EP0395333A2 - Compositions détergentes - Google Patents

Compositions détergentes Download PDF

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Publication number
EP0395333A2
EP0395333A2 EP19900304333 EP90304333A EP0395333A2 EP 0395333 A2 EP0395333 A2 EP 0395333A2 EP 19900304333 EP19900304333 EP 19900304333 EP 90304333 A EP90304333 A EP 90304333A EP 0395333 A2 EP0395333 A2 EP 0395333A2
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EP
European Patent Office
Prior art keywords
tablet
detergent
bleach
powder
ingredients
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.)
Ceased
Application number
EP19900304333
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German (de)
English (en)
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EP0395333A3 (fr
Inventor
Alberto Gomez Carrera
Miguel Raminez Delso
Alan John Fry
Geoffrey Newbold
Jonathan Oster
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.)
Unilever PLC
Unilever NV
Original Assignee
Unilever PLC
Unilever NV
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Publication date
Priority claimed from GB898909254A external-priority patent/GB8909254D0/en
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Priority to EP99122669A priority Critical patent/EP0987320A3/fr
Publication of EP0395333A2 publication Critical patent/EP0395333A2/fr
Publication of EP0395333A3 publication Critical patent/EP0395333A3/fr
Ceased legal-status Critical Current

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    • 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
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0086—Laundry tablets
    • 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
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38609—Protease or amylase in solid compositions only
    • 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
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3905—Bleach activators or bleach catalysts
    • C11D3/3907—Organic compounds
    • C11D3/3917—Nitrogen-containing compounds
    • 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
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3942—Inorganic per-compounds
    • 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
    • C11D3/40—Dyes ; Pigments
    • C11D3/42—Brightening agents ; Blueing agents

Definitions

  • the present invention relates to novel laundry detergent compositions in the form of tablets containing inorganic persalt bleach (sodium perborate) and bleach-sensitive ingredients together without segregation.
  • Modern high-performance detergent powders for use in automatic washing machines normally contain inorganic persalt bleach as well as certain ingredients, notably bleach activators, enzymes and optical brighteners, that are sensitive to bleach.
  • Tablets have several advantages over powdered products: they do not require measuring and are thus easier to handle and dispense into the washload, they are non-dusting and thus their components are less irritating to sensitive skin, and they are more compact, hence facilitating more economical storage.
  • Detergent tablets containing persalt bleach without bleach sensitive ingredients are described, for example, in US 3 953 350 (Kao), JP 60 015 500A (Lion), JP 60 135 497A (Lion) and JP 60 135 498A (Lion).
  • Detergent tablets containing enzyme but no bleach are sold commercially in Spain.
  • GB 911 204 (Unilever) discloses layered detergent tablets containing sodium perborate and certain bleach activators, for example, sodium acetoxybenzene sulphonate and phthalic anhydride, and shows by means of comparative examples that tablets containing those ingredients together, without segregation into separate layers, are unstable.
  • bleach activator is a N-diacylated or N,N′-polyacylated amine, notably tetraacetylethylenediamine (TAED), such segregation is unnecessary.
  • other bleach-sensitive ingredients notably enzymes and fluorescers, can also be included without the need for segregation, thus greatly simplifying tablet manufacture.
  • Fully-formulated detergent tablets in accordance with the invention may be made simply by compressing a powder.
  • the present invention accordingly provides a tablet of compressed detergent powder comprising:
  • ingredients (a) and (b) are not segregated from one another.
  • the invention also provides a process for the preparation of a detergent tablet, which comprises the following steps:
  • the detergent tablet of the invention contains as essential ingredients inorganic persalt bleach (sodium perborate), and at least one bleach-sensitive ingredient - acylated amine bleach activator, enzyme, fluorescer - as well as surfactant, detergency builder and optionally other conventional ingredients.
