MXPA99002258A - Process for preparing high bulk density detergent compositions - Google Patents

Abstract

A process for preparing a granular detergent composition comprises a first step of preparing a liquid component comprising a structurant. A second step comprises admixture of the liquid with a solid component in a granulator. An optional third step comprises drying and/or cooling. The structurant is incorporated in an amount such that the liquid component is pumpable at temperatures of 50°C or more but causes sufficient solidification to form a free-flowing granulated product.

Description

PROCEDURE FOR PREPARING DETERGENT COMPOSITIONS WITH HIGH APPARENT DENSITY FIELD OF THE INVENTION The present invention relates to a process for preparing a granular detergent composition or component, by mixing. More particularly, it relates to a process for the continuous preparation of such detergent compositions. In addition, it relates to a granular detergent composition that is obtained through the process of the present invention.

BACKGROUND OF THE INVENTION Generally speaking, there are two main types of procedures through which detergent powders can be prepared. The first type of process involves spray drying and an aqueous detergent sludge in a spray-drying tower. In the second type of process, the various components are dry mixed and optionally agglomerated with liquid, for example, non-ionic. The latter type of process is more suitable for the production of powders having a relatively high bulk density. That is, principally since the chemical composition of the sludge used in the spray drying process markedly affects the bulk density of the granulated product. This bulk density can only mean ivame te increased by increasing the relatively dense sodium sulfate content. However, sodium sulfate does not contribute to detergency, so that the total function of the powder in the wash is thus reduced. In recent years, there have been several purposes for mechanical mixing processes for the production of high density detergent powders. For example EP-A-265 203 discloses liquid surfactant compositions containing a sodium salt of an alkylbenzene sulfonate or alkyl sulfate, an ethoxylated nonionic surfactant and water. The amount of water does not exceed 10% by weight. Said liquid surfactant composition can be sprayed onto a solid particulate absorbent material, for example, a porous spray dried base powder, having a low bulk density and containing little or no active, to form a detergent base powder having a increased bulk density. EP-A-507 402 describes a process for preparing a composition of the liquid surfactant comprising an anionic surfactant, a nonionic surfactant and having a relatively low water content. The principle of the process is to neutralize the acid corresponding to the anionic surfactant with a neutralizing agent of such a strength that it leads to the desired low level of water in the final product by adding these two materials to a fluid, which comprises the nonionic surfactant and which acts as a solvent or diluent for the neat anionic surfactant. This procedure is carried out continuously, preferably in a reactor or loop. EP-A-420 317 describes a process for the continuous preparation of granular detergent compositions or components having a higher density than that obtainable in spray drying processes. The process consists of three stages, an agglomeration in a high speed mixer, a densification in a moderate speed granulator densifier, by which the material is carried or maintained in a deformable state, and drying and / or cooling of the product ( for example, in a fluid bed). A liquid acid precursor of an anionic surfactant is neutralized in situ through a water-soluble alkaline inorganic material (e.g., sodium carbonate) in a high speed mixer. The deformable state of the material at temperatures above 40 ° C is obtained at least partially from the rate of neutralization of the core. EP-A-544 365 describes a process for the preparation of a granulated composition in the same equipment described in EP 0 420 317 or alternatively in a batch granulation. In this case, a sodium or potassium salt mixture of an alkyl sulfate, for example, a primary alkylsulfate and an alkoxylated nonionic surfactant is used as the liquid phase for granulation in the high speed mixer. To obtain powder powders with good powder properties, the agglomeration process is controlled through a significant increase in the viscosity of the liquid. This is obtained through the addition of one or more components to the liquid surfactant composition. Examples of said velocity raising components are water and fatty acid in combination with a stoichiometric amount of an alkaline material (eg, caustic soda) sufficient to neutralize the fatty acid resulting in soap formation. When the powder to be formulated contains a phosphate builder such as sodium tripolyphosphate, the known mixing processes have a number of disadvantages, which are dangerous for the requirement of producing free flowing powders with good capacity of granulation and a low moisture content. This is probably partly attributable to the low liquid carrying capacity of the phosphate builder particles. Typical problems that can be encountered include the development of hard cakes due to active exothermic hydration and the formation of a glass point. Furthermore, soft granules tend to be formed in the resulting product with a poor powder behavior due to the low adhesive forces of the wet particle surfaces and, therefore, a poor granule structure. A. Naviglio and - A Mariconi ("Detergent Manufacture - A new, low cost, e ne r gy- sai ng, cooland dry process", Soap / Cosmetics / Chemical S pecia 1 ities, Sept. 1987) describes a continuous process with a turbo reactor and a rotating drum agglomerator for the preparation of granular detergent compositions. The dry neutralization reaction occurs in the turbo reactor, where the solids are dosed at the same time (for example, solids "STP, alkaline powder (for example sodium carbonate); liquids: caustic solution, LAS acid, fatty acid). The mixture in the turbo reactor is achieved by special air diffusers that keep the powders and liquids suspended. The cooled air is used to eliminate the heat of reaction. The reactor contains a screw for continuous transport to the agglomeration stage. The agglomeration is provided by spraying on sodium silicate or non-ionic in the rotating drum. This process provides a separation of the neu t r a 1 i z a c ion / hydr a tion and agglomeration. The formation of large lumps of hydrated STP can be prevented by suspending it with a stream of air. Due to the low absorption capacity of STP, the non-ionic spray is not suitable for preparing detergent powders with a high content of active ingredients.

