ES2239176T3 - CLEANING PADS. - Google Patents

Abstract

The invention provides a tablet of compacted particulate detergent composition comprising non-soap surfactant and detergency builder, wherein the tablet or a discrete region thereof contains 1 to 20 %wt based on the total weight of the tablet of a disintegration system comprising;a) water-swellable disintegrant granules with a mean particle size of between 500-1000 micrometers, and b) a hydrophilic starch having a mean particle size of 250 micrometers or below, a solubility in water of less than 1g/100g of water at 20 DEG C and a development of expansion force of 2.0 Newtons/second or less.The tablets exhibit good disintegration properties and use ingredients from renewable sources. A method of making the tablets is also provided.

Description

Cleaning pills

The present invention relates to compositions cleaners in the form of pills. These pills are destined to disintegrate when placed in water and therefore They are intended to be consumed in a single use. Pills may be suitable for use in dishwashers, in the  fabric washing or other cleaning tasks.

Pill-shaped products have several Advantages over powdered products: for example, they do not require measure and, therefore, are easier to handle and be supplied to the wash load. In addition, they are more compact, thus facilitating a cheaper storage

Detergent compositions in the form of pads and intended for washing fabrics have been described in a a number of patent documents that include, for example, GB 911204 (Unilever), US 3953350 (Kao), EP-A-711827 WO-98/42817 and WO-99/20730 (Unilever) and are currently distributed in commerce. Pills Composition suitable for a dishwasher machine have been described in the documents EP-A-318204 and US-A-5691293 and are distributed on trade.

The tablets of a cleaning composition are they generally prepare by compressing or compacting a composition in particle shape Although it is desirable that the tablets have adequate resistance when dry, even if they are dispersed and dissolve quickly when they come in contact with water, you can It is difficult to obtain both properties together. Pills formed using a low compaction pressure tend to crumble and disintegrate in handling and packaging; although the compacted tablets with more force can be sufficiently cohesive but then they fail to disintegrate or disperse to a suitable point in the wash. The formation of pills is will often perform with enough pressure to get a compromise between these desirable but antagonistic properties. Without However, it remains desirable to improve one or the other of these. properties without prejudice to the other so that the global commitment between them. The document US-A-3018267 (Procter & Gamble) exposes that the force and therefore the pressure applied when Compact a tablet-shaped composition must be limited, or otherwise the pills would take too long to dissolve.

If a tablet contains a surfactant organic, this can work as a binder, making the tablet has plastic properties. However, it can delay also the disintegration of the tablet forming a viscous gel when the tablet comes into contact with water. Therefore, the Presence of the surfactant can make it harder to get so much a good resistance as a good speed of disintegration: the problem has been especially acute with pills formed compressing powders containing surfactants and constituted with an insoluble detergency adjuvant such as aluminosilicate of sodium (zeolite).

It is known to include highly soluble materials whose function is to improve the disintegration of pills when they are placed in the wash water. Some pills that are commercially distributed incorporate urea for these purposes. The urea has a very high solubility in water that exceeds 100 g per 100 ml of water at 20 ° C. The document EP-A-711827 (Unilever) exposes the use of sodium citrate for these purposes and the document EP-A-838519 (Unilever) exposes the Use of sodium acetate trihydrate for these purposes.

Some of these highly soluble materials, for example sodium acetate, they are hygroscopic and need a careful handling of the material during production and Storage of laundry pads. Therefore it is desirable to use a disintegrating laundry material other than hygroscopic and does not require the same careful handling during production or storage of the tablet.

Generally, the above soluble compounds They are produced by synthetic reactions. The alternatives to these soluble compounds are always sought from sources "renewable" in order to increase the content "natural" detergent tablets. One more product "natural" is increasingly desired by consumers.

A certain number of documents have stated that the Disintegration of tablets of a cleaning composition can be accelerated by incorporating an amount of an insoluble material in water but inflatable in water that serves to favor the disintegration when the tablet is placed in water at the time of be used Two of these documents are WO 98/40462 (Rettenmaier and Henkel) and WO 98/40463 (Henkel). EP 1043391 (Stockhausen GmbH) describes detergent tablets comprising water and cellulose swellable disintegrating granules microcrystalline US 4642197 describes that the tablets of washing additives may comprise disintegrating agents.

EP 0846756 (Procter & Gamble Company) describes a detergent tablet comprising CMC disintegrant and perfume capsules for which the material Encapsulant is starch.

Therefore, it is an objective of the present invention address one or more of the problems above mentioned. In particular, the present invention seeks provide an alternative to the known pills, which have a disintegration efficiency and resistance of the tablet satisfactory and / or, in which a substantial proportion of the system of disintegration in the tablet is derived from sources "renewable."

It has been found that the foregoing may be achieved using an additive disintegration system that comprises water swellable and starch disintegration granules hydrophilic

This result is surprising because, between other things, the hydrophilic starches used according to the invention they have an extremely low solubility in water and are preferably insoluble in water. Therefore, it would not be expected that the level of water entry in the tablet caused by these Materials were enough to help a good disintegration. Instead, it would be expected that water ingress would be much slower than that achieved with solubility materials very high in water, which are conventionally used as additives of disintegration and therefore a disintegration would not be achieved comparable.

The invention also allows or in a manner alternative that includes a lower level of chemicals Synthetic detergent tablets while they remain satisfactory disintegration properties of the tablets and performance. In addition, the disintegration system according to invention does not present any significant difficulty when it is Factory driven In some cases the total level of additives of disintegration in the tablets can be reduced by means of the present invention

In documents DE 2263940 and DE 2362595 (both Henkel GmbH) describes pads comprising a optical brightener and approximately 60 to 95% by weight of starch Potato Very high levels of starch are used in these pills and there is no explanation of advantages when used these materials with water-doable materials.

It has now been found that two different measures Strength of the tablets are relevant to the properties observed by a consumer. The force to cause the fracture it is a direct assessment of the resistance and indicates the resistance from pills to breakage when handled by the consumer at the time of being used. The amount of energy (or work mechanical) provided before the fracture is a measure of the deformability of the tablet and is relevant to the resistance of the pills to break during transport.

Both properties are relevant to the consumer perception of pills: consumers want pads that are strong enough to be handled, to reach them intact and that quickly and completely disintegrate in The time of use. The present invention makes it possible to achieve a good combination of disintegration and resistance properties while making use, at least in part, of renewable materials.

All amounts are by weight unless Specify something else.

Therefore, according to a first aspect of the invention a tablet of a detergent composition is provided in the form of compacted particles comprising a non-surfactant soapy and a detergency adjuvant, in which the pill or a discrete area of it contains 1 to 20% by weight, based on the total weight of the tablet, of a disintegration system that understands:

a) water swellable disintegrating granules with an average particle size between 500-1000 micrometers, and

b) a hydrophilic starch having an average size of particles of 250 micrometers or less, a water solubility less than 1 g / 100 g of water at 20 ° C and a force development of 2.0 Newtons expansion / second or less.

The tablets according to the invention have the advantage of exhibiting good disintegration properties and resistance and comprise an acceptable level of a system of disintegration without relying on high levels of synthetic ingredients in order to achieve this. In addition, the disintegrating system is convenient to be handled during the Pill production.

According to a second aspect of the invention, provides a disintegrating system for a tablet of one detergent composition in the form of compacted particles, which it comprises a non-soap surfactant and an adjuvant of the detergency, in which the disintegrating system comprises:

a) water swellable disintegrating granules with an average particle size between 500-1000 micrometers, and

b) hydrophilic starch having an average size of particles of 250 micrometers or less, a water solubility of less than 1 g / 100 g of water at 20 ° C and a force development of 2.0 Newtons expansion / second or less.

