EP0122836B1 - Verfahren zur Herstellung von Phenoplastfasern - Google Patents

Verfahren zur Herstellung von Phenoplastfasern Download PDF

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Publication number
EP0122836B1
EP0122836B1 EP84400583A EP84400583A EP0122836B1 EP 0122836 B1 EP0122836 B1 EP 0122836B1 EP 84400583 A EP84400583 A EP 84400583A EP 84400583 A EP84400583 A EP 84400583A EP 0122836 B1 EP0122836 B1 EP 0122836B1
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Prior art keywords
fibres
fibers
composition
temperature
die
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EP84400583A
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English (en)
French (fr)
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EP0122836A1 (de
Inventor
Jacques Seignan
Bernard Kafka
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Saint Gobain Isover SA France
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Saint Gobain Isover SA France
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    • 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
    • D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products

Definitions

  • the invention relates to a process for the production of fibers from phenoplast resins of the resol type.
  • Phenoplast resins are obtained by polycondensation of a phenol and an aldehyde. Most commonly phenoplasts come from the condensation of phenol and formalin. In the following description, we will mainly refer to these phenol resins based on phenol and formaldehyde, but the characteristics of the invention mean that it can be applied to all phenoplast resins provided that they have the properties which will be discussed below.
  • the novolaks are obtained by polycondensation of an excess of phenol relative to the amount of formalin used, in the presence of an acid catalyst.
  • the prepared resin which is hot melt, is crosslinkable using a crosslinking agent such as hexamethylene tetramine or paraformaldehyde in the presence of an acid catalyst. Cross-linking is accelerated by a rise in temperature.
  • the resols come from the polycondensation of an excess of formalin relative to the amount of phenol used, in the presence of a basic catalyst.
  • the formation of the resin which is accelerated when the temperature rises is difficult to control. It results in very diverse products according to the operating conditions and in particular according to the duration of the reaction. If the reaction is not stopped it continues until the formation of a solid product which is infusible and therefore cannot be spinned. To maintain the resin in conditions under which it can be worked, the reaction should be blocked by lowering the temperature and / or neutralizing the mixture. A resin in solution is then obtained, the characteristics of which, in particular of viscosity, vary according to the degree of progress of the reaction.
  • the resin is crosslinkable and crosslinking can be accelerated in the presence of an acid catalyst. The crosslinking is all the faster the higher the temperature.
  • novolak fibers are traditionally obtained by melting the hot-melt resin followed by fiberizing and treatment in an aqueous or gaseous medium with the crosslinking agent and the catalyst.
  • This treatment resulting in crosslinking is very long because of the need to diffuse the crosslinking agent and the catalyst in the solidified resin fiber. It can extend over several hours.
  • the operation leading to the formation of the fibers is particularly delicate. Unlike the novolaks for which the cooling after passage of the molten mixture in the die leads to fibers in a way frozen and well individualized, even if the crosslinking is barely started, the fibering operated with a resol in a state suitable for spinning, c that is to say a resol whose evolution has been stopped at a degree of condensation such that the viscosity is satisfactory, leads to the production of unstabilized fibers which remain sticky.
  • the invention proposes to provide a process for the production of fibers from resols.
  • the resin used the nature and the proportions of the products possibly added, in particular a crosslinking catalyst, are chosen to constitute a mixture whose characteristics, in particular of viscosity, are suitable for the formation of fibers by passage in a sector.
  • composition to be fiberized is immediately directed to a member acting as a die and which is consisting of a centrifuge.
  • the composition introduced into the centrifuge covers the inner peripheral wall of the centrifuge. This wall is pierced with orifices through which the composition passes. The latter is projected out of the orifices in the form of thin filaments which stretch into fibers and the orifices are of dimensions such that each of them gives rise to a separate fiber.
  • the conditions determining the maturation kinetics of the fibers formed, in particular the choice of the possible catalyst and of its proportions, and the temperature conditions of the surrounding atmosphere in which the fibers are projected, are chosen so that during their trajectory in this atmosphere until they are received, the fibers are sufficiently crosslinked and dried to keep a clean shape and do not stick to each other.
