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
  • 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
• • 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
  • C11D17/0082—Coated 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
  • C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
• • 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
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/2075—Carboxylic acids-salts thereof
  • C11D3/2082—Polycarboxylic acids-salts thereof
• • 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
  • C11D3/16—Organic compounds
  • C11D3/36—Organic compounds containing phosphorus
  • C11D3/361—Phosphonates, phosphinates or phosphonites
• • 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
  • C11D3/16—Organic compounds
  • C11D3/36—Organic compounds containing phosphorus
  • C11D3/364—Organic compounds containing phosphorus containing nitrogen
• • 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
  • C11D3/50—Perfumes

Definitions

• the present invention relates to perfumed detergent tablets, especially those adapted for use in washing machines, and to processes for making such tablets.
• perfumed products are well-known in the art. However, consumer acceptance of such perfumed products like laundry and cleaning products is determined not only by the performance achieved with these products but also by the aesthetics associated therewith. The perfume components are therefore an important aspect of the successful formulation of such commercial products.
• a clay mineral compound is a desirable ingredient of such laundry and cleaning product, in particular those products which are in tablet form.
• the clay can provide softening benefit but can also serve as a disintegrant of such detergent tablets.
• a problem encountered with perfumed detergent tablets containing a clay mineral compound is that the clay can have a detrimental effect on the performance of the perfume contained therein.
• the perfume is absorbed into the clay where it can interact with heavy metal ions and acid or base sites within the clay which as result may cause a discoloration of the clay. Still, the interaction between the perfume and the clay may also result in the tablet having a less attractive odour.
• a perfumed detergent tablet comprising a clay mineral compound which exhibit good perfume performance with reduced discoloration of the clay.
• GB-A-0 989 683 published on 22nd April 1965, discloses a process for preparing a particulate detergent from surfactants and inorganic salts; spraying on water- soluble silicate; and pressing the detergent particles into a solid form-retaining tablet.
• a readily water-soluble organic film-forming polymer for example, polyvinyl alcohol
• EP-A-0 716 144 published on 12th June 1996, also discloses laundry detergent tablets with water-soluble coatings which may be organic polymers including acrylic/maleic co-polymer, polyethylene glycoi, PVPVA, and sugar.
• W09518215 published on 6th July 1995, provides water-insoluble coatings for solid cast tablets.
• the tablets are provided with hydrophobic coatings including wax, fatty acid, fatty acid amides, and polyethylene glycoi.
• EP-A-0 846 754 published on the 10 th of June 1998, provides a tablet having a coating comprising a dicarboxylic acid, the coating material typically having a melting point of from 40°C to 200°C.
• EP-A-0 846 755 published on the 10 th of June 1998, provides a tablet having a coating comprising a material insoluble in water at 25°C, such as C12-C22 fatty acids, adipic acid or C8-C13 dicarboxylic acids.
• coated tablets can be provided with a coating so that they can be stored, shipped and handled without damage, the coating being easily broken when the tablet is in the washing machine, releasing the active ingredients into the wash solution.
• Typical of such disclosure can be found in pending European patent applications EP 99870017.3, EP 99870018.1 , and EP 99870019.9.
• the coating also comprises an acid having a melting point of at least 40°C, more particularly with a melting point of at least 145°C.
• the detergent formulator is also faced with the problems of providing a coated tablet having a coating which has satisfactory appearance, is sufficiently hard to protect the tablet from mechanical forces when stored, shipped and handled, and disperses readily in an aqueous solution whilst still giving satisfactory perfume performance.
• Smectite clays are disclosed in the US Patents No.s 3,862,058, 3,948,790, 3,954,632 and 4,062,647 and European Patents No.s EP-A-299,575 and EP-A-313,146 all in the name of the Procter and Gamble Company.
• Suitable smectite clays include those selected from the classes of the montmorillonites, hectorites, volchonskoites, nontronites, saponites and sauconites, particularly those having an alkali or alkaline earth metal ion within the crystal lattice structure.
• Sodium or calcium montmorillonite are particularly preferred.
• Suitable smectite clays are sold by various suppliers including English China Clays, Laviosa, Fordamin, Georgia Kaolin and Colin Stewart Minerals (CSM).
• Preferred smectite clays are sold under the tradename of White Bentonite STP by Fordamin and Detercal P7 by Laviosa Chemical Mineria SPA.
• Clays for use herein may be subjected to an acid washing treatment with any suitable mineral or organic acid. Such clays give rise to an acid pH on dissolution in distilled water.
• a commercially available "acid clay” of this type is sold under the tradename Tonsil P by Sud Chemie AG. Substitution of small cations, such as protons, sodium ions, potassium ions, magnesium ions and calcium ions, and of certain organic molecules including those having positively charged functional groups can typically take place within the crystal lattice structure of the smectite clays.
• a clay may be chosen for its ability to preferentially absorb one cation type, such ability being assessed by measurements of relative ion exchange capacity.
• the smectite clays suitable herein typically have a cation exchange capacity of at least 50 meq/100g.
• U.S. Patent No. 3,954,632 describes a method for measurement of cation exchange capacity.
• a preferred commercially available "hydrophobically activated" clay is a bentonite clay containing approximately 40% by weight of a dimethyl ditallow quaternary ammonium salt sold under the tradename Claytone EM by English China Clays International.
• the clay in the detergent composition is preferably mixed with one or more surfactants and optionally builders and optionally water, in which case the mixture is preferably subsequently dried.
• a mixture is further processed in a spray-drying method to obtain a spray dried particle comprising the clay.
• the intimate mixture comprises a chelating agent.
• the clay will preferably be present in different particles size.
• at least 50% by weight, preferably substantially all (e.g. at least 90% or 95%) by weight of the clay is present as granules.
• granules it is meant that the particles of the clay mineral compound which is present in the detergent composition are included as components of agglomerate particles optionally containing other detergent compounds.
• the term "largest particle dimension" of the clay mineral compound refers to the largest dimension of the clay mineral component as such, and not to the agglomerated particle as a whole.
• the granules will have a particle size of at least 100 micrometers, generally 100-1700 micrometers.
• the tablet is a softening tablet.
• softening tablet it is meant that the level of clay will typically be of at least 5%, preferably at least 8%, and most preferably at least 10% by weight of the tablet. The amount may be less than 25%, usually less than 20%, and preferably not more than 15% by weight of the tablet.
