DE69726440T2 - METHOD FOR PRODUCING A DETERGENT COMPOSITION WITHOUT A TOWER METHOD - Google Patents

Description

Territory of invention

The present invention relates to a non-tower process for making a particulate detergent composition. The invention is even more specific to a continuous process directed while its detergent agglomerates by feeding in a surfactant and coating materials in a number of mixers become. The process provides a free flowing detergent composition their density in a wide range to meet user needs can be set and which is commercially marketable.

background the invention

Until recently existed within the detergent industry has a significant interest in laundry detergents, which are "compact" and therefore a have a low dosage volume. To make this so To facilitate the low-dose detergents mentioned, many Attempts have been made to produce detergents with a high bulk density, for example with a density of 600 g / l or higher. After low-dose detergents there is currently a great demand in that they are the raw material sources gentle and can be sold in small packages, which for the Consumers are more convenient. The degree to which modern detergent products inherently must be "compact" however open. Actually prefer many consumers, especially in developing countries their respective washing processes still higher Dosing.

There are basically two main types of Processes by which detergent granules or powders are made can be. The first type of process involves spray drying an aqueous one Detergensaufschlämmung in a spray drying tower, a highly porous one To produce detergent granules (e.g. a tower process for detergent compositions with low density). In the second type of procedure, the different Detergent ingredients mixed dry, after which they are mixed with a binder, such as a nonionic or anionic surfactant, are agglomerated, to produce a high density detergent composition (e.g. B. Agglomerative process for High density detergent compositions). With the above two methods are the main factors affecting the density of the resulting Detergent composition determine the shape, parosity and particle size distribution the granules, the density of the various raw materials, the shape of the various starting materials and their respective chemical Composition.

There have been many attempts in the art to provide methods that increase the density of detergent granules and powder. Particular attention was paid to the compression of spray-dried granules by post-tower treatment. For example, an experiment involves a batch process in which spray-dried or granulated detergent powders, which contain sodium tripolyphosphate and sodium sulfate, are compacted and spheronized in a Marumerizer ^® . This apparatus comprises a substantially horizontal, roughened, rotating plate which is arranged inside and on the bottom of a substantially vertical, smooth-walled cylinder. However, this process is de facto a batch process and is therefore less suitable for the production-scale production of detergent powders. More recently, other attempts have been made to provide continuous methods for increasing the density of "post tower" or spray dried granules. Such processes typically require a first device which pulverizes or grinds the granules and a second device which increases the density of the pulverized granules by agglomeration. Although these processes achieve the desired increase in density by treating or densifying "post tower" or spray dried granules; their ability to use higher surfactant concentrations without subsequent coating steps is limited. In addition, the treatment or compression of "post-tower" products is not preferable in terms of economy (high capital expenditure) and the complexity of the operation. In addition, all of the aforementioned processes are mainly aimed at the compression or other processing of spray-dried granules. At present, the respective amounts and types of materials which have been subjected to spray drying processes in the manufacture of detergent granules are limited. For example, it was difficult to achieve high levels of surfactant in the resulting detergent composition, a feature that facilitates the more efficient manufacture of detergents. It would therefore be desirable to have a process capable of making detergent compositions without the limitations of conventional spray drying techniques.

To this end, the art is also full of disclosures about processes involving agglomerated detergent compositions. For example, attempts have been made to agglomerate detergent builders by mixing with zeolite and / or layered silicates to form free flowing agglomerates. Although such attempts suggest that their methods can be used form agglomerates, they do not provide a mechanism by which detergent starting materials in the form of pastes, liquids and dry materials can be effectively agglomerated into solid, free-flowing detergent agglomerates.

Accordingly, there exists in the field still need for an agglomeration (non-tower) process for the continuous production of a detergent composition with high density, which directly from the detergent starting materials is provided and its density preferably by adjustment of the process conditions can be achieved. It always exists still need a process that is more efficient, flexible and is more economical to produce detergents on a production scale facilitate (1) in terms of flexibility of maximum density of finished composition, and (2) in terms of flexibility in terms on the incorporation of different types of detergent ingredients in the process, in particular detergent components in liquid form.

The following references refer to the compression of spray-dried granules: Appel et al., U.S. Patent 5,133,924 (Lever); Bortolotti et al., U.S. Patent 5,160,657 (Lever); Johnson et al., BP-A 1,517,713 (Unilever); and Curtis, EP application 451 894.

The following references relate to the production of detergents by agglomeration: Beujean et al., Publication number WO 93/23523 (Henkel); Lutz et al., U.S. 4,992,079 (FMC Corporation); Porasik et al., U.S. 4,427,417 (Korex); Beerse et al., U.S. 5,108,646 (Procter &Gamble); Capeci et al., U.S. Patent 5,366,652 (Procter &Gamble); Hollingworth et al., EP-A 351 937 (Unilever); Swatling et al., U.S. 5,205,958; Dhalewadikar et al., Publication number WO 96/04359 (Unilever).

The publication number WO 93/23523 (Henkel) describes, for example, a process that involves pre-agglomeration with a slow-running mixer and an additional one Agglomeration stage with a high-speed mixer, to a high density detergent composition of less than To obtain 25 wt .-% granules with a diameter of over 2 mm. UNITED STATES 4,427,417 (Korex) describes a continuous process for Agglomeration, which cakes and agglomerates that are too large reduced.

US-A 5,554,587 discloses a method open for the production of detergent compositions, which the Feeding air into a mixer during the agglomeration of one Includes surfactant paste and other detergent ingredients so that at least a small amount of water from the surfactant paste from the air is absorbed.

WO-A 96/09370 sets out a method for the production of high density detergent compositions open, comprising the steps of mixing a surfactant paste and dry detergent ingredients in a mixer to produce first agglomerates to build; Conditioning the first agglomerates to form second agglomerates to obtain with a specific particle size; Return any Agglomerates that do not have the desired particle size for further agglomeration to create second agglomerates with the desired To obtain particle size; Mixing detergent ingredients into the second agglomerates to to form a high density detergent composition.

None of the existing ones in the field The process provides all the advantages and benefits of the present Invention ready.

