NZ509527A

NZ509527A - Method of reducing fines in a powdered product and fabric cleaner produced therefrom

Info

Publication number: NZ509527A
Application number: NZ509527A
Authority: NZ
Inventors: Thomas Mikic; Heather Rae Schramm; Hans J Weitkuhn; Dolores T Rodriguez
Original assignee: S
Priority date: 1998-07-31
Filing date: 1999-07-28
Publication date: 2002-06-28
Also published as: JP2002521556A; ATE226243T1; CA2339169A1; KR20010071058A; AR018961A1; AU5233399A; EP1102835B1; BR9912615A; EP1102835A1; CA2339169C; ZA200101049B; WO2000006681A1; DE69903564D1; AU749030B2

Abstract

A particulate fabric cleaning composition that comprises: a) at least 80% by weight of inorganic salt carrier particulates, b) 1-10% by weight of flow agent particulates and c) 0.1-15% by weight of liquid selected from the group consisting of fragrances, surfactants, solvent, pesticides, and mixtures thereof, wherein at least 90% of the composition particulate have a particle size greater than 0.105 millimeters.

Description

<div class="application article clearfix" id="description"> New Zealand Paient Spedficaiion for Paient Number 509527 WO 00/06681 PCT/US99/16960 METHOD OF REDUCING FINES IN A POWDERED PRODUCT BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to methods of reducing fines in powdered products, and more particularly to a method of reducing fines in powdered textile treating compositions, and powdered textile treating compositions prepared by the method. 2. Description of the Related Art Household cleaning compositions are often supplied in a liquid or a powdered form. For example, carpet cleaning compositions have been widely available for some time in both liquid and powdered form. Liquid carpet cleaning compositions have typically been the first choice of many consumers. However, because of drawbacks in the liquid compositions, such as a tendency to cause shrinking, matting or wicking of carpet fibers, dry powdered carpet cleaning compositions have become quite popular. Examples of dry powdered carpet cleaning compositions can be found in U.S. Patent Nos. 4,666,940, 4,552,777, 4,493,781, 4,395,347 and 4,161,449. INTELLECTUAL PROPERTY OFFICE OF N.Z. 3 0 APR 2002 RECEIVED WO 00/06681 -2- PCT/US99/16960 However, dry carpet cleaners and certain other powdered household products have a tendency to lose their free flowing properties during storage. For instance, powdered products may become compacted or "caked" due to settling and/or their tendency for absorbing moisture from the ambient air. Caked product is difficult to fill as well as dispense from containers. Therefore, flow agents (also known as anti-caking agents) are often added to powdered compositions in order to keep the powder free flowing. Flow agents typically contain particles of small size and low density known as "fines" that can readily become airborne. Fines can be very irritating to nasal passages. In addition, a large number of fines in the ambient air can build up a static charge. In consumer products such as a dry powdered carpet cleaner, fines may be difficult to vacuum. Also, the fines that are removed may not remain trapped inside a typical paper vacuum cleaner bag. As a result, a dust cloud of fines may develop during vacuuming that can be irritating to the nasal passages. In addition, the fines may leave an unsightly residue on shoes, clothing and surfaces in the home. In the field of dry carpet cleaners, efforts at reducing fines have previously focussed on the incorporation of additional components into the cleaning formulation or the use of screening techniques. For instance, U.S. Patent Nos. 4,161,449 and 4,552,777 disclose a conventional process for preparing a dry carpet cleaning composition from dry WO 00/06681 -3- PCT/US99/16960 powdered components. These patents mention that a typical dry powdered carpet cleaning composition may include a dry powder inorganic salt carrier, a dry powder anti-caking agent, a liquid fragrance and a liquid dedusting agent. Typical inorganic salt carriers include sodium sulfate, sodium chloride, sodium carbonate, sodium bicarbonate, sodium borate, sodium citrate, sodium tripolyphosphate and sodium nitrate; suitable anti-caking agents include starch, silica powders, grain flours, wood flour, talc, pumice, clays, and calcium phosphates; conventional fragrances are liquid volatile odorous agents including essential oils and aromatic chemicals; and typical liquid dedusting agents may be