Tile adhesive with improved flexibility

Abstract

In a mortar for tile bonding, flexibility may be improved by incorporating 3 to 15 wt% of recycled composite fibers having an average diameter of no more than 50 microns and an average length of no more than 800 microns into the mortar. In some cases, the dry components may be premixed into a dry blend and then blended in water to make the mortar.

Description

Technical Field

[0001] The present invention relates to the field of cement-based tile adhesives. Background Art

[0002] A tiled surface generally comprises: (a) a substrate, such as a wall or floor, (b) tiles, and (c) an adhesive that bonds the tiles to the substrate.

[0003] In many cases, the adhesive is a cement-based tile adhesive, which is often referred to as mortar. Mortar for tiling typically contains the following dry components mixed with water: (a) a hydraulic binder (also called "cement"), such as Portland cement; (b) an inorganic filler, such as sand; and (c) a water-dispersible organic binder. Some mortars contain additional components, such as cellulose ethers, starch ethers, inorganic rheology modifiers, inorganic or organic fibers, air entraining agents, accelerators, retarders, high-range water reducers, and defoamers.

[0004] Fillers used in mortar have different particle sizes depending on the intended use. See, for example, "Dry Mortar", Ullmann's Encyclopedia of Industrial Chemistry (7th Edition), page 557. Fillers used in tile mortars typically have a maximum particle size of 0.5 mm to 1 mm, while bricklaying mortars may have slightly larger particles, and facing plasters may have smaller particles. In contrast, structural concrete typically contains larger particle sizes, such as 5 mm to 10 mm.

[0005] Mortars are governed by national and international performance standards, such as China's industrial standard JC / T 547-2017, Europe's standard EN 12004 and ISO 13007 worldwide. For some applications, flexible mortars are required. Flexible mortars give the tiled surface greater durability and less brittleness under stress or temperature cycles. These standards require that the "deformable adhesive" must be able to deform laterally by at least 2.5 mm under test conditions. See, for example, European standard EN 12004.

[0006] It would be desirable to find additives that could improve the flexibility of the mortar while maintaining other desirable properties such as adequate tensile adhesion. Summary of the invention

[0007] It has been found that appropriate amounts of recycled composite fibers added to the mortar can improve the flexibility of the mortar while maintaining sufficient tensile adhesion. This result is unexpected because components in recycled composite materials such as fibers and matrix resins are usually selected to have high stiffness and low flexibility.

[0008] One aspect of the present invention is a dry mix composition comprising:

[0009] a) Cement;

[0010] b) an inorganic filler, wherein 95% to 100% by weight of the filler particles will pass through a 2.36 mm sieve;

[0011] c) an organic binder suitable for use in tile mortar;

[0012] d) 3 to 15 weight percent recycled composite fibers having an average diameter of no greater than 50 microns and an average length of no greater than 800 microns, wherein all weight percents are based on the weight of dry components (a)-(d).

[0013] A second aspect of the present invention is a mortar comprising:

[0014] a) Cement;

[0015] b) an inorganic filler, wherein 95% to 100% by weight of the filler particles will pass through a 2.36 mm sieve;

[0016] c) an organic binder suitable for use in tile mortar;

[0017] d) 3 to 15 wt. % recycled composite fibers having an average diameter of no more than 50 microns and an average length of no more than 800 microns; and

[0018] e) water, wherein all weight percentages are based on the weight of dry components (a) to (d) excluding water.

[0019] The third aspect of the present invention is a method for attaching a tile to a substrate using the mortar of the second aspect, the method comprising the steps of:

[0020] a) applying the mortar to the substrate;

[0021] b) applying the plurality of tiles to the mortar on the substrate; and

[0022] c) Allow the mortar to set.

[0023] A fourth aspect of the present invention is a tiled surface comprising:

[0024] 1. Base material;

[0025] 2. Multiple tiles; and

[0026] 3. A set mortar for bonding the tiles to a substrate, wherein the mortar comprises: (a) cement, (b) an inorganic filler, (c) an organic binder suitable for use in tile mortars; and (d) 3% to 15% by weight of recycled composite fibers having an average diameter of no more than 50 microns and an average length of no more than 800 microns,

[0027] All weight percentages are based on the weight of components (a)-(d).

[0028] The present invention provides a useful outlet for short fibers recycled from composite materials. There is a need to economically recycle end-of-life composite parts such as wind turbine blades and automotive, marine and aircraft components. Short milled fibers are easy to manufacture but are generally of low value because they replace inexpensive fillers. The present invention allows the less expensive short milled fibers to add value beyond that of simple fillers. DETAILED DESCRIPTION

[0029] The mortar and dry mix of the present invention contain (a) cement; (b) inorganic filler; (c) organic binder suitable for tile mortar; (d) 3 wt% to 15 wt% of recycled composite fibers, which have an average diameter of no more than 50 microns and an average length of no more than 800 microns, wherein all weight percentages are based on the weight of components (a)-(d). The mortar also contains (e) water.

