EA001548B1 - Production of anionic detergent particles - Google Patents

Abstract

1. A process for producing detergent particles comprising an anionic surfactant, the process comprising the steps of feeding a paste material comprising water and an anionic surfactant into a drying zone, heating the paste material in the drying zone to reduce the water content thereof, average time of the paste material to be in the drying zone is less than 5 minutes and subsequently cooling the paste material in a cooling zone at a temperature not exceeding 50 degree C to form detergent particles, characterised by introducing a layering agent into the cooling zone during the cooling step. 2. A process for producing detergent particles comprising an anionic surfactant, the process comprising the steps of feeding a paste material comprising water and an anionic surfactant into a drying zone, heating the paste material in the drying zone to reduce the water content thereof average time of the paste material to be in the drying zone is less than 5 minutes and subsequently cooling the paste material in a cooling zone at a temperature not exceeding 50 degree C to form detergent particles, characterised by treating the paste material in the cooling zone with a stream of cooling gas. 3. A process according to claim 1 or claim 2, wherein the anionic surfactant comprises a linear alkylbenzene sulphonate. 4. A process according to claim 3, wherein the linear alkylbenzene sulphonate comprises from 10% to 100% by weight of the total anionic surfactant. 5. A process according to any preceding claim, wherein the paste material comprises no more than 50% by weight of water. 6. A process according to any preceding claim, wherein the layering agent comprises an aluminosilicate, a silica or a mixture thereof. 7. A process according to claim 1, wherein the layering agent is dosed into the cooling zone at a weight ratio of from 1:5 to 1:20 relative to the finished particles. 8. A process according to any preceding claim, wherein the anionic surfactant is formed by admixture of the free acid form of the anionic surfactant and a neutralising agent. 9. A process according to any preceding claim, wherein the resultant particles comprise at least 75% by weight of the anionic surfactant and no more than 10% by weight of water. 10. A process according to any preceding claim, wherein the resultant particles have a D(4,3) average particle diameter of from 180 to 1500 microns. 11. Detergent particles produced according to any preceding claim. 12. Detergent particles according to claim 11 comprising at least 60% by weight of the particle of an anionic surfactant, and not more than 5% by weight of water, the particles being coated with a layering agent. 13. Detergent particles according to claim 11 comprising an anionic surfactant, in an amount of at least 60% by weight of the particle, wherein the particles are coated with a layering agent and have a porosity of from 0% to 25% by volume of the particle and a particle size distribution such that at least 80% of the particles have a particle size of 180 to 1500 microns. 14. Detergent particles according to any of claims 11-13, wherein the anionic surfactant comprises a linear alkylbenzene sulphonate. 15. A detergent composition comprising detergent particles according to any of claims 11-14 and a base powder.

Description

The present invention relates to anionic washing particles, a method for their production and their composition. In particular, the present invention relates to a method for producing detergent particles having a high level of anionic surfactant, which comprises drying a detergent paste containing an anionic surfactant, and to particles obtained by this method.

Detergent active compounds commonly used in detergent compositions include anionic surfactants, for example linear alkyl benzene sulfonates (LA8), linear alkyl ethyl sulfates (LE8) and primary alkyl sulfates (PA8) and non-anionic surfactants, for example, alcohol ethoxylates. To improve the washing action, it is desirable to provide a high level of detergent-active substance in the powder.

Often, the maximum level of active substance that can be included is limited by the requirements of the process. Detergent compositions having a high bulk density are usually produced by a process including mixing or granulating the components of the composition and / or the main powder obtained, for example, by spray drying and provide significant consumer benefits compared to lower bulk compositions.

The introduction of detergent-active compounds in such formulations in liquid form is known. However, since it is necessary to control the ratio of liquids and solids to form washing granules, the maximum level of detergent-active substance that can be introduced in this way is limited. It is also known to incorporate an anionic surfactant, for example LA8 or PA8, into detergent compositions by adding in solid form, i.e., a particle containing a surfactant and other components of the composition, for example, sodium carbonate and a component. So far, the level of anionic surfactant present in such additives has been limited due to the need to provide good flow properties and reduce the tendency to agglomerate.

European patent application EP-A506184 describes a method for continuously dry neutralizing a liquid acid precursor of an anionic surfactant. Detergent particles having an active detergent content in the range of 30-40 wt.% Can be prepared by this process.

EP-A572957 describes a method for producing anionic surfactant powder by feeding an aqueous suspension of a surfactant containing 60-80% solids to an evaporator, forming a surfactant film on the wall of the reactor and scraping it from the wall into drying and enrichment time of the suspension.