• the detergent compositions tablet of the invention also contains a heavy metal ion sequestrant, that being either present in the coating if present or in the detergent composition, or even in both the coating and the detergent composition, preferably, it is present in both the coating and the detergent composition or only in the detergent composition.
• heavy metal ion sequestrant it is meant herein components which act to sequester (chelate) heavy metal ions. These components may also have calcium and magnesium chelation capacity, but preferentially they show selectivity to binding heavy metal ions such as iron, manganese and copper.
• Heavy metal ion sequestrants are generally present at a level of from 0.005% to 20%, preferably from 0.1 % to 10%, more preferably from 0.25% to 7.5% and most preferably from 0.5% to 5% by weight of the tablet.
• Heavy metal ion sequestrants which are acidic in nature, having for example phosphonic acid or carboxylic acid functionalities, may be present either in their acid form or as a complex/salt with a suitable counter cation such as an alkali or alkaline metal ion, ammonium, or substituted ammonium ion, or any mixtures thereof.
• a suitable counter cation such as an alkali or alkaline metal ion, ammonium, or substituted ammonium ion, or any mixtures thereof.
• any salts/complexes are water soluble.
• the molar ratio of said counter cation to the heavy metal ion sequestrant is preferably at least 1 :1.
• Suitable heavy metal ion sequestrants for use herein include organic phosphonates, such as the amino alkylene poly (alkylene phosphonates), alkali metal ethane 1-hydroxy disphosphonates and nitrilo trimethylene phosphonates.
• diethylene triamine penta methylene phosphonate
• ethylene diamine tri methylene phosphonate
• hexamethylene diamine tetra methylene phosphonate
• hydroxy-ethylene 1 ,1 diphosphonate nitrilotriacetic acid and polyaminocarboxylic acids such as ethylenediaminotetracetic acid, ethylenetriamine pentacetic acid, ethylenediamine disuccinic acid, ethylenediamine diglutaric acid, 2-hydroxypropylenediamine disuccinic acid or any salts thereof.
• EDDS ethylenediamine-N.N'-disuccinic acid
• Preferred EDDS compounds are the free acid form and the sodium or magnesium salt or complex thereof.
• Examples of such preferred sodium salts of EDDS include Na2EDDS and Na ⁇ EDDS.
• Examples of such preferred magnesium complexes of EDDS include MgEDDS and Mg2EDDS.
• Suitable heavy metal ion sequestrants for use herein are iminodiacetic acid derivatives such as 2-hydroxyethyl diacetic acid or glyceryl imino diacetic acid, described in EP-A-317,542 and EP-A-399,133.
• the iminodiacetic acid-N-2-hydroxypropyl sulfonic acid and aspartic acid N- carboxymethyl N-2-hydroxypropyl-3-sulfonic acid sequestrants described in EP- A-516,102 are also suitable herein.
• the ⁇ -alanine-N,N'-diacetic acid, aspartic acid-N.N'-diacetic acid, aspartic acid-N-monoacetic acid and iminodisuccinic acid sequestrants described in EP-A-509,382 are also suitable.
• EP-A-476,257 describes suitable amino based sequestrants.
• EP-A-510,331 describes suitable sequestrants derived from collagen, keratin or casein.
• EP-A- 528,859 describes a suitable alkyl iminodiacetic acid sequestrant. Dipicolinic acid and 2-phosphonobutane-1 ,2,4-tricarboxylic acid are alos suitable.
• Glycinamide- N,N'-disuccinic acid (GADS), ethylenediamine-N,N'-diglutaric acid (EDDG) and 2- hydroxypropylenediamine- N.N'-disuccinic acid (HPDDS) are also suitable.
• Most preferred heavy metal ions for use herein is alkali metal ethane 1-hydroxy diphosphonates, in particular when used in combination with diethylene triamine penta (methylene phosphonate).
• the tablets of the present invention may also optionally comprise a perfume composition, that being either present in the coating if present or in the detergent composition, or even in both the coating and the detergent composition.
• Suitable perfumes herein include materials which provide an olfactory aesthetic benefit such as to make such tablets more aesthetically pleasing to the consumer, imparting a pleasant fragrance to fabrics treated therewith and/or cover any "chemical" odor that the product may have.
• perfume includes fragrant substance or mixture of substances including natural (i.e., obtained by extraction of flowers, herbs, leaves, roots, barks, wood, blossoms or plants), artificial (i.e., a mixture of different nature oils or oil constituents) and synthetic (i.e., synthetically produced) odoriferous substances.
• natural i.e., obtained by extraction of flowers, herbs, leaves, roots, barks, wood, blossoms or plants
• artificial i.e., a mixture of different nature oils or oil constituents
• synthetic i.e., synthetically produced
• perfumes are complex mixtures of a plurality of organic compounds.
• perfume ingredients useful in the perfume compositions include, but are not limited to, hexyl cinnamic aldehyde; amyl cinnamic aldehyde; amyl salicylate; hexyl salicylate; terpineol; 3,7-dimethyl-c/s-2,6-octadien-1-ol; 2,6- dimethyl-2-octanol; 2,6-dimethyl-7-octen-2-ol; 3,7-dimethyl-3-octanol; 3,7- dimethyl-frans-2,6-octadien-1-ol; 3,7-dimethyl-6-octen-1-ol; 3,7-dimethyl-l- octanol; 2-methyl-3-(para-tert-butylphenyl)-propionaldehyde; 4-(4-hydroxy-4- methylpentyl)-3-cyclohexene-1 -carboxaldehyl
• fragrance materials include, but are not limited to, orange oil; lemon oil; grapefruit oil; bergamot oil; clove oil; dodecalactone gamma; methyl-2-(2-pentyl-3-oxo-cyclopentyl) acetate; beta-naphthol methylether; methyl-beta-naphthylketone; coumarin; decylaldehyde; benzaldehyde; 4-tert- butylcyclohexyl acetate; alpha, alpha-dimethylphenethyl acetate; methylphenylcarbinyl acetate; cyclic ethyleneglycol diester of tridecandioic acid; 3,7-dimethyl-2,6-octadiene-1-nitrile; ionone gamma methyl; ionone alpha; ionone beta; petitgrain; methyl cedrylone; 7-acetyl-1 , 2,3,
• perfume components are geraniol; geranyl acetate; linalool; linalyl acetate; tetrahydrolinalool; citronellol; citronellyl acetate; dihydromyrcenol; dihydromyrcenyl acetate; tetrahydromyrcenol; terpinyl acetate; nopol; nopyl acetate; 2-phenylethanol; 2-phenylethyl acetate; benzyl alcohol; benzyl acetate; benzyl salicylate; benzyl benzoate; styrallyl acetate; dimethylbenzylcarbinol; trichloromethylphenylcarbinyl methylphenylcarbinyl acetate; isononyl acetate; vetiveryl acetate; vetiverol; 2-methyl-3-(p-tert-butylphenyl)-propanal; 2-methyl-3-(
• the perfumes useful in the present invention compositions are substantially free of halogenated materials and nitromusks.
