CZ9904374A3 - Tablet of cleansing agent - Google Patents

Abstract

A tablet of a cleaning agent from a pressed particulate cleaning composition containing a surfactant of from 5 to 50 wt. and an activating detergent component of from 5 to 80% by weight which further it contains water-insoluble and water-swellable polymer material, and disintegrating particles comprising at least 40% (by weight of these particles) of one or more materials selected from compounds with solubility in deionized water at 20 ° C for at least 50 grams per 100 grams water, phase I sodium tripolyphosphate and sodium tripolyphosphate, partially hydrated to contain water hydration in at least 0.5% by weight of sodium tripolyphosphate; these disintegrating particles. The solution goes further a method of making a detergent tablet.

Description

Technical field

The present invention relates to a tablet-shaped cleaning composition for use in fabric washing.

BACKGROUND OF THE INVENTION

Tablet detergent compositions are described, for example, in GB 911204 (Unilever), US 3953350 (Kao), JP 60015500A (Lion), and EP-A-711827 (Unilever), and are commercially marketed in Spain. Tablets have advantages over powdered products in that they do not require metering and are thus easier to handle and easier to dispense into a washing machine.

Tablets of a detergent composition are generally made by compressing or compressing a certain amount of the composition in particulate form. It is desirable that the tablets have adequate dry strength, but that they rapidly disperse and dissolve when added to the wash water. In such tablets, the surfactant functions as a binding agent, and makes the tablet malleable. However, it may also slow the disintegration of the tablet by forming a viscous gel upon contact of the tablet with water.

It may be difficult to obtain both strength and the ability to disperse and dissolve rapidly in a wash solution for a tablet. Tablets shaped using only light compression •

- 2 «· 2 2 2 - 2« 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 The tendency to crumble and disintegrate when handled and packaged, while heavily compressed tablets may be sufficiently cohesive, but they do not disintegrate or disperse to a sufficient extent in the wash solution.

This problem has proven to be particularly acute in tablets formed by compressing powders containing a surfactant and an insoluble activating detergent component such as sodium aluminosilicate (zeolite).

It is known to include materials having the function of promoting the disintegration of the tablet when placed in the wash water. Some tablets sold commercially contain urea for this purpose. Urea has a very high solubility in water exceeding 100 grams per 100 ml of water at 20 ° C.

SUMMARY OF THE INVENTION

The authors have now found that disintegration of the cleaning composition tablets can be accelerated by including in the tablet a certain amount of water-insoluble but water-swellable polymeric material.

However, the authors have also observed that particles of water-swellable water-insoluble material that are effective to cause tablet disintegration tend to be trapped on the laundry as visible residues.

The authors therefore suggest in the present invention that decay a

- 3 tablets were caused by a combination of two materials, a water-swellable but water-insoluble material. The second is the water-soluble compound solubility.

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In accordance with the present invention there is provided a tablet of a compressed particulate cleaning composition comprising a total of from 5 to 10%

50% by weight of the surfactant and from 5 to 80% by weight of the activating detergent component, characterized in that the tablet or its separate region containing the surfactant and the activating detergent component also comprises (i) a water-insoluble and water-swellable agent polymeric material, and (ii) dissolution / disintegration particles comprising at least 40% (by weight of the particles (ii)) of one or more materials selected from * compounds having a solubility in deionized water at 20 ° C of at least 50 grams per 100 grams water; Phase I sodium tripolyphosphate; or * Sodium tripolyphosphate partially hydrated so as to contain water of hydration in an amount of at least 0.5% by weight of the tripolyphosphate in the particles.

As will be further explained below, these disintegrating particles also contain other forms of tripolyphosphate or other salt in the balance of the mixture.

The tablet of the invention may be either homogeneous or heterogeneous.

In this description, the term homogeneous means a tablet made by a physiologist. ·· · * ·· · · · · · · · · · · · ·

4 by pressing one particulate mixture, but this does not mean that all the particles of the mixture will necessarily have the same composition. The term "heterogeneous" refers to a tablet consisting of a number of discrete regions, for example layers, inserts or coatings, each obtained by compressing the particulate mixture. In a heterogeneous tablet in accordance with the present invention, each discrete region of the tablet will preferably have a weight of at least 5 grams.

In a heterogeneous tablet, at least one of the discrete regions comprises said water-swellable polymeric material and disintegration-promoting particles together with a surfactant and an activating detergent component in accordance with the invention.

^{15 Dec}

A preferred tablet or separate region thereof comprises from 2 or 5% to 40 or 50% by weight of a surfactant, from 5 or 10% to 60 or 80% by weight of an activating detergent component, and from 0.5 to 10% by weight of a water insoluble but water swelling polymer material. When the tablet is heterogeneous, these percentage ranges may be applied to the total tablet mixture as well as to at least one discrete region of the tablet.

If the material in the disintegrating particles can act as an activating detergent component (as is the case with sodium tripolyphosphate), then it contributes to the total amount of activating detergent component in the tablet mixture.