BRIEF DESCRIPTION OF THE INVENTION The problems related to the inclusion of STP or other solids that have a low liquids transport capacity and / or have hydratable properties, however, are now overcome by a new although simpler process which can be carried out using a reactor and a mixing equipment that is already conventional in the art, however, also has advantages in the process of different types of solids. This new process constitutes the present invention and which formulates a liquid component with a structurant as well as to remain pumpable at the temperature at which the liquid component is formed and then add it with a solid component at a lower temperature at which the structurant causes the solidification of the mixture. International Patent Specification No. 95/32276 describes a process in which the "liquid" components are formulated as a paste (preferably aqueous) having a viscosity between 5 and 100 Pas at 70 ° C and then granulated with a solid component . however, this method does not disclose the use of a phosphate improver or other inorganic salts to transport liquids and / or similar hydration properties and thus solve the problems by the present invention without being directed. Ad emás, the convenience of being able to pump the liquid component and the solution to provide low relative wet products, is not provided either. For example, the process of the present invention also produces unexpected benefits with different detergency builders such as zeolites, allowing the manufacture of granulated products with a lower relative humidity without the drying presented heretofore. This low humidity allows the percarbonate blakers to be p o s t - d s i f i c a d s, these being preferred - with respect to the perborates under ambient conditions. The resulting granular product, which when formed into tablets, produces tablets having a high degree of hardness as measured by the peak resistance (Pmax) and the modulus (Emod). These parameters can optionally also be used to characterize the solidified mixture in the granulator. Thus, in a first aspect, the present invention provides a process for preparing a granular detergent composition, the process comprises a first step of preparing a liquid component comprising a structuring agent, a second step of mixing the liquid component with a solid component in a granulator and optionally, a third step of drying and / or cooling, the structurant being incorporated in an amount so that the liquid component can be pumped at temperatures of 50 ° C or more (e.g., 50 ° C), but causes sufficient solidification during the second and / or third steps to form a granulate product that flows freely. In a second aspect, the invention provides a granular detergent composition or component prepared through this process.