  • inorganic persalt bleach sodium perborate
  • bleach-sensitive ingredient - acylated amine bleach activator enzyme, fluorescer - as well as surfactant, detergency builder and optionally other conventional ingredients.
  • the sodium perborate (a) and the bleach-sensitive ingredient or ingredients (b) are not segregated from one another in the tablet. This means in effect that those ingredients are randomly mixed with one another rather than isolated from one another in specific areas of the tablet, for example, in separate layers or inserts. It does not, however, preclude the presentation of those ingredients in any of the forms commonly used in detergent powders, for example, bleach activators as granules, enzymes as granules or marumes or coated marumes, even though these forms may involve some measure of protection, coating or dilution. However, in the tablet of the present invention, no additional measures are taken, over and above those normal in detergent powders, to keep the sodium perborate (a) and the bleach-sensitive ingredient or ingredients (b) apart.
  • the tablet of the invention is substantially homogeneous, that is to say, it is preparable by compression of a single, homogeneously mixed powder.
  • the tablet prefferably includes one or more separate layers, inserts or other measures in order to segregate ingredients other than (a) and (b).
  • the ingredients (a) and (b) are randomly mixed and distributed in at least one region of the tablet.
  • the inorganic persalt bleach employed in the detergent tablet of the invention is sodium perborate. This may be in the form of the monohydrate, the tetrahydrate, a mixture of the two, a partially dehydrated tetrahydrate, or any other stable commercially available form.
  • Sodium perborate monohydrate may be either in high-surface-area or low-surface-area form.
  • the sodium perborate is preferably present in an amount within the range of from 1 to 30 wt%, more preferably from 5 to 20 wt%.
  • the tablet of the invention contains as an essential ingredient at least one bleach sensitive ingredient selected from one of the classes (b1), (b2) and (b3). Any combination of more than one bleach-sensitive ingredients from any one or more of these classes may be present.
  • the bleach activator (b1) is the bleach activator (b1)
  • An activator for an inorganic persalt is an organic compound having one or more reactive acyl residues which cause the formation of peracids, the latter providing a more effective bleaching action at a low wash temperature, eg from 20 to 60°C, than is possible using the inorganic persalt alone.
  • the bleach activator used in the tablet of the present invention is an N-diacylated or N,N′-polyacylated amine. These materials are disclosed in GB 855 355 and GB 907 356 (Unilever). In polyamines, at least one nitrogen atom must carry two acyl groups.
  • the preferred bleach activator for use in the tablets of the present invention is tetraacetylethylenediamine (TAED).
  • the ratio by weight of the inorganic persalt (sodium perborate) to the bleach activator in the tablet of the invention may vary from about 30:1 to about 1:1, and is preferably from 15:1 to 2:1.
  • TAED is conveniently employed in granular form, on an inorganic carrier.
  • the amount of TAED itself in the tablet of the invention is preferably from 1 to 15 wt%, more preferably from 2 to 10 wt%.
  • Suitable enzymes include the various proteases, cellulases, lipases, amylases, and mixtures thereof, which are designed to remove a variety of soils and stains from fabrics.
  • the present invention is particularly concerned with proteolytic enzymes (proteases).
  • Preferred proteases are normally solid, catalytically active protein materials which degrade or alter protein types of stains when present as in fabric stains in a hydrolysis reaction. They may be of any suitable origin, such as vegetable, animal, bacterial or yeast origin.
  • proteases of various qualities and origins and having activity in various pH ranges of from 4-12 are available and can be used in the detergent tablet of the invention.
  • suitable proteases are the subtilisins, which are obtained from particular strains of B. subtilis and B. licheniformis , such as the commercially available subtilisins Maxatase (Trade Mark), as supplied by Gist-Brocades N.V., Delft, Holland, and Alcalase (Trade Mark), as supplied by Novo Industri A/S, Copenhagen, Denmark.
  • protease obtained from a strain of Bacillus having maximum activity throughout the pH range of 8-12, being commercially available, e.g. from Novo Industri A/S under the registered trade-names Esperase (Trade Mark) and Savinase (Trade-Mark).
