Fluorine-free durable waterproof composition

Abstract

The present invention relates to a new treatment of fibrous substrates for obtaining durable waterproof effects. The methods described herein are demonstrated to be environmentally friendly and allow the use of renewable starting materials. Specifically, impregnation dispersions, concentrate dispersions, corresponding kits, each comprising candelilla wax and a blocked isocyanate selected from the group consisting of blocked isocyanates having a molecular weight of less than 2000 g / mol are disclosed. The present invention also provides novel methods for preparing concentrate dispersions, impregnating dispersions, and treating fabrics. Fabrics treated with the impregnation dispersion of the present invention exhibit unexpected beneficial properties when compared to known treatments. These beneficial characteristics include improved water resistance even after multiple wash cycles and for a wide variety of fabrics. The fabrics thus obtained can be used in a wide variety of applications, including outdoor garments and protective garments.

Description

[0001] Overview

[0002] The present invention relates to new treatments for fiber substrates for obtaining a durable water-repellent effect. The methods described herein are proven to be environmentally friendly and allow the use of renewable starting materials. In particular, impregnation dispersions, concentrate dispersions, and corresponding kits are disclosed. The present invention also provides new methods for preparing concentrate dispersions, impregnation dispersions, and treating fabrics. Fabrics treated with the impregnation dispersions of the present invention show unexpected beneficial properties when compared to known treatments. These beneficial properties include improved water repellency, even after multiple washing cycles and for a wide variety of fabrics. The fabrics thus obtained can be used in a wide variety of applications, including outdoor clothing, outdoor equipment, and protective clothing. Background Art

[0003] Applying a durable water repellent (DWR) treatment to fabrics is a process widely used in the textile industry to produce high-performance outdoor clothing, outdoor gear and protective clothing. Generally speaking, they can be divided into fluorocarbon (FC) DWR systems and non-fluorine DWR systems. The most widely used application processes are padding and coating processes.

[0004] Fluorocarbon (FC) DWR Systems: Until recently, fluorocarbon (FC) systems were commonly used due to their high effectiveness on a wide variety of fabrics. Such FC-DWR systems consist of an emulsion or dispersion of a FC-polymer in water and typically have an active solids content of about 30% w / w. FC systems are typically applied by a padding or coating process, as outlined in more detail below. However, it has been recognized that low molecular weight impurities associated with fluoropolymers have serious health effects. As a result, many major commercial brands have stopped using fluorocarbon-based products and the demand for alternatives has increased.

[0005] In the padding process, an open width fabric is saturated with a dilute solution of FC polymer and then passed through a mangle, which consists of two synthetic rubber rolls, where hydraulic pressure is applied to one of the rolls (usually the upper roll) so that excess liquid is squeezed out of the fabric. The squeeze pressure is usually adjusted so that the fabric retains 60 grams of liquid / 100 grams of fabric to 100 grams of liquid / 100 grams of fabric. This is called "pick-up" and is important in calculating the amount of product applied to the fabric or the "treatment level". The fabric is passed through a tenter frame, where it is held open width between parallel chains as it passes through a series of drying zones, so that water is removed and the surface of the individual yarns, filaments or fibers in the fabric becomes coated with a very thin film of hydrophobic fluorocarbon polymer.

[0006] An alternative method of applying fluorocarbon polymers to fabrics is to use a coating process in which a continuous film of fluorocarbon polymer is formed on the surface of the fabric. A thickener is added to the fluorocarbon polymer to increase its viscosity and form a paste. There are many different types of coating processes, but the blade coating system is the most commonly used, in which the paste is applied to one surface of the fabric in the form of a thin layer. The coated fabric is then passed through a tenter frame to dry the film on the fabric surface.

[0007] Additionally, crosslinking agents may be added to fluorocarbon polymers to improve the performance and durability of the system. Crosslinking agents are typically based on blocked isocyanate chemistry, where a multifunctional isocyanate reacts with a blocking agent to produce a product that is inert at room temperature but the isocyanate functionality can be reactivated by heat. This type of product is often referred to as an "extender." The temperature of a zone in the tenter may be increased to cause this activation and subsequent crosslinking reaction to occur within the polymer and between the polymer and the fiber surface.

[0008] Non-fluorinated DWR Systems: Currently, non-fluorinated DWR (NF-DWR) systems are being developed that can be applied to textiles. An important requirement for NF-DWR treatments is that they can be applied using exactly the same textile processing machinery and procedures as used to apply fluorine-based DWR systems. This would simplify the introduction of new technologies into the industry at minimal cost, and the present invention meets these requirements.

