ES2201305T3 - PROCEDURE FOR MANUFACTURING A DETERGENT COMPOSITION WITHOUT USING TOWERS. - Google Patents

Abstract

THE INVENTION REFERS TO A PROCEDURE THAT DOES NOT USE A TOWER, TO PREPARE A DETERGENT GRANULAR COMPOSITION OF APPROX DENSITY CONTINUOUSLY. OF 600 G / L. SUCH PROCEDURE UNDERSTAND THE FOLLOWING PHASES: (A) (I) DISPERSE A TENSIOACTIVE AND COVER SUCH TENSIOACTIVE WITH FINE POWDER, IN A MIXER, THEREFORE FORMING FIRST AGLOMERATED AND B (B) PERFECTLY MIXING THE FIRST THINNER, WHAT FORMED SECONDS AGLOMERATED, AND (C) GRANULAR THE SECONDS AGLOMERATED IN ONE OR MORE FLUIDIFICATION DEVICES. SUCH PROCEDURE CAN ALSO UNDERSTAND AN ADDITIONAL PHASE (B '') THAT CONSISTS OF SPRAYING A LIQUID FINALLY ATOMIZED ON THE SECONDS AGLOMERATED, IN A MIXER, BETWEEN PHASE (B) AND PHASE (C).

Description

Procedure to manufacture a composition detergent without using towers.

Field of the Invention

The present invention generally relates to a procedure without towers to produce a composition particulate detergent. More particularly, the invention is refers to a continuous procedure by which they occur detergent agglomerates feeding a surfactant and materials of coating to a series of mixers. The procedure produces a flowing detergent composition whose density can be adjusted for a wide range of consumer needs and that You can sell commercially.

Background of the invention

Recently, in the detergent industry has there was considerable interest in detergents for washing clothes that are "compact" and therefore have low dosage volumes. To facilitate the production of These so-called low dosage detergents have been made many attempts to produce detergents of high apparent density, for example, 600 g / l or more. Low dosage detergents they are currently in high demand because they conserve resources and they can sell in small packages that are more convenient for consumers. However, the degree to which the products Modern detergents need to be of a "compact" nature It is still undetermined. Actually, many consumers, especially in developing countries, they continue preferring higher dosage levels in their respective laundry operations.

Generally, there are two main types of processes by which granules or powders can be prepared detergents The first type of process involves spray drying an aqueous suspension of the detergent in a drying tower by spray, to produce very porous detergent granules (for example, process with towers for low detergent compositions density). In the second type of process, the various components of the detergent are mixed dry after which they agglomerate with a binder, such as a nonionic or anionic surfactant, to produce high density detergent compositions (for example, agglomeration process for high detergent compositions density). In these two processes, the important factors that determine the density of the resulting detergent granules are the shape, porosity and size distribution of those mentioned granules, density and shape of various starting materials and their respective chemical composition.

In the art there have been many attempts to provide processes that increase the density of granules or detergent powders Particular attention has been given to the densification, by treatment after towers, of granules spray dried. For example, an attempt involves a process discontinuous in which granulated detergent powders that contain sodium tripolyphosphate and sodium sulfate densify or they turn spherical granules into a Marumizer®. This apparatus comprises a rough, substantially horizontal rotating table, located at the base of a substantially vertical cylinder of smooth walls However, this process is essentially a discontinuous process and therefore less suitable for Large-scale detergent powder production. More recently, other attempts have been made to provide continuous processes to increase the density, after the towers, of granules spray dried detergents. Typically, such processes require a first device that pulverizes or crushes the granules and a second device that increases the density of the powdered granules. Although these processes get the desired increase in density by treating or densifying "after of the towers "spray dried granules, have a limited ability to have higher levels of surfactant without a subsequent stage of coating. In addition, the treatment or densification "after the towers" is not favorable as far as a economy (higher capital cost) and complexity of operation. In addition, all the aforementioned processes refer mainly to densify or process dried granules by aspersion. Currently, relative amounts have been limited and types of materials subjected to spray drying processes for the production of detergent granules. For example, it has been difficult to achieve high levels of surfactant in the composition resulting detergent, a feature that facilitates production of detergents in a more efficient way. Thus, it would be desirable. have a process whereby compositions could be produced detergents without having the limitations imposed by techniques Conventional spray drying.

To this end, the technique is full of process descriptions that involve agglomerating compositions detergents For example, attempts have been made to agglomerate detergent additives by mixing in a zeolite and / or silicate mixer in layers, to produce flowing agglomerates. Although said attempts suggest that these processes can be used to produce detergent agglomerates, do not provide a mechanism by which starting detergent materials in the form of pastes, liquids or dry materials can be effectively formed agglomerated agglomerates consistent flowing detergents.

Consequently, in the technique the need to have an agglomeration process (without towers) to continuously produce a detergent composition that has a high density provided directly by the ingredients starting detergents and preferably the density adjusting process conditions. Also subsists the need for such a process to be more efficient, flexible and Economical to facilitate the production of large-scale detergents (1) by flexibility in the final density of the final composition and (2) for flexibility in incorporating several in the process different kinds of detergent ingredients (especially liquid ingredients).

Numerous processes are known in which agglomerates are formed in a mixer from a surfactant and a fine powder and it is described that the resulting agglomerates should be dried, with fluid bed drying being the usually proposed drying method. Examples include US-A-5,554,587, WO96 / 09370, EP-A-0,663,439, WO93 / 25378, WO 95/12659, US-A-5,489,392, WO92 / 01036 and US-A-4,992 .979. It is also known to use a fluidized bed for other purposes in the manufacture of particulate detergents. For example, in GB-A-2,209,172 it is proposed to spray a liquid material on a fluidized particulate material comprising a detergent additive and, in particular, it is proposed to use this to achieve an in situ reaction in the fluidized bed between the fluidized particulate material comprising at least one alkaline support and the liquid material that is sprayed on the bed and comprising at least one acidic precursor of an anionic surfactant compound.

Although processes like those listed above to prepare granular detergents by agglomeration (that is, without towers) provide advantages over drying processes by sprinkling, especially for the manufacture of products that they have a density of at least 600 g / l, they are not totally satisfactory Consequently, an object of the present invention is to provide a procedure to continuously produce a detergent composition that has flexibility with respect to the density of the final product controlling energy consumption, residence time and peripheral speed in the mixers. Also an object of the invention is to provide a method that is more efficient, flexible and economical and that facilitates the large scale production.

The present invention meets the needs mentioned above in the art by providing a procedure that It produces a high density granular detergent composition. The The present invention also meets the needs before mentioned in the art by providing a procedure that produces a granular detergent composition for flexibility in final density of the final composition by a process of agglomeration (for example, without towers). The procedure does not use the conventional spray drying towers that are limited to produce compositions with high surfactant loading. In addition, the Procedure of the present invention is more efficient, economical and flexible with respect to the diversity of compositions detergents that can be produced in the process. In addition, the procedure is more sensitive to environmental conditions because does not use spray drying towers that typically emit to the Atmospheric particulate and volatile organic compounds.

Here, the term "agglomerates" refers to particles formed by agglomerating raw materials with binders, such as surfactants and / or solutions inorganic / organic solvents and polymer solutions. In the In this report, the term "granulation" refers to fluidize agglomerates to produce granulated agglomerates round shaped flowers. Here, the term "average residence time" refers to the following definition:

Average residence time (h) = [mass (kg)] / [hourly production (kg / h)]

All percentages used herein Memory are percentages by weight, unless otherwise indicated. All proportions are proportions by weight, unless indicate otherwise. Here, the term "which comprises "means that other steps and others can be added ingredients that do not affect the result. This term covers the terms "consisting of" and "consisting essentially in".

