ES2606383T3 - Non-woven of very fine fibers and paper-type products as well as procedures for their production - Google Patents
Non-woven of very fine fibers and paper-type products as well as procedures for their production Download PDFInfo
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- ES2606383T3 ES2606383T3 ES13718498.2T ES13718498T ES2606383T3 ES 2606383 T3 ES2606383 T3 ES 2606383T3 ES 13718498 T ES13718498 T ES 13718498T ES 2606383 T3 ES2606383 T3 ES 2606383T3
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/009—Condensation or reaction polymers
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
Procedimiento para la producción de no tejidos de fibras finísimas o productos de tipo papel a partir de masas fundidas de resina de bajo peso molecular, termoplásticas, reactivas, caracterizado por que se producen las masas fundidas de resina en medios gaseosos con una velocidad del gas en el intervalo de 0,2 < Ma < 1,0 a una temperatura del medio gaseoso por encima de la temperatura de fusión de la resina de bajo peso molecular usada, usándose una barra de hilado y generando la corriente de gas de soplado un campo de flujo heterogéneo, de tal manera que las masas fundidas de resina que salen de la tobera se estiran en primer lugar hasta dar formaciones de fibras finísimas y se dividen y se produce una formación de copos, los copos se depositan hasta dar un no tejido de fibras finísimas o productos de tipo papel y las resinas de bajo peso molecular termoplásticas se transforman mediante condensación en resinas duroplásticas.Process for the production of nonwovens of very fine fibers or paper-type products from low molecular weight, thermoplastic, reactive resin melts, characterized in that the resin melts are produced in gaseous media with a gas velocity in the range of 0.2 <Ma <1.0 at a temperature of the gaseous medium above the melting temperature of the low molecular weight resin used, using a spinning rod and the flow of blowing gas generating a field of blowing heterogeneous flow, in such a way that the resin melts that leave the nozzle are stretched first to give very fine fiber formations and divide and form a flake formation, the flakes are deposited until a non-woven fiber Very fine or paper-type products and thermoplastic low molecular weight resins are transformed by condensation into duroplastic resins.
Description
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DESCRIPCIONDESCRIPTION
No tejidos de fibras fimsimas y productos de tipo papel as^ como procedimientos para su produccionNon-woven of very fine fibers and paper-type products as well as procedures for their production
La invencion se refiere a no tejidos de fibras fimsimas y a productos de tipo papel que comprenden formaciones de copos fibrosas, depositadas en plano, de masas fundidas de resina de bajo peso molecular que han solidificado de forma vftrea, reactivas y capaces de formar polfmeros. Una formacion de polfmeros continua y/o funcionalizacion se desencadena mediante la accion exterior posterior dirigida de reactantes o catalizadores lfquidos o gaseosos. Ademas, la invencion se refiere a un procedimiento para la produccion de los no tejidos de fibras fimsimas y productos de tipo papel.The invention relates to non-woven of very fine fibers and paper-type products comprising fibrous flake formations, deposited in flat form, of low molecular weight resin melts that have solidified vortex, reactive and capable of forming polymers. A continuous formation of polymers and / or functionalization is triggered by the directed rearward external action of liquid or gaseous reactants or catalysts. In addition, the invention relates to a process for the production of nonwovens of very fine fibers and paper-type products.
Habitualmente, en la produccion de no tejidos de fibras fimsimas a partir de masas fundidas de polfmero con diametros de fibra por debajo de 10 pm se usan los denominados procedimientos de soplado en estado fundido (meltblown). A este respecto, el chorro de masa fundida que sale de la tobera se estira hasta dar fibras finas mediante una corriente de gas. Existe una pluralidad de distintas realizaciones. Es caractenstica una disposicion en paralelo o desplazada de toberas de hilado y el uso de aire caliente a alta velocidad para el estiramiento de los filamentos individuales. En caso de una corriente masica suficientemente alta de gas de soplado, el hilo individual se estira mucho y se rompe al alcanzar el lfmite de rotura. Se produce una distribucion estocastica de la longitud de fibra. En el documento de patente WO 2006 / 037371 se describe un procedimiento en el que se estiran de manera muy fina fibras sin fin. A este respecto, la corriente de gas que se aplica esta muy limitada mediante una presion previa maxima y las temperaturas del aire se situan en el intervalo de 15 a 120 °C a temperaturas del polfmero fundido de 300 a 400 °C. El planteamiento de objetivos del procedimiento es generar filamentos sin fin sin roturas de hilo y sin adherencias de las fibras finas entre sf. A este respecto, la corriente masica de aire de soplado esta limitada por las condiciones indicadas de presion, se emplean polfmeros termoplasticos.Usually, in the production of nonwovens of very fine fibers from polymer melts with fiber diameters below 10 pm, the so-called meltblown melting processes are used. In this regard, the jet of molten mass leaving the nozzle is stretched to fine fibers by a gas stream. There is a plurality of different embodiments. A parallel or displaced arrangement of spinning nozzles and the use of hot air at high speed for stretching the individual filaments is characteristic. In case of a sufficiently high mass flow of blowing gas, the individual wire stretches a lot and breaks when it reaches the breaking limit. Stochastic distribution of fiber length occurs. WO 2006/037371 describes a process in which endless fibers are stretched very thinly. In this regard, the gas stream that is applied is very limited by a maximum prepressure and the air temperatures are in the range of 15 to 120 ° C at molten polymer temperatures of 300 to 400 ° C. The objective of the procedure is to generate endless filaments without thread breakage and without adhesion of fine fibers between sf. In this regard, the mass flow of blow air is limited by the indicated pressure conditions, thermoplastic polymers are used.
