ES2184514T5 - DETERGENT COMPOSITIONS IN THE FORM OF PILLS. - Google Patents

Abstract

A detergent tablet of a composition in the form of compressed particles, in which the tablet or an area thereof comprises an organic detergent and a water-soluble detergency builder, characterized in that the tablet or zone thereof is compacted from of a composition containing: (i) particles containing at least 45% of their own weight of non-ionic detergent, and (ii) other ingredients.

Description

Detergent compositions in the form of pills

This invention relates to compositions detergents in the form of pills, especially pills to be used in fabric washing. Such pills have the advantage of that do not require the user to measure a volume of powder or liquid. Instead, one or more pills provide an amount appropriate composition to wash a single load on a machine Washing machine or possibly by hand. Therefore, they are easier to handle and supply for the consumer.

Detergent compositions in the form of pills have been described in a certain number of documents and They are distributed in commerce.

Such pills are usually prepared compressing or compacting an amount of detergent composition in particle shape It is desirable that the tablets have a adequate mechanical strength when dry before being used, even if they disintegrate and disperse / dissolve rapidly when they are added to the wash water. There is a difficulty for Get both properties simultaneously. As it is used more pressure when a tablet is compacted, the density rises and the resistance of the tablet, but there is also a reduction in disintegration / dissolution rate when the tablet enters contact with the wash water at the time of use. He Organic detergent serves as a binder, but an amount normal of this detergent can also delay the breakdown and dissolution of a pill. The document EP-A-466485 of the same applicant explains that as a pill is moistened, the detergent anionic can form various viscous phases that delay the water penetration inside the tablet.

This document EP-A-466485 describes tablets of detergents in which the anionic detergent is contained in a first particulate component of the composition. This first particulate component provides 2 to 40% of The overall composition. In most of the examples in this document, the non-ionic detergent was mixed with particles or led in them that provided a majority of the composition total. The detergent compositions and tablets comprising a nonionic surfactant as a minor proportion of the particles in which the surfactant is present are described also in EP 716,144, EP 711,827, EP 839,906, EP 838.519 and WO 98/42817.

In some pills that are distributed currently in commerce, anionic and non-ionic detergents are incorporated together in a base powder that is mixed with other ingredients to form the compressed composition in form of pills. Spray-dried base powder constitutes approximately 40% of the composition. Contains active detergent as about 25% of the base powder and non-ionic detergent as about 12% of the same powder.

In the present invention, the tablets of detergents are prepared using particles that incorporate a higher proportion of non-ionic detergent. According to this invention, a tablet of composition in the form of compressed particles, in which the tablet or an area thereof comprises organic detergent and soluble detergency builder in water, characterized in that the tablet or area thereof is compacted from a composition that contains

(i) particles that contain themselves in minus 45% of its own weight of non-ionic detergent, and

(ii) other ingredients.

These pills can be homogeneous or heterogeneous In the present specification, the term "homogeneous" is used to indicate a tablet produced by compaction of a single composition in the form of particles, but does not imply that all the particles of the composition are necessarily of equal composition. The term "heterogeneous" It is used to indicate a tablet consisting of a plurality of discrete areas, for example, layers, inserts or coatings, each derived by compaction from a composition in particle shape In a heterogeneous tablet, each discrete area of the tablet preferably constitutes at least 10% of the weight Global pickup.

Using such particles, it has been possible prepare pills with a good combination of properties, particularly resistance before being used and rapid disintegration when placed in contact with water at the time of being used

The particles may contain enough non-ionic detergent to constitute at least 50% of its own weight. Preferably, the composition of the tablet or zone contains 1 to 40% by weight of non-ionic detergent, of which at least Half is present in the form of solid particles.

Anionic detergent will also be present. frequently and can be provided in the form of particles that contain at least 20% of its own weight of non-anionic detergent soapy.

A tablet of this invention intended for fabric washing will generally contain, globally

at least 5%, preferably at least 8%, up to no more than 40%, possibly not above 30% by weight of non-soapy organic detergent which is preferably a combination of anionic and non-ionic detergents;

at least 15%, better at least 20 or 25%, up to 80%, possibly not above 70 or 60% by weight of one or more detergency builders that can be water soluble, insoluble in water or a mixture of soluble improvers and insoluble;

optionally, other ingredients that they can be at least 10% by weight of the tablet.

The invention could also be carried out in the form of dishwasher machine pads, with a small percentage of non-ionic detergent present as 1 to 8% by weight, with the condition that the tablet comprises said particles containing the minus 45% of non-ionic detergent, from 20 to 99% of the detergency and possibly nothing at all detergent anionic

The constituent materials of the tablets of detergents will be discussed in more detail, and mentioned various optional and preferred features.

Nonionic detergent particles

The particles of non-ionic detergents used in this invention they contain at least 45%, preferably at least 50% of its own weight of non-ionic detergent (i.e. one or more organic compounds that are nonionic and have properties detergent surfactants). Preferably, they contain less than 10% by weight of synthetic anionic detergent (i.e., not soapy) and, preferably, substantially no anionic detergent no soapy.

