Method for preparing recyclable textile products and said products

Abstract

The present invention relates to a method for producing a (recyclable) polyester textile product, comprising providing a first polyester sheet, stitching polyester yarn through the first sheet to form a pile on a first surface of the first sheet and a yarn loop at an opposite second surface of the first sheet, the pile extending from the first surface, applying a first amount of a dispersion comprising an aqueous dispersion medium and polyester particles dispersed in the medium to the second surface of the first sheet, then removing the aqueous dispersion medium from the aqueous dispersion, heating the polyester particles to a temperature above the temperature at which the polyester of the particles softens, and subsequently cooling the polyester of the particles to a temperature below the temperature at which the polyester solidifies, thereby interconnecting the loop and the first sheet with the solidified polyester, wherein the polyester particles are composed of a polyester material having an HLB (hydrophile-lipophile balance) value of 7.6 to 10.5. The invention also relates to the (recyclable) textile product itself.

Description

[0001] General Field of the Invention

[0002] The present invention generally relates to a method for producing recyclable textile products, in particular floor coverings such as carpets, carpet tiles, rugs or mats, and their production. In particular, the invention relates to the production of textile products in which yarn is sewn to a sheet material (commonly referred to as a primary backing) to form a pile on a first surface of the sheet material and to form yarn loops at an opposing second surface of the first sheet material, thereby permanently connecting the yarn to the sheet material at the second surface. The invention also relates to the recyclable textile products themselves. Background of the Invention

[0004] Typically, textile products such as floor coverings are manufactured using latex (natural latex or a corresponding synthetic latex) as an adhesive applied to the back of a primary backing to durably bond the yarn to the primary backing by embedding the loops. Latex-based floor coverings have several disadvantages. First, latex coverings tend to be moisture-resistant. They can allow moisture to pass through, which can lead to the formation of mildew and mold. This not only reduces the quality of the floor covering but can also cause environmental hazards such as poor air quality. Therefore, when latex-based floor coverings are placed in areas with humidity, such as in lobbies, they may need to be replaced frequently. Second, and more importantly, because latex-based floor coverings use different materials for the yarn, primary backing, adhesive, and often also for the secondary backing (if present), such coverings cannot be fully recycled, or at least not in a simple, economically viable process. Carpet recycling technologies have been developed, but they are expensive and do not achieve complete recovery of the materials used, primarily due to the dense embedding of the yarn and backing in vulcanized latex. As a result, most ground covers are simply discarded, incinerated, or shredded. In the best-case scenario, the shredded ground cover ends up in landfill, but because the vulcanized latex is virtually non-biodegradable (even though the yarn and primary backing are), the shredded remnants will remain for years.

[0005] Alternatively, conventional latexes can be replaced by adhesives composed of synthetic polymers, such as polyolefins and polyurethanes. This is known, for example, from US 2010 / 0260966, which discloses a carpet tile comprising a face fabric having a top surface and a base, and a dimensionally stable nonwoven backing material into which a stabilizing material is incorporated. The nonwoven backing material is attached to the face fabric using a synthetic polymer adhesive, in which the backing material and the fabric are embedded to achieve a sufficient bond. However, in addition to the fact that this method is relatively complex, complete recycling of this known carpet tile is virtually impossible due to the face fabric and backing material being embedded in the polymer.

[0006] Another solution proposed in the art is the use of hot-melt adhesives. These adhesives are popular for traditional roll-type carpets because they are relatively inexpensive, readily available, and can be easily recycled. Hot-melt adhesives are also used in carpet tiles, as described, for example, in WO 2007 / 127222. Nevertheless, complete recycling remains difficult, given that the bonding of the fabric to the backing when using hot-melt adhesives requires substantial embedding of the material in the adhesive. The fabric, backing, or both are inevitably contaminated with significant amounts of adhesive. Furthermore, the achievable tuft bond strength when using hot-melt adhesives is relatively low. Consequently, such products are typically used in low-end applications.

[0007] A method for preparing a textile product is known from EP1598476. The method comprises providing an intermediate product comprising a primary backing and a yarn applied to the backing, and feeding the intermediate product along a body having a heated surface, the backing surface being pressed against the heated surface to at least partially melt the yarn present in the intermediate product to form the textile product. Thereafter, the textile product is cooled to normal room temperature, thereby solidifying the molten yarn material. Using this method, the yarn can be properly anchored in the backing without the need for a secondary backing or, for example, latex. Therefore, the method known from EP1598476 offers significant advantages not only in terms of recycling but also in terms of energy and raw material conservation. However, the strength of the yarn anchoring in the backing is insufficient for applications in which the textile product is subjected to high mechanical loads, such as in the interiors of cars, trains, airplanes, offices, shops, etc. This is why, before the intermediate product is pressed against the heated surface to anchor the yarn, a thermoplastic adhesive is preferably applied to the back of the intermediate product.

[0008] Yet another solution is proposed in WO2012 / 076348. This method improves upon the method known from EP1598476 by ensuring that the portion of the back surface pressing against the heated surface has a relative speed relative to the heated surface. In the '476 patent, the heated drum rotates together with the intermediate product, ensuring that the portion of the back surface pressing against the heated surface has essentially the same speed as the heated surface. This, in turn, causes no, or at least minimal, mechanical interference with the placement of the yarn into the backing, and in particular ensures that the yarn is not pulled out of the backing. However, as described in the '348 patent, significantly improved textile products can be achieved when a relative speed exists between the portion of the back surface pressing against the heated surface and the heated surface itself. By enforcing the relative speed, additional mechanical force is applied to the molten material that actually spreads the yarn. This has the advantage of providing a more secure anchoring and, for many applications, eliminates the need for applying additional adhesive. This also makes product recycling easier. Despite this, the resulting tufting bond is still considered insufficient for many high-end applications.

[0009] An improved process is again described in US 1,0428,250, in which the process disclosed in WO 2012 / 076348 is combined with the use of a hot melt adhesive to provide additional tuft bond strength and the option of applying a secondary backing. Although recycling is less complicated when compared to latex due to the presence of the hot melt adhesive, the process is quite complex and requires unconventional production equipment when compared to conventional latex floor covering machinery, essentially consisting of a first station for applying a latex dispersion to the back of the tufted primary backing and a long oven for curing the latex.

[0010] US2018 / 0119339 discloses a method for producing a textile product in which a thermoplastic polymer coating is used as an adhesive. The method comprises applying an aqueous dispersion of thermoplastic polymer particles having an average particle size of 1 to 1,000 microns to the back of a primary backing of a tufted textile product. The method comprises heating the aqueous dispersion to a temperature sufficient to remove water therefrom, and heating the thermoplastic particles on the primary backing to a temperature equal to or greater than the melting temperature of the thermoplastic particles. The method also comprises cooling the heated thermoplastic polymer particles to below their melting temperature, thereby adhering the back of the coil to the primary backing. This method has the advantage that conventional production equipment for latex floor coverings can be used. However, recycling is still not necessary, especially when the goal is to produce high-end textile products with durable, waterproof tufted bonds.

[0011] Purpose of the Invention

[0012] One object of the present invention is to devise an alternative method for producing a textile product that is very easy to recycle in its entirety, but which is relatively simple, preferably based on known equipment for producing latex floor covering products, while at the same time achieving a high and durable tuft bind under normal load conditions and ambient conditions, making the product suitable for high-end applications. Another object of the present invention is to provide a textile product that is easy to recycle and is suitable for said high-end applications. SUMMARY OF THE INVENTION

[0014] To achieve the objects of the present invention, a new method for preparing a textile product is devised, the method comprising providing a first polyester sheet, stitching polyester yarn through the first sheet to form a pile on a first surface of the first sheet and to form yarn loops at an opposite second surface of the first sheet, the pile thus extending (in a perpendicular direction) from the first surface, applying a first amount of a dispersion to the second surface of the first sheet, the dispersion comprising an aqueous dispersion medium and polyester particles dispersed in the medium, and then removing the aqueous dispersion medium from the amount of aqueous dispersion, heating the polyester particles to a temperature above the temperature at which the polyester of the particles softens, and subsequently cooling the polyester of the particles to a temperature below the temperature at which the polyester solidifies, thereby interconnecting the loops and the first sheet with the solidified polyester, wherein the polyester particles are composed of a polyester material having an HLB (hydrophile-lipophile balance) value of 7.6 to 10.5.

[0015] A key feature of this approach is the application of only polyester materials—that is, polyester for the primary backing (i.e., sheet), yarn, and adhesive. While this might seem like an open door for ease of recycling, as any experienced practitioner will understand, the strict constraints imposed by requiring all essential components to be polyester and meeting very different mechanical requirements make it difficult to design a product that meets high-end demands while also being easily manufactured using existing latex-based manufacturing technologies. The type of adhesive is particularly critical, as the application process limits the type of polyester that can be used, but it's worth noting that the desired properties for tuft bond and durability are difficult to achieve without sacrificing manufacturing technology. This is widely recognized in the art. The solution is typically to add fillers, viscosity modifiers, lubricants, plasticizers, wetting agents, and the like to the polyester adhesive to ensure that the polyester can be applied as a normal dispersion while preventing any negative impact of the adhesive on the pile structure, while ensuring a strong and durable tuft bond. For example, the recent patent application US2018 / 0119339 discloses that fillers are typically used in an amount of 10% to 50%, and up to 5% each of plasticizers, thickeners, wetting agents, etc. (see Table 1 of US2018 / 0119339). However, the addition of fillers and other substances is a serious disadvantage for easy recycling, because the polyester may need to be purified when it is recycled, for example by using filters, chemical degradation methods, specific absorption using activated carbon or other agents, etc. However, the inventors have found that when a polyester with an HLB value of 7.6 to 10.5 is used as an adhesive, the preparation using a polyester dispersion is feasible while achieving high tuft bonding and durable bonding without the need to add large amounts of fillers, tackifiers, plasticizers, wetting agents, etc.