[0030] In some embodiments, the mortar is prepared by first preparing a dry mix and then mixing water into the dry mix. In some embodiments, the mortar is prepared by first mixing one or more components of the mortar with water and then mixing the remaining components of the mortar, either alone or together, into the aqueous mixture. Both embodiments may prepare the same mortar, but the first embodiment prepares and uses a dry mix of the present invention and the second embodiment does not. The selection and relative proportions of the components, except water, are the same in the mortar and the dry mix.

[0031] The dry mix / mortar contains cement. ASTM recognizes five types of cement: Type 1 (ordinary Portland cement); Type 2 (medium sulfate-resistant cement); Type 3 (rapid hardening cement), Type 4 (low heat cement), and Type 5 (high sulfate-resistant cement). Any of these cements can be used in the dry mix / mortar. In some embodiments, the cement is ordinary Portland cement. In some embodiments, the cement is a variant of ordinary Portland cement, known as white cement. In some embodiments, the cement is a more specialized cement, such as high alumina cement or calcium sulfoaluminate cement. Suitable cements are commercially available.

[0032] The dry mix / mortar should contain enough cement to be effective as a tile adhesive. In some embodiments, the dry mix / mortar contains at least 15 wt % or at least 20 wt % or at least 22 wt % or at least 25 wt % or at least 30 wt % or at least 35 wt % cement, based on dry components and excluding water. In some embodiments, the dry mix / mortar contains at most 60 wt % or at most 55 wt % or at most 50 wt % or at most 45 wt % cement, based on dry components and excluding water.

[0033] The dry mix / mortar contains an inorganic filler, wherein 95% to 100% by weight of the filler will pass through a 2.36 mm (8 mesh) sieve. Examples of inorganic fillers include silica sand, quartz sand, kaolin, calcium carbonate, magnesium carbonate, talc, or mixtures thereof. Suitable inorganic fillers are commercially available.

[0034] In some embodiments, 95% to 100% of the inorganic filler has a particle size of no more than 1.5 mm or 1.2 mm or 1.0 mm or 0.8 mm or 0.7 mm or 0.6 mm. In some embodiments, the inorganic filler contains at least 5% particles of at least 0.1 mm or at least 0.2 mm or at least 0.3 mm in size.

[0035] In some embodiments, the dry mix / mortar contains at least 20 wt % or at least 24 wt % or at least 30 wt % or at least 40 wt % or at least 45 wt % or at least 50 wt % of inorganic filler, based on dry components and excluding water. In some embodiments, the dry mix / mortar contains at most 80 wt % or at most 70 wt % or at most 65 wt % or at most 60 wt % or at most 55 wt % of inorganic filler, based on dry components and excluding water.

[0036] The dry mix / mortar contains an organic binder suitable for use in tile mortar. In some embodiments, the organic binder is water dispersible. In some embodiments, the organic binder is a dry powder before the components are mixed with water, referred to as a "redispersible powder". The redispersible powder contains an organic polymer and optionally a surfactant, which can form a stable polymer emulsion when mixed with water. In some embodiments, the redispersible powder is prepared by: (1) forming a polymer emulsion containing an organic polymer and a surfactant (if any), and (2) drying the emulsion to form a powder, such as by spray drying. In this case, the redispersible powder can contain both the organic polymer and the surfactant present in the emulsion. In some embodiments, the redispersible powder can sometimes also contain additives, such as anti-caking agents. Calcium carbonate and kaolin are examples of commonly used anti-caking agents.

[0037] In some embodiments, the organic binder comprises an acrylic copolymer, a vinyl ester copolymer, or a styrene-butadiene (SB) copolymer.

[0038] In some embodiments, the organic binder comprises a vinyl ester copolymer. Examples of suitable vinyl ester copolymers are described in U.S. Pat. No. 6,890,975. In some embodiments, the vinyl ester copolymer is a vinyl acetate-ethylene (VAE) copolymer. In some embodiments, the vinyl ester copolymer is a vinyl ester of versatate (VEOVA) copolymer.

[0039] Vinyl ester copolymers include repeating units derived from one or more vinyl ester monomers, such as vinyl acetate, vinyl n-butyrate, vinyl isobutyrate, vinyl 2-ethylhexanoate, vinyl laurate, 1-methylvinyl acetate, vinyl pivalate, and vinyl esters of C-branched monocarboxylic acids having 9 to 11 carbon atoms, such as vinyl neodecanoate. In some embodiments, the vinyl ester copolymers include vinyl acetate. In some embodiments, the vinyl ester copolymers include both vinyl acetate and vinyl esters of C-branched monocarboxylic acids having 9 to 11 carbon atoms; examples of such polymers are commercially available under the trade name VeoVa.