alkyl phthalates, mineral oil, glycols, ethoxylated alcohols, alcohols, glycol ethers, vegetable oils, naphtha, mineral spirits and naphthalene sulfonates. In preparing a dry carpet cleaning composition in accordance with the prior methods described in U.S. Patent Nos. 4,161,449 and 4,552,777, (1) the dry powders, such as the carrier and the agglomerating agent, are dry blended in a first step, (2) the liquid components, such as the fragrance and any dedusting agent, are separately mixed together in a second step, (3) the mixtures prepared in steps (1) & (2) are admixed, and (4) if necessary, the final product is screened to remove undesirable lumps and fines. Therefore, it is apparent that the methods described in these patents rely on liquid dedusting agents and screening to control fines in the final dry carpet cleaning product. These extra ingredients (i.e., dedusting agents) or process WO 00/06681 -4- PCT/US99/16960 steps (i.e., screening) increase manufacturing costs, and in the case of screening, may call for measures to control the fines removed by screening. Thus, further advances are desired to provide a solution to the problem of fines. SUMMARY OF THE INVENTION It is envisioned that improved methods of blending and agglomerating powdered products can be used to reduce fines in a final powdered product without the need for dedusting agents or screening techniques. Accordingly, these improved methods can be used to produce a particulate textile fiber or fabric cleaning composition that satisfies the need for a dry textile cleaning composition that has a minimal level of fines. Agglomeration is the process of bringing together fine powders or particulates into larger masses with pressure, agitation and/or other mechanisms. Agglomerating techniques include: (1) pressure compacting, such as briquetting, tableting and using a pellet mill; (2) tumbling or granulation; and (3) spray congealing. In the context of dry powdered or particulate household cleaning chemicals, tumbling or granulation is typically the process of choice. A method is disclosed for producing a particulate textile fiber or fabric cleaning composition that includes the steps of introducing at least one particulate material into a mixing vessel, introducing at least one liquid ) material into the mixing vessel to form a mixture, blending the mixture for a first time period, chopping the mixture for at least a portion of the first time period, and thereafter blending the mixture without chopping for a second time period. The method produces a particulate fabric cleaning composition having acceptable flow characteristics yet results in a reduced level of fines without the need for a screening step to remove fines. For the purposes of this patent, fabric includes natural and/or synthetic fiber products such as carpets, upholstery, drapes, and even clothing. Without intending to be bound by theory, at is believed that chopping creates greater surface area (which is otherwise lessened by mixing liquid with solids} and that the greater area permits fine particles of the particulate materials (such as silica fines in a dry carpet cleaning composition) to become attached to the larger particles in the mix by agglomeration. Note that this is surprising as chopping might have been expected to increase dust/fines. Also, in the method of the present invention, the inclusion of a time period of blending and chopping the mixture serves to agglomerate particles and at the same time break up any large agglomerated particles that might clog the container. In other words, the blending serves to agglomerate smaller particles while the chopping serves to breakup larger oversized agglomerations. This helps to distribute any liquid materials and to create additional exposed sticky surfaces to which fines may attach. It is particularly desirable to reduce particles in the size range of 200 mesh (0.074 mm opening) and finer. INTELLECTUAL PROPERTY OFFICE OF N.Z. 3 0 APR 2002 RECEIVED 20 The chopping process is a high shear mixing that generally shears large agglomerated particles at the liquid interface between particles. However, individual particles may shear through the particle body- Therefore, as used herein, the term " chopping" refers to an action that can shear particle agglomerations at a liquid-solid interface or a solid-solid interface. The step of introducing liquid material into the mixing vessel and the step of blending and chopping