EP1505187A1 - Spunbonded nonwoven fabric and process for making the same - Google Patents
Spunbonded nonwoven fabric and process for making the same Download PDFInfo
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- EP1505187A1 EP1505187A1 EP03018108A EP03018108A EP1505187A1 EP 1505187 A1 EP1505187 A1 EP 1505187A1 EP 03018108 A EP03018108 A EP 03018108A EP 03018108 A EP03018108 A EP 03018108A EP 1505187 A1 EP1505187 A1 EP 1505187A1
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- Prior art keywords
- filaments
- spunbonded
- low
- component
- melting component
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Classifications
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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
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
- D04H3/147—Composite yarns or filaments
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
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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
- D04H3/007—Addition polymers
-
- 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
- D04H3/011—Polyesters
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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
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
Definitions
- the invention relates to a spunbonded nonwoven of continuous fibers and a method for producing such a spunbonded web.
- continuous fibers and by the term Filaments are theoretically infinite within the scope of the invention meant long threads, from which formed the spunbonded fabric becomes. To distinguish from this are staple fibers in which they are relatively short threads, at least in the Average much shorter than the above Filaments.
- the filaments used in the invention consist in particular of a thermoplastic material or of thermoplastic materials.
- spunbonded nonwovens which consist in particular of monofilaments, leave something to be desired with regard to their mechanical properties, in particular with regard to the tensile strength and the work absorption (maximum tensile force work). This is especially true for spunbonded nonwovens with medium and heavy basis weights from about 30 to 40 g / m 2 . Due to the limited thermal conductivity of the plastics used, it is difficult in the thermal consolidation of these spunbonded nonwovens with higher basis weights to bring sufficient energy input into the center of the spunbonded nonwoven.
- the invention is the technical problem of increasing the strength or tensile strength of spunbonded nonwovens with higher basis weights from 40 g / m 2 . Furthermore, the invention is the technical problem of specifying a method for producing such a spunbonded nonwoven.
- the invention teaches a spunbonded nonwoven fabric, wherein the continuous filaments are multi-component filaments, in particular bicomponent filaments with at least one low-melting component on the outer surface, wherein it is a spunbonded thermally bonded in a calender with a stamping surface under 22%, and wherein the spunbonded fabric has a basis weight of over 40 g / m 2 .
- Embossing surface of the calender means the effective area, the during thermal consolidation, the connection points in Spunbond or between the filaments manufactures. It So it is the area that directly adjoins the Filaments acts.
- the embossing surface of Engraving points of the gravure roll of the calender formed. It lies within the scope of the invention that as a calender Engraving roller / smooth roller pair is used. It is located in Frame of the invention that the spunbonded in a calender with an embossing surface of at least 10%, preferably of at least 12% is thermally consolidated.
- filaments used with titers between 1.8 - 2.5 denier are advantageously filaments used with titers between 1.8 - 2.5 denier. It can but also finer filaments can be used. in principle Therefore, it is within the scope of the invention with filaments Titers between 0.8 to 2.5 denier to use.
- the filaments used in the invention are preferably from a low-melting component, the the outer surface of the filament is arranged and made a higher melting component, which is the core of the Filêts forms.
- the multi-component filaments used according to the invention in particular bicomponent filaments a core-shell structure on and forms the low melting component of the coat.
- the at least one higher Melting component forms the core of the filament. It is within the scope of the invention that at a Filament with core-shell structure of the core completely of surrounded by the sheath of the low-melting component is. Moreover, it is within the scope of the invention that both the core and the coat over the entire length a filament extends.
- the low melting component has a melting point, the at least 5 ° C, preferably at least 10 ° C and very preferably at least 15 ° C lower than that Melting point of the higher melting component.
- the melting point is low melting component at least 20 ° C lower than that Melting point of the higher melting component.
- the melting point of the low-melting Component is at 120 ° C and higher.
- the low-melting Component is a polyolefin or a mixture of Polyolefins and their copolymers. According to one Embodiment of the invention is in the low-melting component to polyethylene and in the higher melting component to polypropylene.
- Polyethylene in the context of a core-shell structure so the Coat and polypropylene the core of the filament.
- a Core-shell structure realized, wherein the polypropylene copolymer the jacket and the polypropylene the core of the Fil noirs forms.
- the polypropylene copolymer it is preferably a polypropylene-polyethylene copolymer. This copolymer can be heterophasic be.
- heterophasic polypropylene-polyethylene copolymers preferably polyethylene contents of 2 to 6 Wt .-% included.
- polypropylene copolymer may instead of the polypropylene copolymer also Polypropylene terpolymer as low-melting component be used, which is preferably a Polypropylene-polyethylene-polybutylene terpolymer.
- polyethylene or polypropylene be used and as higher melting Component of a polyester can be used.
- At a preferred core-shell structure forms the polyethylene or polypropylene the jacket and the polyester the core.
- the proportion of low-melting component in the filaments 10 to 40 wt .-%, preferably 15 to 35 wt .-% is. there are the percentages by weight on the entire filament based.
- the proportion of the higher melting component Accordingly, it is preferably 90 to 60% by weight, preferably 85 to 65 wt .-%.
- the spunbonded nonwoven fabric according to the invention is expediently a spunbonded nonwoven thermally consolidated in a calender with an embossing area of less than 20%.
- the spunbonded nonwoven has a basis weight of about 50g / m 2, preferably of more than 60g / m 2.
- the invention further teaches a method for producing a spunbonded nonwoven fabric, wherein a nonwoven web is formed from continuous fibers formed as multicomponent filaments, in particular as bicomponent filaments, which filaments have a low-melting component on their outer surface, wherein the nonwoven web is thermally solidified in a calender with an emboss area less than 22% and wherein a spunbonded fabric having a basis weight of over 40g / m 2 is produced.
