MXPA02000066A - Process for making a granular detergent composition. - Google Patents

Abstract

A process for detergent composition which has improved solubility or dissolution in laundering solutions, especially in solutions kept at cold temperatures (i.e., less than about 30 °C), is disclosed. The process includes mixing in at least one high-speed, low-speed, or a moderate-speed mixer, and various combinations of such mixers, at least two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray dried granules, and detergent adjunct ingredients to form particles. Optionally a conditioning apparatus may also be used. The granular detergent composition made from this process is aesthetically pleasing to consumers and has improved flowability.

Description

PROCEDURE TO MAKE A COMPOSITION GRANULAR DETERGENT FIELD OF THE INVENTION The present invention relates to a process for making an improved granular detergent composition having superior solubility, especially in laundry solutions of cold temperature (i.e. less than about 30 ° C), excellent flowability, aesthetics or appearance and friability.

BACKGROUND OF THE INVENTION Recently, there has been considerable interest within the detergent laundry detergent industry which have the comfort, aesthetics and solubility of liquid laundry detergent products, but maintain the cleaning performance and cost of the granular detergent products. The problems, however, associated with past granular detergent compositions with respect to aesthetics, solubility and comfort of the user are formidable. Such problems have been exacerbated by the advent of "compact" or low dosage granular detergent products that typically do not dissolve in laundry solutions as well as their liquid detergent laundry counterparts. These low dosage detergents are commonly in high demand, as they conserve resources and can be sold in small packages that are more comfortable for consumers before use, but less comfortable when supplied to the washing machine compared to liquid detergent. laundry that can be simply poured directly from the bottle, as opposed to "scooping" out of the box and then supplying to the washing solution. As mentioned, such low dosage or "compact" detergent products unfortunately experience dissolution problems, especially in cold temperature laundry solutions (ie less than about 30 ° C). More specifically, poor dissolution results in the formation of "lumps" that appear as solid white masses that remain in the washing machine or on washed clothes after conventional washing cycles. These "lumps" are especially frequent in cold temperature washing conditions and / or when the order of addition to the washing machine is laundry detergent first, clothes second and water (finally commonly known as "reverse order"). of addition "u" OÍDA "). Such undesirable "lumps" are also formed if the consumer loads the washing machine in the order of clothes, detergent and then water. Similarly, this phenomenon of lump formation can contribute to incomplete detergent supply in washers equipped with supplier drawers or in other delivery devices, such as a grander. In this case, the undesired result is undissolved detergent residue in the delivery device. It has been found that the cause of the aforementioned dissolution problem is associated with the "bridging" of a "gel-like" substance between particles containing surfactant to form undesirable "lumps". The gel-like substance, responsible for the undesirable "bridging" of particles to "lumps", originates from the partial dissolution of surfactant in aqueous laundry solutions, wherein such partial dissolution causes the formation of a viscous surfactant phase or paste that unites or otherwise "bridges" other particles containing surfactant to the "lumps". Commonly referred to are these undesirable phenomena of dissolution as "grumo-gel" formation. In addition to the "bridging" effect of viscous surfactants, the inorganic salts have a tendency to hydrate which can also cause "bridging" of particles that were linked together by hydration. In particular, the inorganic salts are hydrated with each other to form a cage structure which exhibits a deficient solution and finally ends up as a "lump" after the wash cycle. It would therefore be convenient to have a detergent composition that does not experience the dissolution problems identified above in a manner that results in improved cleaning performance. The prior art is replete with expositions that address the dissolution problems associated with granular detergent compositions. For example, the prior art suggests limiting the use and manner of inorganic salts that may cause lumps by "bridging" hydrated salts during the laundry cycle. Specific ratios of selected inorganic salts are contemplated in order to minimize dissolution problems. Such a solution, however, restricts the flexibility of formulation and procedure that are necessary for the common commercialization of detergent products on a large scale. Various other mechanisms have been suggested in the prior art, all of which involve alteration of the formulation and thus reduce the flexibility of the formulation. As a consequence, it would therefore be convenient to have a process by which detergent compositions having improved dissolution can be produced without significantly inhibiting the flexibility of the formulation. Generally, there are two main types of procedures by which granules or detergent powders can be prepared. The first type of process involves spraying an aqueous detergent suspension from a spray-drying tower to produce highly porous detergent granules (eg, tower process for low density detergent compositions). In the two processes mentioned above, the important factors that govern the density of the resulting detergent granules are the shape, the porosity, the particle size distribution of said angles, the density of the various detergent adjunct ingredients, the shape of the various ingredients attached detergents and their respective chemical composition.

More recently, other attempts have been made to provide continuous processes to increase the density of "after tower" detergent granules or spray-dried. Typically, such processes require a first apparatus that pulverizes or crushes the granules and a second apparatus subjects the density of the pulverized granules by agglomeration. The technique is also replete with process exposures involving agglomerating and / or spray-drying detergent compositions of various detergent adjunct ingredients. Accordingly, there remains a need in the art to have a process for producing a detergent composition that exhibits improved solubility that is more aesthetically pleasing to consumers, has improved flowability and exhibits improved cleaning performance. In addition, there remains a need to have a process for producing a detergent composition in which the density can be achieved by adjusting the condition of the process. Also, there remains a need for such a process that is more efficient, flexible and economical to facilitate the large-scale production of detergents 1) in terms of flexibility the ultimate need for the final composition 2) in terms of flexibility in terms of incorporating to the process several different kinds of detergent ingredients (such as liquid ingredients). None of the existing technique provides all the advantages in the benefits of the present invention.

BRIEF DESCRIPTION OF THE INVENTION The invention satisfies the aforementioned needs by providing a process for making a detergent composition having improved solubility or dissolution in laundry solutions, especially in solutions maintained at cold temperatures (ie less than about 30 ° C), either aesthetically pleasing to consumers and have improved flowability. According to one aspect of the invention, there is provided a process for forming a granular detergent composition with improved solubility, aesthetics and flowability: mixing at least two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray-dried granules and detergent ingredients attached in a high speed, low speed or moderate speed mixer, and various combinations of such mixers to form particles in which the granular detergent composition has at least about 50% by weight of particles having a geometric mean particle diameter from about 500 microns to about 1500 microns with a geometric regular deviation of about 1 about 2. These and other features, aspects and advantages of the present invention will be better understood, with a reading of the following description and the appended claims.