[0009] Traditionally, the water repellent effect is produced on textile products by melting wax onto the fabric using coating techniques or applying the wax from a water-based dispersion. However, unlike FC-DWR systems, conventional wax-based systems are very non-durable. Recently, in the development of NF-DWR systems, methods of improving the durability of wax-based systems have been investigated.

[0010] The wax dispersion used in these traditional DWR systems may be a synthetic wax such as paraffin, or a natural wax. In the development of NF-DWR systems, natural waxes will be preferred because they increase the content of biochar and thus improve the sustainability of the treatment. Beeswax and carnauba wax are examples of natural waxes, which are used in industrial applications for producing a waterproof effect on hard surfaces, such as floor and car polishes. Although it is well known that paraffin can be used to produce a waterproof effect on textiles, natural waxes are not commonly used because they give low performance levels and lack durability in the way they were previously applied. For example, Sworen et al. (WO2015 / 191326) discloses an aqueous dispersion for treating a fiber substrate, which comprises a wax and a polymer extender. Beeswax is recommended as a suitable wax. As a suitable extender, a fully reacted specific polyurethane polymer is disclosed. Although suitable, the results obtained and indicated in Table 4 of the document are considered to be insufficient for many applications. The document proposes a padding process using an aqueous dispersion. It should be noted at this point that the polyurethane extender mentioned by Sworen is completely different in chemical structure and behavior from the blocked isocyanate system according to the present invention. This isocyanate functionality cannot be restored by heating the polyurethane.

[0011] EP 3702522 discloses a resorcinol- and formaldehyde-free aqueous impregnating composition for coating textile reinforcement materials, comprising rubber latex, blocked isocyanate and at least one hydrocarbon wax.

[0012] Therefore, there is a need to provide improved DWR systems. In particular, such systems should target the performance of FC-DWR systems, but avoid the health and / or environmental impacts. Furthermore, it would be beneficial if such systems could be used with already available machinery to facilitate conversion to such new systems.

[0013] One or more of the above objects are achieved by the impregnation dispersion described in claim 1. Further aspects of the invention are disclosed in the description and the independent claims, and preferred embodiments are disclosed in the description and the dependent claims. The invention thus provides:

[0014] ● In a first aspect, an impregnation dispersion suitable for obtaining a durable water repellent effect on textile and fiber substrates;

[0015] ● In a second aspect, a concentrate dispersion and a kit for preparing the above impregnation dispersion;

[0016] ● In a third aspect, a textile product having durable water-repellent properties;

[0017] ●In a fourth aspect, a method for making an impregnation dispersion, a concentrate dispersion, and a kit;

[0018] ● In a fifth aspect, a method for making a textile product having a durable water repellent effect.

[0019] The present invention will be described in more detail below.It should be understood that multiple embodiments, preferred solutions and scopes as provided / disclosed in this specification can be combined arbitrarily.Specifically, "preferred" scopes can be combined, and "particularly preferred scopes can be combined".In addition, depending on the specific embodiment, the selected definition, embodiment or scope may not be applicable.As used herein, unless otherwise indicated herein or clearly contradictory to the context, the terms "one", "a kind of", "said" and similar terms used in the context of the present invention (especially in the context of the claims) should be understood to cover both the singular and the plural.The term "comprises / includes" should cover "comprises / includes", "essentially consisting of" and "consisting of". DETAILED DESCRIPTION

[0020] exist First aspect In the present invention, the present invention relates to impregnation dispersions comprising candelilla wax and blocked isocyanate, as further described below. These impregnation dispersions are suitable for obtaining a durable waterproofing effect on fiber substrates, they are proven to be environmentally friendly, compatible with existing equipment and safe for users. In the industry, such impregnation dispersions are also called "treatment liquids" because they can be directly applied to a suitable substrate. This aspect of the invention will be further described below.