• · · · 4 4 »·

Suitably the amount of disintegrating particles is from 5 or 8% by weight up to 25 or 40% by weight of the tablet or region thereof. A water-insoluble water-swellable polymeric material may be beneficial when contained in an amount of from 0.5, preferably from 0.9 to at least 2.7, or 3.5% by weight of the tablet or region thereof. It may optionally be used in larger amounts, such as up to 5 or 8% by weight.

In a heterogeneous tablet, the polymeric material may be contained in only some of a number of separate regions (e.g., only one or two), while the other region (s) contain less concentration or more polymeric material. Such an arrangement may be used to cause disintegration and dissolution of the tablets (insofar as their components are soluble) at different rates.

Water swelling polymer

Suitable water-swellable polymer materials preferably have sufficient water absorbency so that they can absorb at least four times their own weight of water, i.e., take up at least 4 grams of water per gram.

A number of such materials are known, and generally are based on cellulose, which can be chemically treated to increase its water-acquisition capacity. Sometimes such modified celluloses have ionic substituents, but for the present invention it is preferred that any substituents

- 6 • 9 9

9

9 9 9 9 9 9 9 were non-ionic.

Surprisingly, the authors have found that such a material is more effective when it has a relatively large particle size. Therefore, it is preferred that the polymer material has a particle size of at least 400, more preferably at least 500 microns. Such a polymer material having a particle size of at least 400 microns is preferably an agglomerate of smaller particles whose largest dimensions do not exceed 150 or 200 microns, more preferably do not exceed 50 microns. This allows at least some polymer particles to break up during the wash cycle, and these do not remain as visible residues on the fabric.

This material may be in the form of relatively rounded particles, or as relatively flat particles, such as flakes or discs. In the latter case, the size (diameter) of the flakes will be larger, possibly substantially larger than the diameter of a ball of equal volume.

The largest particle size of the polymeric material can be determined by sieve analysis, and the shape of the particles can be observed under a microscope. It is customary to use carboxymethyl sodium cellulose (SCMC) in detergent compositions, usually no more than

3% by weight of the mixture. The authors found that such amounts of SCMC are generally ineffective to promote tablet disintegration.

The authors have found it desirable to use water-swellable polymeric materials of low ionic or nonionic character. Such materials can be polysaccharides with little φφ ··· «

- 7 or no ionic substitution.

The absence or near absence of ion substitution can be expressed by claiming that the charge density of the polymer material is small, such as less than 10, preferably less than 6 x 10, or even zero. The term charge density refers to the number of charges per polymer molecule divided by the molecular weight of the polymer. It is essentially the same as the amount of charge per repeating unit of polymer divided by the average molecular weight of the repeating unit.

The water-insoluble water-swellable polymer material is preferably added as particles containing such a material as at least 75% by weight of the anhydrous weight of the particles (i.e. ignoring their moisture content). They will usually contain little or nothing other than the polymer and accompanying moisture.

Decay-supporting particles

One possibility is that the particles comprise at least 40% of their own weight, preferably at least 50%, of a material having a solubility in deionized water at 20 ° C of at least 50 grams per 100 grams of water.

Said particles may provide such a material in an amount of at least 7 or 12% by weight of the total tablet composition or its separate region.

• • • •

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

10 Some highly water soluble materials are possible used, are listed below, with their solubilities expressed in grams of solid required to form saturated solution in 100 grams of water at 18 ° C: Material Water solubility (g / 100g) sodium citrate dihydrate 72 potassium carbonate 112 15 Dec urea > 100 sodium acetate 119 sodium acetate trihydrate 76 magnesium sulfate 7H ₂ O 71 20 May In contrast to that solubility at 20 ° C are as follows: some common materials Material Water solubility (g / 100g) sodium chloride 36 25 sodium sulfate decahydrate 21.5

anhydrous sodium carbonate anhydrous sodium percarbonate

anhydrous sodium perborate 3.7 anhydrous sodium tripolyphosphate 15 Dec

Preferably, the highly water-soluble material is contained as particles of the material in substantially pure form (i.e., each such particle contains more than 95% by weight of the material). However, said particles may comprise a material with such solubility in admixture with another material, provided that the material of said determined solubility is at least 40% by weight of the particles.

It may be preferred that the highly water-soluble material be a salt that dissolves in ionized form in water. When such a salt dissolves, this leads to a transient local increase in ionic action, which may aid the disintegration of the tablet by preventing swelling of the nonionic surfactant, which prevents the dissolution of other materials.

Another possibility is that said disintegrating particles are particles containing sodium tripolyphosphate with more than 40% (by weight of these particles) in the anhydrous form of phase I.