  • the preparation of resolated fibers is subject to conflicting requirements.
  • it may seem desirable to form a mixture capable of accelerating the evolution process and on the other hand when such a mixture is actually carried out, it is difficult to sufficiently control the evolution so as to maintain the mixing under conditions suitable for passing through a die and drawing the fibers.
  • compositions used according to the invention To be able to fiberize the compositions used according to the invention and taking into account the fact that they evolve rapidly towards a state in which precisely they could no longer be used for the formation of fibers, it is necessary to ensure that the mixture formed is very quickly used .
  • the mixture is therefore formed as it is used. Once the mixture has been formed, the means used to produce the fibers must retain this mixture for as short a time as possible.
  • the amount of composition held in the centrifuge can be extremely small. It can correspond to the quantity passing in a few seconds, so that the average residence time is very short and that there is no risk of "freezing" the composition before it passes through the orifices.
  • the fibers being projected out of the centrifuge they must be stabilized as quickly as possible.
  • the time interval separating the appearance of the fibers at the outlet of the centrifuge from their deposition on the collecting member is necessarily limited by the dimensions of the installation used.
  • the formation of these bubbles is not desirable.
  • the bubbles break the homogeneity of the structure of the fibers and in particular harm their mechanical properties.
  • the temperature of the fibers in the atmosphere surrounding the centrifuge is preferably kept below the boiling temperature of the water, or of the water / solvent mixture, present in the composition.
  • the temperature not to be exceeded corresponds approximately to that of boiling water.
  • the temperature of the fibers, at least in the region closest to the centrifuge does not exceed 80 ° C.
  • the temperature of the atmosphere itself can be significantly higher than that of the fibers as a result of the cooling caused on them by evaporation. We will see in the examples that the gas temperature can reach and even exceed 200 ° C.
  • the fibers are subjected to a temperature which increases when they move away from the centrifuge.
  • the exchanges taking place very quickly due to the fineness of the fibers, the crosslinking progressing and the drying taking place, it is possible to reach in the areas remote from the centrifuge temperatures higher than the limit temperatures indicated above. above.
  • the hot gas stream is preferably driven at a relatively low speed when it is directed transversely to the direction of projection of the fibers out of the centrifuge to avoid folding the fibers too early on each other when they are not yet perfectly stabilized.
  • the resin or resin-catalyst mixture should have a viscosity suitable for the mode of fiber formation envisaged.
  • a viscosity of the order of 500 to 30,000 mPas and preferably from 1,500 to 10,000 mPas is advantageously chosen.
  • the resin or the mixture is neither too fluid, which would lead to premature rupture of the filaments generating droplets and / or products that are insufficiently drawn, or too viscous, which would require the use of relatively large orifices and the fibers obtained would not meet the characteristics of fineness ordinarily sought.
  • the viscosity of the composition used is determined first of all by that of the resin, which itself depends on how the resin is prepared. It is thus necessary to take into consideration the reaction time and temperature, as well as the molar ratio of the formalin and the starting phenol. Condensation must be stopped when the viscosity suitable for spinning is reached.
  • the viscosity of the resin can however be modified by the addition of solvents.
  • the resin used preferably has a molecular mass of between 100 and 1000 and more particularly between 400 and 800.
  • the resin is preferably prepared from phenol and formaldehyde introduced in a molar ratio of formaldehyde to phenol of between 1.3 and 1.7.
  • a third solvent is advantageously used in as small a quantity as possible.
  • a compound which is both miscible with water and with resin and which is capable of being easily removed during the subsequent treatment of the fibers is used as a third solvent.
  • the third solvent is an alcohol, in particular methanol.
  • the viscosity of the assembly added to the resin can also be adjusted to avoid that, at the time of mixing, a too strong modification of the viscosity is observed.
  • thickening agents for example glycols, and preferably di- or triethylene glycol.