Organic detergent compounds do not ionic products include in particular the products that can be obtained by reaction of alkylene oxides, especially oxide of ethylene with compounds that have a hydrophobic group and an atom of reactive hydrogen, for example, aliphatic alcohols, acids, amides or alkyl phenols.

Nonionic and non-ethoxylated detergents include alkyl polyglycosides, glycerol monoethers and polyhydroxy amides (glucamide).

Nonionic detergent compounds specific are condensed from (C 8-22) alkyl - phenol oxide of ethylene, the condensation products of primary alcohols or C 8-20 linear aliphatic secondary or branched with ethylene oxide, and products prepared by condensation of ethylene oxide with the reaction products of propylene oxide and ethylenediamine.

Especially preferred are the ethoxylates of primary and secondary alcohols, especially primary alcohols and secondary of C_ {15-15} and C 12-15 ethoxylates with an average of 3 to 20 moles of ethylene oxide per mole of alcohol.

Nonionic detergent particles preferably contain an inorganic carrier material that is Probably insoluble in water. The insoluble carrier material it can comprise silica or aluminosilicate, such as a zeolite. Without However, if aluminosilicate is present, it is preferred that the amount is less than 10% by weight of the particles. The amount of non-ionic detergent can exceed 50% by weight of the particle, for example, 52% or more.

Particles containing a detergent do not ionic absorbed in a solid carrier material can be prepared spraying the non-ionic detergent onto the carrier material in a granulator or some other type of mixing device.

Other materials may also be included, that serve to improve the physical properties of the particles. Such materials are often referred to as "agents. structuring. "Examples thereof that may be present are polyethylene / polypropylene glycol with a molecular weight medium in the range of 4,000-12,000, soap sodium, polyvinyl alcohol with an average molecular weight in the range of 30,000-200,000, metal succinate alkaline, etc. The preferred amount of structuring agent is in the range of 0.5 to 20% by weight. A structuring agent can be added with other ingredients or during a second stage of granulation.

A preferred carrier is silica that has a oil absorption capacity of at least 1.0 ml / g. The capacity Oil absorption is a parameter that is well known and can be measured by the technique described in DIN ISO 787/5. Preferably, the oil absorption capacity is at least 1.5 ml / g, more preferably at least 2.0 ml / g.

Preferably, there is at least 10%, more preferably at least 15% of this silica in the particles, and the Amount of silica in the particles is greater than the amount of aluminosilicate, if any. The particles may contain less than 10% of its own aluminosilicate weight.

The particles of non-ionic detergents are can elaborate in a single stage or two stage procedure mixing together the components in a granulator (for example, an Eirich RV02 granulator, or an installation like the Fukae mixer from Fukae Powtech Co. of Japan, the series Diosna V supplied by the company Dierks & Sohne, Germany, the Pharma Matrix of the company TH Fielder Ltd., England, the series Lodige CB and the Dais T160 series from Daiz Werke GmbH, Mannheim, Germany).

Nonionic detergent particles have preferably an average particle size in the range of 200 at 2,000 µm, so that at least 80% of these particles they have a particle size in the range of 180 to 2,000 \ mum. Nonionic detergent particles can provide of 1, better 2 or 3% up to 30% or possibly more than one tablet or An area of a pill. More specifically, these particles they can constitute 8 to 20% of a pill or an area of a tablet.

Generally, a pill or an area of a tablet according to this invention will contain 1%, preferably from 3 to 40% by weight of non-ionic detergent, of which at least half is present in the form of said particles that contain at least 40% of your own detergent weight not ionic.

Anionic detergent

A pill will often contain a anionic detergent that is one or more organic compounds not Soaps with detergent surfactant properties.

The anionic detergent may comprise, total or predominantly linear alkyl benzene sulphonate formula

one

Where R is linear alkyl of 8 to 15 atoms carbon and M + is a solubilizing cation, especially sodium.

A primary alkyl sulfate that has the formula

ROSO_ {3} {} - M +}

in which R is an alkyl chain or alkenyl of 8 to 18 carbon atoms, especially 10 to 14 carbon atoms and M + is a solubilizing cation, it is also commercially significant as an anionic detergent and can be used in this invention.

Often this linear alkyl benzene sulphonate or primary alkyl sulfate of the above formula, or a mixture thereof, will be the non-soapy anionic detergent desired and may provide 75 to 100% by weight of the detergent not soapy anionic.

Examples of other anionic detergents not Soaps that can be used include olefin sulphonates, alkane sulphonates, dialkyl sulphosuccinates and sulphonates of esters of fatty acids.

Anionic detergent particles can contain some nonionic detergent. Detergent particles Anionic may also contain minor ingredients such as water, sodium carboxymethyl cellulose, fluorescent, dyes, etc.