[0016] The reason why the HLB value of polyesters used as adhesives is so crucial is not entirely clear. The HLB system, which is specifically used to identify surfactants for oil and water emulsification, is also used in the art to characterize (polyester) polymers (see, for example, "Anticancer efficiency of curcumin-loaded invertible polymer micellarnanoassemblies" in Ivan Hevus et al., Nanostructures for Cancer Therapy, 2017, Chapter 14, 351-382). It is specifically used to identify agents capable of emulsifying two separate phases, rather than to characterize one of these phases itself. However, since the HLB value represents the relationship between the hydrophilic and hydrophobic groups of a surfactant, it is likely related to the nature of the polyester yarn loops that fit closely to the back surface of the backing. In order to achieve high tufting adhesion and good durability, it is necessary, on the one hand, that the polyester (in its molten / softened state) be able to flow around the yarn loops and wet the back surface of the backing, and on the other hand, that the polyester not be released under the influence of moisture, load, and temperature, for example, due to washing procedures involving water. Clearly, for all-polyester textile products, the HLB value appears to be critical to the preparation and durability of the product. In any case, when polyester adhesives meet the currently discovered HLB values, products can be prepared using techniques that correspond to commonly used latex application and drying equipment while achieving high tuft binding and durable bonding without the need to add large amounts of fillers and other materials to the polyester.

[0017] The molecular weight of the polyester does not appear to be critical to the present invention. Generally, any molecular weight (Mn) between 1000 and 100,000 can be used in dispersions according to the present invention, as long as the HLB standard is met. A preferred range is 5000 to 10,000. The molecular weight (Mn) can be determined, for example, by gel permeation chromatography. This is a polymer-specific method that belongs to the category of size exclusion chromatography (SEC).

[0018] In order to achieve the second object of the present invention, a (recyclable) polyester textile product has been designed, which includes a first polyester sheet, a polyester yarn sewn through the first sheet to form a pile on a first surface of the first sheet, the pile extending from the first surface and forming yarn loops at the opposite second surface of the first sheet, and a polyester adhesive provided at the second surface of the first sheet to interconnect the loops and the first sheet, wherein the polyester adhesive is composed of a polyester material having an HLB (hydrophilic-lipophilic balance) value of 7.6 to 10.5.

[0019] It is noteworthy that US Pat. No. 5,472,763 discloses a method for preparing textile products using an aqueous dispersion medium and polyester particles dispersed therein. However, the HLB value of the polyester used is not disclosed.

[0020] GB2097005 discloses aqueous dispersions of polyester particles. The HLB value of the polyester used is not disclosed. However, given that a water-soluble organic compound is required to increase the hydrophilicity of the polyester resin and thereby enable and disperse these resins in water, this suggests that the HLB value of the resin is not within a range that allows the particles to be dispersed themselves, contrary to the present invention.

[0021] EP3196351 provides a fiber sizing composition containing a polyester resin (A) and a reactive compound (B), wherein the polyester resin (A) is a polyester resin having an HLB of 4 to 18 and a viscosity at 30°C of 10 to 1,000,000 Pa.s, and wherein the reactive compound (B) is at least one reactive compound selected from blocked isocyanates, tertiary amines, tertiary amine salts, quaternary ammonium salts, quaternary phosphonium salts and phosphine compounds, and the weight ratio of the polyester resin (A) to the reactive compound (B) [(A) / (B)] in the fiber sizing composition is 99.9 / 0.1 to 10 / 90.

[0022] DATABASE WPI, Week 199649, Thomson Scientific, London, GB; AN 1996-493568XP002802296, & JP HOS 253729 A (TOYOBO KK) 1 October 1996 (1996-10-01) discloses an aqueous polyester dispersion in which the polyester particles have a size of less than 1000 nm. The HLB value is not disclosed.

[0023] EP0604897 discloses a thermoplastic tufted carpet comprising a primary backing, tufts tufted into the primary backing, a secondary backing, and a polyester hot melt adhesive disposed between the primary backing and the secondary backing. Such a carpet can be recycled by known methods for recycling polyester, including saccharolysis or methanolysis.

[0024] US2014 / 272262 discloses a polyester floor covering product comprising a 100% polyester solution-dyed face yarn, a polyester primary backing layer, a polyester adhesive layer, and a 100% polyester secondary backing layer having a weight of 200 gsm to 1000 gsm.

[0025] definition

[0026] A textile product is a product that includes a textile (i.e., a material primarily made of natural or man-made fibers, commonly referred to as thread or yarn), optionally with other components such as a backing layer, a carrier layer, and / or an adhesive. Laminated textile products typically include an upper pile layer attached to a backing (wherein the pile fibers are also referred to as the "pile" of the product), but may also be plain woven. Such products can have a variety of different constructions, such as woven, needle felt, knotted, tufted, and / or embroidered, but tufted products are the most common type. The pile can be cut (as in plush carpets) or formed into loops (as in Berber carpets).

[0027] Polyesters are polymers in which monomer units are linked together by ester groups. They are generally formed by the polymerization of polyols and polyacids and are primarily used to prepare resins, plastics and textile fibers. It is well known that polyesters can be prepared by a condensation polymerization process in which monomers (including ester-forming derivatives thereof) providing an "acid component" are reacted with monomers providing a "hydroxyl component." It will be understood that the polyester polymers described herein may optionally contain autoxidisable units in the backbone or side chains, and such polyesters are referred to as autoxidisable polyesters. If desired, the polyesters may also contain other linking groups, for example by including an appropriate amino-functional reactant as part of the hydroxyl component or alternatively all of the hydroxyl component may contain an amino-functional reactant and contain a proportion of carbonylamino linking groups -C(=O)-NH- (i.e., an amide linking group) or -C(=O)-NR 2 -(tertiary amide linking group), thereby producing a polyesteramide resin, or any other copolyester known in the art.

[0028] There are many dicarboxylic acids (or their ester-forming derivatives, such as anhydrides, acid chlorides or lower (i.e. C 1-6 Examples of suitable acids and their derivatives that can be used to obtain polyesters include adipic acid, succinic acid, sebacic acid, 1,4-cyclohexanedicarboxylic acid, 1,3-cyclohexanedicarboxylic acid, 1,2-cyclohexanedicarboxylic acid, isophthalic acid, terephthalic acid, 2,6-naphthalene dicarboxylic acid, 2,5-furan dicarboxylic acid and / or their metal salts, any suitable mixtures thereof, combinations thereof and / or any suitable derivatives thereof (e.g., esters, such as di(C 1-4 alkyl) esters, metal salts and / or anhydrides).

[0029] Similarly, there are many examples of diols that can be used in (optionally autoxidisable) polyester resin synthesis to provide monomers that provide hydroxyl components. Such diols can be of the type having only carbon atoms in their backbone. Suitable diols are, for example, 1,4-butanediol, 2,3-butanediol, 1,6-hexanediol, 2,2-dimethyl-1,3-propanediol (neopentyl glycol), 1,2-, 1,3- and 1,4-cyclohexanediol and the corresponding cyclohexanedimethanol, diethylene glycol (preferably less than 5, 4, 3, 2, 1, e.g. 0 mol % diethylene glycol), dipropylene glycol and diols such as alkoxylated bisphenol A products, e.g. ethoxylated or propoxylated bisphenol A. The most widely used type of polyester is polyethylene terephthalate, commonly abbreviated as PET, which is made from terephthalic acid and monoethylene glycol.

[0030] To introduce amide functionality into the polyester, amino-functional reactants such as 1,2-diaminoethane, 1,6-diaminohexane or 2-aminoethanol can be used.

[0031] Sulfopolyester is a kind of polyester containing sulfonate ions (SO3 - ) group, for example, synthesized using a sulfomonomer such as 5-sodiosulfoisophthalic acid (5-SSIPA or SIP) or dimethyl 5-sodiosulfoisophthalate as one of the diacids or dialkyl esters in the polyester composition.

[0032] A yarn loop is the length of time a yarn can bend away from its base (this doesn't exclude the possibility that the loop is longer than the base itself). For textile products, the base is the portion of the yarn that forms the upper, visible part of the product. For example, in a carpet, this is the portion of the yarn that forms the pile. In clothing, this is the portion of the yarn that forms the outer surface of the garment. A loop is the portion of the yarn that extends from the back surface of the product.

[0033] A sheet is a substantially two-dimensional substance or material, ie, wide and thin, usually (but not necessarily) rectangular, and inherently having two opposing surfaces.

[0034] A dispersion is a system containing particles dispersed in a liquid medium.

[0035] Stitching is a method of mechanically making a yarn part of an object by stitching or as if stitching, for example by tufting, knitting, sewing, weaving, etc.

[0036] The polyester material is its continuous phase, i.e. the basic constituent phase, consisting of at least 90% (w / w), preferably 91, 92, 93, 94, 95, 96, 97, 98, 99 up to 100% polyester. This does not exclude that the material contains, for example, up to 50% or even more fillers or other discontinuous materials.

[0037] A polyester product (article) is a product (article) the constituent polymeric material of which is made of at least 90% (w / w), preferably 91, 92, 93, 94, 95, 96, 97, 98, 99 up to 100% polyester.

[0038] Amorphous polymers are polymers having a crystallinity of less than 2% w / w (ie less than 2% by mass of the polymer is present as crystalline polymer, exhibiting a first order transition upon melting), preferably less than 1%, or even less than 0.5%.

[0039] Aqueous means freely miscible with water at room temperature. Preferably, it means that the liquid content is at least 90%, such as 91, 92, 93, 94, 95, 96, 97, 98, 99 or even 100%, of water. Even more preferably, aqueous excludes the presence of water-soluble organic compounds (also known as organic solvents), such as aliphatic and cycloaliphatic alcohols, ethers, esters and ketones.

[0040] To soften a polymer is to heat it so that it becomes at least tacky and ductile. A polymer can also become fluid if heated above its melting temperature.

[0041] Foam is a material formed by trapping pockets of gas in a liquid. Typically, the gas is contained in bubbles of varying sizes separated by regions of liquid that form a film (i.e., the material is polydisperse).

[0042] A layer is a thickness of material laid or spread over a surface. A layer may be non-uniform in thickness and may be discontinuous in the sense that it may have holes in it.