The German patent application IE-A-4304015 describes a method for forming surfactant granules having a reduced stickiness by introducing a surfactant paste into a fluidized bed device containing particulate material, while granulating and drying the fluidized bed material , and the subsequent addition of an anticoagulant to the particles exiting the device from the air stream. Through this method, washing particles can be produced having an active component content of from 15 to 90% by weight.

In European patent application EP-A572957 it is described that the wall of the reactor is at a temperature in the range of 50-1400 ° C, and as an example of the highest wall temperature is 1300 ° C. It is said that higher temperatures cause thermal splitting and a change in color tone and are thus unfavorable. In addition, this document describes that the blades in the reactor are driven to provide a peripheral speed, preferably in the range of 2-20 m / s with an exemplary maximum peripheral speed of 10.5 m / s. Bulk weights up to about 0.5 g / cm ^{3 are given} .

However, as described in international patent application No. 96/06916 (unpublished prior to the priority date of this patent application), detergent particles having a high bulk density, a high level of anionic surfactant and excellent powder properties can be produced by heating a paste containing a surfactant, in the first zone even at a higher temperature and then cooling the particles thus formed.

Typically, the aforementioned method comprises feeding a paste-like material containing water in an amount usually exceeding 10% by weight of the paste and an anionic surfactant into the drying zone.

The paste is heated in the drying zone to reduce the water content and subsequently cooled in the cooling zone to obtain detergent particles.

The method described in international patent application XVO 96/06916 is particularly applicable to the use of PA8 as an anionic particle detergent component. Unfortunately, the larger the amount of LA8 in the anionic component, the greater the tendency to form granules with an adhesive surface, which is harmful to meet the requirement of obtaining dry homogeneous granules in the final product.

It was found that this problem can be solved by introducing a layering agent (coating agent) into the cooling zone.

European patent application EP-A390251 describes the use of a layering agent as granulating aid in the production of washing granules, the components being processed in a high speed mixer and then held or delivered to the deformable stage in the mixer at a moderate speed.

Thus, the first object of the present invention is a method for the production of detergent particles containing an anionic surfactant, comprising the steps of feeding a paste-like material containing water and an anionic surfactant into a drying zone in which there is no fluidized bed, heating the paste-like material in the drying zone in order to reduce the water content in it and the subsequent cooling of the paste-like material in the cooling zone for the formation of washing particles, characterized in that in the cooling zone tions during cooling operation lamination administered agent.

Instead of using a layering agent, the same effect can be achieved by treating the paste in the cooling zone with a cooling gas. Thus, a second embodiment of the present invention is a method for producing detergent particles containing an anionic surfactant comprising the steps of feeding a paste material containing water and an anionic surfactant into a drying zone in which there is no fluidized bed, heating the paste material in drying zone to reduce the water content in it and subsequent cooling of the paste-like material in the cooling zone for the formation of washing particles, characterized by the processing of paste of the material in the cooling zone of the cooling gas flow.

It is necessary that the cooling gas is generally dry, and it can be, for example, air or nitrogen at a temperature below 0 ° C. The cooling gas may be used as a countercurrent gas stream.

However, the present invention is not limited only to compositions in which the anionic component contains or consists of L8. It is also advantageous to use formulations with other anionic components, including RL8 or L8.

The layering agent may be any material capable of coating particles in a cooling step to improve its grain size. To this end, comparatively inert materials are preferred materials, but especially any of those inert materials that have a beneficial effect in the washing liquid, for example, aluminosilicates, silica talc and clay. A mixture of such materials may be used. Examples of aluminosilicates and silicas are described in more detail below. The presence of any such material as a coating on the finished particles does not preclude the possibility of the presence of material inside the particles.

Relative to other common particle materials, the metering weight ratio of the layering materials in the cooling step is preferably in the range of 1: 3 to 1:20, more preferably in the range of 1: 9 to 1:20.

It is possible that a slight vacuum may be created in the drying zone to facilitate the removal of water and volatile substances. The sparseness can be from a pressure of 13.3 kPa up to atmospheric pressure, as this gives the process considerable flexibility. However, pressures in excess of 66.5 kPa up to atmospheric pressure have the advantage of lowering capital investment when creating vacuum conditions.

Control of residence time and particle size can be provided, and process performance can be increased by mixing the material in the drying and / or cooling zone.

Preferably, the process is continuous, as this facilitates the continuous movement of particles. In a continuous process, the volumetric flow rate of the paste is accordingly in the range of about 10-25 kg / m ² / h, and preferably in the range of 17-22 kg / m ² / h, for example, is 20 kg / m ² / h.

