Abstract: A grout composition comprising - an Acrylic Polymer component of about 12 – 14 percent by weight; a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight; a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillers and other functional additives by weight percentage.
Claims:
1. A grout composition comprising :-
anAcrylic Polymer component of about 12 – 14 percent by weight;
a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight;
a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillersand other functional additives by weight percentage.
2. The grout composition as claimed in claim 1, wherein one of the primary filler includes coated silica sand or manufactured sand of about 60 to 70 percentage by weight.
3. The grout composition as claim 1, wherein the other functional additives includes acrylic thickener component of about 0.1 to 0.2 percentage by weight, Defoamer component of about 0.04 – 0.05 percentage by weight.
4. The grout composition as claimed in claim 1, wherein the other functional additives further includes cross linking compound of about 1 - 2 percentage by weight and fiber of about 0.05 – 0.08 percentage by weight.
5. The grout composition as claimed in claim 1, wherein thesecond filler isan ultra-fine mineral filler, in the form of calcium carbonate.
6. The grout composition as claimed in claim 1, wherein the third filler is light weight inert filler in the form of recycled glass beads or cenosphericalumino silicate hollow spheres.
7. The grout composition as claimed in claim 1, wherein the acrylic polymer is dispersed in water and a solvent preferably Aqueous styrene-acrylate copolymer dispersion, and hard polymer with high glass transition temperature, in dispersion form dispersed in water preferably water based styrene butadiene dispersions and a solvent which provides cross linking characteristics.
8. The grout composition as claimed in claim 1, wherein the Polyurethane Dispersion (PUD) includes one or more air curable water soluble components.
9. The grout composition as claimed in claim 1, wherein the said grout composition, when cured, develops a flexible, hard surface and smooth finish.
10. The grout composition as claimed in claim 1, wherein the tertiary filler, clay - in the form of alumino silicate kaolinite clay which imparts rheology to the paste, and the tertiary filler. .
11. The grout composition as claimed in claim 1, wherein the other functional additives includes a slightly hazy liquid polyether siloxane copolymer containing fumed silica, a highly effective defoamer concentrate for the paste system, a wetting agent, a nonionic, octylphenolethoxylate surfactant, and a cross linking diluent in the form of methyl ethyl glycol (MEG), a polyester fiberor equivalent synthetic material which helps in shrinkage reduction and higher tensile strength.
12. A grout composition comprising :-
an Acrylic Polymer component of about 12 – 14 percent by weight;
a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight;
a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillersand other functional additives by weight percentage wherein the filler includes of a light weight inert filler in the form recycled glass beads or cenosphericalumino silicate hollow spheres, imparting flowability and curing property to the grout system.
13. The grout composition as claimed in claim 12 wherein the acrylic polymer is in the form of anionic water based dispersion of a butadiene acrylate copolymer imparting stability to the paste on long term storage.
14. A grout composition comprising :-
an Acrylic Polymer component of about 12 – 14 percent by weight;
a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight;
a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillers by weight percentage wherein the filler includes of a light weight inert filler in the form of recycled glass beads or cenosphericalumino silicate hollow spheres, imparting flowability and curing property to the grout system and wherein the Polyurethane Dispersion Component (PUD) is in the form of a solvent-free non-ionic rheology additive with high thickening properties at low shear stress-achieve higher pseudoplastic viscosity.
15. A grout composition comprising :-
an Acrylic Polymer component of about 12 – 14 percent by weight;
a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight;
a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillers by weight percentage wherein the filler includes about 50% to 75%, by weight of inert filler in the form of silica sand or manufactured sand having an average particle size in the range from 90 microns to 800 microns; about 1% to 8%, by weight, of second fine inert mineral particles having an average particle size in the range from 5 microns to 150 microns; and 1% to 5%, by weight, of a light weight inert aggregate having an average particle size in the range from 90 microns to 500 microns; and 2% to 10%, by weight of an air curable water soluble polyurethane dispersion.
16. The grout composition as claimed in claim 15, wherein the fillers includes silicon di oxide, calcium carbonate, and /or any other mineral inert fillers or clay incorporated in the composition in the range from 25% to 85%, by weight, preferably 60% to 80%, by weight.
17. A grout composition comprising :-
an Acrylic Polymer component of about 12 – 14 percent by weight;
a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight;
a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillers by weight percentage wherein filler includes about 2% to 12%, by weight of hard polymer with high glass transition temperature in dispersion form dispersed in water, styrene butadiene dispersions,(S); about 4% to 20%, by weight, of second water based resin polymeric dispersion in the form of a flexible acrylic polymer dispersed in water and solvent, aqueous styrene-acrylate copolymer dispersion (A), 2% to 12%, by weight, of one or more air curable water soluble Polyurethane Dispersion polymer, PUD (P).
18. The grout composition as claimed in claim 17, wherein the acrylic polymers include homopolymers of acrylate, homopolymers of alpha-methyl acrylate and the like.
19. The grout composition as claimed in any of the preceding claims wherein,during application / use, thegrout composition further includes water and organic solvents for adjusting the viscosity in the range of 80000 cps and 20000 cps to provide adequate workability to the composition.
20. The grout composition as claimed in any of the preceding claims wherein, following application, substantially all of the above solvent evaporates, leaving a cured mixture of PUD, stain resistant polymer resins, mineral fillers and other non-volatile components.
21. The grout composition as claimed in any of the preceding claims, wherein the grout composition comprises 0.05% to 0.60%, by weight of acrylic thickeners in the form of anionic water based dispersion of a butadiene acrylate copolymer of acrylic based thickener; about 0.05% to 0.50%, by weight, of thickener in the form of in the form of a solvent-free non-ionic rheology additive with high thickening properties at low shear stress-in order to achieve higher pseudoplastic viscosity polyurethane dispersion.
