MXPA98007210A - Thread for carpet that has high resistance to the ensuciamie - Google Patents

Abstract

This invention relates to carpet yarn comprising a plurality of filaments of a thermoplastic polymer with a fluorochemical or non-fluorochemical compound imparting hydrophilicity, dispersed within said filaments. In still another aspect, the invention relates to a method for producing yarn for carpet, and to the use of yarn for carpet for the production of carpets having high resistance to soiling.

Description

THREAD FOR CARPET THAT HAS HIGH RESISTANCE TO MESSAGE TECHNICAL FIELD This invention relates to the yarn for carpets, more particularly yarn for carpets comprising a plurality of filaments of a thermoplastic polymer. In still another aspect, the invention relates to a method for producing a yarn for carpets. In a further aspect, the invention relates to the use of carpet yarn for the production of carpet having high fouling resistance.

BACKGROUND OF THE INVENTION In the formation of textile materials from extruded thermoplastic polymers, such as poly (alpha-olefin) s, it is standard practice to apply an oil to spin the filaments, yarns, or other textile modalities thereof. Spinning oil, also called spin finish, is an essential lubrication composition deposited on the surface of the fiber made by REF. 28192 \ -.

The man, to reduce the friction of fiber to fiber and the friction developed according to hi-it passes on the metallic surfaces of the machinery. The primary function of a spin oil is to provide surface lubricity to the yarn. Spinning oils also reduce static charges on hydrophobic fibers. These reduce the electrical resistance of the fibers, which allows faster dissipation of the loads.

Spinning oils help prevent breakage of fiber yarn. Spinning oil contains a large number of chemical components, the main components being lubricant, antistatic agent and emulsifier. Also, this can also contain small portions of additives such as antioxidant, corrosion inhibitors, defoamer and antibacterial product. The amount of spinning oil required depends on the producer and the manufacturing steps that follow to convert fibers to useful end products. Typically between approximately 0.9% and 5% of the spinning oil is necessary. A major advantage is that residues of the spinning oil on the extruded fiber reduce the resistance to fouling of the finished product.

In the industrial production of textiles, such as carpets and clothing, it is common to treat such substrates, with a composition for imparting desirable properties added thereto, such as resistance to fouling by particulate or dry dirt. Certain fluorochemical compositions are commercially used for this purpose. These can be applied to various substrates by methods including, for example, spraying, foaming, pad placement, and immersion in a finishing bath. U.S. Patent No. 4,264,484 discloses a liquid composition for the treatment of carpets, containing a water-insoluble addition polymer derived from polymerizable, ethylenically unsaturated monomer, free of non-vinyl fluorine and having at least a transition temperature greater than about 25 ° C, and an ester containing fluoroaliphatic radical insoluble in water and aliphatic chlorine, having at least one higher transition temperature greater than about 25 ° C. U.S. Patent No. 4,107,055 discloses a fabric coating composition, which includes a polymer having a vitreous transition temperature higher than room temperature, an ionic fluorinated surfactant and a carrier. The polymer is preferably applied to the fabric at a ratio that gives a dry solids content of about 0.25 to 10%, to give resistance to dry dirt. U.S. Patent No. 4,043,964 discloses a coating that provides a durable, fouling-resistant carpet, which contains (a) at least one phase of a specified water-soluble addition polymer, derived from a polymerizable ethylenically unsaturated monomer, free from vinyl fluorine and (b) at least one phase of a water-insoluble fluorinated component, specified, containing a fluoroaliphatic radical of at least 3 carbon atoms. The monomer from which the fluorinated component is formed may contain dicarboxylic acid, glycol, diamine, hydroxyamine, etc. A common feature of the treatment or coating compositions described in the aforementioned US Patents Nos. 4,264,484, 4,107,055 and 4,043,964 is that they will be applied to the carpet or the cloth after its production in a separate treatment step. The application equipment and the time required for such a treatment step are added to the cost of the final product. The textile fibers and yarns can be treated by incorporating the fluorochemical product into the spin finishing bath. For example, U.S. Patent Nos. 4,190,545 and 4,192,754 describe the finishing compositions for spinning and yarn finishing for incorporation with the synthetic organic polymer yarn or yarn products, to make them oil repellent and fouling-resistant. . The composition comprises (a) a solution of a salt of dioctylsulfosuccinate, propylene glycol and water, and (b) a fluorochemical compound consisting of polycarboxybenzene esterified with certain partially fluorinated alcohols and with hydroxyl-containing organic radicals, such as 2-hydroxyethyl, glyceryl and chlorohydril and bromohydryl. Alternatively, the treated textile fibers and yarns can be obtained by extruding in a molten form a mixture of a synthetic fiber-forming polymer and a fluorochemical composition. Such extrusion in molten form is described for example in U.S. Patent No. 3,839,312. This patent discloses that the dirt or stain repellency of the extruded filaments of a synthetic resin can be improved by incorporating into the resin a small amount, about 1 percent, of an unfriendly compound having from one to four outstanding fluoroalkyl groups of an organic radical. The repellency is provided by the fluoroalkyl groups, which tend to concentrate on the surface of the fiber. International Patents WO 92/18569 and WO 95/01396 describe polymer compositions permanently resistant to fouling such as fibers and yarns having a fluorochemical product dispersed throughout the length of the polymer. These polymeric compositions are prepared by extruding in molten form the fluorochemical product with the desired polymer. Polymers that can be used with the fluorochemical product include polyester, polypropylene, polyethylene and polyamide. U.S. Patent No. 5,025,052 discloses certain oxazolidinone compositions containing fluoroaliphatic groups. The patent also discloses fibers, films, and molded articles prepared, for example, by injection molding a mixture of synthetic organic polymers, fiber or film formers, and certain fluorochemical oxazolidinones. The resulting fibers, films and molded articles are said to have low surface energy, oil and water repellency, and anti-fouling properties. European Patent No. 0,516,271 describes durable hydrophilic thermoplastic fibers, comprising thermoplastic polymer and nonionic compounds containing fluoroaliphatic group. While many fluorochemical compositions currently used have proven useful in the provision of carpets with resistance to fouling, unfortunately a significant amount of the manufactured carpet can not be treated to obtain the desired properties. The reason is that significant quantities and variants of spinning oil frequently remain on the front pile of the carpet, decreasing the resistance to soiling of the carpet, or acting as contaminants that interfere with the fluorochemical treatment and diminish or prevent the desired result thereof. . Since in each line of carpets can be observed different amounts of oil for residual spinning, it is difficult in the operation of a carpet textile factory to predict which of the carpet lines will present problems in obtaining satisfactory resistance to soiling. Thorough washing of the carpet should be a solution to this problem. However, this method is acceptable in the industry for economic reasons. An object of the present invention is to provide a yarn for carpet, more particularly yarn for carpet comprising a plurality of filaments of a thermoplastic polymer, which can overcome the aforementioned drawbacks due to a reduced amount of spinning oil necessary to provide lubrication of the filaments, or, because in one embodiment, the spinning oil can be replaced by water. A further objective of the present invention is to provide a method for producing a carpet yarn having improved resistance to fouling. Furthermore, an object of the invention is to provide a process for converting the yarn to a carpet having high resistance to fouling.

