EP0839906B1 - Composition détergente - Google Patents

Composition détergente Download PDF

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Publication number
EP0839906B1
EP0839906B1 EP97308608A EP97308608A EP0839906B1 EP 0839906 B1 EP0839906 B1 EP 0839906B1 EP 97308608 A EP97308608 A EP 97308608A EP 97308608 A EP97308608 A EP 97308608A EP 0839906 B1 EP0839906 B1 EP 0839906B1
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EP
European Patent Office
Prior art keywords
particles
sodium tripolyphosphate
tablet
weight
detergent
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EP97308608A
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German (de)
English (en)
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EP0839906A1 (fr
Inventor
François Delwel
James William Gordon
Henning Wagner
Jelles Vincent Boskamp
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Unilever PLC
Unilever NV
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Unilever PLC
Unilever NV
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Publication of EP0839906A1 publication Critical patent/EP0839906A1/fr
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0078—Multilayered tablets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0086—Laundry tablets

Definitions

  • This invention relates to cleaning compositions in the form of tablets, e.g. for use in fabric washing.
  • Detergent compositions in tablet form are described, for example, in GB 911204 (Unilever), US 3953350 (Kao), JP 60-015500A (Lion), JP 60-135497A (Lion) and JP 60-135498A (Lion); and are sold commercially in Spain. Tablets have several advantages over powdered products: they do not require measuring and are thus easier to handle and dispense into the washload, and they are more compact, hence facilitating more economical storage.
  • Detergent tablets are generally made by compressing or compacting a detergent powder, which includes detergent active and detergency builder. It is desirable that tablets have adequate strength when dry, yet disperse and dissolve quickly when added to wash water. Detergent included in such tablets functions as a binder for other solids.
  • Sodium tripolyphosphate is very well known as a sequestering builder in detergent compositions.
  • phase II which is the low temperature form
  • phase I which is stable at high temperature.
  • the conversion of phase II to phase I proceeds fairly rapidly on heating above the transition temperature, which is about 420°C, but the reverse reaction is slow. Consequently phase I sodium tripolyphosphate is metastable at ambient temperature.
  • Phase I material is known to hydrate to the hexahydrate more rapidly than phase II material. It is also known to dissolve somewhat more rapidly when there is no obstacle to dispersion in the solution. However, during dissolution, this phase I material can form a viscous or solid mass which, in a confined space can hinder dissolution. For instance when making a slurry for spray drying, phase I tripolyphosphate can form so-called "grit", which is a mass of interlocked crystals.
  • GB-A-1375131 includes a comparison of the dissolution of sodium tripolyphosphate samples containing 38% and 75% phase I material. Each also contained 5% water of hydration. The sample with 38% of phase I sodium tripolyphosphate dissolved very slightly faster, but both formed a viscous mass during dissolution. A sample with 4% phase I and 12% water of hydration dissolved even more slowly. This document teaches that a powdered dishwasher composition should contain partially hydrated sodium tripolyphosphate with a phase I content which is between 4 and 14% of the anhydrous tripolyphosphate.
  • EP-A-178986 teaches that sodium tripolyphosphate intended for incorporation into a spray-dried detergent powder should have over 50% phase I material, with some water of hydration present.
  • US-A-4362641 teaches that granular sodium tripolyphosphate for a dishwasher composition should contain some phase I material to enhance absorption of free water during manufacture and packing.
  • EP-A-219314 and EP-A-220024 teach that phase I anhydrous tripolyphosphate should be avoided in a spray-dried component of a particulate detergent composition which is formulated to dissolve rapidly.
  • any material incorporated as an aid to dissolution should have high solubility and should not impede contact with water by the formation of a poorly mobile mass which could block pores in the tablet.
  • DE-A-1467595 discloses tablets containing tripolyphosphate of phase 1 form having a water of hydration content of 0.2 to 2% preferably 0.3 to 0.8% by weight.
  • the tripolyphosphate has a water of hydration content of 0.5% by weight and a particle size distribution such that 90% was in a size range from 100 ⁇ m to 400 ⁇ m and 70% in a range from 200 ⁇ m to 400 ⁇ m.