- connection points means in the frame the invention, the areas of the filaments due to the Exposure of the calender are softened and where Connecting points formed with adjacent filaments become.
- Connecting points formed with adjacent filaments become.
- the connection points only the outer areas of a Filaments in relation to the cross section of the filament softens and a core area is not softened or remains free of softening. This possibility offers itself especially when the melting point difference with respect to low-melting and higher-melting component is relatively high, so for example in a polyolefin as a low-melting component and a polyester as a higher melting component.
- the invention is based on the finding that due to the inventive design of the spunbonded fabric or the filaments of the spunbonded fabric in the thermal consolidation of the energy input in the middle of the nonwoven sufficient to connect the filaments on the low-melting outer material. On the other hand, a disadvantageous heat deterioration of the remaining filament areas does not take place.
- the spunbonded nonwoven according to the invention is distinguished by a surprisingly high strength or tensile strength. It can spunbonded webs with highêth facilitateen of about 40g / m 2, particularly about 50g / m 2 and especially about 60 g / m 2 are produced, which have such a surprisingly high strength or tensile strength. Specific longitudinal strengths higher than 3 are achieved at these high basis weights.
- a spunbonded non-woven fabric formed as a fine denier non-woven fabric of fibers having a denier of 1.1 was made from bicomponent filaments having a core-shell structure.
- the core of these filaments consisted of polypropylene and the coat. Polyethylene.
- the proportion of the core component was 70 wt .-% and the proportion of the shell component was 30 wt .-%.
- the fine fiber fleece had a basis weight of 45 g / m 2 . It has a longitudinal strength of 220 N / 5cm achieved and a specific longitudinal strength of 4.9.
- a fine fiber non-woven fabric of bicomponent filaments having a denier of 1.1 denier having a core-shell structure was produced.
- the core was made of polypropylene and the jacket of polyethylene.
- the proportion of the core component was 70 wt .-% and the proportion of the shell component 30 wt .-%.
- the fine fiber fleece had a basis weight of 55 g / m 2 .
- the single FIGURE shows a cross section through a with bicomponent filament used according to the invention Core-shell structure.
- the jacket 1 preferably the core and completely surrounds in the embodiment for example, polyethylene or polypropylene copolymer.
- the completely surrounded by the jacket 1 Core 2 may consist of polypropylene in the embodiment.
- this core can 2 but also made of a polyester or another Plastic with a relation to the shell component higher Softening exist.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nonwoven Fabrics (AREA)
- Multicomponent Fibers (AREA)
- Treatment Of Fiber Materials (AREA)
Abstract
Description
Die Erfindung betrifft ein Spinnvlies aus Endlosfasern sowie ein Verfahren zur Herstellung eines solchen Spinnvlieses. - Mit dem Begriff Endlosfasern und mit dem Begriff Filamente sind im Rahmen der Erfindung theoretisch unendlich lange Fäden gemeint, aus denen das Spinnvlies gebildet wird. Davon zu unterscheiden sind Stapelfasern, bei denen es sich um relativ kurze Fäden handelt, die jedenfalls im Durchschnitt viel kürzer sind als die vorgenannten Filamente. Die erfindungsgemäß eingesetzten Filamente bestehen insbesondere aus einem thermoplastischen Kunststoff bzw. aus thermoplastischen Kunststoffen.The invention relates to a spunbonded nonwoven of continuous fibers and a method for producing such a spunbonded web. - By the term continuous fibers and by the term Filaments are theoretically infinite within the scope of the invention meant long threads, from which formed the spunbonded fabric becomes. To distinguish from this are staple fibers in which they are relatively short threads, at least in the Average much shorter than the above Filaments. The filaments used in the invention consist in particular of a thermoplastic material or of thermoplastic materials.
Aus der Praxis sind eine Vielzahl von Anlagen und Verfahren zur Herstellung von Spinnvliesen bekannt. Die bekannten Spinnvliese, die insbesondere aus Monofilamenten bestehen, lassen in Bezug auf ihre mechanischen Eigenschaften, insbesondere bezüglich der Zugfestigkeit und der Arbeitsaufnahme (Höchstzugkraftarbeit) zu wünschen übrig. Das gilt vor allem für Spinnvliese mit mittleren und schweren Flächengewichten ab etwa 30 bis 40 g/m2. Aufgrund der begrenzten Wärmeleitfähigkeit der eingesetzten Kunststoffe ist es bei der thermischen Verfestigung dieser Spinnvliese mit höheren Flächengewichten schwierig einen ausreichenden Energieeintrag bis in die Mitte des Spinnvlieses zu bringen. Man versucht aber nichtsdestoweniger die Filamente der Spinnvliese bei einer thermischen Verfestigung in einem Kalander über die gesamte Dicke des Spinnvlieses möglichst in jedem Gravurpunkt zu verbinden. Dabei kann es aber zu einer Versprödung der Umgebung kommen, die ein vorzeitiges Versagen bei mechanischer Belastung des Vlieses zur Folge haben kann. - Bei niedrigen Flächengewichten wie beispielsweise 17 g/m2 werden mit üblichen Rohstoffen, zum Beispiel mit Polypropylenfilamenten und Standard-Titern (1,8 - 2 denier) Längsfestigkeiten bis etwa 50 N/5cm