Aparte de las corrientes de gas calientes se describe tambien una construccion tecnica especial de la tobera para la generacion de fibras fimsimas mediante el uso de temperaturas del aire de 140 a 230 °C a temperaturas de fusion de 240 a 330 °C en la patente DE 33 41 590. Resultan fibras finas con diferente longitud. Ciertamente, tambien en este caso es posible generar fibras muy finas < 5 pm, a este respecto, no obstante, el acortamiento de fibra aumenta claramente.Apart from the hot gas streams, a special technical construction of the nozzle for the generation of very thin fibers is also described by using air temperatures of 140 to 230 ° C at melting temperatures of 240 to 330 ° C in the DE patent 33 41 590. Fine fibers with different length result. Certainly, also in this case it is possible to generate very fine fibers <5 pm, in this respect, however, the fiber shortening clearly increases.
En el documento US 7.585.454 B2 estan descritos un procedimiento de soplado en estado fundido y un dispositivo para la produccion de no tejidos de fibras de polfmeros orientables, en particular de poli(tereftalato de etileno). En este procedimiento se extruye una masa fundida de polfmero en forma de fibras, que se estiran por una corriente circundante de aire caliente a alta velocidad. Sin embargo, la corriente de aire caliente no es tan intensa que en ese caso se fraccionen las fibras. Gracias a una conduccion controlada de la temperatura en varios pasos se consigue un entrelazamiento o una adhesion. Las fibras se depositan unas sobre otras en varias capas y se cortan.In US 7,585,454 B2, a meltblowing process and a device for the production of nonwovens of orientable polymer fibers, in particular poly (ethylene terephthalate) are described. In this process, a polymer melt is extruded in the form of fibers, which are stretched by a surrounding stream of hot air at high speed. However, the hot air stream is not so intense that in that case the fibers are fractionated. Thanks to a controlled temperature conduction in several steps, interlacing or adhesion is achieved. The fibers are deposited on top of each other in several layers and cut.
El objeto del documento WO 92/16361 es un procedimiento de moldeo por soplado para la produccion de no tejidos con al menos dos capas de distintos tipos de fibras. Las fibras se mezclan de forma turbulenta despues de la extrusion en, en cada caso, una corriente de gas de alta velocidad, por ejemplo, en una corriente de aire. En las zonas en las que se solapan las corrientes de gas, los distintos tipos de fibras se unen y/o entrelazan entre srThe object of WO 92/16361 is a blow molding process for the production of nonwovens with at least two layers of different types of fibers. The fibers are mixed turbulently after extrusion in, in each case, a high velocity gas stream, for example, in an air stream. In the areas where the gas streams overlap, the different types of fibers are joined and / or intertwined between sr
En el documento DE 199 29 709 esta descrito un procedimiento para la produccion de fibras de no tejido sin fin finas. En este caso se fraccionan las hebras de fibras por una corriente de gas. Este efecto se consigue mediante el empleo de una tobera de Laval y el ajuste de condiciones de flujo supercntico con velocidades del aire en el denominado intervalo supersonico. A este respecto se generan velocidades de gas mayores que la velocidad del sonido. En este procedimiento es desventajoso que se debe observar una construccion especial de la tobera y numeros de Mach Ma > 1 o una relacion de las presiones de gas p(a)/p(i) > 0,525, es decir, una denominada relacion de presion cntica, para conseguir un reventon de la hebra de fibra en muchos filamentos fimsimos sin fin o practicamente sin fin.In DE 199 29 709 a process for the production of fine endless nonwoven fibers is described. In this case the fiber strands are fractionated by a gas stream. This effect is achieved through the use of a Laval nozzle and the adjustment of super-quantum flow conditions with air velocities in the so-called supersonic interval. In this respect, gas velocities greater than the speed of sound are generated. In this procedure it is disadvantageous that a special construction of the nozzle and Mach Ma numbers> 1 or a ratio of the gas pressures p (a) / p (i)> 0.525, that is, a so-called pressure ratio must be observed In order to achieve a burst of the fiber strand in many extremely endless or practically endless filaments.
Las masas fundidas de resina de bajo peso molecular, reactivas, adecuadas para la formacion de polfmero, a causa de las propiedades fisicoqmmicas basicamente no son adecuadas para formar no tejidos de fibras. A pesar de esto esta descrito un procedimiento de este tipo en el documento de patente WO 2006/100041. Las fibras se estiran a traves de una construccion especial de tobera en la corriente de gas, se desprenden con distribucion estocastica y dan lugar a fibras fimsimas en un estrato aleatorio con diferentes longitudes de fibra. A continuacion, las fibras se tratan con un medio que desencadena una reticulacion molecular tridimensional y, en un endurecimiento termico posterior, se autoadhieren y/o endurecen en el no tejido.The low molecular weight resin melts, reactive, suitable for polymer formation, because of the physicochemical properties are basically not suitable for forming fiber nonwovens. Despite this, such a procedure is described in patent document WO 2006/100041. The fibers are stretched through a special nozzle construction in the gas stream, detached with stochastic distribution and give rise to very thin fibers in a random stratum with different fiber lengths. The fibers are then treated with a medium that triggers a three-dimensional molecular cross-linking and, in a subsequent thermal hardening, self-adheres and / or hardens in the nonwoven.