Anionic detergent is incorporated preferably in the form of particles containing at least 20% of  its own weight in anionic detergent, possibly a proportion greater than at least 50% of its own weight. The particles that contain between 20 and 40% anionic detergent can be prepared by spray drying procedures or granulation.

The procedures for producing particles that contain high concentrations of anionic detergent se set forth in WO 96/06916A and WO 96/06917A (Unilever). In these procedures, an aqueous paste containing a detergent anionic or, alternatively, an acid detergent precursor and also an alkaline neutralizing agent are fed to an area drying in which the pulp material is heated to reduce its water content, the material being subsequently cooled drying in a cooling zone to form particles of Detergent.

Desirably, the drying zone is under a slight vacuum to facilitate the separation of water and components volatile The vacuum can be 100 Torr until the pressure atmospheric, as this provides significant flexibility to the procedure However, a vacuum above 500 Torr up atmospheric pressure has the advantage of reducing the investment of capital while providing vacuum operation.

The procedure can be carried out in any suitable apparatus, but it is preferable that a fast reactor. Suitable fast reactors include, by For example, the Flash Drier system available at VRV Spa Impianti Industiali. The drying zone may have an area of heat transfer of at least 10 m2. The area of cooling desirably has a heat transfer area of at least 5 m 2.

As described in WO 97 / 32003A of the same applicant, the material in the cooling zone can be treated with a stream of refrigerant gas. Alternatively, a non-detergent solid material can be introduced into this area finely divided, such as zeolite or silica particles, so that it adhere to the surface of the particles. Such material can provide 3 to 25% of the weight of the particles.

The above procedural paths may provide quick-drying detergent particles that understand at least 60% by weight of the particle of a non-anionic detergent and no more than 5% by weight of the water particle.

These anionic detergent particles may comprise anionic detergent in an amount of at least 66% by weight of the particles, even better at least 70% but possibly not more than 96%. The particles may have a porosity of 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 180-1,500 micrometers. As mentioned, the anionic detergent can be formed in situ by neutralization of a free acid. The neutralizing agent may be a solution of sodium hydroxide or sodium carbonate. However, neutralization in situ is unlikely to be appropriate when the anionic detergent is primary alkyl sulphonate (PAS) because its acid form is unstable.

Anionic detergent particles can provide from 5% to at least 30% of the weight of the tablet or area of a pill. The amount of them can be at least 8% or 10%. Its quantity should not be above 20% of the weight of the pill or area, especially when the particles contain the minus 70 or 75% of its own weight of anionic detergent no soapy.

Other kinds of organic detergents, such as Amphoteric detergents, may be included, but are not preferred.  It is preferred that at least 50%, better at least 90% by weight of the entire non-soapy organic detergent in the tablet or area of a tablet is contained in said particles containing at least 40% non-ionic detergent or other particles containing the minus 20% of its own weight of non-soapy organic detergent.

Particles to improve disintegration

It has been found and described previously that the disintegration rate of the pills can be Enhanced including certain materials. So, the document EP-A-839906 of the same applicant exposes that the speed of disintegration of the tablet can be Enhanced include sodium tripolyphosphate, which has a high contained in the Phase I form of anhydrous sodium tripolyphosphate and It can also be partially hydrated. Documents EP-A-711,827 and EP-A-838-519 of same applicant state that the rate of disintegration of pills with a non-phosphorus detergency builder e Water insoluble can be accelerated including materials highly soluble in water, especially certain salts.

In preferred forms of this invention, a constituent of the tablet or zone is constituted by particles that contain a material that serves to accelerate the disintegration of the tablet in water and is a material of high water solubility either it is a specified form of sodium tripolyphosphate, or a combination of the two. Such material may be present as at at least 15 or 20% of the composition of the tablet or area thereof, possibly at least 25% up to 50, 55 or 60%, and possibly plus.

Highly water soluble materials, which they are one of the two possibilities, they are compounds, especially salts, with a solubility at 20 ° C of at least 50 grams per 100 grams of water

A solubility of at least 50 grams per 100 grams of water at 20 ° C is an exceptionally high solubility: Many materials that are classified as water soluble are less soluble than this.

Some highly water soluble materials that can be used are cited below, with their solubilities  expressed as grams of solid to form a saturated solution in 100 grams of water at 20ºC:

Material Solubility in water (g / 100 g) Sodium Citrate Dihydrate 72 Carbonate potassium 112 Urea > 100 Acetate sodium, anhydrous 119 Acetate trihydrate of sodium 76 Magnesium sulphate 7H 2 O 71 Acetate potassium > 200

On the contrary, the solubilities of some Other common materials at 20ºC are:

Material Solubility in water (g / 100 g) Chloride sodium 36 Sulfate dehydrochloride sodium 21.5 Sodium carbonate anhydrous 8.0 Sodium percarbonate anhydrous 12 Sodium perborate anhydrous 3.7 Sodium tripolyphosphate anhydrous fifteen

Preferably, this highly soluble material in water it is incorporated in the form of particles of the material in a substantially pure form (i.e. each of these particles contains above 95% by weight of the material). But nevertheless, said particles may contain material of this solubility mixed with other material, with the condition that the material of specified solubility provide at least 50% by weight of these particles, preferably at least 80%.