erreicht. Die Messung der Längsfestigkeiten erfolgt hier nach ISO 9073 Teil 3. Das entspricht einer spezifischen Festigkeit von 2,94 N/5cm:g/m2 bzw. N·m2/5cm·g. Bei ansteigendem Flächengewicht wird die spezifische Festigkeit jedoch geringer und fällt auf unter 2,5 und bei noch höherem Flächengewichten bis 2 ab. Durch den Einsatz feinerer Filamente können die Werte für die spezifische Festigkeit zwar etwas verbessert werden, jedoch kann bei höheren Flächengewichten eine 3 übersteigende spezifische Festigkeit nicht erreicht werden.From practice, a variety of plants and processes for the production of spunbonded webs are known. The known spunbonded nonwovens, which consist in particular of monofilaments, leave something to be desired with regard to their mechanical properties, in particular with regard to the tensile strength and the work absorption (maximum tensile force work). This is especially true for spunbonded nonwovens with medium and heavy basis weights from about 30 to 40 g / m 2 . Due to the limited thermal conductivity of the plastics used, it is difficult in the thermal consolidation of these spunbonded nonwovens with higher basis weights to bring sufficient energy input into the center of the spunbonded nonwoven. However, it is nonetheless attempted to connect the filaments of the spunbonded fabric in a thermal consolidation in a calender over the entire thickness of the spunbonded web as possible in each engraving point. However, this can lead to embrittlement of the environment, which can lead to premature failure under mechanical stress on the fleece. - At low basis weights such as 17 g / m 2 are achieved with conventional raw materials, for example with polypropylene filaments and standard titer (1.8 - 2 denier) longitudinal strength to about 50 N / 5cm. The measurement of the longitudinal strength is carried out here by ISO 9073 Part 3. This corresponds to a specific resistance of 2.94 N / 5 cm: g / m 2 or N · m 2 / g · 5cm. However, as the basis weight increases, the specific tenacity decreases and falls to below 2.5 and to even higher basis weights to 2. By using finer filaments, although the values for the specific strength can be improved somewhat, at higher basis weights, a specific strength exceeding 3 can not be achieved.
Demgegenüber liegt der Erfindung das technische Problem zugrunde, die Festigkeit bzw. Zugfestigkeit von Spinnvliesen mit höheren Flächengewichten ab 40 g/m2 zu erhöhen. Fernerhin liegt der Erfindung das technische Problem zugrunde, ein Verfahren zur Herstellung eines solchen Spinnvlieses anzugeben.In contrast, the invention is the technical problem of increasing the strength or tensile strength of spunbonded nonwovens with higher basis weights from 40 g / m 2 . Furthermore, the invention is the technical problem of specifying a method for producing such a spunbonded nonwoven.
Zur Lösung dieses technischen Problems lehrt die Erfindung
ein Spinnvlies aus Endlosfasern, wobei die Endlosfasern
Mehrkomponentenfilamente, insbesondere Bikomponentenfilamente
mit zumindest einer niedrig schmelzenden Komponente
an der Außenoberfläche sind,
wobei es sich um ein thermisch in einem Kalander mit einer
Prägefläche unter 22 % verfestigtes Spinnvlies handelt
und wobei das Spinnvlies ein Flächengewicht von über
40 g/m2 aufweist.To solve this technical problem, the invention teaches a spunbonded nonwoven fabric, wherein the continuous filaments are multi-component filaments, in particular bicomponent filaments with at least one low-melting component on the outer surface,
wherein it is a spunbonded thermally bonded in a calender with a stamping surface under 22%, and wherein the spunbonded fabric has a basis weight of over 40 g / m 2 .
Prägefläche des Kalanders meint die wirksame Fläche, die bei der thermischen Verfestigung die Verbindungspunkte im Spinnvlies bzw. zwischen den Filamenten herstellt. Es handelt es sich also um die Fläche, die unmittelbar auf die Filamente einwirkt. In der Regel wird die Prägefläche von Gravurpunkten der Gravurwalze des Kalanders gebildet. Es liegt im Rahmen der Erfindung, dass als Kalander ein Gravurwalzen-/Glattwalzenpaar eingesetzt wird. Es liegt im Rahmen der Erfindung, dass das Spinnvlies in einem Kalander mit einer Prägefläche von mindestens 10 %, vorzugsweise von mindestens 12 % thermisch verfestigt wird.Embossing surface of the calender means the effective area, the during thermal consolidation, the connection points in Spunbond or between the filaments manufactures. It So it is the area that directly adjoins the Filaments acts. As a rule, the embossing surface of Engraving points of the gravure roll of the calender formed. It lies within the scope of the invention that as a calender Engraving roller / smooth roller pair is used. It is located in Frame of the invention that the spunbonded in a calender with an embossing surface of at least 10%, preferably of at least 12% is thermally consolidated.
Im Rahmen der Erfindung werden zweckmäßigerweise Filamente mit Titern zwischen 1,8 - 2,5 denier eingesetzt. Es können aber auch feinere Filamente verwendet werden. Grundsätzlich liegt es deshalb im Rahmen der Erfindung Filamente mit Titern zwischen 0,8 bis 2,5 denier zu verwenden.In the context of the invention are advantageously filaments used with titers between 1.8 - 2.5 denier. It can but also finer filaments can be used. in principle Therefore, it is within the scope of the invention with filaments Titers between 0.8 to 2.5 denier to use.