A causa del gran poder adhesivo de las masas fundidas de resina reactivas, sin embargo, en el caso de caudales de aire de soplado economicamente razonables por una resina que se adhiere y solidifica rapidamente se producen en la zona de la tobera formaciones de costras descontroladas, que alteran extremadamente el proceso de hilado. Este efecto negativo se intensifica debido al paso de masa fundida habitualmente reducido en los procedimientos convencionales por perforacion de tobera. Estas desventajas se encuentran frente a un rendimiento de hilado y un tiempo de parada de la instalacion economicamente razonables con una realizacion simultanea de la formacion deBecause of the high adhesive power of the reactive resin melts, however, in the case of economically reasonable blow air flow rates by a resin that adheres and solidifies rapidly, uncontrolled scab formations occur in the nozzle area, which extremely alter the spinning process. This negative effect is intensified due to the passage of melt usually reduced in conventional nozzle drilling procedures. These disadvantages are in the face of spinning performance and economically reasonable installation downtime with a simultaneous realization of the formation of
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fibras fimsimas requerida para una posterior formacion continua de poKmero y, dado el caso, funcionalizacion de los no tejidos de resina reactiva.Very minimal fibers required for subsequent continuous formation of polymer and, if necessary, functionalization of nonwoven reactive resin.
Por tanto, un objetivo de la invencion es desarrollar un procedimiento economico para la produccion de no tejidos de fibras fimsimas y productos de tipo papel que trabaje con numeros de Mach Ma < 1, es decir, por debajo de la velocidad del sonido, y que aproveche la autoadherencia de las masas fundidas de resina de bajo peso molecular de forma ventajosa. Ahora se ha encontrado, sorprendentemente, que en la combinacion de resinas de bajo peso molecular con toberas de hilado habituales para el procedimiento de soplado en estado fundido, velocidades de gas preferentemente en el intervalo de flujos de gas compresibles con 0,2 < Ma < 1 y temperaturas de gas por encima de la temperatura de fusion de las resinas, se produce un reventon de las hebras de fibra. De este modo se pueden conseguir de forma asegurada finuras de fibra claramente por debajo de 5 pm, sin que se deba registrar un acortamiento demasiado intenso de la longitud de la fibra. Al mismo tiempo se aprovecha que con una conduccion adecuada de gas, una velocidad adecuada de gas y de masa fundida, temperatura adecuada de gas y de masa fundida y una relacion adecuada de longitud a diametro de la tobera, estas fibras no se fraccionan solo unidimensionalmente, sino que se ensanchen directamente despues de la tobera y, mediante ramificaciones y adherencias, forman preferentemente formaciones bidimensionales que se mantienen sujetas solo a traves de travesanos fibrosos fimsimos. Las mismas se denominan en lo sucesivo copos. Esto se explica porque, adicionalmente a una grna correspondiente del proceso, se usa una barra de hilado, es decir, las toberas estan dispuestas en una fila y terminan con la superficie de la barra de hilado. El gas en primer lugar fluye de forma laminar y en el mismo sentido con la masa fundida de resina saliente, inmediatamente despues se arremolina la corriente de gas. Esto tiene como consecuencia que la corriente de gas que sopla genera un campo de flujo heterogeneo, la presion de gas no es igual a lo largo de todo el penmetro del chorro de masa fundida saliente y pueden aparecer movimientos transversales y turbulencias, lo que conduce a ensanchamientos, en parte con adherencias, de las fibrillas partidas ya despues de la salida de la tobera. Adicionalmente, estos ensanchamientos son causados por las altas temperaturas de gas, que conducen a que con los compuestos de bajo peso molecular comienzan reacciones de reticulacion con formacion de gas. Asimismo se favorece la formacion de copos mediante pequenas burbujas de gas contenidas eventualmente en la masa fundida. Despues de abandonar la tobera y la cafda asociada a ello de presion comienza una separacion de fases y las pequenas burbujas de gas aumentan de tamano, lo que reduce adicionalmente las fuerzas de cohesion en la masa fundida y respalda una formacion de fibras de la masa fundida y, por tanto, la formacion de copos (vease la Figura 1).Therefore, an objective of the invention is to develop an economic process for the production of non-woven of very fine fibers and paper-type products that work with Mach Ma <1 numbers, that is, below the speed of sound, and that take advantage of the self-adhesion of low molecular weight resin melts advantageously. It has now been found, surprisingly, that in the combination of low molecular weight resins with spinning nozzles customary for the melt blowing process, gas velocities preferably in the range of compressible gas flows with 0.2 <Ma < 1 and gas temperatures above the melting temperature of the resins, a burst of the fiber strands occurs. In this way, fiber finenesses can be achieved clearly below 5 pm, without overly shortening the fiber length. At the same time it is used that with an adequate gas line, an adequate gas and melt speed, an adequate gas and melt temperature and an adequate length to diameter of the nozzle, these fibers are not fractionated only one-dimensionally. , but that they widen directly after the nozzle and, by means of ramifications and adhesions, they preferably form two-dimensional formations that remain held only through very thin fibrous crossings. They are hereinafter referred to as flakes. This is explained because, in addition to a corresponding process thread, a spinning rod is used, that is, the nozzles are arranged in a row and terminate with the spinning rod surface. The gas first flows in a laminar form and in the same direction with the molten resin mass, immediately after the gas stream swirls. This has as a consequence that the blowing gas stream generates a heterogeneous flow field, the gas pressure is not equal along the entire penimeter of the outgoing molten jet and transverse movements and turbulence may occur, which leads to widening, partly with adhesions, of the split fibrils and after the exit of the nozzle. Additionally, these widenings are caused by high gas temperatures, which lead to the formation of gas forming crosslinking compounds with low molecular weight. Likewise, flake formation is favored by small gas bubbles eventually contained in the melt. After leaving the nozzle and the coffee associated with it pressure begins a phase separation and the small gas bubbles increase in size, which further reduces the forces of cohesion in the melt and supports a formation of fibers of the melt and, therefore, the formation of flakes (see Figure 1).