Accordingly, the average residence time in the drying zone is less than 5 minutes. Particularly preferred is a residence time of less than 4 minutes and most preferred is the shortest possible residence time to reduce the possibility of decomposition (especially with RL8) and increase the productivity of the product.

Stirring the paste in the heating zone usually provides efficient heat transfer within the paste and facilitates the removal of water. Stirring reduces the contact time of the paste particles with the wall of the drying zone, which together with effective heat transfer reduces the likelihood of formation of overheating points, which can lead to decomposition. In addition, improved drying is provided, thus allowing a shorter residence time / increased throughput to the drying zone.

In the case of PA8, the paste-like material is preferably heated to a temperature not exceeding 170 ° C. to prevent thermal decomposition.

The method according to the present invention enables the production of particles having a bulk density of, for example, greater than 550 g / cm ³ .

The material is cooled in a cooling zone in which a temperature of not higher than 50 ° C and preferably not higher than 40 ° C, for example 30 ° C, is accordingly maintained. It is desirable that mixing takes place within the cooling zone to ensure that the material is effectively cooled. By actively cooling the particles, the likelihood of thermal decomposition occurring due to the heating of the particles to a temperature higher than that indicated above is reduced, and the stickiness can be reduced. Such active cooling can be carried out by circulating, for example, cold water or chilled water (for example, glycol water at a temperature of 5 ° C), around the cooling zone, for example, in a cooling jacket.

Preferably, the paste-like material comprises a mixture of an anionic surfactant and water, although other components may be present that are desired or introduced as impurities from a previous process, for example, a surfactant manufacturing process. Preferably, the paste-like material contains at least 60 wt.%, More preferably at least 65 wt.% And especially at least 70 wt.% Of the anionic surfactant. Accordingly, the paste contains not more than 50 wt.% And preferably not more than 30 wt.% Water. The paste-like material must be capable of pumping at a temperature at which it must be fed into the drying zone and this may limit the maximum level of surfactant present in it.

When the anionic substance contains PA8, the paste is suitably fed into the drying zone at a temperature in the range of 50-70 ° C and preferably in the range of 50-65 ° C.

The method according to the invention can be carried out in any suitable device. However, it is preferable to use a scrubber dryer and especially a spray dryer. A suitable spray dryer is, for example, a spray drying device sold by the company UKU8rA rgoss551 1tr1ai Ιηάι.ΐ5ΐπ; · ι1ί. The ratio of the heat transfer area of the drying zone to the heat transfer area of the cooling zone is usually in the range 3: 1-1: 1, for example, about 2: 1.

Perhaps, if desired, two or more drying zones can be used in front of the cooling zone. A single device can be used to provide a drying zone and a cooling zone or, alternatively, a separate device, for example, dryers and a coolant layer, can be used.

Typically, the cross-sectional drying zone is substantially circular and thus defined by a cylindrical wall. Preferably, this wall is heated by means of a heating jacket through which water, steam or oil can be supplied. Preferably, the inside of the wall is maintained at a temperature of at least 130 ° C and especially at least 140 ° C. Preferably, the drying zone has an evaporation rate of from 3 to 25, and especially in the range of 5-20 kg of water per 1 m ² of heating surface per hour.

Preferably, the cooling zone is defined by a cylindrical wall. In the case of a continuous process, respectively, + the device is designed so that the drying zone and the cooling zone are almost horizontally aligned to facilitate effective drying, cooling and moving the material through the drying and cooling zones in the mainly horizontal direction.

Accordingly, in the drying zone, and preferably in the cooling zone, there is a mixing means that mixes and moves the paste of the surface-active material and forms granules from it when passing through the said zones. Preferably, the mixing means comprises a series of radially extending blades and / or blades mounted on an axially mounted rotating shaft. Preferably, the blades and / or blades are inclined to move the paste and, preferably, spaced from the inner wall by a distance of not more than 10 mm, for example 5 mm.

It was found that the present invention has particular application in the manufacture of high-quality washing particles containing LA8, which otherwise could not be obtained by previously known methods. However, the anionic component may also be in the form of PA8, LE8 or any other anionic surfactant and mixtures thereof with or without LA8.