Die erfindungsgemäß eingesetzten Filamente bestehen vorzugsweise aus einer niedrig schmelzenden Komponente, die an der Außenoberfläche des Filamentes angeordnet ist und aus einer höher schmelzenden Komponente, die den Kern des Filamentes bildet. Nach sehr bevorzugter Ausführungsform der Erfindung weisen die erfindungsgemäß verwendeten Mehrkomponentenfilamente, insbesondere Bikomponentenfilamente eine Kern-Mantel-Struktur auf und dabei bildet die niedrig schmelzende Komponente den Mantel. Die zumindest eine höher schmelzende Komponente bildet dagegen den Kern des Filamentes. Es liegt im Rahmen der Erfindung, dass bei einem Filament mit Kern-Mantel-Struktur der Kern vollständig von dem Mantel aus der niedrig schmelzenden Komponente umgeben ist. Außerdem liegt es im Rahmen der Erfindung, dass sich sowohl der Kern als auch der Mantel über die gesamte Länge eines Filamentes erstreckt.The filaments used in the invention are preferably from a low-melting component, the the outer surface of the filament is arranged and made a higher melting component, which is the core of the Filamentes forms. According to a very preferred embodiment of the invention have the multi-component filaments used according to the invention, in particular bicomponent filaments a core-shell structure on and forms the low melting component of the coat. The at least one higher Melting component forms the core of the filament. It is within the scope of the invention that at a Filament with core-shell structure of the core completely of surrounded by the sheath of the low-melting component is. Moreover, it is within the scope of the invention that both the core and the coat over the entire length a filament extends.
Nach sehr bevorzugter Ausführungsform der Erfindung weist die niedrig schmelzende Komponente einen Schmelzpunkt auf, der zumindest 5 °C, vorzugsweise zumindest 10 °C und sehr bevorzugt zumindest 15 °C niedriger liegt als der Schmelzpunkt der höher schmelzenden Komponente. Zweckmäßigerweise liegt der Schmelzpunkt der niedrig schmelzenden Komponente zumindest 20 °C niedriger als der Schmelzpunkt der höher schmelzenden Komponente. Vorzugsweise liegt der Schmelzpunkt der niedrig schmelzenden Komponente bei 120 °C und höher. Nach einer bevorzugten Ausführungsform der Erfindung ist die niedrig schmelzende Komponente ein Polyolefin oder eine Mischung aus Polyolefinen und ihren Copolymeren. Gemäß einer Ausführungsform der Erfindung handelt es sich bei der niedrig schmelzenden Komponente um Polyethylen und bei der höher schmelzenden Komponente um Polypropylen. Dabei bildet Polyethylen im Rahmen einer Kern-Mantel-Struktur also den Mantel und Polypropylen den Kern des Filamentes. Nach einer anderen Ausführungsform der Erfindung handelt es sich bei der niedrig schmelzenden Komponente um ein Polypropylen-Copolymerisat, dessen Erweichungspunkt bzw. Schmelzpunkt niedriger liegt als bei reinem Polypropylen. Bei dieser letztgenannten Ausführungsform besteht die höher schmelzende Komponente zweckmäßigerweise aus Polypropylen. Auch bei dieser Ausführungsform wird zweckmäßigerweise eine Kern-Mantel-Struktur verwirklicht, wobei das Polypropylen-Copolymerisat den Mantel und das Polypropylen den Kern des Filamentes bildet. Bei dem Polypropylen-Copolymerisat handelt es sich vorzugsweise um ein Polypropylen-Polyethylen-Copolymer. Dieses Copolymer kann heterophasisch sein. Es liegt aber auch im Rahmen der Erfindung nicht heterophasische Polypropylen-Polyethylen-Copolymere einzusetzen, die vorzugsweise Polyethylen-Anteile von 2 bis 6 Gew.-% enthalten. Nach einer Ausführungsform der Erfindung kann statt des Polypropylen-Copolymerisates auch ein Polypropylen-Terpolymerisat als niedrig schmelzende Komponente verwendet werden, wobei es sich bevorzugt um ein Polypropylen-Polyethylen-Polybutylen-Terpolymer handelt. Nach einer weiteren Ausführungsform der Erfindung kann als niedrig schmelzende Komponente Polyethylen oder Polypropylen eingesetzt werden und als höher schmelzende Komponente ein Polyester eingesetzt werden. Bei einer bevorzugten Kern-Mantel-Struktur bildet das Polyethylen bzw. Polypropylen den Mantel und der Polyester den Kern.According to a very preferred embodiment of the invention the low melting component has a melting point, the at least 5 ° C, preferably at least 10 ° C and very preferably at least 15 ° C lower than that Melting point of the higher melting component. Conveniently, the melting point is low melting component at least 20 ° C lower than that Melting point of the higher melting component. Preferably is the melting point of the low-melting Component at 120 ° C and higher. After a preferred Embodiment of the invention is the low-melting Component is a polyolefin or a mixture of Polyolefins and their copolymers. According to one Embodiment of the invention is in the low-melting component to polyethylene and in the higher melting component to polypropylene. It forms Polyethylene in the context of a core-shell structure so the Coat and polypropylene the core of the filament. After a Another embodiment of the invention is the low-melting component around a polypropylene copolymer, its softening point or melting point lower than pure polypropylene. At this the latter embodiment is the higher Melting component expediently of polypropylene. Also in this embodiment is suitably a Core-shell structure realized, wherein the polypropylene copolymer the jacket and the polypropylene the core of the Filamentes forms. In the polypropylene copolymer it is preferably a polypropylene-polyethylene copolymer. This copolymer can be heterophasic be. However, it is not within the scope of the invention use heterophasic polypropylene-polyethylene copolymers, preferably polyethylene contents of 2 to 6 Wt .-% included. According to one embodiment of the invention may instead of the polypropylene copolymer also Polypropylene terpolymer as low-melting component be used, which is preferably a Polypropylene-polyethylene-polybutylene terpolymer. According to a further embodiment of the invention, as low-melting component polyethylene or polypropylene be used and as higher melting Component of a polyester can be used. At a preferred core-shell structure forms the polyethylene or polypropylene the jacket and the polyester the core.