According to a third aspect of the invention, provides a procedure to prepare a composition detergent in the form of compacted particles, comprising a non-soapy surfactant and a detergency adjuvant, procedure comprising:

1) mix 1 to 20% by weight based on weight Total tablet of a disintegrating system comprising:

to)

inflatable disintegrating granules in water with an average particle size between 500-1000 micrometers, and

b)

hydrophilic starch having a size particle medium of 250 micrometers or less, a solubility in water of less than 1 g / 100 g of water at 20 ° C and a development of expansion forces of 2.0 Newtons / second or less, with

2) other constituents of a composition detergent including a non-soap surfactant and an adjuvant of the detergency, place an amount of the composition in shape of particles resulting in a mold and compacting that composition into mold.

The forms of the present invention, including the preferred and optional features, and the materials that they can be used, they will be discussed in more detail below.

A tablet of the present invention may be homogeneous or heterogeneous. In the present specification, the term "homogeneous" is used to indicate a tablet produced by compacting a single composition in the form of particles, but does not imply that all the particles of that Composition will be of the same composition. The term "heterogeneous" is used to indicate a pill consisting of a plurality of discrete areas, for example, layers, inserts or coatings, each derived by compaction from a  composition in the form of particles. In a heterogeneous pill according to the present invention, each discrete area of the tablet preferably have a mass of at least 5 g.

Unless stated otherwise, all percentages in the present specification are percentages in weight over the total weight of the tablet, or area thereof.

Pill Disintegration System

A tablet according to the invention comprises a non-soap surfactant and a detergency adjuvant and the tablet or discrete area thereof contains 1 to 20% by weight, based on the total weight of the tablet, of a system of tablet disintegration as described herein descriptive

The tablet disintegration system comprises a first component (a) which is an inflatable disintegrating granule in water and a second component (b) which is a hydrophilic starch, and said starch acts as a path for the entry of water into The pill.

The tablet, or discrete area of it, it contains 1 to 20% by weight in total of said disintegration system on the total weight of the tablet or area thereof. Preferably the tablet, or discrete area thereof, comprises 5 or 8% by weight to 16% by weight of the disintegration system. They have obtained good results using a total amount of the system disintegrant that is in the range of 8 to 15% by weight, even better in the range of more than 8.5 to 13% by weight, by example, 8.5 to 12.5% by weight based on the total weight of the tablet or zone of it.

(a) Water-swellable disintegrating granule

A certain number of water insoluble materials and water inflatables are known to be useful as disintegrants of pills, in particular for pharmaceutical pills. A Exhibition of these materials can be found in the publication "Drug Development and Industrial Pharmacy", Volume 6, pages 511-536 (1980). Material suppliers Water-swellable disintegrants include J. Rettenmaier & Söhne in Germany and FMC Corporation in the US

The total amount of disintegrating granules Water inflatables in the tablet is preferably between 0.5 and 13% by weight based on the total weight of the tablet, plus preferably between 1 and 11% by weight, such as between 2 and 9% by weight, depending on the type of granule used. For example, the granules water swellable disintegrants containing a material polymer disintegrant has been found to provide good results when they are included in the tablets at levels of 2 to 7% by weight, especially 3 to 6% by weight. However, for a non-polymeric disintegrating material, the amounts are normally higher, for example, 5 to 13% by weight, preferably 6 to 11% by weight  weight.

The disintegrating granule according to the invention is swells by contact with water. It is very preferred that the granule be prepared from a material that is itself a water swellable material before being granulated to produce the water swellable disintegrating granule. However, the granule can be made from a material that shows itself negligible characteristics and swelling unless it is granulated, possibly up to a specific particle size. For example, microcrystalline cellulose, when granulated until a suitable average particle size, for example, 700 to 1000 micrometers, can be used with the condition that the granule in itself is inflatable in water.

The disintegrating system of the invention comprises water swellable disintegrating granules with an average size of particles between 500-1000 micrometers. Preferably, the water swellable disintegrating granules have an average particle size in the range of 550 to 950 micrometers, more preferably 600 to 900 micrometers, such as 650 to 850 micrometers

The particle size referenced in the present specification it is half sieving the granules and picking up the sieves. The weight of the screened fractions is graphically versus the particle size of the fractions and then the average weight size is calculated following the method defined by Rosin and Rammler, J. Inst. Fuel, 7, 29-36 (1933) to provide the average size weight. All particle sizes referenced in the present specification are particle sizes determined by this method unless another one is established thing.

Water-swellable disintegrating granules preferably have a water solubility of less than 2 g / 100 g of water at 20 ° C, more preferably less than 1 g / 100 g, most preferably less than 0.5 g / 100 g. They are especially preferred water-swollen and insoluble disintegrating granules in Water.

Water-swellable disintegrating granules They comprise one or more disintegrating materials. The granules can consist essentially of one or more disintegrating materials that they are inflatable in water by themselves or they are inflatable in water When they are granulated. Alternatively, the granules can comprising one or more of said materials mixed with others materials as carriers.

Disintegrating granules may comprise a polymer material as the disintegrating material. Many of these polymeric materials are of natural origin even if they have subsequently experienced a chemical treatment. Is especially preferred that the swellable disintegrating granules in Water comprise cellulose.

Suitable disintegrating granules include the prepared from starches, for example, corn starches, rice and potato and starch derivatives, such as Primojel®, or Expoltab®, which are the two sodium starch glycolate too known as sodium carboxymethyl starch; celluloses, for example, Arbocel®-B and Arbocel®-BC (cellulose beet), Arbocel®-BE (sulfite-starch beet), Arbocel®-B-SCH (cotton cellulose), Arbocel®-FIC (pine cellulose) as well as additional types of Arbocel® from Rettenmaier and cellulose derivatives, for example, Courlose® and Nymcel®, sodium carboxymethyl cellulose,  crosslinked modified cellulose Ac-di-Sol®, cellulosic fibers microcrystalline and crosslinked cellulose; and various polymers Synthetic organic These materials are referred to herein. Descriptive report disintegrating materials regardless of if they have disintegration properties by themselves, or if they act as a disintegrant only when they are granulated to form the water swellable disintegrating granule.

Fibrous materials containing cellulose that originate from wood can be wood pulps compacted The so-called mechanical pulps incorporate usually lignin as well as cellulose, while the pulps chemicals generally contain cellulose but little remains of the original lignin The pulp obtained by a mixture of methods chemical and mechanical can retain something but not all of the original lignin Cellulose based materials include Nilyn LX-16 which is a cellulose based disintegrant water insoluble compacted, commercially available in the FMC company.

A strongly inflatable disintegrating material may come from a category referred to in the art "super-disintegrating". These "super-disintegrants" tend to be polymer synthetic or natural crosslinked and include crosslinked forms of carboxymethyl cellulose, cellulose, starch, polyvinylpyrrolidone and polyacrylate The crosslinked forms of carboxymethyl cellulose are especially preferred.

Any of these materials that are starch it may be present in the disintegrating granule a) or as the same in addition to being present in component b) or as the same in the disintegrating system, provided they are included in different ways that meet the criteria for both components a) and b).

The disintegrating granules may consist of a water-absorbent carrier material that can swell from the initial contact with water, mixed with a smaller proportion of disintegrating material Disintegrating material may swell more strongly that the carrier material by contact with water. May absorb more water than the carrier material, or swell more Quickly or both. The proportions in the granule disintegrant are preferably 75 to 90, 95 or 99.9% by weight of the carrier material, from 0.1 to 10% of the disintegrating material and from 0% to 24.5% by weight of other material based on the total weight of the disintegrating particles

It is especially preferred if the proportions they are from 75% by weight to 99.9% by weight of the carrier material, from 0.1% to 10%, of the disintegrating material and from 0% to 24.5% by weight of another material based on the total weight of the particles disintegrating

The carrier materials are selected preferably among the compounds containing hydroxy groups. A carrier material can itself be an insoluble material in water, and something inflatable in water. These materials include starches, for example, corn, rice and potato starches, celluloses, microcrystalline cellulosic fibers and some polymers Synthetic organic

Disintegrating granules may also contain up to 15% or 20% by weight of a water soluble polymer that acts as a binder, for example, polyethylene glycol.