According to a first aspect of the invention, an agglomeration process to prepare a composition granular detergent having a density of at least 600 g / l It comprises the stages of:

(a) disperse a surfactant and coat the surfactant with a fine powder having a diameter of 0.1 to 500 micrometers in a first mixer in which the conditions of the mixer include (i) an average residence time of 2 to 50 seconds, (ii) a peripheral speed of 4 to 25 m / s and (iii) a energy condition of 0.15 to 7 kJ / kg, in which some first agglomerates, and

(b) perfectly mixing the first agglomerates in a second mixer in which the conditions of the mixer include (i) an average residence time of 0.5 to 15 minutes and (ii) an energy condition of 0.15 a
7 kJ / kg, in which a few agglomerated seconds are formed,

characterized in that the procedure understands:

(c) granulate the second agglomerates in a fluidized bed apparatus spraying at the same time on the bed droplets of a liquid detergent material in an amount of up to 20%, and in which the conditions of the fluidized bed apparatus include (i) an average residence time of 1 to 10 minutes, (ii) a height of the non-fluidized bed of 100 to 300 mm, (iii) a droplet droplet size not exceeding 50 micrometers, (iv) a spray height of 175 to 250 mm, (v) a speed of fluidization of 0.2 to 1.4 m / s and (vi) a bed temperature of 12 to 100 ° C.

According to a second aspect of the invention, an agglomeration process for preparing a granular detergent composition having a density of at minus 600 g / l comprises the steps of:

(a) disperse a surfactant and coat the surfactant with a fine powder having a diameter of 0.1 to 500 micrometers in a first mixer in which the conditions of the mixer include (i) an average residence time of 2 to 50 seconds, (ii) a peripheral speed of 4 to 25 m / s and (iii) a energy condition of 0.15 to 7 kJ / kg, in which some first agglomerates, and

(b) perfectly mixing the first agglomerates in a second mixer in which the conditions of the mixer include (i) an average residence time of 0.5 to 15 minutes and (ii) an energy condition of 0.15 a
7 kJ / kg, in which a few agglomerated seconds are formed,

characterized in that the procedure understands:

(b ') spray on the second agglomerates a finely atomized liquid in a third mixer in which Mixer conditions include (i) an average time of permanence of 0.2 to 5 seconds, (ii) a peripheral speed of 10 at 30 m / s and (iii) an energy condition of 0.15 to 5 kJ / kg, in the that some agglomerated third parties are formed, and

(c) granulate the third agglomerates in a fluidized bed apparatus spraying at the same time on the bed droplets of a liquid detergent material in an amount of up to 20%, and in which the conditions of the fluidized bed apparatus include (i) an average residence time of 1 to 10 minutes, (ii) a height of the non-fluidized bed of 100 to 300 mm, (iii) a droplet droplet size not exceeding 50 micrometers, (iv) a spray height of 175 to 250 mm, (v) a speed of fluidization of 0.2 to 1.4 m / s and (vi) a bed temperature of 12 to 100 ° C.

Brief description of the drawings

Figure 1 is a flow chart of a method according to an embodiment of the invention that includes the agglomeration procedure used by the first mixer, followed by the second mixer and then the fluidization, to produce a granular detergent composition which has a density of at least 600 g / l.

Figure 2 is a flow chart of a method according to an embodiment of the invention that includes the agglomeration procedure used by the first mixer, followed by the second mixer, then the third mixer and finally the fluidization apparatus, to produce a granular detergent composition having a density of at least 600 g / l.

Detailed description of the preferred embodiment

The present invention relates to a procedure that produces flowing detergent agglomerates granular having a density of at least 600 g / l. The procedure produces agglomerates of granular detergents from of an aqueous and / or non-aqueous surfactant that is then coated with a fine powder having a diameter of 0.1 to 500 micrometers, for obtain low density granules.

Process

Reference is now made to (1) Figure 1 which presents a flow chart illustrating an embodiment of the present invention, that is, a method comprising the first stage, the second stage (i) and the third stage, and (2) the Figure 2 presenting a flow chart illustrating a embodiment of the present invention, that is, a process comprising the first stage, the second stages (i) and (ii) and the third stage

First stage [stage (to)]

In the first stage of the procedure, feed a first mixer 13 a surfactant 11, that is, one or more aqueous and / or non-aqueous surfactants that are in the form of powder, paste and / or liquid, and a fine powder 12 having a diameter from 0.1 to 500 micrometers, preferably from about 1 to approximately 100 micrometers, to prepare agglomerates (the definition of surfactant and fine powder are described in detail later). Optionally, in addition to the fine powder, you can feed the mixer an internal recirculated stream of dust 30, which has a diameter of about 0.1 to about 300 micrometers, generated in the fluidization apparatus 27 which is described later in step 3. The amount of said current  Internal recirculated powder 30 can be 0 to about 60% by weight of the final product 29.

In another embodiment of the invention, the surfactant 11 may initially be fed to a mixer or premixer (for example, a conventional screw extruder or other similar mixer) before the previous stage, after which mixed detergent materials are fed to the mixer of the first stage, as described, for its agglomeration.

The average time spent in the first mixer is in the range of 2 to 50 seconds, the speed peripheral of the first mixer is in the range of 4 to 25 m / s and energy per unit mass (energy condition) in the first mixer is in the range of 0.15 to 7 kJ / kg, more preferably, the average residence time in the first mixer is in the range of about 5 to approximately 30 seconds, the peripheral speed of the first mixer is in the range of about 6 to approximately 18 m / s and energy per unit mass (condition of energy) in the first mixer is in the range of about 0.3 to about 4 kJ / kg, and more preferably the average residence time in the first mixer is in the range of about 5 to approximately 20 seconds, the first peripheral speed mixer is in the range of about 8 to approximately 18 m / s and energy per unit mass (condition of energy) in the first mixer is in the range of about 0.3 to about 4 kJ / kg.

Examples of mixers for the first stage they can be any types of mixers known to the skilled in the art provided that the mixer can maintain the conditions mentioned above for the first stage. An example it can be a Lödige CB mixer manufactured by the Lödige company (Germany). As a result of the first stage, the resulting product 16 (first agglomerates that have fine dust on its surface).

Second stage [stage (b) / stage (b ')]

As a preferred embodiment, there are two types of choice, that is, only a second stage (i), or a second stage (i) followed by another second stage (ii).

Second stage (i) [(stage (b)]

The resulting product 16 (first agglomerates) a second mixer is fed 17. That is, the product resulting 16 is mixed and thoroughly sheared to round and make grow the agglomerates in the second mixer 17. Optionally, it  you can add in the second stage (i) approximately 0-10%, more preferably about 2-5% powder detergent ingredients 16. Preferably, to break undesirable agglomerates of size greater than desired, cutters coupled to the second can be used mixer. Therefore, the procedure that includes the second Mixer 17 with cutters is useful to obtain as final product a reduced amount of agglomerates larger than desired and said method is a preferred embodiment of the present invention.

The average time spent in the second mixer is in the range of 0.5 to 15 minutes and the energy per mass unit (energy condition) in the second mixer is in the range of 0.15 to 7 kJ / kg, more preferably the time permanence medium in the second mixer is in the range of about 3 to about 6 minutes and energy per unit of mass in the second mixer is in the range of about 0.15 to about 4 kJ / kg.

Examples of the second mixer 17 may be any types of mixers known to those skilled in the technique as long as the mixer can maintain the conditions mentioned above for the second stage (i). An example may be the Lödige KM mixer manufactured by the Lödige company (Germany). As a result of the second stage (i), a product is obtained resulting 20 (second agglomerates) round. The product resulting 20 is then subjected to the other second stage (ii) or to the third stage

Second stage (ii) [stage (b ')]

The resulting product 20 (agglomerated seconds) it is fed to a third mixer 21 and then, in mixer 21, a thin liquid is sprayed on the agglomerated seconds atomized 22. Optionally, in the second stage (ii) powder is added  excess fine formed in the first stage and / or in the second stage (i). If in the second stage (ii) excess fine powder is added, it is useful to spray the finely atomized liquid to bond the fine powder in excess to the surface of the agglomerates. To the mixer 21  approximately 0-10% can be added, more preferably about 2-5% of ingredients powder detergents of the type used in the first stage and in the second stage (i) and other detergent ingredients.