Another possibility is that said particles that favor the disintegration be particles that contain sodium tripolyphosphate with more than 50% thereof (by weight of the particles) in the form of anhydrous Phase I. Such particles can contain at least 80% by weight of tripolyphosphate and possibly at minus 95%

Sodium tripolyphosphate is very well known as a sequestering detergent builder in the detergent compositions It exists in a hydrated form and two crystalline anhydrous forms. These are the crystalline anhydrous form normal, known as Phase II which is the low temperature form, and Phase I which is stable at elevated temperature. The conversion of the Phase II in Phase I takes place quite quickly by heating above the transition temperature, which is approximately 420 ° C, but the reverse reaction is slow. Consequently, the Phase I sodium tripolyphosphate is metastable at temperature ambient.

A procedure for the elaboration of particles containing a high proportion of the Phase form I of sodium tripolyphosphate by spray drying below 420 ° C is provided in the document US-A-4,536,377.

The particles that contain this Phase form I will often contain the Phase I form of sodium tripolyphosphate as at least 55% by weight of the tripolyphosphate in the particles. Other forms of sodium tripolyphosphate will usually be present in a smaller scope. Other salts may be included in the particles, although this is not preferred.

Desirably, this sodium tripolyphosphate is partially hydrated The extent of hydration should be at minus 1% by weight of the sodium tripolyphosphate in the particles. Be it can be in the range of 2.5 to 4%, or it can be higher, by example, up to 8%.

The right material is available in the Commerce. Suppliers include the company Rhone-Poulenc of France and Albright & Wilson from United Kingdom.

The product "Rhodiaphos HPA 3.5" of the Rhone-Poulenc company has been found to be particularly suitable. It is a characteristic of this degree of sodium tripolyphosphate that hydrates very quickly in an assay Olten Standard It has been found to hydrate as quickly as anhydrous sodium tripolyphosphate, although prehydration seems which is advantageous to avoid unwanted crystallization of the hexahydrate when the material comes into contact with water in the Time to be used.

Detergency Enhancer

A pill or area of the pill will contain generally a detergency builder. This can be sodium tripolyphosphate of the type just described. May include sodium tripolyphosphate that has more than the Phase form II or that is hydrated. It can be some other kind of improver the detergency It can contain globally 30 to 60% by weight of sodium tripolyphosphate, estimated as anhydrous.

Inorganic detergency builders that contain phosphorus and that are soluble in water include the orthophosphates, metaphosphates, pyrophosphates and metal polyphosphates alkaline, as well as sodium and potassium tripolyphosphates.

Alkali metal aluminosilicates are highly desirable as insoluble detergency builders in water and acceptable for the environment for fabric washing. Alkali metal aluminosilicates (preferably sodium) they can be crystalline or amorphous or mixtures thereof, and have The general formula:

0.8 - 1.5 \ Na_ {2} \ cdot O3 {Al} {2} O_ {3} \ cdot 0.8 - 6 \ SiO_ {2} \ cdot xH_ {2} O

These materials contain some bound water (indicated as "xH_ {2} O") and are required to have a calcium ion exchange capacity of at least 50 mg CaO / g Preferred sodium aluminosilicates contain 1.5-3.5 SiO2 units (in the formula previous). Both amorphous and crystalline materials can be easily prepare by a reaction between sodium silicate and sodium aluminate, as described extensively in the bibliography.

Exchange detergency enhancers Ionic of suitable crystalline sodium aluminosilicates is described, for example, in GB 1429143 (Procter & Gamble). Preferred sodium aluminosilicates of this type with commercially available and well-known zeolites A and X, and the new zeolite P with maximum described aluminum content and claimed in EP 384,070 (Unilever). This form of zeolite P is also called zeolite MAP. A commercial form of This is indicated as zeolite A24. The detergency builder Water insoluble can be a layered sodium silicate as described in US 4664839.

NaSKS-6 is the registered trademark for a crystalline layered silicate marketed by the company Hoechst (commonly abbreviated as "SKS-6"). NaSKS-6 has morphology delta-Na2 SiO5 silica layered. Be can be prepared by methods such as those described in the documents DE-A-3,417,649 and DE-A-3,742,043. Another one of these Layered silicates, which can be used, have the general formula NaMSi_ {O} {2x + 1} \ cdot and H2O in which M is sodium or hydrogen, x is a number from 1.9 to 4, preferably 2 e y is a number from 0 to 20, preferably 10.