[0040] In some embodiments, the vinyl ester copolymer further comprises repeating units derived from ethylene or vinyl chloride. For example, the vinyl ester-ethylene copolymer may comprise at least 1 wt % or at least 5 wt % or at least 10 wt % repeating units derived from ethylene, and the vinyl ester-ethylene copolymer may comprise up to 60 wt % or up to 50 wt % repeating units derived from ethylene.

[0041] In some embodiments, the vinyl ester copolymer further comprises repeating units derived from acrylic acid or methacrylic acid esters (such as n-butyl acrylate or 2-ethylhexyl acrylate). For example, the vinyl ester-acrylate copolymer may comprise 30% to 90% by weight of repeating units derived from vinyl esters, 1% to 60% by weight of repeating units derived from acrylates, and 1% to 40% by weight of repeating units derived from ethylene. In some embodiments, the vinyl ester copolymer comprises an acrylate or methacrylate in an amount that cannot be measured.

[0042] The vinyl ester copolymer may also include a small amount of repeating units derived from ethylenically unsaturated monocarboxylic acids or dicarboxylic acids or their anhydrides, ethylenically unsaturated carboxamides or formonitriles, ethylenically unsaturated sulfonic acids and their salts, and vinyl silanes. Examples of common comonomers in this group include ethylene, acrylic acid, methacrylic acid, acrylamide, acrylonitrile, vinyl trimethoxysilane, vinyl triethoxysilane, vinyl tripropoxysilane, vinyl triisopropoxysilane, and sodium vinyl sulfonate. In some embodiments, the vinyl ester copolymer includes 0 wt % to 2 wt % or 0 wt % to 1 wt % or 0.5 wt % to 1 wt % of repeating units derived from such comonomers.

[0043] In some embodiments, the organic binder comprises an acrylic copolymer.Examples of acrylic polymers include styrene acrylic copolymers such as styrene acrylonitrile copolymers.

[0044] In some embodiments, the organic binder has a weight average molecular weight (Mw) of at least 300,000 Da or at least 350,000 Da or at least 400,000 Da.In some embodiments, the water dispersible organic binder has a weight average molecular weight (Mw) of at most 2,000,000 Da or at most 1,500,000 Da or at most 1,200,000 Da.

[0045] In some embodiments, the organic binder has a glass transition temperature of at least -30°C, or at least -20°C, or at least -10°C, or at least 5°C, or at least 15°C. In some embodiments, the water-dispersible organic binder has a glass transition temperature of at most 40°C, or at most 30°C, or at most 25°C.

[0046] In many embodiments, the organic binder further comprises a surfactant. In some embodiments, the surfactant is an anionic surfactant. Examples of nonionic surfactants include nonylphenol ethoxylates and fats (C6 to C 30 ) Alcohol ethoxylates, such as TERGITOL TM 15-S-40 and TERGITOL TM NP10, which are commercially available from The Dow Chemical Company.

[0047] In some embodiments, the surfactant is polyvinyl alcohol (PVOH). PVOH is polyvinyl acetate, wherein the acetate group has been hydrolyzed into an alcohol group. In some embodiments, PVOH is at least 70% hydrolyzed or at least 80% hydrolyzed or at least 85% hydrolyzed or at least 87% hydrolyzed. In some embodiments, PVOH is at most 95% hydrolyzed or at most 90% hydrolyzed or at most 88% hydrolyzed. Examples of suitable PVOH have a weight average molecular weight (Mw) of at least 15,000Da or at least 20,000Da. Examples of suitable PVOH have a weight average molecular weight (Mw) of at most 150,000Da or at most 120,000Da. Examples of suitable PVOH include PVOH 04-88 and PVOH 26-88, which are commercially available.

[0048] In some embodiments, the organic binder and the surfactant are selected so that the organic binder forms an emulsion with a particle size of at least 200 nm, or at least 400 nm, or at least 500 nm, or at least 600 nm. In some embodiments, the organic binder and the surfactant are selected so that the organic binder forms an emulsion with a particle size of at most 1000 nm, or at most 800 nm.

[0049] In some embodiments, the organic binder and surfactant are selected so that the organic binder forms an emulsion that is stable in a cohesive environment. The cement used in the mortar creates an alkaline environment with high calcium ions. This environment can cause some emulsions to decompose. Other combinations of organic binders and surfactants are known to form stable emulsions in this environment, and combinations that form stable emulsions can be advantageously used in the dry mix / mortar of the present invention.