• the perfume composition contains less than 0.6% by weight of the perfume composition of Schiff-base.
• the perfume for use herein is used at levels of up to 5 grams per tablet and preferably is substantially free of Schiff-Base.
• the perfume composition comprises less than 0.4 % by weight of Schiff Base, and more preferably is free of Schiff base.
• Schiff-Bases are the condensation of an aldehyde perfume ingredient with an anthranilate. A typical description can be found in US 4853369.
• the Schiff Bases can be added directly to the perfume composition or can be formed in situ in the perfume composition by adding to it an Anthranilate such as Methyl or Ethyl Anthranilate along with an aldehyde which can react with the Anthranilate to form the Schiff Base.
• an Anthranilate such as Methyl or Ethyl Anthranilate along with an aldehyde which can react with the Anthranilate to form the Schiff Base.
• Typical of Schiff bases are selected from Schiffs base of 4-(4-hydroxy-4- methylpentyl)-3-cyclohexene-1-carboxaldehyde and methyl anthranilate; condensation products of: hydroxycitronellal and methyl anthranilate; 4-(4- hydroxy-4-methyl pentyl)-3-cyclohexene-1-carboxaldehyde and methyl anthranilate; Methyl Anthranilate and Hydroxycitronellal commercially available under the tradename Aurantiol; Methyl Anthranilate and Methyl Nonyl Acetaldehyde commercially available under the tradename Agrumea; Methyl Anthranilate and PT Bucinal commercially available under the tradename Verdantiol; Methyl anthranilate and Lyral commercially available under the tradename Lyrame; Methyl Anthranilate and Ligustral commercially available under the tradename Ligantral; and mixtures
• the perfume composition is free of perfume ingredients selected from Methyl Anthranilate and Hydroxycitronellal commercially available under the tradename Aurantiol; Methyl Anthranilate and Methyl Nonyl Acetaldehyde commercially available under the tradename Agrumea; Methyl Anthranilate and PT Bucinal commercially available under the tradename Verdantiol; Methyl anthranilate and Lyral commercially available under the tradename Lyrame; Methyl Anthranilate and Ligustral commercially available under the tradename Ligantral; and mixtures thereof.
• perfume ingredients selected from Methyl Anthranilate and Hydroxycitronellal commercially available under the tradename Aurantiol; Methyl Anthranilate and Methyl Nonyl Acetaldehyde commercially available under the tradename Agrumea; Methyl Anthranilate and PT Bucinal commercially available under the tradename Verdantiol; Meth
• Suitable solvents, diluents or carriers for perfumes ingredients mentioned above are for examples, ethanol, isopropanol, diethylene glycoi, monoethyl ether, dipropylene glycoi, diethyl phthalate, triethyl citrate, etc.
• the amount of such solvents, diluents or carriers incorporated in the perfumes is preferably kept to the minimum needed to provide a homogeneous perfume solution. Tablets of the present invention as well as coated tablets according to the invention provide improved fabric perfume deposition.
• the perfume composition is present in an amount of 0.001 % to 10%, preferably from 0.005% to 5%, more preferably from 0.01 % to 3%, and even more preferably from 0.02% to 2% by weight of the tablet.
• the perfume can be incorporated to the tablet by any conventional means known to the skilled person.
• One preferred means is by spray-on of the perfume composition onto the tablet.
• the tablets may comprise components such as surfactants, enzymes, detergent etc....
• Typical tablet compositions for the preferred embodiment of the present invention are disclosed in the pending European applications of the Applicant n° 96203471.6, 96203462.5, 96203473.2 and 96203464.1 for example.
• Elements typically entering in the composition of detergent tablets or of other forms of detergents such as liquids or granules are detailed in the following paragraphs.
• the conventional nonionic and amphoteric surfactants such as the C
• the C-I Q-C-I S N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C12-C-I8 N-methylglucamides.
• sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C-
• 8 glucamides can be used for low sudsing.
• C10-C20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C-
• Other conventional useful surfactants are listed in standard texts.
• the tablet comprises at least 5% per weight of surfactant, more preferably at least 15% per weight, even more preferably at least 25% per weight, and most preferably between 35% and 45% per weight of surfactant.
• Non gelling binders can be integrated in detergent compositions to further facilitate dissolution. If non gelling binders are used, suitable non-gelling binders include synthetic organic polymers such as polyethylene glycols, polyvinylpyrrolidones, polyacrylates and water-soluble acrylate copolymers.
• binders classification Acacia, Alginic Acid, Carbomer, Carboxymethylcellulose sodium, Dextrin, Ethylcellulose, Gelatin, Guar gum, Hydrogenated vegetable oil type I, Hydroxyethyl cellulose, Hydroxypropyl methylcellulose, Liquid glucose, Magnesium aluminum silicate, Maltodextrin, Methylcellulose, polymethacrylates, povidone, sodium alginate, starch and zein. Most preferable binders also have an active cleaning function in the laundry wash such as cationic polymers, i.e. ethoxylated hexamethylene diamine quaternary compounds, bishexamethylene triamines, or others such as pentaamines, ethoxylated polyethylene amines, maleic acrylic polymers.
• cationic polymers i.e. ethoxylated hexamethylene diamine quaternary compounds, bishexamethylene triamines, or others such as pentaamines,
• Non-gelling binder materials are preferably sprayed on and hence have an appropriate melting point temperature below 90°C, preferably below 70°C and even more preferably below 50°C so as not to damage or degrade the other active ingredients in the matrix.
