EP1074608A1 - Pastilles détergentes - Google Patents

Pastilles détergentes Download PDF

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Publication number
EP1074608A1
EP1074608A1 EP00306594A EP00306594A EP1074608A1 EP 1074608 A1 EP1074608 A1 EP 1074608A1 EP 00306594 A EP00306594 A EP 00306594A EP 00306594 A EP00306594 A EP 00306594A EP 1074608 A1 EP1074608 A1 EP 1074608A1
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EP
European Patent Office
Prior art keywords
tablet
surface active
active agent
weight
region
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP00306594A
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German (de)
English (en)
Inventor
William John 11 Tarn Close Locke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Robert McBride Ltd
Original Assignee
Robert McBride Ltd
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Filing date
Publication date
Application filed by Robert McBride Ltd filed Critical Robert McBride Ltd
Publication of EP1074608A1 publication Critical patent/EP1074608A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/83Mixtures of non-ionic with anionic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047Detergents in the form of bars or tablets
    • C11D17/0065Solid detergents containing builders
    • C11D17/0073Tablets
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/12Water-insoluble compounds
    • C11D3/124Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246Silicates, e.g. diatomaceous earth
    • C11D3/1253Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/126Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/222Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/37Polymers
    • C11D3/3746Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3757(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
    • C11D3/3761(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in solid compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/37Polymers
    • C11D3/3746Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3769(Co)polymerised monomers containing nitrogen, e.g. carbonamides, nitriles or amines
    • C11D3/3776Heterocyclic compounds, e.g. lactam
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146Sulfuric acid esters
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/662Carbohydrates or derivatives
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/72Ethers of polyoxyalkylene glycols

Definitions

  • the present invention relates to detergent tablets for use in laundering operations, particularly but not exclusively domestic laundering.
  • Such tablets are produced by compression of a particulate mixture which generally comprises a builder (which may be water soluble or water insoluble), a surface active agent system and ancillary components such as a bleach. bleach activator. enzymes etc. as well known in the art.
  • a particulate mixture which generally comprises a builder (which may be water soluble or water insoluble), a surface active agent system and ancillary components such as a bleach. bleach activator. enzymes etc. as well known in the art.
  • the surface active agent system will comprise (based on the weight of the tablet) at least about 5% of nonionic surface active agent and at least about 8% by weight of an anionic surface active agent.
  • a tablet to be introduced in the dispensing drawer of a domestic washing machine must be capable of dissolving in the relatively short time during which water in introduced into that drawer.
  • a tablet to be introduced into the drum of a washing machine a longer dissolution time will be acceptable.
  • a disintegrating agent In order to control the rate at which a tablet disintegrates, it is known to incorporate a disintegrating agent.
  • various substances which have high solubility in water may be used for this purpose.
  • Such water soluble disintegrant arc used particularly for tablets which are to be introduced into the drum of a domestic washing machine.
  • disintegrants which are insoluble in water but which swell in contact therewith.
  • Such water insoluble materials tend to be used for tablets are to be loaded into the dispensing drawer of a washing machine.
  • a first aspect of the present invention relates to tablets of the latter type. i.e. incorporating a water insoluble but water swellable disintegrating agent.
  • a detergent tablet of compressed particulate material said tablet or a region thereof containing at least one surface active agent, a builder and a water insoluble but water swellable disintegrating agent wherein the tablet or region thereof contains at least 5% by weight of solid surface active agent and does not contain more than 3% by weight of liquid non-ionic surface active agent.
  • Tablets in accordance with the first aspect of the invention may have the composition as defined in the previous paragraph throughout the tablet.
  • this composition may be provided in a region of the tablet, e.g. a layer.
  • liquid surface active agent as used herein means a surface active agent having a viscosity of less then 1 Pa s at 20°C.
  • any non-ionic liquid surface active agent in the tablet (or region thereof) has a viscosity of less then 0.5 Pa s at 20°C.
  • improvements in the disintegration of tablets containing a water insoluble but water swellable disintegrating agent may be obtained by controlling the amounts of solid surface active agent and liquid non-ionic surface active agent (which will be present in an absorbed and/or adsorbed form on solid components of the tablet or region thereof). More particularly, the improvement is obtained by ensuring that the amount of liquid non-ionic surface active agent present in the tablet (or region thereof) does not exceed 3% by weight of the tablet or region whilst ensuring that there is at least 5% by weight of solid surface active agent.