[0050] It should be understood that the nominal dry powder may contain a small amount of moisture. In some embodiments, the water-dispersible organic binder contains no more than 5 wt % or no more than 4 wt % or no more than 3 wt % or no more than 2 wt % or no more than 1 wt % moisture based on the weight of the water-dispersible organic binder. In some embodiments, the water-dispersible organic binder may not contain detectable moisture content (0 wt %, based on the weight of the water-dispersible organic binder).

[0051] Examples of suitable organic binders are commercially available, such as those sold under the trade name DOW TM Latex Powder2000 and DOW TMLatex Powder 2001, and under the trade names VaVeova and VaE-Veova. Other organic binders can be prepared in aqueous dispersions by emulsion copolymerization of vinyl ester monomers and ethylene monomers according to known methods, such as described in Lindmann, Vinyl Acetate / Ethylene Emulsion Copolymers, Paint Manufacture, September 1968, 30-36, and in U.S. Pat. No. 5,576,384 and U.S. Application No. 2009 / 0069495A1. The resulting dispersion can be spray dried to produce a redispersible powder.

[0052] In some embodiments, the amount of organic binder in the dry mix / mortar is at least 0.5 wt % or at least 1 wt % or at least 1.5 wt % or at least 2 wt % based on the weight of the dry components and excluding water. In some embodiments, the amount of organic binder in the dry mix / mortar is at most 12 wt % or at most 10 wt % or at most 8 wt % or at most 6 wt % or at most 5 wt % based on the weight of the dry components and excluding water.

[0053] The dry mix / mortar of the present invention contains recycled composite fibers having an average diameter not exceeding 50 microns and an average length not exceeding 800 microns. The recycled composite fibers can be prepared by grinding and / or crushing unwanted composite materials such as end-of-life wind turbine blades, parts of automobiles, ships and aircraft, and sports equipment and waste from composite manufacturing. Methods for recovering recycled composite fibers from composite materials are described in: U.S. Patent 5,569,424 and U.S. Patent Application 2011 / 0301287 and Section 4.1 "Mechanical Recycling" Krauklis et al., Composite Material Recycling Technology—State-of-the-Art and Sustainable Development for the 2020s, 2021(5) Journal of Composite Materials Science (J.Compos.Sci.) 28.( https: / / doi.org / 10.3390 / jcs5010028 ).

[0054] The content of recycled composite fibers reflects the content of the composite materials from which they are made. Composite materials typically contain fibers embedded in a polymer matrix.

[0055] Examples of suitable fibers in composite materials include glass fibers, carbon fibers, basalt fibers, and aramid fibers. All fibers are commercially available. Glass fibers are generally classified as E-glass, S-glass, or R-glass. E-glass fibers contain borosilicate glass. S-glass fibers contain magnesium aluminum silicate glass. R-glass fibers contain calcium aluminosilicate glass. Other possible examples of glass fibers are sold under the trademarks: ECRGLAS, Advantex, and WindStrand.

[0056] In some embodiments, the fibers in the composite material are all one type of fibers, such as glass fiber, carbon fiber, basalt fiber or aramid fiber. In some embodiments, the fiber in the composite material contains a mixture of fibers, such as glass and aramid or glass and carbon. In some embodiments, the fiber in the composite material contains at least 50 weight % or at least 60 weight % or at least 70 weight % or at least 80 weight % or at least 90 weight % of glass fiber. In some embodiments, the fiber in the composite material contains glass fiber and at least 10 weight % or at least 20 weight % or at least 30 weight % of carbon or aramid fiber. In some embodiments, the fiber in the composite material contains glass fiber and no more than 50 weight % or no more than 40 weight % or no more than 30 weight % of carbon or aramid fiber.

[0057] In some embodiments, the fibers in the composite material are coated with a sizing. The sizing protects the fibers and promotes bonding to the matrix polymer. Suitable sizing depends on the selected fiber; sizing is commercially available and well known in the composite material industry. Examples of suitable sizings for glass and basalt fibers include chromium oxide, titanium oxide, and organosilane compounds with amine or epoxy functional groups. Examples of sizings for carbon fibers include epoxy resins, polyamides, polypropylene, or polyurethane dispersions. Examples of sizings for aramid fibers include polyvinyl alcohol and certain other polymers.

[0058] Examples of suitable polymer matrices in composite materials include thermosetting and thermoplastic polymers. Examples of suitable thermosetting resins include epoxy resins and polyester resins. Examples of suitable thermoplastic polymers include thermoplastic polyurethanes, nylon polyamides, high density polyethylene, low density polyethylene, polystyrene, and polypropylene. In some embodiments, the polymer matrix is ​​a thermosetting polymer. In some embodiments, the polymer matrix is ​​an epoxy resin.

[0059] Examples of suitable composite materials include composite materials comprising glass fibers and optionally carbon or aramid fibers embedded in an epoxy resin matrix. Other examples of suitable composite materials include composite materials comprising glass fibers and optionally carbon or aramid fibers embedded in a polyester matrix.