LAB8 is usually the most commercially available substance in the form of a free acid. Unlike PA8 acid, which is very unstable, LAB8 acid is very stable and is sold by a number of suppliers, for example, Pc1ga1a550 (Pc1gc5a). Es1sg (Es1sg company). Magysap (Nick company), No. 11ku1sps 540b (U151a firm) and Tkogsiet

B83 (company Yesyesh). It comes in the form of a viscous liquid that is easy to handle, which is easy to store and handle. In any case, the paste in the drying zone can be formed by supplying a liquid anionic precursor of the anionic surfactant and a neutralizing agent to the drying zone or the entrance zone of the drying zone and forming an anionic surfactant in place.

The neutralized L8 acid is commercially available in powder form.

L8 powders are mainly dried in a tumble dryer or spray dryer and may have acceptable powder properties when fresh. However, they are less preferred since they can absorb moisture from the atmosphere and become sticky and difficult to handle. Their fluidity deteriorates and they become prone to caking. Common commercially available powders are MagNap AN (80% LAB8), MagnNap A390 (90% LAB8), and MagnNap A396 (96% LAB8), supplied by the company II or I1agu1 L90 (90% LAB8) Step 1 O85 (85% LAB8) and Step 1 L80 (80% LA8), supplied by Ipdeg.

Now on the market there is PA8 in the form of fine powder or in the form of noodles. Fine powder is usually dusty, having a significant number of particles less than 150 microns in size. PA8 noodles are usually produced by extrusion of a dried PA8, which has the appearance of soap chips and usually has a very large particle size and very low porosity, which leads to poor solubility. To increase the level of detergent active material in the detergent composition, a subsequent dosage of detergent particles is known to provide a composition having a high level of active material content.

However, ONCE in the form of finely ground powder and ONCE noodles are usually unsuitable for subsequent dosing into the detergent composition, since the particles of the composition and particles of the material of the subsequent dosage are usually of different sizes and thus tend to segregate and become unsightly. The method according to the present invention makes it possible to obtain detergent particles having a high level of detergent active material and suitable porosity and particle size characteristics.

Thus, the third object of the invention are detergent particles containing at least 60 wt.% Particles of anionic surfactant, preferably containing or consisting of LA8 and not more than 5 wt.% Water, the particles being coated with a layering agent obtained by the method and according to the invention.

According to one embodiment of the invention, washing particles are provided comprising an anionic surfactant, preferably containing or consisting of LAB8 and preferably in an amount of at least 60 wt.% Particles, the particles being coated with a layering agent and having a porosity of 0 to 25 vol. % and a particle size distribution such that at least 80% of the particles have a size of from 180 to 1500 μm, preferably from 250 to 1200 μm and less than 10%, and preferably less than 5% of the particles have a diameter of less than 180 μm.

Accordingly, the anionic surfactant in the washing particles is present in an amount of at least 70%, preferably at least 80% and preferably at least 85% by weight of the particles. Preferably, the particles also contain water in an amount of from 0 to 8 wt.% And preferably from 0 to 4 wt.% Of the particles. Water in the particle ensures the integrity of the granules, thereby reducing the level of fine particles.

Preferably, the washing particles have a relative elongation not exceeding 2 and, more preferably, are mainly spherical to reduce segregation from other particles in the detergent composition and improve the appearance of the powder.

Preferably, any LA8 anionic surfactant has a chain length of from C ₈ to C ₁₆ , preferably from C ₉ to C _15, and most preferably a narrow range from Ci to C14.

If any TIME surfactant available has a chain length of from C ₁₀ to C ₂₂ , preferably in the range of C _{12 to} C _18, and more preferably in the narrow range of C _{12 to} C ₁₄ , Soso PA8 is particularly desirable.

If desired, the washing particle may contain mixtures of TIMES with other surface-active substances and / or components that are not surface-active substances.

Other suitable surfactants may contain linear linear alkyl ethers of sulfuric acid, oxo-alcohol sulfates, for example, alcohol sulfates with a chain from C to C ₁₅ and a chain from C ₁₃ to C ₁₅ , secondary alcohol sulfates and sulfonates, unsaturated surfactants, for example, sodium oleate, oleulosulfates , olefinsulfonate or mixtures thereof.

Particularly preferred are particles rich in bA8, i.e. particles in which the amount of LA8 exceeds the amount of any other surfactant or non-surface active substance, and more preferably exceeds the total amount of all other surface active and surface inactive components.

The sodium salt is mainly used as a surfactant, however, potassium, calcium or magnesium salts may also be present. However, it is preferable to form the anionic component by feeding the acid form of the anionic surfactant and the neutralizing agent into the drying zone or inlet zone immediately in front of the drying zone, and forming the anionic surfactant ίη δίΐιι.