  • does not exceed 3% by weight we cover the possibility that the tablets (or region thereof) does not contain any liquid non-ionic surface active agent.
  • the present invention renders it possible to produce tablets which are intended for dosing into the dispensing draw of a domestic washing machine and which dissolve rapidly therein during the time that water is passed in to the dispensing draw.
  • Tablet formulations may be produced which leave a residue of less than 1% by weight of the tablet in the draw after the addition of water thereto has terminated.
  • the first aspect of the invention is however also applicable to tablets which arc intended to be loaded into the drum of a domestic washing machine.
  • the disintegrant has an average particle size of 30 ⁇ m to 1500 ⁇ m.
  • the disintegrant may have a particle size of 50 ⁇ m to 500 ⁇ m, preferably 50 ⁇ m to 400 ⁇ m, more preferably 100 ⁇ m to 300 ⁇ m, and even more preferably 300 ⁇ m to 350 ⁇ m.
  • the disintegrant may have a particle size of 300 ⁇ m to 1200 ⁇ m, e.g. 500 ⁇ m to 1200 ⁇ m, more preferably 600 ⁇ m to 1000 ⁇ m, and even more preferably 800 ⁇ m to 1000 ⁇ m.
  • the amount of the disintegrant present in the tablet (or region thereof) will be in the range 0.5% to 12% (e.g. 0.5% to 9%) by weight. more preferably 1% to 5% by weight. If the disintegrant has a particle size of 50 to 500 ⁇ m it is preferably present in an amount of 0.5% to 2.5%. If the disintegrant has a particle size of 300 to 1200 ⁇ m (e.g. 500 ⁇ m to 1200 ⁇ m) it is preferably present in an amount of 3% to 12%.
  • the disintegrant is a cellulose based material.
  • cellulose based material may for example comprise both crystalline and amorphous cellulose.
  • suitable materials arc disclosed, for example, in WO-A-9855575 (Henkel), WO-A-9840462 (Herzog).
  • the cellulose may be a cross-linked modified cellulose e.g. AC-DI-SOL and/or may comprise micro crystalline cellulose fibres (e.g. HANFLOC).
  • the cellulose based material may be a cellulose derivative which may be cross-linked. e.g. a cross-linked carboxymethyl cellulose.
  • a particularly suitable disintegrant for use in the invention is available under the trade marks Heweten 800G (ex J.Rettenmeyer & Sohne), Norasol 771 (ex Rohn & Haas) and NILYN (ex FMC).
  • the disintegrant may be a cellulose derivative, for example a sodium carboxymethyl cellulose.
  • examples include COURLOSE and NYMCEL.
  • disintegrants which may be used include various starches such as potato, rice. corn or maize starch.
  • the disintegrant may be a starch derivative, e.g. carboxymethyl starch such as available under the trade mark PRIMOGEL or a sodium starch glycolate such as available under the trade mark EXPLOTAB.
  • the disintegrating agent may be a clay.
  • Such clays are generally of the "lamellar type" and may for example be a smectite such as a Laponite, Bentonite, Montmorrillonite, Hectorite or Saponite.
  • the clay may be a Sodium Montmorrillonite, a Sodium Hectorite, a Sodium Saponite, a Calcium Montmorrillonite or a Lithium Hectorite.
  • the disintegrating agent can be a synthetic polymer, for example a cross-linked polyvinyl pyrrolidone, POLYPLASDONE XL or KOLLIDON XL.
  • the disintegrant may be a polyacrylate or derivative thereof.
  • a clay may contribute to fabric softening properties and synthetic polymers may act to prevent deposition of dyes.
  • the tablet does not contain more than 3% by weight of liquid non-ionic surface active agent. Tablets which do not contain any liquid non-ionic surface active agent are within the scope of the invention but it is generally preferred that the tablet contains at least 0.5% by weight of liquid non-ionic surface active agents.
  • the tablet may contain more than 2.5% by weight of liquid non-ionic surface active agent. Certain tablets may contain preferably not more than 2%, even more preferably not more than 1.75% and most preferably not more than 1.5% by weight liquid non-ionic surface active agent. Other tablets may contain 1 to 2.5%, e.g. 1.5 to 2.5% by weight of liquid non-ionic surface active agent.