DETAILED DESCRIPTION OF THE INVENTION Although the specification concludes with the claims that particularly state and distinctly claim the invention, it is believed that the present invention will be better understood with the following description. Accordingly, it is an advantage of the invention to provide a process for making a granular detergent composition that exhibits improved solubility, is more aesthetically pleasing to consumers, has improved flowability and exhibits improved cleaning performance. It is also an advantage to have such a process for making a detergent composition that exhibits such improved dissolution without significantly inhibiting the flexibility of the formulation. In addition, it is also an advantage to have a process in which the desired density can be achieved by adjusting the condition of the process towards a more efficient, flexible and economical process to facilitate the large-scale production of detergents in terms of flexibility in terms of Incorporate several different kinds of detergent ingredients into the process.

Definitions All percentages, ratios and levels of ingredients referred to herein are based on the actual total amount of the composition, unless stated otherwise.

All measurements referred to herein are made at 25 ° C, unless otherwise specified. All publications, patent applications and patents issued that are mentioned herein are hereby incorporated by reference in their entirety. The citation of any reference is not an admission with respect to any determination as to its availability as a prior art to the claimed invention. In the present, "comprises" means that other steps and other ingredients may be added that do not affect the final result. This term encompasses the terms "consists of" and "consists essentially of". In the present, '"mixtures" means that a simple combination of materials and any compounds that may result from their combination are included. In the present, "cold water" means water having a temperature below 30 ° C. Here, "density" or "volumetric density" refers to the volume density of uncompressed, non-crushed powder as measured by pouring an excess of powder sample through a funnel into a plain metal vessel (e.g. a cylinder with 500 ml of volume), removing by rapadura the excess of the pile that is above the edge of the vessel, measuring the remaining mass of powder and dividing the mass between the volume of the vessel.

In the present, "environment" is defined as the temperature and humidity of the environment. As set forth herein, the word "particles" means the entire range of sizes of a final product or component or whole range of particle sizes, agglomerates or separate granules in a final detergent product or mixture of components. It does not specifically refer to a size fraction (that is, it represents less than 100% of the entire range of sizes) of any of those types of particles, unless the size fraction represents 100% of a separate particle in a mixture of particles. For each type of particle component of a mixture, the internal range of sizes of the separated particles of that type has the same or substantially similar composition regardless of whether the particles are in contact with other particles. For the agglomerated components the agglomerates themselves are considered as separate particles and each separate particle can be constituted of a mixed body of smaller primary particles and binder compositions. As used herein, the phrase "geometric mean particle diameter" means the average geometric mass diameter of a set of separate particles as measured by any method of regular particle size measurement based on mass, preferably sieving dry. As used herein, the phrase "geometric regular deviation" or "margin" of a particle size distribution means the geometrical width of the logarithmic normal function best suited to the aforementioned data of the particle size that can be effected. with the ratio of the diameter of the 84.13 percentile divided by the diameter of the 50th percentile of the cumulative distribution (D8 .13 D50); see Goton et al., Powder Technology Handbook, p. 6-11, Meral Dekker 1997. As used herein, the phrase "builder" means any inorganic material having a "builder" performance in the context of detergency and, specifically, organic or inorganic material capable of Remove the hardness of the water from the washing solutions. As used herein, the phrase "average dwell time" refers to the following definition: Average dwell time "hr" = mass (kg) / flow capacity (kg / hr) Process The present invention is directed to a process that produces a regular detergent composition having at least about 50% by weight of particles having a geometric mean particle diameter of about 500 microns to about 1500 microns with a regular geometric deviation of around 1 to about 2.

The present invention is directed to a process for making a regular detergent composition comprising the step of mixing at least two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray dried granules and detergent adjunct ingredients to form particles, wherein the granular detergent composition comprises at least about 50% by weight of particles having a geometric mean particle diameter of about 500 microns to about 1500 microns with a geometric regular deviation of about 1 to about 2. It is added at least two materials selected from the following group at least one mixer: dry agglomerates, wet agglomerates, spray-dried granules and detergent adjunct ingredients. Optionally, for procedures in which a conditioning apparatus is used, any poles in the recycles generated to the mixer could also be added. Wet agglomerates include those particles that are manufactured by a process of the granulation type in which adjunct detergent ingredients as described above are mixed by a liquid binder material such as a surfactant or a precursor thereof in at least one mixer for form granules of detergent materials. These particles are known as "wet agglomerates" until they are dried as "dry agglomerate" immediately after leaving the drying stage and optionally other conditioning steps such as sizing, crushing and cooling. Binders include, but are not limited to, water, anionic surfactants and precursors, nonionic surfactants, cationic surfactants, polyethylene glycol, polyvinylpyrrolidone, polyacrylates, citric acid and mixtures thereof. Spray-dried granules include those particles that are manufactured by a conventional spray-drying process in which a suspension of detergent materials is prepared and sprayed downward to a gas stream that flows upward to dry the particles. A free-flowing material is produced with the process. For example, the suspension is passed to a tower in which the suspension is sprayed into an air stream at temperatures ranging from about 175 ° C to about 450 ° C to remove the detergent suspension and form the detergent particles. Typically, the resulting densities of these particles vary from about 200 to about 650 g / l. The adjunct detergent ingredients include, but are not limited to, carbonates, phosphates, sulfates, zeolites or the like. A list of detergent components that can be used as an adjunct detergent ingredient is described in detail below. Of course, other conventionally known ingredients can also be included. In one embodiment, the mixer contains two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray dried granules and adjunct agent ingredients, or a ratio ranging from about 5:95 to about 95: 5, more preferably in a ratio ranging from around 10:90 to about 90:10 and even more preferably from about 30:70 to about 70:30. At least two types of materials selected from the group are fed, at least to a mixer for agglomeration. In one embodiment of the invention, at least two types of materials can be fed to at least one pre-mixer (eg, a conventional worm extruder, including a double worm extruder or other similar mixer) prior to agglomeration. less to a mixer; after which the mixed materials are fed to the initial mixer as described herein. To achieve the desired geometric mean particle diameter for at least about 50% by weight of the particles in the granular detergent composition, the agglomeration step can be carried out initially in at least one high speed mixer, a moderate speed mixer, a low speed mixer and combinations of mixers thereof. In addition, it can be used in one embodiment in the same type of mixer in a series or in any combination with the other types of mixers, which can also be in a series. The procedure may be intermittent or continuous.