Summary the invention

The present invention is sufficient for everyone aforementioned Requirements in the field by providing a process which is a granular High density detergent composition provides. The present Invention is sufficient also all of the above Requirements in the field of flexibility regarding maximum density of the finished composition from agglomeration (e.g., non-tower) process, by providing a process, which is a granular Detergent composition provides. The process uses none the currently usual Spray drying towers with their Limits in the manufacture of compositions with a high surfactant load. The method according to the invention is also more efficient economical and flexible with regard to the variety of detergent compositions, which can be produced with this method. The procedure is beyond Environmental considerations in this regard accessible, when it didn't use spray drying towers which are typically fine particulate and volatile organic Connections to the atmosphere submit.

The term "agglomerates" as used herein refers to particles formed by agglomerating raw materials with binders such as surfactants and / or inorganic solutions / organic solvents and polymer solutions. As used herein, the term "granulating" refers to carefully fluidizing the agglomerates to produce free-flowing, granular, round-shaped agglomerates. The term "mean residence time", as used herein, refers to the following definition: mean residence time (h) = mass (kg) / flow rate (kg / h) All percentages used herein are expressed in "weight percent" unless otherwise stated , All ratios are weight ratios unless otherwise stated. "Comprehensive" as used herein means that Steps and other components that do not adversely affect the result can be added. This term includes the terms "consisting of" and "consisting essentially of".

• (a) Dispergieren eines Tensids und Beschichten des Tensids mit feinem Pulver eines Durchmessers von 0,1 bis 500 um, während das mit feinem Pulver beschichtete Tensid mit einer feinzerstäubter Flüssigkeit benetzt wird, in einem Mischer, wobei Bedingungen des Mischers beinhalten (i) 0,2 bis 5 Sekunden mittlere Verweilzeit, (ii) 15 bis 26 m/s Spitzengeschwindigkeit und (iii) 0,2 bis 3 kj/kg Energiezustand, wobei erste Agglomerate gebildet werden;
• (b) sorgfaltiges Mischen der ersten Agglomerate in einem Mischer mit Choppern, wobei Bedingungen des Mischers beinhalten (i) 0,5 bis 15 Minuten mittlere Verweilzeit und (ii) 0,15 bis 7 kj/kg Energiezustand, wobei zweite Agglomerate gebildet werden; und
• (c) Granulieren der zweiten Agglomerate in einem Wirbelbett-Trockner und Wirbelbett-Kühler, wobei Bedingungen jeder der Fluidisierungsvorrichtungen umfassen (i) 1 bis 10 Minuten mittlere Verweilzeit, (ii) 100 bis 300 mm Tiefe an nichtfluidisiertem Bett, (iii) nicht mehr als 50 μm Tropfensprühgröße, (iv) 175 bis 250 mm Sprühhöhe, (v) 0,2 bis 1,4 m/s Fluidisierungsgeschwindigkeit und (vi) 12 bis 100°C Betttemperatur, wobei die mittlere Verweilzeit in Schritt (c) insgesamt 2 bis 12 Minuten beträgt, und wobei eine Beschichtungsmittel, gewählt aus der Gruppe, bestehend aus Aluminosilicaten, Silicaten, Carbonaten und Mischungen hiervon zu Schritt (c) gegeben wird, entweder direkt nach dem Wirbelbett-Kühler oder Wirbelbett-Trockner; und/oder zwischen dem Wirbelbett-Trockner und Wirbelbett-Kühler; und/oder direkt zu dem Wirbelbett-Trockner.

In accordance with one aspect of the invention, there is provided a method of making a granular detergent composition having a density of at least 600 g / l, comprising the steps of:

• (a) dispersing a surfactant and coating the surfactant with fine powder of 0.1 to 500 µm in diameter while the surfactant coated with fine powder is wetted with a fine atomized liquid in a mixer, conditions of the mixer including (i) 0 , 2 to 5 seconds mean residence time, (ii) 15 to 26 m / s top speed and (iii) 0.2 to 3 kj / kg energy state, whereby first agglomerates are formed;
• (b) carefully mixing the first agglomerates in a mixer with choppers, the conditions of the mixer including (i) 0.5 to 15 minutes mean residence time and (ii) 0.15 to 7 kj / kg energy state, whereby second agglomerates are formed; and
• (c) granulating the second agglomerates in a fluid bed dryer and fluid bed cooler, conditions of each of the fluidizing devices comprising (i) 1 to 10 minutes mean residence time, (ii) 100 to 300 mm depth of non-fluidized bed, (iii) no more as a 50 μm drop spray size, (iv) 175 to 250 mm spray height, (v) 0.2 to 1.4 m / s fluidization speed and (vi) 12 to 100 ° C bed temperature, the mean residence time in step (c) being a total of 2 is up to 12 minutes, and wherein a coating agent selected from the group consisting of aluminosilicates, silicates, carbonates and mixtures thereof is added to step (c) either directly after the fluidized bed cooler or fluidized bed dryer; and / or between the fluid bed dryer and fluid bed cooler; and / or directly to the fluid bed dryer.

There are also granular detergent compositions provided with a high density of at least 600 g / l according to any of the embodiments of the method described herein.

Accordingly, it is an object of the invention a process for the continuous production of a detergent composition to provide, which by controlling the energy expenditure, the residence time ratios and the top speed ratios in the mixers with respect to End product density is flexible. It is also a job the invention to provide a method which is more efficient and is more economical to manufacture on a production scale facilitate. These and other tasks, characteristics and the related Advantages of the present invention will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiment below and the appended claims.

detailed Description of the preferred embodiment

The present invention is based on directed a process which free-flowing, granular detergent agglomerates with a density of at least 600 g / l. The procedure represents granular Detergent agglomerates from an aqueous and / or non-aqueous Surfactant, which then with a fine powder with a diameter of 0.1 to 500 µm coated to obtain granules with high density.

method

First stage [step (a)]

In the first stage of the process will be one or more watery and / or non-aqueous surfactant (s), which are in the form of powder, paste and / or liquid, and fine Powder with a diameter of 0.1 to 500 μm, preferably from 1 to 100 μm, in one first mixer fed, μm To produce agglomerates. While the process becomes the surface of the surfactant, which is coated with the fine powder, with finely atomized liquid wetted to deposit more fine powder on the surface of the agglomerates (The definition of surfactants and fine powder, the atomized liquid are described in detail below). In addition to Addition of the fine powder can optionally be internal to the fluidization device (e.g. fluidized bed dryer and / or fluidized bed cooler) generated recyclate stream from powder with a diameter of 0.1 up to 300 µm can be fed into the mixer. The powder content Such an internal recyclate stream can contain 0 to 60% by weight of the end product be.