The detergency builders soluble in Non-phosphorous water can be organic or inorganic. The inorganic detergency builders that may be present include alkali metal carbonates (generally sodium); while organic detergency builders include polycarboxylate polymers, such as polyacrylates and acrylic / maleic copolymers, monomeric polycarboxylates such as citrates, gluconates, oxidisuccinates, mono-, di- and glycerol tri-succinates, carboxymethyloxysuccinates, carboxymethylximalonates, dipicolinates and hydroxyethyliminodiacetates.

Pill compositions include preferably polycarboxylate polymers, more especially Acrylic / maleic polyacrylates and copolymers that can work as detergency builders and also inhibit the deposit not desired on the fabrics from the washing liquid.

The detergency builder materials they can be incorporated in the form of particles containing 40 at 80% by weight of detergency builder, the rest being another material, probably not detergent. Such particles can provide 10 to 60% of the composition of the tablet or area of the tablet.

Proportions

Generally, a tablet prepared according with this invention it will contain globally from 2 to 5% by weight up to 40 or 50% by weight of non-soap detergent, and 5 or 10% by weight up to 60 or 80% by weight of detergency builder. A discreet area of a heterogeneous pill may or may not contain these proportions of detergent and detergency builder.

Other ingredients

The detergent tablets according to the invention They may contain a bleaching system. This includes preferably one or more peroxygen bleaching compounds, for example, inorganic persalts or organic peroxyacids, which can be used in conjunction with activators to improve the bleaching action at low wash temperatures. Nap present a peroxygen compound, the amount is likely to be place in a range of 10 to 25% by weight of the tablet.

Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate and percarbonate sodium. Bleach activators have been widely described in The technique. Preferred examples include acid precursors peracetic, for example, tetracetylethylenediamine (TAED) and perbenzoic acid precursors. Bleaching activators quaternary ammonium and phosphonium described in US 4751015 and US 4818426 (Lever Brothers Company) are also of interest. Other type of bleach activator that can be used, but which is not a bleaching precursor, is a transition metal catalyst as described in the documents EP-A-458397, EP-A-458398 and EP-A-549272. A bleaching system may also include a bleach stabilizer (sequestrant heavy metals) as ethylenediamine tetramethylene phosphonate Y diethylenetriamine-pentamethylene phosphonate.

The bleach activator is present usually in an amount of 1 to 10% by weight of the tablet, possibly less in the case of a metal catalyst than transition that can be used as 0.1% or more by weight of the tablet.

The detergent tablets of the invention they can also contain one of the detergency enzymes well known in the art for its ability to various gradients soils and stains and thus help its suppression. Enzymes Suitable include various proteases, cellulases, lipases, Amylases and mixtures thereof, which are designed to suppress a Dirt diversity and fabric stains. Enzymes of detergency are commonly employed in the form of particles or conglomerates, optionally with a protective coating, in a amount from about 0.1% to about 3.0% by weight of The pill.

The detergent tablets of the invention may also contain a fluorescent (optional brightener), for example, Tinopal (registered trademark) DMS or Tinopal CBS available at Ciba-Geigy AG, Basel, Switzerland. The Tinopal DMS is 4,4'-bis- (2-morpholino-4-amylino-s-triazin-6-ylamino) stilbene disulfonate of disodium; and Tinopal CBS is 2,2'-bis (phenyl-styryl) disulfonate of disodium

A material is advantageously included antifoam, especially if a detergent tablet is primarily intended for use in washing machines Automatic drum type with front loading. The materials Defoamers in granular form are described in EP 266863A (Unilever). These antifoam particles comprise normally a mixture of silicone oil, petroleum jelly, silica hydrophobic and alkyl phosphate as active material antifoam, absorbed in an inorganic carrier material based in a water soluble, absorbed and porous carbonate.

It may also be desirable that a tablet of detergent of the invention include an amount of a silicate of alkali metal, particularly ortho-, meta- or sodium di-silicate. The presence of these alkali metal silicates can be advantageous for provide corrosion protection of the parts metallic in washing machines, apart from providing some detergency enhancing effect. Preferably, the particles with high detergent content contain 5 to 15% silicate by weight of the particles. This improves resistance and flow free of these particles before the formation of pills

Additionally, the ingredients that can be optionally used in a detergent tablet for the fabric washing of the invention include agents anti-redeposition as sodium carboxymethyl cellulose, linear chain polyvinylpyrrolidone and cellulose ethers as methyl cellulose and ethyl hydroxyethyl cellulose agents fabric softeners; heavy metal sequestrants such as EDTA; perfumes; and colored dyes or specks.

Pill Formation

The formation of the pills includes the compaction of a particulate composition that includes particles containing detergent, particles favoring the disintegration and any other ingredients. A variety of machinery for the formation of pills that can be used. Generally, it will work by compression of a quantity of composition in the form of particles that It is confined in a mold.

The formation of pills can be carried out without heat application, in order to take place room temperature or at a temperature above the ambient. In order to carry out the formation of pills to a temperature that is above the ambient, the composition in particle form is preferably supplied to machinery of pellet formation at an elevated temperature. Naturally, This will supply heat to the tablet forming machinery, but the machinery must also be heated from someone else mode.