Alternatively, two or more mixers can be used in series and / or in parallel for example to adjust the capacity. For example, one embodiment of the method of the present invention may include mixing at least two group materials in at least one high speed mixer, followed by at least one moderate speed mixer, optionally with one conditioning step in one. fluid bed granulator. In another example, mixing can take place in at least one high speed mixer, followed by at least one moderate speed mixer, followed by at least one high speed mixer, followed by at least one conditioning step. in a conditioning apparatus, such as a fluid bed granulator. In another example, at least two materials from the group initially mixed in a moderate speed blender are still selected, the mixture is then fed to a high speed blender and then conditioned in a fluid bed granulator. Alternatively, the same mixture is mixed in a high speed mixer after initial mixing in a moderate speed mixer, before being conditioned. These examples are only a few of the possible variations of mixers, pre-mixers and / or conditioning apparatuses of the process of the present invention. Subsequently, detailed examples are also assumed. The dwell times of the mixes will vary depending on the type of mixer and the operating parameters. For a preferred high speed mixer, the average dwell time is about 0.1 to 60 seconds, more preferably about 0.1 to about 30 seconds, more preferably still 0.1 to about 15 seconds. Other preferred conditions of the high speed mixer include about 3 to 90 m / s of peripheral speed and more preferably about 10 to 60 m / s of peripheral speed, and about 0.005 W / kg to 100 W / kg. of force traction, more preferably from about 0.05 W / kg to 80 W / kg force traction. Preferably, if choppers are used, troceasors may be used within the mixer to comminute undesirable oversized particles at a rotational speed and about 0 to 5000 rpm, more preferably at about 100 to 3000 rpm. Preferably, the wall temperature is from room temperature to about 80 ° C and the separation between the mixer elements and the wall is about 0.01 cm to 25 cm. Some examples of high speed mixer having an average dwell time of about 0.01 to about 60 seconds are the Lodige CB 30 ™ recloser, from Lodige Company, or mixers made by Drais, Schugi, or a similar brand blender. For a preferred mixer of moderate speed, the average dwell time is about 30 to 1800 seconds, more preferably about 30 about 1200 seconds, more preferably about 30 to about 600 seconds. Other preferred conditions of the moderate speed mixer include about 0.1 to 30 m / s of peripheral speed and more preferably about 1 to 25 m / s of peripheral speed, and about 5 W / kg to 1000W / kig. of force traction, more preferably from about 20 W / kg to 500 W / kg force traction. Preferably, if choppers are used, choppers can be used within the mixer to comminute undesirable oversized particles or a rotational speed of about 0 to 5000 rpm, more preferably around 100 to 4000 rpm. Preferably, the wall temperature is about -20 ° C to about 80 ° C, and the separation between the mixer elements and the wall is about 0.01 cm to 25 cm. Some examples of the moderate speed mixer you have that has an average type of permanence of around 30 to about 1800 seconds only the Lodige KM recycler "Ploughshare" 300 ™ and 600 ™, from Lodige Company, the Drais K-T 160 ™ mixer or mixers made by Fukae. The Lodige KM "Plowshare" 600 ™ moderate speed mixer is a particularly preferred mixer, comprising a horizontal and hollow static cylinder having a centrally mounted rotary shaft around which are attached several plow-shaped vanes. Preferably, the shaft rotates at a speed of about 15 rpm to about 140 rpm, more preferably from about 80 rpm to about 120 rpm. In a preferred mixer, grinding or spraying is performed with cutters, generally smaller in size than the rotating shaft, which preferably operates at about 3600 rpm. For a preferred low speed mixer, the average dwell time is from about 30 seconds to about 1800 seconds, more preferably from about 30 seconds to about 1200 seconds and more preferably still from about 30 seconds to about 600 seconds. The peripheral 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 more preferably from about 0.2 m / s to about 3.5 m / s. Some examples of preferred low speed mixers include rotary vessel agglomerators, drum agglomerators, tray agglomerators, fluid bed granulators and extruders. An example of an extruder is a multipleworm extruder from Werner-Pfliedder (Germany). The fluid bed granulators are particularly preferred. The typical granuators of the fluidized bed are operated at an air surface velocity of about 0.1 to 4 m / s, either under positive or negative pressure. Inlet air temperatures generally range from -10 ° C or 5 ° C to 250 ° C. however, the inlet air temperatures are generally lower than 150 ° C or even lower than 100 ° C or 80 ° C. Other conditions include (i) from about 30 seconds to about 20 minutes of the average dwell time, (ii) from about 100 to about 600 mm depth of the non-fluidized bed, (iii) a spray droplet size of less of 2 times the particle size, preferably no 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 fluidization speed and (vi) from about 12 ° C to about 200 ° C bed temperature, more preferably from about 12 ° C to about 150 ° C, more preferably still from about 12 ° C to about 100 ° C. Other operating conditions of the fluidized bed granulator can be, for example, as described in WO 98/58046. One skilled in the art will recognize that the conditions of the fluid bed may vary depending on a number of factors. Optionally, there is a conditioning step. The conditioning step can be at any point in the procedure. For example, the conditioning step may follow mixing in the initial mixer or premixer. If there are a series of mixers and / or combinations of mixers, the conditioning step can take place between two mixers, as well as next to the last mixer in the series. Such a step is useful for many benefits, including improving the flow properties of the particles. The conditioning of the particles includes drying, cooling, coating, grinding and sieving of the particle. This conditioning step can be conducted in any equipment known in the art such as fluid bed dryer, air riser, fluid bed cooler, fluid bed granulator, mass heat exchangers, shredder and sifter, or combinations of air conditioners., including series of conditioning devices. Some examples of characteristics of fluid bed dryer, fluid bed cooler and fluid bed granulator include fixed or vibrating appliances, rectangular bed or round bed and rector or serpentine. Some devices have "stage" or "zone", multiple internal, which are separate areas within the device. The process conditions for these apparatuses may be different or similar to the other steps in the apparatus. Some products manufactured from such conditioning apparatuses include Wurster AG, Niro, Bepex, Spray Systems and Glatt. By way of example, apparatuses such as cooler / dryer / fluid bed regulator or fluidized bed, including combinations thereof, can be used to dry, while an air riser can be used to cool, if necessary. An air riser can also be used to pop out "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 are described below in detail and such conditions are also preferred in the conditioning step. Some examples of apparatus (including the fluid bed granulator) that can be used to coat the particles include Wurster Fluid Bed manufactured by Wurster AG (Germany), Glatt Fluid Bed manufactured by Glatt AG (Germany), Niro Fluid Bed manufactured by Niro Aeromatic . Some examples and apparatus that can be used to crush the particles include the two-cage shredder from Stedman Foundry and Machine Co. (E.U.A), the hammer crusher from Jeffrey Mfg. Co. (E.U.A). Some examples of screens include Grizzly sieves made by W.S. Tyler Company (E.U.A), mechanically vibrated sieves made by Mogensen Co. (E.U.A), rotary sieves made by Allis-Charimers Manufacturing Co. (E.U.A.). In another optional method, the method of the present invention may additionally include a step determined as part of the conditioning step including, but not limited to, mixing and / or spraying additional ingredients such as enzymes, bleach, perfumes, etc. ., or a packing step. An optional step is that the particles can be processed further, by adding a coating agent to improve the color of the particle, increase the "whiteness" of the particle or improve the particle's flowability after the particles leave the mixer or the conditioning apparatus for obtaining the granular detergent composition produced by the present invention. Another optional process step still includes continuously adding a coating agent such as zeolites and fume silica to the mixer to facilitate the free flowability of the resulting detergent particles or to avoid over regulation.