BRIEF DESCRIPTION OF THE INVENTION In summary, in one aspect, the present invention provides a carpet yarn comprising a plurality of filaments of a thermoplastic polymer with a hydrophilicity imparting compound, dispersed within said filaments. It has been found in particular that the presence of the compound imparting hydrophilicity in the filaments allows the production of yarn for carpet with a reduced amount of spinning oil, or even without the spinning oil normally required. In particular, the spinning oil may at least be partially replaced by water. As a result of the reduced amount of spin oil, carpets produced using such yarn are less susceptible to soiling. In addition, it has been found that the yarn for the carpet according to this invention has a more voluminous appearance than the yarn for carpets that the hydrophilicity imparting compound does not have, probably due to the lower cohesion between the filaments as a consequence of the spinning oil. reduced. The hydrophilicity imparting compound in connection with the present invention may be a fluorochemical product or a non-fluorochemical compound or a mixture of these compounds. The use of a hydrophilicity, fluorochemical imparting compound is, however, preferred. In a further aspect, the present invention provides a method for producing a carpet yarn comprising a plurality of filaments of a thermoplastic polymer having improved fouling resistance, which comprises the steps of a) preparing a mixture comprising the thermoplastic polymer and a hydrophilicity imparting compound, b) extruding the mixture to form filaments, c) treating the filaments in a spin finishing bath, and d) stretching a bundle of filaments to obtain a yarn. In still another aspect of the present invention, there is provided a method for utilizing carpet yarn for the production of carpet having high fouling resistance, without the need to thoroughly wash the carpet or to treat it with the fouling-resistant compositions. The carpet yarn of the present invention comprising a hydrophilicity imparting compound dispersed within its filaments, and present on the surface thereof, which can be prepared by the aforementioned method, provides a unique solution to the problems encountered in the prior art, caused by the oil for residual spinning. U.S. Patent No. 3,839,312 describes the addition of fluorochemical compounds having one to four fluoroalkyl groups protruding from an organic radical to the polypropylene fibers. These fluorochemical compounds do not impart hydrophilicity to the fibers. Even if it was not mentioned in the patent, the application of spin oil is necessary in order to ensure lubrication and to avoid electrostatic charging of the fiber. This results in the previously discussed disadvantageous interference of spinning oil and fluorochemical treatment. The same problems are encountered with the polypropylene fiber treated with a fluorochemical oxazolidinone composition of US Patent No. 5, 025, 052. In contrast to this, the carpet fiber of the present invention is hydrophilic due to the presence of the compound hydrophilicity dispenser, which is dispersed within the filaments, and, as can be concluded from the lubricating properties, is also present on the surface of the same. This allows a considerable reduction of the spinning oil or even the use of water as finishing liquid for spinning. The carpet fibers of U.S. Patent Nos. 4,190,545 and 4,192,754 which are treated with a spin finish comprising a fluorochemical having an aromatic group, they become oil repellent. This feature is not achieved with the carpet fibers of the present invention. The polypropylene fiber described in European Patent Publication No. 0,516,271 which is durably hydrophilic due to the presence of a non-ionic compound containing fluoroaliphatic group, which imparts hydrophilicity to the surface thereof, is not a stretched fiber and It is not suitable for use in the production of carpets.

