EP0518014A1 - Mouldable floor carpets - Google Patents
Mouldable floor carpets Download PDFInfo
- Publication number
- EP0518014A1 EP0518014A1 EP92105679A EP92105679A EP0518014A1 EP 0518014 A1 EP0518014 A1 EP 0518014A1 EP 92105679 A EP92105679 A EP 92105679A EP 92105679 A EP92105679 A EP 92105679A EP 0518014 A1 EP0518014 A1 EP 0518014A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- partially crystalline
- floor
- floor carpet
- back coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N7/00—Flexible sheet materials not otherwise provided for, e.g. textile threads, filaments, yarns or tow, glued on macromolecular material
- D06N7/0063—Floor covering on textile basis comprising a fibrous top layer being coated at the back with at least one polymer layer, e.g. carpets, rugs, synthetic turf
- D06N7/0071—Floor covering on textile basis comprising a fibrous top layer being coated at the back with at least one polymer layer, e.g. carpets, rugs, synthetic turf characterised by their backing, e.g. pre-coat, back coating, secondary backing, cushion backing
- D06N7/0076—Floor covering on textile basis comprising a fibrous top layer being coated at the back with at least one polymer layer, e.g. carpets, rugs, synthetic turf characterised by their backing, e.g. pre-coat, back coating, secondary backing, cushion backing the back coating or pre-coat being a thermoplastic material applied by, e.g. extrusion coating, powder coating or laminating a thermoplastic film
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N7/00—Flexible sheet materials not otherwise provided for, e.g. textile threads, filaments, yarns or tow, glued on macromolecular material
- D06N7/0063—Floor covering on textile basis comprising a fibrous top layer being coated at the back with at least one polymer layer, e.g. carpets, rugs, synthetic turf
- D06N7/0071—Floor covering on textile basis comprising a fibrous top layer being coated at the back with at least one polymer layer, e.g. carpets, rugs, synthetic turf characterised by their backing, e.g. pre-coat, back coating, secondary backing, cushion backing
- D06N7/0081—Floor covering on textile basis comprising a fibrous top layer being coated at the back with at least one polymer layer, e.g. carpets, rugs, synthetic turf characterised by their backing, e.g. pre-coat, back coating, secondary backing, cushion backing with at least one extra fibrous layer at the backing, e.g. stabilizing fibrous layer, fibrous secondary backing
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/02—Synthetic macromolecular fibres
- D06N2201/0254—Polyolefin fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/08—Inorganic fibres
- D06N2201/082—Glass fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2203/00—Macromolecular materials of the coating layers
- D06N2203/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N2203/042—Polyolefin (co)polymers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2205/00—Condition, form or state of the materials
- D06N2205/14—Fibrous additives or fillers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2207/00—Treatments by energy or chemical effects
- D06N2207/12—Treatments by energy or chemical effects by wave energy or particle radiation
- D06N2207/123—Treatments by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation, e.g. IR, UV, actinic light, laser, X-ray, gamma-ray, microwave, radio frequency
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2211/00—Specially adapted uses
- D06N2211/06—Building materials
- D06N2211/066—Floor coverings
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/26—Vehicles, transportation
- D06N2211/263—Cars
Definitions
- the invention relates to three-dimensionally deformable, recyclable floor carpets, in particular car floor carpets and a method for their production.
- Three-dimensionally deformable floor carpets currently in use consist of plastic or textile composites, the individual components of which are more or less alien. Such carpets are in several, z. T. labor-intensive process steps obtained as a formable composite, for example by providing a tufting or a needle fleece, which consist predominantly of polyethylene terephthalate (PET), polyacrylic or PET blends with polypropylene fiber components, on the back with a latex application and then layers of different Applies materials that should ensure mechanical stability and good lying behavior.
- PET polyethylene terephthalate
- PET polyacrylic or PET blends with polypropylene fiber components
- a rigid support made of a polyolefin plate which on one or both surfaces without the interposition of adhesives with a flexible layer based on polyolefin, e.g. B. a fabric or nonwoven fabric made of isotactic polypropylene, are known from DE-A-31 00 682.
- their rigidity causes their resonance frequency to be within the audible range; the sound absorption is low. Since they also cannot adapt to the subtleties of the floor geometry, they are unsuitable as floor carpets.
- GB-A 2 072 578 describes sound-absorbing floor carpets whose backing coating contains a polyolefin, a synthetic rubber, petroleum oil in considerable quantities and an inorganic filler.
- a serious disadvantage of this composition is that the very high melt viscosity of the combination of polyolefin / synthetic rubber / filler has to be reduced to a level which is sensible in terms of processing technology by adding the oil.
- the presence of an oil is undesirable for several reasons. Since it naturally tends to exude, it can cause serious fogging problems. Adhesion to the top of the carpet also deteriorates, which is why you have to cover it with latex before applying the backing. Finally, the presence of oil and latex is undesirable for recycling.
- the floor carpets of the present invention are easily recyclable, can be three-dimensionally deformed without difficulty, give no cause for fogging, are easy to produce and have good flexibility and good sound-absorbing and sound-absorbing effects.
- Isotactic polypropylene is preferably used as the material for the top of the carpet for reasons of good recyclability.
- Homopolymers and copolymers can be used; the homopolymer is preferably used.
- the polymer can contain the usual amounts of pigments, stabilizers, processing aids, antistatic agents and the like.
- B atactic polypropylene in the form of homo- or copolymers.
- Atactic polypropylene (APP) and / or binary or ternary copolymers of the monomers butene-1, propene and optionally ethene are preferably used.