If any heat is supplied, it is planned that this is supplied in a conventional manner, as by doing pass the particulate composition through an oven, instead of using any energy application of microwave.

Size and density of the tablets

The size of a pill will vary appropriately in the range of 10 to 160 grams, preferably 15 to 60 grams, depending on the conditions of the intended use, and if represents a dose for a medium load in a washing machine of cloth or dishwasher or a fraction of that dose. The Pills can be any way. However, for greater ease of packaging are preferably section blocks substantially uniform transverse, such as cylinders or cuboids. The overall density of a tablet is preferably located in a range of 1040 or 1050 g / liter, possibly 1100 g / liter, up to 1450 g / liter or more. The density of the tablet can be well placed in a range up to 1350 or 1400 g / liter.

The tablets can be prepared by process comprising mixing said particles containing in themselves at least 45% of its weight of non-ionic detergent with other detergent ingredients, and compact the composition resulting in the form of pills.

Example one

Adjuvant particles of anionic detergent (LAS-A) containing 70% (of its own weight) of linear alkyl benzene sulphonate using a 1.2m2 VRV Flash Drier fast dryer, from the manner described in WO 97/32002. It had three sections of equal jackets. Dosing holes for both liquids such as dusts were placed just before the first hot section, with dosing holes in the middle of the jacketed available in the two final sections. Was added Zeolite through this hole in the final section. A electrically powered oil heater provided the heating to the first two jacket sections, being used oil temperatures between 120 ° C and 190 ° C. Water was used from environmental treatment at 15ºC to cool the jacket in the final section The contribution of air flow through the reactor is controlled between 10 and 50 m 3 / h by opening a shunt in the Exhausted steam extraction fan. The engine was made run at full speed, providing a maximum speed of approximately 30 m / s.

A mono-bomb was calibrated to dose LAS acid at room temperature, and a pump peristaltic was calibrated to dose sodium hydroxide at 47% Spindle distributors were calibrated to dose both sodium carbonate and zeolite A24. Carbonate sodium and liquids were added just before the first hot section, but the zeolite was added in the third section It was cooled.

The product was in the form of particles of free flow that contained

LAS-A: Ingredients % in weight Alkyl benzene sulphonate linear (LAS) 70% Carbonate sodium 2% Zeolite 25% Impurities no detergents and moisture 3%

The non-ionic detergent particles (ND1) that They contained 56% non-ionic detergent were prepared by granulating non-ionic detergent with silica and soap in an Eirisch granulator RVCO2. (For a larger scale, a recycler would be appropriate Loedige).

The silica was Sorbosil TC15 supplied by the Crosfield company, Warrington, UK. Non-ionic detergent It was heated and mixed with a fatty acid, then it was sprayed on the silica in the granulator while simultaneously spraying enough alkali to neutralize the fatty acid. The product was cooled in a fluidized bed that also separated the fine materials. Oversized particles (> 1400 µm) were separated by sieving.

The resulting ND1 particles contained:

LAS-A: Ingredients % in weight Detergent no ionic 56% Silica 30% Soap and humidity 14%

Non-ionic detergent particles comparative (ND2) were produced by granulating zeolite A24 which is P zeolite with maximum aluminum content from Crosfields with trisodium citrate in a Loedige recycler. The detergent does not ionic was mixed with fatty acid and pulverized, while it also sprayed enough 50% aqueous hydroxide to neutralize fatty acid. The resulting product contained

ND2: Ingredient % in weigh Zeolite A24 53.8 Sodium citrate 7.9 Nonionic detergent 24.2 Soap 4.1 Water 10.0

Improver particles of the ZB1 zeolite detergent by continuously dosing zeolite A24, granular trisodium citrate and a 40% solution of copolymer of acrylate / maleate (Sokolan CP5 solution) in a Loedige recycler CB30 The CB30 device was operated at 1500 rpm. The dust that came out was fed through a Lodige KM300 grid (120 rpm), in which densification took place. The resulting powder is dried in a fluidized bed with an air temperature of 110 ° C. The composition of the detergent builder particles resulting was:

ZB1: Ingredient % in weigh Zeolite A24 53.6 Episode Citrate 17.2 Sokolan CP5 19.0 Humidity 10.2

Detergent particles LAS-A and ND1 and the improver particles of the ZB1 detergency and other ingredients were used to prepare Formulation tablets shown in the following table.

Comparative tablets used the particles of ND2 instead of the particles of ND1.