DETAILED DESCRIPTION OF THE PREFERRED MODALITIES The granulated product thus prepared can be considered as free flowing, if it has a dynamic flow rate (DFR) preferably greater than 90 ml / s. Conveniently, the DFR can be measured by a technique whereby the known volume of the powder is allowed to flow through a calibrated orifice and tube. The flow time between the two light sensors is automatically registered and the DFR is calculated with the known volume and the recorded flow time. The granular detergent compositions according to the present invention may be in the form of complete products ready for sale to the consumer. Alternatively, they can be formulated as base powders or auxiliaries for mixing with other detergents. In any case, such compositions may have a bulk density of 550 g / 1, most preferably at least 650 g / 1. However, these products can also be produced with lower apparent densities. Preferred embodiments of the process and composition according to the present invention can be characterized through the strength and modulus E of a sample of: (a) a tablet composition produced by the process; and / or (b) the tablet formed by cooling the liquid component until it solidifies. The resistance measurement (hardness) can be obtained using an Instron pressure device. The powder is formed into tablets in a punch and die to form a tablet with a diameter of 9 mm and a height of 16 mm, formed by exerting a maximum pressure of 10 tons on the surface of the tablet. In the case of a solidified liquid component of the process before it comes into contact with the solid component, the diameter of the tablet is 14 mm and its height is 19 mm. The tablet (powder or liquid component) is destroyed between a fixed plate and a moving plate. The speed of the moving plate is set at 5 m / min, which results in a measuring time of approximately 2 seconds. The pressure curve is recorded in a computer. In this way, the maximum pressure (at the time of rupture of the tablet) is given and the module E is calculated from the inclination. For the granulated product, the minimum value of P raa preferably is 0.5 M Pa, most preferably 2 M Pa and the minimum Emod value is preferably 20 M Pa, most preferably 50 M Pa. However, for the component solidified liquid, Pmax at 20 ° C is preferably a minimum of 0.2 M Pa, for example from 0.3 to 0.5 M Pa. At 55 ° C a typical scale is from 0.05 to Q.25 M Pa. At 20 ° C, Emod for the mixture is preferably a minimum of 3 M Pa, for example 5 to 10 M Pa. The liquid component is preferably prepared in a dynamic shear mixer to pre-mix the components thereof and perform any neutralization of the anionic precursor. The dynamic mixer is preferably located in a loop with a heat exchanger to remove heat from the reaction of said neutralization. In the context of the present invention, the term "structuring" means any component that allows the liquid component to achieve solidification in the granulator and therefore good granulation, even if the solid component has a low liquid carrying capacity. The structurants can be c a t and go s as those that are believed to exert their structuring effect (solidification) through one of the following mechanisms, mainly: recrystallization (eg, silicate or phosphate); creation of a network of finely divided solid particles (eg, silicas or clays); and those that exert spherical effects at the molecular level (eg, soaps or polymers), such as those types commonly used as detergent builders. One or more structurants can be used. Soaps represent a preferred class of structure, especially when the liquid component comprises a liquid ionic surfactant. In many cases, it may be desirable for the soap to have an average chain length greater than the average chain length of the liquid nonionic surfactant but less than twice the average chain length of the latter. If desired, the solid components can be compounded or dispersed in the liquid component. The typical amounts of the essential components of the ingredients of the liquid phase are as follows. Preferably from 10% to 98% by weight of the substantially liquid component comprises a liquid anionic surfactant, most preferably from 30% to 70% by weight and especially from 40% to 50% by weight; and preferably from 98% to 10% by weight of the anionic surfactant, most preferably from 70% to 30% and especially from 50% to 40% by weight. The total amount of structurant of preference is from 2 to 30% by weight of the liquid component, most preferably from 5% to 20% or from 5% to 15% by weight and especially from 10% to 15% by weight. It is generally preferred (although not absolutely in the form of a command) that the liquid component comprises at least some liquid nonionic surfactant. However, in general, other organic components can be used in place of or in addition to the liquid nonionic surfactant. The liquid component is also preferably substantially non-aqueous. That is, the total amount of water in it is not more than 15% by weight of the liquid phase, preferably not more than 10% by weight, typically from 5% to 8%, especially from 6% to 7%. %.