• Most preferred are non-aqueous liquid binders (i.e. not in aqueous solution) which may be sprayed in molten form. However, they may also be solid binders incorporated into the matrix by dry addition but which have binding properties within the tablet.
• Non-gelling binder materials are preferably used in an amount within the range from 0.1 to 15% of the composition, more preferably below 5% and especially if it is a non laundry active material below 2% by weight of the tablet.
• gelling binders such as nonionic surfactants are avoided in their liquid or molten form.
• Nonionic surfactants and other gelling binders are not excluded from the compositions, but it is preferred that they be processed into the detergent tablets as components of particulate materials, and not as liquids.
• Detergent builders can optionally be included in the compositions herein to assist in controlling mineral hardness. Inorganic as well as organic builders can be used. Builders are typically used in fabric laundering compositions to assist in the removal of particulate soils.
• Inorganic or P-containing detergent builders include, but are not limited to, the alkali metal, ammonium and alkanolammonium salts of polyphosphates
• compositions herein function surprisingly well even in the presence of the so-called “weak” builders (as compared with phosphates) such as citrate, or in the so-called "underbuilt” situation that may occur with zeolite or layered silicate builders.
• silicate builders are the alkali metal silicates, particularly those having a SiO2:Na2O ratio in the range 1.6:1 to 3.2:1 and layered silicates, such as the layered sodium silicates described in U.S. Patent 4,664,839, issued May 12, 1987 to H. P. Rieck.
• NaSKS-6 is the trademark for a crystalline layered silicate marketed by Hoechst (commonly abbreviated herein as "SKS-6").
• Hoechst commonly abbreviated herein as "SKS-6”
• the Na SKS-6 silicate builder does not contain aluminum.
• NaSKS-6 has the delta-Na2Si ⁇ 5 morphology form of layered silicate.
• SKS-6 is a highly preferred layered silicate for use herein, but other such layered silicates, such as those having the general formula
• y is a number from 0 to 20, preferably 0 can be used herein.
• Various other layered silicates from Hoechst include NaSKS-5, NaSKS-7 and
• Na2SiO5 (NaSKS-6 form) is most preferred for use herein.
• Other silicates may also be useful such as for example magnesium silicate, which can serve as a crispening agent in granular formulations, as a stabilizing agent for oxygen bleaches, and as a component of suds control systems.
• carbonate builders are the alkaline earth and alkali metal carbonates as disclosed in German Patent Application No. 2,321 ,001 published on November 15, 1973.
• Aluminosilicate builders are useful in the present invention. Aluminosilicate builders are of great importance in most currently marketed heavy duty granular detergent compositions, and can also be a significant builder ingredient in liquid detergent formulations. Aluminosilicate builders include those having the empirical formula:
• aluminosilicate ion exchange materials are commercially available. These aluminosilicates can be crystalline or amorphous in structure and can be naturally-occurring aluminosilicates or synthetically derived. A method for producing aluminosilicate ion exchange materials is disclosed in U.S. Patent 3,985,669, Krummel, et al, issued October 12, 1976. Preferred synthetic crystalline aluminosilicate ion exchange materials useful herein are available under the designations Zeolite A, Zeolite P (B), Zeolite MAP and Zeolite X.
• bleaching agents may optionally contain bleaching agents or bleaching compositions containing a bleaching agent and one or more bleach activators.
• bleaching agents will typically be at levels of from about 1 % to about 30%, more typically from about 5% to about 20%, of the detergent composition, especially for fabric laundering.
• the amount of bleach activators will typically be from about 0.1 % to about 60%, more typically from about 0.5% to about 40% of the bleaching composition comprising the bleaching agent-plus-bleach activator.
• the bleaching agents used herein can be any of the bleaching agents useful for detergent compositions in textile cleaning, hard surface cleaning, or other cleaning purposes that are now known or become known. These include oxygen bleaches as well as other bleaching agents.
• Perborate bleaches e.g., sodium perborate (e.g., mono- or tetra-hydrate) can be used herein.
• Another category of bleaching agent that can be used without restriction encompasses percarboxylic acid bleaching agents and salts thereof. Suitable examples of this class of agents include magnesium monoperoxyphthalate hexahydrate, the magnesium salt of metachloro perbenzoic acid, 4-nonylamino- 4-oxoperoxybutyric acid and diperoxydodecanedioic acid.
• Such bleaching agents are disclosed in U.S. Patent 4,483,781 , Hartman, issued November 20, 1984, U.S. Patent Application 740,446, Burns et al, filed June 3, 1985, European Patent Application 0,133,354, Banks et al, published February 20, 1985, and U.S. Patent 4,412,934, Chung et al, issued November 1 , 1983.
• Highly preferred bleaching agents also include 6-nonylamino-6-oxoperoxycaproic acid as described in U.S. Patent 4,634,551 , issued January 6, 1987 to Burns et al.
• Peroxygen bleaching agents can also be used.
• Peroxidase enzymes are known in the art, and include, for example, horseradish peroxidase, ligninase, and haloperoxidase such as chloro- and bromo- peroxidase.
• Peroxidase-containing detergent compositions are disclosed, for example, in PCT International Application WO 89/099813, published October 19, 1989, by O. Kirk, assigned to Novo Industries A S.
• the clay flocculating agent functions such as to bring together the particles of clay compound in the wash solution and hence to aid their deposition onto the surface of the fabrics in the wash. This functional requirement is hence different from that of clay dispersant compounds which are commonly added to laundry detergent compositions to aid the removal of clay soils from fabrics and enable their dispersion within the wash solution.
• Preferred as clay flocculating agents herein are organic polymeric materials having an average weight of from 100,000 to 10,000,000, preferably from 150,000 to 5,000,000, more preferably from 200,000 to 2,000,000.
• Inorganic clay flocculating agents are also suitable herein, typical examples of which include lime and alum.
• the flocculating agent is preferably present in a detergent base granule such as a detergent agglomerate, extrudate or spray-dried particle, comprising generally one or more surfactants and builders.
• the weight ratio of clay to the flocculating polymer is preferably from 1000:1 to 1 :1 , more preferably from 500:1 to 1 :1 , most preferably from 300:1 to 1 :1 , or even more preferably from 80:1 to 10:1 , or in certain applications even from 60:1 to 20:1.