[0060] The recycled composite fibers contain fibers with an adhered matrix resin that reflects the above selections. In some embodiments, the recycled composite fibers contain at least 10 wt. %, or at least 15 wt. %, or at least 25 wt. %, or at least 30 wt. % matrix resin, based on the total weight of the recycled composite fibers. In some embodiments, the recycled composite fibers contain up to 50 wt. %, or up to 45 wt. %, or up to 40 wt. %, or up to 35 wt. % matrix resin, based on the total weight of the recycled composite fibers.

[0061] The average length of the recycled composite fibers does not exceed 800 microns. In some embodiments, the average length of the recycled composite fibers is at least 100 microns, or at least 200 microns, or at least 250 microns, or at least 300 microns. In some embodiments, the average length of the recycled composite fibers is at most 700 microns, or at most 600 microns, or at most 550 microns, or at most 500 microns.

[0062] The average diameter of the recycled composite fibers does not exceed 50 microns. In some embodiments, the average diameter of the recycled composite fibers is at least 5 microns, or at least 10 microns, or at least 15 microns, or at least 20 microns. In some embodiments, the average diameter of the recycled composite fibers is at most 45 microns, or at most 40 microns, or at most 35 microns, or at most 30 microns.

[0063] In some embodiments, the aspect ratio (average length / average diameter) of the recycled composite fibers is at least 2 or 3 or 4 or 5 or 6 or 7 or 8. In some embodiments, the aspect ratio of the recycled composite fibers is at most 100 or 50 or 30 or 20 or 18 or 15 or 12 or 10.

[0064] The dry mix / mortar contains 3% to 15% recycled composite fibers by weight, based on the weight of the dry components excluding water. In some embodiments, the dry mix / mortar contains at least 4% by weight, or at least 5% by weight, or at least 6% by weight, or at least 7% by weight of recycled composite fibers, based on the weight of the dry components excluding water. In some embodiments, the dry mix / mortar contains up to 12% by weight, or up to 10% by weight of recycled composite fibers, based on the weight of the dry components excluding water.

[0065] Some embodiments of the dry mix / mortar also contain a pozzolan, such as fly ash, calcined kaolin, pumice, or fumed silica. In some embodiments, the dry mix / mortar contains at least 5 wt % or at least 10 wt % or at least 15 wt % pozzolan, based on the weight of the dry components and excluding water. In some embodiments, the dry mix / mortar contains up to 50 wt % or up to 40 wt % or up to 30 wt % pozzolan, based on the weight of the dry components and excluding water. Pozzolans and their use in mortars and concretes are well known and are described in U.S. Pat. No. 9,181,131 B2.

[0066] In addition to cement and fillers, some embodiments of the dry mix / mortar may optionally contain other additives such as cellulose ethers, starch ethers, inorganic rheology modifiers, air entraining agents, accelerators, retarders, high-range water reducers, and defoamers.

[0067] Cellulose ethers (such as methyl cellulose, ethyl cellulose and methyl ethyl cellulose) can increase the water retention of the mortar and extend the open time. Cellulose ethers can also improve the workability and viscosity of the mortar. Suitable cellulose ethers are commercially available, such as those sold under the trade name WALOCEL TM or METHOCEL TM .

[0068] • Starch ethers (such as hydroxypropyl starch ether) can improve the anti-sagging and anti-slip properties of the mortar, as well as extending the open time and providing a smoother surface. Suitable starch ethers are commercially available, such as under the trade name Aqualon.

[0069] • Inorganic rheology modifiers, such as bentonite, organically modified clays, attapulgite, fumed silica and precipitated calcium carbonate, can modify the viscosity and shear-thinning behavior of the mortar. Suitable inorganic rheology modifiers are commercially available with instructions for use.

[0070] Air entraining agents create small air bubbles in the mortar, which improves its resilience during freeze-thaw cycles. Air entraining agents are usually surfactants. Suitable air entraining additives are commercially available with instructions for use.

[0071] ● Accelerators speed up the setting of mortar. They can be particularly useful in cold weather applications.

[0072] Examples of common accelerators include calcium nitrate, calcium nitrite, calcium formate, and certain aluminum compounds.Accelerator formulations are commercially available with instructions for use.

[0073] ● Retarders slow down the setting time of mortar. Examples of common retarders include lignin sulfonic acid, hydroxycarboxylic acids (such as hydroxy acid), carbohydrates, lead oxide, zinc oxide,

[0074] Calcium, sodium and ammonium salts of phosphates, borates and fluorides. Retarder preparations with instructions for use are commercially available.