If the formation of ίη δίΐιι anionic substance is carried out in the drying zone, the heat of neutralization generated in the drying zone reduces the need for external heating of the drying zone and is advantageous in comparison with technological processes in which the surface-active paste is used as raw material. In addition, it is advantageous if the precursor acid can be supplied to the drying zone in liquid form, rather than in the form of an aqueous solution, and the neutralizing agent can be concentrated. The total amount of water introduced into the drying zone can be significantly reduced in comparison with technological processes that use surface-active paste. In order to be pumped, such pastes must contain at least 30% by weight of water.

It is also possible to form detergent particles prior to dosing the layering agent directly from the previous acidic feed rather than as a two-stage process, including the production of a surfactant and the subsequent formation and drying of the paste to form detergent particles. This is advantageous since it eliminates the need for the production of surface-active paste, which may present technical difficulties due to the need to move and store the paste.

The precursor acid, for example LL§ or RL8 acid, is respectively supplied to the drying zone in the liquid phase. Since the precursor acid may be thermally unstable, it is preferable that the neutralization proceeds quickly and almost completely to minimize and preferably prevent thermal decomposition of the acid due to elevated temperature.

The precursor acid is suitably supplied at a temperature of from 40 to 60 ° C. to ensure its liquid state, but without the possibility of its thermal decomposition. The neutralizing agent can be fed into the drying zone at any desired temperature.

Accordingly, the neutralizing agent is administered in the form of an aqueous solution or suspension or solid material. Conventional neutralizing agents may be used, including alkali metal hydroxides, such as sodium hydroxide, and alkali metal carbonates, such as sodium carbonate, ideally added as a solid material.

Accordingly, the neutralizing agent is present in an amount of from 25 to 55 and, preferably, from 30 to 50 wt.% An aqueous solution or suspension. A high concentration of a neutralizing agent can lead to undesirable crystallization, and a low concentration is undesirable due to the large proportion of water.

The concentration of the solution of the neutralizing agent or suspension may be varied to control the water content in the drying zone. In this way, optimum viscosity characteristics can be obtained, whereby the material in the drying zone remains movable / pumpable.

A stoichiometric excess of a neutralizing agent relative to the acid precursor may be used. The excess neutralizing agent combines with an acid, for example sulfuric acid, which can be produced by thermal decomposition of the precursor acid.

Using the neutralization ίη δίΐη. high throughput can be achieved compared to a process in which a paste containing a pre-neutralized surfactant is used.

The mixing of the precursor and the neutralizing agent (hereinafter referred to as raw materials) in the heating zone usually provides efficient heat transfer and facilitates the removal of water. Mixing reduces the contact time between the raw material and the wall of the drying zone; which, together with efficient heat transfer, reduces the likelihood of overheating points that can lead to thermal decomposition. In addition, improved drying is provided, thereby allowing a reduction in residence time / increase throughput in the drying zone.

Other non-surface active components that may be present in the washing particles are dispersing agents, preferably polymeric materials and, more preferably, urea, sugars, polyalcohols and the components described below.

If desired, the washing particles may contain an organic and / or inorganic salt, for example a hydratable salt. Suitable materials in salts, preferably sodium, are tripolyphosphate, citrates, carbonates, sulfates, chlorides. Aluminosilicates, clays, silicas and other inorganic materials may also be included.

The particles may also contain one or more non-anionic surfactants, for example, as mentioned below in the context of the main powder with which the particles are mixed.

Similarly, organic materials, such as PEC and another polymeric component or soap, may be included in the particles, as also mentioned below.

It is particularly preferred that the salt is present in the particle when the anionic surfactant component contains LA8.

The salt content can reach up to 50 wt.% And, preferably, up to 30 wt.% Particles.

Detergent particles may have a subsequent dosage directly to the base powder obtained by any conventional method of manufacturing detergent, including a non-towed method in which the components of the detergent composition are mixed and granulated, as described, for example, in European patent application EP-A-367339 and a spray drying method followed by a tower seal. Since the washing particles produced according to the present invention can have a subsequent dosage to such powders, a significant degree of flexibility in the formation of the composition is achieved and, if desired, the level of active material in the fully formed composition can be very high. Another advantage is that a basic powder can be produced which is practically free of detergent active compounds, since the latter can be administered almost entirely as particles of a subsequent dosage.

Thus, an object of the invention is a detergent composition containing the detergent particles according to the invention and a base powder.

The ability to reduce the level of detergent active material in the main powder is particularly advantageous where the main powder is produced by the spray drying method, since the lower level of the detergent active compound in the spray drying method makes it possible to provide higher productivity, thereby increasing the overall economic efficiency of the production.