  • this invention provides a tablet of compacted particulate detergent composition, containing one or more detergent-active compounds together with sodium tripolyphosphate and other ingredients, wherein the tablet or a region thereof comprises particles which contain sodium tripolyphosphate with a content of the phase I form which is more than 40% by weight of the sodium tripolyphosphate in the said particles, wherein the sodium tripolyphosphate in said particles contains water of hydration distributed throughout the tripolyphosphate in an amount of more than 2% and less than 5% by weight of the sodium tripolyphosphate in the particles.
  • These particles may contain sodium tripolyphosphate as their only ingredient, or at least as a high proportion of the particles, such as at least 80% or 90% by weight. However, it is conceivable that they could contain sodium tripolyphosphate mixed with some other constituent of the overall tablet composition.
  • a tablet of the invention may be either homogeneous or heterogeneous.
  • the term “homogeneous” is used to mean a tablet produced by compaction of a single particulate composition, but does not imply that all the particles of that composition will necessarily be of identical composition.
  • the term “heterogeneous” is used to mean a tablet consisting of a plurality of discrete regions, for example layers, inserts or coatings, each derived by compaction from a particulate composition.
  • the composition within the tablet, or region thereof will contain one or more detergent active compounds together with other detergent ingredients.
  • the tablet or region thereof may contain further particles which include detergent, such as a spray dried or granulated detergent composition, plus the said particles containing phase I sodium tripolyphosphate, possibly accompanied by additional particulate ingredients of the overall composition. It is a feature of this invention that the quantity of the particles containing phase I sodium tripolyphosphate can be less than the quantity of the particles which include detergent.
  • the invention provides a tablet of compacted particulate detergent composition, containing one or more detergent-active compounds together with sodium tripolyphosphate and other ingredients, wherein the tablet or a region thereof comprises:
  • this invention provides processes of making tablets by mixing particles as above which contain sodium tripolyphosphate with other material so as to form a particulate detergent composition and compacting the composition to form a tablet or region thereof.
  • sodium tripolyphosphate can be converted to the phase I form by heating to above the transition temperature at which phase II anhydrous sodium polyphosphate is transformed into the phase I form.
  • a process for the manufacture of particles containing a high proportion of the phase I form of sodium tripolyphosphate by spray drying below 420°C is given in US-A-4536377.
  • Suitable material is commercially available. Suppliers include Rhone-Poulenc, Courbevoie, France and Albright & Wilson, Warley, West Midlands, UK.
  • the sodium tripolyphosphate should be partially hydrated, but the phase I anhydrous form should also be present.
  • the sodium tripolyphosphate in the particles contains more than 2% and less than 5% (by weight of the sodium tripolyphosphate in these particles) of water of hydration.
  • the extent of hydration is desirably more than 2% to 4%.
  • the sodium tripolyphosphate in these particles is preferably hydrated by a process which leads to a homogeneous distribution of the water of hydration within the tripolyphosphate.
  • the particles preferably consist solely of sodium tripolyphosphate with a high content of the phase I form.
  • the particles preferably contain sodium tripolyphosphate in a porous form so as to have high surface area.
  • a blowing agent that is a compound such as ammonium carbonate which decomposes to yield a gas during the course of the spray drying. This gives the dried material a higher surface area than hollow beads of tripolyphosphate obtained without blowing agent.
  • the particles which contain or consist of sodium tripolyphosphate preferably have a small mean particle size, such as not over 300 ⁇ m, better not over 250 ⁇ m. Small particle size can if necessary be achieved by grinding.
  • Rhodiaphos HPA 3.5 is a grade of sodium tripolyphosphate from Rhone-Poulenc which has been found to be particularly suitable. It consists of porous particles of small particle size (mean size below 250 ⁇ m) with 70% phase I and prehydrated with 3.5% water of hydration.
  • the said particles containing sodium tripolyphosphate with more than 40% of phase I material provide this phase I tripolyphosphate as at least 3%, better at least 8% by weight of the tablet or region thereof. More preferably they provide sodium tripolyphosphate, including the phase I tripolyphosphate, in a quantity which is from 12% up to 30% or 35% by weight of the tablet or region thereof. A quantity of at least 25% has been found useful in some tablets.