DETAILED DESCRIPTION The thermoplastic polymers useful in the invention include poly (alpha) olefins, polyesters and fiber-forming polyamides,. Preferred thermoplastic polymers are poly (alpha) olefins. The poly (alpha) olefins of the present invention include the normally solid homo-, co- and terpolymers of aliphatic mono-1-olefins (alpha-olefins) as these are generally recognized in the art. Usually, the monomers used in the manufacture of such poly (α-fa) olefins contain 2 to 10 carbon atoms per molecule, although monomers of higher molecular weight are sometimes used as comonomers. The invention is also applicable to mixtures of polymers and copolymers prepared mechanically or in situ. The monomers used include ethylene, polypropylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, and 1-octene, alone, or in admixture, or in sequential polymerization systems. Examples include polyethylene, the currently preferred polypropylene, polypropylene / ethylene copolymers, polybutylene, and mixtures thereof. Processes for the preparation of various polymers are well known, and the invention is not limited to a polymer made with a particular catalyst or process. The hydrophilicity imparting compounds, suitable for use in this invention, may be fluorochemical or non-fluorochemical compounds, or a mixture of such compounds. The non-fluorochemical hydrophilicity imparting compounds are substantially free of fluorine (preferably containing less than 10% by weight and more preferably less than 5% by weight of fluorine) and are generally hydrophilic in nature or contain at least a portion hydrophilic such that hydrophilicity or wettability can be provided to the surface of the thermoplastic polymer filaments. Low molecular weight compounds, oligomers as well as polymers are included. Suitable hydrophilic, non-fluorochemical imparting compounds are preferably incompatible with the melt of the thermoplastic polymer and are preferably sufficiently stable at the required extrusion temperatures. Suitable non-fluorochemical hydrophilicity imparting compounds may be anionic, cationic, nonionic or amphoteric. The preferred compounds are surfactants. Particularly preferred non-fluorochemical hydrophilicity imparting compounds are those containing a poly (oxyalkylene) group.