Este resultado es sorprendente, ya que segun la comprension hasta la fecha en cuanto a la tecnologfa de soplado en estado fundido ciertamente era posible observar basicamente un estiramiento de los filamentos individuales y un desprendimiento estocastico de esos filamentos dependiendo de la velocidad de la corriente de gas. Hasta ahora, una division de fibra con formacion de fibras sin fin finas se habfa observado solo con una construccion especial de tobera (tobera de Laval) en condiciones de flujo supercntico, en caso del uso de compuestos de bajo peso molecular se formaban fibras fimsimas (fibridas) mediante corrientes de gas laminares alrededor del chorro de masa fundida saliente, hasta ahora no se habfa informado de una formacion de copos. Ademas, es sorprendente que a pesar de la formacion de copos, es decir, de la aparicion de autoadherencias y ramificaciones, se deposita, antes de la deposicion de no tejido, una tela no tejida uniforme que presenta un gramaje uniforme y una superficie regular.This result is surprising, since according to the understanding to date in terms of melt blown technology, it was certainly possible to observe basically a stretch of the individual filaments and a stochastic detachment of those filaments depending on the velocity of the gas stream . Until now, a fiber division with formation of fine endless fibers had been observed only with a special nozzle construction (Laval nozzle) under super-quantum flow conditions, in case of the use of low molecular weight compounds, very thin fibers were formed ( fibrides) by means of laminar gas streams around the jet of molten outgoing mass, until now no formation of flakes had been reported. In addition, it is surprising that despite the formation of flakes, that is, the appearance of self-adhesions and ramifications, a uniform non-woven fabric having a uniform weight and a regular surface is deposited before the non-woven deposition.
Para este procedimiento, las toberas estan dispuestas preferentemente no en la punta de conos de tobera, tal como en el documento WO 2006/100041 A1, sino unas al lado de otras en una barra de hilado. Son condiciones preferentes del proceso: un paso de masa fundida por tobera de entre 1,0 y 1,8g/min, de forma particularmente preferente de aproximadamente 1,44g/min, una temperatura de la masa fundida entre 120 y 130 °C, de forma particularmente preferente 130 °C, una temperatura de la corriente de gas entre 190 y 230 °C, de forma particularmente preferente 220 °C y velocidades de la corriente de gas de 300 m/s. La corriente de gas es preferentemente una corriente de aire caliente.For this procedure, the nozzles are preferably arranged not at the tip of nozzle cones, such as in WO 2006/100041 A1, but next to each other in a spinning bar. Preferred process conditions are: a melt passage per nozzle of between 1.0 and 1.8g / min, particularly preferably about 1.44g / min, a melt temperature between 120 and 130 ° C, particularly preferably 130 ° C, a gas stream temperature between 190 and 230 ° C, particularly preferably 220 ° C and gas stream velocities of 300 m / s. The gas stream is preferably a stream of hot air.
Por consiguiente, el objeto de la invencion es un procedimiento para la produccion de no tejidos de fibras fimsimas y productos de tipo papel a partir de masas fundidas de resina de bajo peso molecular, termoplasticas, reactivas, que esta caracterizado por que las masas fundidas de resina se producen en medios gaseosos con una velocidad de gas en el intervalo de 0,2 < Ma < 1,0 a una temperatura del medio gaseoso por encima de la temperatura de fusion de la resina de bajo peso molecular usada, estirandose las masas fundidas de resina que salen de la tobera en primer lugar hasta dar formaciones de fibras fimsimas y fraccionandose y realizandose una formacion de copos, depositandose los copos hasta dar un no tejido de fibras fimsimas o hasta dar productos de tipo papel y transformandose las resinas de bajo peso molecular termoplasticas mediante condensacion en resinas duroplasticas.Accordingly, the object of the invention is a process for the production of nonwovens of very thin fibers and paper-type products from low molecular weight, thermoplastic, reactive resin melts, which is characterized in that the melts of Resins are produced in gaseous media with a gas velocity in the range of 0.2 <Ma <1.0 at a temperature of the gaseous medium above the melting temperature of the low molecular weight resin used, the melts being stretched of resin that leave the nozzle in the first place until forming very thin fibers and fractioning and forming a formation of flakes, depositing the flakes until giving a non-woven of very thin fibers or even giving paper-type products and transforming the resins of low weight molecular thermoplastics by condensation in duroplastic resins.