  • the remainder of the tablet composition may include additional sodium tripolyphosphate.
  • additional sodium tripolyphosphate This may be in any form, including anhydrous sodium tripolyphosphate with a high content of the phase II form, hydrated sodium tripolyphosphate or some combination of the two.
  • the total quantity of sodium tripolyphosphate, in all forms, present in the tablet composition will generally lie in a range from 15% to 60% by weight of the tablet. Therefore it will be appreciated that the overall quantity of sodium tripolyphosphate may be provided at least partially by other material in addition to the said particles.
  • Tablet compositions of this invention generally contain one or more organic detergent-active compounds. Preferably these provide from 5% to 50% by weight of the composition of the overall tablet or of a region thereof, more preferably from 8% or 9% by weight of the composition up to 40% or 50% by weight.
  • Organic detergent-active compounds may be anionic (soap or non-soap), cationic, zwitterionic, amphoteric, nonionic or a combination of these, especially combinations of non-soap anionic, nonionic and possibly soap.
  • Anionic detergent-active compounds may be present in an amount from 0.5% to 50% by weight, preferably from 2% or 4% up to 30% or 40% by weight of the composition of the tablet or of a tablet region.
  • Synthetic (i.e. non-soap) anionic surfactants are well known to those skilled in the art.
  • alkylbenzene sulphonates particularly sodium linear alkylbenzene sulphonates having an alkyl chain length of C 8 -C 15 ; olefin sulphonates; alkane sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.
  • Linear alkyl benzene sulphonate of the formula where R is linear alkyl of 8 to 15 carbon atoms and M + is a solubilising cation, especially sodium, is also a commercially significant anionic detergent active.
  • such linear alkyl benzene sulphonate or primary alkyl sulphate of the formula above, or a mixture thereof will be the desired anionic detergent and may provide 75 to 100 wt % of any anionic non-soap detergent in the composition.
  • the amount of non-soap anionic detergent lies in a range from 5 wt % to 15 wt % of the composition of the tablet or a tablet region.
  • soaps of fatty acids are preferably sodium soaps derived from naturally occurring fatty acids, for example, the fatty acids from coconut oil, beef tallow, sunflower or hardened rapeseed oil.
  • Suitable nonionic detergent compounds which 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 alkyl phenols with alkylene oxides, especially ethylene oxide ether alone or with propylene oxide.
  • nonionic detergent compounds are alkyl (C 8-22 ) phenol-ethylene oxide condensates, the condensation products of linear or branched aliphatic C 8-20 primary or secondary alcohols with ethylene oxide, and products made by condensation of ethylene oxide with the reaction products of propylene oxide and ethylene-diamine.
  • Other nonionic detergent compounds include alkyl polyglycosides, long-chain amine oxides, tertiary phosphine oxides, and dialkyl sulphoxides.
  • the primary and secondary alcohol ethoxylates especially the C 9-11 and C 12-15 primary and secondary alcohols ethoxylated with an average of from 3 or 5 moles to 20 moles of ethylene oxide per mole of alcohol.
  • the amount of nonionic detergent lies in a range from 4% to 40%, better 4% or 5% to 30% by weight of the composition of the tablet or a tablet region.
  • nonionic detergent-active compounds are liquids. These may be absorbed onto particles of the composition.
  • composition of a tablet or of a region of a tablet will generally contain from 15% to 80%, more usually 15% to 60% by weight of detergency builder. This may be provided solely by sodium tripolyphosphate, or part of it may be provided by other material with water-softening properties.
  • Watersoluble builders may be organic or inorganic.
  • Inorganic builders that may be present include alkali metal (generally sodium) carbonate; while organic builders include polycarboxylate polymers, such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphonates, monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono- di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates and hydroxyethyliminodiacetates.
  • alkali metal generally sodium
  • organic builders include polycarboxylate polymers, such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphonates, monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono- di- and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates and
  • Tablets may include polycarboxylate polymers, more especially polyacrylates and acrylic/maleic copolymers which can function as builders and also inhibit unwanted deposition onto fabric from the wash liquor.