Hydrophilicity imparting compounds, fluorochemicals, which are useful in the art of this invention are hydrophilic in nature and include compounds, oligomers, and polymers. For convenience, these are generally referred to herein as fluorochemical compounds. Such materials will contain at least about 10% by weight of fluorine, for example fluorine bonded to carbon. These contain one or more fluorochemical radicals (Rf), and one or more polar groups of water solubilization (Z), whose radicals and groups are usually connected together by suitable linking groups (Q). The fluorochemical radical, Rf, in the agent can generally be described as a fluorinated, preferably saturated, monovalent radical of at least 4 carbon atoms. Preferably, the fluorochemical radical is a fluoroaliphatic, non-aromatic radical. The aliphatic chain may be linear or branched or, if large enough, cyclic and may include oxygen, di- or hexavalent sulfur, or trivalent nitrogen atoms bonded only to the carbon atoms. A fully fluorinated radical is preferred, but hydrogen or chlorine atoms may be present as substituents, with the proviso that not more than one atom of either is present for every two carbon atoms. Fluoroaliphatic radicals containing about 5 to about 12 carbon atoms, are the most preferred. The group or polar portion of water solubilization, Z, of the fluorochemical agent may be a nonionic, anionic, cationic, or amphoteric portion, or combinations of said groups or portions, which may be the same or different. Preferably, the water solubilization group comprises a poly (oxyalkylene) group, (OR ') x, where R' is an alkylene group having from 2 to 4 carbon atoms, such as -CH2CH2-, CH2CH2CH2-, -CH (CH3) CH2) -, and -CH (CH3) CH (CH3) - or mixtures thereof, and x is an integer from about 6 to about 20. The oxyalkylene units in the poly (oxyalkylene) may be the same , as a poly (oxypropylene), or present with a mixture, such as in a linear or branched heteric chain of randomly distributed oxyethylene and oxypropylene units, poly (oxyethylene-co-oxypropylene), or as in a straight or branched chain of blocks of oxyethylene units and blocks of oxypropylene units. The poly (oxyalkylene) chain can be interrupted by or include one or more catenary linkages, providing bonds such that they do not substantially alter the character of water solubilization of the poly (oxyalkylene) chain, and are preferably terminated with hydroxyl or ether portions of lower alkyl, for example -OCH3 or -OCH2CH3. Typical anionic groups include C02H, C02M, S03H, SO3M, OSO3H, OSO3M, 0P0 (0H) 2 and 0P0 (0M) 2, where M is a metal ion (such as sodium or potassium), or ammonium ion, or other cation Not me. Typical cationic groups include NR3 + A ~, where R is a lower alkyl group such as methyl, ethyl, butyl, hydroxyethyl or hydrogen, and A is an anion such as chloride, sulfate, phosphate, hydroxide or iodide. Typical mixed or amphoteric groups could include N + (CH3) 2C2H4COO ", N + (CH3) 2C3H6S03 ~ or an amine oxide The linking group, Q, is a multivalent, generally divalent linking group, such as alkylene, arylene , sulfonamidoalkylene, carbonamidoalkylene, and other heteroatom-containing groups such as siloxane, including combinations of such groups In some cases more than one fluoroaliphatic radical can be coupled to a single linker group, and in other cases a simple fluoroaliphatic radical can be linked by a simple linking group to more than one polar solubilization group, Q can also be a covalent bond.A particularly useful class of fluorochemical agents that can be used in the invention are those of the formula (Rf) nQaZ where Rf is the fluoroaliphatic radical, n is 1 or 2, Q is the linker group, a is zero or one and Z is the water solubilization group. Hydrophilicity-imparting fluorochemical compounds useful in the present invention can be prepared using known methods such as those described in U.S. Patent No. 2,915,554 (Albrecht et al.). Albrecht's patent describes the preparation of non-ionic compounds, containing fluoroaliphatic group, from fluorochemical intermediates containing active hydrogen, such as fluoroaliphatic alcohols, for example RfC2H4OH, acids, for example, RfS02N (R ') CH2COOH, and sulfonamides, for example, RfS02N (R ') H, by reaction of the intermediates for example with ethylene oxide to produce, respectively RfC2H40 (C2H4) nH, RfS02N (R ') CH2CO2 (C2H4O) nH7 and RfS02N (R') (C2H4O) "H, where n is a number greater than about 3, and R 'is hydrogen or lower alkyl (eg, 1 to 6 carbons). Analogous compounds can be prepared by treating the intermediates with propylene oxide, or a mixture of ethylene oxide and propylene oxide. See also the fluoroaliphatic oligomers described in U.S. Patent No. 3,787,351 (Olson), and certain condensates of fluorinated alcohol-ethylene oxide described in U.S. Patent No. 2,723,999 (Cowen et al.). The fluorochemical imparting hydrophilicity compound is added in amounts of between about 0.05 and 2% by weight, preferably between about 0.5 and 1.5% by weight, based on the total weight of the thermoplastic polymer and the fluorochemical compound. In accordance with the present invention, a yarn for carpet can be produced by providing a mixture comprising a thermoplastic polymer and one or more hydrophilicity imparting compounds. This mixture can be extruded to form filaments which are then treated in a spin finishing bath. The filaments are preferably cooled before such treatment. To obtain a thread for carpet, a bundle of filaments is stretched. Stretching can be carried out on a pair of rolls that are at a sufficiently high temperature to soften the thermoplastic polymer. By rotating the rollers in a pair at different speeds, the stretching of the filaments can be obtained. While the stretching can be carried out with a pair of rollers, it may be desirable to stretch the filaments over two pairs. Typically, they will be stretched 3 to 4 times the extruded length. Subsequent to stretching, it will often be desirable to texture the carpet yarn with pressurized air at an elevated temperature or with a steam jet, and subject it to an entanglement. The spin finish which is useful in the present invention includes any conventional spinning oil, used for the extrusion of thermoplastic polymers. Surprisingly, the spin finish can also be water without any spin oil added to it. The spin finish can be applied using methods known in the art. An example includes the application of tangential roller. The lower part of the tangential roller is immersed in the finishing bath, while the yarn moves tangentially on the upper part. The aggregate level of the spinning oil can be varied by changing various parameters, such as the geometry between the yarn and the roller, the speed of the roll and the concentration of the oil for spinning in the spin finishing bath. When spinning oil is used, the parameters will be adjusted so that the residual amount of spun oil on the filament will be between about 0.01% and 1.2% by weight, preferably between about 0.01% and 0.6% by weight, based on the total weight of the filaments and spinning oil. More preferably, the residual amount of spinning oil will be less than 0.4%. It may also be desirable to wet the filaments during or subsequent to the stretching operation applied thereto. In this way the lubrication can be improved when the filaments leave the stretching unit. Loss of lubrication may occur during stretching as a result of water evaporation during stretching. Similarly, prior to or subsequent to texturing, yarn wetting can compensate for the loss of lubrication during texturization.