The average time spent in the third mixer is in the range of 0.2 to 5 seconds, the speed peripheral of the third mixer is in the range of 10 to 30 m / s and energy per unit mass (energy condition) in the third mixer is in the range of 0.15 to 5 kJ / kg, more preferably the average residence time in the third mixer is in the range of about 0.2 to approximately 5 seconds, the peripheral speed of the third mixer is in the range of about 10 to approximately 30 m / s and energy per unit mass in the third mixer is in the range of about 0.15 to approximately 5 kJ / kg, most preferably the average time of permanence in the third mixer is in the range of about 0.2 to about 5 seconds, the speed peripheral of the third mixer is in the range of approximately 15 to approximately 26 m / s and energy per unit of mass (energy condition) in the third mixer is in the range from about 0.2 to about 3 kJ / kg.

Examples of the mixer 21 can be any types of mixers known to those skilled in the art as long as the mixer can maintain the conditions before mentioned for stage (ii). An example can be the model Flexomic manufactured by the company Schugi (Netherlands). How result of the second stage, a product can be obtained resulting 24, that is, agglomerated with excess fines over they. The resulting product 24 (third agglomerates) is submitted Then to the third stage.

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Third stage [stage (c)]

In the third stage of the procedure, the resulting product 20 (second agglomerates) or the product resulting 24 (third agglomerates) is fed to an apparatus of fluidized bed spraying droplets from a bed at the same time liquid detergent material in an amount of up to 20%, for favor granulation and produce high flow granules density. At this stage, the product resulting from the stage previous fluidizes completely so the granules resulting have a round shape. Optionally, at this stage about 0 to about 10% can be added, plus preferably about 2-5% of materials powder detergents of the kind used in the first stage and / or Other detergent ingredients. Liquid detergent materials sprayed on the bed may be of the kind used in the first stage and / or other ingredients can be added at this stage detergents to favor granulation and coat on the surface of the granules.

To get the density of at least approximately 600 g / l, preferably a density greater than 650 g / l, the conditions of the fluidized bed apparatus can be:

Average residence time: 1 10 minutes

Bed height no fluidized: 100 to 300 mm

Droplet Size sprayed: not exceeding 50 micrometers

Spray Height: 175 to 250 mm

Fluidization Rate: 0.2 at 1.4 m / s

Bed temperature: 12 a 100 ° C;

plus preferably:

Average residence time: about 2 to about 6 minutes

Bed height no fluidized: approximately 200 to approximately 250 mm

Droplet Size sprayed: less than about 50 micrometers

Spray Height: approximately 175 to approximately 200 mm

Fluidization Speed: approximately 0.3 to 1.0 m / s

Bed temperature: about 12 to about 80 ° C.

The fluidized bed stage can use more of a fluidization apparatus (for example, combining classes different from fluidizing apparatus, such as a bed dryer fluid and a fluid bed cooler). If there is more than one device fluidization, each can operate under the same intervals of conditions but the atomized liquid must be present only in One of the beds. If two different kinds of device are used fluidization, the total average time spent in the second stage can be from about 1 to about 20 minutes, more preferably about 2 to 12 minutes.

A coating agent can be added to improve fluidity and / or minimize excessive agglomeration of the detergent composition, in one or more of the following points of the Present procedure: (1) the coating agent can be add directly after the fluid bed cooler or fluid bed dryer, (2) the coating agent can be add between the fluid bed dryer and the bed cooler fluid, and / or (3) the coating agent can be added directly to the third mixer 21 and the fluid bed dryer. The coating agent is preferably selected from the group formed by aluminosilicates, silicates, carbonates and mixtures of the same. The coating agent not only increases the fluidity of the resulting detergent composition desirable by consumers because it allows easy dosing of the detergent during use It also serves to control agglomeration by avoiding or minimizing excessive agglomeration. How you know them well Those skilled in the art, excessive agglomeration can cause Undesirable fluidity and aesthetic properties in the product final detergent

In the case of performing the procedure of the present invention using (1) a thong CB mixer flexibility to inject at least two liquid ingredients, (2) a KM mixer that has flexibility to inject so less a liquid ingredient, (3) a Schugi mixer that has flexibility to inject at least two liquid ingredients and (4) a fluidized bed (fluid) that has flexibility to inject at least two liquid ingredients, the procedure can incorporate seven different kinds of liquid ingredients in the procedure Therefore, the proposed procedure is beneficial for those skilled in the art to incorporate into a manufacturing process of detergent material granules of heading that are in liquid form and that are expensive and sometimes more difficult in terms of handling and / or storage that solid materials

The proposed invention is also useful in view of industrial requirements because those skilled in the art can fix a series of devices in a plant and use diverters able to connect / disconnect each device so the experts in the art they can select variations of the procedure for satisfy the desired properties (for example, size of particles, density, formulation) of the final product. These variations include not only the procedure of the present invention, that is, (i) first mixer - second mixer - fluidization apparatus, and (ii) first mixer - second mixer - third mixer - fluidization apparatus, but also includes (iii) first mixer - third mixer - apparatus of fluidization, (iv) first mixer, third mixer - second mixer - fluidizing apparatus, and (v) first mixer - fluidization apparatus.

Starting detergent materials

The total amount of surfactants in products prepared by the present invention, which are included in the following detergent materials, finely atomized liquid e auxiliary detergent ingredients, is generally of about 5% to about 60%, more preferably of about 12 to about 40%, even more preferably from about 15 to about 35%, by weight. The surfactants that are included in the aforementioned materials may come from any part of the procedure herein invention, for example, of any one of the first stage, the second stage and / or the third stage of the present invention.

Detergent surfactant (aqueous / non-aqueous)

The amount of surfactant in the present procedure can be from about 5 to about 60%, more preferably from about 12 to about 40%, still more preferably from about 15 to about 35%, referred to the total amount of final product obtained by the procedure of the present invention.

The surfactant of the present process, which it is used in the first stage in the starting detergent materials mentioned above, it is in the form of liquid material, paste or powder.

The surfactant is preferably selected from anionic, nonionic, hybrid, amphoteric and cationic and compatible mixtures thereof. Surfactants detergents useful in the present invention are described in the U.S. Patents 3,664,961, Norris, granted on 23 May 1972, and 3,929,678, Laughlin et al., granted on 30 December 1975, both incorporated as a reference in the present memory Useful cationic surfactants include also those described in United States patents 4,222,905, Cockrell, granted on September 16, 1980, and 4,239,659, Murphy, granted on December 16, 1980, both incorporated herein also as a reference. Of the surfactants, anionics are preferred and non Ionic and most preferred are anionic.

Non-limiting examples of surfactants Preferred anionics useful in the present invention include the (linear alkyl C 11 -C 18) benzenesulfonates ("LAS") and (primary C 10 -C 20 alkyl), linear and random chain) alkyl sulfates ("AS") conventional; the [C 10 -C 18 alkyl] secondary (2,3)] sulfates of formula CH 3 (CH 2) x (CHOSO 3 - M +) CH 3 Y CH 3 (CH 2) y (CHOSO 3 - M +) CH 2 CH 3 in which x e (y + 1) are integers of at least about 7, preferably at least about 9, and M is a water solubilizing cation, especially sodium; unsaturated sulfates, such as oleyl sulfates, and (alkyl) C 10 -C 18) - alkoxysulfates ("AE_ {x} S", especially EO ethoxy sulfates 1-7).

Useful anionic surfactants include also water soluble salts of acids 2-acyloxyalkano-1-sulfonic containing approximately 2 to 9 carbon atoms in the group acyl and about 9 to about 23 carbon atoms in the rest alkane; water soluble salts of olefinsulfonates that they contain approximately 12 to 24 carbon atoms and β-alkyloxysulfonates containing about 1 to 3 carbon atoms in the alkyl group and approximately 8 to 20 carbon atoms in the alkane moiety.