  • composition which is compacted into tablets or regions thereof contains
  • the particles (ii) may be present in a quantity which is greater than the quantity of particles (i). It is a feature of this invention that particles (i) give effective disintegration even under these circumstances.
  • a composition is required to include nonionic detergent, this is preferably incorporated in particles (ii) along with anionic detergent. It is preferred that particles (i) are substantially free of organic detergent compounds (ie contain less than 5% of their own weight of detergent, better none at all).
  • Incorporating the detergent active into further particles (ii) together with other ingredients has the advantage that these and other particles in the composition can form a reasonably free flowing particulate composition, which is useful for handling prior to compaction into tablet form.
  • the particles (ii) may be made by conventional methods for the manufacture of particulate detergent compositions such as spray drying or granulation.
  • Tablets of this invention may include an organic water-soluble polymer, applied as a coating to some of the constituent particles, and serving as a binder when the particles are compacted into tablets.
  • This polymer may be a polycarboxylate such as those mentioned above.
  • such a binder material should melt at a temperature of at least 35°C, better 40°C or above, which is above ambient temperatures in many temperate countries.
  • the melting temperature is somewhat above 40°C, so as to be above the ambient temperature.
  • the melting temperature of the binder material should be below 80°C.
  • Preferred binder materials are synthetic organic polymers of appropriate melting temperature, especially polyethylene glycol.
  • Polyethylene glycol of average molecular weight 1500 melts at 45°C and has proved suitable.
  • Polyethylene glycol of higher molecular weight notably 4000 or 6000, can also be used.
  • the binder may suitably be applied to the particles by spraying, e.g. as a solution or dispersion. If used, the binder is preferably used in an amount within the range from 0.1% to 10% by weight of the tablet composition, more preferably the amount is at least 1% or even at least 3% by weight of the tablets. Preferably the amount is not over 8% or even 6% by weight unless the binder serves some other additional function.
  • Tablets may include other ingredients which aid tableting.
  • Tablet lubricants include calcium, magnesium and zinc soaps (especially stearates), talc, glyceryl behapate, sugar Myvatex (Trade Mark) TL ex-Eastman Kodak, polyethylene glycols, and colloidal silicas (for example, Alusil (Trade Mark) ex-Crosfield Chemicals Ltd).
  • Tableted detergent compositions according to the invention may contain a bleach system.
  • This preferably comprises one or more peroxy bleach compounds, for example, inorganic persalts or organic peroxyacids, which may be employed in conjunction with activators to improve bleaching action at low wash temperatures. If any peroxygen compound is present, the amount is likely to lie in a range from 10% to 25% by weight of the composition.
  • Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate, advantageously employed together with an activator.
  • Bleach activators also referred to as bleach precursors
  • Preferred examples include peracetic acid precursors, for example, tetraacetylethylene diamine (TAED), now in widespread commercial use in conjunction with sodium perborate; and perbenzoic acid precursors.
  • TAED tetraacetylethylene diamine
  • perbenzoic acid precursors perbenzoic acid precursors.
  • the quaternary ammonium and phosphonium bleach activators disclosed in US 4751015 and US 4818426 are also of interest.
  • bleach activator which may be used, but which is not a bleach precursor, is a transition metal catalyst as disclosed in EP-A-458397, EP-A-458398 and EP-A-549272.
  • a bleach system may also include a bleach stabiliser (heavy metal sequestrant) such as ethylenediamine tetramethylene phosphonate and diethylenetriamine pentamethylene phosphonate.
  • a bleach is present and is a water-soluble inorganic peroxygen bleach, the amount may well be from 10% to 25% by weight of the composition.
  • the detergent tablets of the invention may also contain one of the detergency enzymes well known in the art for their ability to degrade and aid in the removal of various soils and stains.
  • Suitable enzymes include the various proteases, cellulases, lipases, amylases, and mixtures thereof, which are designed to remove a variety of soils and stains from fabrics.
  • suitable proteases are Maxatase (Trade Mark), as supplied by Gist-Brocades N.V., Delft, Holland, and Alcalase (Trade Mark), and Savinase (Trade Mark), as supplied by Novo Industri A/S, Copenhagen, Denmark.