PROOF PROCEDURES The following tests have been used to evaluate the carpet yarn of the present invention.

DETERMINATION OF FLUORIDE IN THE FIBER In order to determine the amount of fluoride in the extruded fiber, the following method is used: a known weight of the sample is placed in an ignition basket made of platinum wires.The sample is then decomposed in a polycarbonate flask sealed, in the presence of oxygen and a known volume of buffer solution, TISAB III (available from Orion) After absorption in the buffer, the fluoride is measured with an Orion 9409 (fluoride sensitive) electrode connected to a potentiometer using mV mode of operation The amount of fluoride is then calculated from the reading of mV using a graph plotted from the standard fluoride solutions All the samples were analyzed in duplicate and the results should show a variation of less than 10 % to be considered uniform When calibrated properly, the electrode measurement will be reproducible with an approximate deviation 9.9o- • Test of_Caminata On the Carpet The fouling resistance properties of the carpets made from the carpet yarn of the present invention were measured following the regulations, the standard test method of the American Association of Textile and Color Chemicals (AATCC) No. 122-1987: "Carpet Fouling: Service Soiling Method", with some deviations as described below. The carpet test specimen was placed in the walking area, without using a standard level of dirt, until a predetermined number of foot traffic was obtained. The foot traffic was measured electronically using an "electronic eye" Hengstler 890, available from Hengstler Brussels, Belgium. After finishing the walk test, all test samples were vacuumed before evaluation. The degree of fouling was measured as a color deviation compared to a white reference plate, using a reflectance meter II Minolta Chroma, obtainable from Minolta Camera Co. , Japan. (The coordinates, printed on the white plate and given by Minolta Camera Co. were Y: 88.7, x: 310 e and: 318). The Minolta Chroma reflectance meter records the color difference as delta E (? E). A smaller value? E represents a lesser degree of soiling; A value of? E of 3 or greater represents a visible difference in fouling.

Abbreviations The following abbreviations and trade names are used in the examples: MeFOSA: C8F17S02NH2 EtFOSEMA: N-Ethyl-perfluorooctyl-sulphonido-ethyl methacrylate BuFOSEA: N-buty 1-perfluorooctyl-sulphonido-ethylacrylate JeffamineMR ED ethylene oxide-propylene oxide 600 amino-terminated, available from Huntsman, United States CW 750 A: acrylate of a methoxy-polyethylene glycol of average molecular weight of 750, commercially available from British Petroleum International Ltd, United Kingdom Pl 44A: acrylate of an ethylene oxide- propylene-ethylene glycol oxide (commercially available from Pluronic ™ 44 from BASF AG, Germany) Genopol ™ 26-L-80: C 2 2-6H25-33 (OCH 2 CH 2) 9.5OH, derived from a primary alcohol, commercially available from Hoechst Celanese Corp. , United States Ej emplos All parts, proportions, percentages, etc. in the following examples and in the remainder of the specification, they are by weight, unless otherwise indicated. Mixtures of the hydrophilicity imparting compounds and the thermoplastic polymer were prepared and extruded into filaments according to methods known in the art. The extrusion temperature is maintained below 310 ° C in order to prevent decomposition. A bundle of filaments was treated in a finishing spin bath comprising an aqueous solution of spin oil or only water, after which the bundle was stretched to form a yarn. The thread was subsequently knotted to form the carpet.

Hydrophilicity imparting compounds: Fluorochemical compounds FC-1 C8 F17 S02N (C2H5) CH2CH20 (CH2CH20) 7CH3 (prepared according to Patent No. 2, 915, 554).