• detergent compositions include chelating agents, soil release agents, soil antiredeposition agents, dispersing agents, suds suppressors, fabric softeners, dye transfer inhibition agents and mixtures thereof.
• a solution is prepared as follows comprising de-ionised water as well as 20 grams per litre of a specific compound: 1- 20 g of the specific compound is placed in a Sotax Beaker. This beaker is placed in a constant temperature bath set at 10°C. A stirrer with a marine propeller is placed in the beaker so that the bottom of the stirrer is at 5 mm above the bottom of the Sotax beaker. The mixer is set at a rotation speed of
• Step 3 is repeated after 20, 30, 40, 50, 1 min, 2 min, 5 min and 10 min after step 2.
• 5- The measurement taken at 10 min is used as the plateau value or maximum value.
• composition comprising a highly soluble compound as well as a surfactant is disclosed in EP-A-0 524 075, this composition being a liquid composition.
• the dissolution of the tablet or layer is further facilitated, resulting in a synergy leading to facilitated dissolution for a tablet according to the invention.
• the ingredients such as builder and surfactant can be spray-dried in a conventional manner and then compacted at a suitable pressure.
• the tablets according to the invention are compressed using a force of less than 100000N, more preferably of less than 50000N, even more preferably of less than 5000N and most preferably of less than 3000 N.
• the components of the particulate material may be mixed together by any conventional means. Batch is suitable in, for example, a concrete mixer, Nauta mixer, ribbon mixer or any other. Alternatively the mixing process may be carried out continuously by metering each component by weight on to a moving belt, and blending them in one or more drum(s) or mixer(s).
• Non-gelling binder can be sprayed on to the mix of some, or all of, the components of the particulate material.
• Other liquid ingredients may also be sprayed on to the mix of components either separately or premixed. For example perfume and slurries of optical brighteners may be sprayed.
• a finely divided flow aid dustting agent such as zeolites, carbonates, silicas
• the tablets may be manufactured by using any compacting process, such as tabletting, briquetting, or extrusion, preferably tabletting.
• Suitable equipment includes a standard single stroke or a rotary press (such as Courtoy®, Korch®,
• the tablets prepared according to this invention preferably have a diameter of between 20mm and 60mm, preferably of at least 35 and up to 55 mm, and a weight between 25 and 100 g.
• the ratio of height to diameter (or width) of the tablets is preferably greater than 1 :3, more preferably greater than 1 :2.
• the compaction pressure used for preparing these tablets need not exceed 100000 kN/m 2 , preferably not exceed 30000 kN/m 2 , more preferably not exceed 5000 kN/m 2 , even more preferably not exceed 3000kN/m 2 and most preferably not exceed 1000kN/m 2 .
• the tablet has a density of at least 0.9 g/cc, more preferably of at least 1.0 g/cc, and preferably of less than 2.0 g/cc, more preferably of less than 1.5 g/cc, even more preferably of less than 1.25 g/cc and most preferably of less than 1.1 g/cc.
• Multi layered tablets are typically formed in rotating presses by placing the matrices of each layer, one after the other in matrix force feeding flasks. As the process continues, the matrix layers are then pressed together in the pre- compression and compression stages stations to form the multilayer layer tablet. With some rotating presses it is also possible to compress the first feed layer before compressing the whole tablet.
• a highly soluble compound having a cohesive effect may be integrated to a detergent tablet, whereby this compound is also a hydrotrope compound.
• Such hydrotrope compound may be generally used to favour surfactant dissolution by avoiding gelling.
• a specific compound is defined as being hydrotrope as follows (see S.E. Friberg and M. Chiu, J. Dispersion Science and Technology, 9(5&6), pages 443 to 457, (1988-1989)):
• a solution is prepared comprising 25% by weight of the specific compound and 75% by weight of water.
• Octanoic Acid is thereafter added to the solution in a proportion of 1.6 times the weight of the specific compound in solution, the solution being at a temperature of 20°Celsius.
• the solution is mixed in a Sotax beaker with a stirrer with a marine propeller, the propeller being situated at about 5mm above the bottom of the beaker, the mixer being set at a rotation speed of 200 rounds per minute.
• the specific compound is hydrotrope if the the Octanoic Acid is completely solubilised, i.e . if the solution comprises only one phase, the phase being a liquid phase. It should be noted that in a preferred embodiment of the invention, the hydrotrope compound is a flowable material made of solid particles at operating conditions between 15 and 60° Celsius. Hydrotrope compounds include the compounds listed thereafter:
• Compounds of interest also include:
• Solvent hydrotropes such as alkoxylated glycerines and alkoxylated glycerides, esters slakoxylated glycerines, alkoxylated fatty acids, esters of glycerin, polyglycerol esters.
• Preferred alkoxylated glycerines have the following structure:
• R represents H, CH 3 or
• R1 and R2 are each C n COO or -(CH2CHR 3 -0)*-H
• R 3 H, CH 3 or C 2 H 5 and I is a number from 1 to about 60
• n is a number from about 6 to about 24.
• R is H or a C1-C10 alkyl group or is a hydrophilic functional group; R1 is H a lower alkyl group or an aromatic group, R2 is H or a cyclic alkyl or aromatic group.
• the polymer typically has a molecular weight of between about 1000 and 1000000.
• Such compound would further increase the dissolution rate of the tablet, as a hydrotrope compound facilitates dissolution of surfactants, for example.
• a hydrotrope compound facilitates dissolution of surfactants, for example.
• Such a compound could be formed from a mixture or from a single compound.
• the layer may be considered as a tablet itself.
• the used compacting force may be adjusted to not affect the tensile strength, and the disintegration time in the washing machine.
• This process may be used to prepare homogenous or layered tablets of any size or shape.
• the tensile strength corresponds to the diametrical fracture stress (DFS) which is a way to express the strength of a tablet or layer, and is determined by the following equation :
• DFS diametrical fracture stress
• F is the maximum force (Newton) to cause tensile failure (fracture) measured by a VK 200 tablet hardness tester supplied by Van Kell industries, Inc.
• D is the diameter of the tablet or layer, and t the thickness of the tablet or layer. For a non round tablet, ⁇ D may simply be replaced by the perimeter of the tablet.