2

The tablets were prepared containing 43 grams of the comparative composition or 46 grams of the composition of Example 1. These tablets contained all 3.8 parts of alkylbenzene sulphonate, 1.67 parts of non-ionic detergent, 8.5 parts of zeolite and 10.4 parts of acetate trihydrate sodium. The tablets were compacted with an applied force of 9.7 kN

The dissolution rate of the constituents Soluble pills was tested by a procedure of test in which a pill was placed in a plastic sieve with a mesh size of 2 mm, submerged in 9 liters of water current at room temperature of 20 ° C. The sieve was subjected to a stirrer, which rotated at 200 rpm. The conductivity of the water is verified until it reached a constant value. The time for Dissolution of the tablets was taken as time (T90) for that the change in the conductivity of the water will reach 90% of its final magnitude

The resistance of the pills was tested by a procedure in which a cylindrical tablet is radially compressed between the plates of a test machine materials until the tablet breaks. When failing, the pill it cracks and decreases the applied force necessary to Maintain plate displacement. The measurement is interrupted when the force applied necessary to maintain displacement It has fallen to 25% of its maximum value.

The maximum force is the force in the fault (F_ {f}). From this force measurement, a test parameter called diametral fracture tension, using the equation

\ sigma = 2 \ frac {Ff} {\ pi DT}

in the that

sig is the tension of diametral fracture in pascals,

F_ {f} is the force applied in Newtons to cause the fracture,

D is the diameter of the tablet in meters and

t is the thickness of the tablet in meters.

The force to cause fracture and tension of the diametral fracture calculated from it are a direct assessment of resistance and indicate the resistance of pills to break when handled by a consumer in the Time to be used. The amount of energy (or mechanical work) applied before fracture is a measure of the deformability of the tablet and is relevant to the resistance of the tablet to the breakage during transport. This energy or work before failure it is valued as the "breaking energy" which is the area under a graph of force versus displacement, to the point of break. It is provided by the equation:

E_ {b} = \ int \ limits ^ {x_ {f}} _ {o} F \ (x) \ dx

in the that

E_ {b} is the breaking energy in joules,

x is the displacement in meters,

F is the force applied in Newtons for a displacement x, y

x_ {f} is the offset in the fault.

The values of dissolution time, voltage of fracture and breakage energy are shown in the following table:

Comparative Example 1 DFS (kPa) 18.9 21.5 T_ {90} (s) 123 120 E_ {b} (mJ) 9.2 17.3

It can be seen that the breaking energy of the pills in Example 1 was better than the pills comparatives, although other properties were similar.

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Examples 2 and 3

Adjuvant particles of anionic detergent (LAS-B) as described in the Example 1, but with a higher detergent content. They contained

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LAS-B: Ingredients % in weight Alkyl benzene sulphonate linear (LAS) 82% Carbonate sodium 4% Zeolite 10% Impurities no detergents and moisture 4%

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The LAS-B of the particles above and the ND1 of the non-ionic particles described in the Example above were mixed with other materials to prepare two detergent compositions set forth in the table below. These included sodium tripolyphosphate particles that were specified that they contained 70% of phase I form and contained 3.5% of hydration water (Rhodia-Phos HPA 3.5 available in the company Rhone-Poulenc).

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3

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A detergent composition was prepared comparative, starting from a spray-dried base powder (BP1) of the following composition:

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BP1: Ingredient Parts by weight Sodium alkylbenzene sulphonate linear 11.00 Alcohol C13-15 fatty 7EO 2.60 Alcohol C13-15 fatty 3EO 2.40 Soap 0.20 Sodium tripolyphosphate* 16.90 Copolymer of acrylate / maleate 1.50 Sodium silicate 4.00 Carboxymethyl cellulose particles of sodium 0.30 Fluorescent on support inert 0.15 Humidity e impurities 5.95 Total 45.00 * Added to the suspension as anhydrous sodium tripolyphosphate containing at least 70% form Phase II

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This powder was mixed with other ingredients such as follow:

Ingredient Parts by weight Powder base (BP1) 45.0 Rhodiaphos HPA3.5 tripolyphosphate 30.2 Sodium percarbonate 15.1 TAED particles 3.4 Particles of anti-foaming 3.2 Sequestrant, dirt release polymer and particles 2.7 colored of sodium carbonate Total 99.6

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These compositions are also exposed together to another in the following table

4

40 grams portions of each were compressed composition in the form of cylindrical pads 44 mm in diameter. Various amounts of compaction force were used. The composition of Example 2 was also compressed in the form of 32 grams pills, in order to provide pills of this composition that contained the same amount of detergent as the comparative tablets of 40 grams.