[0075] ● High-range water reducers allow the production and use of mortars with lower water content. Examples of high-range water reducers include sulfonated melamine-formaldehyde condensates, sulfonated naphthalene-formaldehyde condensates, modified lignin sulfonates, and polycarboxylates. High-range water reducer formulations with instructions for use are commercially available.

[0076] Defoamers reduce air entrapment and voids in the mortar. Examples of defoamers include mineral oil, polyethylene glycols, and polyether siloxanes. Defoamers are commercially available with instructions for use.

[0077] In some embodiments, the dry mix / mortar contains at most 20 wt % or at most 10 wt % or at most 5 wt % or at most 2 wt % of other additives, based on the dry components and excluding water. In some embodiments, the dry mix / mortar contains an unmeasurable amount of other additives (essentially 0 wt %) or at least 1 wt % or at least 2 wt %, based on the weight of the dry components and excluding water.

[0078] To prepare a dry blend, the dry components are blended together. Suitable dry blending techniques are known and suitable equipment for carrying out these techniques is commercially available.

[0079] To prepare the mortar, the dry components are thoroughly mixed with water, either individually or as a dry mix, as previously described. The optimal amount of water varies depending on the dry components and their intended use, and can be easily determined by experimentation. In some embodiments, the amount of water is at least 20% by weight, or at least 22% by weight, or at least 24% by weight, or at least 26% by weight of the weight of the dry components. In some embodiments, the amount of water is at most 60% by weight, or at most 50% by weight, or at most 40% by weight, or at most 30% by weight of the weight of the dry components.

[0080] In some embodiments, the amount of water is selected to provide a mortar (when wet) that is fluid enough so that it can be smoothly applied to the substrate, and viscous enough so that it holds the tile to the substrate without excessive sliding or falling of the tile before the mortar sets. In some embodiments, the mortar has a viscosity of at least 300 Pa·s or at least 350 Pa·s or at least 400 Pa·s or at least 450 Pa·s or at least 500 Pa·s or at least 525 Pa·s or at least 550 Pa·s. In some embodiments, the mortar has a viscosity of at most 800 Pa·s or at most 700 Pa·s or at most 650 Pa·s or at most 600 Pa·s.

[0081] In one embodiment, the mortar contains:

[0082] a) 20 to 50 wt. % cement;

[0083] b) 25 to 65% by weight of an inorganic filler;

[0084] c) 1 to 10% by weight of an organic binder suitable for tile mortar;

[0085] d) 3 to 15 wt. % recycled composite fibers having an average diameter of no more than 50 microns and an average length of no more than 800 microns;

[0086] e) water, wherein all weight percentages are based on the weight of dry components (a)-(d) excluding water. The mortar may also optionally contain 0 wt % to 20 wt % of other additives as previously described. The selection and amount of each component may optionally reflect the embodiments and examples previously described.

[0087] Among other uses, mortar can be used for ordinary tile laying. First, the mortar is applied to the substrate. Second, the tile is pressed onto the applied mortar. Third, the mortar is allowed to set. Each of these steps is well known.

[0088] Examples of suitable substrates include any known rigid building material, such as drywall, wood, plaster or concrete. Examples of suitable tiles include any known tiles, such as ceramic, glass, porcelain, stone or marble, terracotta or concrete.

[0089] The average thickness of the mortar varies according to many factors, such as the smoothness of the substrate and the tile and the intended use. In some embodiments, the mortar is applied with a thickness of at least 2 mm, or at least 3 mm, or at least 4 mm (when wet). In some embodiments, the mortar is applied with a thickness of at most 10 mm, or at most 9 mm, or at most 8 mm, or at most 6 mm, or at most 5 mm (when wet). Solidification causes the mortar to shrink. In some embodiments, the solidified mortar is at least 1 mm, or at least 1.25 mm, or at least 1.5 mm thick. In some embodiments, the solidified mortar is at most 6 mm, or at most 5 mm, or at most 4 mm, or at most 3 mm thick.

[0090] The setting time of the mortar depends on many factors, such as temperature, water content, and mortar components. In some embodiments, the setting time is between 300 minutes and 700 minutes. In some embodiments, the setting time may be longer or shorter.

[0091] In some embodiments, the mortar provides at least 0.5 N / mm after curing at room temperature when tested according to the test method. 2 or at least 0.75N / mm 2 or at least 1N / mm2 or at least 1.1N / mm 2 or at least 1.2N / mm 2 or at least 1.3N / mm 2 There is no maximum desired stretch bond, but in many embodiments, it is higher than 3 N / mm 2 or 2N / mm 2 The adhesion provides little added value.

[0092] In some embodiments, the mortar has a lateral deformation of at least 2.5 mm, or at least 2.6 mm, or at least 2.8 mm, or at least 3 mm when tested according to the Test Methods. In some embodiments, the mortar has a lateral deformation of at most 8 mm, or at most 6 mm, or at most 5 mm, or at most 4.5 mm, or at most 4 mm, or at most 3.75 mm when tested according to the Test Methods.