• the rate of dispensing of a detergent tablet can be determined in the following way:
• the water supply to the washing machine is set to a temperature of 20 °C and a hardness of 21 grains per gallon, the dispenser water inlet flow-rate being set to 8 l/min.
• the level of tablet residues left in the dispenser is checked by switching the washing on and the wash cycle set to wash program 4 (white/colors, short cycle).
• the level of residues is determined by repeating the procedure 10 times and an average residue level is calculated based on the ten individual measurements.
• Effervescency as defined herein means the evolution of bubbles of gas from a liquid, as the result of a chemical reaction between a soluble acid source and an alkali metal carbonate, to produce carbon dioxide gas, i.e. C 6 H8 ⁇ 7 + 3NaHC03 ⁇ » Na 3 C 6 H 5 ⁇ 7 + 3C0 2 + 3H20
• acid and carbonate sources and other effervescent systems may be found in : (Pharmaceutical Dosage Forms : Tablets Volume 1 Page 287 to 291 ).
• An effervescent may be added to the tablet mix in addition to the detergent ingredients.
• the addition of this effervescent to the detergent tablet improves the disintegration time of the tablet.
• the amount will preferably be between 5 and 20 % and most preferably between 10 and 20% by weight of the tablet.
• the effervescent should be added as an agglomerate of the different particles or as a compact, and not as separated particles. Due to the gas created by the effervescency in the tablet, the tablet can have a higher D.F.S. and still have the same disintegration time as a tablet without effervescency. When the D.F.S. of the tablet with effervescency is kept the same as a tablet without, the disintegration of the tablet with effervescency will be faster.
• dissolution aid could be provided by using compounds such as sodium acetate or urea.
• suitable dissolution aid may also be found in Pharmaceutical Dosage Forms: Tablets, Volume 1 , Second edition, Edited by H.A. Lieberman et all, ISBN 0-8247-8044-2.
• Solidity of a tablet may be improved by making a coated tablet, the coating covering a non-coated tablet, thereby further improving the mechanical characteristics of the tablet while maintaining or further improving dissolution.
• the tablets may then be coated so that the tablet does not absorb moisture, or absorbs moisture at only a very slow rate.
• the coating is also strong so that moderate mechanical shocks to which the tablets are subjected during handling, packing and shipping result in no more than very low levels of breakage or attrition.
• the coating is preferably brittle so that the tablet breaks up quickly when subjected to stronger mechanical shock.
• the coating material is dissolved under alkaline conditions, or is readily emulsified by surfactants. This contributes to avoiding the problem of visible residue in the window of a front-loading washing machine during the wash cycle, and also avoids deposition of undissolved particles or lumps of coating material on the laundry load.
• Water solubility is measured following the test protocol of ASTM E1148-87 entitled, "Standard Test Method for Measurements of Aqueous Solubility". Fracture of the coating in the wash is improved by adding a disintegrant in the coating. This disintegrant will swell once in contact with water and break the coating in small pieces. This will improve the dissolution of the coating in the wash solution. Typically, the disintegrant is suspended in the coating melt at a level of up to 30%, preferably between 5% and 20%, most preferably between 5 and 10% by weight.
• Clay mineral compound as above described, is a disintegrant for use herein.
• disintegrants include starch: natural, modified or pregelatinized starch, sodium starch gluconate; gum: agar gum, guar gum, locust bean gum, karaya gum, pectin gum, tragacanth gum; croscarmylose Sodium, crospovidone, cellulose, carboxymethyl cellulose, algenic acid and its salts including sodium alginate, silicone dioxide, clay, polyvinylpyrrolidone, soy polysacharides, ion exchange resins, polymers containing cationic (e.g. quaternary ammonium) groups, amine-substituted polyacrylates, polymerised cationic amino acids such as poly-L-lysine, polyallylamine hydrochloride) and mixtures thereof.
• cationic e.g. quaternary ammonium
• the coating material has a melting point of at least 40°C, preferably of from 40°C to 200 °C.
• melting point is meant the temperature at which the material when heated slowly in, for example, a capillary tube becomes a clear liquid.
• the coating material which has a melting point of at least 40°C is an acid.
• Acid having a melting temperature of at least 40°C are for example dicarboxylic acids.
• Particularly suitable dicarboxylic acids are selected from the group consisting of oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid and mixtures thereof. Most preferred is adipic acid.
• the coating can be applied in a number of ways. Two preferred coating methods are a) coating with a molten material and b) coating with a solution of the material.
• the coating material is applied at a temperature above its melting point, and solidifies on the tablet.
• the coating is applied as a solution, the solvent being dried to leave a coherent coating.
• the substantially insoluble material can be applied to the tablet by, for example, spraying or dipping. Normally when the molten material is sprayed on to the tablet, it will rapidly solidify to form a coherent coating. When tablets are dipped into the molten material and then removed, the rapid cooling again causes rapid solidification of the coating material. During the solidification phase, the coating undergoes some internal stress (e.g.
• the coating comprises a component which is liquid at 25°C.
• this liquid component will allow the coating to better withstand and absorb mechanical stress by rendering the coating structure more flexible.
• the component which is liquid at 25°C is preferably added to the coating materials in proportions of less than 10% by weight of the coating, more preferably less than 5% by weight, and most preferably of less than 3% by weight.
• the component which is liquid at 25°C is preferably added to the coating materials in proportions of more than 0.1 % by weight of the coating, more preferably more than 0.3% by weight, and most preferably of more than 0.5% by weight.
• optional components which are liquid at 25°C includes polyethylene glycols, thermal oil, silicon oil, esters of dicarboxylic acids, mono carboxylic acids, parafin, triacetin, perfumes or alkaline solutions.
• polyethylene glycols thermal oil, silicon oil, esters of dicarboxylic acids, mono carboxylic acids, parafin, triacetin, perfumes or alkaline solutions.
• NaOH solution particularly good results were obtained by use of NaOH solution as alkaline solution.
• the structure of the components which is liquid at 25°C is close to the material forming the crystallised structure, so that the structure is not excessively disrupted.
• the optional component which is liquid at 25°C may advantageously have a functionality in the washing of laundry, for example silicone oil which provides suds suppression benefits or perfume oil.