The resulting composition after mixing at least the group materials forms a granular detergent composition having at least 50% of particles having a geometric mean particle diameter of about 500 microns to about 1500 microns as a geometric standard deviation of about 1 to about 2. When a conditioning step is used in the process and fine powders or "fine" particles are generated as a result of using a conditioning apparatus, it is preferred that the fine powders are recycled back to the process. There are many alternatives in how fine powders are recycled back to their inner agglomeration to the desired particle size. The fine powders can be recycled again to any or any mixers. Fine powders or "fine" particles are defined as particles having a geometric mean particle diameter that is less than about 1.65 of regular deviation lower than the geometric mean particle diameter of the granular detergent composition at a given geometric regular deviation.

Physical Properties The regular detergent composition made of the process of the present invention achieves the desired benefits of solubility, improved aesthetics and flowability by optimal selection of the geometric mean particle diameter of certain particle-free in the composition. By "Improved aesthetics" is understood to mean that the consumer contemplates a granular detergent product that has a more uniform appearance of particles in contrast to the past granular detergent products that contained particles of varying size and composition. In that purpose, at least 50%, more preferably at least about 75%, more preferably still at least about 90% and preferably at least about 95%, by weight of the front particles of the detergent product, has the selected average diameter of the particle size. In this way, a substantial portion of the granular detergent product will have a uniform size in order to provide the aesthetic appearance desired by consumers. Preferably, 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 adjusted geometric regular deviation or "stretch", in order not to have too many particles outside the target size. Accordingly, the geometric regular deviation is preferably from about 1 to about 2, more preferably is from about 1.0 to about 1.7, more preferably still from about 1.0 to about 1.4 and most preferably is from about 1.0 to about 1.2 . the volumetric density of the particles is preferably in the range of about 400 g / l to about 850 g / l, more preferably from about 550 g / l about 800 g / l and more preferably still from about 600 to about 750 g / l. l. Although not wishing to be bound by theory, it is believed that solubility is enhanced as a result of the particles in the detergent composition having more than the same size. Specifically, as a result of the particles being more uniform in size, the actual "points of contact" between the particles in the detergent composition are reduced which, in turn, produces the "puncturing effect" commonly associated with the difficulties of "grumo-gel" solution of the granular detergent compositions. The previous granular detergent compositions contained particles of varying sizes which results in more points of contact between the particles. For example, a large particle could have many smaller particles in contact with it making the particle site conducive to the formation of grumo-gel. The level and uniform size of the particles in the granular detergent composition of the present invention avoid such problems. further, it is believed that the particles have better chemical homogeneity, for example the particles are more uniform in quality. By "a portion" of the particles, it is understood that at least some particles in the detergent composition contain a detersive surfactant and / or builder to provide the building blocks of a typical detergent composition. The present surfactants and detergency builders are thus discussed herein with their respective levels in the composition. Typically, the detergent composition will contain from about 1% to about 50% by weight of detersive surfactant and from about 1% to about 75% by weight of a builder. Color is a particularly important attribute of detergent powders. The color is measured on a Hunter colorimeter and it is referred to as three "L", "a" and "b" parameters. Particularly preferably for the consumer of powder detergent is the powder whiteness determined by the equation L-3b. In general, whiteness values less than about 60% are considered deficient. Whiteness can be improved by various means known to those skilled in the art. For example, coating granules with titanium dioxide. Another important attribute of the granular detergent products of this invention is the shape of the individual particles. The shape can be measured in several different ways known to those skilled in the art. One such method is to use an optical microscope with a logical support (V5.0) for image analysis for image analysis. The important calculated parameters are: "Circularity" that are defined as (measured perimeter length of the particle image) 2 / (measured area of the particle image). The circularity of a perfectly smooth sphere (minimum circularity) is 12.57; and "Aspect ratio" which is defined as the length / width of the particle image. Each of these attributes is important and can be averaged over the granular detergent composition in bulk. And the combination of the two parameters defined by the product of the parameters by the product of the parameters is also important (that is, both must be continued to obtain a product with good appearance). Preferably, the granular detergent compositions produced by the process of the present invention have circularities of less than about 50, preferably less than about 30, more preferably less than about 23, most possibly less than about 18. Detergent compositions are also preferred. granules relative to this aspect of less than about 2, preferably less than about 1.5, more preferably less than about 1.3, most preferably less than about 1.2. Additionally, it is preferred to have a uniform distribution of shapes between the particles in the composition. Specifically, the granular detergent compositions of this invention have a regular deviation from the circularity number distribution of less than about 20, which is preferably less than about 10, more preferably less than about 7, most preferably less than about 4. And the regular deviation of the number distribution of the aspect ratio is preferably less than about 1, more preferably less than about 0.5, more preferably still less than about 0.3, most preferably less than about 0.2. In an especially preferred process of the present invention, granular detergent compositions are produced in which the product of circularity 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. Granular detergent compositions are also preferred with the regular deviation of the product number distribution from the circularity and aspect ratio of less than about 45, preferably less than about 20, more preferably less of about 7, most preferably less than about 2.