Es liegt im Rahmen der Erfindung, dass der Anteil der niedrig schmelzenden Komponente in den Filamenten 10 bis 40 Gew.-%, vorzugsweise 15 bis 35 Gew.-% beträgt. Dabei sind die Gew.-%-Angaben jeweils auf das gesamte Filament bezogen. Der Anteil der höher schmelzenden Komponente beträgt dementsprechend vorzugsweise 90 bis 60 Gew.-%, bevorzugt 85 bis 65 Gew.-%. It is within the scope of the invention that the proportion of low-melting component in the filaments 10 to 40 wt .-%, preferably 15 to 35 wt .-% is. there are the percentages by weight on the entire filament based. The proportion of the higher melting component Accordingly, it is preferably 90 to 60% by weight, preferably 85 to 65 wt .-%.
Zweckmäßigerweise handelt es sich bei dem erfindungsgemäßen Spinnvlies um ein thermisch in einem Kalander mit einer Prägefläche unter 20 % verfestigtes Spinnvlies. - Nach sehr bevorzugter Ausführungsform der Erfindung weist das Spinnvlies ein Flächengewicht von über 50g/m2, vorzugsweise von über 60g/m2 auf.The spunbonded nonwoven fabric according to the invention is expediently a spunbonded nonwoven thermally consolidated in a calender with an embossing area of less than 20%. - According to a very preferred embodiment of the invention, the spunbonded nonwoven has a basis weight of about 50g / m 2, preferably of more than 60g / m 2.
Zur Lösung des technischen Problems lehrt die Erfindung
fernerhin ein Verfahren zur Herstellung eines Spinnvlieses,
wobei eine Vliesbahn aus als Mehrkomponentenfilamente,
insbesondere als Bikomponentenfilamente ausgebildeten
Endlosfasern gebildet wird, welche Endlosfasern eine
niedrig schmelzende Komponente an ihrer Außenoberfläche
aufweisen,
wobei die Vliesbahn thermisch in einem Kalander mit einer
Prägefläche unter 22 % verfestigt wird
und wobei ein Spinnvlies mit einem Flächengewicht von über
40g/m2 erzeugt wird.To solve the technical problem, the invention further teaches a method for producing a spunbonded nonwoven fabric,
wherein a nonwoven web is formed from continuous fibers formed as multicomponent filaments, in particular as bicomponent filaments, which filaments have a low-melting component on their outer surface,
wherein the nonwoven web is thermally solidified in a calender with an emboss area less than 22%
and wherein a spunbonded fabric having a basis weight of over 40g / m 2 is produced.
Mit Hilfe des Kalanders werden Verbindungspunkte zwischen den Filamenten erzeugt. Verbindungspunkte meint im Rahmen der Erfindung die Bereiche der Filamente, die aufgrund der Einwirkung des Kalanders erweicht werden und an denen Verbindungsstellen mit benachbarten Filamenten gebildet werden. Bei einer Ausführungsform der Erfindung werden an den Verbindungspunkten lediglich die Außenbereiche eines Filamentes in Bezug auf den Querschnitt des Filaments erweicht und ein Kernbereich wird nicht erweicht bzw. bleibt erweichungsfrei. Diese Möglichkeit bietet sich insbesondere wenn die Schmelzpunktdifferenz bezüglich der niedrig schmelzenden und der höher schmelzenden Komponente relativ hoch ist, also beispielsweise bei einem Polyolefin als niedrig schmelzende Komponente und bei einem Polyester als höher schmelzende Komponente. Nach einer Ausführungsform der Erfindung wird dabei lediglich die Außenoberfläche bzw. der Mantel aus der niedrig schmelzenden Komponente zumindest zum Teil erweicht bzw. aufgeschmolzen und bleibt der Kern aus der höher schmelzenden Komponente völlig erweichungsfrei. Es liegt auch im Rahmen der Erfindung, dass die Außenoberfläche bzw. der Mantel aus der niedrig schmelzenden Komponente erweicht bzw. aufgeschmolzen wird und dass lediglich Oberflächenbereiche des Kerns erweicht bzw. aufgeschmolzen werden und der Kern ansonsten im Wesentlichen erweichungsfrei bleibt. Eine sehr bevorzugte Ausführungsform der Erfindung ist dadurch gekennzeichnet, dass die thermische Verfestigung mit der Maßgabe durchgeführt wird, dass die höher schmelzende Komponente im Bereich der Verbindungspunkte bzw. an den Verbindungspunkten vollständig oder aber im Wesentlichen erweichungsfrei bleibt. Im Wesentlichen erweichungsfrei meint dabei vorzugsweise, dass in Bezug auf den Querschnitt des Filaments an dem Verbindungspunkt 75 bis 90 Gew.-% der höher schmelzenden Komponente erweichungsfrei bleiben.With the help of the calender connecting points between produced the filaments. Connection points means in the frame the invention, the areas of the filaments due to the Exposure of the calender are softened and where Connecting points formed with adjacent filaments become. In one embodiment of the invention are on the connection points only the outer areas of a Filaments in relation to the cross section of the filament softens and a core area is not softened or remains free of softening. This possibility offers itself especially when the melting point difference with respect to low-melting and higher-melting component is relatively high, so for example in a polyolefin as a low-melting component and a polyester as a higher melting component. According to one embodiment The invention is only the outer surface or the coat of the low-melting Component at least partially softened or melted and remains the core of the higher melting component completely softening free. It is also within the scope of Invention, that the outer surface or the jacket of the softens low melting component or is melted and that only surface areas the core is softened or melted and the core otherwise remains substantially free of softening. A very preferred embodiment of the invention is characterized characterized in that the thermal consolidation with the The condition is that the higher melting Component in the area of the connection points or on the Connection points completely or in essence softening remains. Essentially softening free preferably means that in relation to the cross section of the filament at the point of connection 75 to 90% by weight of remain softening-free higher melting component.