The compositions according to the invention may also contain, in addition to the detergent-active compound, a detergent component and additionally whitening components and other active ingredients to improve performance and properties.

The detergent compositions according to the invention may contain, in addition to subsequent dosage particles, one or more detergent compounds (surfactants), which can be selected from soap and non-soap anionic, cationic, nonionic, amphoteric and amphionic detergent compounds, described in detail in the technical literature, for example , in the publication ZigGass-AsOss Adspy upb Os1sgdsp15. Wo1ishs5 I apb II Ly 8s11 \\ ar1 / s1s. Preferred detergent-active compounds that can be used are soap and synthetic non-soap anionic and non-anionic compounds.

Anionic surfactants are well known to those skilled in the art. Examples are alkyl benzene sulfonates, in particular linear alkyl benzene sulfonates with a C ₈ -C ₁₅ alkyl chain; primary and secondary alkyl sulfates, in particular C ₁₂ -C ₁₅ primary alkyl sulfates; alkyl ether sulfates; olefinsulfonates; alkyl xylene sulfonates; dialkyl sulfosuccinates; and fatty estersulfonates. Sodium salts are generally preferred.

Non-ionic surfactants that can be used include primary and secondary alcohol ethoxylates, especially C ₈ -C ₂₀ aliphatic alcohols, ethoxylated with an average amount of 1 to 20 moles of ethylene oxide to 1 mole of alcohol, and especially primary and secondary aliphatic alcohols with a chain length of C ₁₀ -C ₁₅ ethoxylated with an average amount of from 1 to 10 moles of ethylene oxide per mole of alcohol. Non-ethoxylated non-ionic surfactants include alkyl polyglycosides, glycerol monoesters and polyhydroxyamides (glucamide).

The total amount of surfactant present in the detergent composition, respectively, is from 5 to 40 wt.%, Although amounts outside this range can be used if desired.

The detergent compositions of the invention also typically contain a detergent component. The total amount of detergent components in the compositions is from 1 0 to 80 wt.%, Preferably from 15 to 60 wt.%. This component may be present in addition to other components or, if desired, individual component particles containing one or more component materials may be used.

Inorganic components that may be present include sodium carbonate, if desired, in combination with crystallization seed for calcium carbonate, as described in UK patent application No. 1437950; crystalline and amorphous aluminosilicates, for example zeolites, as described in UK patent application No. 1473201; amorphous aluminosilicates, as described in UK patent application No. 1473202; and mixed crystalline / amorphous aluminosilicates, as described in UK patent application No. 1470250; and layered silicates as described in European Patent Application EP-A-164514. Inorganic phosphate components may also be present, for example sodium ortho-phosphate, pyrophosphate and tripolyphosphate, but in view of the environment, they are no longer preferred.

The aluminosilicates or used as layering agents and / or incorporated into the mass of particles can respectively be present in a total amount of from 10 to 60 wt.% And preferably in an amount of from 15 to 50 wt.%. The zeolite used in the most commercially popular granular detergent compositions is zeolite A. However, maximally aluminized zeolite P (zeolite MAP) described and subject to the claims of European patent application EP-A384070 can be advantageously used. Zeolite MAP is a type P zeolite having a silicon to aluminum ratio not exceeding 1.33, preferably not exceeding 1.15, and more preferably not exceeding 1.07.

Organic components that may be present include polycarboxylated polymers, such as polyacrylates, acrylic / maleic copolymers and acrylic phosphinates, monomeric polycarboxylates, such as citrates, gluconates, oxidisuccinates, glycerol mono-, di- and trisuccinates, carboxymethyloxymethyl aminates, - and alkenyl malonates and succinates; and sulfonated salts of fatty acids. Particularly preferred are a copolymer of maleic acid, acrylic acid and vinyl acetate, as it is biodegradable and is thus desirable from an environmental point of view. This list is not intended to be exhaustive.

Particularly preferred organic components are citrates, suitably used in amounts of 5 to 30% by weight, preferably in an amount of 1 to 10% by weight. Preferably, the component is present in the form of an alkali metal salt, especially a sodium salt.

Accordingly, the component system contains crystalline layered silicate; for example, brand 8K8-6 from the company Nossy. zeolite, for example zeolite A, and, optionally, alkali metal citrate.

The detergent compositions according to the invention may also contain a whitening component, preferably a peroxide compound, for example, an inorganic peroxide acid capable of yielding hydrogen peroxide in an aqueous solution. The peroxide whitening compound can be used together with the whitening activator (whitening precursors) to improve the whitening effect at low washing temperatures. A particularly preferred whitening component comprises a peroxide whitening compound (preferably sodium percarbonate optionally together with a whitening activator) and a transition metal whitening catalyst, as claimed in European patent applications EP 458397 and EP-A-509787.