In another embodiment according to the invention can the surfactant for the first stage before the above practice in a mixer or Premixer (e.g. a conventional screw extruder or similar Mixer) after which the mixed detergent materials in the mixer the first stage, as hereinbefore for agglomeration described.

All in all, the middle lies Residence time in the first mixer is preferably in the range from 0.2 to 5 s and the top speed of the first mixer in the range from 10 m / s to 30 m / s; the energy per unit mass of the first Mixer (energy state) is in the range of 0.15 kj / kg to 5 kj / kg; more preferably the mean residence time is in the first Mixer in the range of 0.2 to 5 s and the top speed of the first mixer in the range of 10 m / s to 30 m / s; the energy per Unit of mass of the first mixer (energy state) is in the range from 0.15 kj / kg to 5 kj / kg, most preferably the middle one Dwell time in the first mixer in the range of 0.2 to 5 s, the top speed in the first mixer is in the range from 15 m / s to 26 m / s and the Energy per unit mass of the first mixer (energy state) 0.2 kj / kg to 3 kj / kg.

As an example of the mixer, any Serve the type of mixer known to those skilled in the art as long as the mixer those mentioned above Conditions for complete the first stage can. As an example, this can be done by the Schugi Society (Netherlands) manufactured Flexomic Model serve. As a result of the first stage then get the first agglomerates.

Second stage [step (B)]

With the discharge from the first stage (i.e. the first agglomerates) a second mixer is loaded. The first agglomerates become main in the second mixer mixed and thorough sheared to round and enlarge the agglomerates. to second stage can optionally 0-10%, more preferably 2-5% powdery Detergent ingredients of the type added in the first stage can be used and / or other detergent ingredients. Preferably can Chopper used in the third mixer to unwanted oversized agglomerates break. The procedure including the second stage with Chopping is useful in order to obtain a smaller amount of oversize agglomerates as the end product, and such a method is a preferred embodiment the invention.

All in all, the middle lies Residence time in the second mixer is preferably in the range from 0.5 to 55 min and the energy per unit mass of the second mixer (energy state) is in the range of 0.15 kj / kg to 7 kj / kg, more preferably is the average residence time in the second mixer 3 to 6 min and the Energy per unit mass of the second mixer (energy state) lies in the range from 0.15 kj / kg to 4 kj / kg,

Example of the second stage mixer can be any type of mixer known to those skilled in the art, as long as the mixer the aforementioned Conditions for meet the second stage can. As an example, the Lödig Gesellschaft (Germany) manufactured Lödige KM mixers serve. As a result of the second stage, agglomerates then become preserved with a round shape.

Third stage [step (C)]

The second agglomerates are lighter than 600 g / l or further agglomeration is preferred, to the optimal condition for the end product of the method according to the invention to be enough a fluidizing device, such as a fluidized bed, with the second agglomerates are fed to the granulation for production of a free flowing Reinforcing granules with high density. The third stage can in one or more than one fluidization devices (e.g. by Combine different types, such as a fluid bed dryer and a fluid bed cooler) respectively. Can go to the second stage optionally 0-10%, more preferably 2-5% powdery Detergent materials are added by the way they are in the first stage can be used and / or other detergent ingredients. At this stage you can optionally also 0 to 20%, more preferably 2 to 10%, liquid detergent materials by the way they are added in the first stage. The second Stage and / or other detergent ingredients to reinforce the granulation and around the surface to coat the granules.

In order to achieve a density of at least 600 g / l, preferably 650 g / l, the conditions for a fluidization device can all in all include: Average retention: 1 to 10 min; Depth of non-fluidized bed: 100 to 300 mm: spray droplet size: not more than 50 μm; Spray height: 175 to 250 mm; fluidization: 0.2 to 1.4 m / s; Bed temperature: 12 to 100 ° C; more preferably: Average residence time: 2 to 6 min; Depth of non-fluidized bed: 100 to 250 mm: Sprithtropfengröße: not more than 50 μm; Spray height: 175 to 200 mm; fluidization: 0.3 to 1.0 m / s; Bed temperature: 12 to 80 ° C;

would used two different types of fluidization devices the mean residence time of the third stage can be a total of 2 to 20 minutes, more preferably 2 to 12 minutes.

A coating agent for improvement the flow behavior and / or to minimize over-agglomeration The detergent composition is added to one or more of the following Places added to the present process: (1) The coating agent can be placed right after the fluidized bed cooler or fluidized bed dryer be added; (2) The coating agent can be between the Fluidized bed cooler and added to the fluid bed dryer; (3) The coating agent can be added directly to the fluid bed dryer. The coating agent is preferably chosen from the group consisting of aluminosilicates, silicates, carbonates and mixtures thereof. The coating agent does not promote only free flow the resulting detergent composition, which the consumer insofar desired than the slight dimension of the detergent during the Allows use but also serves to prevent agglomeration by preventing over-agglomeration to minimize. As the expert knows very well, over-agglomeration can too undesirable flow properties and aesthetic Properties of the finished detergent product.

Detergent raw materials

The total amount of surfactants produced in accordance with the invention Products found in the detergent materials below, atomized liquids and detergent additive ingredients are included in the percentage range from 5% to 60%, more preferably 12% to 40%, more preferably 15% to 35%. The surfactants described in the preceding can be included originate from any part of the method according to the invention, e.g. B. either from the first stage, the second stage and / or the third stage of the present invention.

Detergent surfactant (aqueous / non-aqueous)

The surfactant content can be the present Method 5% to 60%, more preferably 12% to 40%, more preferably 12% to 35% of the total amount in the inventive method final product obtained. The surfactant according to the invention, which as the aforementioned Starting surfactant material used in the first stage can in the form of a powder, pasty or liquid Raw material.

The surfactant itself is preferred from the anionic, nonionic, zwitterionic, ampholytic and cationic classes and compatible mixtures thereof selected. Detergent surfactants for use herein are described in US-A 3,664,961, Norris, issued May 23, 1972 and in U.S. 3,929,678, Laughlin et al on Dec. 30, 1975. Usable canonical surfactants also include those described in U.S. Patent 4,222,905, Cockrell, issued Sept. 16. 1980 and U.S. 4,239,659, Murphy, issued Dec. 16, 1980 are. Of the surfactants, the anionic and nonionic are preferred and the anionic most preferred.