• the perfume oil may be the perfume composition as per described herein, or a different perfume composition to that already contained by the tablet, provided it contains less than 0.6% by weight of Schiff-Base.
• the coating may also comprise materials other than the optional component which is liquid at 25°C. Hence, further preferred, is the addition of reinforcing fibres to the coating in order to further reinforce the structure.
• the crystallised structure is made of adipic acid, the component which is liquid at 25°C being available under the name CoasolTM from Chemoxy International, being a blend of the di-isobutyl esters of the glutaric, succinic and adipic acid.
• CoasolTM from Chemoxy International
• the advantage of the use of this component being the good dispersion in the adipic acid to provide flexibility. It should be noted that disintegration of the adipic acid is further improved by the adipate content of CoasolTM.
• the coating comprises an acid having a melting temperature of at least 145°C, such as adipic acid for example, as well as a clay, such as a bentonite clay for example, whereby the clay is used as a disintegrant and also to render the structure of adipic acid more favourable for water penetration, thus improving the dispersion of the adipic acid in a aqueous medium.
• a clay such as a bentonite clay for example
• Preferred clays are bentonite clays.
• the coating further comprises reinforcing fibres.
• Such fibres have been found to improve further the resistance of the coating to mechanical stress and minimise the splitting defect occurence.
• Such fibres are preferably having a length of at least 100 ⁇ m, more preferably of at least 200 ⁇ m and most preferably of at least 250 ⁇ m to allow structure reinforcement.
• Such fibres are preferably having a length of at less than 500 ⁇ m, more preferably of less than 400 ⁇ m and most preferably of less than 350 ⁇ m in order not to impact onto dispersion of the coating in an aqueous medium.
• Materials which may be used for these fibres include viscose rayon, natural nylon, synthetic nylon (polyamides types 6 and 6,6), acrylic, polyester, cotton and derivatives of cellulose such as CMCs. Most preferred is a cellulosic material available under the trade mark Solka-FlocTM from Fibers Sales & Development. It should be noted that such fibres do not normally need pre-compression for reinforcing the coating structure. Such fibres are preferably added at a level of less than 5% by weight of the coating, more preferably less than 3% by weight. Such fibres are preferably added at a level of more than 0.5% by weight of the coating, more preferably more than 1 % by weight.
• a coating of any desired thickness can be applied according to the present invention.
• the coating forms from 1 % to 10%, preferably from 1.5% to 5%, of the tablet weight.
• a preferred process for making a tablet according to the invention comprises the steps of:
• Another preferred process for making a tablet according to the invention comprises the steps of :
• a packaging system may be formed from a sheet of flexible material.
• Materials suitable for use as a flexible sheet include mono-layer, co-extruded or laminated films.
• Such films may comprise various components, such as poly-ethylene, polypropylene, poly-styrene, poly-ethylene-terephtalate.
• the packaging system is composed of a poly-ethylene and bi-oriented-poly-propylene co- extruded film with an MVTR of less than 5 g/day/m 2 .
• the MVTR of the packaging system is preferably of less than 10 g/day/m 2 , more preferably of less than 5 g/day/m 2 .
• the film (2) may have various thicknesses. The thickness should typically be between 10 and 150 ⁇ m, preferably between 15 and 120 ⁇ m, more preferably between 20 and 100 ⁇ m, even more preferably between 25 and 80 ⁇ m and most preferably between 30 and 40 ⁇ m.
• a packaging material preferably comprises a barrier layer typically found with packaging materials having a low oxygen transmission rate, typically of less than 300 cm 3 /m 2 /day, preferably of less than 150 cm 3 /m 2 /day, more preferably of less than 100 cm 3 /m 2 /day, even more preferably of less than 50 cm 3 /m 2 /day and most preferably of less than 10 cm 3 /m 2 /day.
• Typical materials having such barrier properties include bi oriented polypropylene, poly ethylene terephthalate, Nylon, poly(ethylene vinyl alcohol) , or laminated materials comprising one of these, as well as SiOx (Silicium oxydes), or metallic foils such as aluminium foils for example.
• Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and
• the abbreviated component identifications have the following meanings: LAS Sodium linear C-
• Nai2(A1 ⁇ 2Si ⁇ 2)i2-27H2 ⁇ having a primary particle size in the range from 0J to 10 micrometers (weight expressed on an anhydrous basis)
• Citric acid Anhydrous citric acid
• Amylase II Amylolytic enzyme, as disclosed in PCT/ US9703635 Lipase Lipolytic enzyme, having 2.0% by weight of active enzyme, sold by NOVO Industries A/S under the tradename Lipolase
• Lipase II Lipolytic enzyme, having 2.0% by weight of active enzyme, sold by NOVO Industries A/S under the tradename Lipolase Ultra
• Endolase Endoglucanase enzyme, having 1.5% by weight of active enzyme, sold by NOVO Industries A/S PB4 Sodium perborate tetrahydrate of nominal formula
• NACA-OBS (6-nonamidocaproyl) oxybenzene sulfonate LOBS Dodecanoyloxybenzene sulfonate in the form of the sodium salt DOBS Decanoyloxybenzene sulfonate in the form of the sodium salt
• DOBA Decanoyl oxybenzoic acid
• TAED Tetraacetylethylenediamine DTPA
• DTPMP Diethylene triamine penta (methylene phosphonate), marketed by Monsanto under the Tradename
• Brightener 1 Disodium 4,4'-bis(2-sulphostyryl)biphenyl
• Brightener 2 Disodium 4,4'-bis(4-anilino-6-morpholino-1.3.5- triazin-2-yl)amino) stilbene-2:2'-disulfonate
• PEO Polyethylene oxide with an average molecular weight of 50,000
• PEI Polyethyleneimine with an average molecular weight of 1800 and an average ethoxylation degree of 7 ethyleneoxy residues per nitrogen
• Flocculating agent III polymer of acrylamide and/ or acrylic acid of average molecular weight of 200,000 and 400,000
• SRP II Polysaccheride soil release polymer
• SRP 1 Nonionically end capped poly esters
• SRP 2 Diethoxylated poly (1 , 2 propylene terephtalate) short block polymer Silicone antifoam Polydimethylsiloxane foam controller with siloxane- oxyalkylene copolymer as dispersing agent with a ratio of said foam controller to said dispersing agent of 10:1 to 100:1
• Opacifier Water based monostyrene latex mixture, sold by BASF Aktiengesellschaft under the tradename Lytron 621
• a detergent base powder of composition A was prepared as follows: all the particulate material of base composition were mixed together in a mixing drum or spray drum to form a homogenous particulate mixture, apart from the binder spray-on system, the fluorescer or brightener, and the photobleach
• Zinc Phthalocyanine sulphonate The particulate mixture was thereafter divided in two equal parts, one part for making a white layer, another part for making a green layer.