El diametro de fibra individual en los no tejidos de fibras fimsimas de acuerdo con la invencion o productos de tipo papel asciende a menos de 5 pm. Ya que se trata de formaciones a modo de copos, no se quiere decir el diametro de fibras individuales en el sentido mas riguroso. Se quiere decir mas bien el diametro de las ramificaciones fibrosas y travesanos en los copos que presentan tambien siempre una distribucion de diametro de fibra. Estos diametros de fibras se encuentran en un intervalo de 0,5 a 5 pm. Las fibras estan compuestas de masas fundidas de resina que han solidificado de forma vftrea, reactivas y que son capaces de formar polfmeros y estan presentes en forma de copos de fibras. Los copos presentan en primer lugar todavfa propiedades termoplasticas. La consecucion de unaThe diameter of individual fiber in the nonwovens of very thin fibers according to the invention or paper type products amounts to less than 5 pm. Since these are flake-like formations, the diameter of individual fibers in the strictest sense is not meant. Rather, it is meant the diameter of the fibrous and transverse branches in the flakes that also always have a fiber diameter distribution. These fiber diameters are in a range of 0.5 to 5 pm. The fibers are composed of resin melts that have solidified in a reactive form, are reactive and are capable of forming polymers and are present in the form of fiber flakes. The flakes first have thermoplastic properties. The achievement of a
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formacion continua de poKmero, dado el caso con una funcionalizacion acoplada, es causada mediante la accion posterior dirigida de catalizadores Kquidos o gaseosos u otros reactantes. Solo entonces existen propiedades duroplasticas.Continuous formation of polymer, if necessary with a coupled functionalization, is caused by the directed subsequent action of liquid or gaseous catalysts or other reactants. Only then do duroplastic properties exist.
Descripcion de las figuras:Description of the figures:
La Figura 1 muestra, esquematicamente, una tobera de hilado (1) de la que sale un chorro de masa fundida (2). Debido a la cafda asociada a ello de la presion comienza un crecimiento de las burbujas de gas (3).Figure 1 shows, schematically, a spinning nozzle (1) from which a jet of molten mass (2) comes out. Due to the coffee associated with it the pressure begins a growth of gas bubbles (3).
La Figura 2 muestra la disposicion de las cadenas moleculares en termoplasticos habituales. Las cadenas moleculares estan entrelazadas entre sf.Figure 2 shows the arrangement of molecular chains in usual thermoplastics. The molecular chains are intertwined with each other.
La Figura 3 muestra la disposicion de los oligomeros termoplasticos en la masa fundida de resina de bajo peso molecular, tal como se usa en la presente invencion. Las masas fundidas de resina estan caracterizadas por una estructura globular con un plano de deslizamiento reactivo en la superficie. Por tanto, la masa fundida de resina no muestra ningun comportamiento marcado de viscosidad intrmseca, a diferencia de los termoplasticos con cadenas moleculares lineales.Figure 3 shows the arrangement of thermoplastic oligomers in the low molecular weight resin melt, as used in the present invention. The resin melts are characterized by a globular structure with a reactive sliding plane on the surface. Therefore, the resin melt does not show any marked behavior of intrinsic viscosity, unlike thermoplastics with linear molecular chains.
La Figura 4 muestra la distribucion de la temperatura en el chorro de masa fundida (2). Gracias a la corriente de gas caliente (4), la masa fundida en la zona marginal (6) muestra una viscosidad disminuida con respecto a la zona central (5), lo que posibilita la formacion de fibras del chorro de masa fundida y la formacion de copos.Figure 4 shows the temperature distribution in the melt stream (2). Thanks to the hot gas stream (4), the melt in the marginal zone (6) shows a decreased viscosity with respect to the central zone (5), which allows the formation of melt jet fibers and the formation of flakes
Las masas fundidas de resina pueden contener adicionalmente otros aditivos que influyen en las propiedades, por ejemplo, negro de humo (carbon black) como antiestatico o pigmentos para la coloracion. Son concebibles tambien agentes igmfugos para optimizar el efecto de proteccion contra llamas o agentes modificadores de la viscosidad, por ejemplo, hasta el 1 % en peso de agua o butanodioles, aparte de otros aditivos.The resin melts may additionally contain other additives that influence the properties, for example, carbon black as antistatic or coloring pigments. Fireproof agents are also conceivable to optimize the effect of protection against flame or viscosity modifying agents, for example, up to 1% by weight of water or butanediols, apart from other additives.
Los no tejidos de fibras fimsimas que se pueden obtener segun el procedimiento y los propios productos de tipo papel tambien son parte de la presente invencion. El diametro de las fibras individuales en su interior se encuentra en el intervalo de 1 a 5 pm. Con ello, las figuras individuales son claramente mas delgadas que las obtenidas segun el procedimiento de acuerdo con el documento WO 2006/100041 A1.The non-woven of very fine fibers that can be obtained according to the process and the paper-type products themselves are also part of the present invention. The diameter of the individual fibers inside is in the range of 1 to 5 pm. Thus, the individual figures are clearly thinner than those obtained according to the procedure according to WO 2006/100041 A1.
Son resinas adecuadas para este tipo de formacion de no tejido, por ejemploThey are suitable resins for this type of nonwoven formation, for example
• antudridos de hexosa mono-, di- y oligomericos, en particular antndrido de 1,2-glucosa. El antndrido de 1,2- glucosa se puede obtener mediante deshidratacion de a-glucosa al vacfo a aproximadamente 140 °C.• mono-, di- and oligomeric hexose antiseases, in particular 1,2-glucose antidrido. The 1,2-glucose antidrido can be obtained by dehydration of vacuum a-glucose at approximately 140 ° C.
• resinas de melamina-formaldetndo eterificadas con metanol (MER), en particular aquellas de acuerdo con el documento WO 2006/100041.• melamine-formaldetndo resins etherified with methanol (MER), in particular those in accordance with WO 2006/100041.
