a pour objet un procédé de production de fibres inorganiques dans lequel on extrude un polymère organométallique à l'état fondu à partir d'une première buse qui débouche à l'extérieur au niveau de la partie centrale d'une filière, et on extrude simultanément un polymère organique hydrophobe à l'état fondu contenant peu de résidu de pyrolyse à partir d'une deuxième buse qui débouche à l'extérieur en entourant concentriquement la première buse de manière i obtenir par tirage, des fibres composites du polymère organométallique revêtues extérieurement par le polymère organique, dans lequel on soumet ensuite les fibres composites à un traitement thermique à une température suffisamment élevée dans une atmosphère de gaz inerte pour décomposer et volatiliser la couche de polymère organique et pour provoquer simultanément la pyrolyse des fibres de polymère organométallique et les transformer à l'état inorganique. The subject of the present invention is a process for the production of inorganic fibers in which an organometallic polymer is extruded in the molten state from a first nozzle which opens out at the level of the central part of a die, and a hydrophobic organic polymer in the molten state containing little pyrolysis residue is simultaneously extruded from a second nozzle which opens to the outside by concentrically surrounding the first nozzle so as to obtain by drawing fibers composed of the organometallic polymer coated externally with the organic polymer, in which the composite fibers are then subjected to a heat treatment at a sufficiently high temperature in an atmosphere of inert gas to decompose and volatilize the layer of organic polymer and to simultaneously cause the pyrolysis of the fibers of organometallic polymer and transform them to the inorganic state.

Conformément au procédé de la présente invention, puisque le polymère organométallique à l'état fondu n'est pas directement en contact avec l'air, on empêche son hydrolyse ou son oxydation, le filage dans l'air devient réalisable et par l'effet de renforcement apporté par le polymère organique extérieur, il est possible d'effectuer sans problème le bobinage avec des dispositifs de bobinage classiques. According to the process of the present invention, since the organometallic polymer in the molten state is not directly in contact with the air, its hydrolysis or its oxidation is prevented, spinning in the air becomes feasible and by the effect reinforcement provided by the external organic polymer, it is possible to carry out the winding without problem with conventional winding devices.

Ces fibres composites dans lesquelles les âmes sont en fibres brutes, sont chauffées dans l'atmosphère de gaz inerte afin d'élever progressivement leur température et de volatiliser d'abord par pyrolyse le polymère organique qu'elles comportent et transformer ensuite par pyrolyse les fibres brutes en fibres inorganiques attendues. These composite fibers in which the cores are made of crude fibers, are heated in the inert gas atmosphere in order to gradually raise their temperature and to volatilize first by pyrolysis the organic polymer which they contain and then transform by pyrolysis the fibers crude inorganic fibers expected.

La température finale de traitement thermique est en général de 800 à 1500C.  The final heat treatment temperature is generally 800 to 1500C.

Pour le polymère organique utilisé à l'extérieur, il est approprié de choisir et d'utiliser un polymère choisi parmi ceux qui sont hydrophobes, qui contiennent peu de résidu de pyrolyse et qui ont un point de fusion voisin de celui du polymère organométallique. Comme exemple de ce polymère, on peut mentionner les polyoléfines et comme matériaux particulièrement adaptés, on peut mentionner le polyéthylène et le polypropylène. For the organic polymer used outside, it is appropriate to choose and use a polymer chosen from those which are hydrophobic, which contain little pyrolysis residue and which have a melting point close to that of the organometallic polymer. As an example of this polymer, mention may be made of polyolefins and as particularly suitable materials, mention may be made of polyethylene and polypropylene.

Pour les polymères organométalliques avec lesquels le procédé de production de la présente invention peut être mis efficacement en oeuvre et qui sont facilement hydrolysés ou oxydés, ou qui ont une faible résistance à l'état de fibres brutes, on peut mentionner par exemple les polycarbosilanes, les polysilazanes et les polysilanes.  For the organometallic polymers with which the production process of the present invention can be carried out efficiently and which are easily hydrolyzed or oxidized, or which have low resistance in the state of crude fibers, mention may be made, for example, of polycarbosilanes, polysilazanes and polysilanes.

Les polysilazanes obtenus par polymérisation à chaud de Si(NHCH3)4 préparé en faisant réagir SiC14 avec CH3NH2 comme cela est décrit dans la demande de brevet japonais n0 137 289/1985, déposée par la demanderesse, ont par exemple un point de fusion de 120 à 200du en fonction du degré de polymérisation. The polysilazanes obtained by hot polymerization of Si (NHCH3) 4 prepared by reacting SiC14 with CH3NH2 as described in Japanese patent application No. 137 289/1985, filed by the applicant, for example have a melting point of 120 to 200du depending on the degree of polymerization.

Dans ce cas, puisque ce point de fusion est voisin du point de fusion du polyéthylène ou du polypropylène haute densité, il est suffisant d'utiliser ces composés comme polymère organique extérieur. En outre, puisque les polyoléfines ont peu de groupes fonctionnels, qu'elles sont inertes et qu'elles ne réagissent pas avec un polysilazane, elles constituent des matériaux appropriés comme revêtement protecteur d'un polysilizane.In this case, since this melting point is close to the melting point of high density polyethylene or polypropylene, it is sufficient to use these compounds as an external organic polymer. In addition, since polyolefins have few functional groups, are inert and do not react with a polysilazane, they are suitable materials as a protective coating for a polysilizane.