22. A grout composition as claimed in any of the preceding claims, wherein the said grout composition is applicable for tile surfaces; natural and synthetic stone surfaces of vertical and / or horizontal nature from 1 mm joint width to 12 mm joint width and tiles and the exposed temperatures ranging from 0 Deg C to 60Deg C without shrinking or cracking.
, Description:Field of the Invention
The present invention relates to premix joint material or premix grouts. More particular the present discloses Ready To Use(RTU) or premix grouts containing water based Styrene- Acrylic- Polyurethane dispersions (SAP)formulated in an optimized proposition as the main binding components in the composition, and methods of using thereof.
Prior Art
Several ready to use or premixed grout compositions exist in the market. For instance premixed grouts having an acrylic binder (e.g., acrylic polymers and copolymers) were among some of the first premixed grouts commercially available. These types of acrylic binder premixed grouts are designed for use in low demand applications, such as, for use in kitchen backsplashes and/or areas that are not subjected to water. U.S. Pat. Nos. 3,859,233 and 4,472,540 (both to Barker) describe the use of acrylic binder dispersions in grout compositions.
Other premixed grouts on the market include those containing mere simple blends of polyurethane and acrylic. In these grouts, the polyurethane and acrylic components reside in the composition as separate constituents, and may be individually identified, isolated and separated from such composition. In these grouts, a polyurethane component is added to the composition to improve performance of the acrylic-based material including, for instance, improving hardness, abrasion resistance and stain resistance of the resultant grout. U.S. Pat. No. 5,569,696 (to Abramson, et al.) discloses such a premixed grout containing a blend of a polyurethane part in combination with an acrylic part.
Grouts including water-borne polyurethane binder systems have been developed for the purpose of joining objects, such as tile and masonry, and for filling joints and voids between tiles and masonry. Such grout may be used to join tile to floors, walls, and ceilings and to fill the joints between such tiles so as to join the tiles into a continuous surface. U.S. Pat. No. 7,183,338 (Warren) describes grouts including water-borne polyurethane binder systems and grout products including water-borne polyurethane binder systems are commercially available from Star quartz Industries, Inc. of Baltimore, Md. under the QUARTZ-LOCK® brand.
Another U.S. Publication No. 556996 A, discloses a stain resistant grout composition comprises a mixture of an acrylic latex, an aliphatic urethane and a paraffin. The composition of this invention is a mixture of a mixture of an acrylic latex, an aliphatic urethane and a paraffin. Preferably, the composition is 5% to 40% by weight of acrylic latex, 0.5% to 15% by weight of aliphatic urethane and 0.5% to 6% by weight of paraffin.
Another U.S. Pat No. 8263694 B1 discloses an invention having a binder including water-borne polyurethane and a filler are described herein. An accelerator component is provided to control the rate of grout curing, thereby decreasing the time required between grout application and grout use. This result is achieved while providing sufficient time for grout application. Grout may be light-transmissive and include light-transmissive binder and filler.
Another US publication No. US 4476276A discloses a sealing composition prepared by reacting water-soluble polyurethane prepolymer with water containing latex to provide a gelled viscous mass which will cure to a cross-linked latex-reinforced gel capable of preventing or inhibiting leakage in various structures, when applied at the site of the leakage in the viscous state. The sealing composition of the invention also preferably contains up to 60% by weight of fillers of the total weight of the composition to provide a high compressive strength, shrink-resistant sealing composition.
Another US publication No.US 5569696 A discloses a stain resistant grout composition comprises a mixture of an acrylic latex, an aliphatic urethane and a paraffin. Preferably, the composition is an aqueous composition and is a low volatile organic compound (VOC) composition.
Another US patent No. US 6590025 B1: Latex compositions having improved drying speed. The invention relates generally to latex compositions, particularly one-pack storage-stable latex compositions. The present invention is especially useful for latex compositions which are capable of undergoing radiation-curing. Such latex compositions are useful in coatings (especially on wood and wood products, metal, plastic, and leather), adhesives, inks, and caulks. Such compositions exhibit improved dry speed.
Yet another US patent application No. US 20120160414 A1discloses Polyurethane-acrylic polymer dispersions and uses thereof: relates to compositions combining an acrylic component with another polyurethane component, and uses thereof, for example, as liquid membranes for roofs.
Limitations of the Prior Art:
However such inventions which are in use are commonly known for slow curing, and restrictions to use: most of these inventions limits the grout usage in interior floors or walls, not necessarily recommended for use in exterior and exposed applications. Another major limitation of those reported inventions is the lack of stability in water immersed applications like swimming pools or bath rooms. Therefore there is a strong need for the ready to use/premix grout systems where the grout can be applied in all conditions and all weather applications. In another words, it is desirable to have RTU with the ability to apply on substrates, surfaces to accommodate foot or vehicular traffic without grout damage or discoloration, or the ability of the grout to be in contact with water or moisture, for example in an exterior application (e.g., external wall cladding with large format tiles/stones, an exterior patio or pool deck or exposed drive way) or in an interior or exterior high-humidity application (e.g., a shower).
The other desirable property for the ready to use grout is that these grouts should be capable of curing when applied over a larger width up to 12 mm and depth up to 25 mm which is a limitation with the existing technologies.
Summary of the invention
In view of the above deficiencies of the prior art, the present invention is designed to provide grout compositions with unique binder blend system (Styrene-Acrylic-Polyurethane system- SAP) having stability in the bucket for long term storage, develop adequate hardness after 24 hour foot traffic, develop adequate strength to withstand the heavy traffic and use after 72 hours, develop high durability and high flexibility needed for all weather and all area applications, and adequate long term stability for water immersion applications.
The present invention is designed to provide grout compositions that uses a Styrene-Acrylic-Polyurethane system(SAP) as a binder in combination with filler materials. The filler material may be natural sand, silica sand, coloured silica sand, fine silica, glass, recycled glass, limestone, minerals, any other known filler, or any combinations thereof.