Typically, from 3% to 4% by weight of the liquid component can be water as a reaction byproduct and the rest of the water present will be the solvent where the alkaline material dissolves. The "liquid phase" preferably does not have all the water in place of that of the above-mentioned sources, perhaps, except for the amounts of oxygen / impurities It is very preferred to form some or all of the anionic surfactant in situ in the liquid component through an appropriate acid precursor and an alkaline material such as an alkali metal hydroxide, for example NaOH, since the latter usually must be dosed as an aqueous solution, which inevitably incorporates some water. The reaction of an alkali metal hydroxide and acid precursor also produces some water as a byproduct, however, in principle, any inorganic alkaline material can be used for neutralization, but inorganic alkaline materials soluble in water are preferred. is sodium carbonate, alone or in combination with one or more other water-soluble inorganic materials, eg bicarbonate or sodium silicate. As described above, sodium carbonate can provide the alkalinity necessary for the washing process, but can also serve as a builder. In this case, the invention can be advantageously used for the preparation of detergent powders wherein the calcium carbonate is the only detergency builder or the main detergency builder. Then, substantially more carbonate will be present than that required for the neutralization reaction with the acid anionic surfactant precursor. The liquid component optionally can comprise dissolved solids and / or finely divided solids which are dispersed therein. The only limitation is that with or without dissolved or dispersed solids, the liquid component must be pumpable at temperatures of 5 ° C or higher, or at any speed, 60 ° C or higher, for example 75 ° C. Preferably, it is solid below 50 ° C, preferably at 25 ° C or less. Generally speaking, pumpable liquid components have a viscosity not greater than 1 Pa at a shear stress of shear stress. The structurants cause the solidification in the mixer preferably to produce the mixture and the tablet strength as described above. Typically the temperature in the granulation is greater than 10 ° C, preferably greater than 20 ° C below the temperature at which the mixture is prepared and pumped into the granulator. If the solid component comprises or substantially consists of a phosphate builder, the weight ratio of the liquid component to the solid component when the two are contacted for "mixing is from 0.25: 1 to 0.5: 1. The solid comprises or consists substantially of an aluminosilicate builder, this ratio preferably being from 0.4: 1 to 0.7: 1. Suitable anionic surfactants are well known to those skilled in the art Examples suitable for incorporation in the liquid phase include alkylbenzene sulfonate, particularly linear alkyl benzene sulphonates having an alkyl chain length of 8 to 15 carbon atoms; primary and secondary alkyl sulphates, particularly primary alkyl sulphates of 12 to 15 carbon atoms; alkyl ether sulphates; olefin sulfonates, alkyl xylene sulphonates, dialkyl sulfosuccinates, and fatty acid ester sulfonates. s are the sodium salts. The nonionic surfactant component of the liquid phase can be any one or more of the liquid nonionics selected from primary and secondary alcohol ethoxylates, especially aliphatic alcohols of 8 to 20 carbon atoms ethoxylated with an average of 1 to 20. moles of ethylene oxide per mole of alcohol, and very especially the primary and secondary aliphatic alcohols of 10 to 15 carbon atoms, ethoxylated with an average of 1 to 10 moles of ethylene oxide per mole of alcohol. The ethoxylated non-ionic surfactants include 1 quot 1 i g 1 i, 2 monoethers, and 1 i co s, and 1 i i i i i i i i i (glucamide). The liquid acid precursor can be selected from linear alkylbenzene sulphonic acids, alpha olefin sulfonic acids, internal olefin sulphonic acids, fatty acid ester sulfonic acids, and combinations thereof. The process of the invention is especially useful for producing compositions comprising alkyl benzene sulphonates through the reaction of alkylbenzene sulphonic acid cx >; corresponding, for example, Dobanoico ex Shell acid. The linear or branched primary alkyl sulphates having from 10 to 15 carbon atoms can also be used. The solid component with which the liquid phase is mixed preferably comprises a builder. The total amount of builder in the final compositions is conveniently 10 to 80% by weight, preferably 15 to 60% by weight. The builder may be present in an auxiliary together with other components or, if desired, separated from builder particles containing one or more builders materials which may be employed. The present invention is especially applicable for use, wherein the solid component comprises hydratable salts, preferably in substantial amounts such that at least 25% by weight of the solid component preferably at least 10%. in weigh. Hydratable solids include inorganic sulphates and carbonates, as well as inorganic phosphate builders, for example, sodium orthophosphate, pyrophosphate and tripolyphosphate. Other suitable improvers include crystalline and amorphous aluminosilicates, for example zeolites as described in GB-A-1 473 201; amorphous aluminosilicates as described in GB-A-1 473 202; and mixed crystalline / amorphous aluminosilicates as described in GB 1 470 250; and layered silicates as described in EP-B-164 514. The aluminosilicates may conveniently be present in a total amount of 10 to 60% by weight, and preferably in an amount of 15 to 50% by weight. The zeolite used in most conventional particulate detergent compositions is zeolite A. However, advantageously, maximum aluminum zeolite P (zeolite MAP) described and claimed in EP-A-384 070 can be used. MAP zeolite is an alkali metal aluminosilicate of type P having a silicon to aluminum ratio not exceeding 1.33, preferably not exceeding 1.15, and most preferably not exceeding 1.07. Other inorganic builders that may be present include sodium carbonate (as mentioned above, an example of a hydratable solid), if desired in combination with a crystallization seed for calcium carbonate as described in GB-A-1. 437 950. As mentioned above, said sodium carbonate may be the residue of an inorganic alkaline neutralizing agent used to form a non-ionic structuring agent in situ. Organic builders that may be present include polycarboxylate polymers such as polyacrylates, co-polymers and acrylic phosphinates; monomeric polycarboxylates such as citrates, gluconates, oxy di succinates, glycerol mono-, di- and tri-succinates, carboxymethyl 1-oxy-succinates, carb ox ime ti 1-ox imates, dipico-1-inmates, hydroxyethyl iminiocetates, aminopolycarboxylates such as tri-nitric oxide (NTA), ethylene terephthalate (EDTA) and imino-diacetates, alkyl and alkenylmalonates and succinates; and salts of sulfonated fatty acid. A copolymer of maleic acid, acrylic acid and vinyl acetate is especially preferred since it is biodegradable and thus environmentally desirable. This list is not intended to be exhaustive.