  • these thickening agents are introduced which, while allowing a higher final viscosity to be reached, also promote the homogenization of the mixture.
  • the crosslinking catalysts used are strong acids, mineral or organic, alone or as a mixture. Acids such as sulfuric acid, phosphoric acid or hydrochloric acid and their mixtures in aqueous solution are preferably used.
  • the use of a catalyst in solution allows a good dispersion thereof within the resin provided that the miscibility has been ensured as we have indicated above.
  • the dispersion of the catalyst in the resin is a determining factor for the way in which the crosslinking takes place. Good dispersion naturally favors rapid and homogeneous crosslinking, which is desirable under the conditions used according to the invention.
  • the characteristics of the spun compositions used according to the invention can be further modified to improve the formation and drawing of the fibers.
  • surfactant it is also usual in the processes of formation of fibers from synthetic resins to add small proportions of a surfactant, always to improve the characteristics during fiberizing, and in particular to avoid early hair breaks.
  • these are nonionic surfactants, such as sorbitan or cationic fatty alcohols, which exhibit better stability in an acid medium.
  • Preferred surfactants are those sold under the names “TWEEN” and “SPAN” (registered trademarks). They are introduced into the composition in an amount of 0.5 to 3% by weight.
  • FIG. 1 The installation shown diagrammatically in FIG. 1 is particularly representative of those which can be used according to the invention. It performs the conditioning of the composition, the fiberizing of this composition and the stabilization of the fibers formed.
  • the resin previously prepared and optionally containing the various fiberizing additives is placed in a tank 1 in which it is maintained at a temperature which allows its conservation.
  • the resin in the liquid state taken from the tank 1 by means appropriate to its state: pump, screw, etc. is conducted in a determined quantity in a mixer 2.
  • the mixer also optionally receives in metered quantities the catalyst originating from 'a tank as shown in 24.
  • the mixing operation is very vigorous to obtain a composition that is as homogeneous as possible.
  • the volume offered in the mixer is small so that the composition stays there as short as possible.
  • the composition is then sent directly to the centrifuge device.
  • the line 8 leading the composition to be fiberized in the centrifuge device is as short as possible.
  • the mixer 2 is advantageously located near the centrifuge device.
  • the device comprises a centrifuge 3 fixed on a shaft 4 which is rotated by an electric motor 5 by means of belts 6.
  • the shaft 4 is mounted on bearings 7.
  • the shaft 4 is hollow.
  • Line 8 leading the composition to the centrifuge is housed in this tree.
  • the centrifuge device itself comprises a basket 9 on the bottom of which the composition is poured.
  • the basket is pierced on its peripheral wall 10 with regularly spaced holes 11.
  • the composition reaches the inner face of the wall 10 and escapes through the orifices 11 in the form of large composition nets, which are projected onto the peripheral wall 12 of the centrifuge proper 3.
  • the presence of the basket 9 allows a first equalization of the distribution of the composition on the inner peripheral wall of the centrifuge.
  • the use of a basket is all the more advantageous when the centrifuge is larger.
  • the "natural" distribution of the composition is more likely to be unbalanced. It is very important for the quality of the fibers to have at all points of the centrifuge the same "reserve", that is to say the same thickness of composition so that the centrifugation conditions are everywhere the same and therefore that the fibers are formed under the same conditions.
  • composition which forms the reserve escapes from the centrifuge through the orifices 14 arranged at the periphery.
  • the orifices 14 have dimensions such that each of them gives rise to a single fiber which is then projected into the surrounding atmosphere.
  • the internal profile of the centrifuge is determined so as to facilitate the flow of the composition.
  • the orifices are preceded by a part of triangular cross section 15 which leads the composition towards the orifices 14. This profile notably avoids the stagnation of composition in blind spots, stagnation which could lead to deposits of crosslinked resins.