Therefore the present invention include the Styrene-Acrylic-Polyurethane system(SAP) grout formulations of in combination with a natural silica sand or quartz filler material, as well as one or more additional constituents including, but not limited to, a freeze-thaw stabilizer co-solvent, plasticizer, short fibers, polyester fibers, an adhesion promoter, a preservative, biocide, cellulose or starch ether, a thickening agent, silica fume, fumed silica, silica fume, a deaerator, defoamer, and/or surfactant.
Such as herein described is a grout composition comprising an Acrylic Polymer component of about 12 – 14 percent by weight;a Polyurethane Dispersion (PUD) component of about 6 to 9 percent by weight;a Styrene Butadiene component of about 3 to 5 percent by weight; and rest component includes any one or a combination of a plurality of fillers and other functional additives by weight percentage.
Brief Description of the Accompanying Drawings
Figure -1 illustrates 1”x1” compressive moulds used to prepare samples for RTU grout systems for the purposes of testing physical and chemical parameters / properties in accordance with the present invention;
Figure 2 illustrates a graph exhibiting comparative results of compressive Strength of Styrene Acrylic Polyurethane System vs 2 binder systems in accordance with the present invention;
Figure 3 illustrates a graph exhibitingwater Absorption Rate of Styrene Acrylic Polyurethane System vs 2 binder systems in accordance with the present invention.
Detailed Description
The invention describes a ready to use grout composition in a paste form that consists of one or more air curable water soluble Polyurethane Dispersion polymer (PUD), aultra-fine mineral filler, a flexible low glass transition temperature acrylic polymer dispersed in water and a solvent. The grout composition, when cured, develops a hard surface, yet highly flexible, smooth finish similar to conventional sanded grouts.
The disclosed compositions are especially suitable in grouting applications and filling the joints between ceramic tiles. This invention relates to the compositions, the method of grouting using said compositions and the installed product wherein said compositions are used to bond the individual tiles, grouting and bonding ceramic tile, cement tile, bricks, natural stones, mineral chips, glass tessera and glass plates, employing said compositions.
In an embodiment, the grout composition consists of one or more air curable water soluble Polyurethane Dispersion polymer (PUD), a ultra-fine mineral filler, a flexible acrylic polymer dispersed in water and solvent (Aqueous styrene-acrylate copolymer dispersion), and hard polymer with high glass transition temperature in dispersion formdispersed in water(water based styrene butadiene dispersions)and a solvent which provides cross linking characteristics. Preferably, the grout composition, when cured, develops a flexible, hard surface, smooth finish similar to conventional sanded grouts.
In another embodiment, the grout compositionhither by described as Styrene-Acrylic-Polyurethane system (SAP) consists of hard polymer with high glass transition temperature in dispersion form dispersed in water, styrene butadiene dispersions,(S), a flexible acrylic polymer dispersed in water and solvent, Aqueous styrene-acrylate copolymer dispersion,(A), one or more air curable water soluble Polyurethane Dispersion polymer, PUD (P), a primary filler in form of silica sand or manufactured sand (silica sand or manufactured sand is mandatory but coating is optional. Silica sand is available in nature whereas manufactured sand is processed from rocks to have a similar gradation of silica sand. Both are inert in nature and doesn’t alter the workability of the grout), dye, inorganic iron oxide pigments, a second filler, a ultra-fine mineral filler, in the form of calcium carbonate. The grout composition can include one or more other ingredients such as clay in the form of alumino silicate kaolinite clay which imparts rheology to the paste, an anti-foam, in the form of TEGO® Foamex 810, a slightly hazy liquid polyether siloxane copolymer, and contains fumed silica, a highly effective defoamer concentrate for the paste system, a wetting agentin the form of Vibton X 50, a nonionic, octylphenolethoxylate surfactant that is an excellent emulsion stabilize), and a cross linking diluent in the form of methyl ethyl glycol (MEG), a polyester fibre, in the form of RECRON S or equivalent synthetic or natural in nature,which helps in shrinkage reduction and higher tensile strength. Preferably, the grout composition, when cured, develops a flexible, hard, smooth finish similar to conventional sanded grouts.
In another embodiment, the grout composition hither by described as Styrene-Acrylic-Polyurethane system (SAP) consists of hard polymer with high glass transition temperature in dispersion form dispersed in water, styrene butadiene dispersions,(S), a flexible acrylic polymer dispersed in water and solvent, Aqueous styrene-acrylate copolymer dispersion, (A), one or more air curable water soluble Polyurethane Dispersion polymer, PUD (P), a primary filler in form of silica sand or manufactured sand, dye, inorganic iron oxide pigments, a second filler, a ultra-fine mineral filler, in the form of calcium carbonate. The grout composition can include one or more other ingredients such as clay in the form of alumino silicate kaolinite clay which imparts rheology to the paste, an anti-foam, in the form of TEGO® Foamex 810, a slightly hazy liquid polyether siloxane copolymer, and contains fumed silica, a highly effective defoamer concentrate for the paste system, a wetting agent in the form of VibtonX 50, a nonionic, octylphenolethoxylate surfactant that is an excellent emulsion stabilize), and a cross linking diluent in the form of methyl ethyl glycol (MEG), a polyester fibre, in the form of RECRON S or equivalent synthetic or natural in nature, which helps in shrinkage reduction and higher tensile strength. The SAP system also consists of a light weight inert filler in the form of recycled glass beads or cenosphericalumino silicate hollow spheres, imparting flowability and curing property to the grout system. The SAP grout system also consists of acrylic thickeners in the form of anionic water based dispersion of a butadiene acrylate copolymer which imparts stability to the paste on long term storage.Preferably, the grout composition, when cured, develops a flexible, hard, smooth finish similar to conventional sanded grouts.