Las masas fundidas de resina de bajo peso molecular reactivas son capaces de formar polfmeros. Se diferencian en su estructura fundamentalmente de las masas fundidas de polfmero clasicas que se emplean para la produccion de fibras textiles.Reactive low molecular weight resin melts are capable of forming polymers. They differ in their structure fundamentally from the classic polymer melts that are used for the production of textile fibers.
Las mismasThe same
• estan compuestas de monomeros y/u oligomeros con 1 a 8 constituyentes de base (unidades de monomero),• are composed of monomers and / or oligomers with 1 to 8 base constituents (monomer units),
• contienen por molecula de resina al menos un grupo capaz de formar polfmeros, ademas de una gran cantidad de grupos capaces de formar puentes de hidrogeno,• contain at least one group capable of forming polymers per resin molecule, in addition to a large number of groups capable of forming hydrogen bonds,
• poseen, a causa de su gran cantidad de grupos reactivos con capacidad de formar puentes de hidrogeno, una elevada adhesividad (poder de adhesion),• have, due to their large number of reactive groups capable of forming hydrogen bonds, high adhesiveness (adhesion power),
• se pueden conformar solo con procedimientos de autohilatura hasta dar formaciones fibrosas (copos)• can conform only with self-spinning procedures to give fibrous formations (flakes)
• tienden a la formacion de oligomeros/polfmeros desencadenada termicamente,• tend to thermally triggered oligomer / polymer formation,
• solidifican a T > temperatura ambiente hasta dar cuerpos vttreos,• solidify at T> room temperature to give ground bodies,
• reticulan, en particular con la accion de compuestos cataltticos y reactantes (por ejemplo, diisocianatos, acidos organicos o inorganicos).• cross-link, in particular with the action of catalytic compounds and reactants (for example, diisocyanates, organic or inorganic acids).
Sorprendentemente, se ha encontrado que tales masas fundidas de resina reactivas a causa de su comportamiento de flujo y de formacion de hilos espedfico se dividen tambien en condiciones de flujo subcntico p(a)/p(i) < 0,528. El intervalo de velocidad requerido para ello del flujo de gas comprende el intervalo de medios gaseosos compresibles en el intervalo de 0,2 < Ma < 1,0. La temperatura del medio gaseoso se ha de seleccionar, a este respecto, por encima de la temperatura de fusion de la resina de bajo peso molecular usada. La relacion de la temperatura de gas y de fusion, medida en °C, se encuentra en T(g)/T(s) > 1,0 a 3,0.Surprisingly, it has been found that such reactive resin melts because of their flow behavior and specific thread formation are also divided into sub-quantum flow conditions p (a) / p (i) <0.528. The required speed range of the gas flow comprises the range of compressible gaseous media in the range of 0.2 <Ma <1.0. The temperature of the gaseous medium must be selected, in this regard, above the melting temperature of the low molecular weight resin used. The gas and melting temperature ratio, measured in ° C, is found in T (g) / T (s)> 1.0 to 3.0.
La condicion lfmite requerida para el efecto de la division de fibra de la mayor temperatura del flujo de gas en relacion con la temperatura de fusion de la resina en ese caso tiene un efecto adicionalmente positivo y permite una hilatura sin alteraciones con formacion de copos con alta calidad y productividad.The limit condition required for the effect of the fiber division of the higher temperature of the gas flow in relation to the melting temperature of the resin in that case has an additionally positive effect and allows a spinning without alterations with the formation of flakes with high quality and productivity.
55
1010
15fifteen
20twenty
2525
3030
3535
4040
45Four. Five
50fifty
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Otras posibilidades de influencia radican en la influencia de turbulencias a la salida del chorro de masa fundida de las toberas mediante variacion de la diferencia de velocidad entre corriente de masa fundida y corriente de gas, en la influencia de la uniformidad del flujo de gas a lo largo del penmetro del chorro de masa fundida (tobera en fila, tobera conica) y en la geometna de tobera (rendija de aire, rendija terminal, desplazamiento hacia atras (air gap, end gap, set back)).Other possibilities of influence lie in the influence of turbulence at the outlet of the jet of molten mass of the nozzles by varying the difference in velocity between melt stream and gas stream, in the influence of the uniformity of the gas flow at length of the melt jet penimeter (row nozzle, conical nozzle) and nozzle geometry (air slit, terminal slit, backward displacement (air gap, end gap, set back)).