Sodium tripolyphosphate is well known as a protective component in detergent compositions. It exists in hydrated form and in two crystalline anhydric forms. These are normal crystalline anhydrous forms, known as phase II, which is a low temperature phase, and phase I, which is stable at high temperature. The conversion of Phase II to Phase I proceeds relatively rapidly when heated above a transition temperature of about 420 ° C, but the reverse reaction is slow. Phase I of sodium tripolyphosphate is in ····

As a result metastable at ambient temperature.

A process for the production of particles containing a large portion of phase I sodium tripolyphosphate by spray drying at a temperature below 420 ° C is described in US-A-4536377.

Particles comprising this phase form I will often contain phase form I of sodium tripolyphosphate as at least 50 or 55% by weight of sodium tripolyphosphate in the particles.

A suitable material is commercially available. Suppliers include Rhone-Poulenc, France, and Albright & Wilson, UK.

Another possibility is that the disintegrating particles are particles containing at least 40% by weight of partially hydrated sodium tripolyphosphate. The extent of hydration should be at least 0.5% by weight of the sodium tripolyphosphate in the particles. It can range from 0.5 to 4% or higher. Fully hydrated sodium tripolyphosphate may also be used for these particles.

It is possible for the particles to contain at least 40% by weight of sodium tripolyphosphate with a high phase I content but which is also sufficiently hydrated to contain at least 0.5% water by weight of the sodium tripolyphosphate.

The remainder of the tablet mixture used to form the tablet or region thereof may comprise an additional sodium tripolyphosphate. He can

- 11 ·· ··· 4

4 4 4 4 9 • 4 · 4 · 4 · 99 99 · in any form, including sodium tripolyphosphate with a high anhydrous phase II form. When said particles comprise sodium tripolyphosphate, it is preferred to provide sodium tripolyphosphate in an amount of at least 8%, e.g. 8 to 30%, by weight of the tablet composition or region thereof.

A zero phosphate-containing tablet in accordance with the invention will utilize a disintegration-promoting particle comprising a material having a solubility of at least 50 grams / 100 grams.

Such a material can also be used with phosphate component tablets, but is more likely to utilize phase I and / or hydrated sodium tripolyphosphate particles.

When the particles contain sodium tripolyphosphate, it will act as a binding component after the tablet or region thereof disintegrates and dissolves in the wash solution.

The total amount of sodium tripolyphosphate present in all forms in the tablet mixture may range from 15 to 60% by weight of the tablet. It will therefore be appreciated that the total amount of sodium tripolyphosphate may be provided in part as another material in addition to said particles.

Said disintegrating particles will generally be mixed with other particles comprising a surfactant, at least some activating detergent component, and other components of the composition so as to obtain a total composition that is compressed into do »♦ ···

- 12 • 9 9 9 9 9 9 9 9 9 9 9 9 9 9

99 or tablet area.

Surfactant compounds

Compositions which are compressed to form tablets or tablet areas of the present invention will generally contain one or more organic surfactants. In the fabric wash composition, these will preferably be from 5 to 50% by weight of the total tablet composition, more preferably from 8 or 9% by weight of the total composition up to 40 or 50% by weight. The surfactant may be anionic (soap or non-soap), cationic, zwitterionic, amphoteric, nonionic, or combinations thereof.

The anionic surfactant may be present in an amount of from 0.5 to 50% by weight, preferably from 2 or 4% to from 30 or 40% by weight of the tablet composition.

Synthetic (i.e., non-soap) anionic surfactants are well known in the art. Examples include alkylbenzene sulphonates, particularly linear alkylbenzene sulphonates having an alkyl chain length _of C ₈ _ ₁₅ alkane sulphonates, dialkyl sulphosuccinates and fatty acid ester sulphonates.

Primary alkyl sulfate of formula

ROSO ₃ ~ M ⁺

00

0 0 0 0 0000 0 0

0 0 • 0 0

0 0 0

00 • 0 00 · 0 0

0 0 0 0 0 0

Wherein R is an alkyl or alkenyl chain of 8 to 18 carbon atoms, in particular 10 to 14 carbon atoms, and M ⁺ is a cationic solubility, is commercially significant as an anionic surfactant.

Linear alkylbenzene sulfonate of formula

wherein R is a linear alkyl of 8 to 15 carbon atoms, and M ⁺ is a cationic solubility, especially sodium, is also a commercially significant anionic surfactant.

Such a linear alkylbenzene sulphonate or primary alkyl sulphate according to the above formula, or a mixture thereof, will often be desirable for an anionic surfactant, and may be 75 to 100% of any anionic non-soap surfactant in the composition.

In some embodiments, the amount of non-soap anionic surfactant is in the range of 5 to 20% by weight of the tablet composition.

It may also be desirable to include one or more fatty acid soaps. They are preferably sodium soaps derived from naturally occurring fatty acids, for example fatty acids

9

999

9 9

0 9

99 ·· ····

0 9

9 9

9

9 9 9

99

99 • 9 9

4 9 4

0 0 0 • ·· 0 ·· 00 of coconut oil, beef tallow, sunflower or hardened rapeseed oil.