Detergent Components The detergent components described herein can be used as an adjunct detergent ingredient in the process of the invention. The surfactant system of the detergent composition may include anionic, nonionic, zwitterionic, ampholytic and cationic classes, and compatible mixtures thereof. Detergent surfactants are disclosed in the U.S. Patent. 3,664,961, issued May 23, 1972, and in the U.S. Patent. 3,919,678, Laughiin et al., Issued December 30, 1975, both of which are incorporated herein by reference. Cationic surfactants include those described in the U.S. Patent. 4,222,905 Cockrell, issued September 16, 1980, and in the U.S. Patent. 4,239,659, issued December 16, 1980, both of which are also incorporated herein by reference. Some non-limiting examples of surfactant systems include the alkyl benzene sulfonates ("LAS") of Cn-Cis and the primary, branched-chain and random C10-C20 alkyl sulfates ("AS"), the secondary alkyl sulfates (2.3) of C10- C18 of the formulas CH3 (CH2) x (CHOS? 3"M +) CH3 and CH3 (CH2) and (CHOSO3" M +) CH2CH3, where x and (y +1) are integers equal to at least about 7, preferably at least at about 9, and M is a water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfates, C10-C18 alkylalkoxy sulfates ("AEXS", especially EO 1-7 ethoxysulfates), alkylalkoxycarboxylates C-is (especially the ethoxycarboxylates of EO 1-5), the glycerol ethers of C-io-C-iß, the alkyl polyglycosides of C10-C18 and their corresponding sulfated polyglycosides, and the esters of alpha-sulfonated fatty acids of C12 -C18. If desired, conventional non-ionic and amphoteric surfactants such as C12-C18 alkyl ethoxylates ("AE") including the so-called narrow peak alkyl ethoxylates and the C6-C12 alkyl phenyl ether alkoxylates may also be included in the surfactant system. especially ethoxylates and ethoxy / mixed propoxy), betaines and sulfobetaines ("sultaines") of C12-C18, C12-C18 amine oxide, and the like. N-alkyl polyhydroxy fatty acid amides can also be used. Some typical examples include C12-C18 N-methylglucamides. It is already WO 9,206,154. Other surfactants derived from sugar include the N-alkoxy-polyhydroxy fatty acid amides, such as C10-C18 N- (3-methoxypropyl) glucamide. The C12-C18 N-propyl-N-hexylglucamides can be used for low foaming. Conventional C10-C2o soaps can also be used. If high foaming is desired, the branched-chain C-io-C-iß soaps can be used. Hydrophobic secondary alkyl sulfates are also preferred. Mixtures of anionic and nonionic surfactants are especially useful. Other useful conventional surfactants are listed in regular texts. The detergent composition can include, and preferably does, a builder. The detergency builders are generally selected from various water-soluble phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, silicates, borates, polyhydroxysulfonates, polyacetates, caboxyiates and polycarboxylates of alkali metal, ammonium or substituted ammonium. The alkali metal salts, especially sodium of the above, are preferred. Preferred for their use are phosphates, carbonates, silicates, C10-C18 fatty acids, polycarboxylates and mixtures thereof. More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate, mono- and disuccinates, sodium silicate, and mixtures thereof (see below). Some specific examples of inorganic phosphate builders are tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of about 6 to 21, and orthophosphate, sodium and potassium. Some examples of polyphosphonate builders are sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethan-1-hydroxy-1, 1-diphosphonic acid and the sodium and potassium salts of ethane, acid 1, 1, 2-triphosphonic. Other phosphorous builder compounds are described in the U.S. Patents. 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148, which are incorporated herein by reference. Some examples of non-phosphorus, inorganic detergency builders are sodium and potassium carbonate, bicarbonate, sesquicarbonate, tetraborate decahydrate, and silicates having a weight ratio of S¡O 2 to alkali metal oxide of about 0.5 to about 4.0, preferably from about 1.0 to about 2.4. The non-phosphorous, water-soluble organic builders useful in the present invention include various alkali metals, ammoniums and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxysulfonates. Some examples of polyacetate and polycarboxylate detergent builders are sodium, potassium, lithium, ammonium salts and substituted ammonium salts of etiiendiamintetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acids and citric acid. Polymeric polycarboxylate builders are set forth in the U.S.A. 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 carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylenemalonic acid. Some of these materials are useful as the water soluble anionic polymer as described herein below, but only if they are in intimate admixture with the anionic surfactant without soap. Other polycarboxylates suitable for use herein are polyacetal carboxylates described in the U.S.A. 4,144,226, issued March 13, 1979 to Crutchfield et al., And patent of E.U.A. 4,246,495, issued March 27, 1979 to Crutchfield et al., Both are incorporated herein by reference. These polyacetal carboxylates can be prepared by bringing together a glyoxylic acid ester and a polymerization initiator under polymerization conditions. The resulting polyacetal ester carboxylate is then attached to chemically stable end groups to stabilize the polyacetal carboxylate against rapid depolymerization in alkaline solution, which is converted to the corresponding salt, and added to a detergent composition. Particularly preferred polycarboxylate builders are ether carboxylate builder compositions comprising a combination of tartrate monosuccinate and tartrate disuccinate which is described in the U.S.A. 4,663,071, Bush et al., Issued May 5, 1987, the disclosure of which is incorporated herein by reference. The water-soluble silicate solids represented by the formula SiO2 »M2 ?, M is an alkali metal, and has a weight ratio Sl? 2: M2? from about 0.5 to about 4.0, are useful salts in the detergent granules of the invention at levels of from about 2% to about 15% on an anhydrous basis, preferably about 3% to about 8%. The silicate in anhydrous or hydrated particles can also be used. Any number of additional ingredients can be included as components in the granular detergent composition. These include other detergency builders, bleaches, bleach activators, foaming boosters or foaming suppressants, anti-rust and anti-corrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, non-improving alkalinity sources of detergency, chelating agents, smectite clay, enzymes, enzyme stabilizing agents and perfumes. See the patent of E.U.A. 3,936,537, issued February 3, 1976 to Baskerville, Jr. et al., Which is incorporated herein by reference.