  • a detergent tablet of compressed particulate material said tablet or a region thereof containing at least one surface active agent and a builder wherein the tablet or region thereof contains at least 5% by weight of solid surface active agent of which at least a portion is provided by a solid non-ionic surface active agent and not more than 1.5% by weight of liquid non-ionic surface active agent.
  • Tablets in accordance with the second aspect of the invention may include disintegrant. e.g. a water soluble disintegrant as described above or a water soluble disintegrant (i.e. a highly water soluble salt). Tablets in accordance with the second aspect of the invention may have the composition as defined in the previous paragraph throughout the tablet. Alternatively this composition may be provided in a region of the tablet, e.g. a layer.
  • disintegrant e.g. a water soluble disintegrant as described above or a water soluble disintegrant (i.e. a highly water soluble salt).
  • Tablets in accordance with the second aspect of the invention may have the composition as defined in the previous paragraph throughout the tablet. Alternatively this composition may be provided in a region of the tablet, e.g. a layer.
  • Tablets in accordance with the invention may be produced by admixing the solid surface active agent (including the solid non-ionic surface active agent), liquid non-ionic surface active agent (if any) and other components of the formulation e.g. disintegrant builder, enzymes bleach. etc and compacting the resultant formulations.
  • the formulation from which the tablet is compacted
  • a liquid non-ionic surface active agent may for example an alcohol ethoxylate.
  • the alcohol residue (which may be of a primary or secondary alcohol) may for example comprise 8 to 18 carbon atoms and be ethoxylated with an average of 3 to 20 moles of ethylene oxide per mole of alcohol.
  • Suitable liquid non-ionic surface active agents are available from ICI under the designations SYNPERONIC A3 and SYNPERONIC A7. Mixtures of the A7 and A3 active agents may also be used. Also suitable are LUTENSOL AO3 and LUTENSOL AO7 (ex BASF).
  • Tablets in accordance with the first and second aspects of the invention also contain at least 5% by weight at least one solid surface active agent.
  • the amount of the solid surface active agent is in the range 5% to 25% by weight, more usually 5% to 15% by weight.
  • the tablets in accordance with the first and second aspects of the invention contain a relatively low amount of liquid non-ionic surface active agent, if any at all.
  • a proportion of the solid surface active agent in the tablet (or region thereof) is a non-ionic surface active agent.
  • the amount of solid non-ionic surface active agent may be at least 0.25%, preferably at least 0.5% and more preferably at least 1% by weight.
  • the amount of this surface active agent may be at least 4% or 5% by weight.
  • Most preferably the total amount of non-ionic surface active agent present in the tablet is at least 2.5%, preferably at least 3%. more preferably at least 4% and even more preferably at least 5% of the weight of the tablet or region thereof.
  • solid non-ionic surface active agents which may be used in the formulation in accordance with the first aspect of the formulation include alkyl(C 8-22 )polyglycosides.
  • the preferred glycoside employed in the present invention is a glucoside (i.e. based on glucose), functionalised with a primary alcohol (e.g. C 12 -C 14 ). More preferably the glucoside is in the form of a polyglucoside. with a preferred degree of polymerisation of between 1-2, most preferably about 1.4.
  • solid non-ionic surface active agent is used in the form of particles or granules containing at least 20% by weight, preferably at least 30% by weight, more preferably at least 40% by weight of solid non-ionic surface active agent.
  • a suitable polyglycoside is available under the name Glucopon (Henkel), preferably used as Glucopon G50 granules (50% APG Glucon, 50% sulphate).
  • the solid surface active agent in the tablet (or region thereof) is provided by an anionic surface active agent.
  • an anionic surface active agent typically the amount of such an anionic agent will generally be at least 2%, more preferably at least 4%. even more preferably at least 5%. still more preferably at least 6% and may be at least 8% by weight of the tablet (or region) thereof.
  • the amount of the anionic surface active agent will not exceed 25%, more usually not more than 20%, by weight of the tablet (or region).
  • the anionic surface active agent may be present in an amount of 2 to 20%, more preferably 4 to 15% (e.g. 10% to 15% or 10% to 13%), more preferably 6 to 12% on the same weight basis.
  • solid anionic surface active agent is used in the form of particles or granules containing at least 70%, more preferably at least 80% and even more preferably at least 90% by weight of anionic surface active agent.
  • anionic surfactant may he provided as an extrudate.
  • the anionic surface active agent may comprise at least one alkyl sulphate. most preferably a C 8-22 alkyl sulphate.
