Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
  • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads

Definitions

• the present invention relates to a process for making an improved granular detergent composition which has superior solubility, especially m cold temperature launde ⁇ ng solutions (i.e., less than about 30°C), excellent flowability, aesthetics or appearance and friability.
• this clumping phenomenon can contribute to the incomplete dispensing of detergent in washing machines equipped with dispenser drawers or in other dispensing devices, such as a granulette.
• the undesired result is undissolved detergent residue in the dispensing device.
• inorganic salts In addition to the viscous surfactant "bridging" effect, inorganic salts have a tendency to hydrate which can also cause “bridging” of particles which linked together via hydration. In particular, inorganic salts hydrate with one another to form a cage structure which exhibits poor dissolution and ultimately ends up as a "clump" after the washing cycle. It would therefore be desirable to have a detergent composition which does not expe ⁇ ence the dissolution problems identified above so as to result in improved cleaning performance.
• the prior art is replete with disclosures addressing the dissolution problems associated with granular detergent compositions. For example, the prior art suggests limiting the use and manner of inorganic salts which can cause clumps via the "bridging" of hydrated salts du ⁇ ng the laundering cycle.
• the first type of process involves spray-drymg an aqueous detergent slurry m a spray-drymg tower to produce highly porous detergent granules (e.g., tower process for low density detergent compositions).
• the va ⁇ ous detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant, to produce high density detergent compositions (e.g., agglomeration process for high density detergent compositions).
• a binder such as a nonionic or anionic surfactant
• the invention meets the needs above by providing a process for making a detergent composition which has improved solubility or dissolution m laundering solutions, especially m solutions kept at cold temperatures (i.e., less than about 30°C), is aesthetically pleasing to consumers and has improved flowabihty.
• a process is provided to form a granular detergent composition with improved solubility, aesthetics and flowabihty: mixing at least two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray d ⁇ ed granules, and detergent adjunct ingredients m a high-speed, low-speed, or a moderate-speed mixer, and various combinations of such mixers to form particles, wherein the granular detergent composition has at least about 50% by weight of particles having a geometric mean particle diameter of from about 500 microns to about 1500 microns with a geometric standard deviation of from about 1 to about 2.
• mixtures is meant to include a simple combination of mate ⁇ als and any compounds that may result from their combination.
• cold water means water which has at a temperature of below 30°C.
• density or “bulk density” refers to the uncompressed, untapped powder bulk density, as measured by pou ⁇ ng an excess of powder sample through a funnel into a smooth metal vessel (e.g., a 500 ml volume cylinder), scraping off the excess from the heap above the ⁇ m of the vessel, measuring the remaining mass of powder and dividing the mass by the volume of the vessel
• a smooth metal vessel e.g., a 500 ml volume cylinder
• ambient is defined as the temperature and humidity of the environment.
• particles means the entire size range of a detergent final product or component or the entire size range of discrete particles, agglomerates, or granules in a final detergent product or component admixture. It specifically does not refer to a size fraction
• the size fraction represents 100% of a discrete particle in an admixture of particles.
• the entire size range of discrete particles of that type have the same or substantially similar composition regardless of whether the particles are m contact with other particles.
• the agglomerates themselves are considered as discrete particles and each discrete particle may be comprised of a composite of smaller primary particles and binder compositions.
• the phrase "geomet ⁇ c mean particle diameter" means the geometric mass median diameter of a set of discrete particles as measured by any standard mass-based particle size measurement technique, preferably by dry sieving.
• the phrase "geometric standard deviation" or “span” of a particle size dist ⁇ bution means the geometric breadth of the best-fitted log-normal function to the above-mentioned particle size data which can be accomplished by the ratio of the diameter of the 84.13 percentile divided by the diameter of the 50 th percentile of the cumulative distribution (D 8 - 3 D 50 ); See Gotoh et al, Powder Technology Handbook, pp. 6-11, Meral Dekker 1997
• builder means any inorganic mate ⁇ al having “builder” performance the detergency context, and specifically, organic or inorganic material capable of removing water hardness from washing solutions
• the present invention is directed to a process which produces a granular detergent composition having at least about 50% by weight of particles having a geometric mean particle diameter of from about 500 microns to about 1500 microns with a geometric standard deviation of from about 1 to about 2
• the present invention is directed towards a process for making a granular detergent composition
• a process for making a granular detergent composition comprising the step of mixing at least two mate ⁇ als selected from the group consisting of dry agglomerates, wet agglomerates, spray d ⁇ ed granules, and detergent adjunct ingredients to form particles, wherein the granular detergent composition comp ⁇ ses at least about 50% by weight of particles having a geomet ⁇ c mean particle diameter of from about 500 microns to about 1500 microns with a geometric standard deviation of from about 1 to about 2.