An apparatus to measure an increase in volume (swelling) is illustrated in the publication "The Mechanisms of Disintegrant Action ", Kanic & Rudnic, Pharmaceutical Technology, April 1984, pages 50-63. This article also refers to documents that describe others types of devices to measure swelling.

Another parameter that can be used to characterize inflatable materials is the force they exert if they are allowed to absorb water while being confined in an enclosure closed.

It has now been found that the materials and particles that swell by contact with water are effective as disintegrating if there is a rapid development of strength when they enter contact with water. Measurements have been carried out using a relatively simple piece of apparatus shown in the drawing that accompanies and a material testing machine Instron type 5566 of the company Instron, United Kingdom (hereinafter referred to as "the Instron machine ").

The apparatus consists of a cylinder (10) with a internal diameter of 25 mm and a length of 20 mm. This cylinder it is perforated by a ring of holes (12) adjacent to a extreme. There are 36 of these holes, 1 mm in diameter, with centers 2.5 mm from the end of the cylinder.

This end of the cylinder is attached to the base of a glass vessel (14) with an internal diameter of 73 mm

To test a sample of disintegrant powder, 1.5 grams of the disintegrant are placed in the cylinder and hit gently so that it forms a level bed (16) that has usually a depth of 6 mm to 10 mm depending on the bulk density of dust.

A piston (18) of the Instron machine moves in the upper cylinder assembly, on this bed of dust. Under computer control of the Instron machine, the plunger is applied to the top of the powder bed (16) with a force of 1 Newton.

50 ml of distilled water are dripped at 22 ° C in the annular space (20) around the cylinder. This water passes to through the holes (12) towards the bed of dust. Machine Instron is programmed to keep the cylinder in position against the inflatable bed of dust, and the force is recorded required for this.

It is especially preferred that the material disintegrant used in the disintegrating granule when tested by itself, have the ability to absorb at least twice its own volume of water and have a development of forces of expansion exceeding 1.5 Newton / second. Is especially preferred that the disintegrating material has a development of expansion forces of more than 2.2 Newtons / second, such as 2.5 Newtons / second or more.

Specifically, a super-disintegrant can absorb more than double and possibly more than 2.5 or 3 times its own volume of water, and / or develop expansion forces that exceed 1.5 Newton / second, while a vehicle for this absorbs less water by volume that the super-disintegrant and develops less strength of expansion

The development of expansion forces for a certain number of materials was measured, as set out in the following table. The data are taken from the publication of C. Caramella et al .; "The role of swelling in the disintegration process" Int. J. Pharm. Tech. & Prod. Mfr. 5 (2), 1-5, (1984).

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(Table goes to page next)

one

The significant parameter is the maximum slope of the force of expansion versus time.

The swelling measurement can be recorded With the same device. The plunger is again applied to the part top of a bed of dry powder, and is pressed against it with a force of 1 Newton. 50 ml of water is poured as previously. The Instron machine is programmed to allow expansion of the powder bed, while maintaining a force on the same as 1 Newton. The piston displacement is recorded.

Water-swellable disintegrating granules they can be prepared by mixing the disintegrating material with the carrier material, if any, compacting the mixture and, if it is necessary, shredding the compacted mixture in the form of granules

The mixing of these materials can be carried carried out by means of a standard apparatus for mixing solids in particle shape Other ingredients can be incorporated into this stage. If a polymer binder is incorporated, it can be added in particulate form during this mixing operation.  Alternatively, if this can be molten, the molten polymer it can be sprayed on the mixture or on an ingredient in particle form of the mixture.

The compaction of the mixture can lead to out by passing it between a pair of rollers. The device suitable, a roller compactor, has a spindle power supplying the mixture to the contact line of the rollers The speed of the feed spindle and therefore the amount of material supplied to the contact line of the rollers must be high enough to pass the uninterrupted flow of material through the rollers, but not so high that the material becomes a paste.

The sheet of material that comes out of the rollers is then decomposed and crushed to particle size necessary.

The manufacturers of both a compactor Rollers like crushing machinery include Hosokawa Bepex, located in Heilbronn, Germany, Alexanderwerk located in Remschied, Germany and Fitzpartick located in Elmhurst, USA

(b) Hydrophilic starch

The second component of the disintegration system It is a hydrophilic starch.

The starch has an average particle size of 250 micrometers or less, preferably 200 micrometers or less, more preferably 150 micrometers or less. The average sizes of particles in the range of 2 to 70 micrometers have been found They are especially suitable. The average particle sizes of the present specification are measured according to the method previously established.

Hydrophilic starch has a solubility in water of less than 1 g / 100 g of water at 20 ° C, preferably less than 0.5 g / 100 g, more preferably less than 0.2 g / 100 g. The Water insoluble starches are especially preferred.

The hydrophilic starch has an expansion force development, as defined above, of 2.0 Newtons / second or less, preferably 1.8 Newtons / second or less, more preferably 1.5 Newtons / se-
Gundo or less, like 1.3 Newtons / second or less. The development of the expansion forces of some hydrophilic starches suitable for use as component b) in the disintegration system are provided in the Table above in the description of the disintegration granule. The tablet preferably comprises 1 to 15% by weight of the hydrophilic starch based on the total weight of the tablet, more preferably 2 or 3 to 12% by weight, even more preferably 4 to 10% by weight. The amounts between 4 and 8% by weight have been found to be very effective, such as 4.5 to 7% by weight. Especially good results have been found using approximately 4% by weight of the disintegrating granule with approximately 6 to 8% by weight of starch and using approximately 5% by weight of the disintegrating granule with approximately 4-6% by weight of starch.

The hydrophilic starch is preferably a native starch By the term "native", as used in This specification indicates a starch that is of natural origin

If the hydrophilic material is a native starch, the Starch can be any native starch available in the Commerce. Native sources of starch include potato, tapioca, corn, rice, wheat, barley, tritical, millet, arrowroot, banana, sweet potato starches or starches with high content of amylose such as amilomaíz, chickpea starch, pea starch mung or amylopectin rice starches such as waxy corn, barley waxy, waxy wheat, waxy rice, amylopectin leg, tapioca de amylopectin, amylopectin sweet potato or starch Banana amylopectin. Amylopectin starches can derive  of plants that selectively produce amylopectin such as cereals waxy or amylose-free potato mutants and / or varieties of genetically modified plants like modified potatoes for selectively produce amylopectin. Preferably, the starch native is corn starch, tapioca, rice or potato, the most preferably corn or potato starch.

Hydrophilic starch can be used as the material by itself. Alternatively it can be combined, by example, jointly granulated with a carrier material. The Suitable carrier materials are described above for the water swellable disintegrating granule. If a carrier material, then the combination of the hydrophilic material and the carrier must still have an average particle size of 250 micrometers or less.

Although character links are not desired theoretically, it is believed that hydrophilic starches are suitable for be used in the disintegration system of the present invention because they combine rapid water absorption with an increase limited in the viscosity of the penetrating water.

A hydrophilic cellulosic material may be used. in addition to hydrophilic starch. The hydrophilic cellulosic material preferably has the same properties as described above for hydrophilic starch. Cellulosic materials Suitable hydrophilic include microcrystalline cellulose, alpha-cellulose, citric acid, cellulose intra-crosslinked and cellulose grafted with sulfur.

According to the invention, a mixture of different starches and mixtures of starches and celluloses. In In particular, mixtures of native starches with non-native and / or native or non-native cellulose starches. The non-native starches include starches chemically or physically modified even if they are of native origin, for example, starch pregelatinized

Surfactant compounds

The compositions that are compacted to form pills or their discrete areas of this invention contain one or more non-soap surfactants. In a composition for washing of fabrics, these preferably provide 5 to 50% by weight of the composition of the tablet or area thereof, more preferably 8 or 9% by weight of the composition at 35% or 40% in weight. If the tablet is composed of more than one discrete area, then these preferred amounts of surfactant can be apply to the tablet as a whole or to a discrete area of the same.