Suitable nonionic surfactant compounds that may be used include, in particular, the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides, or alkylphenols with alkylene oxides, especially ethylene oxide.

Specific compounds of nonionic surfactants are alkyl (C _g _ ₂ 2) phenol-ethylene oxide condensates, the condensation products of linear or branched aliphatic C _g _ ₂₀ primary or secondary alcohols with ethylene oxide, and the condensation products of ethylene oxide with reakóními products of propylene oxide and ethylene-diamine.

Especially preferred are the primary and secondary alcohol ethoxylates, especially a C ₁₂ _ ₁₅ primary and secondary alcohols ethoxylated with an average of 5 to 20 moles of ethylene oxide per mole of alcohol.

In certain embodiments of the invention, the amount of nonionic surfactant is in the range of 4 to 40%, preferably 4 or 5 to 30% by weight of the composition. Many nonionic surfactants are liquids. These can be absorbed on the mixture particles prior to compression into tablets.

- 15 Activating detergent component

The composition compressed to form tablets or tablet areas will generally contain from 5, preferably from 15% by weight to up to 80%, more usually from 15 to 60% by weight, of an activating detergent component. This may consist entirely of water-soluble materials, or may for the most part or entirely consist of a water-insoluble material having water-softening properties. The water-insoluble activating detergent component may be present in an amount of from 5 to 80% by weight, preferably from 5 to 60% by weight of the composition.

Alkali aluminosilicates are strongly preferred as environmentally acceptable water-insoluble activating

detergentní alkaline ingredients for washing metal (preferably of fabrics. sodium) Aluminosilicates they can be either crystalline or amorphous, or their mixtures, p common pattern 0.8 - 1.5 Na ₂ O.Al ₂ O ₃ . 0.8 - • 6 SiO ₂ . xh ₂ o.

These materials contain some bound water (denoted as x 25 H 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 SiO ₂ units (in the formula above).

Both amorphous and crystalline materials can be readily prepared by the reaction between sodium silicate and sodium aluminate, as widely described in the literature.

• ·

Suitable crystalline sodium aluminosilicates as ion exchange activating detergent ingredients are described, for example, in GB 1429143 (Procter & Gamble). Preferred sodium aluminosilicates of this type are the well known commercially available zeolites A and X, and the more recent zeolite P described and claimed in EP 384070 (Unilever), and mixtures thereof.

It is also possible for the water-insoluble activating detergent component to consist of a layered sodium silicate as described in US 4664839. The trademark for crystalline layered silicate manufactured by Hoechst is NaSKS-6 (usually abbreviated as SKS-6). NaSKS-6 takes the form of delta-Na ₂ SiO ₅ layered silicate morphology. It can be prepared by methods such as those described in DE-A-3,417,649 and DE-A-3,742,043. Other such layered silicates may also be used, such as with the general formula

NaMSi _x O _{2 + 1} .yH ₂ O, where M is sodium or hydrogen, x is a number from 1.9 to 4, preferably 2, and y is a number from 0 to 20, preferably may be selected as 0.

Water-soluble phosphorus containing inorganic activating detergent ingredients include alkali metal orthophosphates, metaphosphates, pyrophosphates and polyphosphates. Specific examples of inorganic phosphate activating detergent ingredients include sodium and potassium tripolyphosphates, orthophosphates and hexametaphosphates. As mentioned above, tripolyphos30 sodium (if present) included in the particles to support

Disintegration will also be part of this activating detergent component.

The non-phosphorus water-soluble activating detergent builders may be organic or inorganic. Inorganic components that may be present include alkali metal (generally sodium) carbonate, while organic components include polycarboxylate polymers such as polyacrylates, acrylic / maleate copolymers, and acrylic phosphonates, monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono- di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates and hydroxyethyliminodiacetates.

Tablet compositions preferably include polycarboxylate polymers, especially polyacrylates and acrylic / maleate copolymers, which can act as activating detergent ingredients and also can prevent unwanted deposits on the fabric from the wash solution.

Bleaching system

The detergent compositions in the tablets of the invention may contain a bleaching system. It preferably contains one or more bleaching peroxy compounds, for example inorganic peroxy salts or organic peroxyacids, which can be used together with activators to improve bleaching action at low wash temperatures. If any peroxy compound is present, the amount will probably be in the range of 10 to 25% by weight of the composition.

Preferred organic peroxy salts are sodium perborate monohydrate and tetrahydrate and sodium percarbonate, preferably used together as an activator. Bleach activators, also referred to as bleach precursors, have been widely disclosed in the art. Preferred examples include peracetic acid precursors, for example tetraacetylethylenediamine (TAED), now in widespread commercial use in conjunction with sodium perborate, and peroxybenzoic acid precursors. Also of interest are the ammonium and phosphonium bleach activators disclosed in US 4751015 and US 4818426 (Lever Brothers Company). Another type of bleach activator that may be used but which is not a bleach precursor is a transition metal catalyst as disclosed in EP-A-458397, EP-A-459398, and EP-A-549272. The bleach system may also include a bleach stabilizer (heavy metal based preservative) such as ethylenediamine tetramethylene phosphonate and diethylenetriamine pentamethylene phosphonate.