- Such copolymers can be produced by targeted polymerization on classic Ziegler catalysts or their further developments, as described for example in DE-PS 23 06 667 or DE-PS 29 30 108.
- the largely amorphous polyolefins have a degree of crystallization of at most 25%, determined by X-ray diffraction.
- largely amorphous polyolefins have a softening point between 90 and 150 ° C, a melt viscosity at 190 ° C between 5,000 and 150,000 mPa s and a needle penetration between 15 and 40 0.1 mm.
- any polymer that is also suitable for the top of the carpet can be used as the semi-crystalline polyolefin for the back coating.
- higher molecular weight PP random or block copolymers are preferably used.
- At least part of the largely amorphous polyolefin and / or the partially crystalline polyolefin can be grafted with free radicals with monomers containing double bonds which carry at least one functional group.
- Suitable polymer mixtures are described, for example, in EP-A 0 309 674, to which reference is hereby expressly made.
- chalk, talc, mica, heavy spar, similar rock flour, glass fibers and / or glass balls can be used as fillers be used.
- Chalk and / or heavy spar are preferably used.
- the average particle diameter should not exceed 150 ⁇ m.
- the molding compound of the back coating can be produced from the components by all customary methods, in particular by melt mixing.
- the back coating has a thickness of approximately 0.2 to approximately 5 mm.
- the back coating contains a fleece, support grid, mesh or knitted fabric, from which it is usually embedded.
- the same polymers are suitable as materials as they can also be used for the top of the carpet.
- the composite can be produced in various ways, for example by lamination or coating. It can be obtained particularly advantageously by extrusion coating.
- the composite After manufacture and, if necessary, cutting, the composite can be deformed three-dimensionally, for example by compression molding or vacuum molding. For this purpose, it first runs through a heating field in which the molded part is brought to a temperature at which the back coating softens, but the fibers on the top of the carpet are still dimensionally stable.
- Floor carpets of this type are particularly suitable for use in motor vehicles, where in this way the composite can easily be adapted to the contours of, for example, the footwell or the trunk.
- the punching waste or the entire molded part can be easily recycled.
- the material is crushed in the usual way and fed to an extruder, where other substances can be mixed.
- the mass obtained can be used, for example, for the back coating. Since only thermoplastic polymers of the same type are contained, no delamination or speck formation is observed.
- This carpet velor was fed from a 3-roll smoothing calender (working width 2.40 m). After passing through the first roller, a melt film consisting of an extruder was then passed through a slot die 33 1/3% random copolymer VESTOLEN P 8400, 33 1/3% amorphous directly polymerized atactic polypropylene VESTOPLAST 891 and 33 1/3% heavy spar batch, consisting of 70% by weight heavy spar and 30% by weight polypropylene homopolymer on the back against the carpet velor with a 60 g / m2 polyolefin net (grid size 1.2 x 1.5 mm) made of VESTOLEN A 6012.
- a single-screw extruder (120 mm ⁇ screw diameter) with a dynamic mixer, melt pump, static mixer and flex-lip nozzle (2.20 m working width) was used as the extruder.
- the union was brought together via the smoothing calender.
- Adequate bond adhesion was achieved by setting the smoothing roll gap 10% less than the total thickness of the bond to be produced.
- the carpet produced in this way can be fed to the thermoforming process in rolls or in format sizes.
- the carpet composite was held by means of a needled chain feed (with a stylus) and transported to the forming station.
- the heating process was carried out on both sides by infrared radiators via separately controllable longitudinal heating controls below the melting range of the fiber top, so that this was not thermally damaged.
- a perfect, sharp-contoured deformation was then carried out by press molding. The molded part was punched out during this pressing process.
- the punching waste (approx. 40% by weight) was used in a further production approach of the same type as a component of the back coating, the calculated amounts of the individual primary components of the back coating (in total 48% by weight) being substituted by the corresponding amount of the crushed punching waste .
- a composite of equal quality was obtained.
Abstract
Description
Die Erfindung betrifft dreidimensional verformbare, recyclingfähige Bodenteppiche, insbesondere Autobodenteppiche sowie ein Verfahren zu ihrer Herstellung.The invention relates to three-dimensionally deformable, recyclable floor carpets, in particular car floor carpets and a method for their production.
Derzeit im Einsatz befindliche, dreidimensional verformbare Bodenteppiche bestehen aus Kunststoff- bzw. Textilverbunden, deren einzelne Komponenten mehr oder weniger artfremd sind. Derartige Bodenteppiche werden in mehreren, z. T. arbeitsaufwendigen Verfahrensschritten als formfähiger Verbund erhalten, indem man beispielsweise ein Tufting oder ein Nadelvlies, die überwiegend aus Polyethylenterephthalat (PET), Polyacryl oder PET-Mischungen mit Polypropylen-Faseranteilen bestehen, auf der Rückseite mit einem Latexauftrag versieht und anschließend noch Schichten aus verschiedenen Materialien aufträgt, die mechanische Stabilität und gutes Liegeverhalten gewährleisten sollen.Three-dimensionally deformable floor carpets currently in use consist of plastic or textile composites, the individual components of which are more or less alien. Such carpets are in several, z. T. labor-intensive process steps obtained as a formable composite, for example by providing a tufting or a needle fleece, which consist predominantly of polyethylene terephthalate (PET), polyacrylic or PET blends with polypropylene fiber components, on the back with a latex application and then layers of different Applies materials that should ensure mechanical stability and good lying behavior.