Examples of preferred anionic surfactants for use in the present invention include, but are not limited to, conventional C ₁₁ -C ₁₈ alkyl benzenesulfonates ("LAS"), primary branched chain and random C ₁₀ -C ₂₀ alkyl sulfates ("AS "), the secondary C ₁₀ -C ₁₈ - (2,3) alkyl sulfates with the formula CH ₃ (CH ₂ ) _x (CHOSO ₃ ^- M ⁺ ) CH ₃ and CH ₃ (CH ₂ ) _Y (CHOSO ₃ ^- M ⁺ ) CH ₂ CH ₃ , wherein x and (y + 1) are integers of at least about 7, preferably at least about 9, and M is a water-soluble cation, in particular sodium, unsaturated sulfates such as oleyl sulfate and the C ₁₀ -C ₁₈ -Alkylalkoxysulfate ("AExS"; in particular EO (1-7) -ethoxysulfate).

Anionic surfactants that can be used also include water-soluble Salts of 2-acyl-oxyalkane-1-sulfonic acids, which have 2 to 9 carbon atoms in the acyl group and 9 to 23 carbon atoms contained in the alkane unit; water-soluble salts of olefin sulfonates, which contain 12 to 24 carbon atoms; and beta-alkyloxyalkanesulfonates, which have 1 to 3 carbon atoms in the alkyl group and 8 to 20 Contain carbon atoms in the alkane unit.

Other surfactants for use in the paste according to the invention optionally include, for example, the C ₁₀ -C ₁₈ alkyl alkoxy carboxylates (in particular the EO (1-5) ethoxy carboxylates), the C ₁₀ -C ₁₈ glycerol ethers, the C ₁₀ -C ₁₈ glycol polyglycosides and the corresponding sulfated polyglycerides and the alpha-sulfonated C ₁₂ -C ₁₈ fatty acid esters. If desired, conventional nonionic and amphoteric surfactants can be included in the overall compositions, such as the C ₁₂ -C ₁₈ alkyl ethoxylates ("AE"), including the so-called alkyl ethoxylates with a narrow molecular weight distribution and the C ₆ -C ₁₂ alkyl phenol ethoxylates (especially ethoxylates with mixed ethoxy / propoxy), and C ₁₀ -C ₁₈ amine oxides. The C ₁₀ -C ₁₈ -N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C ₁₂ -C ₁₈ -N-methylglucamides. Compare WO-A 92/06154. Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C ₁₂ -C ₁₈ -N- (3-methoxypropyl) glucamide. The N-propyl to N-hexyl-C ₁₂ -C ₁₈ glucamides can be used for low foaming. Conventional C ₁₀ -C ₂₀ soaps can also be used. If strong foaming is desired, the branched-chain C ₁₀ -C ₁₆ soaps can be used. Mixtures of anionic and nonionic surfactants are particularly useful.

Cationic surfactants can also be used here as detergent surfactants, suitable quaternary ammonium surfactants being selected from mono-C ₆ -C ₁₆ , preferably C ₆ -C ₁₀ -N-alkyl or alkenylammonium surfactants, in which the remaining N positions are represented by methyl , Hydroxyethyl or hydroxypropyl groups are substituted.

Ampholytic surfactants can also be used herein as detergent surfactants, including aliphatic derivatives of heterocyclic secondary and tertiary amines; zwitterionic surfactants, which are derivatives of aliphatic. include quaternary ammonium, phosphonium and sulfonium compounds; water-soluble salts of esters of alpha-sulfonated fatty acids; alkyl ether; water soluble salts of olefin sulfonates; Beta-alkyloxy; Betaines having the formula R (R ¹ ) ₂ N ⁺ R ² COO ^- , wherein R is a C ₆ -C ₁₈ hydrocarbyl group, preferably a C ₁₀ -C ₁₆ alkyl group or C ₁₀ -C ₁₆ acyl amidoalkyl group, 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 acylamidopropyldimethylbetaine; Hexadecyldimethylbetain; C ₁₂ -C ₁₄ acylamidopropyl betaine; C ₈ -C ₁₄ acylamidohexlyl diethyl betaine; 4 [C ₁₄ -C ₁₆ acylmethylamidodiethylammonio] -1-carboxybutane; C ₁₆ -C ₁₈ acylamidodimethylbetaine; C ₁₂ -C ₁₆ acydopentanediethyl betaine; and [C ₁₂ -C ₁₆ acylmethylamido] dimethylbetaine. Preferred betaines are C ₁₂ -C ₁₈ dimethylammoniohexanoate and the C ₁₀ -C ₁₈ acylamidopropane (or ethane) dimethyl (or diethyl) betaines; and the sultaine with the formula R (R ¹ ) ₂ N ⁺ R ² SO ₃ ^- , wherein R is a C ₆ -C ₁₈ hydrocarbyl group, preferably a C ₁₀ -C ₁₆ alkyl group, more preferably a C ₁₂ -C ₁₃ - Is alkyl group, each R ^{1 is} typically C ₁ -C ₃ alkyl, preferably methyl and R ^{2 is} a C ₁ -C ₆ hydrocarbyl group, preferably a C ₁ -C ₃ alkylene, or preferably hydroxyalkylene group. Examples of suitable sulphates include C ₁₂ -C ₁₄ dimethylammonio-2-hydroxypropyl sulfonate, C ₁₂ -C ₁₄ dihydroxyethyl ammoniopropane sulfonate and C ₁₆ -C ₁₈ dimethylammoniohexane sulfonate, with the C ₁₂ -C ₁₄ amidopropylammonio-2-hydroxypropyl sulfate being preferred ,

Fine powder

The proportion of fine powder in the present method, which is used in the first stage 94% to 30%, preferably 86% to 54%, of the total amount of the starting material for the first stage. The fine powder used as the raw material of the present method, which is preferably chosen from the group consisting of ground soda ash, powdered Sodium polyphosphate (STPP), hydrated tripolyphoshate, ground Sodium sulfate, aluminosilicates, crystalline layered silicates, Nitrilotriacetates (NTA), phosphates, precipitated silicates, polymers, Carbonates, citrates, powdered surfactants (such as powdered alkane sulfonic acids) and an internal recyclate stream of powder from the process according to the invention, has an average powder diameter of 0.1 to 500 μm, preferably 1 to 300 μm, more preferably 5 to 100 μm. In the case of using hydrated STPP as a fine powder In the present invention, an STPP that is up to is hydrated to a degree of not less than 50%. That here aluminosilicate ion exchange material used as a detergent builder both, a high calcium ion exchange capacity and one high exchange rate. Without being limited by theory It is believed that such a high calcium ion exchange rate and capacity is a function different related Factors is derived from the process by which the Aluminosilicate ion exchange material is produced. Regarding then the aluminosilicate ion exchange materials used herein preferably in agreement with Corkill et. al., U.S. 4,605,509 (Procter & Gamble).