[0043] Hot melt adhesives are thermoplastic adhesives designed to be melted, i.e. heated, to transition from a solid to a liquid state to adhere materials after solidification. Hot melt adhesives are typically non-reactive, crystalline, and contain little or no solvent, so curing and drying are usually unnecessary to provide adequate adhesion.

[0044] The static contact angle (also known as the sessile drop contact angle) is the contact angle measured when a liquid droplet rests on a flat surface and the three-phase boundary between the droplet, the surface, and the surrounding air is not moving.

[0045] Recyclable products are products that can be recycled, i.e. processed so that they can be returned to a previous stage in the recycling process.

[0046] Further embodiments of the present invention

[0047] In a further embodiment of the method according to the present invention, the polyester particles are composed of a polyester material having an HLB value of 7.9 to 10.0. It was found that a higher bottom value of the HLB corresponds to an easier preparation method because the conditions required to produce the dispersion are less stringent. For HLB values ​​below 8.0, it appears that it is generally necessary to melt the polyester to produce a dispersion of the particles in the dispersion medium, even if the starting material is a fine powder, or a solvent (such as MEK) is used, while above 8.0 this is generally not necessary. In addition, the stability of the dispersion is improved, requiring less or no mixing to maintain dispersion in the production environment. It was found that a lower top value of the HLB is beneficial for improving durability, particularly in conventional indoor environments where temperature and humidity levels may be relatively high. The above effects are further enhanced when an HLB value of 8.0 to 9.3 is met.

[0048] In another embodiment, it has been found to be advantageous when the polyester particles are composed of a polyester material having a static contact angle with water greater than 75° (e.g., 75°, 76°, 77°, 78°, 79°, 80°, 81°, 82°, 83°, etc.), in particular greater than 80°, such as 81°, 82°, 83°, 84°, 85°, etc. Higher contact angles are particularly associated with better resistance of the tuft bond to degradation under the influence of moisture, temperature, and load. Although contact angles of 120° can be achieved with certain polymers, such as fluorine-rich olefins, the maximum practically achievable with polyesters will likely be around 85-90°.

[0049] In yet another embodiment, the polyester particles have a number average particle size of less than 1000 nm. In the art, particles larger than 1000 nm are preferred. This is because it is believed that a sufficient amount of adhesive needs to be applied with a limited amount of dispersion. This, in turn, requires preventing the product from being completely saturated with the dispersion, making the drying process more cumbersome. However, it has been found that below the 1000 nm limit, the preparation process can be further simplified because the dispersion is inherently more stable and therefore requires less mixing to maintain sufficient dispersion quality while still being able to apply a sufficient amount of polyester to induce sufficient bonding. Obviously, when the HLB values ​​of the present invention are met, less adhesive is required to achieve good and lasting tuft bonding in an all-polyester product. Preferably, the polyester particles have a number average particle size of 10 to 500 nm, more preferably 50 to 400 nm. In this way, a very stable dispersion can be easily provided while at the same time a sufficient amount of adhesive can be applied.

[0050] In another embodiment, the aqueous dispersion medium contains 90% to 100% water, such as 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98% or 99% (w / w). Water is environmentally friendly, found to be suitable when the HLB value of the present invention is achieved, and is easy to reuse.

[0051] In one embodiment, the dispersion is applied to the second surface of the first sheet as a foam. It has been found that for certain polyesters, the foam can even improve the process and the resulting product, although this may seem counterintuitive, realizing that the polyester adhesive needs to be applied topically between the coil and the backing as an adhesive.

[0052] Sulfopolyesters have been found to be particularly suitable for use as the polyester for the polyester particles in the dispersion. This is a well-known polyester, but it is not generally known to be used as an adhesive. However, surprisingly, such polyesters appear to be very suitable for use in the present process when the HLB values ​​of the present invention are achieved. Preferably, the sulfopolyester comprises 1 to 20 mol % of at least one dicarboxylic acid sulfomonomer (e.g., sodium sulfoisophthalic acid, abbreviated as SSIPA), for example, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, or 19 mol % of the dicarboxylic acid sulfomonomer.

[0053] In another embodiment, the polyester particles consist of amorphous polyester. (Semi)crystalline polyesters are preferred in the art because they melt and solidify easily at a predetermined temperature. However, these polyesters are generally more brittle and therefore require a larger amount to obtain a durable tuft bond. Amorphous polyesters are more natural (especially above their Tg), which is beneficial for the durability of the tuft bond, even when using less adhesive. Preferably, the amorphous polyester has a glass transition temperature above 20°C. Although the Tg can be below room temperature (which would seem to be a disadvantage given the fact that the polymer would be sticky at room temperature, since the adhesive is applied to the back surface of the backing and is therefore directed away from the pile, this has no negative impact during actual use), it is preferably above room temperature. This has been found to be advantageous during production, as the adhesive is non-sticky at processing temperatures. More preferably, the amorphous polyester has a glass transition temperature of 20°C to 50°C, for example, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48 and 49°C.

[0054] In one embodiment, the steps of removing the aqueous dispersion medium from the amount of aqueous dispersion and heating the polyester particles to a temperature above the temperature at which the polyester softens are performed simultaneously by heating the first sheet in an oven. For example, this can be an oven of the type commonly used to make latex carpets.

[0055] In yet another embodiment, the first amount of dispersion is applied so that the amount of polyester particles is from 50 to 250 g / m 2(e.g. 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, 200, 210, 220, 230, 240 g / m 2 ), preferably 80 to 150 g / m 2 It was found that even at such low levels of polymeric adhesive, high and durable tuft bonding can be achieved in the process of the present invention.

[0056] In another embodiment of the method according to the invention, a second sheet is adhered to the second surface of the first sheet. Such a second sheet is also referred to as a secondary backing.

[0057] In one embodiment, the second sheet is applied to the second surface of the first sheet after heating the polyester particles to a temperature above the softening temperature of the polyester and before subsequently cooling the polyester, or by reheating the polyester particles after said cooling.

[0058] Alternatively, after the polyester has cooled, a second amount of the dispersion is applied to a second surface of the first sheet, the aqueous dispersion medium is then removed from the second amount of aqueous dispersion, the polyester particles are heated to a temperature above the temperature at which the polyester of the particles softens, a second sheet is applied, and the polyester of the particles is subsequently cooled to a temperature below the temperature at which the polyester solidifies, thereby joining the second sheet.

[0059] As yet another option, after the polyester has cooled, a layer of hot melt adhesive is applied to the second surface of the first sheet and then the second sheet is applied, thereby joining the second sheets.

[0060] All the above further embodiments also relate to the textile product of the invention itself.The invention will now be described in further detail using the following non-limiting examples. Example

[0061] Example 1 is an example describing how to determine the HLB value of a polymer.

[0062] Example 2 describes how to determine the static contact angle.

[0063] Example 3 provides various tests used to determine the quality of textile products.

[0064] Example 4 provides various analytical methods.

[0065] Example 5 provides various examples of preparing polyester particle dispersions.

[0066] Example 6 describes an example of a method for applying an aqueous dispersion of polymer particles to produce a textile product.

[0067] Example 7 describes several carpet examples used in Examples 8-18.

[0068] Examples 8 to 18 serve to illustrate the preparation and analysis of various textile products prepared according to the present invention.

[0069] Example 1

[0070] The HLB value of any compound in the sense of the present invention can be determined by the method disclosed in the document "A quantitative kinetic theory of emulsion type I. Physical chemistry of the emulsifying agent" by JT Davies, published in Gas / Liquid and Liquid / Liquid Interfaces. Proceedings of 2nd International Congress Surface Activity, Butterworths, London 1957. This document provides the HLB group number that can be used to calculate the HLB value of polyesters. These and other HLB group numbers can be found in recent literature, for example in Chapter 11 of the Handbook of Applied Surface and Colloid Chemistry edited by Krister Holmberg, 2001 John Wiley & Sons, Ltd, James R. Kanicky et al., entitled Surface Chemistry in the Petroleum Industry, and in Calculation of hydrophile-lipophile balance for polyethoxylated surfactants by group contribution method, Xiao Wen Guo et al., Journal of Colloid and Interface Science 298 (2006) 441-450, although the latter provides a very low number (11) for the -SO3Na group, which is clearly wrong. For the present invention, this number is set to 37.4, that is, the value of -SO4Na (38.7) minus the value of -O- (1.3).

[0071] Thus, the HLB values ​​of several experimental polyesters A to N were calculated (see below). The results are shown in Table 1. The ratios between the monomers used and the origin of these monomers were different in each case. This leads to differences in the HLB values ​​and other properties even for the same polymer type. The reference material is pure PET with an HLB value of 7.5. This polymer cannot be used in the current preparation method because it cannot be dispersed in water without the use of fillers and emulsifiers. Other experimental polyesters that meet the HLB requirements of the present invention can be used in the present method without any fillers, emulsifiers, viscosity modifiers, etc.

[0072]

[0073]

[0074] Abbreviations in Table 1:

[0075] IPA = Isophthalic acid

[0076] TPA = terephthalic acid

[0077] SSIPA = 5-sodium sulfoisophthalic acid

[0078] DEG = diethylene glycol

[0079] TMP = trimethylolpropane

[0080] CHDM = cyclohexanedimethanol

[0081] 1,6HD = 1,6-hexanediol

[0082] NPG = Neopentyl Glycol

[0083] EG = ethylene glycol

[0084] MP-diol = 2-methyl-1,3-propanediol

[0085] TBT = Tetrabutyl Titanate

[0086] DBTO = Dibutyltin Oxide

[0087] MBTO = Monobutyltin oxide

[0088] AV = acid value

[0089] OHV = Hydroxyl Value

[0090] Mn = number average molecular weight

[0091] As an example only, the following details the Davies method for calculating the HLB value of resin K. The basic formula is given as:

[0092]

[0093] in:

[0094] m-number of hydrophilic groups in the molecule

[0095] H i - Value of the i-th hydrophilic group (see table)

[0096] n- the number of lipophilic groups in the molecule

[0097] The raw material amounts used in the synthesis (note: catalysts and additives are not included in the calculation): 17.6 g SSIPA, 49.7 g IPA (isophthalic acid), 23.1 g CHDM (cyclohexanedimethanol), 29.7 g DEG (diethylene glycol) (7.1 g of which will be removed during the synthesis process). The final resin composition: 17.6 g SSIPA, 49.7 g IPA, 23.1 g CHDM, 22.6 g DEG. The mole fractions of the raw materials are calculated based on 1 mol of resin (Table 2).