  • Esperase Trade Mark
  • Savinase Trade-Mark
  • Other commercial proteases are Kazusase (Trade Mark) (obtainable from Showa-Denko of Japan), Optimase (Trade Mark) (from Miles Kali-Chemie, Hannover, West Germany), and Superase (Trade Mark) (obtainable from Pfizer of U.S.A.).
  • Detergency enzymes are commonly employed in the form of granules or marumes, optionally with a protective coating, in amounts of from about 0.1% to about 3.0% by weight.
  • fluorescer optical brightener
  • Any fluorescer (optical brightener) suitable for use in a detergent powder may be used in the detergent tablet of the present invention.
  • fluorescers are those belonging to the classes of diaminostilbene-sulphonic acid derivatives, diarylpyrazoline derivatives and bisphenyl-distyryl derivatives.
  • diaminostilbene-sulphonic acid derivative type of fluorescer examples include disodium 4,4′-bis-(2- diethanolamino-4-anilino-s-triazin-6-­ylamino) stilbene- 2:2′-disulphonate, disodium 4,4′-bis-(2-morpholino-4-anilino-s-triazin-6-ylamino­stilbene-2:2′-disulphonate, disodium 4,4′-bis-(2,4-dianilino-s-triazin-6-ylamino) stilbene-2:2′-disulphonate, disodium 4,4′-bis-(2-­anilino-4-(N-methyl-N-2-hydroxyethylamino)-s-triazin-6-­ylamino) stilbene-2,2′-disulphonate, disodium 4,4′-bis­(4-phenyl-2,1,3-triazol-2-yl) stilbene-2,2′-bis
  • Tinopal DMS is disodium 4,4′bis-(2-morpholino-4-anilino-s-triazin-6-ylamino) stilbene disulphonate
  • Tinopal CBS is disodium 2,2′-­bis-(phenyl-styryl) disulphonate.
  • fluorescers suitable for use in the invention include the 1,3-diaryl pyrazolines and the 7-alkylaminocoumarins.
  • Fluorescer is preferably present in an amount within the range of from 0.02 to 0.8 wt%, more preferably from 0.03 to 0.5 wt%.
  • the total amount of detergent-active material (surfactant) in the detergent tablet of the invention is suitably from 2 to 50% by weight, and is preferably from 5 to 40% by weight.
  • the detergent tablet of the invention may contain one or more soap or non-soap anionic, nonionic, cationic, amphoteric or zwitterionic surfactants, or combinations of these.
  • suitable detergent-active compounds are available and are fully described in the literature, for example, in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch.
  • the preferred detergent-active compounds that can be used are soaps and synthetic non-soap anionic surfactants and nonionic surfactants.
  • Synthetic anionic surfactants are well known to those skilled in the art. Examples include alkylbenzene sulphonates, particularly sodium linear alkylbenzene sulphonates having an alkyl chain length of C8-C15; primary and secondary alkyl sulphates, particularly sodium C12-C15 primary alcohol sulphates; olefin sulphonates; alkane sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.
  • alkylbenzene sulphonates particularly sodium linear alkylbenzene sulphonates having an alkyl chain length of C8-C15
  • primary and secondary alkyl sulphates particularly sodium C12-C15 primary alcohol sulphates
  • olefin sulphonates alkane sulphonates
  • dialkyl sulphosuccinates and fatty acid ester sulphonates.
  • Suitable nonionic detergent compounds which may be used include in particular the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene oxides, especially ethylene oxide either alone or with propylene oxide.
  • nonionic detergent compounds are alkyl (C 6-22 ) phenol-ethylene oxide condensates, the condensation products of linear or branched aliphatic C 8-20 primary or secondary alcohols wih ethylene oxide, and products made by condensation of ethylene oxide with the reaction products of propylene oxide and ehylenediamine.