Derartige Bodenteppiche besitzen neben der aufwendigen Herstellung den besonderen Nachteil, daß wegen der Kombination artfremder Materialien weder der Stanzabfall bei der Formung, der bis zu 40 % betragen kann, noch das Formteil bei der Altautoentsorgung wiederverwertet werden kann.Floor carpets of this type have, in addition to the elaborate production, the particular disadvantage that, because of the combination of foreign materials, neither the punching waste during the shaping, which can be up to 40%, nor the molded part can be recycled in the disposal of used cars.
Es stellte sich daher die Aufgabe, Bodenteppiche zur Verfügung zu stellen, die folgende Bedingungen erfüllen:
- 1) Der Bodenteppich muß aus einer Kombination artgleicher Materialien bestehen, um eine Wiederverwertung zu ermöglichen;
- 2) die Rückenbeschichtung muß bei Heiztemperaturen verformbar sein, bei denen die Teppichoberseite nicht geschädigt wird;
- 3) die Rückenbeschichtung muß einerseits eine ausreichende Flexibilität besitzen, andererseits unter den Gebrauchsbedingungen formstabil sein;
- 4) der Teppichboden muß unter Vermeidung von Vielfachverbund-Kombinationen einfach herstellbar sein.
- 1) The floor carpet must consist of a combination of identical materials in order to enable recycling;
- 2) the back coating must be deformable at heating temperatures at which the top of the carpet is not damaged;
- 3) the back coating must on the one hand have sufficient flexibility and on the other hand be dimensionally stable under the conditions of use;
- 4) the carpet must be easy to produce, avoiding multiple composite combinations.
Diese Aufgabe wurde gelöst durch Bodenteppiche, die aus folgenden Komponenten zusammengesetzt sind:
- a) Die Teppichoberseite, üblicherweise ein Gewebe, Gewirke, Tufting oder Nadelvlies, besteht aus teilkristallinem Polyolefin, vorzugsweise Polypropylen.
- b) Die Rückenbeschichtung besteht aus einer Formmasse, die folgende Komponenten enthält:
- 10 bis 95 Gew.-% eines oder mehrerer weitgehend amorpher Polyolefine der Monomerenzusammensetzung
0 bis 80 Gew.-% eines α-Olefins mit 4 bis 10 Kohlenstoffatomen,
20 bis 100 Gew.-% Propen und
weniger als 20 Gew.-% Ethen; - 5 bis 90 Gew.-% eines oder mehrerer teilkristalliner Polyolefine, vorzugsweise Polypropylen;
- maximal 70 Gew.-% Füllstoffe.
- 10 bis 95 Gew.-% eines oder mehrerer weitgehend amorpher Polyolefine der Monomerenzusammensetzung
- c) Rückenverstärkung in Form eines Vlieses, Stützgitters, -gewebes oder -gewirkes aus teilkristallinem Polyolefin, vorzugsweise Polypropylen, oder aus Glas.
- a) The top of the carpet, usually a fabric, knitted fabric, tufting or needle fleece, consists of partially crystalline polyolefin, preferably polypropylene.
- b) The back coating consists of a molding compound that contains the following components:
- 10 to 95 wt .-% of one or more largely amorphous polyolefins of the monomer composition
0 to 80% by weight of an α-olefin with 4 to 10 carbon atoms,
20 to 100 wt .-% propene and
less than 20 wt% ethene; - 5 to 90% by weight of one or more partially crystalline polyolefins, preferably polypropylene;
- maximum 70% by weight fillers.
- 10 to 95 wt .-% of one or more largely amorphous polyolefins of the monomer composition
- c) back reinforcement in the form of a fleece, support grid, woven or knitted fabric made of partially crystalline polyolefin, preferably polypropylene, or of glass.
Selbsttragende Polyolefinschichtstoffe auf der Grundlage eines steifen Trägers aus einer Polyolefinplatte, die an einer oder beiden Oberflächen ohne Zwischenschaltung von Klebstoffen mit einer biegsamen Schicht auf Polyolefinbasis, z. B. einem Gewebe oder Faservlies aus isotaktischem Polypropylen, überzogen sind, sind aus der DE-A-31 00 682 bekannt. Ihre Steifigkeit bewirkt jedoch, daß ihre Resonanzfrequenz innerhalb des hörbaren Bereichs liegt; die Schalldämpfung ist gering. Da sie sich zudem nicht an Feinheiten der Bodengeometrie anpassen können, sind sie als Bodenteppich ungeeignet.Self-supporting polyolefin laminates on the basis of a rigid support made of a polyolefin plate, which on one or both surfaces without the interposition of adhesives with a flexible layer based on polyolefin, e.g. B. a fabric or nonwoven fabric made of isotactic polypropylene, are known from DE-A-31 00 682. However, their rigidity causes their resonance frequency to be within the audible range; the sound absorption is low. Since they also cannot adapt to the subtleties of the floor geometry, they are unsuitable as floor carpets.
In der GB-A 2 072 578 werden schalldämpfende Bodenteppiche beschrieben, deren Rückenbeschichtung ein Polyolefin, einen Synthesekautschuk, Petroleumöl in beträchtlichen Mengen sowie einen anorganischen Füllstoff enthält. Ein gravierender Nachteil dieser Zusammensetzung ist, daß die sehr hohe Schmelzviskosität der Kombination Polyolefin/Synthesekautschuk/Füllstoff durch Zusatz des Öls auf ein verarbeitungstechnisch sinnvolles Maß verringert werden muß. Die Anwesenheit eines Öls ist jedoch aus mehreren Gründen unerwünscht. Da es naturgemäß zum Ausschwitzen neigt, kann es zu ernsthaften Foggingproblemen führen. Auch die Haftung an der Teppichoberseite wird verschlechtert, weshalb man diese vor dem Auftrag der Rückenbeschichtung mit Latex kaschieren muß. Schließlich ist bei der Wiederverwertung die Anwesenheit von Öl und Latex unerwünscht.GB-A 2 072 578 describes sound-absorbing floor carpets whose backing coating contains a polyolefin, a synthetic rubber, petroleum oil in considerable quantities and an inorganic filler. A serious disadvantage of this composition is that the very high melt viscosity of the combination of polyolefin / synthetic rubber / filler has to be reduced to a level which is sensible in terms of processing technology by adding the oil. However, the presence of an oil is undesirable for several reasons. Since it naturally tends to exude, it can cause serious fogging problems. Adhesion to the top of the carpet also deteriorates, which is why you have to cover it with latex before applying the backing. Finally, the presence of oil and latex is undesirable for recycling.