[0021] Advantageously, the impregnation dispersion comprises a continuous phase and a dispersed phase, wherein the continuous phase is an aqueous system, and the dispersed phase comprises a wax and a blocked isocyanate, characterized in that the wax is a candelilla wax; and the blocked isocyanate is selected from blocked isocyanates having a molecular weight of less than 2000 g / mol. The amount of water in the impregnation dispersion can vary over a wide range, but is generally in the range of 886 mL / L to 993 mL / L. Such impregnation dispersions are used in industry, for example, for padding processes or coating processes. Such dispersions are generally described as "finishing baths" and may comprise additional components, such as those described below. It was unexpectedly found that if a candelilla wax dispersion is applied to a fabric in combination with a specific blocked isocyanate as disclosed herein, a high level of water repellency can be obtained using a candelilla wax dispersion. This result is unexpected because candelilla wax only produces a low level of repellency if applied without a blocked isocyanate, and a blocked isocyanate alone does not produce a repellent effect when a wax is not present. A true synergistic effect was observed. Even more surprising is that other natural waxes such as carnauba wax do not show these significant effects.

[0022] Candelilla wax: Candelilla wax is a known component identified by CAS 8006-44-8 and E 902. It includes natural products extracted from plants of the genus Euphorbia (e.g., Euphorbia antisyphilitica and Euphorbia bracteata) and their synthetic equivalents, known as, for example, Kahlwax 6605.

[0023] Crude candelilla wax is obtained by first boiling the dried stems of a suitable candelilla wax-containing plant in water acidified with sulfuric acid to release the wax. The molten wax is then skimmed off and allowed to solidify and refined by further treatment with sulfuric acid and subsequently through a filter press.

[0024] Candelilla wax is mainly composed of odd-numbered normal alkanes (C29 to C33) and esters of acids and alcohols with even-numbered carbon chains (C28 to C34). Free acids, free alcohols, sterols, neutral resins and minerals are also present. Therefore, suitable candelilla wax can have a purity as determined by one or more of the following parameters: melting range 68.5°C to 72.5°C, acid value 12 to 22 and saponification value 43 to 65.

[0025] Blocked isocyanates: Blocked isocyanates are well known in the art and are commercial items. In the present invention, suitable blocked isocyanates are based on isocyanate chemistry, where a polyfunctional isocyanate is reacted with a blocking agent as described below to produce a product that is inert at room temperature and has no isocyanate functionality. The functionality can be restored by heating the blocked isocyanate above its activation temperature, where the blocking effect is reversed and the isocyanate groups become available to react with suitable functional groups. During the fabric treatment process, the surface temperature of the fabric can be increased to cause this activation and subsequent crosslinking reactions to occur within the polymer within the fabric and between the polymer and the fiber surface. In the context of the present invention, suitable blocked isocyanates with a Mw of less than 2000 g / mol are used.

[0026] Capping agents for isocyanates are known per se and include organic compounds having at least one active hydrogen; they can be selected by the skilled person. Advantageously, the capping agent is selected from compounds such as alcohols, lactams, phenols, oximes and pyrazoles. The capping agent can also be selected from plant-based phenolic compounds to provide a system with an increased biocarbon content and a higher degree of sustainability. This type of capping agent includes cardanol (3-pentadeca-dienyl-phenol), which can be derived from cashew nut shell liquid.

[0027] Advantageously, the isocyanate is chosen from aliphatic isocyanates including hexamethylene diisocyanate, isophorone diisocyanate, trimethylhexamethylene diisocyanate, hydrogenated diphenylmethane diisocyanate.

[0028] Commercial examples of suitable blocked isocyanates include: Blocked isocyanate TTL (available from Beyond Surface Technologies AG), Baygard EDW and Baygard FBI (available from Tanatex). Blocked isocyanates are generally insoluble in water and are usually provided as a dispersion in water.

[0029] Additional components: As known in the art, additional functional components such as pH adjusters (e.g., acids or buffers), emulsifiers (e.g., nonionic emulsifiers), biocides, softeners, or wetting agents may be included. These components are commercial items and may be selected according to the specific application and included in amounts conventional in the art. In an advantageous embodiment, a wetting agent is included or used during the impregnation. In another advantageous embodiment, one or more emulsifiers and one or more wetting agents and one or more pH adjusters are included or used during the impregnation.

[0030] Concentration: The finishing bath contains the above components (wax+blocked isocyanate+optional additional components) in relatively low amounts (usually 5 wt% or less). The finishing bath is usually obtained by diluting the concentrate described below (second aspect) with a dilution factor of 3 to 60.

[0031] exist Second aspect In the present invention, the present invention relates to a concentrate dispersion comprising candelilla wax and a blocked isocyanate as further described herein, and a kit comprising candelilla wax and a blocked isocyanate as further described herein. These concentrate dispersions and kits are suitable for preparing the impregnation dispersions described herein and prove to be valuable commercial items that can be used in the textile industry. This aspect of the invention will be further described below.