En la combinacion descrita de las masas fundidas de resina de bajo peso molecular reactivas, de las velocidades de gas en el intervalo de los medios compresibles con 0,2 < Ma < 1,0 y temperaturas de la corriente de gas que se encuentran en la relacion 1,0 a 3,0 por encima de la temperatura de fusion de la resina resulta que es suficiente ya una resistencia de forma F suficientemente grandeIn the described combination of reactive low molecular weight resin melts, the gas velocities in the range of compressible media with 0.2 <Ma <1.0 and gas stream temperatures found in the ratio 1.0 to 3.0 above the melting temperature of the resin turns out to be sufficient and a sufficiently large resistance F
F = k ■ (p /2 > ■ w2 ■ A (St)F = k ■ (p / 2> ■ w2 ■ A (St)
para dividir la corriente de masa fundida con una posterior formacion de copos. La velocidad de la corriente de gas es menor queto divide the melt stream with subsequent flake formation. The speed of the gas stream is less than
w = ^TK'R(kyT(a)w = ^ TK'R (kyT (a)
conwith
dondewhere
k = factor de resistencia de forma, p = densidad del gas, w = velocidad de la corriente de gas,k = form strength factor, p = gas density, w = gas stream velocity,
A(St) = seccion transversal de afluencia,A (St) = cross section of influx,
T(a) = temperatura de gas en el exterior,T (a) = outside gas temperature,
T(i) = temperatura de gas en el interior (dentro del recipiente a presion), p(a) = presion de gas en el exterior,T (i) = gas temperature inside (inside the pressure vessel), p (a) = gas pressure outside,
p(i) = presion de gas en el interior (dentro del recipiente a presion)p (i) = gas pressure inside (inside the pressure vessel)
K = exponente de isentropfa y R(k) = constante de gas)K = isentropha exponent and R (k) = gas constant)
Las masas fundidas de resina de bajo peso molecular reactivas se pueden fundir en una extrusora o se pueden suministrar a traves de un evaporador de capa delgada directamente a la barra de hilado de una instalacion de soplado en estado fundido. Al observar las condiciones lfmite en la zona de la tobera se obtienen fibras muy finas con un diametro menor de 5 pm, que entonces mediante autoadherencia y ramificaciones abandonan la barra de hilado en forma de copos. Estos copos se depositan sobre una cinta transportadora. Las condiciones de temperatura y separacion entre la tobera y la cinta de deposicion y transportadora son variables, de tal manera que se pueden ajustar el tamano de los copos asf como la densidad de deposicion. Se pueden producir estructuras de no tejido y de tipo papel mas sueltas, pero tambien muy compactas.The reactive low molecular weight resin melts can be melted in an extruder or can be supplied through a thin layer evaporator directly to the spinning rod of a molten blow molding installation. When observing the limit conditions in the area of the nozzle, very fine fibers with a diameter of less than 5 pm are obtained, which then by means of self-adhesion and branches leave the spinning bar in the form of flakes. These flakes are deposited on a conveyor belt. The temperature and separation conditions between the nozzle and the deposition and conveyor belt are variable, so that the size of the flakes can be adjusted as well as the deposition density. Looser non-woven and paper type structures can be produced, but also very compact.
En una forma de realizacion particular, el no tejido depositado se puede procesar tambien sin las etapas necesarias para la produccion de papel de la suspension y el arremolinado de las fibras individuales directamente hasta dar productos de tipo papel. Para esto solo se tiene que humedecer el no tejido depositado y prensarse en caliente posteriormente. A este respecto, el lfquido anadido actua como lubricante y causa una reorganizacion de los copos fibrosos. En una forma de realizacion particular se puede emplear agua como lubricante. Se produce un material plano de tipo papel con una superficie lisa. A este respecto, las fuerzas de sujecion entre las fibras individuales no resultan tal como en papeles "clasicos" a partir de enlaces qmmicos y enlaces de puente de hidrogeno, o como en los estratos aleatorios termoplasticos calandrados a partir de las fusiones de las fibras entre sf, sino a partir de los entrelazamientos y enganches de los copos aminoplasticos de fibras fimsimas y su alta resistencia a la flexion. Tambien se puede prescindir de la adicion de fibras de union o aglutinantes para una mejor resistencia de los papeles.In a particular embodiment, the deposited nonwoven can also be processed without the necessary steps for the production of paper from the suspension and the swirling of the individual fibers directly to give paper products. For this, you just have to moisten the deposited nonwoven and heat press it later. In this regard, the added liquid acts as a lubricant and causes a reorganization of the fibrous flakes. In a particular embodiment, water can be used as a lubricant. A flat paper-like material with a smooth surface is produced. In this regard, the clamping forces between the individual fibers do not result as in "classical" papers from chemical bonds and hydrogen bridge bonds, or as in the thermoplastic random strands calendered from the fusions of the fibers between sf, but from the entanglements and hooks of the aminoplastic flakes of very thin fibers and their high resistance to bending. It is also possible to dispense with the addition of binding fibers or binders for better paper strength.
Los papeles que se producen se caracterizan por una elevada resistencia a la llama y al calor y se pueden emplear como aislante electrico. Poseen una elevada resistencia a descarga disruptiva, elevada resistencia de formaThe papers produced are characterized by high resistance to flame and heat and can be used as an electrical insulator. They have a high resistance to disruptive discharge, high resistance of form
despues del procesamiento y presentan solo una reducida deformacion de retorno elastica. Los papeles de materiales duroplasticos se producen a partir de un precursor termoplastico de los precondensados oligomericos en un procedimiento directo. La parte en peso de aminoplasto en el papel asciende al 95 % o mas. Puede ascender tambien al 100 % en peso. Gracias a la etapa del prensado en caliente se pueden ajustar el espesor del papel y laafter processing and have only a reduced elastic return deformation. Duroplastic material papers are produced from a thermoplastic precursor of oligomeric precondensates in a direct process. The weight part of aminoplast in the paper amounts to 95% or more. It can also amount to 100% by weight. Thanks to the hot pressing stage you can adjust the thickness of the paper and the
5 resistencia de union. Para aumentar la resistencia, la flexibilidad y la union de fibras, antes del calandrado en5 bond strength. To increase strength, flexibility and fiber bonding, before calendering in
caliente se puede anadir hasta el 5 % en peso de precondensado duromerico (dispersion, solucion, polvo) o partes termoplasticas, tales como PVC, PA o PEEK, en forma de dispersion, solucion o polvo.Hot can add up to 5% by weight of duromeric pre-condensate (dispersion, solution, powder) or thermoplastic parts, such as PVC, PA or PEEK, in the form of dispersion, solution or powder.