[0093] The method produces a tiled surface comprising:

[0094] 1. Base material;

[0095] 2. Multiple tiles; and

[0096] 3. A setting mortar for bonding the tiles to a substrate, wherein the mortar comprises: (a) cement, (b) an inorganic filler, (c) an organic binder suitable for use in tile mortars; and (d) 3 to 15 weight percent of recycled composite fibers having an average diameter of no more than 50 microns and an average length of no more than 800 microns, wherein all weight percentages are based on the weight of the dry components (a)-(d).

[0097] The selection and specific embodiments of the substrate, tile and mortar are as previously described, except that the mortar has been allowed to set so that it no longer contains high levels of water in the wet mortar. The proportions of the dry components are as previously described.

[0098] Example

[0099] Test Method

[0100] The parameters described in this application can be measured using the following measurement methods:

[0101]

[0102]

[0103] Molecular weight

[0104] The Mark-Houwink plots of molecular weight / molecular weight distribution and branching structure analysis were measured using triple detector gel permeation chromatography. The methods and formulas used are described in U.S. Patent No. 8,871,887. U.S. Patent No. 8,871,887 is incorporated herein by reference. For gel permeation chromatography (GPC) methods (conventional GPC, light scattering (LS) GPC, viscometric GPC, and gpcBR), a triple detector gel permeation chromatography (3D-GPC or TDGPC) system was used. The system includes a Robotic Assistant Delivery (RAD) high temperature GPC system [other suitable high temperature GPC instruments include Waters (Milford, Mass.) Model 150C High Temperature Chromatograph; Polymer Laboratories (Shropshire, UK) Model 210 and Model 220; and Polymer Char GPC-IR (Valencia, Spain)], equipped with a Precision Detectors (Amherst, Mass.) two-angle laser light scattering (LS) detector Model 2040, an IR4 infrared detector from Polymer ChAR (Valencia, Spain), and a 4-capillary solution viscometer (DP) (other suitable viscometers include Viscotek (Houston, Tex.) 150R4-capillary solution viscometer (DP)). A GPC having at least one of these latter two independent detectors and the former detector may be referred to as a "3D-GPC" or "TDGPC", while the term "GPC" alone generally refers to a conventional GPC. Data collection is performed using software (eg, Polymer Char GPC-IR). The system is also equipped with an online solvent degasser (eg, from Polymer Laboratories).

[0105] The eluent from the GPC column set flows through each detector arranged in series in the following order: LS detector, IR4 detector, followed by DP detector. The systematic method for determining multi-detector offset is similar to that of Balke, Mourey et al. (Mourey and Balke, Chromatography Polym., Chapter 12, (1992)) (Balke, Thitiratsakul, Lew, Cheung, Mourey, Chromatography Polym., Chapter 13, (1992)). Olexis LS columns are used. The sample transport chamber is operated at 140°C and the column chamber is operated at 150°C. The sample is prepared at a concentration of 0.1 grams of polymer in 50 milliliters of solvent. The chromatographic solvent and sample preparation solvent are 1,2,4-trichlorobenzene (TCB) containing 200 ppmw of 2,6-di-tert-butyl-4-methylphenol (BHT). The solvent is purged with nitrogen. The polymer sample is gently stirred at 160°C for four hours. The injection volume is 200 microliters. The flow rate through the GPC was set to 1 mL / min.

[0106] For conventional GPC, an IR4 detector is used, and the GPC column is calibrated by running 21 narrow molecular weight distribution polystyrene standards. The molecular weight of the standards ranges from 580 g / mol to 8,400,000 g / mol, and the standards are contained in six "mixed liquid" mixtures. Each standard mixture is at least ten steps apart between individual molecular weights. Polystyrene standards are prepared under the following conditions: for molecular weights equal to or greater than 1,000,000 g / mol, 0.025 g is prepared in 50 mL of solvent, and for molecular weights less than 1,000,000 g / mol, 0.05 g is prepared in 50 mL of solvent. The polystyrene standards are dissolved at 80 ° C by gentle stirring for 30 minutes. The number average molecular weight, weight average molecular weight, and z average molecular weight are calculated according to formulas, for example, as described in U.S. Patent No. 8,871,887.