Bleaching agents and activators are described in the US patent. 4,412,934, Chung et al., Issued November 1, 1983 and in the U.S. patent. 4,483,781, Hartman, issued November 20, 1984, both are incorporated herein by reference. Chelating agents are also described in the US patent. 4,663,071, Bush et al., From column 17, line 54 to column 18, line 68, which is incorporated herein by reference. Foaming modifiers are also optional ingredients and are described in the U.S. patent. 3,933,672, issued January 20, 1976 for Bartoletta et al., And 4,136,045, issued January 23, 1979 to Gault et al., Both are hereby incorporated by reference. Smectite clays suitable for use herein are described in the US patent. A. 4,762,645, Tucker et al., Issued August 9, 1988, column 6, line 3 to column 7, line 24, which is incorporated herein by reference. Additional builders suitable for use herein are listed in the Baskerville patent, column 13, line 54 to column 16, line 16, and in the US patent. 4,663,071, Bush et al., Issued May 5, 1987, both are incorporated herein by reference.

EXAMPLES The following examples are presented for the purpose of illustrating only and are not intended to be construed as limiting the scope of the appended claims in any way. These examples illustrate a process according to this invention that produces high density, brittle, free flowing, uniform detergent particles of the desired size.

EXAMPLE 1 The following is an example for obtaining powder-free high density granules with a narrow particle size distribution, improved fluidity and better solubility. In Example 1 and all the examples that follow, the spray-dried granule is comprised of 11% surfactant, 74% inorganic salts, 5% polyacrylate polymer, 5% soap, and 5% humidity. The composition of the dry agglomerate is comprised of 30% surfactant, 62% inorganic salts, 4% sodium aluminosilicate, and 4% moisture.

Step 1 360 kg / hour of a spray-dried granule (particle size 400 microns, density per unit volume of 400 g / l) and 360 kg / she of a dry agglomerate (particle size 450 microns, density per unit of volume of 780 g / l) are introduced in a moderate speed KM-600 ™ Lodige mixer with 8 toothed blades and 4"Christmas tree" shaped pieces that are mounted perpendicular to the blades along the length of the mixer. The mixer is divided into four zones. The space between the blades and the wall of the mixer is around 3 cm. The temperature of the wall is maintained at 30 ° C.

Step 2 105-115 kg / hr of an aqueous linear alkylbenzene sulphonate paste (C11-C18, active 60%) is dispersed by the first chopper in the moderate speed mixer and 70 kg / h of crystalline sodium aluminosilicate 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: Average dwell time: 7.5-10 minutes Peripheral speed: 2-3 m / s Force fraction: 20-500 W / kg RPM of the chopper: 3600 Step 3 The product from the moderate speed is gas fluidized bed drying conditioning operations, gas fluidized bed cooling and measurement. The air temperature in the dryer is 120 ° C and the air speed is 1 m / s. The humidity of the incoming air in the dryer is 10%. The incoming air temperature in the freezer is 10 ° C, the air speed is 1 m / s and the incoming air humidity is 40%. The measurement is carried out on a Mogensen meter with an upper sieve of 1180-1900 micras separation and a lower sieve of 300-450 micras separation. The resulting granules have a density per unit volume of 800 g / l, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are found by above 1180 microns.

EXAMPLE 2 Step 1 800 grams of the spray-dried granule (400 micron particle size, density per unit volume of 400 g / l) are premixed for 2 minutes on a Tilt-a-plow bench-scale Mixer Processal ™ with a total volume of 4 liters. The mixer is equipped with standard blades and a first tulip-shaped chopper mounted on the bottom in the center of the mixer.

Step 2 200 grams of the linear aqueous alkylbenzene sulphonate paste (C11-C18, 60% active) are injected into the mixer and dispersed with the action of the chopper leaves in the powders for a period of 5 minutes. The paste is at 50 ° C and the powders at room temperature.

Step 3 After the paste is added, the mixture is continued for 2.5 minutes and then 100 grams of crystalline sodium aluminosilicate are added to the mixer. The operating conditions of the mixer are as follows: Total intermittent time: 15 minutes Peripheral speed: 0.05-1 m / s RPM of the chopper: 3600 After mixing for an additional 3 minutes, the contents are fed in a fluidized bed drying. The incoming air temperature is 105 ° C, the air speed is 0.6 m / s and the drying time is 5 minutes. Subsequently, the dry granules are sieved using a Ro-tap sieve vibrator with an upper sieve of 1180 microns and a lower sieve of 300 microns. The resulting granules have a density per unit volume of 650-680 g / liter, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are find above 1180 microns.