the mixture for a first period of time may all be performed simultaneously. Although the liquid material may be added to the mixing vessel in any manner, it is preferred that the liquid materials be introduced into the mixing vessel at a uniform flow rate, most preferably by a sprayer that provides a spray in order to produce a uniform powder. As used herein, the term u acceptable flow characteristics" for a fabric cleaner means that the composition may be dispensed without clogging from conventional shaker-type containers that are widely used for packaging household cleaning compositions and have outlets of about 5 millimeters in diameter. One version of a particulate textile fiber or fabric cleaning composition produced in accordance with the invention includes at least 80% by weight of inorganic salt carrier particulates, 1-10% by weight of flow agent particulates, and 0.1-15* by weight of a liquid active material selected from fragrances, surfactants, solvents, pesticides, and mixtures thereof. For example, the liquid may comprise 1-10% by weight of an acaricidal agent. Other standard fabric cleaner additives may also be included. 7 ^ f) 6 o i At least 9 0% of the composition particulates have a particle size greater than 0.105 millimeters. The composition may be applied without dusting to natural or synthetic textile fibers or fabric and 5 removed by vacuuming. Disclosed but not claimed is a method for preparing a dry particulate fabric cleaning composition that has a level of fines lower than ^ dry particulate fabric cleaning compositions typically 10 produced by conventional methods. Further disclosed but not claimed is a method of reducing the fines in a particulate fabric cleaning composition .produced by agglomeration techniques without the need for dedusting agents or 15 screening techniques. Yet further disclosed but not claimed is a a method for preparing a dry fabric cleaning composition that reduces the amount of fines that can become airborne during manufacturing and use, and that maintains 20 the de3ired flow, fragrancing and/or active delivery properties of the cleaning composition. It is an object of the present invention to go some way towards providing a particulate fabric cleaning composition prepared from particulate and liquid materials that has a low level of fines that can become airborne during use, and that has the desired flow properties of a particulate textile fiber or fabric cleaning composition and/or to provide the public with a useful choice. intellectual PROPER OFFICE OF N.Z. 3 0 APR 2002 RECEIVED 25 WO 00/06681 PCT/US99/16960 -8- These and other objects and advantages of the present invention will be apparent from the description which follows. The description is merely of the preferred embodiments. To evaluate the full scope of the invention, the claims should be reviewed. DETAILED DESCRIPTION OF THE INVENTION The compositions of the invention are particularly and beneficially adapted for use in the cleansing of pile fabrics of the type knitted or woven principally into yarns or fibers. The compositions are believed most useful in the treatment of rugs and carpets. The formed textile fabric may be of vegetable, synthetic or animal origin, including mixtures thereof. Typical synthetic fabrics which may be beneficially treated by the present composition include viscose rayon, acetate rayon, polyamide, polyester polyolefin and acrylic. Other fibers of a vegetable or animal origin which can be treated include cotton, jute, ramie, wool and the like. The compositions of the present invention may also be designed for maintaining textile fabrics by including vacuuming aids. In practice, the cleaning composition is applied to the surface, allowed to stand (e.g. a few minutes to a few hours) and thereafter removed by vacuuming or the like. The composition may be applied to the carpet by sprinkling from a shaker type container or through the use of any conventional particulate dispensing means. The term " liquid active material" preferably designates a material that provides active properties to a WO 00/06681 PCT/US99/16960 -9- particulate textile fiber or fabric cleaning composition. For example, the liquid active material used in the textile fiber or fabric cleaning composition may be a fragrance for odor control, a surfactant for cleaning, a solvent for cleaning, or a pesticide for pest control, such as an acaricide for control of mites and ticks. The liquid