[0098] Table 2 Final resin composition of resin K

[0099]

[0100] The contribution of the lipophilic groups was calculated based on the mole fraction.

[0101] Lipophilic groups are: -CH-, -CH2-, CH3-, =CH-

[0102] According to the Davies method, the group number contribution value is -0.475. The number of lipophilic groups in SSIPA, IPA, DEG, and CHDM is 6, 6, 4, and 8, respectively. The total contribution value of lipophilic groups is 2.78 (Table 3).

[0103] Table 3 Contribution value of resin K lipophilic group

[0104]

[0105] The contribution of hydrophilic groups is based on mole fraction.

[0106] The hydrophilic groups are: ester bonds formed by condensation reaction, -SO3Na from SSIPA, ether bonds from DEG, and the end groups (-OH and -COOH) of the polyester resin. The group number contributions of these groups can be found in Table 4.

[0107] Table 4 Contribution value of the hydrophilic group of resin K

[0108]

[0109] The ester groups were calculated using the amounts of acid, 0.405 mol IPA, and 0.089 mol SSIPA (a total of 0.494 mol). Both starting materials have two reactive COOH groups. This gives a total of 0.988 mol COOH, and thus a maximum of 0.988 mol ester can be formed in the resin composition.

[0110] For the -SO3Na group of SSIPA, a value of 37.4 was assumed based on subtracting the ether group contribution (1.3) from the -SO4Na group contribution (38.4), resulting in a value of 37.4.

[0111] The end groups of the resin are calculated based on the acid number (from the carboxyl group), hydroxyl number and theoretical molecular weight. First, the number of ester bonds per chain length is determined. This is done by calculating the average molecular weight of the repeating unit - [acid-diol] -, assuming that two water molecules are formed during the reaction. The average acid molecular weight is 150 g / mol and the average diol molecular weight is 120 g / mol. This means that the molecular weight of the repeating unit is 270 g / mol.

[0112] Resin K has an acid value (AV) of 4.5 mg KOH / g and a hydroxyl value (OHV) of 15.6 mg KOH / g. Based on these functional groups, the theoretical molecular weight is 5582 g / mol (MW = (F x 56100) / (AV + OHV), where F is the resin functionality (F = 2 in the case of linear resins). This means that there are 5582 / 270 = about 20 repeating units in the polymer chain. Each repeating -acid-diol-unit leads to the formation of 2 ester bonds. Therefore, there are 40 ester bonds in total. Each linear chain has 2 end groups, so the ester bonds (40) are connected to the end groups ( 2) is 20:1. The number of ester bonds used in the composition is calculated to be 0.988 for the HLB. Therefore, the total number of end groups in the composition is 0.988 / 20 = 0.0494. Using an end group ratio AV / OHV of 4.5 / 15.6, this means that the -COOH contribution is (4.5 x 0.0494) / 20.1 = 0.0111, and the -OH contribution is (15.6 x 0.0494) / 20.1 = 0.0383

[0113] The final HLB value of resin K was calculated according to the formula given in the Davies method: HLB = 7 + 6.17 - 2.78 = 10.4.

[0114] Example 2

[0115] The static contact angle can be measured by a contact angle goniometer (KSV CAM200, available from MechSE, Illinois) using an optical subsystem that is used to capture the profile of a pure liquid on a solid substrate. The substrate needs to be smooth (flat), as is well known, and can be polished if necessary. The angle formed between the liquid-solid interface and the liquid-gas interface is the contact angle. A microscope optical system with backlighting can be used. The current generation of systems uses high-resolution cameras and software to capture and analyze the contact angle. The static contact angle is obtained at room temperature, where the angle is measured 30 seconds after the liquid (water) is applied to the surface. See also Volpe et al.: Contact Angle, Wettability and Adhesion, 4: 79-100 CD, 2006, "About the possibility of experimentally measuring an equilibrium contact angle and its theoretical and practical consequences".

[0116] Static contact angles have been measured for some of the polyesters described in Table 1. These values ​​are again provided here in Table 5 below.

[0117] Table 5 Static contact angles of various polyesters (after 30 seconds, RT)

[0118]

[0119]

[0120] Example 3

[0121] Tufting bonding strength

[0122] Tuft bond, also known as tuft bond strength, can be measured according to test method ASTM D1335-12, which is a standard test method for determining the tuft bond of pile yarn floor coverings. In this test, the test sample is mounted in a special fixture and fixed to the base of a tensile testing machine. A hook (for loop specimens) or a tuft clamp (for cut pile specimens) is used to remove the specimen from the sample. The force to pull the specimen away from the test sample is measured as the tuft bond. For the data in this patent application, a Lloyd Ametek LS 1 tensile tester was used with the following settings: tuft clamp, speed 300 mm / min, temperature 23°C, and humidity ~64%.

[0123] Tuft bonding after exposure to water

[0124] In order to establish the durability of tuft bond under high humidity conditions, a test was developed to measure the tuft bond of a textile product after it has been exposed to water. To this end, samples (circular, 100 cm2 in area) were immersed in water. In a first type of test, the sample was immersed in a container filled with cold water (600 ml) for 5 minutes (20°C), and in a second type of test, the sample was immersed in a container filled with warm water (600 ml) at 50°C for 5 minutes. The tuft bond strength is preferably determined before the immersion process, just after the immersion (within 5 minutes, so using a wet sample containing about 150-200% water) and after drying for four days at room temperature and atmospheric pressure. The tuft bond itself was measured according to ASTM D1335-12 as described above.

[0125] Anti-delamination

[0126] To determine the delamination resistance of the secondary backing, also known as "delamination strength," test method ASTM D3936-05, which is a standard test method for delamination resistance of secondary backings for pile yarn floor coverings, was used. In the test, the specimens were manually separated a distance of approximately 38 mm (exactly 1.5 inches). Each layer was then placed in opposing grips of a tensile tester, and the force required to continue separation the specified distance was recorded. The peak forces within the specified length interval were averaged and the delamination resistance was calculated. The equipment used was the same Lloyd Ametek LS1 tensile testing machine mentioned above, with the following settings: test type tear -180°, crosshead speed 300 mm / min, propagation speed 150 mm / min, sample width 50 mm, sample area 5600 mm2, temperature 23°C, and humidity ~64%.

[0127] Taber test

[0128] The Taber test is a method published by SAE International and is designated as a test method for determining the fiber loss resistance, abrasion resistance, and impact resistance of automotive carpet materials. The SAE International code for the test is SAE J1530. Common settings are: 2000 cycles, H18 wheels, climate chamber (temperature 23°C and 50% humidity). The carpet specimen is circular with a surface area of ​​100 cm. 2 .

[0129] Velcro testing

[0130] This test is typically used to identify defects in carpet systems with regard to filament binding (i.e., the bonding of small (individual) fibers within a yarn). This is a qualitative test that uses a device consisting of a weighted roller with a specific Velcro surface applied to its surface. After rolling over the sample a predetermined number of times, the degree of fuzz is visually assessed. This test is only suitable for loop pile carpets, as Velcro cannot grip cut pile filaments.

[0131] Foam volume of dispersion

[0132] 100 ml of the liquid dispersion were foamed and the volume increase was measured using a graduated cylinder.

[0133] Example 4

[0134] Glass transition temperature

[0135] The glass transition temperature (Tg) of a polymer can be measured using differential scanning calorimetry (DSC) according to ASTM E1356-08 (2014). This DSC method provides a rapid method for determining changes in specific heat capacity in a homogeneous material. The glass transition is characterized by a step change in specific heat capacity. This method is applicable to amorphous and semi-crystalline materials.

[0136] Tg was measured by DSC using a TA Instruments DSC Q1000 with a standard TA Instruments alumina cup of 50 μl. The nitrogen flow rate was 50 ml / min, and the sample was loaded at a temperature of 20 to 25°C. For amorphous polyesters, the sample was then cooled to -20°C and heated from -20°C to 60°C at a rate of 5°C / min. For semi-crystalline polyesters, the sample was cooled to -50°C and heated from -50°C to 200°C at a rate of 5°C / min, followed by an isothermal step at 200°C for 1 minute, followed by a cooling step from 200°C to -50°C at a rate of 5°C / min.

[0137] granularity

[0138] The particle size of the polyester particles in the dispersion can be determined using a Malvern Mastersizer 3000, which accurately determines particle size and its distribution in the range of 10 nm to 3500 μm. Particle size measurement is accomplished by angular diffraction of red (632.2 nm) and blue (470 nm) lasers using an array of 60 detectors. The sample is diluted in water to an obscuration of 1-7% and measured after equilibration at room temperature for 3 minutes with 25% ultrasonic power and 3000 rpm stirring. The result is the average of three measurements taken over 30 seconds. The particle size (spherical) can be calculated according to Mie (ISO 13320) and Fraunhofer theory. The results are automatically generated by the software provided by the instrument supplier.

[0139] Molecular weight

[0140] To determine the molecular weight and molecular weight distribution of the polymers, the method used to obtain data for the current polymer materials was gel permeation chromatography. The number molecular weight (Mn) of the polymers was determined using size exclusion chromatography (SEC) using a mixture of tetrahydrofuran / water / lithium bromide / acetic acid (1000 / 30 / 5 / 1) as the eluent. Molecular weight calculations were based on polystyrene standards.

[0141] Solid content of dispersion

[0142] The solids content of the dispersion can be measured by heating a sample of known mass at elevated temperature (160°C for the present polyester dispersion) using a halogen dryer (e.g. Halogen Moisture Analyzer HR73), dispersed on a glass fiber mat of known weight until constant weight is achieved, indicating that all solvent has been removed. The mass of the solids can then be easily determined.