[0032] In one embodiment, the present invention provides a concentrate dispersion comprising candelilla wax, blocked isocyanate and additional components (additives), all of which are as described in the first aspect of the present invention (forming a dispersed phase), and the remainder is water (forming a continuous phase) in an amount of 450 mL / L to 990 mL / L. Therefore, the difference between the concentrate as described herein and the impregnation dispersion is mainly in the water content. Although the concentrate has a low water content, making them more efficient for transportation and storage, the impregnation dispersion is suitable for use in the machines used in the textile industry. Typically, for efficiency reasons, the concentration is selected to be as high as possible, but stability and dispersibility are ensured at the same time.

[0033] In one embodiment, the concentration of candelilla wax in the concentrate dispersion is in the range of 1% (w / w) to 55% (w / w). In a preferred embodiment, the concentration of candelilla wax in the concentrate dispersion is in the range of 10% (w / w) to 40% (w / w). In an exemplary embodiment, the concentration of candelilla wax in the concentrate dispersion is 30%.

[0034] In one embodiment, the amount of water in the concentrate dispersion is in the range of 450 mL / L to 990 mL / L, preferably 600 mL / L to 900 mL / L. In an exemplary embodiment, the amount of water in the concentrate dispersion is 700 mL / L.

[0035] In another embodiment, the present invention provides a kit comprising a first container and a second container (a first cartridge and a second cartridge).

[0036] The first container comprises a first composition comprising candelilla wax as defined herein, water, optionally a pH adjuster as defined herein, a biocide, a wetting agent and an emulsifier. The concentration of candelilla wax in the first container is generally within the same range as described above.

[0037] The second container comprises a second composition comprising a blocked isocyanate as defined herein, preferably in the form of an aqueous dispersion.

[0038] Rather than providing a single concentrate, a kit containing two concentrates may be provided. Separating the wax from the blocked isocyanate may be beneficial in the textile industry as it increases shelf life and provides a higher degree of flexibility. Typically, the kit is combined with a suitable amount of water to obtain an impregnation dispersion.

[0039] In a preferred embodiment, the kit comprises a candelilla wax dispersion in a first container and a blocked aliphatic isocyanate using a petrochemical based blocked isocyanate in a second container. This embodiment is believed to provide the ultimate performance to the product.

[0040] In an alternative and preferred embodiment, the kit comprises candelilla wax in a first container and a blocked aliphatic isocyanate in which both the isocyanate and / or the blocking agent are bio-based in a second container. This embodiment is believed to provide a particularly environmentally friendly product.

[0041] In an alternative and preferred embodiment, the kit contains candelilla wax mixed with NF-DWR polymer in a first container and a blocked aliphatic isocyanate using a petrochemical based blocked isocyanate in a second container. This embodiment is believed to provide a product that optimally balances cost and performance.

[0042] In an alternative and preferred embodiment, the kit comprises a candelilla wax dispersion in a first container and a carefully selected blocked aliphatic isocyanate in a second container. This embodiment is believed to provide a product particularly suitable for treating natural fiber supports such as, but not exclusively, wool and cotton.

[0043] In an alternative and preferred embodiment, the kit comprises a candelilla wax dispersion in a first container and a carefully selected blocked aliphatic isocyanate in a second container. This embodiment is believed to provide a product particularly suitable for treating synthetic fiber supports such as polyesters and polyamides.

[0044] The invention also relates to the corresponding uses as outlined below:

[0045] In an embodiment, the present invention relates to the use of the dispersion and kit as defined herein for impregnating / treating a fibrous substrate, including a fabric or textile product as disclosed herein.

[0046] In an embodiment, the present invention relates to the use of a candelilla wax as described herein in combination with a blocked isocyanate as an impregnating material.

[0047] In an embodiment, the present invention relates to the use of a candelilla wax as described herein in combination with a blocked isocyanate and in combination with a wetting agent or an emulsifier or a pH adjusting agent, typically an acid, as an impregnating material.

[0048] In an embodiment, the present invention relates to the use of candelilla wax as described herein in combination with a blocked isocyanate and in combination with a wetting agent and an emulsifier and a pH adjuster, typically an acid, as an impregnating material.

[0049] In an embodiment, the present invention relates to the use of a kit as described herein for preparing an impregnation dispersion as described herein.