Optionally, other useful typical surfactants in the pulp of the invention include (alkyl C 10 -C 18) alkoxycarboxylates (especially EO 1-5 ethoxycarboxylates), (rent C 10 -C 18) - glycerol ethers, the (C 10 -C 18 alkyl) polyglycosides and the corresponding sulfated polyglycosides, and esters of C 12 -C 18 fatty acids α-sulphonates. If desired, you can also include non-ionic surfactants in the compositions and conventional amphoteric, such as (alkyl) C 12 -C 18) - ethoxylates ("AE"), including so-called (peak alkyl) narrow) ethoxylates and (alkyl C 6 -C 12) Phenolalkoxylates (especially mixed ethoxylates and ethoxy / propoxy), amine oxides C_ {10} -C_ {18}, etc. You can also use the N-alkylamides of polyhydroxy fatty acids C_ {10} -C_ {18}. Typical examples include the C 12 -C 18 N-methylglucamides. See WO 9,206,154. Other surfactants derived from sugars include acid N-alkoxyamides polyhydroxy fatty acids, such as N- (3-methoxypropyl) glucamide C_ {12} -C_ {18}. You can also use the N-propyl a N-hexyl glucamides C_ {12} -C_ {18}. If you want a lot of training foam, C 10 -C 16 soaps of branched chain Mixtures of anionic and nonionic surfactants. In standard texts they are listed other useful conventional surfactants.

As detergent surfactants can also be use cationic surfactants and suitable surfactants of the type of quaternary ammonium are selected from compounds of [mono-N-alkyl (or alkenyl) C 6 -C 16, preferably C 6 -C 10] - ammonium, in the that the remaining positions of N are replaced by groups methyl, hydroxyethyl or hydroxypropyl.

As detergent surfactants, amphoteric surfactants can also be used, including aliphatic derivatives of secondary and tertiary heterocyclic amines; hybrid surfactants, including derivatives of aliphatic quaternary ammonium, phosphonium and sulfonium compounds; water soluble salts of α-sulphonated fatty acid esters; alkyl ether sufatos; water soluble salts of olefinsulfonates; β-alkyloxyalkanesulfonates; betaines that have the formula
R (R 1) 2 N + R 2 COO - in which R is a C 6 -C 18 hydrocarbyl group, preferably a C_ alkyl group {10} -C 16 or a group (acyl C 10 -C 16) amidoalkyl, each R 1 is typically C 1 -C 3 alkyl, preferably methyl, and R ^ {2} is a C 1 -C 5 hydrocarbyl group, preferably a C 1 -C 3 alkylene group, more preferably a C 1 -C 2 alkylene group. Examples of suitable betaines include (coconut acyl) amidopropyl dimethyl betaine, hexadecyldimethyl betaine, (C 12 -C 14 acyl) amidopropyl betaine, (C 8 -C 14 acyl) -amidohexyldiethyl betaine, 4 - [(C acyl] 14} -C_ {16}) methylamidodyethylammonium] -1-carboxybutane, (acyl C 16 -C 18) amidodimethyl betaine, (acyl C 12 -C 16) amidodiethyl betaine, (acyl C 12) - C 16) -amidopentanediethylbetaine and (acyl C 12 -C 16) amidodimethyl betaine. Preferred betaines are (C 12 -C 18) dimethylammonium hexanoate and the (C 10 -C 18 acyl) amido-propane (or ethane) dimethyl (or diethyl) betaines; and the sultains having the formula R (R 1) 2 N + R 2 SO 3 - in which R is a C 6 hydrocarbyl group - C 18, preferably a C 10 -C 16 alkyl group, more preferably a C 12 -C 13 alkyl group, each R 1 is typically C 1 -C 14 alkyl 3, preferably methyl, and R 2 is a C 1 -C 6 hydrocarbyl group, preferably an alkylene group or, preferably, C 1 -C 3 hydroxyalkylene. Examples of suitable sultains include (C 12 -C 14) dimethyl-ammonium-2-hydroxypropylsulfonate, (C 12 -C 14) amidopropylammonium-2-hydroxypropyl-sultaine, (C 12 -C_ {14}) dihydroxyethylammoniumpropanesulfonate and (C 16 -C 18) dimethylammonium-hexanesulfonate, with (C 12 -C 14) amidopropylammonium-2-hydroxypropyl-sultaine being preferred.

Fine powder

The amount of fine powder used in the First stage of the present procedure may be approximately 94 to 30%, preferably 86 to 54%, based on the total amount of starting material of the first stage. The fine starting powder of the present process is preferably selected from the group formed by ground sodium carbonate, sodium tripolyphosphate (STPP) powder, hydrated tripolyphosphate, hydrated sodium sulfates, aluminosilicates, layered crystalline silicates, nitrilotriacetates  (NTA), phosphates, precipitated silicates, polymers, carbonates, citrates, powdered surfactants (such as alkanesulfonic acids in dust) and an internal recirculated stream of dust from the method of the present invention, wherein the average diameter of the powder is 0.1 to 500 micrometers, preferably 1 to 300 micrometers, more preferably 5 to 100 micrometers. In the case of using hydrated STPP as the fine powder of the present invention, it prefers hydrated STPP at a level not less than 50%. The ion exchange materials of the type of aluminosilicates used as detergent additives they preferably have a high capacity Calcium ion exchange and high exchange rate of calcium ions. Without pretending to be limited by particular theory some, it is believed that such high capacity and high speed of Calcium ion exchange are a function of several factors interrelated derivatives of the method by which the aluminosilicate. In this regard, exchange materials ionic type aluminosilicates used herein Compositions are preferably produced according to Corkill et al., U.S. Patent No. 4,605,509 (Procter & Gamble), whose description is incorporated as a reference in the present memory

Preferably the ion exchange material of the aluminosilicate type is in "sodium" form since the hydrogenated and potassium forms of aluminosilicate do not have a capacity or exchange rate as high as the provided by the sodium form. Additionally, the material of ion exchange of the aluminosilicate type is preferably in dry form to facilitate the production of agglomerates of detergents such as those described herein. The ion exchange materials of the aluminosilicate type used in the present compositions preferably have particle diameters that optimize their effectiveness as additives detergents Here, the term "average diameter of particles "represents the average particle diameter of a particular aluminosilicate, determined by analytical techniques conventional, such as microscopic determination and microscopy scanning electronics (SEM). The preferred mean diameter of aluminosilicate particles is about 0.1 to about 10 micrometers, more preferably of about 0.5 to about 9 micrometers. The most preferably, the average particle diameter is about 1 to about 8 micrometers.

\hbox{Na _{z} [(AlO _{2} ) _{z} (SiO _{2} ) _{y} ]}

\cdotxH_{2}O en la que z e y son números enteros de por lo menos 6, la relación molar de z a y es de aproximadamente 1 a aproximadamente 5 y x es de aproximadamente 10 a aproximadamente 164. Más preferiblemente, el aluminosilicato tiene la fórmula Na_{12}[(AlO_{2})_{12}(SiO_{2})_{12}]\cdotxH_{2}O en la que x es de aproximadamente 20 a aproximadamente 30, preferiblemente aproximadamente 27. Estos aluminosilicatos preferidos están disponibles comercialmente, por ejemplo, bajo las designaciones de zeolita A, zeolita B y zeolita X. Alternativamente, materiales de intercambio iónico del tipo de aluminosilicatos naturales o sintéticos adecuados para uso en las presentes composiciones se pueden preparar como describen Krummel et al., patente de los Estados Unidos número 3.985.669, cuya descripción se incorpora como referencia en la presente memoria.Preferably, the ion exchange material of the aluminosilicate type has the formula

 ? {Na z [(AlO2) z (SiO2) y]]} 

• O 2 where z and y are integers of at least 6, the molar ratio of z and is from about 1 to about 5 and x is from about 10 to about 164. More preferably, the aluminosilicate has the formula Na_ { 12} [(AlO 2) 12 (SiO 2) 12] • x O in which x is from about 20 to about 30, preferably about 27. These preferred aluminosilicates are commercially available, for example, under the designations of zeolite A, zeolite B and zeolite X. Alternatively, ion exchange materials of the type of natural or synthetic aluminosilicates suitable for use in the present compositions can be prepared as described by Krummel et al., patent of the United States number 3,985,669, the description of which is incorporated by reference herein.