[0107] For LS GPC, a precision detector PDI2040 detector model 2040 is used. For 3D-GPC, the absolute weight average molecular weight is calculated according to the formula, for example, as described in U.S. Patent No. 8,871,887. The gpcBR branching index is determined by calibrating the light scattering, viscosity and concentration detectors and subtracting the baseline. The integration window is set for the integration of the low molecular weight retention volume range in the light scattering and viscometer chromatograms, and the chromatogram indicates the presence of detectable polymers from the refractive index chromatogram. Linear polyethylene standards are used to establish polyethylene and polystyrene Mark-Houwink constants. This constant is used to construct two linear reference conventional calibrations of polyethylene molecular weight and polyethylene intrinsic viscosity as a function of elution volume, for example, as described in U.S. Patent No. 8,871,887. In order to determine the gpcBR branching index, the light scattering elution area of ​​the sample polymer is used to determine the molecular weight of the sample. The final Mark-Houwink constant is used for analysis, for example, as described in U.S. Patent No. 8,871,887.

[0108] Example

[0109] A series of dry blends were prepared by blending the dry ingredients listed in Table 1. Examples labeled IE are inventive examples containing recycled composite fibers. Examples labeled CE are comparative examples without recycled composite fibers. Each dry blend was blended with water to prepare mortar.

[0110] Each mortar was used to prepare specimens for lateral deformation testing according to ISO 130007-2 using a rectangular frame (Template A) with internal dimensions of (280 ± 1) mm × (45 ± 1) mm × (5 ± 0.1) mm and a non-absorbent mold (Template B) with dimensions of (300 ± 1) mm × (45 ± 1) mm × (3 ± 0.1) mm. Form A was firmly fixed on a polyethylene film. Sufficient adhesive was applied to the form and then scraped clean to neatly and completely fill the holes in the form. The mold was firmly clamped to the flow table and the sample was compacted using 70 vibrations. The soil mound was gently lifted from the flow table and the form was carefully removed vertically. A layer of release agent was applied to form B and it was positioned centrally on the sample. The form was loaded with a mass capable of applying a force of (100 ± 0.1) N and an approximate cross-sectional area of ​​(290 × 45) mm. The applied pressure ensured that the material completely filled the recess of the form to the required thickness. Any excess material was removed from the sides of the template and after 1 hour, lumps were removed. The samples were demoulded 48 hours after preparation. The samples were cured in an airtight plastic container at (23 ± 2) ° C for 12 days and then cured for an additional 14 days at (23 ± 2) ° C and (50 ± 5)% RH. The thickness of the sample needed to be (3.0 ± 0.1) mm. Any sample beyond the thickness required for the lateral deformation test was discarded.

[0111] For the tensile bond strength test, the fresh mortar paste was applied as a thin layer to the concrete slab with a straight-edged trowel. A thicker layer was then applied and combed with a 6*6 mm notched trowel. The trowel was held at an angle of approximately 60° to the substrate, at right angles to one edge of the blank, and pulled across the board parallel to that edge (in a straight line). The tiles were then left for 5 minutes after the mortar was applied, and a load of (20±0.05)N was placed on the tiles for 30 seconds to ensure that the tiles were set in the wet mortar. The tiles were cured for 28 days at (23±2)°C and (50±5)%R.

[0112] The transverse direction deformation and tensile adhesion were tested using the test methods listed above. The results are listed in Table 1.

[0113]

Claims

1. A dry blend, comprising: (a) Cement; (b) an inorganic filler, wherein 95% to 100% by weight of the filler particles will pass through a 2.36 mm sieve; (c) an organic binder suitable for use in tile mortar; (d) 3 to 15 weight percent recycled composite fibers having an average diameter of no greater than 50 microns and an average length of no greater than 800 microns, wherein all weight percentages are based on the weight of dry components (a)-(d).

2. The dry blend of claim 1, wherein the dry blend contains 5 to 10 wt% recycled composite fibers.

3. The dry blend of any one of claims 1 or 2, wherein the average diameter of the recycled composite fibers is from 10 microns to 40 microns.

4. The dry blend of any one of claims 1 to 3, wherein the average length of the recycled composite fibers is from 200 microns to 500 microns.

5. The dry blend of any one of claims 1 to 4, wherein the recycled composite fibers comprise glass fibers.

6. The dry blend of any one of claims 1 to 5, wherein the recycled composite fibers comprise a cured thermosetting resin adhered to the fibers.

7. The dry blend of any one of claims 1 to 6, wherein the recycled composite fiber comprises 20 to 40 wt% cured epoxy resin and 60 to 80 wt% fiber, wherein the weight percentages are based on the total weight of the recycled composite fiber.

8. The dry blend according to any one of claims 1 to 7, wherein 95% to 100% of the filler particles have a diameter of no more than 1 mm.

9. A mortar comprising the dry mix component according to any one of claims 1 to 8 and further comprising (e) water.

10. A method of attaching a tile to a substrate using the mortar according to claim 9, the method comprising the steps of: (a) applying the mortar to a substrate; (b) applying a plurality of tiles to the mortar on the substrate; as well as (c) allowing the mortar to set.

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