Diese Schrift gibt auch keine Hinweise darauf, ob die dort beschriebenen Bodenteppiche nach ihrer Herstellung dreidimensional verformt werden können.This document also gives no information as to whether the floor carpets described there can be three-dimensionally deformed after they have been manufactured.
Die Bodenteppiche der vorliegenden Erfindung sind hingegen problemlos wiederverwertbar, lassen sich ohne Schwierigkeiten dreidimensional verformen, geben keinen Anlaß zu Fogging, sind einfach herstellbar und besitzen eine gute Flexibilität und gute schalldämmende und schalldämpfende Wirkung.The floor carpets of the present invention, on the other hand, are easily recyclable, can be three-dimensionally deformed without difficulty, give no cause for fogging, are easy to produce and have good flexibility and good sound-absorbing and sound-absorbing effects.
Als Material für die Teppichoberseite wird aus Gründen guter Recyclingfähigkeit bevorzugt isotaktisches Polypropylen verwendet. Es können Homo- und Copolymere verwendet werden; bevorzugt setzt man das Homo-polymere ein. Gemäß dem Stand der Technik kann das Polymere die üblichen Mengen an Pigmenten, Stabilisatoren, Verarbeitungshilfsmitteln, Antistatika und dergleichen enthalten.Isotactic polypropylene is preferably used as the material for the top of the carpet for reasons of good recyclability. Homopolymers and copolymers can be used; the homopolymer is preferably used. According to the prior art, the polymer can contain the usual amounts of pigments, stabilizers, processing aids, antistatic agents and the like.
In der Rückenbeschichtung kann als weitgehend amorphes Polyolefin z. B. ataktisches Polypropylen in Form von Homo- oder Copolymeren verwendet werden. Bevorzugt setzt man ataktisches Polypropylen (APP) und/oder binäre oder ternäre Copolymere aus den Monomeren Buten-1, Propen und ggf. Ethen ein. Derartige Copolymere können durch gezielte Polymerisation an klassischen Ziegler-Katalysatoren bzw. deren Weiterentwicklungen hergestellt werden, wie es beispielsweise in der DE-PS 23 06 667 oder der DE-PS 29 30 108 beschrieben ist. Generell besitzen die weitgehend amorphen Polyolefine einen Kristallisationsgrad von höchstens 25 %, bestimmt über Röntgenbeugung.In the back coating as a largely amorphous polyolefin z. B. atactic polypropylene in the form of homo- or copolymers. Atactic polypropylene (APP) and / or binary or ternary copolymers of the monomers butene-1, propene and optionally ethene are preferably used. Such copolymers can be produced by targeted polymerization on classic Ziegler catalysts or their further developments, as described for example in DE-PS 23 06 667 or DE-PS 29 30 108. In general, the largely amorphous polyolefins have a degree of crystallization of at most 25%, determined by X-ray diffraction.
In einer bevorzugten Ausführungsform setzt man ein weitgehend amorphes Polyolefin mit einem Erweichungspunkt (Ring- und Kugelmethode) zwischen 70 und 160 °C, einer Schmelzviskosität entsprechend ASTM D 3236-73 bei 190 °C zwischen 2 000 und 200 000 mPa s, einer Dichte kleiner als 0,90 g/cm³ und einer Nadelpenetration 100/25/5 gemäß DIN 52 010 zwischen 5 und 50 0,1 mm ein. Besonders bevorzugte, weitgehend amorphe Polyolefine besitzen einen Erweichungspunkt zwischen 90 und 150 °C, eine Schmelzviskosität bei 190 °C zwischen 5 000 und 150 000 mPa s und eine Nadelpenetration zwischen 15 und 40 0,1 mm.In a preferred embodiment, a largely amorphous polyolefin with a softening point (ring and ball method) between 70 and 160 ° C, a melt viscosity according to ASTM D 3236-73 at 190 ° C between 2,000 and 200,000 mPa s, a density lower as 0.90 g / cm³ and a needle penetration 100/25/5 according to DIN 52 010 between 5 and 50 0.1 mm. Particularly preferred, largely amorphous polyolefins have a softening point between 90 and 150 ° C, a melt viscosity at 190 ° C between 5,000 and 150,000 mPa s and a needle penetration between 15 and 40 0.1 mm.
Als teilkristallines Polyolefin kann für die Rückenbeschichtung grundsätzlich jedes Polymere eingesetzt werden, das auch für die Teppichoberseite geeignet ist. Bevorzugt werden jedoch höhermolekulare PP-Random- oder Blockcopolymere eingesetzt.In principle, any polymer that is also suitable for the top of the carpet can be used as the semi-crystalline polyolefin for the back coating. However, higher molecular weight PP random or block copolymers are preferably used.