In another embodiment, the grout composition hither by described as Styrene-Acrylic-Polyurethane system (SAP) consists of hard polymer with high glass transition temperature in dispersion form dispersed in water, styrene butadiene dispersions,(S), a flexible acrylic polymer dispersed in water and solvent, Aqueous styrene-acrylate copolymer dispersion, (A), one or more air curable water soluble Polyurethane Dispersion polymer, PUD (P), a primary filler in form of silica sand or manufactured sand, dye, inorganic iron oxide pigments, a second filler, a ultra-fine mineral filler, in the form of calcium carbonate. The grout composition can include one or more other ingredients such as, clay in the form of alumino silicate kaolinite clay which imparts rheology to the paste, an anti-foam, in the form of TEGO® Foamex 810, a slightly hazy liquid polyether siloxane copolymer, and contains fumed silica, a highly effective defoamer concentrate for the paste system, a wetting agent in the form of VibtonX 50, a nonionic, octylphenolethoxylate surfactant that is an excellent emulsion stabilize), and a cross linking diluent in the form of methyl ethyl glycol (MEG), a polyester fibre, in the form of RECRON S or equivalent synthetic or natural in nature, which helps in shrinkage reduction and higher tensile strength. The SAP system also consists of a light weight inert filler in the form of recycled glass beads or cenosphericalumino silicate hollow spheres, imparting flowability and curing property to the grout system. The SAP grout system also consists of acrylic thickeners in the form of anionic water based dispersion of a butadiene acrylate copolymer which imparts stability to the paste on long term storage. The SAP system also consists of a polyurethane thickeners, in the form of Rheovis 1190, a solvent-free non-ionic rheology additive with high thickening properties at low shear stress-achieve higher pseudoplastic viscosity. Preferably, the grout composition, when cured, develops a flexible, hard, smooth finish similar to conventional sanded grouts. A Typical composition of Styrene- Acrylic- Polyurethane dispersions (SAP) RTU grout is shown in Table “A”
S. NO Raw Material Name Weight %
1 Styrene Butadiene (water based styrene butadiene dispersions) (S) 3 - 5
2 Emulsion polymer of acrylic ester and styrene (A) 12 - 14
3 Polyurethane Dispersion (PUD) (P) 6 -9
4 Kaolinite clay 0.80 – 1.80
5 Silica Sand Filler 60- 70
6 Defoamer 0.04-0.05
7 Cross Linking Compound 1.00 – 2.00
8 Surfactant 0.20- 0.32
9 Acrylic Thickener 0.10 - 0.20
10 Recron S Fiber 0.05 – 0.08
11 Calcium carbonate fine filler 4.00- 5.00
12 PU Thickener Rheovis 1190 0.10 – 0.30
One example of this grout composition comprises 50% to 75%, by weight of inert filler in the form of silica sand having an average particle size in the range from 90 microns to 800 microns; about 1% to 8%, by weight, of second fine inert mineral particles having an average particle size in the range from 5 microns to 150 microns; and 1% to 5%, by weight, of a light weight inert aggregate having an average particle size in the range from 90 microns to 500 microns; and 2% to 10%, by weight, of an air curable water soluble polyurethane dispersion. The overall mineral and light weight fillers of the chemical nature as silicon di oxide, calcium carbonate, any other mineral inert fillers incorporated in the composition should be in the range from 25% to 85%, by weight, preferably 60% to 80%, by weight.
One example of this grout composition comprises 2% to 12%, by weight of hard polymer with high glass transition temperature in dispersion form dispersed in water, styrene butadiene dispersions,(S); about 4% to 20%, by weight, of second water based resin polymeric dispersion in the form of a flexible acrylic polymer dispersed in water and solvent, Aqueous styrene-acrylate copolymer dispersion (A), 2% to 12%, by weight, of one or more air curable water soluble Polyurethane Dispersion polymer, PUD (P); Examples of suitable acrylic latex polymers include homopolymers of acrylate, homopolymers of alpha-methyl acrylate. The grout composition comprises of water and organic solvents to provide adequate workability to the composition. For example the solvents and water are added to adjust the viscosity in the range of 80000 cps and 20000 cps. Following application, substantially all of the above solvent evaporates, leaving a cured mixture of PUD, stain resistant polymer resins, mineral fillers and any other non-volatile components.
In another example of this grout composition comprises 0.05% to 0.60%, by weight of acrylic thickeners in the form of anionic water based dispersion of a butadiene acrylate copolymer of acrylic based thickener; about 0.05% to 0.50%, by weight, of second thickener in the form of in the form of Rheovis 1190, a solvent-free non-ionic rheology additive with high thickening properties at low shear stress-achieve higher pseudoplastic viscositypolyurethane dispersion.
The grout composition described here has an important advantage that it can be applied on a variety of tile surfaces; stone surfaces from 1 mm joint width to 12 mm joint width without shrinking or cracking. The important advantage of this grout is that it can be applied on horizontal or vertical tile or stone joints from 1 mm width to 12 mm width. The other important advantage of this grout is that it can be applied on exterior surfaces where the temperature varies from 0Deg C to 60Deg C where high flexibility of the grout is needed to accommodate the structural expansion or contraction of the tile or stone surfaces. The other important advantage of this grout is that it can be applied in wet areas and immersed water bodies.
The grout composition described here has a unique advantage that the grout can be cleaned from 15 minutes after application to several days. The grout can be cleaned using a special grout cleaner which removes the haze completely whether it is on the same day or after 2 months. The unique grout cleaner can break attack one of the binder component of the grout thereby rendering the breakage of the binder strength. This is a unique property compared to other comparative grout of similar nature. This unique property makes the application of the grout very easy and flexibility for the installer.
The important advantage of this grout composition is that the grout can resist the shrinkage where higher depth of the filling is required. The another important advantage of this grout is that the grout can provide high flexibility to withstand any stress developed in the tile or stone structure due to movements in the matrix due to variation in the climatic conditions. The important advantage of this grout composition is that the grout is high water resistant and can be used in wet areas and water immersed applications.