  • Other so-called nonionic detergent compounds include long-chain tertiary amine oxides, tertiary phosphine oxides, and dialkyl sulphoxides.
  • the primary and secondary alcohol ethoxylates especially the C 12-15 primary and secondary alcohols ethoxylated with an average of from 5 to 20 moles of ethylene oxide per mole of alcohol.
  • soaps of fatty acids are preferably sodium soaps derived from naturally occurring fatty acids, for example, the fatty acids from coconut oil, beef tallow, sunflower or hardened rape seed oil.
  • Detergent compositions suitable for use in automatic fabric washing machines generally contain anionic surfactant, or nonionic surfactant, or a combination of the two in any proportions. Soap may also be present if desired, in any amount from 0 to 40% by weight of the composition. Generally, compositions of this type may successfully be presented in the form of tablets in accordance with the present invention.
  • the detergent tablets of the invention contain one or more detergency builders, suitably in an amount of from 5 to 80 wt%, preferably from 20 to 80 wt%.
  • alkali metal phosphates Especially preferred are alkali metal phosphates, alkali metal aluminosilicates, and combinations thereof.
  • Preferred alkali metal phosphates are sodium orthophosphate, sodium pyrophosphate and sodium tripolyphosphate.
  • Sodium tripolyphosphate is especially preferred. It may generally be present in amounts up to 50% by weight of the composition.
  • Alkali metal (preferably sodium) aluminosilicates may generally be incorporated in amounts up to 60% by weight of the composition, and may be either crystalline or amorphous or mixtures thereof, having the general formula: 0.8-1.5 Na2O. Al2O3.0.8-6 SiO2
  • the preferred sodium aluminosilicates contain 1.5-3.5 SiO2 units (in the formula above). Both the amorphous and the crystalline materials can be prepared readily by reaction between sodium silicate and sodium aluminate, as amply described in the literature.
  • Suitable crystalline sodium aluminosilicate ion-exchange detergency builders are described, for example, in GB 1 429 143 (Proctor & Gamble).
  • the preferred sodium aluminosilicates of this type are the well-known commercially available zeolites A and X, and mixtures thereof. Especially preferred is zeolite 4A.
  • Inorganic builders that may be present include alkali metal (generally sodium) carbonate; while organic builders include nitrilotriacetates, citrates and carboxymethyloxysuccinates.
  • Especially preferred supplementary builders are polycarboxylate polymers, especially those containing (meth)acrylate and/or maleate units. These polymers also provide certain additional benefits, for example, reduced soil redisposition.
  • the polymers are suitably used in amounts of from 0.5 to 10% wt%, more preferably from 1 to 6 wt%.
  • the polymers may be in acid form or in wholly or partially neutralised salt form.
  • Preferred polymers are homopolymers and copolymers of acrylic acid.
  • anti-redeposition agents such as sodium carboxymethylcellulose, polyvinyl pyrrolidone and the cellulose ethers such as methyl cellulose and ethyl hydroxyethyl cellulose; stabilisers such as ethylenediamine tetramethylene phosphonate and diethylenetriamine pentamethylene phosphonate; fabric-softening agents; lather control agents or lather boosters as appropriate; heavy metal sequestrants such as EDTA; perfumes; colourants; and inorganic salts such as sodium and magnesium sulphate.
  • Sodium sulphate may if desired be present as a filler material in amounts up to 40% by weight of the composition; however as little as 10% or less by weight of the composition of sodium sulphate, or even none at all, may be present.
  • An antifoam material is advantageously included in the detergent tablet of the invention, especially if the tablet is primarily intended for use in front-loading drum-type automatic washing machines.
  • Suitable antifoam materials are usually in granular form, such as those described in EP 266 863A (Unilever).
  • Such antifoam granules typically comprise a mixture of silicone oil, petroleum jelly, hydrophobic silica and alkyl phosphate as antifoam active material, sorbed onto a porous absorbent water-soluble carbonate-based inorganic carrier material.