• At least two materials selected from the following group are added to at least one mixer: dry agglomerates, wet agglomerates, spray dried granules, and detergent adjunct ingredients
• dry agglomerates dry agglomerates
• wet agglomerates wet agglomerates
• spray dried granules and detergent adjunct ingredients
• detergent adjunct ingredients any recycled fines generated could also be added to the mixer
• Wet agglomerates include those particles that are manufactured via a granulation type process wherein detergent adjunct ingredients such as described below are admixed with a liquid binder material such as surfactant or a precursor thereof in at least one mixer to form granules of detergent materials. These particles are known as “wet agglomerates” until dried and as “dry agglomerates” upon exiting a drying stage, and optionally other conditioning stages such as sizing, grinding and cooling.
• Binders include but are not limited to water, anionic surfactants and their precursors, nonionic surfactants, cationic surfactants, polyethylene glycol, polyvmyl pyrro done, polyacrylates, citric acid, and mixtures thereof.
• Spray dried granules include those particles which are manufactured via a conventional spray-drymg technique wherein a slurry of detergent materials is prepared and sprayed downward into an upwardly flowing stream of gas to dry the particles A dry, free flowing mate ⁇ al is produced from the process
• the slurry is passed to a tower where the slurry is sprayed into a stream of air at temperatures ranging from about 175°C to about 450°C to dry the detergent slurry and form detergent particles.
• resultant densities of these particles range from about 200 to about 650 g/1.
• Detergent adjunct ingredients include but are not limited to, carbonates, phosphates, sulfates, zeolites, or the like.
• a list of detergent components which can be used as a detergent adjunct ingredient is desc ⁇ bed m detail below. Of course other conventionally known ingredients may be included as well.
• the mixer contains two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray dried granules, and detergent adjunct ingredients, at a ratio ranging from about 5:95 to about 95:5, more preferably at a ratio ranging from about 10:90 to about 90:10, and even more preferably from about 30:70 to about 70:30.
• At least two types of matenals selected from the group are fed into at least one mixer for agglomeration.
• the at least two types of matenals can be fed into at least one pre -mixer (e.g. a conventional screw extruder, including a twm-screw extruder or other similar mixer) prior to agglomeration in at least one mixer, after which the mixed matenals are fed into the initial mixer as desc ⁇ bed herein.
• the agglomeration step can be earned initially m at least one high-speed mixer, a moderate-speed mixer, a low-speed mixer, and combinations of mixers thereof.
• the same type of mixer can be used in a series, or in any combination with the other types of mixers, which may also be m a se ⁇ es
• the process can be batch or continuous.
• two or more mixers can be used in series and/or in parallel, for example to accommodate thoroughput.
• one embodiment of the process of the present invention may include mixing at least two materials from the group in at least one high-speed mixer, followed by at least one moderate-speed mixer, with optionally a conditioning step in a fluid bed granulator.
• mixing may take place m at least one high-speed mixer, followed by at least one moderate-speed mixer, followed by at least one high-speed mixer, followed by a conditioning step in at least one conditioning apparatus, such as a fluid bed granulator.
• the same mixture is mixed in a high-speed mixer after the initial mixing in a moderate-speed mixer, before being conditioned.
• a high-speed mixer the mean residence time is from about 0.1 to 60 seconds, more preferably from about 0.1 to about 30 seconds, even more preferably 0.1 to about 15 seconds.
• Other preferred conditions of the high-speed mixer include from about 3 to 90 m/s of tip speed, and more preferably from about 10 to 70 m/s of tip speed, and from about 0.005 W/kg to 100 W/kg of power draw, more preferably from about 0.05 W/kg to 80 W/kg of power draw.
• choppers can be used inside the mixer to break up undesirable oversized particles at an rpm of from about 0 to 5000 ipm, more preferably from about 100 to 3000 ⁇ m.
• the wall temperature is from ambient to about 80°C and the spacing between the mixer elements and the wall is from about 0.1 cm to 25 cm.
• Examples of a high-speed mixer having a mean residence time of from about 0.1 to about 60 seconds are Lodige Recycler CB 30TM, by Lodige Company, or mixers made by Drais, Schugi, or a similar brand mixer.
• the mean residence time is from about 30 to 1800 seconds, more preferably from about 30 to about 1200 seconds, more preferably from about 30 to about 600 seconds.