The important advantage of this grout composition is that the grout can be applied by any laymen who doesn’t have formal training in grout application. The grout can also be applied in small areas and in part applications. The grout is user friendly and can be applied in indoor areas where high indoor air quality is needed. The grout doesn’t emit any volatile organic contents.
The Styrene-Acrylic-Polyurethane system (SAP) compositions have superior flexibility, water resistance and stain resistance as compared to commercially available Styrene-Polyurethane system (SBR- PUD) or PUD-Acrylics grouts or SBR-Acrylics grouts. Various experiments have been performed with the various combination of SBR- PUD, PUD-Acrylics, and SBR-Acrylics to see the effect of these combinations on the flexibility, curing, and water resistance. As illustrates in various examples and experiments, the composition with Styrene-Acrylic-Polyurethane system (SAP) have shown superior performance in flexibility and water resistance.
The comparative studies were set up for several physical and mechanical properties of the ready to use grout. The comparative studies were conducted by varying the composition of PUD, SBR, Acrylics and inert filler. The properties such as ease of application, clean ability, no shrinkage on wide tile joints, compressive strength using modified method, waterabsorption and stain resistance were measured using the methods as described in Annexure A.For the compressive strength test, a standard one-inch cylindrical mold was filled with the material as per ANSI 118.3. The molds were heat cured for 7 days in a 70 deg.C oven. The samples were then de-molded and cured in a controlled temp chamber and tested after 25 days (28 day measurement from the day of filling the molds). The result indicate that the 3 binder combination has its own properties and the property is the mixed combination of all the 3 binder use in the combination. Strength and other physical properties were balanced to get the hybrid property. Acrylic and PUD combination will provide excellent flexibility. But the compressive strength or the tensile strength reduces due the unavailability of Styrene system. It dries faster than the 3 base hybrid. When styrene combines with PUD the strength will increase. But the physical properties like stain and chemical resistance are poor. The styrene provides a rough surface than the 3 binder system. Styrene and Acrylic will provide better mechanical properties. But will fail to provide the surface properties like stain, chemical and abrasion resistance. It has the higher water absorption properties compared to any dispersions.
The experimental results as shown in tables illustrate that Styrene-Acrylic-Polyurethane system having stability in the bucket for long term storage, develop adequate hardness after 24 hour foot traffic, develop adequate strength to withstand the heavy traffic and use after 72 hours, develop high durability and high flexibility needed for all weather and all area applications, and adequate long term stability for water immersion applications compared to other commercially available similar RTU grouts.
1) Compressive Strength Determination of Styrene-Acrylic-Polyurethane (SAP) RTU Grout
Sample preparation procedure:
RTU grout systems curing is directly related to the thickness of the RTU grout. Higher the thickness the longer the time it needs for the final curing. Hence the normal compressive strength measurement standards used for the cementitious or resinous grouts systems is not applicable for any Ready to Use Grouts.
Accelerated curing procedure is proposed for the measurement of the Styrene-Acrylic-Polyurethane (SAP). The compressive strength measurement of the Styrene-Acrylic-Polyurethane (SAP) is done by using a 1 inch *1 inch compressive moulds made of MS steel or MS coated fixtures. A typical compressive strength mould used for the Styrene-Acrylic-Polyurethane (SAP) sample preparation is shown in Fig 1. Any lubricants (grease) compatible with the product should be used as a grout releasing agent.
The mouldsare filled with the Styrene-Acrylic-Polyurethane (SAP) grout using a spatula or tongue depressor and tap few times to release any air voids from the grout matrix. After filling the moulds, keep the moulds in the laboratory condition for about 30 minutes. After the 30 minute slaking period, transfer the moulds to an oven which is pre-set to the temperature range of 70±20C.Initially the moulds should be allowed to cure for 7 days inside the oven (70±20C). After the 7 day curing in the oven, de-mould the cubes and continue the curing process in the oven at 70±20C for another 7 days (total 14 days). After the 14 days of curing inside the oven, cure the compressive cubes under the standard conditions (23±20C and 50±5% humidity) for the additional 14 days (total 28 days).After completing the total curing cycle of 28 days, test the cubes for compressive strength using UTM. Use the loading rate of 1000 kg-f/ minutes.
Performance of Styrene Acrylic Polyurethane System (SAP)vs 2 binder systems.
Raw Material Composition Styrene-Acrylic-Polyurethane System- SAP Acrylic and PUD PUD and Carboxylated Styrene Acrylic and Styrene
Styrene Butadiene (water based styrene butadiene dispersions) (S) 3 - 5 0 4 – 6 4 - 6
Emulsion polymer of acrylic
ester and styrene (A) 12 - 14 12 - 14 0 12 - 14
Polyurethane Dispersion (Water based PUD) (P) 6 - 9 6- 9 10 - 12 0
China Clay 0.8 - 1.8 0.8 - 1.8 0.8 - 1.8 0.8 - 1.8
Color coated Silica sand or manufactured sand 60 - 70 60 - 70 60 - 70 60 - 70
Defoamer 0.04 - 0.05 0.04 0.04 0.04
Cross Linking Agent 1.0 - 2.0 1.0 - 2.0 1.0 - 2.0 1.0 - 2.0
Surfactant 0.2-0.32 0.2-0.32 0.2-0.32 0.2-0.32
Acrylic Thickener 0.1 - 0.2 0.1 - 0.2 0.1 - 0.2 0.1 - 0.2
Recron S 0.05-0.08 0.05-0.08 0.05-0.08 0.05-0.08
Limestone powder 4 - 5 4 - 5 4 - 5 4 - 5
PU Thickener 0.1 - 0.2 0.1 - 0.2 0.1 - 0.2 0.1 - 0.2
Property
Paste stability Uniform Consistency No separation Separated inside the pail Latex bleeding on the top Soupy consistency
Working Time 10 min 5 min 5 min 5 min
24 hour hardness Cures hard. Foot traffic can be allowed Soft- foot traffic not possible Soft- foot traffic not possible Soft- foot traffic not possible
Compressive Strength at the age of 28 Days (Mpa) as per modified A 118.3 22 12 20 10
Flexibility Measurement as per ASTM C 531 7 7 5 5
Water Absorption after 24 hrs (g) - as per Taber Abrasion Weight Loss Method 0.02 0.06 0.05 0.09
Wet Shower Exposure test - in house method Stable- No erosion of the grout after exposure to wet shower conditions Unstable Unstable Unstable
Chemical resistance as per modified A 118.3 Passed Passed Passed-Medium level performance Passed-Low performance
Tensile strength (psi) - as per modified ASTM C 371 120 Psi 70 Psi 180 Psi 125 Psi
Styrene-Acrylic-Polyurethane system (SAP) provides the perfect balance in mechanical strength and physical/surface properties.