Especially preferred organic builders are preferably suitable in amounts of 5 to 30% by weight, preferably 10 to 25% by weight; and acrylic polymers, very especially copolymers, which are conveniently used in amounts of 0.5 to 15% by weight, preferably 1 to 10% by weight. The detergency builder is preferably present in an alkali metal salt, especially in a sodium salt form. The granular detergent compositions of the invention may contain, in addition to the nonionic and ionic surfactants of the liquid mixture, one or more other detergent active compounds (surfactants), which may be selected from soap and detergent actives without soap anionic, cationic, nonionic, amphoteric and z wi teri or cosy mixtures thereof. These can be dosed at any stage before or during the procedure. Many suitable detergent active compounds are available and fully described in the literature, for example in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch. The preferred detergent-active compounds that can be used are soaps and synthetic soap-free anionic and non-ionic compounds. The detergent compositions according to the invention may also contain a bleach system, desirably a peroxy bleach compound, for example, an inorganic persalt or organic peroxyacid, capable of producing hydrogen peroxide in aqueous solution. The peroxy bleach compound can be used in conjunction with a bleach activator (bleach precursor) to improve the bleaching action at low wash temperatures. An especially preferred bleaching system comprises a peroxy bleach compound (preferably sodium percarbonate optionally together with a bleach activator), and a transition metal bleach catalyst as described and claimed in EP 458 397A and EP-A-509 787 Usually, any bleach and other sensitive ingredients such as enzymes and perfumes will be sifi ed after granulation as minor ingredients. Typical minor ingredients include sodium silicates, corrosion inhibitors including silicates; anti-redeposition agents such as cellulosic polymers; fluorescent agents; inorganic salts such as sodium sulfate, foam control agents or foam boosters as appropriate; proteolytic and lipolytic enzymes; colorants; sparks of color; perfumes; foam controllers; and fabric softening compounds. This list is not intended to be exhaustive. The powder flow can be improved through the incorporation of a small amount of an additional powder structure, for example, a fatty acid (or fatty acid soap), a sugar, an acrylate or an acrylate polymer. or sodium acetate, or sodium silicate, which is suitably present in an amount of 1 to 5% by weight. With respect to the equipment used for the mixing steps of the process (ie, after the mixing of the liquid and solid components), the liquid component is preferably mixed with the solid components in a first mixing step in a metal cleaner. / high speed sensor to form a granular detergent material. Op.c ona lme nt e, the granulated detergent material of the first mixing step can subsequently be treated in a second mixing step in a moderate speed granulator / densifier. If a product of high bulk density is desired, in this stage it can be combined or maintained in the required deformable state. In any case, the product of the first mixing step or the second mixing step can then be cooled and / or dried. The residence time in the first step of the high speed mixing in the first mixing step 'is preferably around 5., to 30 seconds. The residence time in the moderate-speed mixer / densifier during any optional (optional) secondary mixing step is preferably about 1 to 10 minutes. It is possible to use any of these procedures as a continuous procedure, but it can be performed as an intermittent procedure in a high shear or low shear rate mode. In the first mixing step, the solid components of the. The material is thoroughly mixed with the liquid mixture through a high speed mec cient / den i f i ctor. Said mixer provides a high energy stirring inlet and obtains complete mixing in a very short time. As a high-speed metering device, the Lodige (Commercial Trademark) CB 30 recirculator can be used. This appliance essentially consists of a large, static hollow cylinder having a diameter of approximately 30 cm. which is placed horizontally. Halfway, it has a rotating arrow with several different types of blades mounted on it. This can be rotated at speeds between 100 and 2500 rpm, depending on the degree of densification and the desired particle size. The blades on the arrow provide a complete mixing action of solids and liquids, which can be mixed at this stage. The average residence time depends a little on the rotational speed of the arrow, the position of the blades and the weir in the exit opening. Other types of high-speed densitometer can also be contemplated having a comparable effect on detergent powders. -For example, a Shugi (Trade Mark) or Drais (Trade Mark) K-TTP 80 granulator can be used. In a first mixing step, the components of the material are thoroughly mixed in the me zc 1 a do r / ns The high velocity material is for a relatively short time of about 5-30 seconds, preferably under conditions whereby the starting material is still carried, or maintained in a deformable state, which will be subsequently finished. In the case of the production of high bulk density products, after the first mixing step, if the resulting detergent material still has a considerable porosity, then instead of selecting a longer residence time in the me zc 1 a do r In order to obtain a further increase in bulk density, it can then be subjected to the second additional mixing period in which the detergent material is treated for 1-10 minutes, preferably for 2-5 minutes, in a moderate speed granulator / densifier. During this second processing step, the conditions are such that the powder is brought to, or maintained in a deformable state. As a consequence, the porosity of the particle will be further reduced. The main differences with the first step lie in the lower mixing speed and the longer residence time of 1-10 minutes, and the need for the powder to be deformable. The second optional mixed step can be successfully performed on a Lódige (Trade Mark) KM 300 mixer, also known as the Plowshare Lódige. This apparatus essentially consists of a hollow static cylinder that has a rotation arrow in half. In this arrow, several blades are mounted in the form of an electrical outlet. This can be rotated at a speed of 40-160 rpm. Optionally, one or more high speed cutters can be used to avoid excessive agglomeration. Another suitable machine for this step is, for example, Drais (Trade Mark) KT 160. However, instead of using a high-speed mech machine 1 / to do / nsific of high speed, followed by a machine me zc 1 to do / speed rating - moderately, the same effect can be obtained using an individual machine operated at two speeds. It can be operated first at a high speed for the milling / de-firing and then at a moderate speed for the granulation / densification. Suitable machines include mixers of the Fukae '' 'FS-G series; the series Diosna V ex Dierks Sohne, Germany; Pharma MatrixR ex T.K. Fielder Ltd; England; FujiR VG-C series ex Fuji Sangyo Co., Japan; the Roto1 ex Zanchetta & Co. Srl, Italy and the SchugiR granulator F 1 e_x omi x. For use, handling and storage, the densifying detergent powder must be in a free-flowing state, therefore, in a final step, the powder can be dried and / or cooled if necessary. This step can be carried out in a known manner, for example, in a fluid bed apparatus (drying, cooling) or in an air filter (cooling). It is advantageous if the powder needs a cooling step only, since the required equipment is relatively simple and more economical. For the production of high bulk density products, any optional second mixing step and preferably also for the first mixing step, the detergent powder can be brought to a deformable pitch in order to obtain optimum densification. The high speed mixer / densifier and / or the moderate speed granulator / densifier are then able to effectively deform the particulate material in such a way that the particulate porosity is considerably reduced or maintained at a low level, and consequently the apparent density it is increased. The invention will now be explained in more detail with reference to the following non-limiting examples.