The aluminosilicates used herein compositions are also characterized by their ability to ion exchange, which is at least about 200 milliequivalents-grams of CaCO 3 hardness per gram, calculated on an anhydrous basis, and which is preferably in the range of approximately 300 to 353 milliequivalents-grams of CaCO 3 hardness per gram.

Finely atomized liquid

The amount of finely atomized liquid sprayed on the fluidized bed of the present process can be from about 1 to about 10% (active base), preferably from 2 to about 6% (active base), referred to the total amount of the final product obtained in the procedure of the present invention. The finely atomized liquid of This procedure can be selected from the group formed by liquid silicate, anionic or cationic surfactants in form liquid, aqueous or non-aqueous solutions of polymers, water and mixtures thereof. Other optional examples of the liquid finely atomized of the present invention can be solution of sodium carboxymethyl cellulose, polyethylene glycol (PEG) and solutions dimethylenetriaminepentamethylphosphonic acid (DETMP).

Preferable examples of solutions anionic surfactants that can be used as a thin liquid atomized in the present invention are HLAS of approximately 88-97% of active compound, NaLAS of approximately 30-50% active compound, solution of AE3S of approximately 28% active compound, silicate liquid of about 40-50% compound active, etc.

As a finely atomized liquid it is also they can use cationic surfactants and suitable surfactants of the quaternary ammonium type are selected from compounds of [mono-N-alkyl (or alkenyl) C 6 -C 16, preferably C 6 -C 10 {] ammonium in which the remaining positions of N are substituted by methyl groups, hydroxyethyl or hydroxypropyl.

Preferred examples of aqueous solutions or not aqueous polymers that can be used as a finely liquid atomized in the present invention are modified polyamines that They comprise a main chain that corresponds to the formula:

\uelm{N}{\uelm{\para}{H}}

---R]_{m}---[

\uelm{N}{\uelm{\para}{}}

---R]_{n}---NH_{2}[H 2 N --- R] n + 1} [

 \ uelm {N} {\ uelm {\ para} {H}} 

--- R] m --- [

 \ uelm {N} {\ uelm {\ para} {}} 

--- R] n --- NH2

which has a modified polyamine formula V_ {n + 1} W_ {m} Y_ {n} Z, or a main string corresponding to the formula

\uelm{N}{\uelm{\para}{H}}

---R]_{m}---[

\uelm{N}{\uelm{\para}{}}

---R]_{n}---[

\uelm{N}{\uelm{\para}{\uelm{R}{\uelm{\para}{}}}}

---R]_{k}---NH_{2}[H 2 N --- R] n-k + 1} --- [

 \ uelm {N} {\ uelm {\ para} {H}} 

--- R] m --- [

 \ uelm {N} {\ uelm {\ para} {}} 

--- R] n --- [

 \ uelm {N} {\ uelm {\ para} {\ uelm {R} {\ uelm {\ para} {}}}} 

--- R] k --- NH2

which has a modified polyamine formula V_ {n-k + 1} W_ {m} Y_ {n} Y 'k {Z}, where k is equal to or less than n, having said main chain of polyamine a molecular weight, before modification, greater than approximately 200 daltons, and in the what:

(i) V units are terminal units that They have the formula:

\delm{N}{\delm{\para}{E}}

---R---

\hskip1cm

o

\hskip1cm

E---

\melm{\delm{\para}{E}}{N ^{+} }{\uelm{\para}{E}}

---R—X^{-}

\hskip1cm

o

\hskip1cm

E---

\melm{\delm{\para}{E}}{N}{\uelm{ \uparrow }{O}}

---R---AND---

 \ delm {N} {\ delm {\ para} {E}} 

--- R ---

 \ hskip1cm 

or

 \ hskip1cm 

AND---

 \ melm {\ delm {\ para} {E}} {N ^ {}} {\ uelm {\ para} {E}} 

--- R — X ^ -

 \ hskip1cm 

or

 \ hskip1cm 

AND---

 \ melm {\ delm {\ para} {E}} {N} {\ uelm {\ uparrow} {O}} 

--- R ---

(ii) W units are units of the chain Main that have the formula:

\delm{N}{\delm{\para}{E}}

---R---

\hskip1cm

o

\hskip1cm

---

\melm{\delm{\para}{E}}{N ^{+} }{\uelm{\para}{E}}

---R—X^{-}

\hskip1cm

o

\hskip1cm

---

\melm{\delm{\para}{E}}{N}{\uelm{ \uparrow }{O}}

---R------

 \ delm {N} {\ delm {\ para} {E}} 

--- R ---

 \ hskip1cm 

or

 \ hskip1cm 

---

 \ melm {\ delm {\ para} {E}} {N ^ {}} {\ uelm {\ para} {E}} 

--- R — X ^ -

 \ hskip1cm 

or

 \ hskip1cm 

---

 \ melm {\ delm {\ para} {E}} {N} {\ uelm {\ uparrow} {O}} 

--- R ---

(iii) Y units are units of Branches that have the formula:

\delm{N}{\delm{\para}{}}

---R---

\hskip1cm

o

\hskip1cm

---

\melm{\delm{\para}{}}{N ^{+} }{\uelm{\para}{E}}

---R—X^{-}

\hskip1cm

o

\hskip1cm

---

\melm{\delm{\para}{}}{N}{\uelm{ \uparrow }{O}}

---R------

 \ delm {N} {\ delm {\ para} {}} 

--- R ---

 \ hskip1cm 

or

 \ hskip1cm 

---

 \ melm {\ delm {\ para} {}} {N + {}} {\ uelm {\ para} {E}} 

--- R — X ^ -

 \ hskip1cm 

or

 \ hskip1cm 

---

 \ melm {\ delm {\ para} {}} {N} {\ uelm {\ uparrow} {O}} 

--- R ---

Y

(iv) Z units are terminal units that They have the formula:

\delm{N}{\delm{\para}{E}}

---E---

\hskip1cm

o

\hskip1cm

---

\melm{\delm{\para}{E}}{N ^{+} }{\uelm{\para}{E}}

---E—X^{-}

\hskip1cm

o

\hskip1cm

---

\melm{\delm{\para}{E}}{N}{\uelm{ \uparrow }{O}}

---E------

 \ delm {N} {\ delm {\ para} {E}} 

---AND---

 \ hskip1cm 

or

 \ hskip1cm 

---

 \ melm {\ delm {\ para} {E}} {N ^ {}} {\ uelm {\ para} {E}} 

--- E — X ^ {}

 \ hskip1cm 

or

 \ hskip1cm 

---

 \ melm {\ delm {\ para} {E}} {N} {\ uelm {\ uparrow} {O}} 

---AND---

in which the linker units R of the chain Main are selected from the group formed by alkylene C 2 -C 12, alkenylene C 4 -C 12, hydroxyalkylene C 3 -C 12, dihydroxyalkylene C 4 -C 12, dialkylarylene C 8 -C 12, - (R 1 O) x R 1 -, - (R 1 O) x R 5 (OR 1) x -, - [CH 2 CH (OR 2) CH 2 O] z (R 1 O) and R 1 [OCH 2 CH (OR ^ {2} CH2] w -,  -C (O) (R 4) r C (O) -, -CH 2 CH (OR 2) CH 2 - and mixtures of the same, in which R1 is alkylene C 2 -C 6 or mixtures thereof; R2 is hydrogen, - (R 1 O) x B or mixtures thereof; R 3 is C 1 -C 18 alkyl, arylalkyl C 7 -C 12, alkyl substituted aryl C 7 -C 12, aryl C 6 -C 12 or mixtures thereof; R 4 is C 1 -C 12 alkylene, C4-C12 alkenylene, arylalkylene C 8 -C 12, arylene C 6 -C 10 or mixtures thereof; R 5 is C 1 -C 12 alkylene, hydroxyalkylene C 3 -C 12, dihydroxyalkylene C 4 -C 12, dialkylarylene C_ {8} -C_ {12}, -C (O) -, -C (O) NHR 6 NHC (O) -, -R 1 (OR 1) -, -C (O) (R 4) r C (O) -, -CH 2 CH (OH) CH 2 -, -CH 2 CH (OH) CH 2 O (R 1 O) and R 1 OCH 2 CH (OH) CH 2 - or mixtures thereof; R 6 is alkylene C 2 -C 12 or C 6 -C 12 arylene; the E units are selected from the group consisting of hydrogen, alkyl C 1 -C 22, alkenyl C 3 -C 22, arylalkyl C 7 -C 22, hydroxyalkyl C 2 -C 22, - (CH 2) p CO 2 M, - (CH 2) q SO 3 M, -CH (CH 2 CO 2 M) CO 2 M, - (CH 2) p PO 3 M, - (R 1 O) x B, -C (O) R3 or mixtures thereof; B is hydrogen, C 1 -C 6 alkyl, - (CH 2) q SO 3 M, - (CH 2) p CO 2 M, - (CH 2) q (CHSO 3 M) CH 2 SO 3 M, - (CH 2) q (CHSO 2 M) CH 2 SO 3 M, - (CH 2) p PO 3 M, -PO 3 M or mixtures of the themselves; M is hydrogen or a water soluble cation in quantity enough to balance the load; X is a water soluble anion; m has the value of 4 to 400; n has the value from 0 to 200; p has the value from 1 to 6; q has the value from 0 to 6; r has the value 0 or one; w has the value 0 or 1; x has the value from 1 to 100; and has the value from 0 to 100; and z has the value 0 or 1. An example of the most preferred polyethyleneimines is a polyethyleneimine having a molecular weight of 1,800 and that has been modified by ethoxylation to a degree of approximately 7 ethyleneoxy moieties by nitrogen (PEI 1899, E7). It is preferable that the polymer solution is a precomplex with an anionic surfactant, such as NaLAS.

Other preferable examples of aqueous solutions or non-aqueous polymers that can be used as a finely liquid atomized in the present invention are dispersants of the type of polymeric polycarboxylates that can be prepared by polymerizing or copolymerizing suitable unsaturated monomers, preferably in its acid form. Monomeric unsaturated acids that can be polymerize to form suitable polymeric polycarboxylates include acrylic acid, maleic acid (or maleic anhydride), acid fumaric acid, itaconic acid, aconitic acid, mesaconic acid, acid citraconic and methyleneomalonic acid. The presence of segments monomers that do not contain carboxylate radicals, such as vinyl methyl ether, styrene, ethylene, etc., in these polycarboxylates polymeric is appropriate with the proviso that said segments do not constitute more than about 40% by weight of the polymer.

Preferred are polycarboxylates homopolymers that have molecular weights greater than 4,000 described below. Homopolymeric Polycarboxylates particularly suitable can be derived from acrylic acid. Such acrylic acid based polymers that are useful in Present compositions are the water soluble salts of acid polymerized acrylic. The average molecular weight of said polymers in acid form it preferably ranges from more than 4,000 to 10,000, preferably from more than 4,000 to 7,000 and most preferably from more than 4,000 to 5,000. The water soluble salts of said Acrylic acid polymers may include, for example, salts. of alkali metals, ammonium and substituted ammonium.

Polycarboxylates can also be used. copolymers, such as acrylic / acid based copolymers Maleic Such materials include water soluble salts of copolymers of acrylic acid and maleic acid. Molecular weight medium of said acidic copolymers generally varies from about 2,000 to 100,000, more preferably of approximately 5,000 to 75,000 and most preferably of approximately 7,000 to 65,000. The ratio of acrylate segments to maleate segments in said copolymers will generally vary from about 30: 1 to about 1: 1, more preferably of approximately 10: 1 to 2: 1. The water soluble salts of said Acrylic / maleic acid polymers may include, by example, alkali metal, ammonium and ammonium salts replaced. It is preferable that the solution of the polymers before mentioned be a precomplex with an anionic surfactant, such as THE.

Auxiliary detergent ingredients

The starting detergent material of the present procedure may include additional detergent ingredients and / or any number can be incorporated into the detergent composition of additional ingredients during later stages of the present process. These auxiliary ingredients include other additives detergency builders, bleaches, activators bleaches, intensifiers or foam suppressants, agents anti-corrosion and anti-slip, stain suspension agents, staining agents, germicides, agents pH regulators, alkalinity sources that are not additive detergency builders, chelating agents, clays smectites, enzymes, enzyme stabilizing agents and perfumes. See U.S. Patent 3,936,537, issued on 3 February 1976 to Baskerville Jr. et al., incorporated as Reference herein.

The detergency builder additives are they can generally select from the various phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxysulfonates, polyacetates, carboxylates and polycarboxylates Water soluble alkali metal, ammonium or substituted ammonium. From these salts are preferred alkali metal salts, especially sodium. Preferred for use in the present compositions are those phosphates, carbonates, fatty acid salts C 10 -C 18, polycarboxylates and mixtures of the same. More preferred are sodium tripolyphosphate, pyrophosphate tetrasodium, citrates, tartratomono- and disuccinates and mixtures of the same (see below).

Compared to amorphous sodium silicates, the layered crystalline sodium silicates have a capacity Clearly better calcium and magnesium ion exchange. Further, layered sodium silicates prefer magnesium ions to calcium ions, a necessary feature to ensure that substantially all the "hardness" is removed from the water of washed. However, these layered crystalline sodium silicates they are generally more expensive than amorphous silicates and than others detergency builder additives. Consequently, for provide an economically viable detergent, it should be properly determine the proportion of sodium silicates Layered crystals. Said layered crystalline silicates are discussed in U.S. Patent No. 4,605,509, Corkill et al., Incorporated hereinbefore as reference.

Specific examples of inorganic phosphates useful as detergency builders are tripolyphosphates, pyrophosphates, polymeric metaphosphates that have a degree of polymerization of approximately 6 to 21 and sodium orthophosphates and Potassium Examples of polyphosphonates useful as additives detergency builders are the sodium and potassium salts of ethylenediphosphonic acid, the sodium and potassium salts of the acid ethane-1-hydroxy-1,1-diphosphonic and the sodium and potassium salts of the acid ethane-1,1,2-triphosphonic. Others phosphorous builder detergent compounds are described in 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 as a reference herein.

Examples of additives improving the non-phosphorus inorganic detergents are tetraborate decahydrate and silicates having a weight ratio of SiO2 to oxide of alkali metal from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4. Non-phosphorous organic detergency builder additives Water soluble, useful in the present compositions, include the various polyacetates, carboxylates, polycarboxylates and alkali metal, ammonium and substituted ammonium polyhydroxysulfonates. Examples of polyacetates and polycarboxylates are sodium salts, potassium, lithium, ammonium and substituted ammonium acids ethylenediaminetetraacetic, nitrilotriacetic, oxidisuccinic, Melitic, benzene polycarboxylic and citric.

In U.S. Patent 3,308,067, Diehl, granted on March 7, 1967, whose description is incorporated herein by reference, are described detergency builder additives of the polycarboxylate type polymeric Such materials include water soluble salts of homo- and copolymers of aliphatic carboxylic acids, such as acid maleic acid, itaconic acid, mesaconic acid, fumaric acid, acid aconitic, citraconic acid and methylenomonic acid. Some of These materials are useful as soluble anionic polymers in water, described above, but only intimately mixed with an anionic surfactant that is not a soap.

Other polycarboxylates suitable for use in Present compositions are the polyacetalcarboxylates described in U.S. Patents 4,144,226, issued on 13 March 1979 to Crutchfield et al., and 4,246,495, granted on 27 March 1979 to Crutchfield et al., both incorporated as Reference herein. These polyacetalcarboxylates are can be prepared by mixing an ester under polymerization conditions of glyoxylic acid and a polymerization initiator. The ester resulting polyacetalcarboxylate then binds to final groups chemically stable to stabilize the polyacetalcarboxylate against rapid depolymerization in alkaline solution, it convert to the corresponding salt and add to the composition Detergent. Particularly preferred are the ether carboxylates that comprise a combination of tartratomonosuccinate and tartratodisuccinate, described in US Pat. 4,663,071, Bush et al., Issued May 5, 1987, whose description is incorporated herein by reference memory.