The aluminosilicate ion exchange material is preferably in the "sodium" form because the potassium and hydrogen forms of the present aluminosilicates do not have the exchange rate and capacity as high as the sodium form offers. The aluminosilicate ion exchange material is also preferably in an over-dried form, which facilitates the preparation of the solid detergent agglomerates described herein. The aluminosilicate ion exchange materials used herein have a particle size diameter that optimizes their effectiveness as detergent builders. The expression "particles Size Diameter ", as used herein, represents the mean particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical methods such as microscopic determination and scanning electron microscopy (SEM). The preferred particle diameter of the aluminosilicate is 0.1 µm to 10 µm, more preferably 0.5 µm to 9 µm Most preferably, the particle size diameter is 1 µm to 8 µm.

The aluminosilicate ion exchange material preferably has the formula Na ₁₂ [(AlO ₂ ) _Z (SiO ₂ ) _Y ] .xH ₂ O wherein z and y are integers of at least 6, the molar ratio of z _to y is about 1 to 5 and x is 10 to 264. More preferably, the aluminosilicate has the formula Na ₁₂ [(AlO ₂ ) ₁₂ (SiO ₂ ) ₁₂ ] .xH ₂ O wherein x is about 20 to about 30, especially about 27. These preferred aluminosilicates are commercially available, for example, under the names Zeolite A, Zeolite B _and Zeolite X. Alternatively, naturally occurring or synthetically derived aluminosilicate ion exchangers suitable for use herein can be made as described in Krummel et al., U.S. Patent 3,985,669.

The aluminosilicates used herein are further characterized by their ion exchange capacity, which is equivalent to at least 200 mg equivalents of CaCO ₃ hardness / g, calculated on an anhydrous basis, and which is preferably in the range from 300 mg to 352 mg equivalents / g CaCO ₃ hardness / g lies.

Finely atomized liquid

The proportion of finely atomized liquid can be 1% to 10% (active basis) in the present method, preferably 2% to 6% (active basis), based on that in the method according to the invention total amount. The finely atomized liquid can be present Process chosen are from the group consisting of liquid silicate, anionic or cationic surfactants, which are in liquid form; aqueous or non-aqueous polymer solutions Water and mixtures thereof. Other optional examples of fine atomized liquids can in the present invention from sodium carboxymethyl cellulose solution, polyethylene glycol (PEG) and solutions of dimethylene triamine pentamethylphosphonic acid (DETMP).

The preferred examples of anionic surfactant solutions, which as finely atomized liquids can be used in the present invention 88-97% active HLAS, 30–50% active NaLAS, 28% active AE3S solution, 40-50% active liquid Silicate.

Cationic surfactants can also be used here as finely atomized liquids, suitable quaternary ammonium surfactants being selected from C ₆ -C ₁₆ -, preferably C ₆ -C ₁₀ -N-alkyl or alkenylaminonium surfactants, where the remaining N positions are methyl , Hydroxyethyl or hydroxypropyl groups are substituted.

mit einer modifizierten Polyamin-Formel V_(n+1)W_mY_nZ oder ein Polyamingrundgerüst, entsprechend der Formel:

mit einer modifizierten Polyamin-Formel V_(n–k+1)W_mY_mY'_kZ, worin k kleiner oder gleich n ist, das Polyamingrundgerüst vor der Modifizierung ein Molekulargewicht von größer als etwa 200 Dalton besitzt, wobei

• i) V-Einheiten Endeinheiten sind mit der Formel:
  
• ii) W-Einheiten Grundgerüsteinheiten sind mit der Formel:
  
• iii) Y-Einheiten Verzweigungseinheiten sind mit der Formel:
  
  und
• iv) Z-Einheiten Endeinheiten sind mit der Formel:
  

wobei Grundgerüst-Verbindungs-R-Einheiten aus der Gruppe gewählt sind, bestehend aus C₂-C₁₂-Alkylen, C₄-C₁₂-Alkenylen, C₃-C₁₂-Hxydroxyalkylen, C₄-C₁₂-Dihydroxyalkylen, C₈-C₁₂-Dialkarylen, -(R¹O)_XR¹-, -(R¹O)_XR⁵(OR¹)_X-, -(CH₂-CH(OR²)CH₂O)_Z(R¹O)_YR¹(OCH₂CH(OR²)CH₂)_W-, -C(O)(R⁴)_rC(O)-, -CH₂CH(OR₂)CH₂- und Mischungen hievon; worin R¹ C₂-C₆-Alkylen und Mischungen hiervon ist; R² Wasserstoff, -(R¹O)_XB und Mischungen hiervon ist; R³ C₁-C₁₈-Alkyl, C₇-C₁₂-Aryl-alkyl, C₇-C₁₂-alkylsubstituiertes Aryl, C₆-C₁₂-Aryl und Mischungen hiervon ist; R⁴ C₁-C₁₂-Alkylen, C₄-C₁₂-Alkenylen, C₈-C₁₂-Arylalkylen, C₆-C₁₀-Arylen und Mischungen hiervon ist; R⁵ C₁-C₁₂-Alkylen, C₃-C₁₂-Hydroxyalkylen, C₄-C₁₂-Dihydroxyalkylen, C₈-C₁₂-Dialkylarylen, -C(O)-, -C(O)NHR⁶NHC(O)-, -R¹(OR¹)-, C(O)(R⁴)_rC(O)-, -CH₂CH(OH)CH₂-, -CH₂CH(OH)CH₂O)(R¹O)_YR¹OCH₂CH(OH)CH₂und Mischungen hiervon ist; R⁶ C₂-C₁₂-Alkylen oder C₆-C₁₂-Arylen ist; E-Einheiten aus der Gruppe gewählt sind, bestehend aus Wasserstoff, C₁-C₂₂-Alkyl, C₃-C₂₂-Alkenyl, C₇-C₂₂-Arylalkyl, C₂-C₂₂-Hydroxyalkyl, -(CH₂)_PCO₂M, -(CH₂)_qSO₃M, -CH(CH₂CO₂M)CO₂M, -(CH₂)_PPO₃M, -(R¹O)_XB, -C(O)R³ und Mischungen hiervon; Oxid; B Wasserstoff, C₁-C₆-Alkyl, -(CH₂)_qSO₃M, -(CH₂)_PCO₂M, -(CH₂)_q(CHSO₃M)-CH₂SO₃M, -(CH₂)_q(CHSO₂M)CH₂SO₃M, -(CH₂)_PPO₃M und Mischungen hiervon ist; W Wasserstoff oder ein wasserlösliches Kation in einer ausreichenden Menge ist, um dem Ladungsausgleich zu genügen; X ein wasserlösliches Anion ist; m den Wert von 4 bis 400 hat; n den Wert von 0 bis 200 hat; p den Wert von 1 bis 6 hat, q den Wert von 0 bis 6 hat; r den Wert von 0 oder 1 hat; w den Wert von 0 oder 1 hat; x den Wert von 1 bis 100 hat; y den Wert 0 bis 100 hat; z den Wert 0 oder 1 hat. Ein Beispiel der am meisten bevorzugten Polyethylenimine wäre ein Polyethylen mit einem Molekulargewicht von 1800, welches zusätzlich durch Ethoxylierung bis zu einem Grad von etwa 7 Ethylenoxidresten pro Stickstoff ethoxyliert ist (PEI1800, E7). Die vorstehende Polymerlösung sollte vorzugsweise mit einem anionischen Tensid wie NaLAS einen Vor-Komplex bilden.Preferred examples of aqueous or non-aqueous polymer solutions which can be used as finely atomized liquids in the present invention are modified polyamines which comprise a polyamine backbone, according to the formula:

with a modified polyamine formula V _{(n + 1)} W _m Y _n Z or a polyamine backbone, according to the formula:

with a modified polyamine formula V _{(n-k + 1)} W _m Y _m Y ' _k Z, where k is less than or equal to n, the polyamine backbone has a molecular weight greater than about 200 daltons prior to modification, wherein

• i) V units are end units with the formula:
  
• ii) W units of basic scaffolding units are of the formula:
  
• iii) Y units branching units are of the formula:
  
  and
• iv) Z units are end units with the formula:
  

wherein backbone compound R units are selected from the group consisting of C ₂ -C ₁₂ alkylene, C ₄ -C ₁₂ alkenylene, C ₃ -C ₁₂ hydroxylalkylene, C ₄ -C ₁₂ dihydroxyalkylene, C ₈ -C ₁₂ -dialkarylene, - (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) _Y R ¹ (OCH ₂ CH (OR ² ) CH ₂ ) _W -, -C (O) (R ⁴ ) _r C (O) -, -CH ₂ CH (OR ₂ ) CH ₂ - and mixtures thereof ; wherein R ^{1 is} C ₂ -C ₆ alkylene and mixtures thereof; R ^{2 is} hydrogen, - (R ¹ O) _X B and mixtures thereof; , C ₇ -C, C, C ₆ -C ₁₂ aryl, and mixtures thereof R ^{3 is} C ₁ -C ₁₈ alkyl ₁₂ aryl-alkyl ₇ -C ₁₂ alkyl substituted aryl; R ^{4 is} C ₁ -C ₁₂ alkylene, C ₄ -C ₁₂ alkenylene, C ₈ -C ₁₂ arylalkylene, C ₆ -C ₁₀ arylene and mixtures thereof; R ⁵ C ₁ -C ₁₂ alkylene, C ₃ -C ₁₂ hydroxyalkylene, C ₄ -C ₁₂ dihydroxyalkylene, C ₈ -C ₁₂ dialkylarylene, -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) _Y R ¹ OCH ₂ CH (OH) CH ₂ and mixtures thereof; R ^{6 is} C ₂ -C ₁₂ alkylene or C ₆ -C ₁₂ arylene; E units are selected from the group consisting of hydrogen, C ₁ -C ₂₂ alkyl, C ₃ -C ₂₂ alkenyl, C ₇ -C ₂₂ arylalkyl, C ₂ -C ₂₂ hydroxyalkyl, - (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) R ³ and mixtures thereof; Oxide; B 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 and mixtures thereof; W is hydrogen or a water-soluble cation in an amount sufficient to satisfy charge balancing; X is a water soluble anion; m has the value from 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 1; w has the value 0 or 1; x has the value from 1 to 100; y has the value 0 to 100; z has the value 0 or 1. An example of the most preferred polyethyleneimines would be a 1800 molecular weight polyethylene which is additionally ethoxylated to about 7 ethylene oxide residues per nitrogen by ethoxylation (PEI1800, E7). The above polymer solution should preferably precomplex with an anionic surfactant such as NaLAS.

Other preferred examples of water or non-aqueous Polymer solutions, which in the present invention as finely atomized liquids can be used are polymeric polycarboxylate dispersants which are obtained by polymerization or copolymerizing suitable unsaturated monomers in their acid form can be produced. unsaturated monomeric acids, which can be polymerized to form suitable polymeric polycarboxylates include acrylic acid, maleic acid, (or Maleic anhydride), fumaric acid, itaconic, aconitic, mesaconic, citraconic and methylene malonic acid on. In the presence of monomeric segments in the polymeric polycarboxylates herein which contain no carboxylate residues, such as vinyl methyl ether, Styrene, ethylene, etc. is appropriately taken care of to bear such segments no more than 40% by weight of the polymer include.

Homopolymeric carboxylates with molecular weights from above 4000, as will be described below, are preferred. Especially Suitable homopolymeric polycarboxylates are derived from acrylic acid. Such on acrylic acid based polymers for use herein are the water soluble ones Salts of polymerized acrylic acid. The average molecular weight of such polymers in the acid form preferably ranges from over 4,000 to 10,000, preferably from over 4,000 to 7,000 and am most preferably from 4,000 to 5,000. Water soluble salts of such acrylic acid polymers can for example the alkali metal, ammonium and substituted ammonium salts lock in.

Copolymers Polycarboxylates such as acrylic / maleic based copolymers can also be used. Such materials include the water-soluble salts of the copolymers of acrylic acid and maleic acid. The average molecular weight of such copolymers in the acid form preferably ranges from 2,000 to 100,000, more preferably from 5,000 to 75,000, most preferably from 7,000 to 65,000. The ratio of acrylate to maleate segments in such copolymers generally ranges from 30: 1 to 1: 1, more preferably from 10: 1 to 2: 1. Water-soluble salts of such acrylic acid / maleic acid copolymers can, for example, the alkali metal, Include ammonium and substituted ammonium salts. The above polymer solution should preferably precomplex with an anionic surfactant such as LAS.