FC-2 2 C8F? 7S03H. Jeffamine ED-600 di-salt (compound No. 1 in U.S. Patent No. 4,975,363). FC-3 an EtFOSEMA / CW 750A copolymer in a ratio of 30/70, prepared in accordance with US Pat. No. 3,787,351 ex. 2. FC-4 a copolymer of BuFOSEA / Pl 44A in a ratio of 30 / 70 and prepared in accordance with US Pat. No. 3,787,351 ex. 1. FC-5 a non-ionic compound containing fluorochemical group of the structure C8H17S02N (C2H5) (CH2CH20) 2- (CH (CH3) CH20) 6H prepared in accordance to US Patent No. 2,915,554 FC-6 C8F17S02N (CH3) -Genopol® 26-L-80 made from C8F17S02NH2 and Genopol® 26-L-80 according to the following procedure. To a three-neck round bottom flask, equipped with an overhead stirrer, thermometer, reflux condenser and two gas flushing bottles coupled, the second bottle containing a 10% aqueous solution of sodium hydroxide, were charged - 200.83 g (0.337 eq.) Of Genapol ™ 26-L-80 and 5.5 g of Celite ™ filter agent (commercially available from Aldrich Chemical Co.). The mixture was heated to 60 ° C, then 48.12 g (0.4045 eq., A molar excess of 20%) of thionyl chloride was added via an addition funnel over a period of about 22 minutes, raising the temperature of the mixture to 75 ° C. Then nitrogen was bubbled through the reaction mixture for 4 hours, during which time the temperature of the mixture varied from 68 to 71 ° C. The reflux condenser and the flushing bottles were replaced by a stationary head, and the reaction mixture was stirred while applying a vacuum of approximately an absolute pressure of 50 torr. After the reaction was complete by 13 C and 1 H analysis of an aliquot, the reaction mixture was filtered hot through a Buffered glass funnel of porosity C, to produce Genapol ™ 26-L-80 chloride. A 125 g (0.244 eq.) Of C8F17S02NH2 (MeFoSA), 179.93 g (0.249 eq.), Or a solution was charged to a three-neck round bottom flask equipped with an overhead stirrer, reflux condenser and adapter for nitrogen inlet. 2% molar excess) of Genapol ™ 26-L-80 chloride (from the preparation given above), 37.71 g (0.355 eq., or 50% molar excess) of sodium carbonate and 2.76 g (0.0141 eq. ., or 8.5 mol percent with respect to MeFOSA) of potassium iodide. The reaction mixture was heated to 120 ° C for 8 hours, at which time the MeFOSA had disappeared according to the analysis using gas chromatography. After cooling to 95 ° C, the reaction mixture was washed with 157 g of 10% aqueous sulfuric acid followed by 157 g of deionized water. The washed reaction mixture was concentrated by evaporation on a rotary evaporator at 70 ° C and an absolute pressure of 50 torr, to give a straw-colored liquid, whose structure was characterized by 13 C and 1 H NMR spectroscopy to be consistent with the adduct of desired ether.

Non-fluorochemical hydrophilicity imparting compounds: HC-1 Triton ™ X-100, an ethoxylated alkylphenol (9.5) commercially available from Union Carbide Corp., United States. Thermoplastic polymer: polypropylene with a melt index of 12, available from Borealis NV, Brussels, Belgium.

Carpet Thread In a first step, master batches of polypropylene containing varying amounts of the hydrophilicity imparting compound were prepared. The method of forming the mixture is not critical. The mixture can be formed by injecting an FC or HC compound into a twin screw extrusion barrel in which the polypropylene is already in a molten state. The extruded compound was then cut into granules or pellets. In a second step, the granules were further mixed with polypropylene in various amounts to give different proportions of polypropylene / hydrophilicity imparting compound, as given in tables 1 and 5. Comparative examples C-1 to C-4 were made from pure polypropylene , without any addition of FC or HC compound. The mixtures thus formed were extruded with a Thermo Alfa single screw extruder (triple extruded - one end) at approximately 230 ° C on rotating plates with a trilobal cross section.

After leaving the extruder, the filaments passed through a cooling zone on a tangential roller, where a water solution was applied with a conventional spinning oil, such as Lertisan 2515 (examples 1 to 8, C-1 to C -3) or FA 2825 (examples 10 to 17, C-4) available from Zschimmer and Schwartz. Alternatively, the spin finishing bath contained only water (example 9). The amount of spinning oil applied to the yarn was varied by adjusting the speed of the tangential roller and the concentration of the spinning oil in the finishing spin bath. In the experiments, the speed of the tangential roll was varied between 19 and 7.5 rpm, and the concentration of the spinning oil in the finishing spin bath was varied between 0 and 15%. The yarn for carpet was then stretched approximately 3-4 times the extruded length, to obtain a yarn with one tex (weight (g) / 1000m) of about 165 (examples 1 to 9 and C-1 to C-3) or approximately 200 (examples 10-17 and C-4). The yarn was textured at a temperature of 140 ° C to 180 ° C to produce a bulky or fluffed yarn that is particularly useful for the production of carpets.

The foamed yarn was visually inspected for mechanical quality after spinning and texturing. The foamed yarn made according to the present invention had no visible broken filaments. The thread was then knotted in carpet form by conventional means: Table 1: Composition of polypropylene filaments Notes:% of oil for spinning *: oil for residual spinning on the fiber; determined by extraction with acetone.

The fiber of example 1 shows a higher level of oil for residual spinning than the fiber of comparative example C-1, although the finishing conditions for spinning were the same (the same tangential roll speed and the same spin oil concentration) in the bathroom) . Through the imparting effect of hydrophilicity of the fluorochemical compound more oil is collected for spinning the tangential roller. Comparative example C-3, which does not contain fluorochemical compound or HC compound and only 0.3% spin oil, could be processed on the pilot equipment used under close supervision. The conditions were nevertheless in the limit line and are not practical for large-scale experiments. High constitution or static formation is unacceptable for large scale production. Due to the low level of spinning oil used, filament repellency occurs. The filament bundle widens causing problems during additional production steps, such as texturing and entanglement. On the other hand, Example 9, which does not contain spin oil (treated in a spin finishing bath containing only water, thus without any addition of spin oil), but containing 0.8% fluorochemical, does not shows production problems at all. No static production is perceived. The Thermo Alfa single screw extruder used for the extrusion of the fibers, requires a constant pressure before the pump for yarn of 5000 KPa. In order to maintain this pressure, the extruder unit automatically adjusts the speed of the extruder screw. It has been observed that by using the fluorochemical compound, the extrusion pressure is more constant, resulting in less fluctuation of the extruder screw speed. As a result, the extrusion process runs smoother, less motor current is required (checked periodically during the extrusion process and recorded in table 2) and a reduction in the noise level is observed.