  • the alkyl group of the alkyl sulphate has 12-18, e.g. 8-16, carbon atoms.
  • the alkyl sulphate may be a single compound or may comprise a mixture of alkyl sulphates of different chain lengths.
  • the alkyl groups are primary alkyl groups and preferably straight chain.
  • the alkyl sulphate is preferably an alkali metal alkyl sulphate, the preferred alkali metal being sodium.
  • Suitable alkyl sulphates for use in the invention is available under the trade mark SULPHOPON, e.g. SULPHOPON 1218GF (a C 12-18 alkyl sulphate), and MARANIL 2g (ex Cognis)
  • the alkyl group of the ether sulphate may be as described for the alkyl sulphate.
  • anionic surface active agents which may be used include alkylaryl sulphonates (e.g. alkylbenzene sulphonates. (e.g. Nansa HS90OF ex Albright & Wilson) alpha olefin sulphonates and ether carboxylates.
  • alkylaryl sulphonates e.g. alkylbenzene sulphonates. (e.g. Nansa HS90OF ex Albright & Wilson) alpha olefin sulphonates and ether carboxylates.
  • the solid surface active agent may be provided at least partially by an amphoteric surface active agent which may for example be a betaine.
  • Preferred betaines may be either of the formula (I) or (II).
  • R 1 and R 2 may be the same or different C 1-4 alkyl groups whereas R 3 is an alkyl group having 8-22 carbon atoms, more preferably 12 to 18 carbon atoms e.g. mixed C 10 to C 14 .
  • cocoamidopropyl betaine also known as cocodimethyl acetic acid betaine (CAS Registry No.66415-29-6).
  • Further betaines which may be used are lauryl dimethyl betaine (CAS Registry No. 683-10-3), cocoa dimethyl amidopropyl betaine (CAS Registry No.61789-40-0) and the products identified as CAS Registry Nos. 70851-07-09 and 4292-10-8.
  • amphoteric surface active agent for use in the tablet of the invention is a glycinate of the formula R 3 NHCH 2 CO 2 H where R 3 is as defined above.
  • a further glycinate which may be used is of the formula
  • R 3 is as defined above (more preferably C 12-22 ) and n is 1 to 3.
  • Tablets in accordance with the inventions may contain up to 80% by weight amphoteric surfactant, more preferably up to 5%.
  • the solid surface active agent it is also possible for at least a portion of the solid surface active agent to be provided by a cationic surface active agent although in this case there will generally be no anionic surface active agent present in the tablet.
  • Tablets in accordance with the invention also incorporate at least one builder.
  • the builder will be present in the tablets (or region thereof) in an amount of 10% to 70% by weight, more preferably 20% to 50% by weight.
  • the builder is water soluble salt and a wide range of such salts known as builders in the art may be employed in the present invention. It is particularly preferred that the builder is an alkali metal phosphate or an alkali metal phosphate or an alkali metal carbonate.
  • a particularly preferred builder for use in the invention is sodium triphosphate for example of the type, or of a type similar to that. disclosed in EP-A-0 839 906. Alternatively the builder may be sodium carbonate.
  • the tablet may incorporate a bleach, for example an activated bleaching system.
  • a bleach for example an activated bleaching system.
  • Such a system may comprise a hydrogen peroxide precursor (e.g. sodium percarbonate, sodium perborate monohydrate or sodium perborate tetrahydrate) together with a bleach activator.
  • the activator may be an N-acyl compound, particularly one having two or more N-acyl groups.
  • the activator may be tetraacetyl ethylene diamine (TAED) as conventionally used as a activator in detergent tablets.
  • TAED tetraacetyl ethylene diamine
  • the bleach activator may be an ester of a polyhydric alcohol having at least 5 carbon atoms and at least 3 hydroxyl groups esterified with C 2-5 acyl groups, the polyhydric alcohol residue of said activator not having substituents with 6 or more carbon atoms.
  • Such an activator may have an HLB value of at least 7. more preferably at least 9, and even more preferably at least 11.
  • the HLB value may be as high as 14 or 15.
  • the alcohol residue of the activator preferably has a maximum of 12 carbon atoms and a minimum of five hydroxyl groups esterified with C 2-5 acyl groups.
  • suitable alcohols are sugar and sugar derived alcohols such as sorbitol, glucitol, mannitol, glucose and sucrose.