Bleaching and activating agents are described of bleaching agents in U.S. Patents 4,412,934, Chung et al., Granted on November 1, 1983, and 4,483,781, Hartman, granted on November 20, 1984, incorporated both as a reference herein. Agents are also described. Chelators in U.S. Patent 4,663,071, Bush et al., from column 17, line 54, to column 18, line 68, incorporated herein by reference. The foam modifiers are other optional ingredients and it described in U.S. Patents 3,933,672, granted on January 20, 1976 to Bartoletta et al., and 4,136,045, granted on January 23, 1979 to Gault et al., incorporating both as a reference herein.

Smectite clays suitable for use in present compositions are described in the United States patent 4,762,645, Tucker et al., Issued August 9, 1988, from column 6, line 3, to column 7, line 24. They are listed additional detergency builder additives suitable for use in the present compositions in the Baskerville patent, of column 13, line 54, to column 16, line 16, and in the patent of the United States 4,663,071, Bush et al., granted May 5 of 1987, both incorporated herein by reference memory.

       \ newpage
    

Optional stages of the procedure

Optionally, the procedure may comprise the step of spraying an optional binder in one or more of one of the first, second and / or third mixer of this invention. A binder is added in order to improve the agglomeration for providing a "binder" or "adherent" of detergent components. The binder is preferably selects from the group consisting of water, surfactants  anionic, nonionic surfactants, liquid silicates, polyethylene glycol, polyvinylpyrrolidone, polyacrylates, acid citrus and mixtures thereof. Other suitable binders, including those related herein, are described in Beerse et al., U.S. Patent No. 5,108,646 (Procter & Gamble), whose description is incorporated as Reference herein.

Other optional stages contemplated by the present process include screening the agglomerates of detergents larger than desired in an appliance screening that can take a variety of forms, including, but without limitation, conventional sieves chosen for the Desired particle size of the final detergent product. Other Optional stages include conditioning the agglomerates of detergents subject to additional drying by apparatus described above.

Another optional stage of the present procedure is finish the resulting detergent agglomerates by means of a diversity of processes, including spraying and mixing with others conventional detergent ingredients. For example, the stage of finish includes spraying perfumes, optical brighteners and enzymes on the finished agglomerates, to provide a composition more complete detergent. These techniques and ingredients are good. known in the art.

Another optional stage of the procedure is a process of structuring a paste of a surfactant, for example, harden an aqueous paste of an anionic surfactant by incorporating a paste hardener material using an extruder, before procedure of the present invention.

To make the present invention understood more easily, reference is made to the following examples that they are only illustrative but not limiting the scope of the present invention

Examples Example 1

The following is an example to get agglomerates that have a high density using a Lödige mixer CB (CB-30), followed by a Lödige KM mixer (KM-600) and followed by a fluid bed apparatus to get more agglomeration.

Stage 1

In a CB-30 mixer, disperse 250-270 kg / h of an aqueous paste of a surfactant [(coconut fatty alcohol C 12 -C 18) sulfate; 71.5% of  active compound] together with 220 kg / h of sodium tripolyphosphate  powder (average particle size 40-75 micrometers), 160-200 kg / h sodium carbonate ground (average particle size 15 micrometers), 80-120 kg / h of ground sodium sulfate (medium size of particles 15 micrometers) and 200 kg / h of recirculated current internal dust. The surfactant paste is fed to a temperature of about 40 to 52 ° C and the powders feed at room temperature. The conditions of the mixer CB-30 are the following:

Average time of permanence 10-18 seconds Speed peripheral 7.5-14 m / s Condition of Energy 0.5-4 kJ / kg Speed mixer 550-900 rpm Temperature shirt 30ºC

Stage 2 (i)

The agglomerates from the mixer CB-30 are fed to the mixer KM-600 to achieve greater agglomeration, rounded and growth of agglomerates. They are added to the mixer 15-30 kg / h of HLAS [an acid precursor of a (alkyl  linear C 11 -C 18) benzenesulfonate; 94-97% active compound] and 0-60 kg / h of ground sodium carbat (average particle size 15 micrometers) To reduce the amount of size agglomerates higher than desired, KM mixer cutters can be used. The KM mixer conditions are as follows:

Average time of permanence 3-6 minutes Condition of Energy 0.15-2 kJ / kg Speed mixer 100-150 rpm Temperature shirt 30-40 ° C

       \ newpage
    

Stage 3

The agglomerates from the KM mixer are feed a fluid bed drying apparatus for drying, rounding and growth of agglomerates. To the drying apparatus of fluid bed at 35 ° C 20-80 kg / h of silicate are added  liquid (43% solids; R 2.0). The conditions of the device Drying fluid bed are as follows:

Average time of permanence 2-4 minutes Bed height not fluidized 200 mm Spray droplet size smaller than 50 micrometers Height of sprayed 175-250 mm (above the plate of distribution) Speed of fluidization 0.4-0.8 m / s Temperature bed 40-70 ° C

The granules resulting from stage 3 have a density of approximately 700 g / l and can be subjected optionally to optional cooling processes, separation by sizes and / or crushing.

Example 2

The following is an example to get agglomerates that have a high density using a Lödige mixer CB (CB-30), followed by a Lödige KM mixer (KM-600) and a Schugi mixer FX-160 and finally a fluid bed apparatus to get more agglomeration.

Stage 1

In a CB-30 mixer, disperse 15-30 kg / h of HLAS [an acid precursor of a (linear alkyl C 11 -C 18) benzenesulfonate; 95% of active compound] at approximately 50 ° C and 20 kg / h of (alkyl C 10 -C 18) liquid alkoxysulfates (AE 3 S; EO-3; 28% active compound) together with 220 kg / h of sodium tripolyphosphate powder (average size of particles 40-75 micrometers), 160-200 kg / h of ground sodium carbonate (size particle size 15 micrometers), 80-120 kg / h of ground sodium sulfate (average particle size 15 micrometers) and 200 kg / h of internal recirculated dust stream. The pasta of Surfactants are fed at a temperature of approximately 40 to 52 ° C and the powders are fed at room temperature. The CB-30 mixer conditions are the following:

Average time of permanence 10-18 seconds Speed peripheral 7.5-14 m / s Condition of Energy 0.5-4 kJ / kg Speed mixer 550-900 rpm Temperature shirt 30ºC

Stage 2 (i)

The agglomerates from the mixer CB-30, which have a density of 600-700 g / l, are fed to the mixer KM-600 to achieve greater agglomeration, rounded and growth of agglomerates. They are added to the mixer 0-60 kg / h of ground sodium carbonate (medium size 15 micrometer particles) or can also be added to the KM 0-30 kg / h Zeolite mixer. To reduce the quantity of agglomerates larger than desired can be use KM mixer cutters. KM mixer conditions They are as follows:

Average time of permanence 3-6 minutes Condition of Energy 0.15-2 kJ / kg Speed mixer 100-150 rpm Temperature shirt 30-40 ° C

Stage 2 (ii)

The agglomerates from the KM mixer are feed the Schugi FX-160 mixer. In the Schugi mixer disperses 30 kg / h of HLAS [an acid precursor of a (linear alkyl C 11 -C 18) benzenesulfonate; 95% of active compound] in the form of a finely atomized liquid at a temperature of about 50 to 80 ° C. The Schugi mixer is add 20-80 kg / h of sodium carbonate. The Schugi mixer conditions are as follows:

Average time of permanence 0.2-5 seconds Speed peripheral 16-26 m / s Condition of Energy 0.15-2 kJ / kg Speed mixer 2,000-3,200 rpm

Stage 3

The agglomerates from the Schugi mixer they are fed to a fluid bed drying apparatus for drying, rounding and growth of agglomerates. To the drying apparatus of fluid bed at 35 ° C 20-80 kg / h of silicate are added  liquid (43% solids; R 2.0). The conditions of the device Drying fluid bed are as follows:

Average time of permanence 2-4 minutes Bed height not fluidized 200 mm Spray droplet size smaller than 50 micrometers Height of sprayed 175-250 mm (above the plate of distribution) Speed of fluidization 0.4-0.8 m / s Temperature bed 40-70 ° C

The granules resulting from stage 3 have a density of approximately 650 g / l and can be subjected optionally to optional cooling processes, separation by sizes and / or crushing.