Other detergent ingredients

The detergent tablets of the invention may also contain one or more detergent enzymes well known in the art for their ability to break down and assist in the removal of various soils and stains. Suitable enzymes include various proteases, cellulases, lipases, amylases, and mixtures thereof that are intended to remove a variety of soils and stains from fabrics. Examples of suitable proteases are Maxatase (Trade Mark), available from

Gist-Brocades N.V., Delft, The Netherlands, and Alcalase (Commercial •

- 19 · · · • • • ♦ A A 19 19 19 19 19 19 19 19 19 19 19 19 19 19 19 19 19 19 19 A 19 And Savinase (trademark), supplied by Novo Industri A / S, Copenhagen, Denmark. Detergent enzymes are generally used in the form of granules, optionally with a protective coating, in an amount of from 0.1 to about 3.0% by weight, and these granules do not cause problems in compression and tablet formation.

The detergent tablets of the invention may also contain a fluorescent agent (optical brightener), for example Tinopal (Trade Mark) DMS or Tinopal CBS available from Ciba-Geigy AG, Basel, Switzerland. Tinopal DMS is disodium 4,4'bis- (2-morpholino-4-anilino-s-triazin-6-ylamino) stilbendisulfonate, and Tinopal CBS is disodium 2,2'-bis- (phenylstyryl) disulfonate.

Advantageously, an antifoam material is included, especially when the detergent tablet is primarily intended for use in front-loading drum washing machines.

Suitable antifoam materials are generally in the form of granules, as described in EP 266863A (Unilever). Such antifoam granules typically comprise a mixture of silicone oil, petroleum jelly, hydrophobic quartz, and alkyl phosphate as antifoam active material absorbed on a porous water-soluble carbonate-based inorganic carrier material. The antifoam granules may be present in an amount up to 5% by weight of the composition.

It may also be desirable for the tablet of the invention to contain a certain amount of alkali metal silicate, especially ortho-silicate.

sodium meta- or disilicate. The presence of such alkali metal silicates in an amount of, for example, 0.1 to 10% by weight may be advantageous in providing corrosion protection of the metal parts of the washing machines, in addition to some beneficial effect on the formation and processing of the particulate material being compressed into tablets.

The laundry detergent tablet will generally not contain more than 15% by weight of silicates. The machine dishwashing tablet will often contain at least 20% by weight of silicates.

Other ingredients that may optionally be used in the laundry detergent tablet composition of the present invention include antifouling agents such as carboxymethyl sodium cellulose, straight-chain polyvinylpyrrolidone, and cellulose ethers such as methylcellulose and ethylhydroxyethylcellulose, fabric softeners, preservatives for heavy metal bases such as EDTA, perfumes, and dyes or stains.

Particle dimensions and their distribution

The detergent tablet of the invention, or a separate region thereof, is a matrix of compressed particles.

Preferably, the particulate composition has an average particle size in the range of 200 to 2000 microns, more preferably 250 to 1400 microns. Fine particles smaller than 180 or 200 micrometers are »· ·« to · · ’·· ··

- 21 ···· can be avoided by sieving before compression of tablets, if desired, although the authors have observed that this is not always essential.

While the starting particulate composition may have substantially any total density, the present invention particularly relates to tablets made by compressing powders of relatively high overall density, due to their greater propensity to exhibit disintegration and dispersion problems. Such tablets have the advantage over tablets obtained from a powder of low overall density that a given dose of the mixture may be in a smaller tablet.

Thus, the starting particulate composition suitably may have a total density of at least 400 g / liter, preferably at least 500 g / liter, and possibly at least 600 g / liter.

The mixture that is compressed into a tablet or tablet region may contain particles prepared by spray-drying or granulation, which contain a mixture of ingredients. Such particles may comprise a surfactant and some or all of the activating detergent component.

Basically suitable for use in the present invention are high total density granular detergent compositions prepared by granulation and concentration in a high speed mixer / granulator as described and claimed in EP 340013A (Unilever), EP 352135A (Unilever), and EP 425277A (Unilever) ) or continuous granulation / thickening processes,

22 described and claimed in EP 367339A (Unilever), and EP 390251A (Unilever).

The separated particles of water-insoluble water-swellable polymer material and said disintegrating particles are preferably mixed with the remainder of the particulate mixture prior to compression.

Production of tablets

The manufacture of tablets involves compression of the particulate mixture. A number of tablet making machines are known which can be used. In general, it will function by embossing a certain amount of the particulate composition contained in the die.