The compositions according to the invention may contain an alkali metal carbonate, preferably sodium, to enhance the washing action and facilitate processing. Accordingly, sodium carbonate may be present in an amount of from 1 to 60 wt.%, Preferably from 2 to 40 wt.%. However, formulations containing a small amount or not containing sodium carbonate are also included in the scope of the invention.

The fluidity of the powder can be improved by introducing a small amount of a powder structurant, for example, a fatty acid (fat soap), sugar, acrylate or acrylate / maleate polymer, or sodium silicate, which, respectively, are present in an amount of from 1 to 5 wt.%.

Materials that may be present in the detergent compositions of the invention include sodium silicate; corrosion inhibitors, including silicates; redeposition agents, such as cellulosic polymers; fluorescent substances; inorganic salts such as sodium sulfate; soap suds control agents or appropriate foaming aids; proteolytic and lipolytic enzymes; dyes; color blotches; aromatic substances; foam regulators and fabric softening compounds. This list is not intended to be exhaustive.

The main composition is prepared accordingly by spray drying the suspension from compatible heat insensitive ingredients and then spraying, mixing and / or subsequent dosing of those ingredients that are unsuitable for processing through the suspension. Detergent particles produced by the method according to the present invention have a subsequent dosage to the basic composition by conventional methods.

Preferably, the detergent compositions according to the invention have a bulk density of at least 500 g / l, more preferably at least 550 g / l.

Such powders can be prepared either by spray drying, followed by tower compaction of the spray dried powder, or by completely non-towed methods such as dry mixing and granulation. A high speed mixer / granulator can be used for such mixing. Methods using high-speed mixers / granulators are described, for example, in European patent applications EP-A-340013, EP-A-367339, EP-A-390251, EP-A420317.

The invention is illustrated in more detail below through the following non-limiting examples.

Technology

A UKU machine of 1.2 m ^{2 was used} , having three identical sections with a jacket. Dispensing holes for liquids and for powders were located directly in front of the first hot section and in the last two sections there were median dispensing holes. Zeolite was added through one of these openings in the end section. An electric oil heated device provided heating for the first two sections, while the oil temperature was maintained in the range of 120-190 ° C. The surrounding processing water was used at a temperature of 1,5 ° C for the cooling jacket of the final section. The flow of fresh air through the reactor was controlled in the range of 10-50 m ³ / h by opening the bypass valve of the exhaust fan for steam. All experiments were carried out with the engine at maximum speed, giving a peripheral speed of about 30 m / s.

The mono pump was calibrated to dose LA8 acid at ambient temperature and the peristaltic pump was calibrated to supply 47% sodium hydroxide. The screw feeders were calibrated to dose both sodium carbonate and A24 zeolite for layering. Sodium carbonate and liquids were added immediately before the first hot section and zeolite was added for layering in the third cold section. A minimal amount of zeolite was added to allow free flowing granules to exit the dryer.

The following abbreviations are used in the examples below:

Ό (4.3) is the weighted average particle diameter;

ΌΡΒ - dynamic flow rate;

IST is an unconsolidated compression test.

Example 1. LA8 acid and sodium hydroxide.

Experiments were carried out at various amounts of passed material and jacket temperatures. Some of the parameters of the machine and the properties of the powder are given in table. 1. Zeolite layering was necessary in all of the examples below.

Table 1

About- razse Shirt temperature Estimated number of passed material, kg / h Volume weight ΌΡΒ % density ist ϋ / 4.3 /, μm <180, μm > 1400, μm BUT 170 ° C 37, 9 621 142 4.1 0,0 845 1,58 8.2 IN 178 ° C 65,2 617 130 4.7 0,0 1116 3.32 33,2 FROM 178 ° C 76.0 576 129 5.3 0,0 1351 1,11 49.82 Ό 178 ° C 91.9 463 101 17.6 0,0 1522 0,0 78.81 E 178 ° C 41.9 599 128 12,4 0.25 869 2.96 14.44

Sample A had excellent powder properties with an acceptable average particle size. The flowing properties of these powders were considered solely on the basis that they all contain about 90% LA8. With an increase in the amount of transmitted material, samples from B to Ό showed a slight decrease in fluidity associated with an increase in particle size. This increase in particle size was due to the increased residual moisture content inside the granules. When reducing the amount of material passed for the sample

Its fluidity improved and particle size decreased.