The organic surfactant may be present. as a component in granulated particles in an amount between 10 and 70% by weight of the particles, more preferably 15 to 50% in weight based on the total weight of the granulated particles. The all of the surfactant in the composition may be contained in these particles. The surfactant can be anionic (soapy or non-soapy), cationic, hybrid ion, amphoteric, non-ionic or A combination of these.

In a pill for washing fabrics, the anionic surfactant may be present in an amount of 0.5 to 50% by weight, preferably from 2% or 4% to 30% or 35% or 40% by weight of the pill or zone thereof.

In a dishwasher machine composition, the organic surfactant probably constitutes 0.5 to 8%, plus probably 0.5 to 5% of the composition of the tablet or area thereof and is likely to consist of a surfactant not ionic, either alone or in a mixture with a surfactant anionic

Synthetic anionic surfactants (i.e. not soapy) are well known to those skilled in the art. Examples thereof include alkyl benzene sulphonates, particularly sodium alkyl benzene sulphonates linear that have an alkyl chain length of C 8 -C 15; olefin sulphonates; alkane sulphonates; dialkyl sulphosuccinates and sulphonates of esters of fatty acids.

The primary alkyl sulfate has the formula:

ROSO_ {3} {} - \ M +

in which R is a chain of alkyl or alkenyl of 8 to 18 carbon atoms, especially 10 to 14 carbon atoms and M + is a solubilizing cation, it is commercially significant as a surfactant anionic

He linear alkyl benzene sulphonate formula:

2

where R is linear alkyl of 8 at 15 carbon atoms and M + is a solubilizing cation, especially sodium, it is also an anionic surfactant commercially significant.

Often this linear alkyl benzene sulphonate or primary alkyl sulfate of the above formula, or a mixture thereof, will be the desired anionic surfactant and can provide 75 to 100% by weight of any surfactant non-soapy anionic in the composition. In some ways of this invention, the amount of non-soap anionic surfactant is situated in a range of 5 to 20 or 25% by weight of the tablet or area of the same.

It may also be desirable to include one or more. fatty acid soaps. These are preferably soaps of sodium derived from naturally occurring fatty acids, for example, fatty acids from coconut oil, beef tallow, sunflower oil or hydrogenated rapeseed oil.

Suitable non-ionic surfactant compounds which can be used include in particular the products of reaction of compounds having a hydrophobic group and an atom of reactive hydrogen, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide.

Specific non-ionic surfactant compounds 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 alcohols primary and secondary of C_ {9-15} and C 12-15 ethoxylates with an average of 5 to 20 moles of ethylene oxide per mole of alcohol.

In certain forms of this invention the amount of non-ionic surfactant is in a range of 4 to 40%, better 4 or 5 to 30% by weight of the composition of the tablet or area Of the same. Many nonionic surfactants are liquids. These they can be absorbed into particles of the composition before the compaction in the form of pills.

Amphoteric surfactants that can be used in conjunction with anionic or non-ionic surfactants or both include amphipropionates of formula

\uelm{C}{\uelm{\dpara}{O}}

--- NH --- CH_{2}CH_{2} ---

\uelm{N}{\uelm{\para}{CH _{2} CH _{2} OH}}

--- CH_{2}CH_{2}CO_{2}NaR

 \ uelm {C} {\ uelm {\ dpara} {O}} 

--- NH --- CH2 {CH2} ---

 \ uelm {N} {\ uelm {\ para} {CH2CH2OH}} 

--- CH 2 CH 2 CO 2 Na

in which RCO is an acyl group of 8 to 18 carbon atoms, especially coco acyl.

The category of amphoteric surfactants also includes amine oxides and hybrid ion surfactants, particularly betaines of general formula

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3

in which R_ {4} is a string aliphatic hydrocarbon containing 7 to 17 carbon atoms, R 2 and R 3 are independently hydrogen, alkyl of 1 to 4 carbon atoms or hydroxyalkyl of 1 to 4 carbon atoms as  CH 2 OH, Y is CH 2 or of the form CONHCH 2 CH 2 CH 2 (amidopropyl betaine); Z is COO <-> (carboxybetaine) or in the form CHOHCH2SO3 (sulfobetaine or hydroxy-sultaine).

Another example of amphoteric surfactant is the oxide of formula amine:

\uelm{C}{\uelm{\dpara}{O}}

---

\delm{N}{\delm{\para}{R _{4} }}

--- (CH_{2})_{n} ---

\melm{\delm{\para}{R _{3} }}{N}{\uelm{\para}{R _{2} }}

\rightarrowOR_ {1} ---

 \ uelm {C} {\ uelm {\ dpara} {O}} 

---

 \ delm {N} {\ delm {\ para} {R 4}} 

--- (CH2) n ---

 \ melm {\ delm {\ para} {R 3}} {N} {\ uelm {\ para} {R 2}} 

\ rightarrowO

in which R1 is alkyl or C 10 to C 20 alkenyl; R 2, R 3 and R 4 are each hydrogen or C 1 to C 4 alkyl, while n is from 1 to 5.

Possible surfactants can be used cationic These often have a nitrogen atom quaternized in a polar head group and a hydrocarbon group attached of sufficient length to be hydrophobic. A formula general for a category of cationic surfactants is

\melm{\delm{\para}{R}}{N}{\uelm{\para}{R}}

^{+} --- R X^{-}R_ {h} ---

 \ melm {\ delm {\ para} {R}} {N} {\ uelm {\ para} {R}} 

<+> --- R X <->

in which R indicates independently an alkyl group or a hydroxyalkyl group of 1 at 3 carbon atoms and R h indicates an aromatic, aliphatic group or aromatic and aliphatic mixture of 6 to 24 carbon atoms, preferably an alkyl or alkenyl group of 8 to 22 atoms of carbon and X <-> is a counterion

The amount of amphoteric surfactant, if any, it can possibly be 3% to 20 or 30% by weight of the tablet or area of a pill; the amount of cationic surfactant, if there is, it can possibly be 1% to 10 or 20% by weight of the tablet or area of a pill.

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Detergency adjuvant

A tablet according to the present invention comprises a detergency adjuvant that serves to separate or sequester calcium and / or magnesium ions in the water. Therefore the detergency adjuvant acts as a water softener. In detergent tablets, the amount of adjuvant of the detergency is probably 5 to 80%, more usually 10 or 15% at 60% by weight of the tablet.

The detergency adjuvant may be present in granulated particles in an amount of 20 to 80% in weight, more preferably 30 to 60% by weight of the particles granulated

The detergency builders can be fully provided by water soluble materials, or they can be provided largely or even completely by a water insoluble material with softening properties of the Water.

Alkali metal aluminosilicates are highly suitable as acceptable detergency adjuvants for the environment for fabric washing, and are preferred in this invention. Alkali metal aluminosilicates (preferably sodium) can be crystalline or amorphous or mixtures of them, which have the general formula:

0.8 \ - \ 1.5 \ Na_ {2} O.Al_ {2} O_ {3}. \ 0.8 \ - 6 \ SiO_ {2} .xH_ {O}

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

The ion exchange materials of suitable crystalline sodium aluminosilicates are described, by example, in GB 1429143 (Procter & Gamble). The Preferred sodium aluminosilicates of this type are zeolites A and X commercially available and well known, the zeolite P plus Recent described and claimed in EP 384070 (Unilever) and its mixtures. This form of zeolite P is called also "zeolite MAP". A commercial form of it is indicated as "zeolite A24".