[0143] Viscosity of dispersion

[0144] The viscosity of the dispersion can be measured using a Brookfield viscometer equipped with a small sample adapter and a spindle SC4-21. For the present dispersion, a water bath controlled at 23.0° C. and a cup characterized by Chamber 13R, diameter = 19.05 mm, depth = 64.77 mm were used. The procedure was as follows:

[0145] - Attach spindle S21 to the viscometer;

[0146] -Fill the cup with approximately 8 ml of dispersion;

[0147] - Place the cup in the Brookfield viscometer;

[0148] - Start the viscometer at a speed of 20 rpm and read the viscosity; this specific combination of spindle and speed should result in a viscosity measurement range of 23-230 mPa.s. When the viscosity is <23 mPa.s, change the speed to 50 rpm; when the viscosity is >230 mPa.s, change the speed to 10 rpm and read the viscosity (viscosity range 47-468 mPa.s). If it is still too high, adjust to 5 rpm (viscosity range 94-936 mPa.s). If it is still too high, adjust to 0.5 rpm (viscosity range 936-9360 mPa.s).

[0149] - Condition the dispersion at 23°C and wait until the viscosity reading stabilizes.

[0150] - Stop the rotation. Restart the motor and repeat the measurement again. The relative difference between the measurement results should not exceed 3%.

[0151] Example 5

[0152] In this example, a method is described for preparing dispersions of different polyester polymers ranging from relatively low HLB (8.0) to high HLB (10.4).

[0153] Polyester resin I (HLB 8.0)

[0154] synthesis

[0155] The polyester was prepared using a standard polyester synthesis as described below. Ingredients 5-(sodiosulfo)isophthalic acid (50 g), 2-methyl-1,3-propanediol (229 g), ethylene glycol (32 g), sodium acetate (0.13 gr), butylstannoic acid (0.50 g), and lithium hydroxide (0.13 g) were heated in a reactor at 200°C. Water produced during the reaction was removed until the acid value of the mixture was less than 1 mgKOH / g, and then the reactor was cooled to 160°C.

[0156] Decanediol (50 g; = sebacic acid), isophthalic acid (352 g) and recycled PET (407 g) were added to a reactor and the mixture was heated to 250° C. The water of reaction was removed until the acid value of the mixture was less than 25 mg KOH / g, and then the reactor was cooled to 240° C. The remaining water was removed under reduced pressure until the acid value was less than 5 mg KOH / g to obtain a polyester having the following characteristics: hydroxyl value = 16.9 mg KOH / g, acid value = 1.5 mg KOH / g; Tg = 38° C., contact angle = 85°

[0157] Dispersion of Resin I

[0158] Polyester resin (200 g) was dissolved in methyl ethyl ketone (MEK) (200 g) in a reactor at 60°C. Demineralized water (341 g) was added over 30 minutes while stirring. Sodium acetate (0.2 g) was added to the mixture. Vacuum was applied to remove the MEK. The pH was set to above 5.0 (preferably between 5.0 and 8.0) by adding sodium hydroxide.

[0159] The characteristics of the polyester dispersion are as follows: solids content = 39.5%, viscosity = 1700 mPa.s, pH = 5.4 and particle size = 71 nm, residual MEK is below the detection limit of 0.001%.

[0160] Polyester resin K (HLB 10.4)

[0161] synthesis

[0162] The polyester was prepared using a standard polyester synthesis as described below. The ingredients 5-(sodiosulfo)isophthalic acid (SSIPA) (176 g) and demineralized water (352 g) were heated in a 60° C. reactor to dissolve the SSIPA. Diethylene glycol (297 g), 1,4-cyclohexanedimethanol (231 g), lithium hydroxide (0.15 g), and butylstannoic acid (0.50 g) were added to the reactor and the mixture was heated to 220° C. Water was removed until the acid value of the mixture was less than 1 mg KOH / g, and the reactor was then cooled to 160° C.

[0163] Isophthalic acid (497 g) was added to the reactor and the mixture was heated to 240° C. The water formed during the reaction was removed until the acid value of the mixture was less than 25 mg KOH / g. The remaining water was removed under reduced pressure until the acid value was less than 5 mg KOH / g to obtain a polyester having the following characteristics: hydroxyl value = 15.6 mg KOH / g, acid value = 4.5 mg KOH / g; Tg = 36° C., contact angle = 76.0°

[0164] Dispersion of resin K

[0165] 422 g of demineralized water were heated to 70° C. in a reactor. 173 g of polyester resin (ground to a fine powder (<1 μm particles) using a grinder) was added to the reactor. The mixture was heated for 1 hour. If necessary, the pH could be increased by adding, for example, sodium hydroxide or sodium acetate.

[0166] The characteristics of the polyester dispersion are as follows: solid content = 29.4%, viscosity = 318 mPa.s, pH = 4.1 and particle size = 71 nm

[0167] Example 6

[0168] The polyester particle dispersion of the present invention can be used to prepare any type of textile product, particularly carpet-type products. The dispersion appears to be suitable for methods known in the art that are designed to apply a thermoplastic polymer coating to act as an adhesive to durably attach the yarn to a primary backing. Such methods are well known in the art. By way of example only, we refer to US2018 / 0119339 (Mashburn and Tambasco, filed November 1, 2016), which generally describes a method comprising applying an aqueous dispersion of thermoplastic polymer particles having an average particle size of less than 1,000 microns to the primary backing and back of the coils of a tufted carpet or tufted synthetic turf. The method further comprises heating the aqueous dispersion to a temperature sufficient to remove water therefrom, and heating the thermoplastic particles on the primary backing and back of the coils to a temperature equal to or greater than the melting temperature of the thermoplastic particles. The method further comprises cooling the heated thermoplastic polymer particles to a temperature below their melting temperature, thereby adhering the back of the coils to the primary backing.

[0169] This method is exemplified in detail in the detailed description of the disclosed embodiment of the '339 patent application, which begins in paragraph

[0019] with "Now referring to the drawings..." and ends in paragraph

[0045] on page 5 of the right-hand column with "...into the primary backing." This description refers to FIG. 1 of the '339 patent application, which is a schematic diagram of an apparatus for making carpet or synthetic turf using the described adhesive system based on an aqueous dispersion of thermoplastic polymer particles. The disclosed apparatus and method are equally suitable for applying the aqueous dispersion of the present invention.

[0170] Example 7

[0171] This example describes several carpet examples used in Examples 8 to 18. The examples are provided herein below, using the following technical terms:

[0172] "Gauge" is the distance between stitches, measured in inches. For example, "1 / 8" means 8 stitches per inch (8 stitches per 2.54 cm).

[0173] The "stitch rate" (or number of needles per 10 cm) defines the number of times a single needle inserts the tuft into the primary backing for a length of 10 cm.

[0174] "Pile weight" is the weight in grams per square meter of tufts and primary backing.

[0175] "Pile height" is the length of the tuft from the primary backing to the tip (expressed in centimeters).

[0176] Carpet A :Polyester cut pile carpet

[0177] Construction: Gauge 1 / 10″, Weave 45 / 10cm, Pile Weight 1730g / m 2 , pile height 1.0cm

[0178] Carpet B :Polyester cut pile carpet

[0179] Construction: Row spacing 1 / 10″, weave length 58 / 10cm, pile weight 2310g / m 2 , pile height 1.0cm

[0180] Carpet C : Polyester loop pile carpet

[0181] Construction: Row spacing 1 / 7″, weave length 42 / 10cm, pile weight 1060g / m 2 , pile height 1.0cm

[0182] Carpet D :Polyester composite cut pile / loop pile carpet

[0183] Construction: Row spacing 1 / 8″, weave length 40 / 10cm, pile weight 980g / m 2 , pile height 0.7cm

[0184] Carpet E :Polyester cut pile carpet

[0185] Construction: Row spacing 1 / 10″, weave gauge 40 / 10cm, pile weight 975g / m 2 , pile height 0.7cm

[0186] Carpet F :Polyester cut pile carpet

[0187] Construction: Row spacing 1 / 8″, weave length 70 / 10cm, pile weight 1460g / m 2 , pile height 0.8cm

[0188] All examples (where applicable, see below) used a 350 g / m 2 Gray polyester secondary backing (Material No. 707385).

[0189] Carpet samples were used in the following examples as shown below.

[0190] Carpet A was used in Example 10.

[0191] Carpet B was used in Example 11.

[0192] Carpet C was used in Examples 8, 9, 10, 12, 14, 15, and 16.

[0193] Carpet D was used in Examples 13 and 17

[0194] Carpet E was used in Example 18.

[0195] Carpet F was used in Example 15.

[0196] Example 8

[0197] Purpose

[0198] The purpose of this experiment was to test the application of polyester dispersions themselves. The tests were conducted at the TFI testing facility in Germany using a small-scale coating line to test (latex) samples for carpet manufacturers. The goal was to test several polyester dispersions on TFI equipment to gather knowledge about the foaming and application processes of current dispersions and the types of latex used in the market, and to compare the in-house application method using a paint roller with the TFI small-scale coating line.

[0199] Material

[0200] • Polyester tufted primary backing, loop pile (see Example 7).

[0201] • TFI mini coating line: All samples were pre-coated at the same line speed and height from the blade (or block) to meter the amount of foaming dispersion.

[0202] Kitchen mixer.

[0203] Ventilated oven.

[0204] Weight balance.

[0205] Foaming additive: BAYGARD FOAMER (0.25-1.0%).

[0206] Laminator: Lacom MBPL-600Pilot-Laminator.

[0207] Secondary backing: polyester material (supplier TWE), 350 g / m2 (see Example 7).

[0208] Polyester hot melt adhesive (DSM).

[0209] method

[0210] Pre-coating using a small coating line

[0211] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer. In some cases, it may be necessary to add a foaming additive (see below).

[0212] Apply the foaming dispersion to the back of the carpet by using a sliding blade. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0213] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0214] Cool the sample at room temperature and allow to cool to room temperature.

[0215] • Then measure the pre-coated tuft bonding force (N).

[0216] Lamination of pre-coated and untreated tufted primary backings

[0217] Laminator settings: speed 8 m / min, oil temperature 140°C, gap between rollers depending on the amount of hot melt adhesive required (range 0.3-0.5 mm).