Der Erfindung liegt die Erkenntnis zugrunde, dass aufgrund der erfindungsgemäßen Ausgestaltung des Spinnvlieses bzw. der Filamente des Spinnvlieses bei der thermischen Verfestigung der Energieeintrag, in die Mitte des Vlieses ausreicht, um die Filamente über das niedrig schmelzende Außenmaterial zu verbinden. Andererseits findet eine nachteilhafte Wärmebeeinträchtigung der übrigen Filamentbereiche nicht statt. Das führt dazu, dass das erfindungsgemäße Spinnvlies sich durch eine überraschend hohe Festigkeit bzw. Zugfestigkeit auszeichnet. Es können Spinnvliese mit hohen Flächehgewichten von über 40g/m2, insbesondere über 50g/m2 und ganz besonders über 60g/m2 hergestellt werden, die eine solche überraschend hohe Festigkeit bzw. Zugfestigkeit aufweisen. Es werden spezifische Längsfestigkeiten höher als 3 bei diesen hohen Flächengewichten erreicht.The invention is based on the finding that due to the inventive design of the spunbonded fabric or the filaments of the spunbonded fabric in the thermal consolidation of the energy input in the middle of the nonwoven sufficient to connect the filaments on the low-melting outer material. On the other hand, a disadvantageous heat deterioration of the remaining filament areas does not take place. The result of this is that the spunbonded nonwoven according to the invention is distinguished by a surprisingly high strength or tensile strength. It can spunbonded webs with high Flächehgewichten of about 40g / m 2, particularly about 50g / m 2 and especially about 60 g / m 2 are produced, which have such a surprisingly high strength or tensile strength. Specific longitudinal strengths higher than 3 are achieved at these high basis weights.
Nachfolgend wird die Erfindung anhand von Ausführungsbeispielen näher erläutert:The invention will be described below with reference to exemplary embodiments explained in more detail:
Es wurde ein Spinnvlies aus Bikomponentenfilamenten hergestellt, wobei die Filamente einen Standard-Titer (1,8 bis 2 denier) aufwiesen. Die Bikomponentenfilamente hatten eine Kern-Mantel-Struktur, und zwar einen Kern aus Polypropylen und einen Mantel aus einem Polypropylen-Colpolymerisat, dessen Schmelzpunkt gegenüber dem Polypropylen im Kern herabgesetzt war. Bei dem Polypropylen-Copolymerisat handelt es sich um ein heterophasisches Polypropylen-Polyethylen-Copolymer. Der Anteil der Kernkomponente betrug 80 Gew.-% und der Anteil der Mantelkomponente 20 Gew.-%. Das hergestellte Spinnvlies hatte ein Flächengewicht von 60 g/m2. Die thermische Verfestigung wurde erfindungsgemäß mit einem Prägekalander durchgeführt. Es wurde eine Längsfestigkeit von 220 N/5cm erzielt und eine spezifische Längsfestigkeit von 3,6.A spunbonded bicomponent filament was made with the filaments having a standard titer (1.8 to 2 denier). The bicomponent filaments had a core-shell structure, namely a polypropylene core and a polypropylene copolymer sheath whose melting point was reduced in core to polypropylene. The polypropylene copolymer is a polypropylene-polyethylene heterophasic copolymer. The proportion of the core component was 80 wt .-% and the proportion of the shell component 20 wt .-%. The produced spunbonded fabric had a basis weight of 60 g / m 2 . The thermal consolidation was carried out according to the invention with a stamping calender. A longitudinal strength of 220 N / 5 cm was achieved and a specific longitudinal strength of 3.6.
Es wurde ein Spinnvlies aus Bikomponentenfilamenten mit Standard-Titer hergestellt. Die Bikomponentenfilamente wiesen eine Kern-Mantel-Struktur auf. Die Kernkomponente war Polypropylen und die Mantelkomponente war Polyethylen. Der Anteil der Kernkomponente betrug 70 Gew.-% und der Anteil der Mantelkomponente betrug 30 Gew.-%. Das Spinnvlies hatte ein Flächengewicht von 55 g/m2. Auch dieses Spinnvlies wurde erfindungsgemäß mit einem Kalander thermisch verfestigt. Es wurde eine Längsfestigkeit von 220 N/5cm erreicht und eine spezifische Längsfestigkeit von 4.A spunbonded bicomponent filament of standard titer was prepared. The bicomponent filaments had a core-shell structure. The core component was polypropylene and the sheath component was polyethylene. The proportion of the core component was 70 wt .-% and the proportion of the shell component was 30 wt .-%. The spunbonded fabric had a basis weight of 55 g / m 2 . Also, this spunbonded nonwoven was thermally consolidated according to the invention with a calender. A longitudinal strength of 220 N / 5 cm was achieved and a specific longitudinal strength of 4.
Ein als Feinfaservlies aus Fasern mit einem Titer von 1,1 denier ausgebildetes Spinnvlies wurde aus Bikomponentenfilamenten hergestellt, die eine Kern-Mantel-Struktur aufwiesen. Der Kern dieser Filamente bestand aus Polypropylen und der Mantel aus. Polyethylen. Der Anteil der Kernkomponente betrug 70 Gew.-% und der Anteil der Mantelkomponente betrug 30 Gew.-%. Das Feinfaservlies hatte ein Flächengewicht von 45g/m2. Es wurde eine Längsfestigkeit von 220 N/5cm erzielt sowie eine spezifische Längsfestigkeit von 4.9. A spunbonded non-woven fabric formed as a fine denier non-woven fabric of fibers having a denier of 1.1 was made from bicomponent filaments having a core-shell structure. The core of these filaments consisted of polypropylene and the coat. Polyethylene. The proportion of the core component was 70 wt .-% and the proportion of the shell component was 30 wt .-%. The fine fiber fleece had a basis weight of 45 g / m 2 . It has a longitudinal strength of 220 N / 5cm achieved and a specific longitudinal strength of 4.9.