• Other preferred conditions of the moderate-speed mixer include from about 0.1 to 30 m s of tip speed, and more preferably from about 1 to 25 m/s of tip speed, and from about 5 W/kg to 1000 W/kg of power draw, more preferably from about 20 W/kg to 500 W/kg of power draw.
• choppers can be used inside the mixer to break up undesirable oversized particles at an rpm of from about 0 to 5000 rpm, more preferably from about 100 to 4000 ⁇ m.
• the wall temperature is from about -20°C to about 80°C and the spacing between the mixer elements and the wall is from about 0.1 cm to 25 cm.
• a moderate-speed mixer having a mean residence time of from about 30 to about 1800 seconds are Lodige Recycler KM "Ploughshare" 300TM and 600TM, by Lodige Company, the Drais K-T 160TM mixer, or mixers made by Fukae.
• the Lodige KM "Ploughshare" 600TM moderate-speed mixer is a particularly preferred mixer, which comprises a horizontal, hollow static cylinder having a centrally mounted rotating shaft around which several plough-shaped blades are attached.
• the shaft rotates at a speed of from about 15 ⁇ m to about 140 ⁇ m, more preferably from about 80 ⁇ m to about 120 ⁇ m.
• the grinding or pulverizing is accomplished by cutters, generally smaller in size that the rotating shaft, which preferably operate at about 3600 ⁇ m.
• the mean residence time is from about 30 seconds to about 1800 seconds, more preferably from about 30 seconds to about 1200 seconds, and even more preferably from about 30 seconds to about 600 seconds.
• the tip speed is preferably from about 0.1 m/s to about 10 m/s, more preferably from about 0.2 m/s to about 7 m/s, and even more preferably from about 0.2 m/s to about 3.5 m/s.
• preferred low-speed mixers include rotating bowl agglomerators, drum agglomerators, pan agglomerators, fluid bed granulators, and extruders
• An example of an extruder is a multiple-screw extruder by Werner-Pfliedder (Germany)
• Fluid bed granulators are particularly preferred Typical fluid bed granulators are operated at a superficial air velocity of from about 0.1 to 4 m/s, either under positive or negative pressure. Inlet air temperatures generally range from -10°C or 5°C up to 250°C.
• inlet air temperatures are generally below 150°C, or even below 100°C or 80°C
• Other conditions include (l) from about 30 seconds to about 20 minutes of mean residence time, (n) from about 100 to about 600 mm of depth of unfluidized bed, (m) a droplet spray size of less than 2 times the particle size, preferably not more than about 100 microns, more preferably less than about 50 microns, (IV) from about 150 to about 1600 mm of spray height from the fluid bed plate, (v) from about 0.1 to about 4.0 m/s of fluidizmg velocity and (vi) from about 12°C to about 200°C of bed temperature, more preferably from about 12°C to about 150°C, even more preferably from about 12°C to about 100°C
• Other operating conditions for the fluidized bed granulator may be for example as described in WO98/58046.
• the conditions in the fluid bed may vary depending on a number of factors.
• the conditioning step can be at any point m the process.
• the conditioning step can follow mixing m the initial mixer, or the pre- mixer. If there is a series of mixers and/or combinations of mixers, the conditioning step can fall between two mixers, as well as also following the last mixer in the series. Such step is useful for many benefits, including improving the flow properties of the particles.
• Conditioning the particles include drying, cooling, coating, grinding, and sieving the particle.
• This conditioning step can be conducted in any piece of equipment known m the art such as a fluid bed dryer, air lift, fluid bed cooler, fluid bed granulator, bulk heat exchangers, grinder, and siever, or combinations of conditioning apparatus, and including series of conditioning apparatus.
• Examples of a fluid bed dryer, fluid bed cooler, and fluid bed granulator' s characteristics include fixed or vibrating; rectangular bed or round bed; and straight or serpentine apparatus
• Some apparatus have multiple internal "stages" or “zones", which are discrete areas within the apparatus. Process conditions for these apparatus could be different or similar to the other stages in the apparatus. Manufactures of such conditioning apparatus include Wurster AG, Niro, Bepex, Spray Systems and Glatt.
• apparatus such as a fluid bed or fluidized bed cooler/dryer/granulator, including combinations thereof, can be used for drying while an airlift can be used for cooling should it be necessary The air lift can also be used to force out the "fine" particles so that they can be recycled. Both air and gas can be used to dry and/or cool.
• a fluid bed granulator is especially preferred as an apparatus for the conditioning step.