  • FIG. 2 shows a centrifuge comprising a single row of orifices 14. It is of course possible to use a centrifuge comprising several rows of orifices, as shown in FIG. 3. In this case, it is necessary to choose the distance between two successive rows so that the fibers formed do not risk re-sticking before being stabilized. The distance between two orifices in the same row is also chosen so as to prevent the fibers from sticking together.
  • the profile of the centrifuge with several rows of orifices represented in FIG. 3 also includes grooves 26 on the internal face, the section of which decreases when approaching the orifices 14, which allow good circulation of the material to be fiberized to each row orifices.
  • the amount of composition in the basket and the centrifuge is kept at the minimum necessary to continuously feed the orifices 14.
  • the "reserve” must suitably cover the orifices 14. This reserve must however be small to shorten the residence time.
  • the composition is sprayed out of the centrifuge in the form of filaments, the dimensions of which are determined by those of the orifices.
  • the orifices ordinarily, taking into account the viscosities of the composition which have been indicated above and in order to obtain fine fibers of the order of 20 micrometers or less, the orifices have a diameter advantageously less than 1 mm and preferably between 0.2 and 0 , 8 mm. For larger diameters, and if the other conditions remain unchanged, the fibers produced are larger. To find finer fibers, it is then necessary to carry out a more violent centrifugation and / or to reduce the flow of composition per orifice.
  • the fibers are projected and stretch substantially in the plane perpendicular to the axis of rotation of the centrifuge. They develop in spirals which can extend at relatively large distances from the centrifuge when the initial acceleration is high.
  • the path of the fibers in the plane, which can reach a meter or more, is usually limited for reasons of the size of the receiving enclosure 19.
  • the path of the fibers is limited by blowing a gas stream along the walls 16, sufficiently intense to fold the fibers before they reach these walls.
  • the blowing can be carried out for example by means of a series of nozzles 18 disposed along a conduit 17 for supplying compressed air.
  • the nozzles 18 are preferably close enough to each other so that the jets fuse very quickly and constitute a practically continuous gas layer which obstructs the passage of the fibers.
  • the fibers from the start of their path towards the wall 16 of the receiving enclosure 19, are subjected to the heat treatment which makes it possible to substantially accelerate the kinetics of crosslinking of the mixture and promotes the elimination of water and / or solvents present in the fibers.
  • This heat treatment is advantageously obtained by means of hot gas streams arranged on the path of the fibers between the outlet of the centrifuge and the point where they are folded down.
  • the hot gaseous layers are directed on the path of the fibers with a speed and at a temperature such that the modification of the path can be limited as much as possible and, consequently, the risks of sticking of the fibers not yet stabilized.
  • the speed of the gases is preferably kept below 20 m / s.
  • Figure 1 shows a double supply of hot gases. These two supplies are made from chambers 20 and 21 arranged concentrically around the centrifuge.
  • the chambers 20 and 21 are supplied by one or more gas burners by means of pipes not shown. They are separated from the receiving enclosure 19 by widely open grids 22 letting the gases pass at low speed.
  • the installation shown comprises two hot gas emission chambers, it is of course possible to regulate the temperature of the gases of these two chambers independently of one another. It is also possible to provide a larger number of gas emission chambers to control even better the progress of the conditions for treating the fibers.
  • centrifuge may be advantageous to protect the centrifuge against heat coming from the neighboring chamber 20 by interposing for example a coil 25 surrounding the shaft 4 and the top of the centrifuge, and in which cooling water circulates .
  • the length of the path required before to gather the fibers is determined at the same time as the gas temperature conditions for each composition treated, it being understood that in all cases it is necessary to collect fibers sufficiently dried and crosslinked so that they do not risk sticking to each other.
  • the distance separating the centrifuge from the receiving belt is such that the time taken by the fibers to travel this path is between 0.1 and 2 s.
  • the fibers carried by the gases are deposited on a conveyor belt 23 where they constitute a felt of entangled fibers.
  • the suction means consist of a box 26 disposed under the conveyor and a fan, not shown.