active materials may be: (1) a fragrance, such as a liquid volatile odorous agent including essential oils and aromatic chemicals; (2) a solvent suitable for cleaning textile fibers, such as an ether alcohol (e.g., ethylene glycol monomethyl ether); (3) a surfactant or surfactant mixture suitable for cleaning textile fibers selected from any of the four basic groups of surface active agents including anionic (such as alkali metal salts of sulfate esters or sulfonates containing higher aliphatic hydrocarbon radicals of 8 or more carbon atoms), non-ionic (such as polyethylene oxide condensates of aliphatic alcohols having 8 or more carbon atoms), cationic (such as quaternary ammonium compounds), and amphoteric (such as tertiary amine oxide salts having a hydrophobic radical attached to the nitrogen atom); (4) an acaricide, such as benzyl benzoate; or (5) mixtures of any of the above listed liquid active materials. In the particulate textile fiber or fabric cleaning composition of the present invention, suitable particulate carriers are inorganic salt carriers such as sodium sulfate, sodium chloride, sodium carbonate, sodium bicarbonate, sodium borate, sodium citrate, sodium tripolyphosphate, sodium nicrate and mixtures thereof. Suitable flow agents include silica, metal oxides such as alumina, and metal ticanacee. One version of a particulate fabric cleaning composition made m accordance with the present invention includes at least 80% by weight of inorganic salt carrier particulates, 1-10% by weight of flow agent particulates, and Q.l-15% by weight of liquids selected from the group consisting of fragrances, surfactants, solvents, pesticides, and mixtures thereof, wherein at least 90% of the composition particulates have a particle size greater than 0.105 millimeters. A preferred version is as hereinafter set forth in claim 10. Also disclosed but not claimed is a method for producing a fabric cleaning composition that includes che steps of introducing at least one particulate material into a mixing vessel, introducing at least one liquid material into the mixing vessel to form a mixture, blending the mixture for a first time period, chopping the mixture for at least a portion of the first time period, and thereafter blending the mixture without chopping for a second time period, wherein at least 90% of the resulting composition is particulates having a particle size greater than o.105 millimeters. An exemplary embodiment of the most preferred version of the composition is produced by: (1) adding 71 vt% sodium sulfate, 20 wt% sodiurr. bicarbonate and 4 wt% hydrated amorphous silica to a ribbon blender having chopper blades; (2) adding a combination of 4.6 wt% liquid benzyl benzoate INTELLECTUAL PROPERTY OFFICE OF N.Z. 3 0 APR 2002 RECEIVED WO 00/06681 PCT/US99/16960 -11- and 0.4 wt% liquid fragrance to the blender while mixing; (3) mixing with ribbons for a total of 2 minutes (or longer if needed to complete the transfer of liquid to the product); (4) mixing with ribbons and high speed chopper blades for 2.5 minutes; (5) turning off the chopper blades and continuing to mix with ribbons for 5.5 more minutes; (6) mixing with chopper blades and ribbons for 0.5 minutes; and (7) turning off the chopper blades and continuing to mix with ribbons for 5 minutes. In certain circumstances, mix times may be extended to accommodate raw materials with more fines. If necessary, a mix and chop step may be run for 1 minute, and then a mix step may be run for two minutes. These extra steps may be repeated as needed. However, it is preferred that every mix and chop step be followed by a blending step without chopping so that any fines generated by the chopping process can be allowed to agglomerate in the further mixing step. It is should noted that this specific embodiment and the Examples that follow are illustrative in nature and should not be used to limit the scope of the invention. The process can be facilitated by use of a paddle mixer equipped with high speed flat or tulip chopper blades or a ribbon blender equipped with high speed flat or tulip chopper blades. One suitable paddle-type mixer is a " Marion" brand paddle mixer equipped with a chopper, and is available from Marion Mixer Company, Marion, Iowa, USA. A suitable ribbon blender has a horizontal 'U' shaped concainer complete with agitator ribbons and chopper blades, and is available from American Process Systems, Gurnee, Illinois, USA, The inner