• the preferred operating conditions of the fluid bed granulator is desc ⁇ bed in detail above, and such conditions are also preferred in the conditioning step.
• apparatus including the fluid bed granulator
• apparatus that can be used for grinding the particles include the Two-cage disintegrator by Stedman Foundry and Machine Co. (USA), Hammer crusher by Jeffrey Mfg. Co (USA).
• sieves include G ⁇ zzly screens made by W.S.Tyler Company (USA), mechanically vibrated Screens made by Mogensen Co. (USA), Gyratory Screens made by Alhs- Chalmers Manufacturing Co. (USA).
• the process of the present invention may additionally include a finishing step as part of the conditioning step including but not limited to, admix and/or spray- on of additional ingredients such as enzymes, bleach, perfumes, etc., or a packaging step.
• a finishing step as part of the conditioning step including but not limited to, admix and/or spray- on of additional ingredients such as enzymes, bleach, perfumes, etc., or a packaging step.
• the particles may be further processed by adding a coating agent to improve the particle color, increase the particle "whiteness", or improve the particle flowabihty after the particles exit the mixer or the conditioning apparatus to obtain the granular detergent composition produced by the present invention.
• Yet another optional processing step includes continuously adding a coating agent such as zeolites and fumed silica to the mixer to facilitate free flowabihty of the resulting detergent particles and to prevent over granulation.
• the resultant composition after mixing at least two matenals from the group form a granular detergent composition having at least about 50% by weight of particles having a geometric mean particle diameter of from about 500 microns to about 1500 microns with a geometric standard deviation of from about 1 to about 2.
• Fines or "fine” particles are defined as particles that have a geometric mean particle diameter that is less than about 1.65 standard deviations below the chosen geometric mean particle diameter of the granular detergent composition at a given geometric standard deviation. Physical Properties
• the granular detergent composition made by the process of the present invention achieves the desired benefits of solubility, improved aesthetics and flowabihty via optimal selection of the geometric mean particle diameter of certain levels of particles m the composition.
• improved aesthetics it is meant that the consumer views a granular detergent product which has a more uniform appearance of particles as opposed to past granular detergent products which contained particles of varying size and composition
• at least about 50%, more preferably at least about 75%, even more preferably at least about 90%, and most preferably at least about 95%, by weight of the total particles in the detergent product have the selected mean particle size diameter.
• a substantial portion of the granular detergent product will have the uniform size so as to provide the aesthetic appearance desired by consumers.
• the geometric mean particle diameter of the particles is from about 500 microns to about 1500 microns, more preferably from about 600 microns to about 1200 microns, and most preferably from about 600 microns to about 1000 microns.
• the particle size distribution is defined by a relative tight geometric standard deviation or "span" so as not to have too many particles outside of the target size. Accordingly, the geometric standard deviation is preferably is from about 1 to about 2, more preferably is from about 1.0 to about 1.7, even more preferably is from about 1.0 to about 1.4, and most preferably is from about 1.0 to about 1.2.
• the bulk density of the particles is preferably in the range of from about 400 g/1 to about 850 g/1, more preferably from about 550 g/1 to about 800 g/1, and even more preferably from about 600 to about 750 g/1. While not intending to be bound by theory, it is believed that solubility is enhanced as a result of the particles m the detergent composition being more of the same size. Specifically, as a result of the particles being more uniform in size, the actual "contact points" among the particles in the detergent composition is reduced which, in turn, reduces the "bridging effect" commonly associated with the "lump-gel" dissolution difficulties of granular detergent compositions. Previous granular detergent compositions contained particles of varying sizes which leads to more contact points among the particles.
• a large particle could have many smaller particles in contact with it rende ⁇ ng the particle site ripe for lump-gel formation.
• the level and uniform size of the particles in the granular detergent composition of the present invention avoids such problems.
• the particles have better chemical homogeneity, e.g. the particles are more uniform in quality.
• the detergent composition contains a detersive surfactant and/or a detergent builder to provide the fundamental building blocks of a typical detergent composition.
• the various surfactants and builders as well as their respective levels in the composition are set forth hereinafter.
• the detergent composition will contain from about 1% to about 50% by weight of a detersive surfactant and from about 1% to about 75% by weight of a detergent builder.
• a particularly important attribute of detergent powders is color. Color is usually measured on a Hunter Colorimeter and reported as three parameters "L", "a” and "b". Of particular relevance to the powdered detergent consumer is the whiteness of the powder determined by the equation L-3b. In general, whiteness values below about 60% are considered poor Whiteness can be improved by a number of means known to those of ordinary skill in the art. For example, coating granules with Titanium Dioxide
• Shape can be measured m a number of different ways known to those of ordinary skill the art.