El no tejido o producto de tipo papel producido de este modo se suministra a otro paso del procedimiento en el que 10 se pone en contacto un reactante o catalizador lfquido o gaseoso con el producto plano. Con ello se consigue una formacion de polfmero o funcionalizacion de la masa fundida de resina. En caso necesario se pueden incluir otros pasos de tratamiento, por ejemplo para la neutralizacion de los reactantes o catalizadores.The nonwoven or paper-like product produced in this way is supplied to another step of the process in which a liquid or gaseous reactant or catalyst is contacted with the flat product. This results in a polymer formation or functionalization of the resin melt. If necessary, other treatment steps may be included, for example for the neutralization of reactants or catalysts.
En una etapa adicional de tratamiento se someten los productos planos a un tratamiento termico. Las temperaturas 15 requeridas de tratamiento se deben ajustar en una relacion de 1,0 a 4,0 en relacion con la temperatura de fusion (enIn an additional stage of treatment the flat products are subjected to a thermal treatment. The required treatment temperatures 15 must be adjusted in a ratio of 1.0 to 4.0 in relation to the melting temperature (in
°C) de la resina.° C) of the resin.
Los no tejidos o productos de tipo papel producidos de este modo se pueden emplear para aplicaciones textiles y tecnicas. Son propiedades particulares de los productos del procedimiento resistencia a la llama, elevada 20 temperatura de uso continuo, capacidad de absorcion del sonido y propiedades electricas espedficas.Nonwovens or paper products produced in this way can be used for textile and technical applications. Particular properties of the products of the process are flame resistance, high temperature of continuous use, sound absorption capacity and specific electrical properties.
Claims (9)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102012007080 | 2012-04-11 | ||
| DE102012007080 | 2012-04-11 | ||
| PCT/EP2013/001062 WO2013152858A1 (en) | 2012-04-11 | 2013-04-11 | Superfine-fibre non-wovens and paper-like products and method for the production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| ES2606383T3 true ES2606383T3 (en) | 2017-03-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| ES13718498.2T Active ES2606383T3 (en) | 2012-04-11 | 2013-04-11 | Non-woven of very fine fibers and paper-type products as well as procedures for their production |
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| Country | Link |
|---|---|
| EP (1) | EP2836632B1 (en) |
| DE (1) | DE102013006212A1 (en) |
| ES (1) | ES2606383T3 (en) |
| PL (1) | PL2836632T3 (en) |
| SI (1) | SI2836632T1 (en) |
| WO (1) | WO2013152858A1 (en) |
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| DE102017123611A1 (en) | 2016-10-11 | 2018-04-12 | Smartmelamine D.O.O. | Low-emission melamine-formaldehyde nonwovens and nonwovens |
| DE102020116689A1 (en) | 2020-06-24 | 2021-12-30 | Thüringisches Institut für Textil- und Kunststoff-Forschung Rudolstadt e.V. | Melamine resin filter fleece |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3972759A (en) * | 1972-06-29 | 1976-08-03 | Exxon Research And Engineering Company | Battery separators made from polymeric fibers |
| US4526733A (en) | 1982-11-17 | 1985-07-02 | Kimberly-Clark Corporation | Meltblown die and method |
| NZ217669A (en) * | 1985-10-02 | 1990-03-27 | Surgikos Inc | Meltblown microfibre web includes core web and surface veneer |
| WO1992016361A1 (en) | 1991-03-20 | 1992-10-01 | Sabee Reinhardt N | Non-woven fabrics with fiber quantity gradients |
| US6368533B1 (en) * | 1997-12-22 | 2002-04-09 | Kimberly-Clark Worldwide, Inc. | Process for forming films, fibers and base webs from thermoset polymers |
| DE19929709C2 (en) | 1999-06-24 | 2001-07-12 | Lueder Gerking | Process for the production of essentially endless fine threads and use of the device for carrying out the process |
| US6667254B1 (en) * | 2000-11-20 | 2003-12-23 | 3M Innovative Properties Company | Fibrous nonwoven webs |
| EP1448814A4 (en) | 2001-10-01 | 2005-09-14 | Rtica Inc | Process of and apparatus for making an insulation product |
| WO2006037371A1 (en) | 2004-09-30 | 2006-04-13 | Saurer Gmbh & Co. Kg | Meltblown method for melt spinning fine non-woven fibres and device for carrying out said method |
| DE102005013420A1 (en) * | 2005-03-21 | 2006-09-28 | Ami-Agrolinz Melamine International Gmbh | Process for the production of thermoset Feinstfaservliesen with high flame, thermal and sound insulation effect |
-
2013
- 2013-04-11 DE DE102013006212A patent/DE102013006212A1/en not_active Withdrawn
- 2013-04-11 ES ES13718498.2T patent/ES2606383T3/en active Active
- 2013-04-11 EP EP13718498.2A patent/EP2836632B1/en active Active
- 2013-04-11 WO PCT/EP2013/001062 patent/WO2013152858A1/en active Application Filing
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- 2013-04-11 PL PL13718498T patent/PL2836632T3/en unknown
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| DE102013006212A1 (en) | 2013-10-17 |
| SI2836632T1 (en) | 2017-01-31 |
| WO2013152858A1 (en) | 2013-10-17 |
| PL2836632T3 (en) | 2017-03-31 |
| EP2836632B1 (en) | 2016-09-14 |
| EP2836632A1 (en) | 2015-02-18 |
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