Tablets can be made at ambient temperature or at a temperature above ambient temperature, which may allow for adequate force to be obtained with less pressure applied during compression. For producing tablets at a temperature above ambient, the particulate composition is preferably fed to the tablet manufacturing machine at elevated temperature. This, of course, supplies heat to this machine, but it can also be heated in another way.

If heat is supplied, it is assumed to be supplied in a conventional manner, such as passing the particulate mixture through the furnace, rather than using microwave energy.

• • · * »

Φ ·· ·· · φφφ

Φ · φ · ΦΦ · φ · φ · φ · φ · φ · φ ·

The size of the tablet will suitably vary from 10 to 160 grams, preferably from 15 to 60 grams, depending on the conditions of intended use and whether the tablet represents the entire dose for the average load in a laundry or dishwasher, or just a portion of that dose. The tablets may have any shape. For ease of packaging, however, they are preferably blocks of substantially uniform cross-section, such as cylinders or blocks. The total density of the tablets is preferably in the range of 1040 or 1050 grams / liter up to 1300 grams / liter. The density of the tablets may well be in the range of no more than 1250 or even 1200 grams / liter.

DETAILED DESCRIPTION OF THE INVENTION

Example 1

Tablets for use in the washing of fabrics, with a spray-dried starting base powder, having the following composition:

Component Parts by weight Sodium linear alkylbenzene sulphonate 11.0 Sodium tripolyphosphate (Added to the slurry as 16.8 Anhydrous sodium tripolyphosphate containing at least 70% phase II form) from 13 to 15 ^{C MAS} groundless alcohol 7E0 2.4 ^C 13-15 ^fatty alcohol 3EO Ý 2.3 Sodium silicate 4.0 Soap 0.21 acrylate / maleate copolymer 1.5 sodium sulphate, moisture and minor components up to 45 parts

- 24 • 0

A number of particulate mixtures were made by mixing this powder with the other ingredients listed in the table below, which included sodium tripolyphosphate particles having the desired 70% phase form content and 3.5% hydration water content (Rhodia Phos HPA 3.5, available from Rhone - Poulenc).

The added components also included particles of a water-insoluble water-swellable polymer material. This material was obtained from cellulose and supplied by Rettenmaier GmbH as Arbocel A1. It was in the form of particles with a certain range of particle shapes and sizes (as determined by screen analysis) with a mean diameter of 1 mm.

For some mixtures, this material was sieved to give a fraction with a narrower particle size range.

The mixtures were made up to 100% by incorporating varying amounts of high density anhydrous sodium carbonate.

The various mixtures contained the following amounts in percent by weight:

9

- 25 * 9 9 9 «· · 9 9

9999 · ·

9 9 9 9 9

9 · 9 · 9

99 • 99

Ingredient base powder granules sodium percarbonate granules TAED antifoam granules perfumes, enzymes, and other minor ingredients tripolyphosphate HPA water swelling polymer sodium carbonate% by weight

45.0

15.0

3.4

3.2

3.5 variable, 15 to 30 variable, 0 to 5 remaining part, 0 to 15

Cylindrical tablets of 44 15 mm diameter were made from 40 g of each mixture using a Fette pilot press to produce tablets with a density ranging from 1100 to 1250 kg / m ³ .

The strength of these tablets was measured using an Instron universal testing machine to compress the tablet until it was broken. The fracture pressure average (DFS) was then calculated using the equation

2P σ = -, π D t where σ is the fracture pressure on average in Pascals, P is the applied fracture load in Newtons, D is the tablet diameter in meters, and t is the tablet thickness in meters.

The disintegration, dispersion and dissolution of the tablets was measured by a test procedure in which the tablet was placed on a plastic sieve with • φ φ φ ♦ φ · · ·

The size of the 2 mm grid was immersed in 9 liters of demineralised water at an ambient temperature of 22 ° C and rotated at 200 rpm. The conductivity of the water was measured until a constant value was reached.

The time required for disintegration and dispersion of the tablets was considered as the time ( _TgQ ) required to reach 90% of the final water conductivity. This was also confirmed by visual observation of the remaining material on the rotating screen. Additionally, the initial gradient of the conductivity curve versus time was recorded and was expressed as a value normalized to one of the mixtures.

The percentages of HPA tripolyphosphate and polymeric material, along with DFS values and conductivity measurements, are as follows:

• *, ”,. .... ..; * ·· · · *! Ί!