• One such method is using optical microscopy with Optimus (V5 0) image analysis software
• Important calculated parameters are:
• the granular detergent compositions produced by the process of the present invention have circularities less than about 50, preferably less than about 30, more preferably less than about 23, most preferably less than about 18. Also preferred are granular detergent compositions with aspect ratios less than about 2, preferably less than about 1.5, more preferably less than about 1.3 most preferably less than about 1.2.
• the granular detergent compositions of this invention have a standard deviation of the number distribution of circulanty less than about 20, that is preferably less than about 10, more preferably less than about 7 most preferably less than about 4.
• the standard deviation of the number distribution of aspect ratios is preferably less than about 1, more preferably less than about 0.5, even more preferably less than about 0.3, most preferably less than about 0.2.
• granular detergent compositions are produced wherein the product of circulanty and aspect ratio is less than about 100, preferably less than about 50, more preferably less than about 30, and most preferably less than about 20. Also preferred are granular detergent compositions with the standard deviation of the number distribution of the product of circularity and aspect ratio of less than about 45, preferably less than about 20, more preferably less than about 7 most preferably less than about 2.
• the detergent components described herein may be used as a detergent adjunct ingredient in the process of the invention.
• the surfactant system of the detergent composition may include anionic, nonionic, zwitte ⁇ onic, ampholytic and cationic classes and compatible mixtures thereof.
• Detergent surfactants are described m U.S. Patent 3,664,961, Nor ⁇ s, issued May 23, 1972, and in U.S. Patent 3,919,678, Laughhn et al., issued December 30, 1975, both of which are incorporated herein by reference
• Cationic surfactants include those described in U.S. Patent 4,222,905, Cockrell, issued September 16, 1980, and in U.S. Patent 4,239,659, Mu ⁇ hy, issued December 16, 1980, both of which are also incorporated herein by reference.
• Nonlimiting examples of surfactant systems include the conventional Cj i-Cjg alkyl benzene sulfonates ("LAS") and primary, branched-chain and random C10-C20 alkyl sulfates (“AS”), the C 10 -C 18 secondary (2,3) alkyl sulfates of the formula CH 3 (CH 2 ) x (CHOS03 " M + ) CH 3 and CH3 (CH 2 ) y (CHOS ⁇ 3 " M + ) CH CH 3 where x and (y + 1) are integers of at least about 7, preferably at least about 9, and M is a water-solubihzmg cation, especially sodium, unsaturated sulfates such as oleyl sulfate, the C j o-C ⁇ g alkyl alkoxy sulfates ("AE X S”; especially EO 1-7 ethoxy sulfates), C ⁇ Q -C j g alkyl alkoxy carboxylates (especially
• the conventional nonionic and amphote ⁇ c surfactants such as the C ⁇ - jg alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and Cg-Cj2 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C ⁇ -C j g betames and sulfobetames (“sultames”), C- IO'C.18 amme oxides, and the like, can also be included m the surfactant system.
• the CjQ-Cig N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C ⁇ -Cj N-methylglucamides.
• sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as CjQ-Ci N-(3-methoxypropyl) glucamide.
• the N-propyl through N-hexyl C ⁇ -Cjg glucamides can be used for low sudsmg.
• C10-C20 conventional soaps may also be used If high sudsmg is desired, the branched-cham C ⁇ Q-C ⁇ soaps may be used Hydrophobic secondary alkyl sulfates are also preferred. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
• the detergent composition can, and preferably does, include a detergent builder.
• Builders are generally selected from the vanous water-soluble, alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, silicates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates.
• the alkali metal especially sodium, salts of the above.
• Preferred for use herein are the phosphates, carbonates, silicates, C. chief . confused fatty acids, polycarboxylates, and mixtures thereof.
• sodium t ⁇ polyphosphate More preferred are sodium t ⁇ polyphosphate, tetrasodium pyrophosphate, citrate, tartrate mono- and di-succinates, sodium silicate, and mixtures thereof (see below).
• inorganic phosphate builders are sodium and potassium t ⁇ polyphosphate, pyrophosphate, polyme ⁇ c metaphosphate having a degree of polymenzation of from about 6 to 21, and orthophosphates.
• polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-l, 1 -diphosphonic acid and the sodium and potassium salts of ethane, 1,1,2-t ⁇ phosphon ⁇ c acid
• Other phosphorus builder compounds are disclosed m U.S. Patents 3,159,581; 3,213,030; 3,422,021, 3,422,137; 3,400,176 and 3,400,148, all of which are incorporated herein by reference.
• nonphosphorus, inorganic builders are sodium and potassium carbonate, bicarbonate, sesquicarbonate, tetraborate decahydrate, and silicates having a weight ratio of S ⁇ O ⁇ to alkali metal oxide of from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4.
• Water-soluble, nonphosphorus organic builders useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates
• polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylene diamme tetraacetic acid, nit ⁇ lot ⁇ acetic acid, oxydisuccmic acid, melhtic acid, benzene polycarboxyhc acids, and citric acid.
• Polymeric polycarboxylate builders are set forth in U.S. Patent 3,308,067, Diehl, issued March 7, 1967, the disclosure of which is incorporated herein by reference.
• Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxyhc acids such as maleic acid, ltacomc acid, mesacomc acid, fuma ⁇ c acid, acomtic acid, citracomc acid and methylenemalomc acid.
• Some of these materials are useful as the water-soluble anionic polymer as hereinafter described, but only if in intimate admixture with the nonsoap anionic surfactant.
• polyacetal carboxylates for use herein are the polyacetal carboxylates descnbed m U.S. Patent 4,144,226, issued March 13, 1979 to Crutchfield et al., and U.S. Patent 4,246,495, issued March 27, 1979 to Crutchfield et al., both of which are incorporated herein by reference.
• These polyacetal carboxylates can be prepared by bringing together under polymenzation conditions an ester of glyoxyhc acid and a polymerization initiator. The resulting polyacetal carboxylate ester is then attached to chemically stable end groups to stabilize the polyacetal carboxylate against rapid depolyme ⁇ zation in alkaline solution, converted to the corresponding salt, and added to a detergent composition.
• Particularly preferred polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tartrate monosuccmate and tartrate disuccmate described in U.S. Patent 4,663,071, Bush et al., issued May 5, 1987, the disclosure of which is incorporated herein by reference
• Water-soluble silicate solids represented by the formula S ⁇ O-»M ⁇ 0, M being an alkali metal, and having a S ⁇ Ofact:MFor0 weight ratio of from about 0.5 to about 4.0, are useful salts m the detergent granules of the invention at levels of from about 2% to about 15% on an anhydrous weight basis, preferably from about 3% to about 8%.
• Anhydrous or hydrated particulate silicate can be utilized, as well.
• any number of additional ingredients can also be included as components in the granular detergent composition.
• these include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anti-corrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, nonbuilder alkalinity sources, chelatmg agents, smectite clays, enzymes, enzyme-stabihzmg agents and perfumes. See U.S. Patent 3,936,537, issued February 3, 1976 to Baskerville, Jr. et al., incorporated herein by reference.
• Bleaching agents and activators are described in U.S. Patent 4,412,934, Chung et al., issued November 1, 1983, and in U.S. Patent 4,483,781, Hartman, issued November 20, 1984, both of which are inco ⁇ orated herein by reference. Chelatmg agents are also described in U.S.
• Patent 4,663,071 Bush et al., from Column 17, line 54 through Column 18, line 68, inco ⁇ orated herein by reference. Suds modifiers are also optional ingredients and are descnbed m U.S.
• Suitable smectite clays for use herein are desc ⁇ bed in U.S. Patent 4,762,645, Tucker et al., issued August 9, 1988, Column 6, line 3 through Column 7, line 24, inco ⁇ orated herein by reference.
• Suitable additional detergency builders for use herein are enumerated m the
• Example 1 The following is an example for obtaining dust-free high density granules with narrower particle size dist ⁇ bution, improved flowabihty and better solubility
• the spray-dried granule is compnsed of 11% surfactant, 74% inorganic salts, 5% polyacrylate polymer, 5% soap, and 5% moisture.
• the dry agglomerate composition is comprised of 30% surfactant, 62% inorganic salts, 4% sodium alummosihcate, and 4% moisture.
• Step 1 360 kg/hr of a spray-dried granule (particle size of 400 microns, bulk density of 400 g/1) and 360 kgs/her of a dry agglomerate (particle size of 450 microns, bulk density of 780 g/1) is introduced into a moderate-speed KM-600TM Lodige Mixer with 8 serrated ploughs and 4 "ch ⁇ stmas-tree" choppers mounted perpendicular to the ploughs along the length of the mixer.
• the mixer is divided into four zones.