  • Antifoam granules may be present in any amount up to 5% by weight of the composition.
  • an amount of an alkali metal silicate particularly sodium ortho-, meta- or preferably neutral or alkaline silicate.
  • alkali metal silicates at levels, for examples of 0.1 to 10 wt%, may be advantageous in providing protection against the corrosion of metal parts in washing machines, besides providing some measure of building and giving processing benefits.
  • the detergent compositions of the invention are made into tablet form by compression of a powder.
  • the tablets of the invention are substantially homogeneous, that is to say, they are formed by compression of a single, substantially homogeneous powder without the addition of inserts, separate layers containing segregated ingredients, coatings, etc.; this greatly facilitates manufacture.
  • the starting powder it is also within the scope of the invention, for example, for the starting powder to contain inserts or other local regions of segregation that will persist into the tablet; or for two or more different powders to be compressed to form separate layers in the final tablet; the only proviso being that the ingredients (a) and (b) should not be segregated.
  • the powder itself may be made by any suitable method, for example, mixing, granulation, or any combination of these, optionally with spray-on of liquid ingredients.
  • solid ingredients may be dry-mixed, water and/or liquid ingredients added, the mixture granulated, and then dried.
  • Another method involves spray-drying an aqueous slurry of detergent components to form granules, and subsequently post-dosing heat-sensitive ingredients, such as bleach and enzymes; again liquid ingredients may be sprayed on at any suitable stage in the process.
  • One preferred process involving spray-drying comprises the steps of:
  • the detergent tablet of the invention may be, and preferably is, formulated for use as a complete heavy-duty fabric washing composition. The consumer does not need to use a mix of tablets having different compositions.
  • each tablet may contain sufficient of all the components to provide the correct amount required for an average washload, it is preferred that each tablet should contain a submultiple quantity of the composition required for average washing conditions, so that the consumer may vary the dosage according to the size and nature of the washload.
  • tablet sizes may be chosen such that two tablets are sufficient for an average washload; one or more further tablets may be added if the washload is particularly large or soiled; and one only tablet may be used if the load is small or only lightly soiled.
  • a zero-phosphate detergent base powder containing fluorescer was prepared to the following composition by spray-drying, followed by spray-on of the 3EO nonionic surfactant: % Linear alkylbenzene sulphonate 9.2 C12-C15 7EO nonionic surfactant 4.2 C13-C15 3EO nonionic surfactant 9.2 Fatty acid soap 2.5 Zeolite 4A (anhydrous basis) 36.8 Acrylic/maleic copolymer (Sokalan* CP5) 6.0 Sodium silicate 0.7 Sodium carboxymethyl cellulose 0.8 Fluorescers (Tinopal** DMS and Tinopal** CBS-X) 0.3 Sodium carbonate 12.9 Water to 100.0 *Trade Mark; ex BASF AG, Ludwigshafen, Germany. **Trade Mark; ex Ciba-Geigy AG, Basel, Switzerland.
  • Tablets and powders were prepared to the compositions given below.
  • the enzyme was the granular protease Savinase (Trade Mark) 6.0T, the sodium perborate was high-surface-area (5.9 m2/g) monohydrate, and the TAED was in granular form (83 wt% TAED, 17 wt% inert zero-phosphate carrier).
  • Tablets were made by compressing the powders at 1.5 kN by means of an Instron (Trade Mark) constant speed extensiometer, using a crosshead speed of 100 mm/min. Each tablet weighed 60 g and had a diameter of 53 mm and a thickness of about 25 mm.
  • Instron Trade Mark
  • the bleach, fluorescer and enzyme performances of the tablets and powders were compared for the freshly made compositions, and after 1 week's and 2 weeks' storage under severe conditions (37°C and 70% relative humidity, unprotected, no carton).
  • the comparisons were carried out by washing selected testcloths in the tergotometer using a 40°C isothermal wash for 15 minutes in 1 litre of 12° (French) hard water.