Table 2: extrusion parameters Notes: For safety reasons, in order not to damage the extruder screw, the speed of the extruder screw is programmed not to exceed 100 rpm. For examples 7-9, the speed of the spinning pump was manually decreased from 20 rpm to 18.5 rpm, because to obtain a pressure of 5000 KPa, the screw needs to exceed 100 rpm. Examples 1-9 show a clear lubricating effect of the fluorochemical compound. Less energy is required to obtain the same pressure (directed at 5000 KPa before the spin pump). The physical properties of the yarn for carpet, polypropylene, were measured using an Instron Dynamometer (caliber: 500 mm; crosshead speed 11 mm / sec.). The results, recorded in Table 3, are the average values of 20 measurements.

Table 3: physical properties of polypropylene yarn for carpet Table 3: physical properties of polypropylene yarn for carpet (continued) Notes: module E-l: module between 1-elongation and 3% modulus E-2: module between an elongation of 1 and 5% tex = weight of the sample (g) / 1000 meters.

As can be seen from the results, the physical properties of the filaments remain very similar, although the amount of fluorochemical compound and / or spin oil is varied.

Carpet production In a third step, the thread was knoton a Cobble ST 85 RE machine 1 meter wide, simulating the industrial knotting equipment. The adjustment was 252 needles / meter. The knot speed was 1200 rpm. The knotsheet used was polypropylene, either woven and non-woven fabric. The carpets produced were tesfor their fouling resistance properties by subjecting them to the walk test for 9000 steps. The results of? E are given in Table 4.

Table 4: Results of the polypropylene carpet walk test Table 4: Results of the polypropylene carpet walk test (continued) As expec no major differences were observed between the carpets with the woven and non-woven reinforcement. The results clearly indicate that carpet with superior fouling resistance can be processed using a lower level of spinning oil than standard practice. Example 9, made from yarn for carpet treawith pure water and without oil for spinning, has the best properties of resistance to fouling. Although it appears that comparative example C-3 also has good anti-fouling properties, as mentioned above, this example can not be practiced on a large scale due to the high static production.

Examples 10 to 17 and comparative example C-4 Examples 10 to 17 were made using different fluorochemical imparting compounds of hydrophilicity and / or different compounds containing non-fluorinapolyoxyethylene group, as given in Table 5. Depending on the viscosity of the compound, master batches having different concentration of the compound were prepared. in polypropylene. The final composition is chosen so that the extruded fiber contains about 1.2% fluorochemical compound. This proportion is higher for the non-fluorinacompound (approximately 2%). Comparative example C-4 is performed without the addition of an FC or HC compound.

Table 5: Composition of polypropylene filaments Table 5: Composition of polypropylene filaments Note: Oil for residual spinning: oil for residual spinning on the fiber; determined by extraction with acetone.

In order to be processable, comparative example C-4 without hydrophilicity imparting compound, required a spin finish bath concentration that was much higher than the samples containing the hydrophilicity imparting compound (finishing for residual spinning preferably from at least 1%). It has been observed that by using the hydrophilic compound, the extrusion process runs smoother. Less current is needed in the motor (checked periodically during the extrusion process and recorded in Table 6) and a reduction in the noise level is observed.

Table 6: Extrusion parameters The physical properties of polypropylene carpet yarn were measured using an Instron Dynamometer (500 mm gauge, cross head speed 11 mm / sec.). The tensile strength (maximum) and the elongation until the thread was broken was measured according to ISO 2062 (1972) (the tex was measured according to ISO 2060 (1972).) The results, registered in the Table 7 are average values of 20 measurements.

Table 7: Physical properties of polypropylene yarn for carpet Note: tex = sample weight (g) / 1000 meters As can be seen from the results, the physical properties of the filaments remain very similar.

Carpet production In a third step, the thread was knotted on a Cobble ST 85 RE machine of a width of 1 meter, simulating the industrial knotting equipment. The adjustment was 252 needles / meter. The knot speed was 1200 rpm. The knotted sheet used was woven polypropylene. The carpets produced were tested for their fouling resistance properties by subjecting them to the walk test for 9000 steps. The walk test described above was modified in that as a reference example, the corresponding non-fouled sample (which was not layered in the walking area) of a sample that is tested was used. This eliminates the slight changes in color of the fiber, caused by some of the additives. The results of? E are given in Table 8.