Supposedly, a detergency adjuvant it could be a layered sodium silicate as described in the US 4,664,839. NaSKS-6 is the brand Registered for a crystalline layered silicate marketed by the Hoechst company (commonly abbreviated "SKS-6"). The NaSKS-6 has the delta-Na2 SiO5 morphology of the silicate in layers. It can be prepared by methods such as those described in DE-A-3417649 and DE-A-3742043. Can be used other of these layered silicates, such as those with the formula general NaMSi_ {O} {2x + 1}. 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 0.

The least preferred category of softeners inorganic containing water soluble phosphorus includes the orthophosphates, metaphosphates, pyrophosphates and metal polyphosphates alkaline Specific examples of detergency builders inorganic phosphates include tripolyphosphates, orthophosphates and sodium and potassium hexametaphosphates.

Water soluble detergency builders Non-phosphorus can be organic or inorganic. The Inorganic that may be present include metal carbonate alkaline (usually sodium); while the organic ones include polycarboxylate polymers, such as polyacrylates, copolymers acrylic / maleic and phosphonates acrylic, polycarboxylates monomers such as citraros, 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 have some function as water softening agents and also inhibit the unwanted deposit on the cloth from the washing liquid.

When the tablet contains an adjuvant of the water soluble detergency, is preferably present in a amount of 10 to 80% by weight based on the total weight of the tablet or zone of it. When the tablet contains an adjuvant of the water insoluble detergency, is preferably present in a amount of 5 to 80% by weight based on the total weight of the tablet or area of it.

The pins comprising 4 to 50% by weight of surfactant and 5 to 80% by weight of detergency adjuvant They are especially preferred for fabric wash tablets. The tablets comprising 1 to 5% by weight of surfactant and 50 at 98% by weight of detergency adjuvant are especially Preferred for tablets for dishwashing machines.

To avoid any doubt, when a pill is heterogeneous, the percentage intervals for the components cited herein may be applied to the complete composition of the tablet, as well as at least one area of the pill.

Optional particles that favor disintegration and water soluble

A pill or an area of a pill can additionally contain water soluble particles to favor additionally the disintegration in addition to the disintegration system claimed. It is preferred that these particles favoring the disintegration constitute 2%, 3%, 5%, 8% or 10% up to 15% by weight of the composition of the tablet or area thereof.

These water soluble particles contain normally at least 40% by weight (of your own weight) of one or more materials that are different from soap or an organic surfactant and which have a solubility in deionized water of at least 30 g / 100 g at 20 ° C.

More preferably, this soluble material in water is selected from compounds that contain at least 40% (per particle weight) of one or more materials selected from the group consisting of compounds with a water solubility that exceeds 50 grams / 100 grams in water at 20 ° C; or tripolyphosphate of sodium containing at least 50% of its own weight of the form anhydrous phase I, or sodium tripolyphosphate that is partially hydrated so that it contains hydration water in an amount which is at least 0.5% by weight of sodium tripolyphosphate in the particles, preferably that is partially hydrated with the so that it contains hydration water in an amount that is at minus 1% by weight of the sodium tripolyphosphate in the particles.

As will be explained in detail later, these particles that favor disintegration may contain also other forms of tripolyphosphate or other salts in the rest of His composition.

If the material in these flattering particles Water-soluble disintegration can function as a detergency adjuvant (as is the case with tripolyphosphate of sodium) then naturally contributes to the total amount of adjuvant detergency in the composition of the tablet.

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

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

Material Solubility in water (g / 100 g) Citrate dihydrate sodium 72 Carbonate potassium 112 Urea > 100 Acetate of sodium 119 Acetate trihydrate sodium 76 Magnesium Sulfate 7 H2O 71

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 water soluble material is incorporated in the form of particles of the material in a substantially pure form (ie, each of these particles contains above 95% by weight of the material). However, said particles may contain material of this solubility mixed with another material, provided that the material of the specified solubility provides at least 50% by weight of these
particles

Preferred water soluble materials that they have a solubility that exceeds 50 g / 100 g of water deionized at 20 ° C are sodium citrate dihydrate, urea, acetate of sodium and sodium acetate trihydrate. Sodium acetate It can be in a partially or completely hydrated form.

It may be preferred that the material be highly Water soluble is a salt that dissolves in water in a form ionized As a salt dissolves, it leads to an increase transient local ionic resistance that can help the tablet disintegration preventing non-ionic surfactant swell and inhibit the dissolution of other materials.

Specifically, the pills of this invention they can contain a water soluble salt, with a solubility that exceed 50 g / 100 g of deionized water at 20 ° C, both in shape of a small percentage in said granulated particles as in form of separate particles that are mixed therewith.

In granulated particles that may contain surfactant and / or detergency adjuvant, this highly water soluble salt may be present in an amount of 1 to 25 or 30% by weight of those particles, preferably 3 or 5 to 10 or 15 % thereof, while an amount of 1, 2 or 5% up to 15% by weight of the formulation of the complete salt tablet can be added to these particles before the formation of the tablets
soluble.

Another possibility, which is less preferred, is that said particles that favor disintegration are particles that contain sodium tripolyphosphate with more than 50% (by weight of particles) of the anhydrous phase I form and which is partially hydrated in order to contain hydration water in a amount that is at least 1% by weight of the tripolyphosphate of sodium.

Sodium tripolyphosphate is very well known as an adjuvant of sequestering detergency in compositions detergents It exists in a hydrated form and two anhydrous forms crystalline These are the normal crystalline anhydrous form, known as phase II, which is the low temperature form, and phase I that It is stable at elevated temperature. The conversion of phase II into phase I proceeds quite quickly by heating above the transition temperature, which is about 420 ° C, but the Reverse reaction is slow. Consequently, tripolyphosphate from Phase I sodium is metastable at room temperature.

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. These particles they must also contain sodium tripolyphosphate which is partially hydrated The extent of hydration should be at minus 1% by weight of the sodium tripolyphosphate in the particles. Be It should be in a range of 1 to 4%, or it may be higher. From in fact, sodium tripolyphosphate can be used completely hydrated to provide particles.

The rest of the composition of the tablet used to form the pill or zone thereof can include additional sodium tripolyphosphate. This can be in any form, including sodium tripolyphosphate with a high content of the anhydrous phase II form. The right material is available on trade. The suppliers include Rhone-Poulenc, France and Albright & Wilson, United Kingdom.

Some countries require that phosphate not be used. For these countries, a zero phosphate tablet according to this invention can use a suitable amount, for example, 15% in weight or more of disintegration-promoting material with a solubility of at least 50 g / 100 g at 20 ° C. Other countries allow use, or at least some limited use of phosphates, making possible use some sodium tripolyphosphate.

The particles that favor disintegration Water soluble are preferably stable up to at least 20% of relative humidity, preferably at least 30% and more preferably at least 60% relative humidity, in which the stability is measured at 25 ° C in the manner described below and as described in WO 01/51600 (Procter and Gamble Company).

The stability of the particles favoring the disintegration can be determined using dynamic vapor absorption isotherms. This test measures moisture absorption in equilibrium at constant temperature as a function of relative humidity (RH). The RH is increased in increasing stages and at each level the sample is given time to equilibrate and subsequently the sample is weighed to determine the mass increase due to water absorption. Experiments can be performed using a DVS-1 instrument, supplied by Surface Measurement Systems Ltd. The instrument comprises mass flow meters to regulate wet / dry air ratios and a Cahn D-200 microbalance. The instrument is housed in an incubator to ensure that all parts of the system are at the same temperature. The test is performed using 15 mg samples with an RH that varies in the range of 0 to 80% at 25 ° C. Disintegration-favoring particles are considered to be stable up to a relative humidity x if the increase in the percentage by weight of the solution additive is less than 5%, preferably less than 1% for absorption above the relative humidity range of 0
ax%

Optional water soluble organic polymer

The tablets of the present invention can include a water soluble organic polymer that is solid at 25 ° C to act as a binder for the composition in the form of particles when compacted. This can be included in granulated particles containing organic surfactant and / or adjuvant detergency.