• the gap between the ploughs and the wall of the mixer is about 3 cm.
• the wall temperature is maintained at 30°C.
• aqueous linear alkyl benzene sulphonate paste (C1 1-C18, 60% active) is dispersed by the first chopper into the moderate -speed mixer and 70 kg/hr of crystalline sodium alummosihcate is added in the last zone of the mixer.
• the surfactant paste is fed at 50°C and the powders are fed at room temperature.
• the condition of the mixer is as follows: Mean residence time- 7.5-10 minutes
• the product from the moderate-speed is subjected to conditioning operations of gas-fluidized bed drying, gas-fluidized bed cooling and sizing.
• the inlet air temperature in the dryer is 120°C and the air velocity is 1 m/s.
• Inlet air humidity in the dryer is 10%.
• the mlet air temperature in the cooler is 10°C, the air velocity is 1 m s and the mlet air humidity is 40%.
• Sizing takes place in a Mogensen Sizer with a top sieve of 1180-1900 micron spacing and a bottom sieve of 300-450 microns spacing.
• the resulting granules have a bulk density of 800 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above 1180 microns.
• aqueous linear alkyl benzene sulphonate paste (C11-C18, 60% active) is injected into the mixer and dispersed with the action of the chopper blades on the powders over a penod of 5 minutes.
• the paste is at 50°C and the powders are at room temperature.
• the contents are fed into a fluidized bed for drying.
• the inlet air temperature is 105°C
• air velocity is 0.6 m/s
• drying time is 5 minutes.
• the dried granules are sieved using a Ro-tap sieve shaker with a top sieve of 1180 microns and a bottom sieve of 300 microns.
• the resulting granules have a bulk density of 650-680 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above
• 360 kg/hr of a spray-dried granule particle size of 400 microns, bulk density of 400 g/1) and 360 kg/hr of a dry agglomerate (particle size of 450 microns, bulk density of 780 g/1) is introduced into a Schugi Mixer.
• 40 kg/hr of aqueous linear alkyl benzene sulphonate paste (Cl l-18, 30% active) is sprayed on the powders using a SU 26 two-fluid nozzle (air pressure: 1-5 kg/cm 2 , liquid pressure: 2-3 kg/cm 2 ). The liquid is sprayed on at 50°C and the powders are at room temperature.
• the operating conditions of the high-speed Schugi Mixer are as follows-
• the output from the high speed mixer is fed into a moderate speed KM-600TM Mixer and 60 kg/hr of aqueous linear alkyl benzene sulphonate paste (Cl 1-C18, 60% active) is dispersed by the first chopper into the moderate speed mixer and 70 kg/hr of crystalline sodium alummosihcate is added in the last zone of the mixer.
• the surfactant paste is fed at 50°C.
• the condition of the moderate-speed mixer is as follows:
• Step 3 The product from the moderate-speed mixer is subjected to conditioning operations of gas- fluidized bed drying, gas-fluidized bed cooling and sizing
• the mlet air temperature in the dryer is 120°C and the air velocity is 1 m/s.
• Inlet air humidity m the dryer is 10%.
• the mlet air temperature in the cooler is 10°C, the air velocity is 1 m/s and the inlet air humidity is 40%.
• Sizing takes place in a Mogensen Sizer with a top sieve of 1180-1900 micron spacing and a bottom sieve of 300-450 microns spacing.
• the resulting granules have a bulk density of 550-600 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above 1180 microns.
• the undersize generated in the process can be recycled via the Schugi at 20% level and the ground overs via the fluid bed at 20% level
• 360 kg/hr of a spray-dried granule (particle size of 400 microns, bulk density of 400 g/1) and 360 kg/her of a dry agglomerate (particle size of 450 microns, bulk density of 780 g/1) is introduced into a high-speed Schugi Mixer.
• 40 kg/hr of aqueous linear alkyl benzene sulphonate paste (Cl l- 18, 30%) active) is sprayed on the powders using a SU 26 two-fluid nozzle (air pressure: 1-5 kg/cm 2 , liquid pressure: 2-3 kg/cm 2 ).
• the liquid is sprayed on at 50°C and the powders are at room temperature.
• the operating conditions of the high-speed Schugi Mixer are as follows: Tip Speed: 24 m/s
• the output from the Schugi is fed into a moderate speed KM-600TM Mixer and 40 kg/hr of aqueous linear alkyl benzene sulphonate paste (C11-C18, 60% active) is dispersed by the first chopper into the moderate speed mixer and 50 kg/hr of crystalline sodium alummosihcate is added in the last zone of the mixer.