Gemäß dem Stand der Technik kann zumindest ein Teil des weitgehend amorphen Polyolefins und/oder des teilkristallinen Polyolefins mit doppelbindungshaltigen Monomeren, die mindestens eine funktionelle Gruppe tragen, radikalisch gepfropft sein. Geeignete Polymergemische sind beispielsweise in der EP-A 0 309 674 beschrieben, auf die hiermit ausdrücklich Bezug genommen wird.According to the prior art, at least part of the largely amorphous polyolefin and / or the partially crystalline polyolefin can be grafted with free radicals with monomers containing double bonds which carry at least one functional group. Suitable polymer mixtures are described, for example, in EP-A 0 309 674, to which reference is hereby expressly made.
Als Füllstoffe können beispielsweise Kreide, Talkum, Glimmer, Schwerspat, ähnliche Gesteinsmehle, Glasfasern und/oder Glaskugeln verwendet werden. Bevorzugt werden Kreide und/oder Schwerspat eingesetzt. Der mittlere Teilchendurchmesser sollte 150 µm nicht übersteigen.For example, chalk, talc, mica, heavy spar, similar rock flour, glass fibers and / or glass balls can be used as fillers be used. Chalk and / or heavy spar are preferably used. The average particle diameter should not exceed 150 µm.
Die Formmasse der Rückenbeschichtung kann aus den Komponenten nach allen üblichen Methoden, insbesondere durch Schmelzemischen, hergestellt werden.The molding compound of the back coating can be produced from the components by all customary methods, in particular by melt mixing.
In der Regel weist die Rückenbeschichtung eine Dicke von ca. 0,2 bis ca. 5 mm auf.As a rule, the back coating has a thickness of approximately 0.2 to approximately 5 mm.
Die Rückenbeschichtung enthält ein Vlies, Stützgitter, -gewebe oder -gewirke, von dem sie in der Regel eingebettet wird. Als Material sind die gleichen Polymere geeignet, wie sie auch für die Teppichoberseite verwendet werden können.The back coating contains a fleece, support grid, mesh or knitted fabric, from which it is usually embedded. The same polymers are suitable as materials as they can also be used for the top of the carpet.
Der Verbund kann auf verschiedene Weise, wie beispielsweise durch Kaschieren oder Beschichten, hergestellt werden. Besonders vorteilhaft kann er durch Extrusionsbeschichtung erhalten werden.The composite can be produced in various ways, for example by lamination or coating. It can be obtained particularly advantageously by extrusion coating.
Nach Herstellen und ggf. Schneiden kann der Verbund beispielsweise durch Preßformen oder Vakuumformen dreidimensional verformt werden. Hierzu durchläuft er zunächst ein Heizfeld, in dem das Formteil auf eine Temperatur gebracht wird, bei der die Rückenbeschichtung erweicht, die Fasern der Teppichoberseite jedoch noch formbeständig sind.After manufacture and, if necessary, cutting, the composite can be deformed three-dimensionally, for example by compression molding or vacuum molding. For this purpose, it first runs through a heating field in which the molded part is brought to a temperature at which the back coating softens, but the fibers on the top of the carpet are still dimensionally stable.
Derartige Bodenteppiche sind insbesondere für die Verwendung in Kraftfahrzeugen geeignet, wo man auf diese Weise den Verbund leicht an die Konturen beispielsweise des Fußraums oder des Kofferraums anpassen kann.Floor carpets of this type are particularly suitable for use in motor vehicles, where in this way the composite can easily be adapted to the contours of, for example, the footwell or the trunk.
Die Stanzabfälle oder das gesamte Formteil können auf einfache Weise wiederverwertet werden. Dazu wird das Material auf übliche Weise zerkleinert und einem Extruder zugeführt, wobei noch andere Stoffe zugemischt werden können. Die erhaltene Masse kann beispielsweise für die Rückenbeschichtung verwendet werden. Da nur artgleiche thermoplastische Polymere enthalten sind, werden keine Delaminierungserscheinungen oder Stippenbildung beobachtet.The punching waste or the entire molded part can be easily recycled. For this purpose, the material is crushed in the usual way and fed to an extruder, where other substances can be mixed. The mass obtained can be used, for example, for the back coating. Since only thermoplastic polymers of the same type are contained, no delamination or speck formation is observed.
Es wurde ein Tufting-Velour aus 100 % Polypropylen-Homopolymerisat von 360 g/m² (ohne Rückenlatizierung wie sonst für Poleinbindung notwendig) in 2 m Breite mit einer Faserpolhöhe von 4,5 mm und einem Fasertiter von 17 dtex eingesetzt.A tufting velor made of 100% polypropylene homopolymer of 360 g / m² (without back bracing as otherwise necessary for pole binding) was used in a width of 2 m with a fiber pile height of 4.5 mm and a fiber titer of 17 dtex.