  • Detergency enzymes are commonly employed in the form of granules or marumes, optionally with a protective coating, in amount of from about 0.1% to about 3.0% by weight of the composition; and these granules or marumes present no problems with respect to compaction to form a tablet.
  • the detergent tablets of the invention may also contain a fluorescer (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) stilbene disulphonate
  • Tinopal CBS is disodium 2,2'-bis-(phenylstyryl) disulphonate.
  • An antifoam material is advantageously included, especially if the detergent tablet is primarily intended for use in front-loading drum-type automatic washing machines.
  • Suitable antifoam materials are usually in granular form, such as those described in EP 266863A (Unilever).
  • Such antifoam granules typically comprise a mixture of silicone oil, petroleum jelly, hydrophobic silica and alkyl phosphate as antifoam active material, sorbed onto a porous absorbed water-soluble carbonate-based inorganic carrier material.
  • Antifoam granules may be present in an amount up to 5% by weight of the composition.
  • a detergent tablet of the invention includes an amount of an alkali metal silicate, particularly sodium ortho-, meta- or disilicate.
  • an alkali metal silicate particularly sodium ortho-, meta- or disilicate.
  • the presence of such alkali metal silicates at levels, for example, of 0.1 wt % to 10 wt %, may be advantageous in providing protection against the corrosion of metal parts in washing machines, besides providing some measure of building and giving processing benefits in manufacture of the particulate material which is compacted into tablets.
  • ingredients which can optionally be employed in the detergent tablet of the invention include anti-redeposition agents such as sodium carboxymethylcellulose, straight-chain polyvinyl pyrrolidone and the cellulose ethers such as methyl cellulose and ethyl hydroxyethyl cellulose, fabric-softening agents; heavy metal sequestrants such as EDTA; perfumes; and colorants or coloured speckles.
  • anti-redeposition agents such as sodium carboxymethylcellulose, straight-chain polyvinyl pyrrolidone and the cellulose ethers such as methyl cellulose and ethyl hydroxyethyl cellulose, fabric-softening agents
  • heavy metal sequestrants such as EDTA
  • perfumes and colorants or coloured speckles.
  • a detergent tablet of this invention or a discrete region of such a tablet, is a matrix of compacted particles.
  • the particulate composition has an average particle size in the range from 200 ⁇ m to 2000 ⁇ m, more preferably from 250 ⁇ m to 1400 ⁇ m. Fine particles, smaller than 180 ⁇ m or 200 ⁇ m may be eliminated by sieving before tableting, if desired, although we have observed that this is not always essential.
  • the starting particulate composition may in principle have any bulk density
  • the present invention is especially relevant to tablets made by compacting powders of relatively high bulk density, because of their greater tendency to exhibit disintegration and dispersion problems.
  • Such tablets have the advantage that, as compared with a tablet derived from a low bulk density powder, a given dose of composition can be presented as a smaller tablet.
  • the starting particulate composition may suitably have a bulk density of at least 400g/litre, preferably at least 500g/litre, and advantageously at least 700g/litre.
  • Granular detergent compositions of high bulk density prepared by granulation and densification in a high-speed mixer/granulator, as described and claimed in EP 340013A (Unilever), EP 352135A (Unilever), and EP 425277A (Unilever), or by the continuous granulation/densification processes described and claimed in EP 367339A (Unilever) and EP 390251A (Unilever), are inherently suitable for use in the present invention.
  • a tablet may be either homogeneous or heterogeneous.
  • the particles with a high content of phase I sodium tripolyphosphate will preferably be distributed throughout the whole of a homogeneous tablet. However, it is possible that they will be contained within one or more discrete regions of a heterogeneous tablet, such as a layer or an insert large enough to constitute from 10% to 90% of the weight of the whole tablet. The presence of such a layer or insert could assist break up of the entire tablet when placed in water.
  • a heterogenous tablet may well contain overall the abovementioned proportions of from 5 to 50 wt% detergent active and from 10 or 15 to 80 wt% detergency builder.
  • Tableting entails compaction of a particulate composition.
  • a variety of tableting machinery is known, and can be used. Generally it will function by stamping a quantity of the particulate composition which is confined in a die.
  • Tableting may be carried out at ambient temperature or at a temperature above ambient which may allow adequate strength to be achieved with less applied pressure during compaction.