and outer ribbons operate in opposite directions to provide an even movement of material and effect a homogeneous friend. The paddle mixer or ribbon blender motors should be sized appropriately for the density of the final dry carpet cleaning formulation. Suitable mixers or blenders include: (1) a 1.7m3 (60 cubic foot) capacity unit with a 75 horsepower main motor and four 20 horsepower chopper blades; and (2) a 2.83 m3 (100 cubic foot) unit with a 100 horsepower main motor and four 20 horsepower chopper blades. All process equipment (including blender, chopping blades and filling equipment) are preferably clean and dry before starting the process, as water as may adversely affect the product. gyaluc^ioii The level of particle agglomeration was evaluated using a * Shake and smoke" test and a sieve test. In the n Shake and Smoke" test, approximately 113.4g (4 ounces) of material were placed in an 226.8g (8 ounce) glass jar and the jar is sealed. The jar is then shaken vigorously by hand. The jar is opened immediately and observed to determine whether any dust particles rise out of the container (i.e., the material " smokes" ) . The * Shake and Smoke" test evaluates the dustiness of a product.. In the sieve test, particle size distributions are identified using standard-sized sieves. One suitable sieve tescer as a CSC Scientific Sieve Shaker Catalog No. 18480. INTELLECTUAL PROPERTY OFFICE OF N.Z. 3 0 APR 2002 RECEIVED A typical sieve test involves loading 100 grams of sample into the sieve tester and using U.S. Standard Sieve sizes 20 (0.84mm opening), 40(0.42mm), 60 (0.25mm), 80 (0.177mm), 100 (0.149mm), 120 (0.125mm), 140 (0.105mm), 170 (0.088mm), 200 (0.074mm), and 230 (0.062mm) to separate the particles by size. Example l A dry carpet cleaning composition was prepared using the following ingredients: Inm-ftdienr. Weight Kg (lbs.) Vic. % SODIUM SULFATE, ANHYDROUS (Carrier) 96.6 (213.0) 71,00 SODIUM BICARBONATE, COARSE GRANULAR (Carrier)27.2 (60.0) 20-00 amu BEUZOATE (Acaricide) 5.4 (12.0) 4.60 SILICA,. HVPRATEO AMORPHOUS (Flaw agent) 6.3 (13.8) 4.00 FRAGRANCE [Fragrance RS 1907/A manufactured 0.54 (1.2) 0,40 fry TftkfrpaaQ ..TPceH*flK fonf1 c°TF, > 136.04 (300.00) 100.00 In preparing the dry carpet cleaning composition, the dry ingredients (sodium sulfate, sodium bicarbonate and silica) were added to a ribbon blender, such as the ribbon blender described above. The benzyl benzoate was inspected for visible evidence of crystallization, as it is preferred that the benzyl benzoate be completely liquid. If needed, the temperature of the benzyl bensoate way be raised to 75° + 5°F (23°± 2°C) to reverse any crystallization. The liquid fragrance and the benzyl benzoate were then mixed together and poured over the dry ingredients in the ribbon blender. The ingredients were then mixed in the ribbon blender in the following sequence: (l) 2 minuses of ribbon blending; (2) 2.5 minutes of ribbon blending with chopper blades turned on? (3) 5.5 minutes of ribbon blending; (4) 0.5 minutes of ribbon blending with chopper intellectual PROPERTY OFFICE OF N.Z. 3 0 APR 2002 WO 00/06681 PCT/US99/16960 -14- blades turned on; and (5) 5 minutes of ribbon blending. The dry powdered carpet composition produced by this method was evaluated using the " Shake and Smoke" test described above, and no " smoking" was evident. Example 2 In an alternative, the sodium sulfate and sodium bicarbonate were charged to the ribbon blender and subjected to 4 minutes of ribbon blending. The liquid ingredients (benzyl benzoate and fragrance) were mixed together and applied to the sodium sulfate and sodium bicarbonate as a spray mist using a pressurized spray vessel with fine conical-style nozzles while all of the ingredients were subjected to 3 minutes of ribbon blending. The ingredients were then subjected to 1 minute of ribbon blending with chopper blades turned on. The silica was then added to the ribbon blender and the ingredients were subjected to 3 minutes of ribbon blending with chopper blades turned on. The ingredients in the ribbon blender were then subjected to 5 minutes of ribbon blending. A sample was obtained from the blender and it was discovered by visual inspection that adding the liquid ingredients through a spray device produced a more homogenous mixture than the mixture of Example 1. Example 3 A carpet cleaning composition was prepared using the ingredients listed in Example 1 and another method of blending and