The term "solid" is used herein. descriptive report to indicate materials that have the appearance of a stationary solid at 25 ° C and can be handled as solid. They are in contrast to liquids that, even if they are viscous, it can be seen that they are capable of a fluid flow. The Organic polymers are generally amorphous materials that are strictly classified as liquids super-cooled, but of such a high viscosity They are solid for practical purposes.

The term "water soluble" is used in the present specification to indicate that when the polymer is placed in water it seems, by visual inspection, that it dissolves. Do not it is important for this invention if the solution is a true Isotropic solution or has some colloidal character.

It is preferred that the polymer material is melted to a temperature of at least 35 ° C, better 40 ° C or more, which is about above ambient temperatures in many temperate countries. For use in warmer countries, it will be preferable that the melting temperature is somewhat above 40 ° C, so that it is above room temperature.

Some polymers that can be used are solids at temperatures up to 100 ° C, that is, retain a solid appearance even if they are in an amorphous state. Be can soften and melt even a mobile liquid when heated additionally, or they can decompose without melting on heating sufficiently above 100 ° C. These polymers generally they are added in the form of a powder during the course of the granulation. Another possibility would be the addition in the form of a solution in a volatile organic solvent, but this is not favorite.

Other molten polymers can be used up to a liquid form at temperatures not exceeding 80 ° C and they can be sprayed in the form of a molten liquid on the mixture of surfactant and detergency adjuvant during granulation course.

Organic polymers are generally solid amorphous A significant parameter that characterizes solids Amorphous is its glass transition temperature. When a polymer amorphous hydrophilic absorbs moisture, moisture acts as a plasticizer and lowers the glass transition temperature of the polymer. Suitable polymers can have a temperature of glass transition, when they are anhydrous, which is 300 to 500ºK (it is say, approximately 25 ° C to 225 ° C) but can be incorporated in a state that contains moisture so that the temperature of glass transition is lower.

A preferred polymer is polyethylene glycol. The Preferred polymeric materials are synthetic organic polymers, especially polyethylene glycol. Weight polyethylene glycol Medium molecular 1500 (PEG 1500) melts at 45 ° C and has been shown to suitable. The higher molecular weight polyethylene glycol can be also used (PEG 4000 melts at 56 ° C and PEG 6000 at 58 ° C). Other  possibilities are polyvinylpyrrolidone and copolymers of water soluble polyacrylates and acrylates.

The amount of water soluble polymer included in particles that may also contain organic surfactant and detergency adjuvant is preferably between 0.2% and 0.5% or 1% and 15% by weight of the particles, possibly at least 1.5 or 3%. It is additionally preferred that the amount is not above 7 or 10% by weight. Alternatively, the amount of polymer Water soluble present can be defined in terms of the complete composition of the tablet or area thereof, in which case is desirably present in an amount between 0.5% and 10% by weight, more preferably at least 1, 2 or 5% by weight. Possibly the amount of polymer does not exceed 7% by weight of the full composition

Optional bleaching system

The compositions in the form of tablets according to invention may contain a bleaching system. This includes preferably one or more peroxy 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. If present a peroxygen compound, the amount is probably at a range of 10 to 25% by weight of the tablet composition or area of it.

Preferred inorganic persalts are sodium perborate monohydrate and sodium percarbonate tetrahydrate, advantageously used in conjunction with an activator. Bleaching activators, also called bleaching percussors have been widely described in the prior art. Preferred examples include peracetic acid precursors, for example, tetracetylethylenediamine (TAED), currently for commercial use extended in conjunction with sodium perborate; and perbenzoic acid precursors. The quaternary and phosphonium ammonium activators described in US 4,751,015 and US 4,818,426 (Lever Brothers Company) are also of
interest.

Another type of bleach activator that can be used, but not a bleaching precursor, it is a catalyst of transition metals 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 phosphonate of ethylenediamine tetramethylene and phosphonate diethylenetriamine-pentamethylene.

Other optional ingredients

The tablets of the invention may contain also one of the well-known detergency enzymes in the technique for its ability to degrade and help suppress various dirt and stains. Suitable enzymes include the various proteases, cellulases, lipases, amylases and mixtures thereof, which are designed to suppress a diversity of dirt and fabric stains. Examples of suitable proteases are Maxatase (registered trademark) supplied by the company Gist-Brocades N.V. Delf, Holland and Alcalase (brand registered) and Savinase (registered trademark) supplied by the Novo Industri A / S company, Copenhagen, Denmark. Enzymes of detergency are commonly employed in the form of granules or agglomerates, optionally with a protective coating, in a amount from about 0.1% to about 3.0% by weight of the composition of the tablet or area thereof, and these granules or agglomerates do not present problems with respect to compaction to form a pill

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

Advantageously a material is included antifoam if an organic surfactant is present, especially if a detergent tablet is intended mainly to be used in automatic washing machines of Front loading drum type. Antifoam materials suitable is usually in granular form, as described in EP 266863A (Unilever). These granules of antifoam usually comprise a mixture of oil silicone, petrolatum, hydrophobic silica and alkyl phosphate as an antifoam active material, absorbed in an inorganic carrier material based on a carbonate Water soluble porous absorption. Antifoam granules they can be present in an amount up to 5% by weight of the composition of the tablet or zone thereof.

It may also be desirable that a tablet of the invention includes an amount of an alkali metal silicate, particularly ortho-, meta- or di-silicate. The presence of these alkali metal silicates at levels, by example, from 0.1 to 10% by weight, can be advantageous for provide protection against corrosion of the parts Metallic washing machines, apart from providing some degree of structuring to the composition and provide advantages of treatment in the manufacture of the particulate material which is compacted in the form of pills. A composition for the fabric washing will generally not contain more than 15% by weight of silicate. A tablet for a dishwasher will contain often at least 20% by weight silicate.

Bulk density and granulation of detergent powder

Although the composition in the form of particles of heading from which the pills are produced may have in principle any apparent density, the present invention may be especially relevant for tablets of the composition detergent prepared by compacting powders of apparent density relatively high, due to its greater tendency to exhibit Disintegration and dispersion problems. These pills have the advantage, compared to a tablet derived from a powder of low apparent density, that a given dose of composition can be presented in the form of a smaller pill.

Therefore, the particulate composition Starting can properly have an apparent density of at minus 400 g / liter, preferably at least 500 g / liter and possibly at least 600 g / liter.

The granular detergent compositions of high apparent density prepared by granulation and densification in a high speed mixer / granulator, such as It is described and claimed in the documents EP-A-340013 (Unilever), EP-A-352135 (Unilever) and EP-A-425277 (Unilever), or by the continuous granulation / densification procedures described and claimed in the documents EP-A-367339 (Unilever) and EP-A-390251 (Unilever) are inherently suitable for use herein invention.

Another procedure particularly suitable for the preparation of a detergent powder of apparent density elevated is described in the document WO-A-98/11193 (Unilever). In this document, a feed stream of the starting acid for Anionic surfactant production is partially neutralized, for example, by means of sodium hydroxide, before be fed to a mixer-densifier to high speed (for example, Lodige CB 30 Recycler) in which the partially neutralized acid feed current is completely neutralized, while mixed with most the other components of the detergent base powder granule. This powder can be further densified by a treatment in a mixer at moderate speed (for example, Lodige KM 300 mixer) before whose stage can be added more adjuvant detergency. The water soluble polymer material It is preferably added before the densification stage additional, although it can be added in the first mixer. He Water soluble polymer material can be heated to urn temperature considerably above its melting point for Get a free flowing liquid. The resulting powder can be cooled and dried using a fluidized bed, after which any particle size control can be exercised wanted.

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Any of the separate particles that contain additional components of the finished formulation may be mixed with the base powder before compaction.