Auch bei diesem Ausführungsbeispiel wurde ein Feinfaservlies aus Bikomponentenfilamenten mit einem Titer von 1,1 denier hergestellt, die eine Kern-Mantel-Struktur aufwiesen. Der Kern bestand aus Polypropylen und der Mantel aus Polyethylen. Der Anteil der Kernkomponente betrug 70 Gew.-% und der Anteil der Mantelkomponente 30 Gew.-%. Das Feinfaservlies hatte ein Flächengewicht von 55g/m2. Nach der erfindungsgemäßen thermischen Verfestigung mit einem Kalander wurde eine Längsfestigkeit von 280 N/5cm festgestellt und eine spezifische Längsfestigkeit von 5,1.Also in this embodiment, a fine fiber non-woven fabric of bicomponent filaments having a denier of 1.1 denier having a core-shell structure was produced. The core was made of polypropylene and the jacket of polyethylene. The proportion of the core component was 70 wt .-% and the proportion of the shell component 30 wt .-%. The fine fiber fleece had a basis weight of 55 g / m 2 . After thermal consolidation with a calender according to the invention, a longitudinal strength of 280 N / 5 cm was determined and a specific longitudinal strength of 5.1.
Die einzige Fig. zeigt einen Querschnitt durch ein
erfindungsgemäß eingesetztes Bikomponentenfilament mit
Kern-Mantel-Struktur. Der Mantel 1, der den Kern vorzugsweise
und im Ausführungsbeispiel vollständig umgibt besteht
beispielsweise aus Polyethylen oder aus Polypropylen-Copolymerisat.
Der von dem Mantel 1 vollständig umgebene
Kern 2 mag im Ausführungsbeispiel aus Polypropylen bestehen.
Nach einer anderen Ausführungsform kann dieser Kern
2 aber auch aus einem Polyester oder aus einem anderen
Kunststoff mit einer gegenüber der Mantelkomponente höheren
Erweichungstemperatur bestehen.The single FIGURE shows a cross section through a
with bicomponent filament used according to the invention
Core-shell structure. The
Claims (8)
wobei es sich um ein thermisch in einem Kalander mit einer Prägefläche unter 22 % verfestigtes Spinnvlies handelt
und wobei das Spinnvlies ein Flächengewicht von über 40 g/m2 aufweist.Spunbonded nonwoven fabric of continuous fibers, wherein the continuous filaments are multi-component filaments, in particular bicomponent filaments with a low-melting component on the outer surface,
which is a spunbond nonwoven thermally consolidated in a calender with an emboss area less than 22%
and wherein the spunbonded web has a basis weight of over 40 g / m 2 .
wobei eine Vliesbahn aus als Mehrkomponentenfilamente, insbesondere als Bikomponentenfilamente ausgebildeten Endlosfasern gebildet wird, welche Endlosfasern eine niedrig schmelzende Komponente an ihrer Außenoberfläche aufweisen,
wobei die Vliesbahn thermisch in einem Kalander mit einer Prägefläche unter 22 % verfestigt wird
und wobei ein Spinnvlies mit einem Flächengewicht von über 40 g/m2 erzeugt wird.A process for producing a spunbonded nonwoven according to any one of claims 1 to 7,
wherein a nonwoven web is formed from continuous fibers formed as multicomponent filaments, in particular as bicomponent filaments, which filaments have a low-melting component on their outer surface,
wherein the nonwoven web is thermally solidified in a calender with an emboss area less than 22%
and wherein a spunbonded fabric having a basis weight of over 40 g / m 2 is produced.
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT03018108T ATE333528T1 (en) | 2003-08-08 | 2003-08-08 | SPUNNED WEB AND METHOD FOR PRODUCING A SPUNNED WEB |
ES03018108T ES2265079T3 (en) | 2003-08-08 | 2003-08-08 | NON-WOVEN MATERIAL OF SPINNING AND PROCEDURE FOR MANUFACTURING A NON-WOVEN MATERIAL OF SPINNING. |
DE50304289T DE50304289D1 (en) | 2003-08-08 | 2003-08-08 | Spunbonded web and method for producing a spunbonded web |
EP03018108A EP1505187B1 (en) | 2003-08-08 | 2003-08-08 | Spunbonded nonwoven fabric and process for making the same |
DK03018108T DK1505187T3 (en) | 2003-08-08 | 2003-08-08 | Spunbonded fiber fabric and method for making a spunbonded fiber fabric |
MYPI20042442A MY140892A (en) | 2003-08-08 | 2004-06-22 | Spunbonded nonwoven fabric and process for making the same |
CNB2004100696438A CN100336956C (en) | 2003-08-08 | 2004-07-15 | Spunbonded nonwoven fabric and process for making the same |
US10/912,740 US20050041312A1 (en) | 2003-08-08 | 2004-07-30 | Nonwoven web and method of making same |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP03018108A EP1505187B1 (en) | 2003-08-08 | 2003-08-08 | Spunbonded nonwoven fabric and process for making the same |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1505187A1 true EP1505187A1 (en) | 2005-02-09 |
EP1505187B1 EP1505187B1 (en) | 2006-07-19 |
Family
ID=33547667
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP03018108A Revoked EP1505187B1 (en) | 2003-08-08 | 2003-08-08 | Spunbonded nonwoven fabric and process for making the same |
Country Status (8)
Country | Link |
---|---|