  • the conditions set out above according to the invention make it possible to collect fibers in which the crosslinking process is very advanced and this in a very short time. If the complete residence time of the fibers in the receiving enclosure is very short, it may happen that the fibers have not reached a degree of maturation (or crosslinking) allowing them to be given the best possible properties. In this case, it is advantageous to complete the crosslinking by a very brief passage in an oven.
  • the temperature during such a heat treatment is greater than 100 ° C., and preferably between 100 and 150 ° C.
  • Example of fiber preparation in the presence of a catalyst Example of fiber preparation in the presence of a catalyst.
  • the reaction is stopped by cooling when the desired viscosity is reached. This is measured by the flow tube method.
  • the reaction is stopped by cooling to 25 ° C.
  • the resin obtained has a viscosity of 1000 mPas at 25 ° C.
  • the dry extract constitutes 70.5% of its mass.
  • the resin is stored at a temperature of 5 to 7 ° C.
  • the viscosity of the fiber premix is 13,000 mPas at 25 ° C.
  • the catalyst is measured at 7 parts.
  • the mixture used to form the fibers is, as the case may be, 100 parts by weight of resin premix for 5 to 10 parts of catalyst.
  • This mixture is in a homogeneous form with a viscosity varying from 3500 to 5000 mPas at 25 ° C.
  • the operation is carried out continuously in an enclosure with a square section, and with a height of approximately 2.5 m of the type shown in FIG. 1.
  • the mixture obtained in 4 is led by a pipe of the mixer in the receiving basket.
  • the centrifuge and the basket rotate at 3000 rpm.
  • the basket is pierced with 40 holes of 1.2 mm in diameter and the centrifuge whose diameter is 200 mm has 150 holes of 0.5 mm in diameter.
  • the fibers deploy in the air blown by 5 concentric chambers.
  • the speed of the gas emitted by these chambers increases as one moves away from the centrifuge, ensuring progressive deflection of the fibers.
  • the air is heated to a regulated temperature between 150 and 160 ° C.
  • a certain amount of air at room temperature is introduced through the walls forming the sides of the enclosure.
  • the air temperature is 80 ° C at the receiving conveyor.
  • the fibers are deposited in a continuous sheet of approximately 50 cm in width, formed of long dried and largely crosslinked fibers.
  • the regulation of the suction allows, by controlling the temperature at the bottom of the hood, to vary the degree of crosslinking.
  • the fiber diameters are between 2 and 19 ⁇ m.
  • the histogram of the diameters is of very tight Gaussian type with an average diameter of 7 micrometers.
  • the average tensile strength is around 300 MPa.
  • the density of the felt is approximately 20 kg / m 3 and its thermal conductivity on the order of 35 mW / m ° K for a thickness of 80 mm.
  • the felt obtained previously can be completely crosslinked by passing through the oven for 5 minutes at 120 ° C.
  • the felt which is not completely crosslinked has a certain thermoplasticity. This can be taken advantage of to constitute a self-bonding felt: For this purpose the felt obtained is subjected for 3 minutes to a temperature of the order of 220 ° C. by slightly compressing it.
  • a felt is thus obtained having a cohesion which makes it easy to handle.
  • the fibers are formed by rotating the system at 3800 rpm.
  • the basket 9 is pierced with 6 holes of 2.5 mm in diameter and the centrifuge has 4 rows of 150 holes of 0.4 mm in diameter.