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The pills were tested as in the Example 1. The results are shown in the following tables, arranged to show the comparison of the pills with a Diametral fracture tension (DFS) similar:

5

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6

It is clear that the invention makes possible increase breakage energy, reduce dissolution time and / or reduce the weight of the tablet needed to supply the same amount of detergent

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Example 4

LAS-B and ND1 of the attached particles described in the previous examples for Prepare pills of the following formulation:

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Parts by weight Anionic Detergent Particles (THE B'S) 16.0 Nonionic Detergent Particles (ND1) 10.0 Rhodiaphos HPA3.5 tripolyphosphate 48.0 Copolymer and acrylate / maleate 2.0 Sodium silicate 4.0 Particles of carboxymethyl cellulose from sodium 0.5 Polyvinylpyrrolidone 1.0 Sodium carbonate 7.0 Sodium sulfate 5.0 Particles of anti-foaming 3.5 Sequestrant, dirt release polymer and particles 3.0 colored of sodium carbonate Total 100.0

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Example 5

The attached particles (LAS-B and ND1) described in the previous examples were used together with additional ingredients to prepare 40 gram pills with two layers of unequal weight (10 grams and 30 grams). The overall formulation was similar to Example 2 but contained slightly more alkylbenzene sulphonate and slightly less tripolyphosphate. A base powder (BP1A) was used with the same composition used in Examples 2 and 3 but taken from a different batch to prepare comparative tablets with two uneven weight layers. The overall formulation was the same as for the previous comparative tablets.

When these two pills were prepared in layers, the composition for a layer was placed in a mold and slightly compacted, and the composition for the other layer was then added to the mold and a force of compaction to mold content.

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The formulations are shown in the table next:

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8

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Pills and comparative tablets were tested in the same ways as for Example 1 previous, with the following results:

10

Claims (17)

1. A detergent tablet of a composition in the form of compressed particles, in which the tablet or an area thereof comprises an organic detergent and a water-soluble detergency builder, characterized in that the tablet or zone thereof is compacted from a composition that contains: (i) particles containing at least 45% itself of its own weight of non-ionic detergent, containing particles an inorganic carrier material insoluble in water and the non ionic is primary or secondary alcohol ethoxylate and (ii) other ingredients. 2. A tablet according to claim 1, in a that the composition contains particles containing at least 50% by weight of non-ionic detergent. 3. A tablet according to claim 1 or the claim 2, wherein the composition of said tablet or zone Contains 3 to 40% by weight of non-ionic detergent, of which at minus half is present as said particles. 4. A tablet according to any one of the previous claims, wherein the composition of said tablet or area also includes particles that contain at least 20% of its own weight of non-soapy anionic detergent. 5. A tablet according to claim 4, in the that the composition of said tablet or zone contains from 5 to 50% in weight of non-soap anionic detergent, of which at least half it is present as said particles containing at least 45% in weight of non-ionic detergent or as particles containing the minus 20% of its own weight of another non-soap detergent. 6. A tablet according to any one of the previous claims, wherein at least 90% of the detergent organic non-soapy in the tablet or area of it is content in said particles containing at least 45% of its own weight of non-ionic or particulate detergent containing minus 20% of its own weight of another non-soap detergent. 7. A tablet according to any one of the previous claims, wherein the composition of said tablet or area includes particles that contain at least 80% of its own weight of one or more selected water soluble materials between compounds with a water solubility that exceeds 50 grams per 100 grams of water at 20 ° C, sodium tripolyphosphate containing at least 50% of its own weight of the anhydrous form of Phase I, and its mixtures 8. A tablet according to claim 7, in that the composition of said tablet or zone contains 15 to 60% in weight of said particles containing at least 80% of their own weight of one or more water soluble materials. 9. A tablet according to claim 7, in that the composition of said tablet or zone contains from 25 to 50% in weight of said particles containing at least 80% of their own weight of one or more water soluble materials. 10. A tablet according to any one of the claims 7 to 9, wherein the composition of the tablet or zone contains from 20 to 60% by weight of said tripolyphosphate which is partially hydrated in order to contain water from hydration in an amount that is at least 1% by weight of the sodium tripolyphosphate. 11. A tablet according to any one of the claims 7 to 9, wherein the composition of the tablet or zone contains up to 55% by weight of particles containing at least 95% of its own weight of said tripolyphosphate, which is partially hydrated in order to contain water from hydration in an amount that is at least 1% by weight of the sodium tripolyphosphate. 12. A tablet according to any one of the claims 7 to 9, wherein the composition of the tablet or zone contains at least 20% by weight of said particles that they contain at least 80% of their own weight of one or more salts with a water solubility that exceeds 50 grams per 100 grams of water at 20 ° C. 13. A tablet according to claim 12, in which said compound is one or more of partial sodium citrate or fully hydrated, partially or completely sodium acetate hydrated and potassium acetate. 14. A tablet according to any one of the previous claims, wherein, overall, said tablet Contains 5 to 40% non-soap organic detergent and 15 to 80% of detergency builder. 15. A tablet according to claim 14, which Globally contains 30 to 60% by weight of tripolyphosphate of sodium, estimated as anhydrous. 16. A tablet according to any one of the previous claims, wherein the composition of the tablet  or zone thereof contains 10 to 60% of particles containing 40 to 80% of its own weight of a detergency builder and 20 to 60% of its own weight of another non-detergent material. 17. A procedure to prepare a pill as defined in any one of the preceding claims,  process comprising mixing said particles containing in themselves at least 45% of their own weight of non-ionic detergent with other detergent ingredients, and then compact the resulting composition in the form of pills.