Without the use of zeolite layering, it would be impossible to produce any of the above powders.

Example 2. LA8 acid and solid sodium carbonate.

Experiments were conducted with varying degrees of neutralization of sodium carbonate. In the table. 2 shows some of the machine parameters and powder properties. Zeolite layering was necessary in all of the examples below.

table 2

About- razse Tem shirts Estimated number of passed material, kg / h % Converted \ 3; WITH _; Volume weight ΌΡΒ % Density ist 0 (4.3), μm <180, μm > 1400, μm BUT 145 ° C 42.7 42 624 131 5.9 0,0 812 1.47 6.25 IN 145 ° C 57.6 63 594 140 7.6 0,0 946 0.3 6.57 FROM 145 ° C 64.9 73 597 131 11.2 0,0 849 0.29 4.64

| 83 I 601 I 141 I 7.1 I 0.0 I | And I 145 ° C I 72.2

The degree of evaporation of water in these experiments was low, since water was not added. Water was taken mainly when neutralizing LAB acid. As a result, a lower jacket temperature of 145 ° C. was used. A fixed stream of sodium carbonate powder was used together with an increase in the amount of BAS acid to match the degree of neutralization of LAB acid from 42% up to 83%, as shown in Table. 2.

All of the powders produced had excellent flow properties and acceptable particle sizes. With an increase in the degree of neutralization and an increase in the amount of passed material, no deterioration of the properties of the powders was observed.

Without the use of zeolite layering, it would be impossible to produce any of the above powders.

In the light of this description, those skilled in the art will appreciate modifications to the described examples, as well as other examples that are within the scope of the present invention as defined in the appended claims.

Claims (15)

CLAIM 1. A method of manufacturing detergent particles containing an anionic surfactant, which consists in the fact that a paste-like material containing water and an anionic surfactant is fed to a dryer with a scraped surface, the paste-like material is heated in the drying zone to reduce the water content in it moreover, the average residence time in the drying zone is less than 5 minutes, and then the paste-like material is cooled in the cooling zone operating at a temperature not exceeding 50 ° C until the formation of washing particles, and uu administered lamination cooling agent in the cooling zone. 2. A method of manufacturing detergent particles containing an anionic surfactant, which consists in the fact that the paste-like material containing water and the anionic surfactant is fed to a dryer with a scraped surface, the paste-like material is heated in the drying zone to reduce the water content in it moreover, the average residence time in the drying zone is less than 5 minutes, then the paste-like material is cooled in the cooling zone operating at a temperature not exceeding 50 ° C until the formation of detergent particles, when it AOR not cooling the paste material is treated with a stream of cooling gas. 3. The method according to claim 1 or 2, characterized in that the anionic surfactant contains linear alkylbenzenesulfonate. 4. The method according to claim 3, characterized in that the linear alkylbenzenesulfonate contains from 10 to 100 wt.% The total anionic surfactant. 5. The method according to any one of the preceding paragraphs, characterized in that the pasty material contains not more than 50 wt.% Water. 6. The method according to any one of the preceding paragraphs, characterized in that the layering agent contains aluminosilicate, silica or a mixture thereof. 7. The method according to p. 1, characterized in that the layering agent is dosed into the cooling zone at a weight ratio of from 1: 5 to 1:20 relative to the finished particles. 8. The method according to any one of the preceding paragraphs, characterized in that the anionic surfactant is formed by admixing the anionic surfactant in the form of a free acid and a neutralizing agent. 9. The method according to any one of the preceding paragraphs, characterized in that the particles contain at least 75 wt.% Anionic surfactant and not more than 1 0 wt.% Water. 1 0. The method according to any one of the preceding paragraphs, characterized in that the particles have an average particle diameter of And (4.3) from 180 to 1,500 microns. 11. Detergent particles obtained by the method according to any one of paragraphs. 1 -1 0. 1 2. Detergent particles according to claim 11, containing at least 60 wt.% Anionic surfactant and not more than 5 wt.% Water, the particles being coated with a layering agent. 13. Washing particles according to claim 11, containing an anionic surfactant in an amount of at least 60 wt.%, And the particles are coated with a layering agent and have a porosity of 0 to 25% and the particle size distribution is such that at least at least 80% of the particles have a particle size of from 180 to 1,500 microns. 1 4. Detergent particles according to any one of paragraphs. 111 3, characterized in that the anionic surfactant contains linear alkylbenzenesulfonate. 1 5. Detergent composition containing detergent particles according to any one of paragraphs. 11-14 and the main powder.