  • a stabilized fiber flow rate is obtained which is greater than that obtained with a single row of orifices.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)

Claims (19)

1. Verfahren zur Herstellung von Fasern auf der Basis von Resol-Harzen, welche aus der Kondensation von Formaldehyd und Phenolen in einem Molverhältnis von Formaldehyd zu Phenol größer als 1 stammen, dadurch gekennzeichnet, daß die für die Bildung der Fasern verwendete Zusammensetzung in einen Zustand gebracht wird, vernetzt zu werden, und ihre Viskosität direkt vor ihrem Eintritt in ein Zerfaserungsaggregat eingestellt wird, wobei das In-Zustand-Bringen und die Einstellung fortlaufend mit einer geringen Menge der Zusammensetzung vorgenommen werden, wobei die so vorbereitete Zusammensetzung einen Schleuderring speist, und durch Offnungen dieses Zerfaserungsaggregats hindurchtritt, wobei jede Offnung eine Faser erzeugt, welche in die das Zerfaserungsaggregat umgebende Atmosphäre geschleudert wird, wo sie ausgezogen wird, wobei die Konstitution der verwendeten Zusammensetzung und die Temperaturbedingungen in der den Schluüderring umgebenden Atmosphäre derart gewählt sind, daß die abgelegten Fasern ausreichend stabilisiert sind, um eine eigene Form beizubehalten und nicht miteinander zu verkleben.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das In-Zustand-Versetzen des Harzes die Zufügung eines Vernetzungskatalysators umfaßt.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Viskosität der Zusammensetzung auf einen Wert zwischen 500 und 30 000 mPa s eingestellt wird.
4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß die Viskosität der Zusammensetzung auf einen Wert zwischen 1500 und 10 000 mPa s eingestellt wird.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Zeit zwischen den In-Zustand-Versetzen der Zusammensetzung und der Bildung der Fasern beim Hindurchtritt durch die Offnungen des Zerfaserungsaggregats geringer als 1 Minute ist.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Atmosphäre, die das Zerfaserungsaggregat auf der Bahn der Fasern umgibt, mittels warmen Gasströmen geheizt wird.
7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die warmen Gasströme mit einer Geschwindigkeit kleiner als 20 m/s geblasen werden.
8. Verfahren nach einem der Ansprüche 6 oder 7, dadurch gekennzeichnet, daß die warmen Gasströme bei einer Temperatur geblasen werden, die ausreicht, um die Wiederverklebung der Fasern zu verhindern.
9. Verfahren nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, daß die Temperatur der Fasern in der den Schleudering umgebenden Atmosphäre auf eine Temperatur gebracht wird, die geringer ist als jene, bei der Blasen in den Fasern auftreten.
10. Verfahren nach Anspruch 9, dadurch gekennzeichnet, daß die Temperatur der Fasern in der den Schleuderring umgebenden Atmosphäre höchstens 80°C beträgt.
11. Verfahren nach Anspruch 10, dadurch gekennzeichnet, daß die Zeit, die die Fasern brauchen, um den Weg zwischen der Zentrifuge und der Produktionsband zu durchqueren, zwischen 0,1 und 2 Sekunden liegt.
12. Verfahren nach einem der Ansprüche 2 bis 11, dadurch gekennzeichnet, daß der Katalysator von einer wässrigen Lösung von Schwefelsäure, Salzsäure oder Phosphorsäure, oder Mischungen aus diesen Säuren gebildet ist.
13. Verfahren nach Anspruch 12, dadurch gekennzeichnet, daß die Mischbarkeit der wässrigen Lösung des Katalysators mit dem Harz durch Zusatz von Metanol verbessert wird.
14. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß ein aus einem langkettigen Polyoxyolefin gebildeter Faserbildner in die zur Bildung der Fasern bestimmte Zusammensetzung eingeführt wird.
15. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß ein grenzflächenaktives Mittel ebenfalls in die zur Bildung der Fasern bestimmte Zusammensetzung eingeführt wird.
16. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, daß die gebildeten Fasern weiterhin einer Wärmebehandlung bei einer Temperatur, die geringer ist als die Temperatur der restlichen Erweichung unterworfen werden während einer Zeit, die nicht länger als 5 Minuten beträgt.
17. Verfahren nach Anspruch 16, dadurch gekennzeichnet, daß die Wärmebehandlung bei einer Gastemperatur zwischen 100 und 150 C durchgeführt wird.
18. Verfahren nach einem der Ansprüche 1 bis 15, dadurch gekennzeichnet, daß die in Form eines Filzes gesammelten Fasern einer Wärmebehandlung bei einer Temperatur unterworfen werden, die größer ist als die Temperatur der restlichen Erweichung.