EXAMPLES 1. Granulation of STP: Preparation of the mixture in the loop reactor with acid LAS 69.4 kg / h Surfactant / fatty acid premix surfactant Nonionic surfactant 7 EO 58.9 kg / h Nonionic surfactant 3 EO 31.7 kg / h Fatty acid C16-C18 17.7 kg / h eutralization with caustic soda at a pH of 11: NaOH solution (50%): 22.3 kg / h This mixture (200 kg / h, water content = 10%) was used for the granulation of 600kg / h STP in the recirculator (Loedige CB30). 2. Granulation of STP, Sulphate and Carbonate: Preparation of the mixture in a loop reactor with: LAS acid 74.7 kg / h Neutralization of AS acid with caustic soda: NaOH solution (50%): 18.4 kg / h Alkaline silicate solution ( 45%): 38.1 kg / h Neutralization of the alkalinity with a pre-mix of nonionic surfactant / fatty acid: Nonionic surfactant 7 EO: 63.3 kg / h Nonionic surfactant 3 EO: 34.1 kg / h Fatty acid C16-C18 17.1 kg / h This mixture (245.6kg / h, water content = 13.2%) was used for the granulation of the following powders in the recirculator (Loedige CB30): STP: 700 kg / h Sulphate: 350 kg / h Carbonate: 100 kg / h To. light of this description, the modification of the examples described, as well as other examples, are all within the scope of the present invention as defined by the appended claims which will now become apparent to those skilled in the art.