; .. ...... · «· ·· ·· ·· ·· ··

designation tripolyphosphate ΗΡΑ (%) polymeric material (%) complementary carbonate (%) # 5 ΙΑ 30 0 0 1Β 27.5 0 2.5 1C 15 Dec 0 15 Dec 1D 24 2 as delivered 4 ΙΕ 15 Dec 5 as delivered 10 10 1F 20 May 1.5 as delivered 8.5 1G 15 Dec 5, 470-800μ 10 1Η 15 Dec 5, 800-1400μ 10 1J 15 Dec 3, 800-1400μ 12 15 Dec designation DFS T _go (minutes) gradient curves # (kPa) conductivity / time ΙΑ 43 3.0 1 1Β 30 2.5 2 1C 32 8.7 1 20 May 1D 32 3.2 3.3 ΙΕ 18 1.6 26 1F 50 6.0 2.3 1G 30 3.2 16 1Η 21 1.4 23 25 1J 33 2.8 16

• fl · · · ·

- 28 ♦ «fl fl fl fl fl fl • • • • • • • • • • * *

99 99 99

99 · f fl f f f f f f f f f f f

Example 2 Tablets with a weight of 40 g were produced as in Example 1, p 5 using the same dried base powder by spraying, but with other additional ingredients, as Yippee mentioned in the following table: Component % weight 10 base powder 58.0 polyvinylpyrrolidone 0.6 anti-foaming granules 4.2 perfumes, enzymes, and other minor ingredients 2.0 sodium citrate dihydrate 20.0 15 Dec water swelling polymer 800-1400μ 3.0 sodium carbonate rest up to 100% Example 3 Tablets were made for use in laundry Fabrics, p 20 May a starting base powder of the following composition: Component % weight sodium linear alkylbenzenesulfonate 10.7 ^c 13-15 fatty alcohol 7EO 1.7 25 ^C 13-15 fatty alcohol 3E0 3.1 zeolite A24 21.0 sodium carbonate 3.7 sodium citrate dihydrate 3.1 moisture and minor components 5.6

48.9 total ·· «· • ftft • · · ·· • 9 1

9 1

11 ·· ····

11

Three particulate mixtures were made by mixing this powder with the other ingredients as shown in the table below. The water swelling polymer was Arbocel Al, and was used as supplied. The amounts of each 40 g blend were compressed into tablets using compression presses such that the tablets had the same values of fracture strength on average (DFS) measured as in Example 1 above. The tablets were tested for disintegration and dissolution as in Example 1, and the conductivity T _go values are shown at the bottom of the table.

Ingredient% by weight

15 Dec base powder 48.9 48.9 48.9 sodium perborate monohydrate 13.9 13.9 13.9 granules TAED 5.3 5.3 5.3 anti-foaming granules 2.0 2.0 2.0 granules of a fluorescent agent 1.2 1.2 1.2 20 May sodium silicate granules 3.7 3.7 3.7 acrylic / maleate copolymer 1.0 1.0 1.0 perfumes, enzymes and other minor ingredients 3.5 3.5 3.5 sodium acetate trihydrate 18 14.5 11.0 a water swelling polymer 0 1.0 2.0 25 sodium carbonate 2.5 5.0 7.5 total 100 ALIGN! 100 ALIGN! 100 ALIGN! T _go (minutes) > 10 8.3 5.7

44 9 ·

- 30 49 9 9 9 9 9

44

9

9

4 9 9 9

9 4 4 9 ·· 94 44

Example 4

The procedure of the previous example was repeated, using a base powder containing as the anionic surfactant a primary alkyl sulfate instead of an alkyl benzene sulfate. One blend contained 3% by weight of Arbocel A1. A _Tg of 2 minutes was observed.

The Arbocel A1-free comparative mixture, produced with the same DFS of 33 kPa, had a _TgQ of 7.5 minutes.

Example 5

Tablets weighing 40 g have been produced for use in fabric washing, with a starting base powder of the following composition:

Component sodium linear alkylbenzene sulfonate ^C 13-15 alcohol 7E0 ^masses groundless ^C 13-15 ^fatty alcohol 3E0 Ý zeolite A24, sodium citrate dihydrate, sodium sulphate, moisture and minor ingredients parts by weight

7.7

3.5

3.7

25.2

2.6

This powder was then mixed with other ingredients to form a particulate mixture which was then compressed into tablets as in the previous examples. These mixtures were as follows:

0 0 0 0 0 0 0

0 0 9 * 9 9 9 9

9 999 00 0 0000 • 0 0 0 · 0 · 000 00 0

00 0 0 00 0 0 00 «« 0 00 0 · 00 00 00

- 31 Ingredient% by weight base powder sodium peroxyborate monohydrate granules TAED antifoam granules granules of fluorescent agent sodium silicate granules sodium acrylate / maleate copolymer water carbonate swelling polymer sodium acetate dihydrate perfumes, enzymes and other minor ingredients

50.0 67.0

14.3 5.5

1.0 2.0

1.0

3.7

1.0 1.8

3.2

3.0 3.0

20 May

2.5 3.0 ψΖ 159V-ΡΖιο

99 99 99 99 99 99 ·

9 9 9 9 9

9,999 9 9 9 0 0 0 0 • * · 000 0 · 00 00 0

00 0 0 00 0 000 0

00 00 ·· 99 00

Patent claims

Claims (18)