Dieser Teppichvelour wurde einem 3-Walzen-Glättkalander (Arbeitsbreite 2,40 m) von der Rolle zugeführt. Nach Passieren der ersten Walze wurde dann von einem Extruder über eine Breitschlitzdüse ein Schmelzefilm bestehend aus
33 1/3 % Randomcopolymerisat VESTOLEN P 8400,
33 1/3 % amorphes direkt polymerisiertes ataktisches Polypropylen VESTOPLAST 891 und
33 1/3 % Schwerspatbatch, bestehend aus 70 Gew.-% Schwerspat und 30 Gew.-% Polypropylen-Homopolymerisat
rückseitig gegen den Teppichvelour bei gleichzeitigem Zulauf eines 60 g/m² schweren Polyolefinnetzes (Gittergröße 1,2 x 1,5 mm) aus VESTOLEN A 6012 zugeführt. Als Extruder wurde hierbei ein Einschnecken-Extruder (120 mm ⌀ Schneckendurchmesser) mit dynamischem Mischer, Schmelzepumpe, Statikmischer und Flexlippdüse (2,20 m Arbeitsbreite) verwendet. Die Zusammenführung des Verbundes erfolgte über den Glättkalander.This carpet velor was fed from a 3-roll smoothing calender (working width 2.40 m). After passing through the first roller, a melt film consisting of an extruder was then passed through a slot die
33 1/3% random copolymer VESTOLEN P 8400,
33 1/3% amorphous directly polymerized atactic polypropylene VESTOPLAST 891 and
33 1/3% heavy spar batch, consisting of 70% by weight heavy spar and 30% by weight polypropylene homopolymer
on the back against the carpet velor with a 60 g / m² polyolefin net (grid size 1.2 x 1.5 mm) made of VESTOLEN A 6012. A single-screw extruder (120 mm ⌀ screw diameter) with a dynamic mixer, melt pump, static mixer and flex-lip nozzle (2.20 m working width) was used as the extruder. The union was brought together via the smoothing calender.
Eine ausreichende Verbundhaftung wurde erreicht, indem der Glättwalzspalt 10 % geringer eingestellt war als die zu erzeugende Gesamtstärke des Verbundes.Adequate bond adhesion was achieved by setting the smoothing roll gap 10% less than the total thickness of the bond to be produced.
Der so hergestellte Teppich kann als Rollenware bzw. in Formatgrößen dem Thermoformvorgang zugeführt werden.The carpet produced in this way can be fed to the thermoforming process in rolls or in format sizes.
Von der Rolle ausgehend wurde der Teppichverbund über genadelte Kettenzuführung (mit Sticheln) gehalten und in die Formstation transportiert.Starting from the roll, the carpet composite was held by means of a needled chain feed (with a stylus) and transported to the forming station.
Der Aufheizvorgang erfolgte beidseitig durch Infrarotstrahler über getrennt steuerbare Längsheizregelungen unterhalb des Schmelzbereichs der Faseroberseite, so daß diese thermisch nicht geschädigt wurde. Durch Preßformung wurde anschließend eine einwandfreie, konturenscharfe Verformung durchgeführt. Die Ausstanzung des Formteils erfolgte während dieses Preßvorgangs.The heating process was carried out on both sides by infrared radiators via separately controllable longitudinal heating controls below the melting range of the fiber top, so that this was not thermally damaged. A perfect, sharp-contoured deformation was then carried out by press molding. The molded part was punched out during this pressing process.
Die Stanzabfälle (ca. 40 Gew.-%) wurden in einem weiteren Produktionsansatz gleicher Art als Bestandteil der Rückenbeschichtung eingesetzt, wobei die berechneten Mengen der einzelnen Primärkomponenten der Rückenbeschichtung (insgesamt 48 Gew.-%) durch die entsprechende Menge der zerkleinerten Stanzabfälle substituiert wurden. Hierbei wurde ein qualitativ gleichwertiger Verbund erhalten.The punching waste (approx. 40% by weight) was used in a further production approach of the same type as a component of the back coating, the calculated amounts of the individual primary components of the back coating (in total 48% by weight) being substituted by the corresponding amount of the crushed punching waste . Here, a composite of equal quality was obtained.
Claims (8)
0 bis 80 Gew.-% eines α-Olefins mit 4 bis 10 Kohlenstoffatomen,
20 bis 100 Gew.-% Propen und
weniger als 20 Gew.-% Ethen;
0 to 80% by weight of an α-olefin with 4 to 10 carbon atoms,
20 to 100 wt .-% propene and
less than 20 wt% ethene;
dadurch gekennzeichnet,
daß, unabhängig voneinander, die Teppichoberseite, die teilkristalline Polyolefin-Komponente der Rückenbeschichtung und/oder die Rückenverstärkung aus Polypropylen bestehen.Floor carpet according to claim 1,
characterized,
that, independently of one another, the top of the carpet, the partially crystalline polyolefin component of the back coating and / or the back reinforcement consist of polypropylene.
dadurch gekennzeichnet,
daß das Polypropylen ein Homo- oder Copolymer ist.Floor carpet according to claim 2,
characterized,
that the polypropylene is a homo- or copolymer.
dadurch gekennzeichnet,
daß als weitgehend amorphes Polyolefin der Rückenbeschichtung ataktisches Polypropylen (APP) und/oder binäre oder ternäre Copolymere aus den Monomeren Buten-1, Propen und ggf. Ethen eingesetzt werden.Floor carpet according to one of claims 1 to 3,
characterized,
that atactic polypropylene (APP) and / or binary or ternary copolymers of the monomers butene-1, propene and optionally ethene are used as the largely amorphous polyolefin of the back coating.
dadurch gekennzeichnet,
daß als Füllstoff der Rückenbeschichtung Kreide, Talkum, Glimmer, Schwerspat, ähnliche Gesteinsmehle, Glasfasern und/oder Glaskugeln verwendet werden.Floor carpet according to one of claims 1 to 4,
characterized,
that chalk, talc, mica, heavy spar, similar rock flour, glass fibers and / or glass balls are used as filler for the back coating.
dadurch gekennzeichnet,
daß die Rückenbeschichtung durch Extrusionsbeschichtung aufgebracht wird und anschließend kalandriert wird.Process for the production of floor carpets according to claims 1 to 5,
characterized,
that the back coating is applied by extrusion coating and then calendered.