Puisque les fibres brutes sous la forme de fibres composites qui sont obtenues par le procédé précité, ont une résistance accrue, il est possible de mettre en oeuvre une vitesse et un rapport d'étirage plus élevés au moment de l'opération de tirage et puisque l'on peut empêcher la dégradation de la surface des fibres brutes intérieures, la résistance des fibres inorganiques obtenues est également élevée. Since the raw fibers in the form of composite fibers which are obtained by the aforementioned process, have an increased resistance, it is possible to use a higher speed and a drawing ratio at the time of the drawing operation and since the degradation of the surface of the inner raw fibers can be prevented, the resistance of the inorganic fibers obtained is also high.

La présente invention va être mieux comprise a la lecture de la description qui va suivre d'un procédé de production de fibres brutes composites qui constitue une partie essentielle du procédé de production de la présente invention, en se référant au dessin annexé sur lequel la figure unique illustre une vue en coupe verticale d'un exemple caractéristique d'une filière utilisée pour la mise en oeuvre du procédé de la présente invention. The present invention will be better understood on reading the following description of a process for the production of raw composite fibers which constitutes an essential part of the production process of the present invention, with reference to the attached drawing in which the figure single illustrates a vertical sectional view of a typical example of a die used for the implementation of the method of the present invention.

Un polymère organométallique faisant office de matière première pour des fibres inorganiques, est extrudé à partir d'une première buse 2 disposée dans la partie centrale d'une filière après avoir passé dans un réservoir 1 du polymère organométallique fondu liquide, et au même moment, un polymère organique est extrudé à partir d'une deuxième buse 4 qui débouche de façon à entourer concentriquement la première buse après avoir passé dans un réservoir 3 du polymère organique liquide fondu afin d'obtenir des fibres composites dans lesquelles les fibres brutes du polymère organométallique extrudé à partir de la première buse, sont revêtues avec le polymère organique. Dans la filière, la référence 5 désigne un dispositif de chauffage.  An organometallic polymer acting as a raw material for inorganic fibers, is extruded from a first nozzle 2 placed in the central part of a die after having passed into a reservoir 1 of the molten organometallic polymer liquid, and at the same time, an organic polymer is extruded from a second nozzle 4 which opens so as to concentrically surround the first nozzle after having passed through a reservoir 3 of the molten liquid organic polymer in order to obtain composite fibers in which the raw fibers of the organometallic polymer extruded from the first nozzle, are coated with the organic polymer. In the sector, the reference 5 designates a heating device.

Claims (5)

REVENDICATIONS 1. Procédé de production de fibres inorganiques, caractérisé en ce qu'on extrude un polymère organométallique à l'état fondu à partir d'une première buse (2) qui débouche à l'extérieur au niveau d'une partie centrale d'une filière, et on extrude simultanément un polymère organique hydrophobe à l'état fondu contenant peu de résidu de pyrolyse à partir d'une deuxième buse (4) qui débouche à l'extérieur en entourant concentriquement la première buse afin d'obtenir par tirage des fibres composites du polymère organométallique revêtues extérieurement par le polymère organique, et en ce qu'on soumet ensuite les fibres composites obtenues au traitement thermique à une température suffisamment élevée dans une atmosphère de gaz inerte pour décomposer et volatiliser la couche de polymère organique et pour provoquer simultanément la pyrolyse des fibres du polymère organométallique et les transformer à l'état inorganique. 1. A method of producing inorganic fibers, characterized in that an organometallic polymer is extruded in the molten state from a first nozzle (2) which opens out at the level of a central part of a die, and a hydrophobic organic polymer in the molten state containing little pyrolysis residue is simultaneously extruded from a second nozzle (4) which opens to the outside by concentrically surrounding the first nozzle in order to obtain by drawing composite fibers of the organometallic polymer coated externally with the organic polymer, and in that the composite fibers obtained are then subjected to the heat treatment at a sufficiently high temperature in an atmosphere of inert gas to decompose and volatilize the layer of organic polymer and to cause simultaneously pyrolysis of the fibers of the organometallic polymer and transform them into the inorganic state. 2* Procédé suivant la revendication 1, caractérisé en ce que ledit polymère organométallique est un polysilazane. 2 * Process according to claim 1, characterized in that said organometallic polymer is a polysilazane. 3. Procédé suivant la revendication 1, caractérisé en ce que ledit polymère organe est du polypropylène. 3. Method according to claim 1, characterized in that said organ polymer is polypropylene. 4. Procédé suivant la revendication 2, caractérisé en ce que ledit polymère organique est du polypropylène. 4. Method according to claim 2, characterized in that said organic polymer is polypropylene. 5. Procédé suivant l'une quelconque des revendications précédentes, caractérisé en ce que ledit traitement thermique est effectué à une température de 800 C à l500 C.  5. Method according to any one of the preceding claims, characterized in that said heat treatment is carried out at a temperature of 800 C to 1500 C.
FR8708733A 1986-06-23 1987-06-22 Process for the production of inorganic fibres Pending FR2600346A1 (en)

Applications Claiming Priority (1)

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JP14670786A JPS636113A (en) 1986-06-23 1986-06-23 Production of inorganic fiber

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008098838A1 (en) * 2007-02-12 2008-08-21 Sgl Carbon Ag Method for producing a fiber-reinforced carbide ceramic component and a carbide ceramic component

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH419432A (en) * 1962-12-22 1966-08-31 Heraeus Gmbh W C Spinneret for the production of core sheath threads
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH419432A (en) * 1962-12-22 1966-08-31 Heraeus Gmbh W C Spinneret for the production of core sheath threads
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 102, no. 8, février 1985, page 264, résumé no. 66308n, Columbus, Ohio, US; & JP-A-59 168 121 (JAPAN ESTER CO., LTD) 21-09-1984 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008098838A1 (en) * 2007-02-12 2008-08-21 Sgl Carbon Ag Method for producing a fiber-reinforced carbide ceramic component and a carbide ceramic component

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