[0050] exist The third aspect In the present invention, the present invention relates to textile products having durable water-repellent properties. These valuable properties are obtained because the textile surface comprises candelilla wax and blocked isocyanate as described herein. This aspect of the invention will be further described below.

[0051] As already discussed, the impregnation dispersions disclosed herein (first aspect, treatment liquids) are suitable for use in the textile industry. A variety of fiber substrates can be treated. Such substrates include fibers, yarns, fabrics (woven, nonwoven and knitted) and finished products (e.g., garments, such as jeans, sportswear), collectively referred to as products of the textile industry or textile products.

[0052] Therefore, the present invention provides a textile product comprising a fiber carrier material and a coating, wherein the coating comprises a candelilla wax and a blocked isocyanate as defined in the first aspect of the present invention. Depending on the blocked isocyanate and the manufacture, a reaction product of the blocked isocyanate and the candelilla wax may also be present. The coating may be present as a layer on a fiber carrier. The amount of the candelilla wax on the textile product may vary over a wide range. Typically, 0.5 wt % to 8 wt % of the candelilla wax on the textile product produces suitable DWR properties. Preferably, 1 wt % to 5 wt % of the candelilla wax is present on the textile product, thereby obtaining a beneficial DWR property.

[0053] In an embodiment, the carrier material (base material) is selected from cellulose-based materials (eg cotton, viscose), wool, polyester and polyamide and yarns or fiber blends of these materials.

[0054] In an embodiment, the textile product is a finished product. Advantageously, such a textile product is selected from sportswear and outdoor clothing and outdoor equipment and protective clothing.

[0055] In an embodiment, the textile product is a fabric selected from the group consisting of a knitted fabric, a nonwoven fabric, and a woven fabric.

[0056] In an embodiment, the textile product is a staple yarn or filament. Such a product may be in the form of a skein or a bale or a continuous web.

[0057] exist The fourth aspect In the present invention, the present invention relates to a method for making the impregnation dispersion, concentrate dispersion and kit as described herein, in particular the first and second aspects of the invention. Such a method of making relies on process steps which are known per se but have not been applied to the specific starting materials and components described herein. This aspect of the invention will be described in further detail below.

[0058] In one embodiment, the present invention provides a method for making an impregnation dispersion as described herein, the method comprising: (i) combining a concentrate dispersion as described herein with water or an aqueous composition, or (ii) combining a first composition and a second composition of a kit as described herein with water or an aqueous composition. In essence, the impregnation dispersion is obtained by diluting a suitable starting material with water, which is conventional in the art. The order in which the components are added can be determined by a person skilled in the art. Typically, water is provided first, and the concentrate or the first and second compositions are added sequentially while stirring the entire mixture. The temperature can be controlled, but typically room temperature is sufficient.

[0059] In one embodiment, the present invention provides a method for making a concentrate dispersion as described herein, the method comprising,

[0060] (i) providing a first composition and a second composition as described herein; (ii) combining the first dispersion and the second dispersion, optionally by controlling the temperature at 3°C ​​to 70°C, thereby obtaining a liquid concentrate; and optionally (iii) diluting the concentrate thus obtained with water or an aqueous solution comprising an additive as described herein, thereby obtaining the concentrate dispersion.

[0061] In one embodiment, the present invention provides a method for making a candelilla wax dispersion as described herein ("first composition"). Candelilla wax is solid at room temperature, but as described below, the aqueous dispersion is formed by high shear mixing of candelilla wax in water heated to a temperature above the melting point of candelilla wax and containing an emulsifier to form a dispersion, and then rapidly cooling (quenching) the mixture. Those familiar with the art will appreciate that other techniques can be used to produce wax dispersions, which will produce the same results. Therefore, a method for obtaining the first composition comprises the steps of: (i) dissolving the emulsifier in water and heating the aqueous composition to 70°C to 90°C; (ii) adding candelilla wax, about 10% by weight; (iv) emulsifying the composition thus obtained, for example by applying high shear forces; (v) quenching the emulsion thus obtained, thereby obtaining the first composition as disclosed herein.

[0062] exist Fifth Aspect In the present invention, the present invention relates to a method for manufacturing a textile product having a durable water-repellent effect, in particular a textile product as described in the third aspect of the present invention. It is considered particularly advantageous that such a manufacturing method relies on process steps known per se and machines already used in the industry. However, such method steps have not been applied to the specific starting materials described herein, in particular the first and second aspects above. This aspect of the present invention will be further described below.