Claims (17)

1. A process for preparing a granular detergent composition, the process comprising a first step of preparing a liquid component comprising a structurant, a second step for mixing the liquid component with a solid component in a granulator, and optionally, a third step of drying and / or cooling, the structurant being incorporated in an amount so that the liquid component can be pumped at temperatures of 50 ° C or more, but causes sufficient solidification during the second and / or third steps to form a granular product that flows freely .

2. The process according to claim 1, wherein the liquid can be pumped at a temperature of 60 ° C or more, preferably at 75 ° C or more.

3. The process according to any of the preceding claims, wherein the liquid component is solid below 50 ° C, preferably at 25 ° C or less.

4. The process according to any of the preceding claims, wherein the liquid component solidifies to form a tablet that at 20 ° C has a value of Pma? of at least 0.2 M Pa, preferably from 0.3 to 0.5 M Pa and / or an Emod value of at least 3 M Pa, preferably from 5 to 10 M Pa.

5. The process according to any of the preceding claims, wherein the liquid component is substantially non-aqueous.

6. The process according to claim 5, wherein the liquid component contains no more than 15% by weight of water.

7. The process according to any one of the preceding claims, wherein the granular detergent composition can be formed into a tablet having a value of P m a, -. of at least 0.5 M Pa and / or an Emod value of 20 M Pa.

8. E. The process according to any of the preceding claims, wherein the solid component comprises a solid hydratable material.

9. The process according to any of the preceding claims, wherein the solid component comprises a builder material.

10. The process according to claim 9, wherein the builder material comprises a phosphate improver.

11. The process according to claim 9 or claim 10, wherein the builder material comprises an aluminosilicate.

12. The process according to any of the preceding claims, wherein the liquid component further comprises a liquid nonionic surfactant.

13. The method according to claim. 12, wherein the liquid component contains from 10% to 98% by weight of that component of the liquid nonionic surfactant.

14. The process according to any of the preceding claims, wherein the liquid component contains from 98% to 10% by weight of that anionic surfactant component.

15. The process according to any of the preceding claims, wherein the liquid component contains up to 30% by weight of the structurant component.

16. The process according to any of the preceding claims, wherein the weight ratio of the liquid component to the solid component is from 0.25: 1 to 0.7: 1.

17. The granular detergent composition prepared through the process according to any of the preceding claims.