dadurch gekennzeichnet,
daß der Verbund anschließend dreidimensional verformt wird.A method according to claim 6,
characterized,
that the composite is then three-dimensionally deformed.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4117275A DE4117275A1 (en) | 1991-05-27 | 1991-05-27 | DEFORMABLE FLOOR CARPETS |
DE4117275 | 1991-05-27 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0518014A1 true EP0518014A1 (en) | 1992-12-16 |
EP0518014B1 EP0518014B1 (en) | 1995-04-05 |
Family
ID=6432524
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP92105679A Expired - Lifetime EP0518014B1 (en) | 1991-05-27 | 1992-04-02 | Mouldable floor carpets |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP0518014B1 (en) |
JP (1) | JP3238468B2 (en) |
DE (2) | DE4117275A1 (en) |
ES (1) | ES2072650T3 (en) |
Cited By (21)
Publication number | Priority date | Publication date | Assignee | Title |
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FR2692602A1 (en) * | 1992-06-23 | 1993-12-24 | Malimo Maschinenbau | Non-woven fabric as well as the method and the device for manufacturing the same. |
WO1994016138A1 (en) * | 1993-01-08 | 1994-07-21 | Bercopa S.A. | Method for manufacturing carpets |
BE1006624A3 (en) * | 1993-01-08 | 1994-11-03 | Bercopa Sa | Recyclable synthetic carpet and method for manufacturing it |
EP0624620A2 (en) * | 1993-05-12 | 1994-11-17 | BASF Aktiengesellschaft | Process for the production of fibres containing polypropylene as main component |
EP0630323A1 (en) * | 1992-02-10 | 1994-12-28 | Polyloom Corporation Of America | Carpet and techniques for making and recycling same |
WO1995003446A1 (en) * | 1993-07-20 | 1995-02-02 | Bercopa S.A. | Woven carpets, and method for the manufacture thereof |
BE1007353A3 (en) * | 1993-07-20 | 1995-05-23 | Bercopa Sa | Method for manufacturing carpet |
NL9400666A (en) * | 1992-12-01 | 1995-12-01 | Spindor Spinnerij Nv | Carpet or cover material and method of manufacturing and processing thereof. |
WO1998038375A2 (en) * | 1997-02-28 | 1998-09-03 | Shaw Industries, Inc. | Carpet, carpet backings and methods |
US5876827A (en) * | 1992-02-10 | 1999-03-02 | Polyloom Corporation Of America | Pile carpet |
WO1999040250A2 (en) * | 1998-02-04 | 1999-08-12 | Mannington Mills, Inc. | Surface coverings containing fused recycled material and processes of making the same |
EP1375731A2 (en) * | 2002-06-26 | 2004-01-02 | Degussa AG | Process for back coating a carpet |
EP1645682A1 (en) * | 2004-10-10 | 2006-04-12 | Centro Tecnologico de Grupo Copo, S.L. | Manufacturing procedure for carpeting with layered undrlay |
WO2014011450A1 (en) * | 2012-07-10 | 2014-01-16 | Exxonmobil Chemical Patents Inc. | Carpet comprising a propylene-based elastomer and methods of making the same |
US9051683B2 (en) | 1997-02-28 | 2015-06-09 | Columbia Insurance Company | Carpet, carpet backings and methods |
US9376769B2 (en) | 1997-02-28 | 2016-06-28 | Columbia Insurance Company | Homogeneously branched ethylene polymer carpet backsizing compositions |
WO2019011725A1 (en) * | 2017-07-14 | 2019-01-17 | Tarkett Gdl | Carpet backing layer composition |
LU100340B1 (en) * | 2017-07-14 | 2019-01-28 | Tarkett Gdl Sa | Carpet backing layer composition |
LU100355B1 (en) * | 2017-08-01 | 2019-02-06 | Tarkett Gdl Sa | Carpet backing layer composition |
LU100738B1 (en) * | 2018-03-19 | 2019-10-01 | Tarkett Gdl Sa | Carpet backing layer composition |
US10563055B2 (en) | 2016-12-20 | 2020-02-18 | Exxonmobil Chemical Patents Inc. | Carpet compositions and methods of making the same |
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EP0590189A1 (en) * | 1992-09-30 | 1994-04-06 | Sincol Co., Ltd. | Tile-shaped carpet |
DE9411993U1 (en) * | 1994-07-26 | 1994-09-29 | Malimo Maschinenbau | Non-woven fabric for coating carpet backs |
WO2001023181A1 (en) * | 1999-09-30 | 2001-04-05 | Marco Alfonso Lepe Cisneros | Method for producing recyclable mats from a single resin or polymer having a textile top or bottom surface and anchoring and secondary lamination by thermofusion of sheets of the same polymer that are embossed and thermomolded in a single operation and product thus obtained |
WO2001045942A1 (en) * | 1999-12-21 | 2001-06-28 | Marco Alfonso Lepe Cisneros | Method for producing 100 % recyclable carpets from a single resin or polymer having backing and secondary lamination by thermofusing laminae made of the same polymer with or without foam insulator and thermomolded in a single operation and product thus obtained |
US20150176201A1 (en) * | 2012-07-10 | 2015-06-25 | Exxonmobil Chemical Patents Inc. | Carpets and Textile Layers Comprising a Polymer Blend and Methods of Making the Same |
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- 1991-05-27 DE DE4117275A patent/DE4117275A1/en not_active Withdrawn
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- 1992-04-02 EP EP92105679A patent/EP0518014B1/en not_active Expired - Lifetime