19. Verfahren nach Anspruch 18, dadurch gekennzeichnet, daß die Wärmebehandlung bei einer Temperatur zwischen 200 und 240° C durchgeführt wird.
EP84400583A 1983-03-23 1984-03-22 Verfahren zur Herstellung von Phenoplastfasern Expired EP0122836B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8304737A FR2543169B1 (fr) 1983-03-23 1983-03-23 Procede de production de fibres phenoplastes
FR8304737 1983-03-23

Publications (2)

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EP0122836A1 EP0122836A1 (de) 1984-10-24
EP0122836B1 true EP0122836B1 (de) 1987-03-18

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US (1) US5055241A (de)
EP (1) EP0122836B1 (de)
JP (1) JPS59179811A (de)
DE (1) DE3462703D1 (de)
FR (1) FR2543169B1 (de)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
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FR2588255A1 (fr) * 1985-10-09 1987-04-10 Saint Gobain Isover Composition pour l'encollage de fibres minerales et fibres minerales encollees
JPH0735610B2 (ja) * 1986-01-24 1995-04-19 三菱石油株式会社 ピツチ系炭素繊維遠心紡糸装置
FR2695413B3 (fr) * 1992-09-09 1994-12-16 Saint Gobain Isover Dispositif pour la formation de fibres phénoplastes.
KR100421306B1 (ko) * 1995-03-03 2004-04-21 데이진 트와론 비.브이. 방사액을 위한 원심방사방법
US6001303A (en) * 1997-12-19 1999-12-14 Kimberly-Clark Worldwide, Inc. Process of making fibers
US6368533B1 (en) * 1997-12-22 2002-04-09 Kimberly-Clark Worldwide, Inc. Process for forming films, fibers and base webs from thermoset polymers
HUP0700795A2 (en) * 2007-12-10 2009-04-28 Miskolci Egyetem Coextrusion centrifugal apparatus to fibre formation
JP5458280B2 (ja) * 2010-01-06 2014-04-02 パナソニック株式会社 ナノファイバ製造装置および製造方法
JP5322112B2 (ja) * 2010-01-18 2013-10-23 パナソニック株式会社 ナノファイバ製造装置および製造方法
US9731466B2 (en) 2012-08-06 2017-08-15 Clarcor Inc. Systems and methods of supplying materials to a rotating fiber producing device
DE102019003795A1 (de) * 2019-05-29 2020-12-03 Bb Engineering Gmbh Vorrichtung und Verfahren zur Herstellung eines Vlieses
CN111910272B (zh) * 2020-06-29 2023-01-24 太原理工大学 一种熔喷纺丝制备酚醛纤维的方法

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JPS5010408B2 (de) * 1971-11-06 1975-04-21
JPS5029817A (de) * 1973-07-19 1975-03-25
GB1573116A (en) * 1977-03-11 1980-08-13 Ici Ltd Production of formaldehyde resin fibres by centrifugal spining
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NZ187979A (en) * 1977-07-29 1982-05-31 Ici Ltd Centrifugal spinning of fibres from liquid
FI68866C (fi) * 1979-04-09 1985-11-11 Ici Ltd Centrifugalspinnkopp och foerfarande foer centrifugalspinnandeav fibrer
EP0019383B1 (de) * 1979-05-15 1982-06-23 Imperial Chemical Industries Plc Spinnverfahren
JPS55163212A (en) * 1979-06-06 1980-12-19 Mitsui Petrochem Ind Ltd Production of phenolic resin fiber

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Publication number Publication date
JPS59179811A (ja) 1984-10-12
FR2543169B1 (fr) 1986-03-28
JPH059525B2 (de) 1993-02-05
FR2543169A1 (fr) 1984-09-28
EP0122836A1 (de) 1984-10-24
US5055241A (en) 1991-10-08
DE3462703D1 (en) 1987-04-23

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