Particle size control

Particle sizes can be controlled in the manufacturing process of any of the particles included in the composition. Oversized particles they are usually separated by sieving (for example, by a Mogensen sieve) at the end of the production procedure, followed by crushing and recycling of the oversized fraction separated. Under-sized particles can be separated also by sieving or, if the manufacturing process employs a fluidized bed, the under-sized particles can be trapped in the air stream and subsequently recover from the same for recycling to the granulation stage.

It is preferred that the average particle size of the granulated particles that form the composition in the form of particles from which the tablet is formed be between 400 and 1,100 micrometers, preferably between 500 and 1,000 micrometers. Preferably no more than 5% of these particles are more smaller than 200 micrometers while no more than 5% are greater than 1,400 micrometers.

The materials that are mixed with the granulated particles can also meet these requirements referred to particle size.

Tablet formation

The formation of the pills includes the compaction of the composition in the form of particles. Is known a diversity of machinery for the formation of pills that They can be used. Generally, it will work by stamping a quantity of the particulate composition that is confined in a matrix. The formation of pills can be carried out at room temperature or above room temperature that can allow adequate resistance to be achieved with less pressure applied during compaction. With the purpose of carry out the formation of tablets at a temperature that is Above the environment, the particulate composition is preferably supplied to the training machinery of pills at an elevated temperature. Naturally this will supply heat to the tablet forming machinery, but The machinery can also be heated in some other way.

If some heat is supplied, it is expected that it will be supplied by conventional means, as if passing the composition in the form of particles through a stove, instead of by any microwave energy application.

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 fabrics or dishwashers or a fractional part of this dose. The Pills can be any way. However, for greater ease of packaging, are preferably section blocks substantially uniform transverse, such as cylinders or cuboid.

The overall density of a tablet for washing of fabrics is preferably in a range of 1,040 or 1,050 g / liter up to 1,400 g / liter, preferably at least 1,100 g / liter up to 1,400 g / liter. The density of the tablet can be placed in an interval up to no more than 1,350 or even 1,250 g / liter. The overall density of a tablet of some other composition of cleaning, such as a tablet for a dishwasher or as a bleaching additive, can vary up to 1,700 g / liter and is often It will range from 1,300 to 1,550 g / liter.

The invention also provides a method. for preparing a tablet according to the invention comprising mixing the disintegrating system with other constituents of a composition detergent including an organic surfactant and an adjuvant of the detergency, place an amount of the composition in the form of resulting particles in a mold and compact that composition into the mold.

Pill trials - disintegration

The speed of disintegration of the tablets is measured by an assay procedure under conditions static in which a previously weighed pill was placed in a metal grid with 1 x 1 cm units and the tablet and the grid were then submerged in an adequate amount of tap water of 15º FH (French hardness) at 10ºC or 20ºC that the pill when submerged was covered by 2 cm of Water. After 60 seconds, the metal grid is removed carefully from the water and the wet tablet residue is weighed. Yes the pill completely disintegrated in this period of time, then the time necessary for a breakdown of 100%

It is preferred that the tablets exhibit 70% in disintegration weight or more in the previous trial, more preferably 75% or more, most preferably 80% or more.

Pill Resistance

The resistance of the pills, in their condition dry as prepared in the compaction press, it can be determined according to its DFS diametral fracture tension, which is Calculate from the equation:

DFS = \ frac {2F_ {max}} {\ pi Dt}

in which DFS is the tension of Diametral fracture in Pascals, F_ {max} is the load applied in Newtons to cause fracture, D is the diameter of the tablet in meters and t is the thickness of the tablet in meters. The essay is carried out using a universal type test instrument Instron to apply a compression force over a diameter of the tablet (i.e. perpendicular to the axis of a tablet cylindrical).

It is preferred that the tablets have a DFS of at least 20 kPa, more preferably at least 25 kPa, such as 30 kPa or plus.

Examples

The invention will be further described. by reference to the following examples. Other examples within the scope of the present invention they will be apparent to the skilled in the art.

Preparation of a granulated base powder

A granular detergent powder of base that had the composition of table 1 granulating the eights first ingredients together in the correct proportions under high shear followed by low densification reduced shear to produce a granular component. The Subsequently dosed ingredients were added to the granular composition to produce the complete composition of the Table 1.

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TABLE 1 Base Powder Formulation

4

       \ dotable {\ tabskip \ tabcolsep # \ hfil \ tabskip0ptplus1fil \ dddarstrut \ cr} {
 * 1 Zeolita A24 is the company's maximum aluminum zeolite P
Crosfields. \ Cr * 2 NDOM is non-detergent organic matter. \ Cr
 \ begin {minipage} [t] {150mm} * ^ {3} Sokalan HP23 is a
grafted copolymer of poly (ethylene oxide) and
poly (vinyl acetate) available in the company
BASF. \ End {minipage} \ cr * 4 Coated percarbonate
available at Onterox. \ cr * ^ {5} Dequest 2047 en
ethylene diamine tetramethylene phosphonate available
in the Monsanto company. \ cr * ^ {6} Dequest 2016 is
hydroxy - ethylene diphosphonate available in the
company
Monsanto. \ Cr}
    

Comparative Examples A to D

The base composition of table 1 was mixed with granule * 7 swellable polymer disintegrant, starch * 8 and / or acetate to form Comparative Examples A, B and D as shown in table 2 that have the approximate compositions provided in table 3. All quantities in table 2 They are provided as part by weight. Example C was prepared at Starting from the base powder formulation only.

TABLE 2 Preparation of Comparative Examples A a D

5

The water-swellable disintegrating granule * 7 It was Nilyn LX-16 from the FMC Corporation, USA.; a compacted cellulosic disintegrating granule insoluble in Water.

Starch * 8 is from Roquette Freres, Lestrem, France and has an average particle size of approximately 15 micrometers

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TABLE 3 Composition of Comparative Examples A, B and D

6

40 g portions of each were prepared comparative composition in the form of cylindrical pads of 44.7 mm in diameter and a height of 19-20 mm using a Graseby Specac laboratory tablet preparation machine. The compaction pressure used for each tablet was adjusted from so that the tablets were compacted all to the same 30 kPa diametral fracture tension. The resistance of the tablet, in its dry state as it is they prepared in the press, and their diametrical fracture tension DFS by the method detailed in the previous description.

Examples 1 to 4

Examples 1 to 4 are examples according to invention. The composition in the form of base particles of the Table 1 was mixed with varying amounts of granule * 7 disintegrating polymer swellable starch * 8 to form the Examples 1 to 4 as shown in Table 4, which had the approximate compositions provided in table 5. All amounts in table 4 are provided as parts by weight. These particulate compositions were compressed as detailed below to produce the tablets of the invention.

TABLE 4 Preparation of Examples 1 to 4

7

Therefore, Examples 1 to 4 had the following approximate complete compositions provided in table 5. 100 parts of Examples 3 and 4 were added 3 parts by weight of polyethylene glycol 1500 at a level of 3 parts in weight to allow a DFS of 30 kPa to be obtained. So, Examples 1 and 2 are as% by weight and Examples 3 and 4 are parts by weight with a total of 103 parts by weight.

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TABLE 5 Composition of Examples 1 to 4

8

9

These compositions were compacted and the Pill resistance was determined according to the methods provided above for Comparative Examples A to D.

Disintegration results of Comparative Examples A to D and Examples 1 to 4

The speed of disintegration of the tablets is measured under static conditions. A pill was placed previously weighed on a metal rack with 1 x 1 units cm and the tablet and grid were then submerged in water current with a French hardness of 15º to 20ºC so that 2 cm of the water were above the top of the pill submerged After 60 seconds the metal grid was removed carefully from the water and the wet pill residue was weighed. Yes the tablet completely disintegrated in this period of time then the time elapsed for a disintegration was recorded 100% The results are provided in table 6.

TABLE 6 Disintegration Results of the Examples 1-4 and Comparative Examples A to D

10

* 9 were obtained Disintegration results in this interval.