  • the particulate composition is preferably supplied to the tableting machinery at an elevated temperature. This will of course supply heat to the tableting machinery, but the machinery may be heated in some other way also.
  • any heat is supplied, it is envisaged that this will be supplied conventionally, such as by passing the particulate composition through an oven, rather than by any application of microwave energy.
  • the size of a tablet will suitably range from 10 to 160 grams, preferably from 15 to 60 g, depending on conditions of intended use, and whether it represents a dose for an average load in a fabric washing or dishwashing machine or a fractional part of such a dose.
  • Tablets may be of any shape. However, for ease of packaging they are preferably blocks of substantially uniform cross-section, such as cylinders or cuboids.
  • Overall density of a tablet preferably lies in a range from 1040 or 1050 grams per litre up to 1300 gm/litre. The tablet density may well lie in a range up to no more than 1250 or even 1200 gm/litre.
  • Tablets for use in fabric washing were made, starting with a spray-dried base powder of the following composition: Sodium linear alkylbenzene sulphonate 11.83% Sodium tripolyphosphate, type 1A 44.83% Nonionic detergent 7.88% Sodium silicate 11.83% Soap 1.13% Sodium carboxymethyl cellulose 0.90% Acrylate/maleate copolymer 3.20% Sodium sulphate and minor ingredients 3.00% Water balance to 100%
  • This powder was mixed with particles of porous sodium tripolyphosphate specified to contain 70% phase I form and contain 3.5% water of hydration (Rhodia-Phos HPA 3.5 from Rhone-Poulenc) and other detergent ingredients as tabulated below.
  • the base powder was mixed with urea and other detergent ingredients.
  • Example 1 Comparative A Base powder 63.25 63.25 Sodium perborate tetrahydrate 10.40 10.40 Tetraacetylethylenediamine (TAED) granules 4.00 4.00 Anti-foam granule 2.00 2.00 Enzymes 0.85 0.85 Phosphonate 0.50 0.50 Sodium carbonate 3.60 3.60 HPA sodium tripolyphosphate 15.00 None Urea None 15.00 35g portions of each composition were made into cylindrical tablets of 44mm diameter, using a Carver hand press.
  • TAED Tetraacetylethylenediamine
  • the break-up, dispersion and dissolution of tablets was measured by a test procedure in which a tablet is placed on a plastic sieve with 2mm mesh size which was immersed in 9 litres of demineralised water at ambient temperature of 22°C and rotated at 200rev/min. The water conductivity was monitored until it reached a constant value.
  • Tablets embodying the invention and comparative tablets were prepared with a formulation as follows:- Ingredient % by weight Base powder 62.00 Sodium perborate tetrahydrate 12.60 TAED granules 3.00 Antifoam granule 2.00 Enzymes 0.85 Phosphonate 0.50 Perfume 0.45 Variable, soluble ingredient 18.60
  • variable, soluble ingredient Various soluble materials were used as the variable, soluble ingredient, as set out in the table below. Tablets were made as in Example 1, using varying levels of compaction force. The resulting DFS and T 90 values are also given in the table below: Variable Soluble Ingredient Compaction force (kN) DFS (kPa) T 90% dissolution (minutes) HPA (high phase I) 2.0 11.0 4.55 3.0 16.0 5.00 4.0 24.7 9.00 Empiphos D (low phase I) 2.0 6.0 7.00 3.0 11.4 16.00 Empiphos E (high phase I) 4.0 20.0 7.00 Urea 2.0 14.8 4.55 3.0 25.2 8.00 Na-sulphate fine granular 2.0 10.4 18.90 HPA grade sodium tripolyphosphate (as used also in Example 1) is specified to contain 70% of phase I, and to contain 3.5% water of hydration.
  • Empiphos D available from Albright & Wilson, has a very high content of phase II tripolyphosphate.
  • the content of phase I is 10% and the water content is 0.2%.
  • Empiphos E available from Albright & Wilson is specified as having 50% of phase I, and to contain 1% water of hydration.
  • HPA according to the invention enhances dissolution, compared to similar comparative tablets containing sodium sulphate and Empiphos D or E. Unlike urea, it functions as a detergency builder in the wash liquor.
  • Tablets were prepared with the following three formulations in which different types of sodium tripolyphosphate were used: INGREDIENT % BY WEIGHT EXAMPLE NO. 3A 3B 3C Base powder as above 45 45 45 Sodium percarbonate 15 15 15 Tetraacetyethylenediamine (TAED) granules 4 4 4 Antifoam granules 2 2 2 Perfume, enzymes and other ingredients 4 4 4 HPA sodium tripolyphosphate 70% phase I; 3.5% water of hydration 30 0 0 Thermphos NW tripolyphosphate 84% phase I; no water of hydration 0 30 0 Thermphos NW tripolyphosphate 84% phase I; 3.5% water of hydration 0 0 30
  • Thermphos NW available from Hoechst, was used in grades containing 84% phase I and either 3.5% water of hydration or no water of hydration.