2) Tensile Strength Measurement of Styrene-Acrylic-Polyurethane (SAP) using the Modified ASTM C307 Test Method:
The modified ASTM C 307 test method is used (with the dumb bell shaped tensile moulds) for the Styrene-Acrylic-Polyurethane (SAP) tensile strength measurements. The dumb bell moulds should be of brass or MS coated make. Before filling the moulds with the Styrene-Acrylic-Polyurethane (SAP) grout, apply the grout releasing agents uniformly over the mould interior surfaces. Fill the mould with the grout sample uniformly and tap gently (5 to 6) to relieve all the air voids from the grout matrix. Let the moulds slack for 30 minutes at the room temperature. After the 30 minutes, place the moulds inside the oven for 7 days (70±20C). De-mould the samples and continue the curing at 70±20C for 7 more days (total 14 days) in the oven. After 14 days of curing inside the chamber, let the sample cure under the standard conditions (23±20C and 50±5% humidity) for additional 14 days (28 days).
Test the tensile strength of the cured samples following the same test parameters as described under ANSI 118.3 (ASTM C 307).
3) Flexural Strength Measurement of Styrene-Acrylic-Polyurethane (SAP) using the Modified ASTM C531 Test Method:
The modified ASTM C 531 test method uses the regular shrinkage/flexural bars used for the cementitious or resinous grouts flexural strength measurements. Before filling the moulds with the Styrene-Acrylic-Polyurethane (SAP) grout apply the grout releasing agents uniformly over the mould interior surfaces. Fill the grout sample uniformly and tap gently (5 to 6) to relieve all the air voids from the grout matrix. Let the moulds slack for 30 minutes in room temperature. After the 30 minutes, place the moulds inside the oven for 7 days (70±20C). De-mould the samples and continue the curing at 70±20C for 7 more days (total 14 days) in the oven. After 14 days of curing in the oven, let the sample cure under the standard conditions (23±20C and 50±5% humidity) for additional 14 days (28 days).
For measuring the flexural strength of the cured samples, follow the same test parameters as described under ANSI 118.3.
Performance Matrix for Styrene Acrylic Polyurethane System vs 2 binder systems.
S. NO Properties Styrene-Acrylic-Polyurethane system- SAP Acrylic and PUD PUD and Carboxylated Styrene Acrylic and Styrene
1 Good workability ? X ? ?
2 Good application ? X ? ?
3 Consistent Paste ? X X ?
4 Smooth finish • • X X
5 24 hour Curing and Foot Traffic ? X ? X
6 Abrasion resistant ? ? ? X
7 Chemical resistant ? ? ? X
8 Stain resistant ? ? ? X
9 Under Water Stability ? X X X
? Positive
• Moderate
X Negative
4)Abrasion Resistance Measurement Procedure (Taber Abrasion Weight Loss Method).
Styrene-Acrylic-Polyurethane (SAP) abrasion resistant test specimens can be prepared with the same circular dimension disc that fits the single or double head Taber Abrader (Model 5135 or 5155). The circular specimen mould should be made of MS coated metal or Teflon make with 6 mm sample depth. Apply the grout releasing agent before filling the sample. The sample thickness should not exceed 6 mm. After filling the Styrene-Acrylic-Polyurethane (SAP) grout material in the disc, allow the mould to slack for 30 minutes in room temperature. After the 30 minutes, place the moulds inside the oven for 7 days (70±20C). De-mould the samples and continue the curing at 70±20C for 7 more days (total 14 days) in the oven. After 14 days of curing inside the chamber, let the sample cure under the standard conditions (23±20C and 50±5% humidity) for additional 14 days (28 days). Minimum 3 samples are prepared for the test.
For measuring the Abrasion Loss of the cured samples, the following steps should be followed:
a) Clean the cured samples using a soft brush
b) Take the initial weight before starting the test as the initial weight (A)
c) Switch on the machine and auxiliary vacuum unit
d) Adjust precision vacuum nozzle
e) Keep the abrading wheel on the abrading arm (it can be calibrade system H-22 or H-18).
f) Run the refacing cycles: For calibrase rollers- If it is new, run 50 refacing cycles 2 times. If the last completed cycles was less than 1000 cycles 25 cycles. If it is more than 1000 cycles run 50 refacing cycles. For Calibrade roller- Run the same procedure given as above and always try to reface before testing each specimen. S11 refacing sheet should be used for the refacing activities. These activities should be done in refacing mode in the machine
g) The machine should be in testing mode before running the test
h) Keep the samples in the specimen holder and tight the specimen on the holder using bolts
i) Keep the speed at 60 RPM for the effective abrasion
j) Keep the abrasion cycles as 300 cycles. Extra weight is not required for the normal usages
k) Press start button for the testing. Both the abrasion heads can be used in the same time
l) Ensure the vacuum unit is working with the test. This will help to take away the abraded mass from the surface
m) After completing the test, demount the samples from the surface.
n) Take the post test weight with precision balance (B). Before weighing make sure all the powder particles were cleaned from the specimen surface
o) It is recommended to have one photograph of the specimen before testing and after testing. It will provide an idea about the visual difference on the sample surface after testing. This can be useful for visual end point technique
p) Tabulate all the values. It will be better to test a specimen by comparing another specimen having same specific gravity. It will help to provide the comparison data and can be utilized for product improvement
q) The abrasion loss results can be obtained as below
i. Calculate the weight difference between initial and final weight of the sample
ii. Calculate the weight loss per cycle in milligrams
Weight loss per cycle in milligrams = A-B/300 cycles
A – Initial weight reading of the sample
B- Final weight reading of the sample
iii. The values can be expressed in abrasion index also by using the formula,
Abrasion Index = Abraded mass of specimen (mg)*1000 cycles/No of test cycles
5) Chemical Resistance Measurement Procedure (ANSI 118.3 Modified).