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The previous results show that with the disintegration system of the invention a good one can be obtained disintegration of the detergent tablet over a period of time acceptable. In the absence of acetate or a polymer material that acts as a hydrophilic path, the disintegrating granule provides a reasonable disaggregation (Example A). The addition of 6% by weight cornstarch improves the breakdown characteristics of the tablet, especially for Examples 1 and 2. The Example Comparative B shows excellent disintegration but has a total 25.0% by weight of the acetate tablet formulation of sodium and disintegrating granule (as a disintegration system) and additionally 3.7% by weight of sodium citrate that can help the disintegration Examples 1 to 4 comprise only between 10% and 16% by weight of the corn starch pill formulation and disintegrating granule (as a disintegration system) and additionally 4.14-4.44% by weight citrate of sodium that can help disintegration. In the absence of the granule disintegrant, sodium acetate or starch, disintegration is poor (Examples D and E).

Comparative Examples E a I

The composition in the form of base particles of Table 1 was mixed with varying amounts of a granule * 7 Inflatable polymer disintegrant and / or acetate to form the Examples Comparatives E to I as shown in table 7 and which have the approximate compositions provided in table 8. All amounts in table 7 are provided in parts by weight.

TABLE 7 Preparation of Comparative Examples E a I

eleven

Therefore, Comparative Examples E to I had the following approximate complete compositions that provided in table 8.

TABLE 8 Composition of Comparative Examples E a I

12

13

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These compositions were compacted and the Pill resistance was determined according to the methods provided above for Comparative Examples A to D.

Examples 5 and 6

Examples 5 and 6 are examples according to the invention. The composition in the form of base particles of Table 1 was mixed with varying amounts of a * 7 swellable polymer disintegrant granule and * 8 starch (as used above) to form examples 5 and 6 shown in Table 9 having the approximate compositions provided in Table 10. All amounts in Table 9 are given in parts by weight. These particle-shaped compositions were compressed as detailed below to produce the tablets of the
invention.

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TABLE 9 Preparation of Examples 5 and 6

14

Therefore, Examples 5 and 6 had the following approximate complete compositions provided in table 10.

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TABLE 10 Complete compositions of Examples 5 and 6

100

fifteen

These compositions were compacted and the Pill resistance was determined according to the methods provided above for Comparative Examples A to D.

Disintegration results of Comparative Examples E to I and in Examples 5 and 6

The speed of disintegration of the tablets is determined as for the previous examples. The results are provided in table 11.

TABLE 11 Disintegration results of Examples 5 and 6 and Comparative examples E to I

16

17

The previous results show that with the disintegration system of the invention a good one can be obtained disintegration of a detergent tablet over a period of time acceptable. In the absence of acetate or a material that acts as a hydrophilic path, the disintegrating granule provides a reasonable disaggregation (Example E). A comparison of the Examples 5 and 6 with Examples F and G respectively show that the use of starch instead of acetate provides characteristics of comparable disintegration. Comparative example I exhibits a excellent disintegration but has a total of 26.0% by weight of the formulation of the sodium acetate tablet and disintegrating granule  (as a disintegration system) and additionally 3.64% by weight of Sodium citrate that can help disintegration. Examples 5 and 6 comprise only between 9 and 11% by weight of the formulation of the corn starch pill and a disintegrating granule (as a disintegration system) and additionally 4.39-4.49% by weight of sodium citrate that can Help the disintegration.

Claims (20)

1. A tablet of a detergent composition in form of compacted particles, comprising a non-surfactant soapy and a detergency adjuvant, in which the pill or a discrete area of it contains 1 to 20% by weight based on the total weight of the tablet of a disintegration system that understands a) water swellable disintegrating granules with an average particle size between 500-1,000 micrometers, and b) a hydrophilic starch having an average size of particles of 250 micrometers or less, a water solubility of less than 1 g / 100 g of water at 20 ° C and a force development of 2.0 Newtons expansion / second or less. 2. A tablet according to claim 1, in the that water swellable granules have a water solubility of less than 0.5 g / 100 g of water at 20 ° C. 3. One tablet according to any of the claims 1 or 2, wherein the disintegrating granules Water inflatables comprise a polymeric material. 4. A tablet according to claim 3, in the that water swellable disintegrating granules comprise cellulose. 5. A tablet according to any one of the previous claims, wherein the disintegrating granules they comprise 75 to 99.9% by weight of carrier material, 0.1 to 10% in weight of disintegrating material and 0% to 24.5% by weight of other material based on the total weight of the disintegrating particles. 6. A tablet according to any one of the previous claims, comprising between 1 and 11% by weight, based on the total weight of the tablet, of disintegrating granules Water inflatables. 7. A tablet according to any one of the previous claims, wherein the disintegrating granules Water inflatables have an average particle size in the 600 to 900 micrometer range. 8. A tablet according to any one of the previous claims, wherein the disintegrating granules Water inflatables comprise a disintegrating material, in which the disintegrating material has a development of expansion forces of more than 2.2 Newtons / second. 9. A tablet according to any one of the previous claims, comprising 1 to 15% by weight of hydrophilic starch. 10. A tablet according to any one of the previous claims, wherein the hydrophilic starch has an average particle size of 150 micrometers or less. 11. A tablet according to any one of the previous claims, wherein the hydrophilic starch has a development of expansion forces of 1.5 Newtons / second or less. 12. A tablet according to any one of the previous claims, wherein the hydrophilic starch is a native starch 13. A tablet according to claim 12, in which the native starch is corn starch, tapioca, rice or potato. 14. A tablet according to any one of the previous claims, wherein the tablet or discrete area thereof comprises said disintegration system in an amount from 8 to 16% by weight based on the total weight of the tablet or area of the same. 15. A tablet according to any one of the previous claims, wherein said pill or zone discrete thereof additionally comprises a material hydrophilic cellulosic. 16. A tablet according to any one of the previous claims, wherein said tablet comprises additionally soluble disintegration promoting particles in water containing at least 40% (by weight of the particles) of one or more materials selected from the group consisting in

?

compounds with a solubility in water that exceeds 50 grams per 100 grams of water at 20ºC

?

sodium tripolyphosphate which It contains at least 50% of its own weight of the anhydrous phase form I

?

sodium tripolyphosphate that is partially hydrated so that it contains hydration water in an amount that is at least 0.5% by weight of the tripolyphosphate of sodium in the particles.

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17. A tablet according to claim 16, in which said compounds with a water solubility that exceeds 50 grams per 100 grams of water are chosen from trihydrate of sodium acetate, sodium acetate, citrate dihydrate sodium or urea 18. One tablet according to any of the claims 16 to 17, wherein the tablet contains 2 to 10% by weight of said particles favoring disintegration water soluble 19. A disintegrating system for a pill of a detergent composition in the form of compacted particles that it comprises a non-soap surfactant and an adjuvant of the detergency, in which the disintegration system comprises a) water swellable disintegrating granules with an average particle size between 500-1,000 micrometers, and b) a hydrophilic starch having an average size of particles of 250 micrometers or less, a water solubility of less than 1 g / 100 g of water at 20 ° C and a force development of 2.0 Newtons expansion / second or less. 20. A procedure to prepare a pill of a detergent composition in the form of compacted particles comprising a non-soap surfactant and an adjuvant of the detergency, procedure comprising 1) mix 1 to 20% by weight based on weight total of the tablet of a disintegration system that understands

to)

inflatable disintegrating granules in water with an average particle size between 500-1,000 micrometers, and

b)

a hydrophilic starch having an average particle size of 250 micrometers or less, a water solubility of less than 1 g / 100 g of water at 20ºC and a development of expansion forces of 2.0 Newtons / second or less, with

2) other constituents of a composition detergent including a non-soap surfactant and an adjuvant of the detergency, place an amount of the composition in shape of particles resulting in a mold and compacting that composition into mold.