[0218] The dosage of polyester hot melt adhesive is about 150g / m2.

[0219] • The laminate tuft bonding force (N) was then measured.

[0220] Polyester dispersion

[0221] Latex A: blend of carboxylated styrene-butadiene and polyester (ratio 75 / 25), solid content (SC) is ~42%

[0222] Latex B 37% solids (~8w% inorganic material and ~29w% organic material. The inorganic portion may be composed of BaSO4, TiO2, CaCO3 and Al2SiO5 used as fillers. The organic portion may be composed of a blend of carboxylated saturated polyester and bisphenol A based epoxy resin. Diethanolamine is used as a neutralizing agent.

[0223] Dispersion of resin A (HLB 7.6)

[0224] Dispersion of resin B (HLB 7.2)

[0225] Dispersion of resin C (HLB 8.2)

[0226] Dispersion of resin D (HLB 7.9)

[0227] Due to the high number of carboxyl groups, the dispersion of Resin B is stabilized with a volatile amine (dimethylethanolamine). During the production of the final carpet product, the amine evaporates (at least partially) as a so-called VOC, a volatile organic compound, which is disadvantageous. Resin B has a relatively high acid number, which reduces its long-term stability.

[0228] result

[0229] The results of the tuft bond forces obtained after application of the precoat only and after lamination are given in Table 6. The force required for delamination is also given. The reference material is a "pure tuft" primary backing (no precoat applied).

[0230] Table 6 Tufting bonding strength of various carpet samples before and after lamination (all in N)

[0231]

[0232] in conclusion

[0233] Latex A: requires foaming additives (otherwise no stable foam will be produced -> penetrate through carpet), apply two pre-coats for sufficient weight (no drying in between)

[0234] Latex B: Hard to foam, almost no volume increase, 1 pre-coat produced adequate layer thickness, fine powder on carpet after drying.

[0235] Dispersion of resin B: Foam-free without additives, 2 layers applied to achieve sufficient layer thickness.

[0236] Dispersion of Resin A: requires foaming additives, carpet pre-coat flow is difficult to spread evenly, difficult to remove moisture (long drying time), 1 pre-coat is sufficient.

[0237] Dispersion of Resin D: No stable foam without additive, 0.5% addition gave a static foam with poor stability, 2 pre-coats were applied.

[0238] Dispersion of Resin C: No foaming additives required, 2 pre-coats.

[0239] • In terms of tuft bond strength, the polyester precoat dispersion appears to be superior to both latex references.

[0240] ·The tuft bonding strength is greatly improved after lamination.

[0241] • Comparative results of application methods (paint roller vs. TFI).

[0242] Even a pre-coat weight of 62 g / m2 is sufficient to obtain good properties (dispersion of resin D).

[0243] Example 9

[0244] Purpose

[0245] The objectives of this experiment were to compare the tuft bond strength achievable with pre-coated carpet using different polyester samples (including a reference sample from the market) and to compare the methods of applying the pre-coat, i.e. spray vs. roller, liquid vs. foam.

[0246] Material

[0247] • Polyester tufted primary backing (35 x 35 cm), loop pile (see Example 7).

[0248] Kitchen mixer (3 liters), model AKM900SDM

[0249] Ventilated oven, Memmert UF1060

[0250] Paint roller (10cm), plant sprayer (500ml)

[0251] Weight balance

[0252] Polyester dispersion:

[0253] Latex A: blend of carboxylated styrene-butadiene and polyester (ratio 75 / 25)

[0254] Dispersion of resin A (HLB 7.6)

[0255] Dispersion of resin B (HLB 7.2): neutralized 70 or 100% with DMEA (dimethylethanolamine)

[0256] Dispersion of resin D (HLB 7.9)

[0257] method

[0258] Pre-coating with a paint roller

[0259] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer.

[0260] Apply the foamed dispersion to the back of the carpet by using a paint roller. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0261] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0262] Allow the sample to cool to room temperature.

[0263] Pre-coat with a plant sprayer

[0264] • The plant sprayer is filled with the dispersion itself.

[0265] • Spray the dispersion onto the back of the carpet. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0266] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0267] - The sample was cooled at room temperature and cooled to room temperature (further described as "to room temperature").

[0268] Pre-coated as a liquid

[0269] Apply the liquid dispersion to the back of the carpet by using a paint roller. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0270] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0271] • Cool the sample to room temperature.

[0272] result

[0273] The results obtained for tuft cohesion are given in Table 7.

[0274] Table 7

[0275]

[0276] in conclusion

[0277] Application method using a paint roller: liquid (Sample III) vs. foamed dispersion (Sample IV): There was no significant difference in tuft bond strength, but when the dispersion was applied as a liquid, it leaked through the carpet. This means that the foaming step is preferred.

[0278] No significant differences in tuft bond strength were observed between the two application methods: spraying and applying the foaming dispersion by roller. However, spraying is usually performed when the particles are relatively small to prevent possible clogging of the spray holes.

[0279] • The carpet sample pre-coated with semi-crystalline polyester (Sample VIII) showed a wide variation in layer thickness due to the difficulty in creating a fine mist with this dispersion.

[0280] Example 10

[0281] Purpose

[0282] The purpose of this example is to test the effect of pre-coat thickness (50 vs. 100 g / m2) and to test different types of paint rollers (fur roller vs. paint roller).

[0283] Material

[0284] • Two types of polyester tufted primary backing (dimensions 50 x 44 cm): loop pile and cut pile (see Example 7).

[0285] Kitchen mixer (3 liters), model AKM900SDM.

[0286] Ventilated oven, Memmert UF1060.

[0287] Paint roller (10 cm), fur roller (25 cm).

[0288] Weight balance.

[0289] Foaming additive: Empigen BB detergent (N,N-dimethyl-N-dodecylglycine betaine).

[0290] Laminator: Lacom MBPL-600Pilot-Laminator.

[0291] Secondary backing: polyester material (supplier TWE), 350 g / m2.

[0292] Polyester hot melt adhesive (DSM)

[0293] Dispersion of resin D (HLB 7.9)

[0294] Dispersion of resin E (HLB 7.7)

[0295] method

[0296] Pre-coating of polyester tufted primary backing

[0297] The dispersion was mixed for 3 minutes using a kitchen mixer to generate foam. The dispersion of Resin E required a foaming additive to generate a stable foam (0.3% for Samples A1 and A2 and 0.7% for Sample A4)

[0298] Apply the foaming dispersion to the back of the carpet using a paint roller, lacquer roller, or fur roller. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0299] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0300] • Cool the sample to room temperature.

[0301] • Then measure the pre-coated tuft bonding force (N).

[0302] Lamination of pre-coated and untreated tufted primary backings

[0303] Laminator settings: speed 8 m / min, oil temperature 140°C, gap between rollers depending on the amount of hot melt adhesive required (range 0.3-0.5 mm).

[0304] The amount of polyester hot melt adhesive used is about 250 g / m2.

[0305] The tuft bonding strength (N) after lamination was then measured.

[0306] result

[0307] The results are given in Table 8.

[0308] Table 8 Tuft bonding results before and after lamination

[0309]

[0310] in conclusion

[0311] Amorphous resins (Samples III and IV) gave better tuft bonding results compared to semi-crystalline resins (Samples I and II)

[0312] The "fur roller" achieved comparable results compared to a paint roller

[0313] Using only hot melt adhesive and no pre-coating provides low tuft bond strength (Sample V)

[0314] Thicker pre-coat layers gave higher tuft bond strength, but this difference was less pronounced for the pre-coat layers after lamination.

[0315] • In this series, additives are required to produce stable foams with the semi-crystalline polyester dispersion (resin E).

[0316] Example 11

[0317] Purpose

[0318] The objectives of this experiment were to evaluate the effect of the solids content (SC) of the dispersion on tuft bond strength, as well as the effect of the dispersion viscosity on foaming behavior and stability. Potential changes in tuft bond strength over time were also evaluated, both after application of the precoat alone and after lamination. Finally, tuft bond strength was tested after the precoated samples were stored at elevated temperature for 2 weeks.

[0319] Material

[0320] • Polyester tufted primary backing (dimensions 35 x 30 cm): cut pile (see Example 7).

[0321] Kitchen mixer (3 liters), model AKM900SDM.

[0322] Ventilated oven, Memmert UF1060.

[0323] Paint roller (10 cm).

[0324] Weight balance.

[0325] Foaming additive: Empigen BB detergent (N,N-dimethyl-N-dodecylglycine betaine).

[0326] Laminator: Lacom MBPL-600Pilot-Laminator.

[0327] Secondary backing: polyester material (supplier TWE), 350 g / m2.

[0328] Polyester hot melt adhesive (DSM).

[0329] Dispersion of resin D (HLB 7.9).

[0330] Dispersion of Resin E (HLB 7.7) with the solids content of the dispersion varied from 44.3% (viscosity of 139 mPa.s) to 34.1% (viscosity of 5 mPa.s) by adding additional water to the dispersion. Sample E-5 contained additional sodium acetate (total 0.25 wt%).

[0331] Dispersion of resin F (HLB 7.5): 80% neutralized with DMEA.

[0332] • Dispersion of Resin G (HLB 8.5).

[0333] method

[0334] Pre-coating of polyester tufted primary backing

[0335] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer.

[0336] • Apply the foaming dispersion to the back of the carpet by using a paint roller. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0337] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0338] • Cool the sample to room temperature.

[0339] Lamination of pre-tufted primary backing

[0340] Laminator settings: speed 4 m / min, oil temperature 140°C, gap between rollers depending on the amount of hot melt adhesive required (range 0.3-0.5 mm).

[0341] The amount of polyester hot melt adhesive used is about 400 g / m2.

[0342] result

[0343] The results are given in Tables 9 and 10 below.

[0344] Table 9 Viscosity and foaming behavior of various dispersions

[0345]

[0346] Table 10 Tuft bonding strength before and after lamination

[0347]

[0348] in conclusion

[0349] The foaming of semi-crystalline resin E depends on the viscosity:

[0350] ○139mPa.s: easy to foam, and the foam formed is stable

[0351] ○5mPa.s: Difficult to foam, unstable foam (needs foaming additives)

[0352] If the foam is not stable, it is more difficult to apply the dispersion evenly and prevent leakage through the carpet.