  • the acyl groups in the activator are aliphatic acyl groups. It is preferred that the acyl group has two or three carbon atoms and is most preferably the acetyl group.
  • the amount of bleach activator incorporated in the tablet of the invention will generally be in the range of 0.5% to 10% by weight of the total formulation, more preferably 1% to 8% and even more preferably 2% to 4% on the same basis.
  • the preferred bleaching system for use in the invention comprises a hydrogen peroxide precursor compound and the bleach activator as defined above which is capable of reacting with the hydrogen peroxide to generate a peracid.
  • the hydrogen peroxide precursor compound may, for example, be an inorganic persalt e.g. a perborate (in the monohydrate and/or tetrahydrate form), a percarbonate or a persulphate.
  • the alkali metal salts of these compounds are preferred, particularly sodium and potassium salts.
  • the bleaching agent may be a urea-hydrogen peroxide complex.
  • the amount of hydrogen peroxide precursor compound present in the formulation of the invention is preferably such as to provide 0.5% to 3% by weight active oxygen, especially 1.0% to 2.5% by weight.
  • the tablet may incorporate a fabric softening agent which may for example be a clay in conjunction with a surface active agent.
  • the fabric softening clay preferably has a particle size of at least 500 ⁇ m.
  • the fabric softening clay may he any such clay having fabric softening properties used in laundry detergent formulations. Such clays are generally of the "lamellar type" and are such that the layers "separate" to become deposited on the garments being washed.
  • the clay may for example be a smectite such as a Laponite, Bentonite, Montmorrillonite, Hectorite or Saponite.
  • the clay may he a Sodium Montmorrillonite, a Sodium Hectorite, a Sodium Saponite, a Calcium Montmorrillonite or a Lithium Hectorite.
  • the amount of clay used as a fabric softener in the detergent tablets will be 5% to 20% by weight.
  • the clay may be used in conjunction with a cationic and/or amide surfactant to help delamination of the clay and absorption thereof onto the garments being laundered.
  • the cationic surfactant may for example be a quaternary ammonium salt having one long chain (e.g. C 8-22 ) alkyl group and three short chain (e.g. C 1-4 ) alkyl groups.
  • a suitable cationic surfactant is coco trimethyl ammonium chloride.
  • the amide surfactant may contain at least one long chain (e.g. C 8-22 ) alkyl group and may for example be stearyl stearamide.
  • a suitable clay formulation may contain 20-30% by weight of the formulation (i.e. clay plus surfactants) of amide surfactant and 1-2% cationic surfactant.
  • the fabric softening agent may be an organic compound.
  • One class of organic fabric softening agents are amides of the formula where n and m are the same or different and are in the range 8 to 22, more preferably 10 to 20. If the alkyl groups are branched then they preferably include a chain of at least 8 carbon atoms.
  • a particularly preferred amide for use in the invention is stearyl stearamide.
  • the organic fabric softening agent may be a quaternary ammonium salt having one long chain (e.g. C 8-22 ) alkyl group and three short chain (e.g. C 1-4 ) alkyl groups.
  • a suitable cationic surfactant is coco trimethyl ammonium chloride.
  • the quaternary ammonium salt be used in combination with the above described amides in which case the quaternary ammonium salt may suitably be employed in an amount of up to 5%, more preferably 1 to 2%, by weight of the clay.
  • organic fabric softening agents which may be used include amine and/or amide functionalised silanes.
  • the tablet may incorporate at least one enzyme.
  • the enzyme may, for example, be a protease, amylase, lipase or cellulase (or mixtures thereof) such as commonly used in detergent formulations.
  • suitable enzymes are available under the names Opticlean, Savinase, Esperase; Termamyl, Maxamayl, Lipomax, Lipolase; Celluzyme and Carezyme.
  • the amount of enzyme incorporated in the tablet will depend on activity but will typically be 0.1 to 3%. This level is particularly suitable for Savinase 6.0T, Termamyl 60T, Celluzyme 0.7T and Lipomax.
  • the tablets of the invention may be mass-produced on a number of tabletting machines. Models that may be used include the Europharma Machinery (UK) generally work by having a rotating circular turret with arrays of punches that compress the tablets from above and below. Tablets may be produced that are single or dual or multi- layer or of the tablet-in-tablet type and variations thereof.