This test covers the evaluation of Styrene-Acrylic-Polyurethane (SAP) grout for resistance to chemical reagents, simulating performance in potential end use circumstances. Chemical reagents can include acids, alkali solutions, organic solvents, lubricants, cleaning agents, or anything else that the test material may be expected to come in contact with. The test includes provisions for reporting changes in weight, dimensions, appearance and strength properties. Provisions are made for various exposure intervals, and elevated temperatures.
Apparatus required:
1) Dispose/plastic glasses – Approx. 30mm dia.
2) Glass beakers (500ml)
3) Weighing balance
4) Holder /Tongue
Chemicals:
Water
Sodium hypochlorite (5%)
Citric acid (5%)
Lactic acid (5%)
Acetic water (5%)
Potassium hydroxide (45%)
Salt water
Specimen Procedure:
? Prepare multiple specimens; at least 3 Specimens are typically used for each chemical. Make an extra set for Reference sample purpose.
? Take disposal glass cups having 30 mm diameter and fill the Styrene-Acrylic-Polyurethane (SAP) grout by weighing 25 grams material in to the glass. Then compact with spatula and tap the glass until top surface becomes smooth and even finish
? Ensure to maintain the specimen thickness approx. 6-8 mm.
? Make sure no pin holes present on the surface of specimen.
? Allow the specimens in air cure for 7 days at Room temperature.
? Remove the specimen carefully from the glass- You can cut the glass to take out the specimen.
? Again store them at the room temp for another 14 days to achieve the full curing (total 21 days curing).
Test Procedure
Once The specimens are well cured then subject them to chemicals immersion treatment:
? Specimens can be weighed and measured prior to contact with the chemical reagent
? Take the initial weight of the each specimen and note down (W1)
? Take750 ml of above mentioned chemicals in 3 glass beakers. Immerse the weighed specimen in separate Beakers containing the test chemicals
? To avoid evaporation of chemicals, the test beakers are sealed tightly with PE or Aluminum sheet, and either left at room temperature
? Remove the specimens from the beaker after 30 minutes, 24 hours and 7 days
? Wipe the specimen surface with Tissue paper or cloth and weigh the Specimen immediately ( W2)
? Rinse the specimens with water to remove any loose material and blotted dry. Then take the weight (W3).
Report the following:
? Weight difference – Yields loss (%) or Rate of chemical absorption (%)
? Physical appearance –Notice surface etching or severe staining
? Dimension of the specimen - Any changes in the size of specimen like swelling & Cracking
? Surface & Nature of the Styrene-Acrylic-Polyurethane (SAP) specimen -Soft or Hard (can also be assessed by Shore-A/Shored-D hardness with respect to the reference sample hardness)
Chemical Resistance of Styrene Acrylic Polyurethane System vs 2 binder systems.
S. No Chemcial Reagents Styrene-Acrylic-Polyurethane system- SAP Acrylic and PUD PUD and Carboxylated Styrene Acrylic and Styrene
1 Con. HCl 0 0 0.5 2
2 Con. H2SO4 1 1 1 1
3 2- Butoxy ethanol 0 0 1 1
4 Toluene 0 0 0 1
5 Sodium hypochlorite 0 0 0 0
6 Oxalic acid 0 0 0 0
7 Vinegar 0 0 0 0
8 Ethyl acetate 0 0 1 1
Average value 0.125 0.125 0.44 0.75
Note: Scale 0 Excellent Chemical resistance
Scale 5 Poor Chemical Resistance
Higher the average value, poor the chemical resistance performance
6) Stain Resistance Measurement of Styrene-Acrylic-Polyurethane (SAP) RTU Grout
This test procedure describes the method for measuring stain rating of Styrene-Acrylic-Polyurethane (SAP) grout surface to the various normal household staining agents. Staining is achieved by prolonged exposure of the Styrene-Acrylic-Polyurethane (SAP) grout surface to test solutions and dry staining agents. The Grout surfaces are visually evaluated after the staining agent has been cleaned off using a combination of cleaning procedures
This test method is designed to check the Styrene-Acrylic-Polyurethane (SAP) grout performance against stains at long exposure (approx. 24 hrs.)
Apparatus and Materials Required for Stain Testing:
? 1 inch (dia) x 1 inch (thickness) plastic cup/Moulds
? Spatula
? Styrene-Acrylic-Polyurethane (SAP) Grout- Bright white
? Small plastic cups/glass beakers.
? Sponge & Cotton cloth.
? Stain agents: The following staining agents were used for the stain resistance evaluation.
Coffee - 5 % solution in water
Cooking oil - as such
Turmeric - 5 % solution in water
Coca-cola - as such
Ketch-up - as such
Fountain pen Ink- as such
Grease - as such
Red wine - as such
Specimen Preparation for Stain Resistance Rating:
? Take Styrene-Acrylic-Polyurethane (SAP) grout (Bright white shade) and fill in 1 inch plastic mould cups- 8 nos (1 no for each Stain) & make one specimen for reference.
? Compact the material and level the top surface smoothly using spatula.
? Even surface finishing can be accomplished by flat edge spatula.