US (1) | US20050041312A1 (en) |
EP (1) | EP1505187B1 (en) |
CN (1) | CN100336956C (en) |
AT (1) | ATE333528T1 (en) |
DE (1) | DE50304289D1 (en) |
DK (1) | DK1505187T3 (en) |
ES (1) | ES2265079T3 (en) |
MY (1) | MY140892A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1988202A1 (en) * | 2007-05-04 | 2008-11-05 | Carl Freudenberg KG | Non-woven fabric cover with low friction coefficients for feminine hygiene, in particular for tampons or for medical purposes, and articles equipped with same |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007011365B4 (en) * | 2007-03-07 | 2009-02-12 | Carl Freudenberg Kg | Position for use in a HEPA filter element and filter element |
TWI627321B (en) * | 2012-09-20 | 2018-06-21 | Asahi Kasei Fibers Corp | Polypropylene non-woven fabric, manufacturing method thereof and sanitary material |
EP3508459A1 (en) | 2018-01-09 | 2019-07-10 | OCV Intellectual Capital, LLC | Fiber reinforced materials with improved fatigue performance |
US20220096282A1 (en) * | 2019-02-15 | 2022-03-31 | Essity Hygiene And Health Aktiebolag | Absorbent article with embossed surface layer |
PL3771761T3 (en) * | 2019-07-30 | 2021-11-02 | Reifenhäuser GmbH & Co. KG Maschinenfabrik | Spunbond nonwoven fabric made from endless filaments and device for producing spunbond nonwoven fabric |
CN113308802A (en) * | 2021-06-03 | 2021-08-27 | 四川亿耐特新材料有限公司 | Non-woven fabric forming process |
Citations (5)
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DE2810429A1 (en) * | 1977-03-11 | 1978-09-14 | Fiber Industries Inc | SELF-TIED FIBER FIBER |
US5425987A (en) * | 1992-08-26 | 1995-06-20 | Kimberly-Clark Corporation | Nonwoven fabric made with multicomponent polymeric strands including a blend of polyolefin and elastomeric thermoplastic material |
WO2000066821A1 (en) * | 1999-04-30 | 2000-11-09 | Kimberly-Clark Worldwide, Inc. | Stretchable nonwoven material |
US20010019931A1 (en) * | 1999-11-29 | 2001-09-06 | Rosaldo Fare | Method for making improved sealability polyolefin fibers, the fibers made thereby and non-woven textile materials including the fibers |
WO2003027374A1 (en) * | 2001-09-26 | 2003-04-03 | E.I. Du Pont De Nemours And Company | A method for making spunbond nonwoven fabric from multiple component filaments |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5336552A (en) * | 1992-08-26 | 1994-08-09 | Kimberly-Clark Corporation | Nonwoven fabric made with multicomponent polymeric strands including a blend of polyolefin and ethylene alkyl acrylate copolymer |
US5662978A (en) * | 1995-09-01 | 1997-09-02 | Kimberly-Clark Worldwide, Inc. | Protective cover fabric including nonwovens |
US7008888B2 (en) * | 2003-07-24 | 2006-03-07 | E. I. Du Pont De Nemours And Company | Multiple component spunbond web |
-
2003
- 2003-08-08 ES ES03018108T patent/ES2265079T3/en not_active Expired - Lifetime
- 2003-08-08 DK DK03018108T patent/DK1505187T3/en active
- 2003-08-08 DE DE50304289T patent/DE50304289D1/en not_active Revoked
- 2003-08-08 AT AT03018108T patent/ATE333528T1/en not_active IP Right Cessation
- 2003-08-08 EP EP03018108A patent/EP1505187B1/en not_active Revoked
-
2004
- 2004-06-22 MY MYPI20042442A patent/MY140892A/en unknown
- 2004-07-15 CN CNB2004100696438A patent/CN100336956C/en not_active Expired - Fee Related
- 2004-07-30 US US10/912,740 patent/US20050041312A1/en not_active Abandoned
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2810429A1 (en) * | 1977-03-11 | 1978-09-14 | Fiber Industries Inc | SELF-TIED FIBER FIBER |
US5425987A (en) * | 1992-08-26 | 1995-06-20 | Kimberly-Clark Corporation | Nonwoven fabric made with multicomponent polymeric strands including a blend of polyolefin and elastomeric thermoplastic material |
WO2000066821A1 (en) * | 1999-04-30 | 2000-11-09 | Kimberly-Clark Worldwide, Inc. | Stretchable nonwoven material |
US20010019931A1 (en) * | 1999-11-29 | 2001-09-06 | Rosaldo Fare | Method for making improved sealability polyolefin fibers, the fibers made thereby and non-woven textile materials including the fibers |
WO2003027374A1 (en) * | 2001-09-26 | 2003-04-03 | E.I. Du Pont De Nemours And Company | A method for making spunbond nonwoven fabric from multiple component filaments |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1988202A1 (en) * | 2007-05-04 | 2008-11-05 | Carl Freudenberg KG | Non-woven fabric cover with low friction coefficients for feminine hygiene, in particular for tampons or for medical purposes, and articles equipped with same |
Also Published As
Publication number | Publication date |
---|---|
EP1505187B1 (en) | 2006-07-19 |
DK1505187T3 (en) | 2006-10-30 |
CN1580345A (en) | 2005-02-16 |
US20050041312A1 (en) | 2005-02-24 |
CN100336956C (en) | 2007-09-12 |
ATE333528T1 (en) | 2006-08-15 |
MY140892A (en) | 2010-01-29 |
ES2265079T3 (en) | 2007-02-01 |
DE50304289D1 (en) | 2006-08-31 |
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