• the surfactant paste is fed at 50°C.
• the condition of the moderate-speed mixer is as follows-
• Chopper RPM 3600 Step 3
• the product from the moderate speed is fed into a second high-speed Schugi Mixer.
• 20 kg/hr of aqueous polyethylene glycol solution (mol.wt.:4000, 40%> active) is sprayed on the powders using a SU 26 two-fluid nozzle (air pressure: 1-5 kg/cm 2 , liquid pressure: 2-3 kg/cm 2 ).
• the liquid is sprayed on at 50°C.
• the operating conditions of the Schugi Mixer are as follows: Tip Speed: 24 m/s
• the output from the Schugi is subjected to conditioning operations of gas-fluidized bed drying, gas-fluidized bed cooling and sizing.
• the mlet air temperature in the dryer is 120°C and the air velocity is 1 m/s. Inlet air humidity the dryer is 10%.
• the mlet air temperature in the cooler is 10°C, the air velocity is 1 m/s and the mlet air humidity is 40%>.
• Sizing takes place in a Mogensen Sizer with a top sieve of 1180-1900 micron spacing and a bottom sieve of 300-450 microns spacing.
• the resulting granules have a bulk density of 500-550 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above 1180 microns.
• 360 kg/hr of a spray-dried granule particle size of 400 microns, bulk density of 400 g/1 and 360 kgs/her of a dry agglomerate (particle size of 450 microns, bulk density of 780 g/1) is introduced into a KM-600TM Mixer.
• 60 kg/hr of aqueous linear alkyl benzene sulphonate paste C11-C18,
• Step 2 The output from the KM-600TM Mixer is fed into a high-speed Schugi mixer and 40 kg/h of aqueous polyethylene glycol solution (mol.wt.:4000, 40% active) is sprayed on the powders using a SU 26 two-fluid nozzle (air pressure. 1-5 kg/cm 2 , liquid pressure: 2-3 kg/cm 2 ). The liquid is sprayed on at 50°C.
• the operating conditions of the Schugi Mixer are as follows.
• the product from the Schugi mixer is subjected to conditioning operations of gas-fluidized bed drying, gas-fluidized bed cooling and sizing.
• the let air temperature in the dryer is 120°C and the air velocity is 1 m/s.
• Inlet air humidity m the dryer is 10%>.
• the mlet air temperature in the cooler is 10°C, the air velocity is 1 m/s and the mlet air humidity is 40%.
• Sizing takes place in a Mogensen Sizer with a top sieve of 1180-1900 micron spacing and a bottom sieve of 300-450 microns spacing.
• the resulting granules have a bulk density of 550-600 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above 1180 microns.
• the output from the Schugi is fed into a moderate speed KM-600TM Mixer.
• 360 kg/hr of a spray- dried granule (particle size of 400 microns, bulk density of 400 g/1) is fed into the mixer and 60 kg/hr of aqueous linear alkyl benzene sulphonate paste (Cl 1-C18, 60% active) is dispersed by the first chopper into the moderate-speed mixer and 70 kg/hr of crystalline sodium alummosihcate is added in the last zone of the mixer.
• the surfactant paste is fed at 50°C and the powder is at room temperature.
• the condition of the KM-600TM mixer is as follows: Mean residence time: 2-3 minutes Tip Speed: 2-3 m/s
• the product from the KM-600TM is subjected to conditioning operations of gas-fluidized bed drying, gas-fluidized bed cooling and sizing.
• the mlet air temperature in the dryer is 120°C and the air velocity is 1 m/s.
• Inlet air humidity in the dryer is 10%.
• the mlet air temperature m the cooler is 10°C, the air velocity is 1 m/s and the mlet air humidity is 40%.
• Sizing takes place m a Mogensen Sizer with a top sieve of 1180-1900 micron spacing and a bottom sieve of 300-450 microns spacing.
• the resulting granules have a bulk density of 450-550 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above 1180 microns.
• the resulting granules have a bulk density of 450-550 g/1, a mean particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are above 1180 microns.

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• 2000
  • 2000-06-20 AT AT00941566T patent/ATE273378T1/de not_active IP Right Cessation
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  • 2000-06-20 ES ES00941566T patent/ES2226865T3/es not_active Expired - Lifetime
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  • 2000-06-20 MX MXPA02000066A patent/MXPA02000066A/es active IP Right Grant
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  • 2000-06-20 WO PCT/US2000/016917 patent/WO2000078913A1/en active IP Right Grant
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