[0353] • The solid content (ie viscosity) of the dispersion has no effect on the tuft bond strength.

[0354] • Tuft bond strength measured 1.5 hours after application and drying of the precoat was comparable to tuft bond strength measured 24 hours later (data not shown).

[0355] • Tuft bond strength after lamination showed no change over time (measured 15 minutes and 1 day after lamination; data not shown).

[0356] The tuft bond strength of the carpet did not change after storage at 50°C for 2 weeks (data not provided).

[0357] • Tuft bond strength of the pre-coated carpet with a (relatively) low Tg resin (Resin G, Tg of about 11°C) showed comparable results in terms of tuft bond, but the pre-coated sample became tacky (without an applied backing).

[0358] • In addition to the same drawbacks as Resin B (see above), an HLB value of 7.5 (Resin F) resulted in tuft bond strengths that were (just) below acceptable levels.

[0359] Example 12

[0360] Purpose

[0361] The purpose of this example was to test the tuft bond strength of dispersions made from resins with relatively high Tg, ie Tg above RT (room temperature), as well as the appearance (particularly brittleness) of the carpet and to test the effect of the viscosity of the dispersion.

[0362] Material

[0363] • Polyester tufted primary backing (dimensions 35 x 35 cm): loop pile (see Example 7).

[0364] Kitchen mixer (3 liters), model AKM900SDM.

[0365] Ventilated oven, Memmert UF1060.

[0366] Paint roller (10 cm).

[0367] Weight balance.

[0368] Dispersion of Resin H (HLB 8.1) (Tg ~ 33°C): SC is adjusted by varying the amount of water in the dispersion:

[0369] Dispersion H-1: SC ~40% -> viscosity ~900 mPa.s

[0370] Dispersion H-2: SC ~38% -> Viscosity ~130 mPa.s

[0371] method

[0372] Pre-coating of polyester tufted primary backing

[0373] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer.

[0374] • Apply the foaming dispersion to the back of the carpet using a paint roller. Apply approximately 100 g / m2 of dry polyester pre-coat to the material.

[0375] The carpet was dried in a ventilated oven at 150°C for 8 minutes.

[0376] Results and Conclusions

[0377] Both dispersions appeared to foam readily, but dispersion H-1 had better foam volume and stability than dispersion H-2 (data not provided). The carpet precoated with the lower viscosity appeared to exhibit a greater spread in tuft bond strength, but the values ​​were slightly higher (material precoated with sample H-1: tuft bond 15 ± 3 N, material precoated with sample H-2: tuft bond 19 ± 6 N). Both carpet samples exhibited some creaking due to the brittleness of the polyester used in the dispersions.

[0378] Example 13

[0379] Purpose

[0380] The purpose of this example was to examine whether the invention could result in a polyester carpet passing a commonly used hook and loop test. Different amounts of pre-coat were applied, different foam volumes were used and different layers were applied.

[0381] Material

[0382] • Polyester tufted primary backing (dimensions 35 x 30 cm): combined loop and cut pile (see Example 7).

[0383] Kitchen mixer (3 liters), model AKM900SDM.

[0384] Ventilated oven, Memmert UF1060.

[0385] Paint roller (10 cm).

[0386] Weight balance.

[0387] Laminator: Lacom MBPL-600Pilot-Laminator

[0388] Secondary backing: polyester material (supplier TWE), 350 g / m2.

[0389] Polyester hot melt adhesive (DSM).

[0390] Dispersion of resin H (HLB 8.1)

[0391] method

[0392] Pre-coating of polyester tufted primary backing

[0393] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer.

[0394] • Apply the foaming dispersion to the back of the carpet by using a paint roller. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0395] The carpet was dried in a ventilated oven at 150°C for 5 minutes.

[0396] • Cool the sample to room temperature.

[0397] In some cases, additional pre-coat layers are applied by repeating the previous steps.

[0398] Lamination of pre-tufted primary backing

[0399] Laminator settings: speed 4 m / min, oil temperature 140°C, gap between rollers depending on the amount of hot melt adhesive required (range 0.3-0.5 mm).

[0400] The amount of polyester hot melt adhesive used is about 250 g / m2.

[0401] result

[0402] The results are shown in Table 11 below. For samples I, II and III, 200 g / m 2 Afterwards, the same effect as shown above, i.e. the layer thickness of the pre-coat affects the tuft bond strength, was observed, but the effect was less pronounced after lamination.

[0403] Afterwards, Sample IV was used to check the hook and loop test after each layer. After two layers, the material already passed the hook and loop test, and the third layer did not show any improvement (the hook and loop test was performed after each layer). Sample V showed comparable tuft bond strength to Sample IV, using an almost similar amount of precoat, but with two layers applied instead of three.

[0404] For Sample VI, a similar pre-coat weight (~150 g / m 2 ), more or less similar tuft bond strengths were found (also after lamination). This indicates that the number of layers as well as the foam volume have no influence on the tuft bond properties.

[0405] Sample II also passed the Velcro test, meaning 1 coat of pre-coating is sufficient.

[0406] Table 11 Tuft bonding strength of various test configurations (set-up) before and after lamination

[0407]

[0408] in conclusion

[0409] • No additional performance was observed when using multiple pre-coats, nor was more dispersion foam volume generated.

[0410] As low as 100g / m 2 The amount of pre-coat is enough to pass the Velcro test.

[0411] Example 14

[0412] Purpose

[0413] The purpose of this experiment was to investigate how different ways of applying the pre-coat relate to the tuft bond strength achieved. The impact of an additional drying step (if any) and the effect of a second pre-coat were also evaluated.

[0414] Material

[0415] • Polyester tufted primary backing (dimensions 35 x 30 cm) (see Example 7).

[0416] Kitchen mixer (3 liters), model AKM900SDM.

[0417] Ventilated oven, Memmert UF1060.

[0418] Paint roller (10 cm).

[0419] Weight balance.

[0420] Dispersion of Resin I (HLB 8.0).

[0421] method

[0422] Pre-coating of polyester tufted primary backing

[0423] The dispersion was mixed for 3 minutes to produce foam using a kitchen mixer.

[0424] • Apply the foaming dispersion to the back of the carpet using a paint roller. Apply approximately 100 g / m2 of dry polyester pre-coat to the material.

[0425] The carpet was dried in a ventilated oven at 150°C for 8 minutes

[0426] The sample is cooled at room temperature

[0427] In some cases, additional pre-coat is applied by repeating the previous steps

[0428] Changes in application methods

[0429] I. Pre-coating is done in two steps: first apply 50g / m2 -> dry > then apply 50g / m2 -> dry (total pre-coating is 100g / m2)

[0430] II. One-step 100g / m2 pre-coating; two drying steps

[0431] III. One-step 100g / m2 pre-coating; first dried in an oven, then dried with a hot air gun

[0432] IV. Reference system: one-step 100g / m2 pre-coating; standard drying step

[0433] V. No pre-coat applied: Tufted primary backing only

[0434] result

[0435] The lowest tuft bond strength was found for sample I (16 ± 6 N), with samples II, III, and IV having comparable tuft bond strengths (25 ± 8, 23 ± 5, and 24 ± 8 N, respectively). The tuft bond strength of the unprecoated sample (V) was 9 ± 2 N.

[0436] in conclusion

[0437] These results indicate that applying the precoat in one layer is more effective and that an additional drying step does not improve tuft bond strength / filament bonding.

[0438] Example 15

[0439] Purpose

[0440] The purpose of this test is to determine how a carpet coated with a water-based adhesive will perform in real life. The Taber test is performed to check (or at least determine) how the carpet will perform after extended use. The test focuses on how well the yarn holds up during use and whether the coating crumbles into powder. Because the polyester used as the precoat in this example has a Tg higher than RT, the material is inherently brittle and presents a risk of crumbling.

[0441] method

[0442] Pre-coating of polyester tufted primary backing

[0443] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer.

[0444] Apply the foaming dispersion to the back of the carpet by using a paint roller using a pre-coating machine. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0445] The carpet was dried in a ventilated oven at 150°C for 5 minutes.

[0446] • Cool the sample to room temperature.

[0447] Lamination of pre-coated tufted primary backing (or untreated tufted primary backing)

[0448] Laminator settings: speed 8 m / min, oil temperature 140°C, gap between rollers depending on the amount of hot melt adhesive required (range 0.2-0.5 mm).

[0449] The polyester hot melt adhesive usage for the loop pile tufted primary backing was approximately 200 g / m2, and the polyester hot melt adhesive usage for the cut pile tufted primary backing was approximately 170 g / m2.

[0450] Material

[0451] Loop-pile polyester tufted primary backing (see Example 7)

[0452] Cut pile polyester tufted primary backing. (See Example 7)

[0453] Polyester dispersion of resin H (HLB 8.1)

[0454] Latex A as a reference (no polyester pre-coat, only hot melt adhesive and secondary backing)

[0455] Results and Conclusions

[0456] The results regarding the tuft bond strengths obtained are provided in Table 12.

[0457] Table 12 Tuft bonding strength after various durability tests

[0458]

[0459] Based on the obtained results, the following conclusions can be drawn:

[0460] Loop pile polyester carpet: The reference had a weight loss of 8%. For the two pre-coated samples, this was 3% and 2% (128 and 182 g / m2), respectively.

[0461] • Cut pile polyester carpet: The reference sample had a weight loss of 5%, and the pre-coated samples had a roughly comparable weight loss (1.2-1.3%).

[0462] Tuft bond strength of samples before and after Taber testing was determined only on cut pile samples. Only a slight decrease in strength was observed.

[0463] After completing the Taber test, the samples were analyzed using a microscope. No signs of crushed pre-coating were observed.

[0464] Example 16

[0465] Purpose

[0466] The purpose of this series of tests was to investigate the effect of using the same amount of pre-coat adhesive and varying amounts of laminating adhesive on tuft bond strength and delamination. Carpet samples containing water-based pre-coat and laminating adhesives were evaluated for dimensional stability.