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Claims (14)

  1. Pastille de composition détergente particulaire compactée contenant un ou plusieurs composés détergents actifs avec du tripolyphosphate de sodium et d'autres ingrédients, dans laquelle la pastille ou une région de celle-ci comprend des particules qui contiennent du tripolyphosphate de sodium avec une teneur en la forme de phase I qui est supérieure à 40 % sur la base du poids du tripolyphosphate de sodium dans lesdites particules, dans laquelle le tripolyphosphate de sodium dans lesdites particules contient de l'eau d'hydratation distribuée dans tout le tripolyphosphate dans une quantité supérieure à 2 % et inférieure à 5 % en poids-du tripolyphosphate de sodium dans les particules.
  2. Pastille selon la revendication 1, dans laquelle le tripolyphosphate de sodium dans lesdites particules a une teneur en la forme en phase 1 qui est d'au moins 50 % en poids par rapport au poids du tripolyphosphate de sodium dans lesdites particules.
  3. Pastilles selon l'une quelconque des revendications précédentes, dans laquelle la quantité de ladite eau d'hydratation est supérieure à de 2 % à 4 % en poids du poids du tripolyphosphate de sodium dans les particules.
  4. Pastille selon l'une quelconque des revendications précédentes, dans laquelle le tripolyphosphate dans lesdites particules est poreux.
  5. Pastille selon l'une quelconque des revendications précédentes, dans laquelle le tripolyphosphate dans lesdites particules s'hydrate à un niveau d'au moins 90 % de son état totalement hydraté en une minute lorsque lesdites particules entrent en contact avec de l'eau à 80°C.
  6. Pastille selon l'une quelconque des revendications précédentes, dans laquelle le tripolyphosphate de sodium dans lesdites particules constitue de 12 % à 35 % en poids de la pastille ou d'une région de celle-ci.
  7. Pastille selon l'une quelconque des revendications précédentes, dans laquelle la pastille ou une région de celle-ci contient également d'autres particules, qui contiennent un actif détergent mélangé avec d'autres matériaux, ces autres particules étant présentes en quantité plus importante que lesdites premières particules contenant du tripolyphosphate.
  8. Pastille de composition détergente particulaire compactée contenant un ou plusieurs composés détergents actifs avec du tripolyphosphate de sodium et d'autres ingrédients, dans laquelle la pastille ou une région de celle-ci comprend :
    (i) des particules qui contiennent le tripolyphosphate de sodium avec une teneur en la forme en phase I qui est supérieure à 40 % en poids du poids du tripolyphosphate de sodium dans lesdites particules, dans lesquelles le tripolyphosphate de sodium dans lesdites particules contient de l'eau d'hydratation dans une quantité supérieure à 2 % et inférieure à 5 % en poids par rapport au poids du tripolyphosphate de sodium dans les particules ; et
    (ii) d'autres particules qui contiennent le détergent actif mélangé avec d'autres matériaux, ces autres particules étant présente dans une quantité supérieure à celle desdites premières particules contenant le tripolyphosphate.
  9. Pastille selon la revendication 7 ou la revendication 8, dans laquelle lesdites premières particules contenant le tripolyphosphate ne contiennent substantiellement pas de détergent actif organique de telle sorte qu'elle ne contiennent pas plus de 5 % de leur propre poids de détergent actif organique, et de préférence elle n'en contiennent pas du tout.
  10. Pastille selon l'une quelconque des revendications 7 à 9, dans laquelle lesdites autres particules contenant le détergent contiennent à la fois du détergent actif anionique et du détergent actif non ionique, avec du tripolyphosphate de sodium.
  11. Pastille selon l'une quelconque des revendications précédentes, dans laquelle la pastille ou une région de celle-ci contient de 5 % à 50 % en poids de détergent actif organique et de 10 % à 80 % en poids d'un édificateur de détergence incluant le tripolyphosphate de sodium.
  12. Pastille selon l'une quelconque des revendications précédentes, dans laquelle la pastille ou une région de celle-ci contient de 2 % à 30 % en poids d'un polycarboxylate soluble dans l'eau.
  13. Procédé de fabrication d'une pastille selon l'une quelconque des revendications précédentes, comprenant le fait de mélanger :
    (a) des particules qui contiennent du tripolyphosphate de sodium avec une teneur en la forme en phase I qui est supérieure à 40 % en poids du poids du tripolyphosphate de sodium dans lesdites particules, dans lesquelles le tripolyphosphate de sodium dans lesdites particules contient de l'eau d'hydratation dans une quantité supérieure à 2 % et inférieure à 5 % en poids du tripolyphosphate de sodium dans les particules, avec
    (b) d'autres matériaux afin de former une composition détergente particulaire et
    de mélanger la composition afin de former une pastille ou une région de celle-ci.
  14. Procédé de fabrication d'une pastille selon l'une quelconque des revendications 8 à 11, comprenant le fait de mélanger :
    (a) des particules qui contiennent du tripolyphosphate de sodium avec une teneur en la forme en phase I qui est supérieure à 40 % en poids du poids du tripolyphosphate de sodium dans lesdites particules, dans lesquelles le tripolyphosphate de sodium dans lesdites particules contient de l'eau d'hydratation dans une quantité supérieure à 2 % et inférieure à 5 % en poids du tripolyphosphate de sodium dans les particules ; et lesdites particules ne contenant substantiellement pas de détergent organique de telle sorte qu'elles contiennent moins de 5 % de leur propre poids de détergent organique, et de préférence qu'elles n'en contiennent pas du tout, avec une quantité plus grande de :
    (b) d'autres particules qui contiennent un détergent actif mélangé avec d'autres matériaux afin de former une composition détergente particulaire, et
    le fait de compacter cette composition afin de former une pastille ou une région de celle-ci.
EP97308608A 1996-11-01 1997-10-28 Composition détergente Expired - Lifetime EP0839906B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9622864A GB2318800A (en) 1996-11-01 1996-11-01 Detergent composition
GB9622864 1996-11-01