• the white layer material is obtained by spraying the brightener or fluorescer together with half of the binder.
• the green layer material is obtained by spraying the photobleach Zinc Phthalocyanine sulphonate together with the rest of the binder.
• the layer where then processed independently in a Loedige KM 600 ® . ii) Using a Bonals ® rotary press both matrices were filled in two independent force feeding flasks. Both layers are compressed together in the pre- compression and compression stations to form a dual layer tablet.
• the tablets have a square cross section of 45 mm side, a height of 24 mm and a weight of 45 gr.
• the height of the green bottom layer corresponded to 50% of the total height of the tablet.
• the tensile strength of the uncoated tablets was 13 kpa.
• the tablet was thereafter coated with 2.5 g of coating formed from 89% by weight of adipic acid and 10% by weight of Bentonite clay from CSM, and 1 % by weight of ethane 1-hydroxy diphosphonate.
• Example 2 i) A detergent base powder of composition A was prepared as follows: all the particulate material of base composition were mixed together in a mixing drum or spray drum to form a homogenous particulate mixture, apart from the binder spray-on system, the fluorescer or brightener, and the photobleach Zinc Phthalocyanine sulphonate. The particulate mixture was thereafter divided in two equal parts, one part for making a white layer, another part for making a green layer. The white layer material is obtained by spraying the brightener or fluorescer together with half of the binder. The green layer material is obtained by spraying the photobleach Zinc Phthalocyanine sulphonate together with the rest of the binder.
• the layer where then processed independently in a Loedige KM 600 ® .
• ii) Using a Bonals ® rotary press both matrices were filled in two independent force feeding flasks. Both layers are compressed together in the pre- compression and compression stations to form a dual layer tablet.
• the tablets have a square cross section of 45 mm side, a height of 24 mm and a weight of 45 gr. The height of the green bottom layer corresponded to 50% of the total height of the tablet.
• the tensile strength of the uncoated tablets was 13 kpa.
• the tablet was thereafter coated with 2.5 g of coating formed from 89% by weight of adipic acid and 10% by weight of Bentonite clay from CSM, and
• Example 3 i) A detergent base powder of composition A was prepared as follows: all the particulate material of base composition were mixed together in a mixing drum or spray drum to form a homogenous particulate mixture, apart from the binder spray-on system, the fluorescer or brightener, and the photobleach Zinc Phthalocyanine sulphonate. The particulate mixture was thereafter divided in two equal parts, one part for making a white layer, another part for making a green layer. The white layer material is obtained by spraying the brightener or fluorescer together with half of the binder. The green layer material is obtained by spraying the photobleach Zinc Phthalocyanine sulphonate together with the rest of the binder.
• the layer where then processed independently in a Loedige KM 600 ® .
• ii) Using a Bonals ® rotary press both matrices were filled in two independent force feeding flasks. Both layers are compressed together in the pre- compression and compression stations to form a dual layer tablet.
• the tablets have a square cross section of 45 mm side, a height of 24 mm and a weight of 45 gr. The height of the green bottom layer corresponded to 50% of the total height of the tablet.
• the tensile strength of the uncoated tablets was 13 kpa.
• the tablet was thereafter coated with 2.5 g of coating formed from 89% by weight of adipic acid and 10% by weight of Bentonite clay from CSM, and
• Example 4 i) A detergent base powder of composition A was prepared as follows: all the particulate material of base composition was mixed together in a mixing drum or spray drum to form a homogenous particulate mixture. The binder system was then sprayed on. The powder where then processed in a Loedige KM 600 ® . ⁇ ) Using a Instron® Laboratory bench press, detergent powder was filled in the die. The powder had been compressed with a force so that the tensile strength of the tablet was 10kpa. iii) In this particular example, the tablets have a diameter of 54 mm side, a height of 24 mm and a weight of 45 gr.
• Example 5 A detergent base powder of composition A was prepared as follows: all the particulate material of base composition were mixed together in a mixing drum or spray drum to form a homogenous particulate mixture. The binder system was then sprayed on. The powder where then processed in a Loedige
• the tablets have a diameter of 54 mm side, a height of 24 mm and a weight of 45 gr.
• the tablet was thereafter coated with 2.5 g of coating formed from 88% by weight of Adipic acid, 10% by weight of bentonite clay from and 1 % of CoasolTM, and 1 % by weight of ethane 1 -hydroxy diphosphonate.
• Example 6 i) A detergent base powder of composition A was prepared as follows: all the particulate material of base composition were mixed together in a mixing drum or spray drum to form a homogenous particulate mixture. The binder system was then sprayed on. The powder where then processed in a Loedige
• the tablets have a diameter of 54 mm side, a height of 24 mm and a weight of 45 gr.
• the tablet was thereafter coated with 2.5 g of coating formed from 86% by weight of Adipic acid, 10% by weight of bentonite clay from and 1% by weight of CoasolTM and.2 % by weight of Solka-FlocTM 1016, and 0.5% by weight of ethane 1-hydroxy diphosphonate and 0.5% by weight of diethylene triamine penta (methylene phosphonate).
• compositions suitable for use herein are compositions suitable for use herein;

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• 1999
  • 1999-04-30 ES ES99870082T patent/ES2300138T3/es not_active Expired - Lifetime
  • 1999-04-30 DE DE69938228T patent/DE69938228T2/de not_active Expired - Fee Related
  • 1999-04-30 AT AT99870082T patent/ATE387486T1/de not_active IP Right Cessation
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• 2000
  • 2000-03-08 WO PCT/US2000/005985 patent/WO2000055294A2/en not_active Ceased
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  • 2000-03-08 AU AU38706/00A patent/AU3870600A/en not_active Abandoned
  • 2000-03-08 EP EP00917788A patent/EP1159398A2/de not_active Withdrawn
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