1. A compressed particulate composition cleaning composition tablet comprising a total of from about 5% to about 50% by weight of a surfactant and from about 5% to about 80% by weight of an activating detergent component, and the tablet or a separate area thereof comprising a surfactant 10 and an activating detergent component, also comprising a water-insoluble water-swellable polymer material, and disintegrating particles comprising at least 40% (by weight of the particles) of one or more materials selected from the group consisting of: 15 * compounds having a solubility in deionized water at 20 ° C of at least 50 grams per 100 grams of water; * Phase I sodium tripolyphosphates; * Sodium tripolyphosphates partially hydrated to contain at least 0.5% by weight water of hydration 20 sodium tripolyphosphates in these particles. 2. A tablet according to claim 1, wherein said disintegrating particles comprise at least 40% (by weight of said particles) of one or more compounds with The solubility in deionized water at 20 ° C of at least 50 grams per 100 grams of water, and said compounds are selected from urea, salts, and mixtures thereof. A tablet according to claim 1, characterized in that 30, said disintegrating-promoting particles in the tablet or its T / 1 ^ 9 9 9 9 9 9 9 99 0 0 0 0 • 0 00 0 0000 0 0 000 0 0 0 0 0 0 0 0 000 000 0 000 000 0 0 0 0 0 0 0 0 0 0 00 00 00 00 00 00 - 33 regions contain at least 40% (by weight of these particles) phase Even sodium tripolyphosphate, which is partially hydrated, so 5 to contain water of hydration ranging from 0.5 to 4% by weight of the particles. A tablet according to any one of claims 1 to 3, wherein the polymeric material has a particle size 10 at least 400 microns. A tablet according to any one of claims 1 to 3, wherein the polymeric material has a particle size of at least 500 microns. A tablet according to any one of claims 1 to 5, wherein the polymeric material is substantially nonionic so that the charge density of the polymeric material does not exceed 10. A tablet according to any one of claims 1 to 6, wherein the polymeric material is a polysaccharide. 25 A tablet according to any one of claims 1 to 7, wherein the tablet or a separate region thereof comprises from 0.1 to 8% by weight of said particles comprising a water-insoluble water-swellable polymer material, and from 5 to 40% by weight of said further particles to 30 disintegration. T> «• 9 9 99 99 9 9 9 9 9 9 · 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 9 99 99 99 99 99 99 A tablet according to any one of claims 1 to 8, wherein the tablet or a separate region thereof 5 contain from 0.5 to 3.5% by weight of polymeric material. Tablet according to claim 8 or 9, characterized in that the tablet or a separate region thereof contains from 8 to 25% by weight of said further disintegrating particles. A tablet according to any one of claims 1 to 10, wherein said activating detergent component in the tablet or region thereof comprises a water-insoluble activating detergent component in an amount of from 5 to 15% by weight of the tablet or said region. A tablet according to any one of claims 1 to 11, wherein the tablet comprises a plurality of discrete regions, and at least one of which comprises certain regions. 20 at least one other region of the tablet contains less or no concentration of the polymer material. A tablet according to any one of claims 1 to 11, wherein the tablet has at least two layers, the mixture in at least one of which comprises a surfactant, an activating detergent component and a polymeric material, while at least one other layer contains a lower concentration or none at all. 99 • 9 9 9 9 9 99 99 9 · - 35 γι / ΜΉ ~ ι &) - ι + 99 9900 99 99 9 9 9 9 9 • 9 9 9 9 9 9 9 9 9 9 9 9 99 9 99 99 99 99 A tablet according to any one of claims 1 to 13, characterized in that the tablet generally comprises 5 to 60% by weight of a water insoluble activating detergent component. A tablet according to any one of claims 1 to 13, characterized in that the tablet generally comprises 10 to 80% by weight of a water-soluble activating detergent component. A tablet according to any one of claims 1 to 15, characterized in that the tablet generally comprises 15 to 49% by weight of a surfactant. A process for the manufacture of a detergent tablet according to any one of claims 1 to 16, comprising mixing the water-insoluble water-swellable 20 polymeric material and particles comprising at least 40% (by weight of these particles) of one or more materials selected from the group consisting of * compounds having a solubility in deionized water at 20 ° C of at least 50 grams per 100 grams of water, 25 * Phase I sodium tripolyphosphate, * Sodium tripolyphosphate partially hydrated, to contain water of hydration in an amount of at least 0.5% by weight of sodium tripolyphosphate in these particles, with other particulate components to form A particulate detergent composition comprising a surfactant - 36 r-Íf-yjLL · * 99 9 · 9999 99 99 * 999 99 9,999 9 9,999 9 9 9 9 9 9 9 9,999,999,999,999 9 9 99 9 9 99 9 99 99 99 99 99 99 of an agent and an activating detergent component, and compressing a certain amount of the particulate composition in a mold so as to form 5 tablet or tablet area. The method of claim 17, wherein the water-swellable polymer material is added to the other particulate components as particles comprising at least 75 10% by their own weight of this polymeric material.