- 1992-04-02 DE DE59201812T patent/DE59201812D1/en not_active Expired - Fee Related
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Publication number | Priority date | Publication date | Assignee | Title |
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EP0630323A4 (en) * | 1992-02-10 | 1995-04-26 | Polyloom Corp | Carpet and techniques for making and recycling same. |
US5876827A (en) * | 1992-02-10 | 1999-03-02 | Polyloom Corporation Of America | Pile carpet |
US5728444A (en) * | 1992-02-10 | 1998-03-17 | Fink; Wilbert E. | Carpet and techniques for making and recycling same |
EP0630323A1 (en) * | 1992-02-10 | 1994-12-28 | Polyloom Corporation Of America | Carpet and techniques for making and recycling same |
US5578357A (en) * | 1992-02-10 | 1996-11-26 | Polyloom Corporation Of America | Carpet and techniques for making and recycling same |
FR2692602A1 (en) * | 1992-06-23 | 1993-12-24 | Malimo Maschinenbau | Non-woven fabric as well as the method and the device for manufacturing the same. |
NL9400666A (en) * | 1992-12-01 | 1995-12-01 | Spindor Spinnerij Nv | Carpet or cover material and method of manufacturing and processing thereof. |
BE1006624A3 (en) * | 1993-01-08 | 1994-11-03 | Bercopa Sa | Recyclable synthetic carpet and method for manufacturing it |
WO1994016138A1 (en) * | 1993-01-08 | 1994-07-21 | Bercopa S.A. | Method for manufacturing carpets |
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EP0624620A2 (en) * | 1993-05-12 | 1994-11-17 | BASF Aktiengesellschaft | Process for the production of fibres containing polypropylene as main component |
EP0624620A3 (en) * | 1993-05-12 | 1995-05-03 | Basf Ag | Process for the production of fibres containing polypropylene as main component. |
BE1007353A3 (en) * | 1993-07-20 | 1995-05-23 | Bercopa Sa | Method for manufacturing carpet |
WO1995003446A1 (en) * | 1993-07-20 | 1995-02-02 | Bercopa S.A. | Woven carpets, and method for the manufacture thereof |
WO1998038375A2 (en) * | 1997-02-28 | 1998-09-03 | Shaw Industries, Inc. | Carpet, carpet backings and methods |
WO1998038375A3 (en) * | 1997-02-28 | 1998-12-03 | Shaw Ind Inc | Carpet, carpet backings and methods |
US8283017B2 (en) | 1997-02-28 | 2012-10-09 | Columbia Insurance Company | Carpet, carpet backings and methods |
US9376769B2 (en) | 1997-02-28 | 2016-06-28 | Columbia Insurance Company | Homogeneously branched ethylene polymer carpet backsizing compositions |
US9051683B2 (en) | 1997-02-28 | 2015-06-09 | Columbia Insurance Company | Carpet, carpet backings and methods |
US8496769B2 (en) | 1997-02-28 | 2013-07-30 | Columbia Insurance Company | Carpet, carpet backings and methods |
WO1999040250A2 (en) * | 1998-02-04 | 1999-08-12 | Mannington Mills, Inc. | Surface coverings containing fused recycled material and processes of making the same |
WO1999040250A3 (en) * | 1998-02-04 | 1999-11-04 | Mannington Mills | Surface coverings containing fused recycled material and processes of making the same |
EP1375731A2 (en) * | 2002-06-26 | 2004-01-02 | Degussa AG | Process for back coating a carpet |
US7014886B2 (en) | 2002-06-26 | 2006-03-21 | Degussa Ag | Tuft and filament binding in unfinished carpet |
EP1375731A3 (en) * | 2002-06-26 | 2004-12-29 | Degussa AG | Process for back coating a carpet |
EP1645682A1 (en) * | 2004-10-10 | 2006-04-12 | Centro Tecnologico de Grupo Copo, S.L. | Manufacturing procedure for carpeting with layered undrlay |
WO2014011450A1 (en) * | 2012-07-10 | 2014-01-16 | Exxonmobil Chemical Patents Inc. | Carpet comprising a propylene-based elastomer and methods of making the same |
US10563055B2 (en) | 2016-12-20 | 2020-02-18 | Exxonmobil Chemical Patents Inc. | Carpet compositions and methods of making the same |
KR20200030072A (en) * | 2017-07-14 | 2020-03-19 | 타케트 지디엘 에스에이 | Carpet backing layer composition |
LU100340B1 (en) * | 2017-07-14 | 2019-01-28 | Tarkett Gdl Sa | Carpet backing layer composition |
WO2019011725A1 (en) * | 2017-07-14 | 2019-01-17 | Tarkett Gdl | Carpet backing layer composition |
RU2745052C1 (en) * | 2017-07-14 | 2021-03-18 | Таркетт Гдл | Composition of carpet base layer |
EP3652376B1 (en) | 2017-07-14 | 2021-09-01 | Tarkett GDL | Carpet backing layer composition |
US11326068B2 (en) | 2017-07-14 | 2022-05-10 | Tarkett Gdl | Carpet backing layer composition |
LU100355B1 (en) * | 2017-08-01 | 2019-02-06 | Tarkett Gdl Sa | Carpet backing layer composition |
LU100738B1 (en) * | 2018-03-19 | 2019-10-01 | Tarkett Gdl Sa | Carpet backing layer composition |
Also Published As
Publication number | Publication date |
---|---|
JP3238468B2 (en) | 2001-12-17 |
DE59201812D1 (en) | 1995-05-11 |
DE4117275A1 (en) | 1992-12-03 |
EP0518014B1 (en) | 1995-04-05 |
JPH05254369A (en) | 1993-10-05 |
ES2072650T3 (en) | 1995-07-16 |
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