agglomerating the ingredients. WO 00/06681 -15- PCT/U S99/16960 The dry ingredients (sodium sulfate, sodium bicarbonate and silica) were fxrst added to the ribbon blender and then the liquid ingredients (benzyl benzoate and fragrance) were mixed together and sprayed over the dry ingredients in the ribbon blender while ribbon blending. The spray was a uniform, coarse spray from a planar fan-style nozzle. The ingredients were mixed in the ribbon blender in the following sequence: (1) 2 minutes of ribbon blending during application of the liquid spray; (2) 2.5 minutes of ribbon blending with chopper blades turned on; (3) 5.5 minutes of ribbon blending; (4) 0.5 minutes of ribbon blending with chopper blades turned on; and (5) 5 minutes of ribbon blending. The dry powdered carpet composition produced by this method was evaluated using the " Shake and Smoke" test described above after 10, 10.5, 13.0 and 15.5 minutes of blending according to the blending sequence. The " Shake and Smoke" test produced the following results: (1) after 10 minutes of blending (which included 2.5 minutes of chopping beginning after two minutes), the " smoking" of the composition began to disappear; (2) after 10.5 minutes of blending, the " smoking" of the composition reappeared as a result of the chopping process; and (3) after 13 and 15.5 minutes of blending, the " smoking" of the composition had disappeared. Agglomeration of the powder was acceptable after 10 minutes. This example shows that application of the liquid ingredients in a coarse spray, rather than a mist, decreases 11 11 WO 00/06681 PCT/US99/16960 -16- g. che level of fines much more significantly^ ^^d^i'tion, the use of a process that includes che alternate steps of a blending for a first time period, chopping for a portion of the first time period, and thereafter blending for a second time period results in a carpet cleaning composition with a low level of fines as measured by che * Shake and Smoke" test. Example 4 A batch of dry carpet cleaner was prepared using the ingredients of Example 1 and the following sequence of steps. The dry ingredients (sodium sulfate, sodium bicarbonate and silica) were first added to the ribbon blender and then the liquid ingredients (benzyl benzoate and fragrance) were mixed together and sprayed over the dry ingredients in the ribbon blender while ribbon blending. The spray was a uniform, coarse spray from a planar fan-style no2zle. The ingredients were mixed in the ribbon blender in the following sequence; (1) 2 minutes of ribbon blending during application of the liquid spray, which took 50 seconds at 103.4 kPa (15 psi); (2) 2.5 minutes of ribbon blending with.chopper blades turned on; (3) 5.5 minutes of ribbon blending; (4) 0.5 minutes of ribbon blending with chopper blades turned on; and (5) 5 minutes of ribbon blending. Samples of the dry powdered carpet composition were taken from the blender after 10, 11, 3,1.5 and 15.5 minutes of blending according to the blending sequence. The samples were evaluated using the sieve test described above, i.e. 100 grams of each sample INTELLECTUAL PROPERTY OFFICE OF N.Z. 3 0 APR 2002 RECEIVED WO 00/06681 PCT/US99/16960 -17- were placed into the sieve tester and separated by size using U.S. Standard Sieve sizes 2 0 (0.84 millimeter opening), 40 (0.42 mm. opening), 60 (0.25 mm.), 80 (0.177 mm.), 100 (0.149 mm.), 120 (0.125 mm.), 140 (0.105 mm.), 170 5 (0.088 mm.), 200 (0.074 mm.), and 230 (0.062 mm.). The results were as follows: TABLE I Grams of Sample Retained by Sieve US Standard Sieve Size Blend/Chop Time (minutes) 10 11 11.5 15.5 20 (0.84 mm) 0.0 0.0 0.0 0.1 40 (0.42 mm) 0.1 0.0 0.1 0.2 60 (0.25 mm) 19.6 24 . 6 22 .2 33.0 80 (0.177 mm) 47.1 45.8 55.0 46.4 100 (0.149 mm) 14 . 9 12 .3 9.2 16.4 120 (0.125 mm) 7.0 5.5 5.4 3.4 140 (0.105 mm) 4 . 8 4.2 3.3 0.4 170 (0.088 mm) 3.2 3.6 2 . 