[0063] The impregnation dispersions can be applied at all levels of the textile industry, ie the substrate is selected from (i) yarns or fibers or filaments; (ii) knitted, woven or nonwoven fabrics; (iii) finished products.

[0064] In one embodiment, the present invention provides a method for making a fabric, the method comprising the steps of: (a) providing a knitted, woven or nonwoven fabric to be coated; then (b) coating or padding using the impregnation dispersion described in the first aspect of the invention; then (c) drying and curing; and optionally then (d) further finishing steps as conventional in the art, thereby obtaining a coated fabric. These method steps are known per se, but have not been applied in the context of an impregnation dispersion as described herein (i.e. comprising candelilla wax and a specific blocked isocyanate). Suitably, the manufacture is a continuous process.

[0065] Step (a): The material to be coated is a fibrous substrate in its broadest sense. In embodiments, such substrates include an initial coating. In alternative embodiments, such substrates are free of coatings. It is considered beneficial that the coating dispersions of the present invention can be applied to both coated and uncoated substrates. The term fibrous substrate includes filaments, fibers, yarns, nonwoven fabrics, and woven fabrics.

[0066] Step (b): The process steps in this step have been applied in the textile industry, such as coating and padding. In an exemplary arrangement, the dispersion concentrate as described in the second aspect contains 20% (weight / weight) candelilla wax. The concentrate is diluted to obtain an impregnation dispersion ("treatment liquid") containing 150 g / L of the concentrate. The treatment liquid is applied to the material of step (a) using a liquid pick-up rate of 70% (weight / weight).

[0067] Step (c): This step preferably includes pressing to remove excess dispersion from the substrate. In one exemplary arrangement, the amount of candelilla wax is such that 2.1% owf is obtained.

[0068] Step (d): This drying step is preferably carried out at an elevated temperature, for example at least 120°, for at least 30 seconds, to remove excess water from the substrate, thereby leaving a thin coating of the concentrate on the substrate.

[0069] In one embodiment, the present invention provides a method for manufacturing a textile product, preferably by a garment impregnation process, the process comprising (a) providing a textile product to be treated; then (b) impregnating, spraying or washing the product by using an impregnation dispersion of the first aspect of the invention as described herein; then (c) drying and curing; and optionally followed by (d) a further finishing step; thereby obtaining a treated textile product.

[0070] Step (a): The product to be treated is a textile product in its broadest sense, such as an article of clothing, for example a pair of jeans. The product to be treated includes a product to be finished or to be coated. The product applied to step (a) may already include an initial coating.

[0071] Step (b): This process step uses treatment steps that have been applied in the textile industry, such as impregnation or washing. In an exemplary arrangement, the dispersion concentrate as described in the second aspect contains 20% (weight / weight) candelilla wax. The concentrate is diluted to obtain an impregnation dispersion ("treatment liquid") containing 150 g / L of the concentrate. The treatment liquid is applied to the textile product of step (a) to obtain a liquid pick-up rate of 70% (weight / weight).

[0072] Step (c) is performed as described above. In one exemplary arrangement, the amount of candelilla wax is 2.1% owf for the textile product obtained.

[0073] To further illustrate the present invention, the following are provided: Example These examples are not intended to limit the scope of the invention. A simple procedure has been designed for producing aqueous dispersions of natural waxes in the laboratory and is described in detail below:

[0074] Laboratory preparation of concentrate dispersions:

[0075] Using a magnetic stirrer with a hot plate, 5 g / l SPAN 20 and 5 g / l TWEEN 20 were heated in a glass beaker to about 10°C above the melting point of the wax.

[0076] 100 g / l of wax was added and stirring was continued at about 250 rpm until the wax was completely melted.

[0077] The resulting composition was emulsified using an Ultraturrax (T25 disperser tool) at 11 000 rpm for 1 minute while continuing to heat.

[0078] As a quenching step, the emulsion thus obtained was poured into a pre-cooled glass bottle (refrigerator) and cooled in an ice bath or refrigerator.

[0079] After the above mentioned quenching step, the blocked isocyanate used (extender TTL) was added to the dispersion.The aqueous dispersion of the blocked isocyanate was slowly added to the wax dispersion using an Ultraturrax (T25 dispersing tool).

[0080] Preparation of impregnation dispersion:

[0081] The above concentrate is diluted with cold water to form a padding or treating solution.