  • the cycle for producing dual layer tablets consists of filling the die with the powder that will make up one of the layers, followed by filling of the powder of second layer.
  • Machines specially designed for dual layer operation usually have a small amount of pre-compression between filling the die with the powders of the first and second layers. This gives a sharper definition between the two layers which may be more aesthetically pleasing, particularly if the two layers are of different colours.
  • the press should have a control to regulate the applied force used in the main compression.
  • the applied pressure should typically be about 10 to 120KN for a 44mm tablet produced at a rate of greater than 20000 tablets per hour.
  • the pressure applied is a crucial part of the tabletting operation as inadequate pressure will gives a tablet which dissolves too slowly.
  • the tablet strength may be monitored by use of equipment to measure its breaking strength such as the Holland CT5 automatic compression tester (see below).
  • the tablet may incorporate additional components as conventionally included in laundry detergent formulations.
  • additional component is a soap which may be used in an amount up to 5% by weight as a processing aid.
  • additional components include anti-foam agents, sequestrants (e.g. of the phosphonate type), whiteness maintenance agents (e.g. CMC, polyoxyethylene terephthalate, polyethylene terephthalate), colourants (e.g. dyestuffs), perfume, flow control agents (e.g. a sulphate) flow enhancer (e.g. a zeolite), pH regulators (e.g. a carbonate or bicarbonate), anti-corrosion agents, dye transfer inhibitors (e.g. PVP) and optical brighteners (e.g. Tinopal CBS-X and Tinopal DMS-X). These components may, for example, each be present in amounts up to 1% by weight of the formulation.
  • the fabric softening agent may be an organic fabric softening agent which is nitrogen containing compound having at least a degree of positive charge on the nitrogen atom.
  • Tablets (45mm diameter, 18mm height, 40g) are placed on an open wire stand (40m diameter, 5cm high) in a beaker containing water at 30°C. The time taken for the bulk of a tablet to fall from the stand was measured. A time of 30 seconds or less indicates suitability of the tablet for the testing in the dispensing drawer of a domestic washing machine.
  • Two tablets flat are placed on their circular faces and side-by-side, in the main (first) dispensing drawer (clean and dry) of a washing machine (drawer empty).
  • Two washing machines are used; a Hotpoint Ultima 1200 washing machine set at 40°C normal cotton wash and a Bosch 20001 set for a 40°C wool wash.
  • a tablet was said to have passed the drawer test if less than 1% of the tablets, by weight when dry, was left in the drawer.
  • the tablet is dropped from a height of 1 meter onto a hard surface.
  • This Example demonstrates the effect of varying the amount of liquid non-ionic surface agent whilst maintaining the total non-ionic surfactant constant in a tablet containing a water insoluble but water swellable disintegrating agent.
  • Tablets of the following compositions 1A - 1D were prepared Component Invention 1A Comparative 1B Comparative 1C Invention 1D STP 41.5 41.5 41.5 41.5 Sodium Disilicate Granules 5.00 5.00 5.00 C 12-18 Primary Alkyl Sulphate 10.00 10.00 10.00 10.00 10.00 Glucopon 50 G 2.00 1.00 0.00 3.00 T.A.E.D 3.00 3.00 3.00 3.00 3.00 CMC Disintegrating 1.50 1.50 1.50 1.50 1.50 Agent 0 0 0 0 Alkyl Ethoxylate (7EO) 3.00 4.00 5.00 2.00 Minor components 1.62 1.62 1.62 1.62 Na Percarbonate Disintegrating 18.00 18.00 18.00 18.00 Agent 4.50 4.50 4.50 4.50 Na Carbonate 9.88 9.88 9.88 Total % 100 100 100
  • the tablets were prepared by spraying the liquid non-ionic surfactant onto those components listed in the Table above the ethoxylate, admixing the products with those components of the formulation listed in the Table below the ethoxylate. and compacting 40g of the admixture at various pressures on a laboratory press using a die of diameter 45mm and a height of 38mm.
  • This example demonstrates the effect of varying the amount of a water insoluble but water swellable tablet disintegrant in a tablet containing 1% of liquid non-ionic surface active agent.
  • tablets were prepared from the following compositions 2A-2G containing a bentonite clay granule (Laundrosil - ex Sud Chemie).