Deterenszusatzbestandteile

The detergent output material valley can additional in the present case Include detergent ingredients and / or it can while any of the subsequent stages of the present process Number of additional Components are incorporated into the detergent composition. Close these additional components other detergent builders, bleaches, bleach activators, foam promoters and foam suppressants, anti-tarnishing agents and anti-corrosion agents, dirt suspending agents, dirt repellants, Germicides, pH regulators, sources of alkalinity without builder effect, chelating agents, smectic clays, enzymes, enzyme stabilizers and fragrances. Compare US-A 3,936,537, issued Feb. 3. 1976 to Baskerville, Jr. et al.

Other builders can generally be selected from the various water-soluble alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxysulfonates, polyacetates, carboxylates and polycarboxylates. The alkali metal, especially sodium salts of the above are preferred. Preferred for use herein are the phosphates, carbonates, C ₁₀ -C ₁₆ fatty acids, polycarboxylates, and mixtures thereof. Sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate, mono- and disuccinates and mixtures thereof are further preferred (see below).

Compared to amorphous sodium silicates, sodium layer silicates have a significantly higher exchange capacity for calcium and magnesium ions. additionally prefer layered sodium silicates magnesium over calcium, a property that is necessary to ensure that so well like all of the "hardness" from the wash water Will get removed. However, these crystalline layered silicates are general more expensive than the amorphous silicates and also as other builders. Around an economically portable detergent must therefore be provided the proportion of crystalline layered sodium silicates used is carefully considered be determined. Such crystalline layered sodium silicates are in Corkill et al., U.S. 4,605,509.

Specific examples of inorganic Phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphates with a degree of polymerization of about 6 to 21, and orthophosphates. Examples of polyphosphonate builders are the sodium and potassium salts of diphosphonic acid, which Sodium and potassium salts of ethane-1-hydroxy-1,1-diphosphonic acid and the sodium and potassium salts of ethane-1,1,2-triphosphonic acid. Other Phosphorus builder 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.

Examples of phosphorus-free, inorganic builders are tetraborate decahydrate and silicates with a weight ratio of SiO ₂ to alkali metal oxide of 0.5 to 4.0, preferably 1.0 to 2.4. Water soluble, phosphorus free organic builders for use herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxysulfonates. Examples of polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilotriacetic acid, ocydisuccinic acid, mellitic acid, benzene polycarboxylic acids and citric acid.

Polymeric polycarboxylate builders are in US-A 3,308,067, Diehl, issued March 7, 1967. Such Close materials the water soluble Salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic, mesaconic, fumaric acid, aconitic, Gitraconsäure and methylene malonic acid Some of these materials are considered water-soluble anionic polymers usable as described hereinafter, but only intimately Mix with the non-soapy anionic surfactant.

Other suitable polycarboxylates for use herein are the polyacetal carboxylates described in US-A 4,144,226, issued on March 13 1979 to Crutchheld et al., And US-A 4,246,495, issued March 27, 1979 to Crutchfield et al. These polyacetal caboxylates can by contacting an ester of polyglycolic acid with a polymerization initiator manufactured under polymerization conditions become. The resulting polycarboxylate ester then becomes chemical stable end groups bound to the polyacetal carboxylate against rapid Depolymerization in an alkaline solution to stabilize, converted to the corresponding salt and a detergent composition added. Particularly preferred polycarboxylate builders are those in US-A 4,663,071, Bush et al., Issued May 5, 1987 Ether carboxylate builder compositions which is a combination of tartrate monosuccinate and tartrate disuccinate include.

Bleaches and activators are described in U.S. 4,412,934, Chung et al., Issued Nov. 1, 1983, and U.S. 4,483,781, Hartman, issued Nov. 20, 2984. Chelating agents are also described in US-A 4,663,071, Bush et al., From column 17, line 54 to column 18, line 68. Foam modifiers are also optional, and are described in U.S. Patents 3,933,672 issued Jan. 20, 1976 to Bartoletta et al. and 4,136,045 issued Jan. 23, 1979 to Gault et al.

Suitable smectic clays for use herein are described in U.S. Patent 4,762,645, Tucker et al., issued Aug. 9. 1988, column 6, line 3 to column 7, line 24. suitable additional Detergent builders for use herein are in the Baskerville patent, Column 13, line 54 to column 16, line 16, and in US-A 4,663,071, Bush et al., Issued May 5, 1987, enumerated.

optional steps

The process can either Spraying step an additional Bin ders in one or more than a first, second and / or third Mixers in the present invention. Becomes a binder added to the agglomeration by providing a "binder" or "adhesive" for the detergent ingredients to reinforce. The binder is preferably chosen from the group consisting of water, anionic surfactants, nonionic Surfactants, liquid Silicates, polyethylene glycol, polyvinyl pyrrolidone, polyacrylates, citric acid and mixtures thereof. Other suitable binder materials including those herein listed are described in Beerse et al., U.S. Patent 5,108,646 (Procter & Gamble Co.).

Other optional steps, which ones are envisaged in the present proceedings, which include Classifying the too big Detergent agglomerates in a screening plant, which is a variety of shapes include can, including, but not limited to conventional Sieves according to the desired Particle size of the finished one Detergent product selected become. Other optional steps include conditioning the Detergent agglomerates by adding the agglomerates using the preceding discussed apparatus an additional Be subjected to drying.

Another optional step in the present process involves post-treatment of the resulting Detergent agglomerates by a variety of processes, including the spray and / or mixing with other conventional detergent ingredients. The post-treatment step includes, for example, spraying the manufacture agglomerates with fragrances, brighteners and enzymes to create a more complete detergent composition. Such Techniques and ingredients are well known in the art.

EXAMPLES

example 1

The following is an example To obtain agglomerates with high density, which includes a Schugi FX-160 mixer, subsequently a Lödige KM mixer (KM-600) and then a fluidized bed device for further granulation is used.