[0082] Textile treatment

[0083] A wide range of fabrics were studied, some of which are summarized in the table below:

[0084] Fabric A Weaving 100% Cotton Fabric B Weaving 94% Polyamide; 6% Elastane Fabric C knitting 100% Cotton Fabric D knitting 100% PES

[0085] The treatment of fabrics described in the present invention was carried out using a Mathis laboratory padding mill (Model-Nr. HF1669) and a Mathis laboratory tenter (Model-Nr. DH 45888). Individual fabric samples measuring approximately 400 mm x 300 mm were prepared, saturated with the treatment solution before passing through the padding mill to remove excess impregnation dispersion and then dried in the tenter.

[0086] The sample was dried at 100°C (fabric surface temperature) for 1 minute and then cured at 160°C (fabric surface temperature) for 1 minute to activate the blocked isocyanate and produce crosslinking.

[0087] The samples were weighed dry before treatment and then after padding to enable calculation of wet pick-up and treatment level.

[0088] Performance Testing

[0089] The DWR performance of the treatments was measured using AATCC test method 22-2017e. The durability of the treatments was measured by washing the samples in a pre-loading washing machine Siemens IQ300 according to test method EN ISO 6330 (5A) where a 2 Kg load was washed using a 5A (40°C) wash cycle.

[0090] Example 1, the present invention (candelilla wax with TTL)

[0091]

[0092]

[0093]

[0094]

[0095]

[0096] The presence of the extender TTL significantly improves the properties, but does not provide any performance on its own (3.3 vs. 3.8 and 3.11). Candelilla wax dispersion itself does not provide any water resistance of market value. By combining the two products, a synergistic effect in terms of performance and durability has been identified.

[0097] Example 2, present invention (padding of candelilla wax plus bio-based blocked isocyanate, based on natural materials)

[0098]

[0099]

[0100]

[0101] The presence of the bio-based blocked isocyanate significantly improves the properties, but does not provide any performance on its own (3.1 / 3.2 vs. 3.8). When comparing Example 3.3 (invention) to 3.2 in Example 1, superior properties were found on cellulose / cotton.

[0102] Example 3, for comparison (padded carnauba wax plus bio-based blocked isocyanate)

[0103] Test serial number serial number 3.1 3.2 3.3 3.6 Product Name / Experiment EMUL 3297-3 (Candelilla 2) ％ 10 10 EMUL 3297-4 (Carnauba) ％ 10 10 Bio-based blocked isocyanates ％ 3 5 3 5 Acetic acid 10% g / l 10 10 10 10

[0104]

[0105]

[0106] Compare this to Example 2; Carnauba wax is inferior when compared to Candelilla (3.1 and 3.2 vs. 3.5 and 3.6)

[0107] Example 4 The present invention (impregnated candelilla wax / Invadine PBN plus bio-based blocked isocyanate)

[0108]

[0109]

[0110]

[0111] This example supplements Example 2. Invadine PBN is a wetting agent, commonly used in the industry to allow treatment liquids to penetrate into fabrics. Surprisingly, even with the inclusion of a wetting agent, the results remained the same.

[0112] Embodiment 5 (present invention)

[0113]

[0114]

[0115]

[0116]

[0117]

[0118] This example supplements Example 1, but by using synthetic candelilla wax instead of natural candelilla wax. The product Kahlwax 6702 (new) is a synthetic equivalent of candelilla. The results for synthetic candelilla were found to be significantly inferior.

Claims

1. An impregnation dispersion comprising a continuous phase and a dispersed phase, wherein the continuous phase is an aqueous system, and the dispersed phase comprises a wax and a blocked isocyanate, characterized in that ● The wax is candelilla wax; ● The blocked isocyanate is selected from blocked isocyanates having a molecular weight lower than 2000 g / mol; and ● The amount of wax+blocked isocyanate+optional further components is 5% by weight or less.

2. The impregnation dispersion according to claim 1, wherein the candelilla wax meets one or more of the following parameters: ● Melting point of 68.5°C to 72.5°C, ● Acid value of 12 to 22, ● Saponification value of 43 to 65.

3. The impregnation dispersion according to claim 1, wherein in the blocked isocyanate ● The blocking group is obtained by reacting an isocyanate having a molecular weight of less than 2000 g / mol with a reagent selected from the group consisting of alcohols, lactams, phenols, oximes and pyrazoles, preferably 3,5-dimethylpyrazole, ● The isocyanate is selected from aliphatic isocyanates.