  • Component 2A 2B 2C 2D 2E 2F 2G STP 40.5 40.5 4.0.5 40.5 40.5 40.5 40.5 Sodium Disilicate Granules 5.00 5.00 5.00 5.00 5.00 C 12-18 Primary Alkyl Sulphate 11.00 11.00 11.00 11.00 13.00 13.00 Glucopon 50 G 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 Disintegrant 0.00 1.00 2.00 3.00 4.00 3.00 4.50 T.A.E.D 3.00 3.00 3.00 3.00 3.00 3.00 3.00 3.00 3.00 3.00 Minor Components 0.65 0.65 0.650 0.65 0.65 0.65 0.65 Alkyl Ethoxylate (7EO) 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 Enzyme 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4
  • This Example demonstrates the effect of varying the liquid non-ionic surface active agent content in a formulation which includes a fabric softener and a water insoluble disintegrant.
  • tablets were prepared from the following compositions 3A-3D.
  • the Example demonstrates the effect of varying builder content in a tablet containing a water insoluble disintegrating whilst maintaining liquid non-ionic surface active agent constant.
  • Non-Bio Formulations Component 4A 4B 4C STP 41.5 39.5 43.5 Disilicate Granules 5.00 5.00 5.00 C 12-18 Primary Alkyl Sulphate 11.00 11.00 11.00 Glucopon 50 G 2.00 2.00 2.00 Disintegrant 6.50 6.50 6.50 T.A.E.D 3.00 3.00 3.00 Minor Components 1.40 1.40 1.40 Alkyl Ethoxylate (7EO) 1.80 1.80 1.80 Na Percarbonate 18.00 18.00 18.00 Na Carbonate 9.80 11.80 7.80 Total % 100 100 100
  • Colour Formulations Component 4D 4E STP 46.5 48.5 Disilicate Granules 5.00 5.00 C 12-18 Primary Alkyl Sulphate 11.00 11.00 Glucopon 50 G 2.00 2.00 Disintegrant 6.50 6.50 PVP 1.14 1.14 Minor Components 1.29 1.29 Alkyl Ethoxylate (7EO)
  • This Example illustrates the effect of varying amounts and/or components in various formulations containing low levels of liquid non-ionic surface active agent.
  • Example 1 tablets were prepared from the following formulation 5A.
  • Component 5A STP 41.5 Layered Silicate 5.00 C 12-18 Primary Alkyl Sulphate 10.00 T.A.E.D 3.00 CMC 1.50 Minor Components 1.62 Alkyl Ethoxylate (7EO) 5.00 Na Percarbonate 18.00 Disintegrant 1.25 Na Bicarbonate 12.88
  • Tablets were also prepared from modified formulations 5B-5D as detailed below.
  • Formulations 5B-5D were produced by adjusting the bicarbonate level to 100%.
  • the tablets were produced at compression pressures of 1000psi on a hand press.
  • the dissolution time of the tablets was measured in beaker of 30°C water.
  • the snap hardness of the tablets was measured on a CT5 compression tester.
  • compositions 6A-6B STP 40.75 40.75 Layered Silicate Primary Alkyl 5.00 5.00 Sulphate 13.00 13.00 Glucopon KE3515 3.00 TAED 3.00 3.00 CMC 1.50 1.50 Glucopon 600 3.00 Na Percarbonate 16.50 16.50 Disintegrant 1.50 1.50 Laundrosil 10.00 10.00 Na Bicarbonate 0.20 0.20 Minor Components to 100% to 100%
  • Glucopon 600 is a 50% aqueous solution of alkyl polyglucoside with a C 12 to C 14 chain length.
  • Glucopon KE3515 is granule containing 50% APG and 50% carboxylate carrier.
  • the Glucopon 600 was sprayed onto the base material using a hand held plastic spray bottle. As Glucopon is too viscous until a temperature of ca. 50°C is reached, the spray bottle was immersed into near-boiling water before use.
  • the Glucopon KE3515 the Glucopon was heated before addition to the powder in a Moulinex Masterchef 20 blender. After addition of the Glucopon, any remaining materials were added e.g. sodium bicarbonate. The mixtures were then left for 24 hours before being tableted on a hand press (600psi).
  • composition B Tablets were prepared at various compression pressures from composition B save that the primary alkyl sulphate was replaced by a lauryl ether sulphate. The resultant tablets were tested and the results are shown below.