Publications (2)

Publication Number Publication Date
EP0839906A1 EP0839906A1 (fr) 1998-05-06
EP0839906B1 true EP0839906B1 (fr) 2004-01-14

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EP97308608A Expired - Lifetime EP0839906B1 (fr) 1996-11-01 1997-10-28 Composition détergente

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BR (1) BR9705211A (fr)
DE (1) DE69727189T2 (fr)
ES (1) ES2213806T3 (fr)
GB (1) GB2318800A (fr)
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Families Citing this family (13)

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Publication number Priority date Publication date Assignee Title
GB9711829D0 (en) 1997-06-06 1997-08-06 Unilever Plc Detergent compositions
ZA984570B (en) 1997-06-06 1999-11-29 Unilever Plc Cleaning compositions.
DE69806406T3 (de) * 1997-10-22 2011-05-05 Unilever N.V. Tablettenförmige waschmittelzusammensetzungen
ES2214844T3 (es) * 1998-02-10 2004-09-16 Unilever N.V. Composiciones de detergente en pastillas.
GB9821190D0 (en) * 1998-09-30 1998-11-25 Unilever Plc Detergent composition
FR2784392B1 (fr) * 1998-10-09 2000-11-17 Rhodia Chimie Sa Tablettes de composition detergente ou anticalcaire et leur mise en oeuvre en lave-vaisselle ou lave-linge
GB9826105D0 (en) * 1998-11-27 1999-01-20 Unilever Plc Detergent compositions
GB9826097D0 (en) 1998-11-27 1999-01-20 Unilever Plc Detergent compositions
DE19859807A1 (de) * 1998-12-23 2000-06-29 Henkel Kgaa Phosphat-Compounds
WO2001002524A1 (fr) * 1999-06-29 2001-01-11 Unilever Plc Composition pour lave-vaisselle
DE10129228B4 (de) * 2001-06-19 2006-03-02 Henkel Kgaa Gelbildung verhindernde Zusätze zu Tensiden und Waschmittelformulierungen und ihre Anwendung in Wasch-und Reinigungsmitteln
US8252122B2 (en) 2009-03-17 2012-08-28 Bbt Bergedorfer Biotechnik Gmbh Use of an agent that contains carbamide and/or at least a derivative thereof as a cleaning agent
ES2379917B1 (es) 2010-10-06 2012-12-26 Jordi Caparros Casco Composiciones detergentes.

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DE1467595A1 (de) * 1963-05-02 1969-01-09 Henkel & Cie Gmbh Waschmitteltabletten und Verfahren zu deren Herstellung

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Publication number Priority date Publication date Assignee Title
BE632423A (fr) * 1962-05-17
CH471891A (de) * 1963-12-31 1969-04-30 Unilever Nv Verfahren zur Herstellung einer Reinigungsmitteltablette
CA812195A (en) * 1964-07-24 1969-05-06 Fmc Corporation Cleaning tablets
ZA663029B (fr) * 1965-06-25
CA789508A (en) * 1965-10-22 1968-07-09 United States Borax And Chemical Corporation Detergent compositions
US4362641A (en) * 1980-03-12 1982-12-07 Occidental Chemical Corporation Composition of an STPP product for dishwasher detergent formulations and method of preparation
DE19502774A1 (de) * 1995-01-27 1996-08-01 Henkel Kgaa Verfahren zur Herstellung von bruchstabilen Reinigungstabletten

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
DE1467595A1 (de) * 1963-05-02 1969-01-09 Henkel & Cie Gmbh Waschmitteltabletten und Verfahren zu deren Herstellung

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Publication number Publication date
GB9622864D0 (en) 1997-01-08
GB2318800A (en) 1998-05-06
EP0839906A1 (fr) 1998-05-06
BR9705211A (pt) 1999-11-23
DE69727189D1 (de) 2004-02-19
ZA979818B (en) 1999-04-30
DE69727189T2 (de) 2004-06-17
IN189814B (fr) 2003-04-26
ES2213806T3 (es) 2004-09-01

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