? Ensure the material is packed closely in the mould and free from air voids.
? After 48 hrs. cover the specimens with Paper/PE sheet to avoid dust accumulation over the surface.
? Allow the specimens in air cure for 21 days at Room temperature.
Stain Rating Procedure:
Test time intervals: 24 hours
Once the stain cookies/specimens attained its curing, subject them to the stain test
Make sure the surface on which the stain will be applied is clean, free from dust, unwanted defects, stains and markings
Apply 2 - 3 ml of staining materials on the Styrene-Acrylic-Polyurethane (SAP) grout surface using small spatula and spread to an approximately 10 mm diameter circular area. Take pictures if required. Leave the stained agents on the grout surface for 24 hours
Take picture before stain washing if required. Wipe each individual stained cookies with clean dry tissue paper or white cotton cloth. Wash the grout surface with water and sponge. Allow the surface to dry at room temperature.
Rate the degree of each individual stain by visual examination as per below classification. Examine the surface with naked eye, with spectacles if usually worn, at a distance of 25 to 30 cm. Daylight or artificial illumination is permitted, but direct sunlight shall be avoided. Staining shall only be reported when the pigment is visible. Oil /Lubricants stains can be reported by their degree of absorption. The rating has to be assessed for each stain specimen vs. Reference specimen.
Assessment of Results:
Very high stain : 5
Highly Stained : 4
Medium stained : 3
Light Stained : 2
Very light stained : 1
No Stain : 0
Stain Resistance of Styrene Acrylic Polyurethane System vs 2 binder systems.
S. No Stain Styrene-Acrylic-Polyurethane system- SAP Acrylic and PUD PUD and Carboxylated Styrene Acrylic and Styrene
1 Wine 1 2 2 3
2 turmeric 1 2 1 2
3 Ink 1 1 2 3
4 Coffee 0 1 0 0
5 Ketchup 0 0 1 1
6 Coke 0 0 0 0
7 Grease 0 0 0 0
8 Oil 0 0 0 0
Average value 0.375 0.75 0.75 1.125
Note: Scale 0 Excellent stain resistance
Scale 5 Poor stain Resistance
Higher the average value, poor the stain resistance performance
7) Modified Water Absorption Measurement of Styrene-Acrylic-Polyurethane (SAP) RTU Grout:
Preparation of Specimen:
Water absorption of Styrene-Acrylic-Polyurethane (SAP) grout can be estimated using the modified A 118.6/7 test method. Using Styrene-Acrylic-Polyurethane (SAP) RTU grout, fill 4 #s 1 in.*1 in. Cylindrical moulds (polyethylene or Teflon molds are acceptable). Before filling the grout material, apply the grout releasing agents inside the moulds. Specimens can be prepared by keeping a plastic PE sheets at the bottom applied with grout releasing agents.
Allow the sample to cure inside the laboratory conditions for 24 hrs. Transfer the sample to an oven with preset temperature range of 70±20C for 7 days (70±20C). After the 7 day curing, de-mould the samples and continue the curing at the 70±20C for additional 7 days (total 14 days) in the oven. After 14 days of curing inside the chamber, let the sample cure under the standard conditions (23±20C and 50±5% humidity) for additional 14 days (28 days).
After 28 day curing, weigh the samples (Wi) and keep the samples inside the container containing water having temperature 23±20C. Keep the samples for 24 hrs. After the testing period remove the specimens from water, pat them dry with a paper towel, and weigh them (Ws)
Calculate the water absorption, using the formula:
(Ws-Wi)/ (Wi)*100
Ws- Saturated weight, Wi– Initial weight
Although the foregoing description of the present invention has been shown and described with reference to particular embodiments and applications thereof, it has been presented for purposes of illustration and description and is not intended to be exhaustive or to limit the invention to the particular embodiments and applications disclosed. It will be apparent to those having ordinary skill in the art that a number of changes, modifications, variations, or alterations to the invention as described herein may be made, none of which depart from the spirit or scope of the present invention. The particular embodiments and applications were chosen and described to provide the best illustration of the principles of the invention and its practical application to thereby enable one of ordinary skill in the art to utilize the invention in various embodiments and with various modifications as are suited to the particular use contemplated. All such changes, modifications, variations, and alterations should therefore be seen as being within the scope of the present invention as determined by the appended claims when interpreted in accordance with the breadth to which they are fairly, legally, and equitably entitled.
| # | Name | Date |
|---|---|---|
| 1 | 201741033960-STATEMENT OF UNDERTAKING (FORM 3) [25-09-2017(online)].pdf | 2017-09-25 |
| 2 | 201741033960-REQUEST FOR EXAMINATION (FORM-18) [25-09-2017(online)].pdf | 2017-09-25 |
| 3 | 201741033960-POWER OF AUTHORITY [25-09-2017(online)].pdf | 2017-09-25 |
| 4 | 201741033960-FORM 18 [25-09-2017(online)].pdf | 2017-09-25 |
| 5 | 201741033960-FORM 1 [25-09-2017(online)].pdf | 2017-09-25 |
| 6 | 201741033960-FIGURE OF ABSTRACT [25-09-2017(online)].pdf | 2017-09-25 |
| 7 | 201741033960-DRAWINGS [25-09-2017(online)].pdf | 2017-09-25 |
| 8 | 201741033960-DECLARATION OF INVENTORSHIP (FORM 5) [25-09-2017(online)].pdf | 2017-09-25 |
| 9 | 201741033960-COMPLETE SPECIFICATION [25-09-2017(online)].pdf | 2017-09-25 |
| 10 | Correspondence by Agent_Form 1,Form 5,Power of Attorney_10-10-2017.pdf | 2017-10-10 |
| 11 | 201741033960-FER.pdf | 2019-06-21 |
| 12 | 201741033960-AbandonedLetter.pdf | 2019-12-26 |
| 1 | 201741033960SEARCH_12-06-2019.pdf |