8 0.0 200 (0.074 mm) 1.9 2.4 1.4 0.0 230 (0.062 mm) 1.1 1.5 0.5 0.0 Pan 0.7 1.2 0.1 0.0 10 Looking at Table I, it can be seen that the level of fines (as defined by particles passing through the 170 sieve) varies depending on the stage of the blending/chopping process. For example: (1) after 10 minutes of blending/chopping according to the blending 15 sequence (i.e., 2 minutes of ribbon blending, 2.5 minutes of ribbon blending with chopping, and 5.5 minutes of ribbon WO 00/06681 -18- PCT/US99/16960 blending), 3.7 grams of the composition passed through the 170 sieve; (2) after 11 minutes of blending/chopping (i.e., 2 minutes of ribbon blending, 2.5 minutes of ribbon blending with chopping, 5.5 minutes of ribbon blending, 0.5 minutes of ribbon blending with chopping, and 0.5 minutes of ribbon blending), 5.1 grams of the composition passed through the 170 sieve; (3) after 11.5 minutes of blending/chopping (i.e., 2 minutes of ribbon blending, 2.5 minutes of ribbon blending with chopping, 5.5 minutes of ribbon blending, 0.5 minutes of ribbon blending with chopping, and 1 minute of ribbon blending), 2.0 grams of the composition passed through the 170 sieve; and (4) after 15.5 minutes of blending/chopping (i.e., 2 minutes of ribbon blending, 2.5 minutes of ribbon blending with chopping, 5.5 minutes of ribbon blending, 0.5 minutes of ribbon blending with chopping, and 5 minutes of ribbon blending), 0.0 grams of the composition passed through the 170 sieve. Without intending to be bound by theory, the variation in the level of fines throughout the blending/chopping process can likely be explained as follows. After 10 minutes of blending/chopping according to the blending sequence, the method of the present invention produces a composition having an acceptable level of fines as demonstrated by the " Shake and Smoke" test performed in Example 3 above. The level of fines (as defined by particles passing through the 170 sieve) was 3.7% (3.7 grams for a 100 gram sample) after 10 minutes. In the first 10 WO 00/06681 -19- PCT/US99/16960 minutes of the blending sequence, the ingredients are subjected to blending, blending with chopping, and blending. After 11 minutes of blending/chopping according to the blending sequence, the level of fines (as defined by particles passing through the 170 sieve) rose to 5.1%. This indicates that the 0.5 minute period of blending and chopping after the first 10 minutes of blending and chopping serves to break up large agglomerations and,free up fines. After 11.5 minutes of blending/chopping according to the blending sequence, the level of fines (as defined by particles passing through the 170 sieve) decreased to 2.0%. This indicates that the use of a blending/chopping step and a blending step after the initial 10 minutes of the blending/chopping sequence serves to further lower the level of fines in the composition. After 15.5 minutes of the blending/chopping sequence, the fines have been effectively eliminated. The data in the above table also indicates that the carpet cleaning powder produced in the examples will be free flowing powders that are acceptable for dispensing in shaker-type containers used in the carpet cleaning field. In addition, the carpet cleaning powder will have reduced level of fines. Referring to Table I, it can be seen that: after 10 minutes of blending/chopping according to the blending sequence, 93.5% of the particles have a particle size greater than 0.105 millimeters; after 11.5 minutes, 95.2% of the particles have a particle size greater than 0.105 WO 00/06681 PCT/US99/16960 -20- millimeters, and 91.9% of the particles have a particle size greater than 0.125 millimeters; and after 15.5 minutes, 99.9% of the particles have a particle size greater than 0.105 millimeters, 99.5% of the particles have a particle size greater than 0.125 millimeters, and 96.1% of the particles have a particle size greater than 0.149 millimeters. At each of these time periods, substantially all of the particles have a particle size less than 0.42 millimeters. The method produces a particulate carpet cleaning product having a low level of fines as measured by the sieve test, but at the same avoids producing a carpet cleaning product with large agglomerations that hinder dispensing from shaker-type containers used in the field. Example 5 A batch of dry carpet cleaner was prepared using the ingredients of Example 1 and the following sequence of steps. The dry ingredients (sodium sulfate, sodium bicarbonate and silica) were first added to the ribbon blender and then the liquid ingredients (benzyl benzoate and fragrance) were mixed together and sprayed over the dry ingredients in the ribbon blender while ribbon blending. The spray was a coarse spray from a planar fan-style nozzle. The ingredients were mixed in the ribbon blender in the following sequence: (1) 2 minutes of ribbon blending during application of the liquid spray; (2) 3.5 minutes of ribbon blending with chopper blades turned on; and (3) 2 0.5 minutes of ribbon blending. Samples of the dry powdered carpet </div>