Example 3

The following is an example to get agglomerates that have a high density using a Lödige mixer CB (CB-30), followed by a Lödige KM mixer (KM-600) and a Schugi mixer FX-160 and finally a fluid bed apparatus to get more agglomeration.

Stage 1

In a CB-30 mixer, disperse 15-30 kg / h of HLAS [an acid precursor of a (linear alkyl C 11 -C 18) benzenesulfonate; 95% of active compound] at approximately 50 ° C and 250-270 kg / h of an aqueous paste of a surfactant [(coconut fatty alcohol C 12 -C 18) sulfate; 71.5% compound active] together with 220 kg / h of sodium tripolyphosphate powder (average particle size 40-75 micrometers), 160-200 kg / h of ground sodium carbonate (size particle size 15 micrometers), 80-120 kg / h of ground sodium sulfate (average particle size 15 micrometers) and 200 kg / h of internal recirculated dust stream. The pasta of Surfactants are fed at a temperature of approximately 40 to 52 ° C and the powders are fed at room temperature. The CB-30 mixer conditions are the following:

Average time of permanence 10-18 seconds Speed peripheral 7.5-14 m / s Condition of Energy 0.5-4 kJ / kg Speed mixer 550-900 rpm Temperature shirt 30ºC

Stage 2 (ii)

The agglomerates from the mixer CB-30 are fed to the mixer KM-600 to achieve greater agglomeration, rounded and growth of agglomerates. To the mixer KM-600 also adds 60 kg / h of sodium carbonate ground (average particle size 15 micrometers). To reduce the quantity of agglomerates larger than desired can be use KM mixer cutters. The conditions of the mixer KM-600 are as follows:

Average time of permanence 3-6 minutes Condition of Energy 0.15-2 kJ / kg Speed mixer 100-150 rpm Temperature shirt 30-40 ° C

Stage 2 (i)

The agglomerates from the mixer KM-600 are fed to the Schugi mixer FX-160 To the Schugi mixer at a temperature of approximately 30-40ºC add 35 kg / h of AE3S liquid (28% active compound) as a liquid finely atomized. To the Schugi mixer are added 20-80 kg / h of sodium carbonate. The conditions of Schugi mixer are as follows:

Average time of permanence 0.2-5 seconds Speed peripheral 16-26 m / s Condition of Energy 0.15-2 kJ / kg Speed mixer 2,000-3,200 rpm

Stage 3

The agglomerates from the Schugi mixer they are fed to a fluid bed drying apparatus for drying, rounding and growth of agglomerates. To the drying apparatus of fluid bed at 35 ° C 20-80 kg / h of silicate are added  liquid (43% solids; R 2.0). The conditions of the device Drying fluid bed are as follows:

Average time of permanence 2-4 minutes Bed height not fluidized 200 mm Spray droplet size smaller than 50 micrometers Height of sprayed 175-250 mm (above the plate of distribution) Speed of fluidization 0.4-0.8 m / s Temperature bed 40-70 ° C

The resulting agglomerates of the drying apparatus of fluid bed are fed to a bed cooling apparatus fluid. The conditions of the fluid bed cooling apparatus They are as follows:

Average time of permanence 2-4 minutes Bed height not fluidized 200 mm Speed of fluidization 0.4-0.8 m / s Temperature bed 12-60ºC

The granules resulting from stage 3 have a density of approximately 700 g / l and can be subjected optionally to optional processes of separation by sizes and trituration.

Claims (9)

1. An agglomeration procedure to prepare a granular detergent composition having a density of at minus 600 g / l, which includes the steps of: (a) disperse a surfactant and coat the surfactant with a fine powder having a diameter of 0.1 to 500 micrometers in a first mixer in which the conditions of the mixer include (i) an average residence time of 2 to 50 seconds, (ii) a peripheral speed of 4 to 25 m / s and (iii) a energy condition of 0.15 to 7 kJ / kg, in which some first agglomerates, and (b) perfectly mixing the first agglomerates in a second mixer in which the conditions of the mixer include (i) an average residence time of 0.5 to 15 minutes and (ii) an energy condition of 0.15 a
7 kJ / kg, in which a few agglomerated seconds are formed, characterized in that the procedure comprises (c) granulate the second agglomerates in a fluid bed apparatus spraying at the same time on the bed droplets of a liquid detergent material in an amount of up to 20% and in which the conditions of the fluid bed apparatus include (i) an average residence time of 1 to 10 minutes, (ii) a height of the non-fluidized bed from 100 to 300 mm, (iii) a size of the droplets sprayed not exceeding 50 micrometers, (iv) a height spray from 175 to 250 mm, (v) a fluidization rate of 0.2 at 1.4 m / s and (vi) a bed temperature of 12 to 100 ° C. 2. An agglomeration procedure to prepare a granular detergent composition having a density of at least 600 g / l, which includes the steps of: (a) disperse a surfactant and coat the surfactant with a fine powder having a diameter of 0.1 to 500 micrometers in a first mixer in which the conditions of the mixer include (i) an average residence time of 2 to 50 seconds, (ii) a peripheral speed of 4 to 25 m / s and (iii) a energy condition of 0.15 to 7 kJ / kg, in which some first agglomerates, and (b) perfectly mixing the first agglomerates in a second mixer in which the conditions of the mixer include (i) an average residence time of 0.5 to 15 minutes and (ii) an energy condition of 0.15 a
7 kJ / kg, in which a few agglomerated seconds are formed, characterized in that the procedure comprises (b ') spray on the second agglomerates a finely atomized liquid, in a third mixer in which Mixer conditions include (i) an average time of permanence of 0.2 to 5 seconds, (ii) a peripheral speed of 10 at 30 m / s and (iii) an energy condition of 0.15 to 5 kJ / kg, in the that some agglomerated third parties are formed, and (c) granulate the third agglomerates in a fluid bed apparatus spraying at the same time on the bed droplets of a liquid detergent material in an amount of up to 20% and in which the conditions of the fluid bed apparatus include (i) an average residence time of 1 to 10 minutes, (ii) a height of the non-fluidized bed from 100 to 300 mm, (iii) a size of the droplets sprayed not exceeding 50 micrometers, (iv) a height spray from 175 to 250 mm, (v) a fluidization rate of 0.2 at 1.4 m / s and (vi) a bed temperature of 12 to 100 ° C. 3. An agreement agglomeration procedure with claim 1 or claim 2, wherein in the bed fluidized is sprayed 2 to 10% (based on active compound) of a liquid detergent material. 4. A procedure according to any preceding claim, wherein the liquid detergent material Spray is selected from silicate solutions, surfactant anionic, cationic surfactant and polymer. 5. The procedure according to the claim 2, wherein an excess fine powder is formed in the stage (a) and / or in stage (b), and in which the fine dust in excess is added to step (b '). 6. A procedure in accordance with the claims 1 or 2, wherein an aqueous or non-aqueous solution of a polymer is dispersed with said surfactant of the step (to). 7. A procedure in accordance with the claims 1 or 2, wherein the fine powder is selected from group consisting of sodium carbonate, sodium tripolyphosphate powder, hydrated tripolyphosphate, sodium sulfates, aluminosilicates, layered crystalline silicates, phosphates, precipitated silicates, polymers, carbonates, citrates, nitrilotriacetates, surfactants powder and mixtures thereof. 8. A method according to claim 2, in that the finely atomized liquid is selected from the group that It consists of liquid silicates, anionic surfactants, cationic surfactants, aqueous polymer solutions, solutions non-aqueous polymer, water and mixtures thereof. 9. A procedure in accordance with the claims 1 or 2, wherein it is also added to step (a) an internal recirculated stream of dust from the apparatus of fluidization.