EXAMPLE 3 Step 1 360 kg / hr of a spray-dried granule (particle size 400 microns, density per unit volume of 400 g / liter) and 360 kg / hr of a dry agglomerate (particle size 450 microns, density per unit of volume of 780 g / liter) are introduced in a Schugi mixer. 40 kg / hr of a linear aqueous alkylbenzene sulphonate paste (C11-18, 30% active) is sprinkled into the powders using a two fluid nozzle SU 26 (air pressure: 1-5 kg / cm2, liquid pressure: 2 -3 kg / cm2). The liquid is sprayed at 50 ° C and the powders are at room temperature. The operating conditions of the Schugi high-speed mixer are as follows: Peripheral speed: 24 m / s Average dwell time: 0.1-1 second Force fraction: 1-5 kW / kg The output from the high-speed mixer is fed in a moderate speed KM-600 ™ mixer and 60 kg / hr of linear aqueous alkylbenzene sulfonate paste (C11-C18 60% active) is dispersed by the first chopper in the moderate speed mixer and 70 kg / hr of the sodium aluminosilicate crystalline 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: Average dwell time: 2-3 minutes Peripheral speed: 2-3 m / s Force fraction 20-500 W / kg RPM of the chopper: 3600 Step 3 The product from the moderate speed mixer is subjected to gas fluidized bed drying conditioning operations, gas fluidized bed cooling and measurement. The air temperature in the dryer is 120 ° C and the air speed is 1 m / s. The humidity of air entering the dryer is 10%. The incoming air temperature in the cooler is 10 ° C, and the air speed is 1 m / s and the incoming air humidity is 40%. The measurement is carried out on a Mogensen meter with an upper sieve of 1180-1900 micras separation and a lower sieve of 300-450 micras separation.

The resulting granules have a density per unit volume of 550-600 g / liter, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are find above 1180 microns. Optionally, the smaller size that is generated in the process can be recycled by means of Schugi at a level of 20% and the larger ones by means of the fluidized bed at a level of 20%.

EXAMPLE 4 Step 1 360 kg / hr of the spray-dried granule (particle size 400 microns, density per unit volume of 400 g / liter) and 360 kg / she of a dry agglomerate (particle size 450 microns, density per unit) volume of 780 g / liter) are introduced in a Schugl high-speed mixer. 40 kg / hour of linear aqueous alkylbenzene sulfonate paste (C11-18, 30% active) is sprinkled on the powders using a two fluid nozzle SU 26 (air pressure: 1-5 kg / cm2, liquid pressure: 2- 3 kg / cm2). The liquid is sprayed at 50 ° C and the powders are at room temperature. The operating conditions of the Schugi high-speed mixer are the following: Peripheral speed: 24 m / s Average dwell time: 0.1-1 seconds Force fraction: 1-5 kW / kg Step 2 The output from Schugi is fed into a moderate speed KM-600 ™ mixer and 40 kg / hr of linear aqueous alkylbenzene sulfonate paste (C11-C18 60% active) is dispersed by the first chopper in the moderate speed mixer and 50 kg / hour of the crystalline sodium aluminosilicate is added in the last zone of the mixer. The surfactant sd paste is fed at 50 ° C. The condition of the moderate speed mixer is as follows: Average dwell time: 2-3 minutes Peripheral speed: 2-3 m / s Force fraction 20-500 W / kg RPM of the chopper: 3600 Step 3 The product from the moderate speed is fed into a second Schugi high-speed mixer. 20 kg / hr of the aqueous polyethylene glycol solution (weight: 4000, 40% active) is sprayed into the powders using a two-fluid nozzle SU 26 (air pressure: 1-5 kg / cm2, liquid pressure) : 2-3 kg / cm2). The liquid is sprayed at 50 ° C. The operating conditions of the Schugi mixer are as follows: Peripheral speed: 24 m / s Average dwell time: 0.1-1 seconds Force fraction: 1-5 kW / kg Step 4 The output from Schugi is subjected to gas fluidized bed drying, fluidized gas bed cooling and metering conditioning operations. The air temperature in the dryer is 120 ° C and the air speed is 1 m / s. The humidity of air entering the dryer 10%. The incoming air temperature in the freezer is 10 ° C, the air speed is 1 m / s and the incoming air humidity is 40%. The measurement is carried out on a Mogensen meter with an upper sieve of 1180-1900 micras separation and a lower sieve of 300-450 micras separation. The resulting granules have a density per unit volume of 500-550 g / l, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are find above 1180 microns.

EXAMPLE 5 Step 1 360 kg / hr of a spray-dried granule (particle size 400 microns, density per unit volume of 400 g / l) and 360 kg / s of a dry agglomerate (particle size 450 microns, density per volume unit of 780 g / l) are fed into a KM-600 ™ mixer. 60 kg / hr of a linear aqueous alkylbenzene sulphonate paste (C11-C18, 60% active) is dispersed by the first the first chopper at moderate speed and 50 kg / hr of crystalline sodium aluminosilicate is added in the last zone of the mixer . The surfactant paste is fed at 50 ° C and the powders are at room temperature. The condition of the KM-600 ™ mixer is as follows: Average dwell time: 2-3 minutes Peripheral speed: 2-3 m / s Force fraction: 20-500 W / kg RPM of the chopper: 3600 Step 2 The output from the mixer KM-600 - > TI IVI is fed in a Schugl high speed mixer and 40 kg / h of the aqueous polyethylene glycol solution (weight: 4000, 40% active) is sprinkled in the powders using a two fluid nozzle SU 26 (air pressure : 1-5 kg / cm2, liquid pressure: 2-3 kg / cm2). The liquid is sprayed at 50 ° C. The operating conditions of the Schugi mixer are the following: Peripheral speed: 24 m / s Average dwell time: 0.1-1 second Force fraction: 1-5 kW / kg Step 3 The product from the Schugi mixer is subjected to drying conditioning operations of the fluidized bed in gas, gas fluidized bed cooling and measurement. The air temperature in the dryer of 120 ° C and the air speed is 1 m / s. The humidity of air entering the dryer is 10%. The incoming air temperature in the cooler is 10 ° C, the air speed is 1 m / s and the incoming air humidity is 40%. The measurement is carried out on a Mogensen meter with an upper sieve of 1180-1900 micras separation and a lower sieve of 300-400 micras separation. The resulting granules have a density per unit volume of 550-600 g / l, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are they find 1180 mieras above.