Table 8: Results of the polypropylene carpet walk test Table 8: Results of the polypropylene carpet walk test (continued) It is noted that in relation to this date, the best method known to the applicant to carry out the aforementioned invention, is that which is clear from the present description of the invention.

Having described the invention as above, property is claimed as contained in the following:

Claims (23)

RE IVINDICACI ONE S

1. A yarn for carpet, characterized in that it comprises a plurality of filaments of a thermoplastic polymer with a fluorochemical compound imparting hydrophilicity, dispersed within said filaments.

2. A carpet yarn according to claim 1, characterized in that the thermoplastic polymer is a poly (alpha) olefin.

3. A carpet yarn according to claim 2, characterized in that the poly (alpha) olefin is polypropylene.

4. A yarn for carpet according to claim 1, characterized in that the fluorochemical compound is a fluoroaliphatic compound.

5. A carpet yarn according to claim 4, characterized in that the fluoroaliphatic compound is represented by the formula wherein Rf is a fluorinated monovalent residue having at least 4 carbon atoms, Q is a linking group or a covalent bond and Z is a hydrophilicity imparting group.

6. A yarn for carpet according to claim 5, characterized in that the fluoroaliphatic compound comprises poly (oxyalkylene) units as hydrophilicity imparting groups.

7. A yarn for carpet according to claim 1, characterized in that the amount of fluorochemical compound imparting hydrophilicity is 0.05 to 2.0% by weight, based on the total weight of the thermoplastic polymer and the fluorochemical compound imparting hydrophilicity.

8. A yarn for carpet according to any of claims 1 to 7, characterized in that it comprises oil for spinning in an amount of less than 0.4% by weight, based on the total weight of the yarn for carpet and the oil for spinning, on its surface.

9. A carpet yarn, characterized in that it comprises a plurality of filaments of a thermoplastic polymer with a hydrophilicity imparting compound dispersed within said filaments, and the carpet yarn comprises oil for spinning in an amount of 0.01 to 0.4% by weight, based on in the total weight of the yarn for carpet and the oil for spinning, on its surface.

10. A carpet yarn according to claim 9, characterized in that the hydrophilicity imparting compound is a non-fluorochemical compound.

11. A yarn for carpet according to claim 1 or 10, characterized in that it comprises dispersed in the filaments, a mixture of a non-fluorochemical compound imparting hydrophilicity and a fluorochemical compound imparting hydrophilicity.

12. A yarn for carpet according to claim 10 or 11, characterized in that the non-fluorochemical compound imparting hydrophilicity comprises poly (oxyalkylene) units.

13. A method for producing a yarn for carpet, comprising a plurality of filaments of a thermoplastic polymer having improved resistance against fouling, characterized in that the method comprises the steps of: a) preparing a mixture comprising a thermoplastic polymer and a fluorochemical compound imparting hydrophilicity, b) extruding the mixture to form filaments, c) treating the filaments in a spin finishing bath, and d) stretching a bundle of filaments to obtain a yarn.

14. A method according to claim 13, characterized in that the amount of the fluorochemical compound is from 0.05 to 2% by weight, based on the total weight of the thermoplastic polymer of the fluorochemical compound.

15. A method for producing a yarn for carpet, comprising a plurality of filaments of a thermoplastic polymer having improved resistance against fouling, characterized in that the method comprises the steps of: a) preparing a mixture comprising a thermoplastic polymer and a hydrophilicity imparting compound, b) the extrusion of the mixture to form filaments, c) the treatment of the filaments in a finishing bath for spinning containing an amount of spin oil such that a residual amount of the spin oil of 0.01 to 0.4% by weight, based on the total weight of the filaments and the spin oil, is retained on the filaments after the treatment, and d) the stretching of a bundle of filaments to obtain a yarn.

16. A method according to claim 15, characterized in that the hydrophilicity imparting compound is a non-fluorochemical compound.

17. A method according to claim 13 or 16, characterized in that the hydrophilicity imparting compound is a mixture of a fluorochemical imparting hydrophilicity and a non-fluorochemical imparting hydrophilicity compound.

18. A method according to claim 16 or 17, characterized in that the non-fluorochemical compound comprises poly (oxyalkylene) units.

19. A method according to claim 13, characterized in that the finishing bath for spinning consists of water.

20. A method according to any of claims 13 to 18, characterized in that the finishing bath for spinning comprises water and an oil for spinning.

21. A method according to any of claims 13 to 20, characterized in that the filaments are wetted during and / or subsequent to the stretching.

22. A method according to any of claims 13 to 21, characterized in that the yarn obtained is further textured and the yarn is wetted before and / or subsequent to texturization.

23. A carpet, characterized in that it comprises a carpet yarn according to any of claims 1 to 12.