4. The impregnation dispersion according to claim 1, comprising one or more of the following components ● a pH adjusting agent, preferably an acid or a buffer; and / or ● an emulsifier, preferably a nonionic emulsifier; and / or ● Biocides; and / or ● Wetting agents; and / or ● Softener.

5. A concentrate dispersion comprising ● Candelilla wax according to claim 1 or 2, and ● The blocked isocyanate according to claim 1 or 3, and optionally ● One or more additives selected from the group consisting of pH adjusters, emulsifiers, biocides, emollients and wetting agents; and ● The remainder is water in an amount of 60 to 90% by weight.

6. A kit comprising a first container and a second container ● The first container comprises a first composition comprising a wax as defined in claim 1 or 2, water, optionally a pH adjusting agent as defined in claim 4, and optionally an emulsifier as defined in claim 4; and ● The second container comprises a second composition comprising a blocked isocyanate as defined in claim 1 or 3, preferably in the form of an aqueous dispersion.

7. The kit according to claim 6, wherein ● The first container contains a candelilla wax dispersion, and the second container contains a blocked aliphatic isocyanate selected from petrochemical based blocked isocyanates; or ● The first container contains candelilla wax and the second container contains a blocked aliphatic isocyanate wherein the isocyanate and / or the blocking agent is bio-based, or ● The first container comprises candelilla wax in combination with a non-fluorinated durable water repellent (NF-DWR) polymer, and the second container comprises a blocked aliphatic isocyanate selected from petrochemical based blocked isocyanates; or ● The first container contains a candelilla wax dispersion and the second container contains a blocked aliphatic isocyanate that is compatible with a natural fiber carrier; or ● The first container contains a candelilla wax dispersion and the second container contains a blocked aliphatic isocyanate that is compatible with a synthetic fiber support.

8. A method for producing a concentrate dispersion according to claim 5, comprising the following steps x. Providing a first composition as defined in claim 6 and a second composition as defined in claim 6; y. combining the first dispersion and the second dispersion, optionally by maintaining the temperature at 3°C ​​to 70°C, preferably 20°C to 40°C, to obtain a liquid concentrate; and optionally z. diluting the concentrate thus obtained with water or an aqueous solution containing an additive as defined in claim 4; The concentrate dispersion is thereby obtained.

9. A method for producing an impregnation dispersion according to any one of claims 1 to 4, comprising ● combining the concentrate dispersion of claim 5 with water or an aqueous composition; or ● The first composition and the second composition of the kit of claim 6 are combined with water or an aqueous composition.

10. A textile product, including finished products, fabrics, yarns and fibers, comprising a base material and a coating, characterized in that The coating comprises a wax according to claim 1 or 2 and a blocked isocyanate according to claim 1 or 3 and optionally a reaction product thereof; preferably, wherein the amount of the wax is in the range of 0.5 wt % to 8 wt %.

11. The product according to claim 10, wherein the base material is selected from cellulose-based materials, wool, polyester and polyamide and blends thereof.

12. The textile product according to claim 10 or 11, wherein the textile product is ● Finished product, preferably selected from sportswear and outdoor equipment and outdoor clothing, or ● Fabric, the fabric is selected from nonwoven fabrics and woven fabrics and knitted fabrics, or ● Yarn, said yarn is selected from natural or synthetic fibers or synthetic filaments.

13. A method for manufacturing a fabric, comprising the following steps a. providing a knitted or woven fabric to be coated; then b. coating or padding the fabric with a dispersion according to any one of claims 1 to 4; subsequently c. drying and curing; and optionally subsequently d. Further finishing steps A coated fabric is thereby obtained.

14. The method according to claim 13, wherein ● The fabric of step (a) may or may not include an initial coating; and / or ● Step (c) is carried out at an elevated temperature, preferably at least 120°, for at least 30 seconds; and / or ● Step (b) comprises extrusion.

15. A method for manufacturing a textile product, preferably by a garment dipping process, comprising a. Provide textile products to be processed; Afterwards b. impregnating or washing the product by using a dispersion according to claim 1; Afterwards c. drying and curing; and optionally subsequently d. Further finishing steps Thereby a treated textile product is obtained.

16. Use of a dispersion or a kit according to any one of claims 1 to 4 for impregnating / treating fabrics or textile products.

17. Use of candelilla wax in combination with one or more blocked isocyanates having a molecular weight of less than 2000 g / mol and optionally with one or more wetting agents as impregnating material.

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