  • the tablets were crushed prior to the wash, and dosed at 5 g/litre; the powders were also dosed at 5 g/litre.
  • Table 1 shows the enzyme results, obtained using an enzyme-sensitive testcloth (casein soil on polyester/cotton fabric), expressed as reflectance differences (delta R at 460 nm).
  • Table 1 Time (weeks) Example 0 1 2 1 (tablet) 26.9 26.8 26.9 P (powder) 27.0 26.6 26.4
  • Table 2 shows the fluorescer results, obtained using a fluorescer-sensitive testcloth, and expressed as the difference between the reflectances (delta R 460) in the presence and in the absence of ultraviolet light.
  • Table 2 Time (weeks) Example 0 1 2 1 (tablet) 15.7 16.6 15.7 P (powder) 15.6 16.2 15.3
  • Table 3 shows the bleach results, obtained using a tea-stained cotton testcloth and expressed as reflectance differences (delta R at 460 nm).
  • Table 3 Time (weeks) Example 0 1 2 1 (tablet) 5.3 4.3 4.0 P (powder) 3.8 3.1 3.2
  • a phosphate-built base detergent base powder containing fluorescer was prepared to the following composition by spray-drying, followed by spray-on of the 3EO nonionic surfactant: % Linear alkylbenzene sulphonate 8.3 C12-C15 7EO nonionic surfactant 5.3 C13-C15 3EO nonionic surfactant 3.5 Fatty acid soap 0.7 Sodium tripolyphosphate 29.3 Acrylic/maleic copolymer (Sokalan CP5) 1.2 Sodium silicate 7.0 Sodium carboxymethyl cellulose 0.4 EDTA 0.15 Fluorescers (Tinopal DMS and Tinopal CBS-X) 0.35 Sodium carbonate 5.9 Sodium sulphate, water to 100.0
  • Example 2 Tablets and powders were prepared as described in Example 1 to the compositions given below.
  • the enzyme, sodium perborate monohydrate and TAED were as in Example 1.
  • Example 2 Q Tablet Powder Base 85.4 85.4 Enzyme 1.0 1.0 Perborate 10.0 10.0 TAED granules 3.6 3.6
  • Example 1 The bleach, fluorescer and enzyme performances of the tablets and powders were compared as described in Example 1. Enzyme results are shown in Table 4, fluorescer results in Table 5, and bleach results in Table 6. Table 4 (enzyme) Time (weeks) Example 0 1 2 2 (tablet) 26.6 27.1 25.8 Q (powder) 26.8 26.1 25.7 Table 5 (fluorescer) Time (weeks) Example 0 1 2 2 (tablet) 16.1 15.4 15.6 Q (powder) 15.0 15.5 15.3
  • Tablets and powders were prepared to the following compositions, Examples 3, 4 and 5 being tablets and Examples R, S and T being powders: Example 3, R 4, S 5, T Base 89.0 89.0 84.0 Enzyme 1.0 1.0 1.0 Perborate : Mono (HSA) 10.0 - - Mono (LSA) - 10.0 - Tetra - - 15.0
  • Example 6 The exercise of Examples 3 to 5 was repeated using a similar series of compositions additionally containing TAED (83 wt% zero-phosphate granules as used in Example 1). Tablets and powders were prepared to the following compositions, Examples 6, 7 and 8 being tablets and Examples U, V and W being powders: Example 6, U 7, V 8, W Base 85.4 85.4 80.4 Enzyme 1.0 1.0 1.0 Perborate : Mono (HSA) 10.0 - - Mono (LSA) 10.0 - Tetra - 15.0 TAED granules 3.6 3.6 3.6 3.6 3.6
  • Examples 3 and 6 were repeated using the phosphate-built base powder of Example 2 instead of the zero-phosphate base powder of Example 1. Tablets and powders were prepared to the following compositions, Examples 9 and 10 being tablets and Examples X and Y being powders: Example 9, X 10, Y Base 89.0 85.4 Enzyme 1.0 1.0 Perborate (mono, HSA) 10.0 10.0 TAED granules - 3.6