[Stage 1] 120-160 kg / h HLAS (an acid precursor of C ₁₁ -C ₁₈ alkylbenzenesulfonate; 98% active) is in a highly turbulent air stream of the Schugi FX-160 mixer together with 220 kg / h powdered STPP (average particle size 40–75 μm), 160–280 kg / h ground soda ash (average particle size 15 μm), 80–120 kg / h ground sodium sulfate (average particle size 15 μm) and 200 kg / h internal recyclate stream from powder dispersed. The surfactant is fed in at about 50 to 60 ° C and the powders are added at room temperature. Then 30 kg / h HKAS (an acid precursor of C ₁₁ -C ₁₈ alkylbenzenesulfonate; 94-97% active) are dispersed as a finely atomized liquid at about 50 to 60 ° C. in the FX-160 mixer. 20-80 kg / h soda ash (average particle size 10-20 μm) are added to the Schugi mixer. The condition of the Schugi mixer is as follows: Average residence time: 0.2-5 s Top speed: 16-26 m / s Energy state: 0.15-2 kj / kg Mixer speed: 2000-3200 rpm

[Stage 2] The agglomerates from the Schugi FX-160 mixer are placed on the KM-600 mixer for further agglomeration, rounding and growing of the agglomerates. 30 kg / h of zeolite are also added to the KM mixer. Choppers can be used in the KM mixer to reduce the proportion of oversized agglomerates. The condition of the KM mixer is as follows: Average residence time: 3-6 min; Energy state: 0.15-2 kj / kg Mixer speed: 100-150 rpm Jacket temperature: 30-40 ° C.

[Level 3] A fluid bed dryer is used with the agglomerates from the KM mixer for drying, rounding and Feeding the agglomerates.

In the fluidized bed drying plant, 20-80 kg / h of liquid silicate (43% solids, 2.0 R) can also be added at 35 ° C. The conditions in the fluidized bed drying plant are as follows: Average residence time: 2 to 4 min; Depth of non-fluidized bed: 200 mm: spray droplet size: less than 50 μm; Spray height: 175 to 250 mm (above the inflow floor); fluidization: 0.4 to 0.8 m / s; Bed temperature: 40 to 70 ° C;

The resulting granules from the Level 3 has a density of 700 g / l and can optionally be the optional Cooling process, Classifying and / or crushing.

Example 2

The following is an example Obtain high density agglomerates, including a Schugi FX-160 Mixer and then a Lödige KM mixer (KM-600) is used.

[Stage 1] 120-200 kg / h HLAS (an acid precursor of C ₁₁ -C ₁₈ alkylbenzenesulfonate; 98% active) is in a highly turbulent air stream of the Schugi FX-160 mixer together with 220 kg / h powdered STPP (middle particles size 40–75 μm), 160–280 kg / h ground soda ash (average particle size 15 μm), 80–120 kg / h ground sodium sulfate (average particle size 15 μm) and 200 kg / h internal recyclate stream from powder at approx. 50 ° C dispersed. The condition of the Schugi mixer is as follows: Average residence time: 0.2–5 s: Top speed: 16-26 m / s Energy state: 0.15-2 kj / kg Mixer speed: 2000-3200 rpm

[Stage 2] The agglomerates from the Schugi FX-160 mixer are placed on the KM-600 mixer for further agglomeration, rounding and growing of the agglomerates. 60 kg / h of ground soda ash (average particle size 15 μm) are also added to the KM mixer. Choppers can be used in the KM mixer to reduce the proportion of oversized agglomerates. The condition of the KM mixer is as follows: Average residence time: 3–6 min: Energy state: 0.15-2 kj / kg Mischergeschwiridigceit: 100-150 rpm Jacket temperature: 30-40 ° C.

The resulting granules from step 2 has a density of 650 g / l and can optionally be the optional Cooling process, Classifying and / or crushing.

Now that the invention is on this way has been described in detail, it will be for the skilled person it can be seen that various changes can be made without to depart from the scope of the invention and that the invention is not limited to that should be what is described in the specification.

Claims (7)

A non-tower process for making a granular detergent composition having a density of at least about 600 g / l, comprising the steps of: (a) dispersing a surfactant and coating the surfactant with fine powder of 0.1 to 500 microns in diameter during the surfactant coated with fine powder is wetted with a finely atomized liquid in a mixer, the conditions of the mixer including (i) 0.2 to 5 seconds mean residence time, (ii) 15 to 26 m / s tip speed and (iii) 0.2 up to 3 kj / kg energy state, first agglomerates being formed; (b) carefully mixing the first agglomerates in a mixer with choppers, the conditions of the mixer including (i) 0.5 to 15 minutes mean residence time and (ii) 0.15 to 7 kj / kg energy state, whereby second agglomerates are formed; and (c) granulating the second agglomerates in a fluid bed dryer and fluid bed cooler, wherein Bedin Each of the fluidization devices includes (i) 1 to 10 minutes mean residence time, (ii) 100 to 300 mm depth of non-fluidized bed, (iii) no more than 50 µm drop spray size, (iv) 175 to 250 mm spray height, (v) 12 up to 100 ° C. bed temperature, the mean residence time in step (b) being a total of 2 to 12 minutes, and a coating agent selected from the group consisting of aluminosilicates, silicates, carbonates and mixtures thereof being added to step (b), either directly after the fluidized bed cooler or fluidized bed dryer; and / or between the fluid bed dryer and fluid bed cooler; and / or directly to the fluid bed dryer. The method of claim 1, wherein the surfactant is from the Group selected is composed of anionic surfactant, nonionic surfactant, cationic Surfactant, zwitterionic surfactant, ampholytic surfactant and mixtures hereof. The method of claim 1, wherein the surfactant is from the Group selected consisting of alkylbenzenesulfonates, alkylalkoxysulfonates, Alkyl ethoxylates, alkyl sulfates, coconut fatty alcohol sulfates and Mixtures of these. The method of claim 1, wherein an aqueous or non-aqueous polymer solution is dispersed with the surfactant in step (a). The method of claim 1, wherein the fine powder chosen from the group consisting of soda ash, powdered sodium tripolyphosphate, hydrated tripolyphosphate, sodium sulfates, aluminosilicates, crystalline layered silicates, phosphates, precipitated silicates, Polymers, carbonates, citrates, nitrilotriacetates, powdered surfactants and mixtures thereof. The method of claim 1, wherein the atomized liquid chosen from the group is composed of liquid Silicates, anionic surfactants, canonical surfactants, aqueous Polymer solutions, non-aqueous Polymer solutions, Water and mixtures thereof. The method of claim 1, wherein an internal recyclate stream of powder from the fluidization device continues to step (a) is given.