  • Compression Hardness Beaker Test 100psi 2.43kg 24 sec 1200 psi 3.45kg 25 sec 1400 psi 4.09kg 30sec

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EP00306594A 1999-08-02 2000-08-02 Pastilles détergentes Withdrawn EP1074608A1 (fr)

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GBGB9918087.9A GB9918087D0 (en) 1999-08-02 1999-08-02 Detergent tablets
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1219700A1 (fr) * 2000-12-28 2002-07-03 Unilever Plc Compositions de nettoyage
EP1249489A1 (fr) * 2001-04-12 2002-10-16 Cognis Deutschland GmbH & Co. KG Corps moules d'agents de lavage et de nettoyage présentant des proprietés de décomposition améliorées
EP1336651A1 (fr) * 2001-12-21 2003-08-20 Cognis Deutschland GmbH & Co. KG Préparations à action lavante et nettoyante, comprenant des tensioactifs non-ioniques solides granulés
WO2004046292A1 (fr) * 2002-11-15 2004-06-03 Unilever N.V. Detergent ayant une composition amelioree
EP1133548B2 (fr) 1998-11-27 2006-07-12 Unilever Plc Compositions detergentes sous forme de comprimes
EP2103675A1 (fr) * 2008-03-18 2009-09-23 The Procter and Gamble Company Composition détergente comprenant un polymère cellulosique
CN102453631A (zh) * 2010-11-02 2012-05-16 郑州大学 医用液体多酶洗涤剂
WO2024223718A1 (fr) 2023-04-28 2024-10-31 Unilever Ip Holdings B.V. Comprimé de dose unitaire

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0863200A2 (fr) * 1997-03-07 1998-09-09 Henkel Kommanditgesellschaft auf Aktien Compositions détergentes sous forme de tablettes
DE19803410A1 (de) * 1998-01-28 1999-07-29 Henkel Kgaa Mehrphasige Waschmitteltabletten
DE19807321A1 (de) * 1998-02-20 1999-08-26 Henkel Kgaa Wasch- und Reinigungsmittelformkörper mit verbessertem Eigenschaftsprofil
DE19903288A1 (de) * 1999-01-28 2000-08-03 Henkel Kgaa Mehrphasige Waschmitteltabletten

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0863200A2 (fr) * 1997-03-07 1998-09-09 Henkel Kommanditgesellschaft auf Aktien Compositions détergentes sous forme de tablettes
DE19803410A1 (de) * 1998-01-28 1999-07-29 Henkel Kgaa Mehrphasige Waschmitteltabletten
DE19807321A1 (de) * 1998-02-20 1999-08-26 Henkel Kgaa Wasch- und Reinigungsmittelformkörper mit verbessertem Eigenschaftsprofil
DE19903288A1 (de) * 1999-01-28 2000-08-03 Henkel Kgaa Mehrphasige Waschmitteltabletten

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1133548B2 (fr) 1998-11-27 2006-07-12 Unilever Plc Compositions detergentes sous forme de comprimes
EP1219700A1 (fr) * 2000-12-28 2002-07-03 Unilever Plc Compositions de nettoyage
EP1249489A1 (fr) * 2001-04-12 2002-10-16 Cognis Deutschland GmbH & Co. KG Corps moules d'agents de lavage et de nettoyage présentant des proprietés de décomposition améliorées
EP1336651A1 (fr) * 2001-12-21 2003-08-20 Cognis Deutschland GmbH & Co. KG Préparations à action lavante et nettoyante, comprenant des tensioactifs non-ioniques solides granulés
WO2004046292A1 (fr) * 2002-11-15 2004-06-03 Unilever N.V. Detergent ayant une composition amelioree
RU2323963C2 (ru) * 2002-11-15 2008-05-10 Юнилевер Н.В. Композиция очищающего средства
CN100393863C (zh) * 2002-11-15 2008-06-11 荷兰联合利华有限公司 改进的洗涤剂组合物
EP2103675A1 (fr) * 2008-03-18 2009-09-23 The Procter and Gamble Company Composition détergente comprenant un polymère cellulosique
WO2009117341A1 (fr) * 2008-03-18 2009-09-24 The Procter & Gamble Company Composition de détergent comprenant un polymère cellulosique
CN102453631A (zh) * 2010-11-02 2012-05-16 郑州大学 医用液体多酶洗涤剂
WO2024223718A1 (fr) 2023-04-28 2024-10-31 Unilever Ip Holdings B.V. Comprimé de dose unitaire

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