Claims

<div class="application article clearfix printTableText" id="claims"> WO 00/06681 PCT/US99/16960 -21- coraposition were taken from the blender after blending and evaluated using " Shake and Smoke" test described above. After blending, no " smoking" of the composition could be detected. This indicates that the use of another process 5 that includes the alternate steps of a blending, a blending with chopping, and a blending results m a carpet cleaning composition with a low level of fines as measured by the w Shake and Smoke" test. INDUSTRIAL APPLICABILITY 10 The method of the present invention may be readily utilized with currently known filling techniques and production equipment for granular or powdered treating compositions. In addition, carpet cleaning compositions produced by the present method may be applied to a carpet by 15 sprinkling from a shaker type container or through the use of any conventional particulate dispensing means. Other modifications and variations of the present invention will become apparent to those skilled in the art from an examination of the above specification. Therefore, 20 other variations of the present invention may be made even though such variations were not specifically discussed above. WO 00/06681 -22- PCT/US99/16960 CLAIMS We claim:

1. A particulate fabric cleaning composition comprising: at least 80% by weight of inorganic salt carrier particulates; 1-10% by weight of flow agent particulates; and 0.1-15% by weight of liquid selected from the group consisting of fragrances, surfactants, solvents, pesticides, and mixtures thereof, wherein at least 90% of the composition particulates have a particle size greater than 0.105 millimeters.

2. The composition of claim 1 wherein: at least 95% of the composition particulates have a particle size greater than 0.105 millimeters.

3. The composition of claim 1 wherein: at least 99% of the composition particulates have a particle size greater than 0.105 millimeters.

4. The composition of claim 1 wherein: at least 90% of the composition particulates have a particle size greater than 0.125 millimeters.

5. The composition of claim 1 wherein: at least 99% of the composition particulates have a particle size greater than 0.125 millimeters. WO 00/06681 -23- PCT/US99/16960 (

6. The composition of claim 1 wherein: the liquid comprises 1-10% by weight of an acaricidal agent. 5

7. The composition of claim 6 wherein: the acaricidal agent is benzyl benzoate.

8. The composition of claim 1 wherein: 10 the flow agent particulates comprise silica.

9. The composition of claim 1 wherein: the inorganic salt carrier particulates are selected from the group consisting of sodium sulfate, sodium 15 bicarbonate, and mixtures thereof.

10. A powdered carpet cleaner comprising: at least 8 0% by weight of inorganic salt carrier particulates selected from the group consisting of sodium I 20 sulfate, sodium chloride, sodium carbonate, sodium bicarbonate, sodium borate, sodium citrate, sodium tripolyphosphate, sodium nitrate and mixtures thereof; 1-10% by weight of silica; 1-10% by weight of benzyl benzoate; and 25 0.1-5% by weight of a fragrance, wherein at least 90% of the composition particulates have a particle size greater than 0.105 millimeters. WO 00/06681 5f PCT/US99/16960 -24-

11. The composition of claim 10 wherein: at least 99% of the composition particulates have a particle size greater than 0.105 millimeters and less than 0.42 millimeters.

12. The composition of claim 10 wherein: at least 99% of the composition particulates have a particle size greater than 0.125 millimeters and less than 0.42 millimeters. / / INTELLECTUAL PROPERTY OFFICE OF N.Z. 3 0 APR 2002 1TECEIVED </div>