EXAMPLE 6 Step 1 360 kg / s of dry agglomerate (particle size 450 microns, density per unit volume of 780 g / l) is fed into a Schugi high-speed mixer. 40 kg / hr of the linear aqueous alkylbenzene sulphonate paste (C11-18, 30% active) are sprinkled into the powders using a two fluid nozzle SU 26 (air pressure: 1.5 kg / cm2, liquid pressure: 2-3 kg / cm2). The liquid is sprayed at 50 ° C and the powder at room temperature. The operating conditions of the Schugi mixer are the following: Peripheral speed: 24 m / s Average dwell time: 0.1-1 second Force fraction: 1-5 kW / kg Step 2 The output from the Schugi is powered by a moderate speed KM-600 ™ mixer. 360 kg / hr of a spray-dried granule (400 micron particle size, density per unit volume of 400 g / l) are fed in a mixer and 60 kg / hr of the linear aqueous alkyl benzene sulfonate paste (C11-C18) , 60% active) is dispersed by the first chopper in the moderate speed mixer and 70 kg / hr of the crystalline sodium aluminosilicate 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-600 ™ mixer is as follows: Average dwell time: 2-3 minutes Peripheral speed: 2-3 m / s Force fraction: 20-500 W / kg RPM of the chopper: 3600 Step 3 The product from the KM-600 ™ is subjected to gas fluidized bed drying, gas fluidized bed, and metering conditioning operations. The air temperature in the dryer 120 ° C and the air speed is 1 m / s. The humidity of air entering the dryer is 10%. The incoming air temperature in the cooler is 10 ° C, the air speed is 1 m / s and the incoming air humidity is 40%. The measurement is carried out on a Mogensen meter with an upper sieve of 1180-1900 micras separation and a lower sieve of 300-450 micras separation. The resulting granules have a density per unit volume of 450-550 g / l, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are find over 180 micras. The resulting granules have a density per unit volume of 450-550 g / l, an average particle size of 600 microns, less than 3% of the granules are below 300 microns and less than 3% of the granules are find above 1180 microns. Having described the invention in detail, it will be apparent to those skilled in the art that various changes can be made without departing from the scope of the invention and the invention is not intended to be construed as limiting what is described in the specification.

Claims (12)

NOVELTY OF THE INVENTION CLAIMS

1. - A process for making a granular detergent composition comprising the steps of mixing at least two materials selected from the group consisting of dry agglomerates, wet agglomerates, spray-dried granules, and detergent adjunct ingredients in at least one mixer selected from the group consisting of in a low speed mixer, a moderate speed mixer, a high speed mixer, and combinations of mixers thereof, to form particles, characterized in that the granular detergent composition comprises at least 50% by weight of the particles having a geometric average particle diameter of about 500 microns to about 1500 microns with a geometric standard deviation of about 1 to about 2.

2. The method according to claim 1, further characterized by comprising the step of conditioning the resulting particles in at least one device of a conditioning

3. The method according to claim 1, further characterized in that the average dwell time of the low speed mixer is from about 30 seconds to about 1800 seconds, the average dwell time of the moderate speed mixer is about 30 to about 1800 seconds, and the average dwell time of the high speed mixer is from about 0.1 to about 60 seconds.

4. The process according to claim 2, further characterized in that the step of conditioning includes at least one granulator of the fluidized bed.

5. The method according to claim 3, further characterized in that the peripheral speed of the low speed mixer is about 0.1 m / s to about 10 m / s, the peripheral velocity of the moderate speed mixer is about 0.1 m / s at about 30 m / s, and the peripheral velocity of the high-speed mixer is from about 3 m / s to about 90 m / s.

6. The process according to claim 4, further characterized in that the fine particles generated from the fluidized bed granulator are recycled in at least one mixer.

7. The process according to claim 1, further characterized in that the mixer contains a ratio of dry agglomerates to spray-dried granules of about 5.95 to about 95.5.

8. The process according to claim 4, further characterized in that the fluidized bed granulator has an average residence time of about 30 seconds to about 20 minutes.

9. - The process according to claim 1, further characterized in that the low shear mixer is a fluidized bed granulator. 10. A process for preparing a granular detergent composition comprising the steps of: (a) mixing at least two materials selected from the group consisting of dry, agglomerated agglomerates * wet, spray-dried granules, and detergent adjunct ingredients in at least one mixer selected from the group consisting of a low speed mixer, a moderate speed mixer, a

10 high-speed mixer, and combinations of mixers thereof, to form particles, and (b) condition the resulting particles in at least one conditioning apparatus, characterized in that the average dwell time of the low-speed mixer is about 30 t seconds at approximately 1800 seconds, the dwell time The average of the moderate speed mixer is from about 30 to about 1800 seconds, and the average dwell time of the high speed mixer is from about 0.1 to about 60 seconds, and wherein the granular detergent composition comprises at least 50%. by weight of the particles having a particle diameter 20 geometric average of about 500 microns to about 1500 microns with a geometric standard deviation of about 1 to about 2.

11. - The method according to claim 10, further characterized in that the step of conditioning includes at least one fluidized bed granulator.

12. The process according to claim 11, further characterized in that the operating conditions of the fluidized bed granulator include (i) from about 30 seconds to about 20 minutes of the average dwell time, (ii) of about 100 mm to about 600 mm depth of the non-fluidized bed, (ii) no more than about 100 microns of the spray droplet size, (iv) from about 150 mm to about 1600 mm of spray height, (v) from about 0.1 to about 4.0 m / s fluidizing velocity and (vi) from about 12 ° C to about 200 ° C bed temperature.