[0467] Material

[0468] • Polyester tufted primary backing (dimensions 20 x 30 cm) (see Example 7).

[0469] Kitchen mixer (3 liters), model AKM900SDM

[0470] Ventilated oven, Memmert UF1060

[0471] Paint roller (10 cm)

[0472] Weight balance

[0473] Water bath (20℃)

[0474] Laminator: Lacom MBPL-600 Pilot Laminator

[0475] Secondary backing: polyester material (supplier TWE), 350g / m2

[0476] Polyester hot melt adhesive (DSM)

[0477] Polyester dispersion of resin I (HLB 8.0)

[0478] method

[0479] Pre-coating of polyester tufted primary backing

[0480] • Create foam by mixing the dispersion for 3 minutes using a kitchen mixer.

[0481] • Apply the foaming dispersion to the back of the carpet by using a paint roller. Use the solids content of the dispersion to calculate the amount needed to pre-coat the carpet.

[0482] The carpet was dried in a ventilated oven at 150°C for 6 minutes.

[0483] • Cool the sample to room temperature.

[0484] Lamination of pre-tufted primary backing

[0485] Laminator settings: speed 8 m / min, oil temperature 140°C, gap between rollers depending on the amount of hot melt adhesive required (range 0.2-0.3 mm).

[0486] The amount of polyester hot melt adhesive used was about 128 g / m2 for sample 1 and about 146 g / m2 for sample 2. Both samples had the same pre-coat amount (75 g / m2) (see Table 13).

[0487] For the dimensional stability test, the polyester hot melt adhesive was applied at a dosage of 180 g / m2. The pre-coating amount was 50 or 100 g / m2 (see Table 14).

[0488] The assessment is conducted as follows:

[0489] For dimensional stability testing, samples were placed flat and stress-free in an oven and a water bath.

[0490] Step 1: Take the initial value of tuft bond strength

[0491] Step 2: Oven at 60°C for 2 hours;

[0492] Step 3: 2 hours in a water bath at 20°C

[0493] Step 4: 24 hours in an oven at 60°C

[0494] Step 5: 8 hours at 20°C (standard humidity)

[0495] Step 6: Determine Tuft Bond Strength and Visual Inspection

[0496] result

[0497] The results are shown in Tables 13 and 14 below.

[0498] Table 13 Delamination test

[0499]

[0500] Table 14 Dimensional stability test

[0501]

[0502] in conclusion

[0503] Using higher water-based pre-coat levels results in higher tuft bond strength

[0504] • Delamination resistance depends on the amount of hot melt adhesive.

[0505] Dimensional stability (visual inspection): No difference in appearance was observed

[0506] Example 17

[0507] Purpose

[0508] The purpose of this experiment was to evaluate the filament bonding of three different carpet samples using a performance cleaning test.

[0509] Material

[0510] • Polyester tufted primary backing (dimensions 50 x 30 cm): combined loop and cut pile (see Example 7).

[0511] Kitchen mixer (3 liters), model AKM900SDM.

[0512] Ventilated oven, Memmert UF1060.

[0513] Paint roller (10 cm).

[0514] Weight balance.

[0515] Laminator: Lacom MBPL-600 Pilot-Laminator.

[0516] Secondary backing: polyester material (supplier TWE), 350 g / m2.

[0517] Polyester hot melt adhesive (DSM180g / m 2 ).

[0518] Water-based pre-coat: dispersion of resin I. Two different pre-coat weights were tested, 50 and 100 g / m 2 .

[0519] QMC-007 Carpet Tester.

[0520] Evaluate:

[0521] The test method used was developed by James: "Quality Maintenance Control", abbreviated as QMC-007 (see EP2198263B1). Using this unique testing machine, the cleaning and maintenance performance of different materials (especially different types of carpets) can be evaluated.

[0522] The changes in the appearance of the carpet caused by the mechanical brushes were visually assessed using standard EN 1471. The assessment was made on a scale of 1 to 5, with 1 being strong and 5 being no difference compared to the untreated carpet.

[0523] Results and Conclusions

[0524] The counter-rotating brushes were able to pull out at least some of the filaments on all samples. 50 g / m 2 The quality shows the most filament drawn out, 100g / m 2 The quality shows almost nothing. After 30 rotation brush cycles, 50g / m 2 The appearance evaluation value of the sample is 3, and 100g / m 2 The appearance evaluation value of the sample is 4.5

[0525] After 60 rotation brush cycles, 50g / m 2 The appearance evaluation value of the sample is 2, and 100g / m 2 The appearance evaluation value of the sample was 4.

[0526] Example 18

[0527] Purpose

[0528] The purpose of this experiment was to test two types of experimental polyester adhesives representing the (almost) outermost range of adhesives for use in the present invention, namely:

[0529] Dispersion of resin K (HLB 10.4)

[0530] Dispersion of Resin I (HLB 8.0)

[0531] The samples were all all-polyester cut-pile carpet (see Example 7). The polyester adhesive was applied as a foaming dispersion at 100 g / m² (100 g polyester solids). After application of the foaming dispersion, the samples were dried in a ventilated oven at 150°C for 6 minutes. These samples were subjected to the water immersion test described in Example 3. The data are described in Table 15 below.

[0532] Table 15 Water sensitivity of tuft bonding

[0533]

[0534] Both products have acceptable water resistance at 20°. However, at an HLB value of 10.4, resistance to loss of tuft bond due to water exposure is low, especially when the sample is still wet. Therefore, when durability in the face of regular water treatment is the goal, a lower HLB value is preferred.

Claims

1. A method for preparing a polyester textile product, the method comprising: - providing a first polyester sheet, - stitching polyester yarn through the first sheet to form a pile on a first surface of the first sheet and to form yarn loops at an opposing second surface of the first sheet, the pile extending from the first surface, - applying a first amount of a dispersion comprising an aqueous dispersion medium and polyester particles dispersed in said medium to the second surface of said first sheet, - then removing said aqueous dispersion medium from said first amount of aqueous dispersion, - heating the polyester particles to a temperature above the temperature at which the polyester of the particles softens, - and subsequently cooling the polyester of the particles to a temperature below the temperature at which the polyester solidifies, thereby interconnecting the coils and the first sheet with the solidified polyester, The polyester particles are composed of polyester materials with a hydrophilic-lipophilic balance value of 7.6 to 10.

5.

2. The method according to claim 1, characterized in that The polyester particles are composed of a polyester material having a hydrophilic-lipophilic balance value of 7.9 to 10.

0.

3. The method according to claim 2, characterized in that The polyester particles are composed of a polyester material having a hydrophilic-lipophilic balance value of 8.0 to 9.

3.

4. The method according to any one of claims 1 to 2, characterized in that The polyester particles are composed of a polyester material having a static contact angle with water greater than 75°.

5. The method according to claim 4, characterized in that The polyester particles are composed of a polyester material having a static contact angle with water greater than 80°.

6. The method according to any one of claims 1 to 3, characterized in that The polyester particles have a number average particle size of less than 1000 nm.

7. The method according to any one of claims 1 to 3, characterized in that The polyester particles have a number average particle size of 10 to 500 nm.

8. The method according to any one of claims 1 to 3, characterized in that The polyester particles have a number average particle size of 50 to 400 nm.

9. The method according to any one of claims 1 to 3, characterized in that The aqueous dispersion medium contains 90% to 100% water.

10. The method according to any one of claims 1 to 3, characterized in that The dispersion is applied as a foam to the second surface of the first sheet.

11. The method according to any one of claims 1 to 3, characterized in that The polyester of the polyester particles in the dispersion is a sulfopolyester.

12. The method according to claim 11, characterized in that The sulfopolyester comprises 1 to 20 mol % of at least one dicarboxylic acid sulfomonomer.

13. The method according to any one of claims 1 to 3, characterized in that The polyester particles are composed of amorphous polyester.

14. The method according to claim 13, characterized in that The amorphous polyester has a glass transition temperature above 20°C.

15. The method according to claim 14, characterized in that The amorphous polyester has a glass transition temperature of 20°C to 50°C.

16. The method according to any one of claims 1 to 3, characterized in that The steps of removing the aqueous dispersion medium from the first amount of aqueous dispersion and heating the polyester particles to a temperature above the temperature at which the polyester softens are performed simultaneously by heating the first sheet in an oven.

17. The method according to any one of claims 1 to 3, characterized in that The first amount of dispersion is applied so that the amount of polyester particles is 50 to 250 g / m 2 .

18. The method according to any one of claims 1 to 3, characterized in that The first amount of dispersion is applied so that the amount of polyester particles is 80 to 150 g / m 2 .

19. The method according to any one of claims 1 to 3, characterized in that A second sheet is adhered to the second surface of the first sheet.

20. The method according to claim 19, characterized in that After heating the polyester particles to a temperature above the softening temperature of the polyester, and before subsequently cooling the polyester or by reheating the cooled polyester particles, the second sheet is applied to the second surface of the first sheet.

21. The method according to claim 19, wherein After cooling the polyester, a second amount of the dispersion is applied to a second surface of the first sheet, the aqueous dispersion medium is then removed from the second amount of the aqueous dispersion, the polyester particles of the second amount of the aqueous dispersion are heated to a temperature above the temperature at which the polyester of the particles softens, the second sheet is applied, and the polyester of the particles is subsequently cooled to a temperature below the temperature at which the polyester solidifies, thereby connecting the second sheet.

22. The method according to claim 19, wherein After cooling the polyester, a layer of hot melt adhesive is applied to the second surface of the first sheet and then the second sheet is applied, thereby joining the second sheets.

23. A polyester textile product comprising: - a first polyester sheet, - a polyester yarn stitched through the first sheet to form a pile on a first surface of the first sheet and to form yarn loops at an opposing second surface of the first sheet, the pile extending from the first surface, - A polyester adhesive provided at the second surface of the first sheet material to interconnect the coil and the first sheet material, wherein the polyester adhesive is composed of a polyester material having a hydrophilic-lipophilic balance value of 7.6 to 10.5.

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