  • a phosphate-built detergent powder containing sodium perborate tetrahydrate bleach in conjunction with proteolytic enzyme (Savinase) and fluorescers was prepared, by spray-drying and postdosing, to the following composition: % Linear alkylbenzene sulphonate 18.0 C12-C15 7EO nonionic surfactant 8.0 Fatty acid soap 2.0 Sodium tripolyphosphate 30.0 Acrylic/maleic copolymer (Sokalan CP5) 1.5 Alkaline sodium silicate 10.0 Sodium carboxymethyl cellulose 0.5 EDTA 0.25 Fluorescers: Tinopal DMS 0.13 Tinopal CBS-X 0.08 Sodium sulphate 3.6 Sodium perborate tetrahydrate 10.0 Enzyme (Savinase 6CM) 0.75 Antifoam granules 3.0 Perfume 0.22 Moisture, salts to 100.0
  • the powder had a bulk density of 400-425 g/litre. It was compressed to approximately half its volume, using a pilot-scale tabletting machine, to form tablets weighing 32 g and having a diameter of 50 mm and a height of 23 mm.
  • the tablets displayed effective washing and cleaning performance in the washing machine, two tablets being an appropriate dosage for soft water and three for hard water.
  • a phosphate-built detergent powder containing sodium perborate tetrahydrate bleach in conjunction with TAED granules, proteolytic enzyme (Savinase) and fluorescers was prepared, by spray-drying and postdosing, to the following composition, and then compressed as described in Example 11 to form tablets: % Linear alkylbenzene sulphonate 18.0 C12-C15 7EO nonionic surfactant 8.0 Fatty acid soap 2.0 Sodium tripolyphosphate 30.0 Acrylic/maleic copolymer (Sokalan CP5) 1.5 Alkaline sodium silicate 10.0 Sodium carboxymethyl cellulose 0.5 EDTA 0.25 Fluorescers: Tinopal DMS 0.13 Tinopal CBS-X 0.08 Sodium sulphate 1.3 Sodium perborate tetrahydrate 10.0 TAED granules (83 wt% active) 2.4 Enzyme (Savinase 6CM) 0.75 Antifoam granules 3.0 Perfume 0.
  • the tablets displayed effective cleaning and washing performance when used at a dosage of two to three tablets per wash.
  • a phosphate-built detergent powder with enhanced bleaching performance containing sodium perborate monohydrate bleach in conjunction with TAED, proteolytic enzyme (Savinase) and fluorescers, was prepared to the following composition by spray-drying and postdosing: % Linear alkylbenzene sulphonate 18.0 C12-C15 7EO nonionic surfactant 8.0 Fatty acid soap 2.0 Sodium tripolyphosphate 30.0 Acrylic/maleic copolymer (Sokalan* CP5) 1.5 Alkaline sodium silicate 10.0 Sodium carboxymethyl cellulose 0.5 EDTA 0.25 Fluorescers: Tinopal DMS 0.13 Tinopal CBS-X 0.08 Salts 4.24 Water 8.0 Sodium perborate monohydrate 10.0 TAED 3.33 Enzyme (Savinase 6CM) 0.75 Antifoam granules 3.0 Perfume 0.22
  • the powder was compressed as described in Example 11 to form tablets, each weighing 26-28 g, having a diameter of 40 mm and a thickness of 26 mm.
  • the tablets displayed effective washing and cleaning performance when used at a dosage of two or three tablets per wash.
  • zero-phosphate detergent powders containing sodium perborate monohydrate bleach in conjunction with TAED, proteolytic enzyme (Savinase) and fluorescers, prepared by spray-drying and postdosing, are suitable for compression to form 40 g tablets according to the present invention.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
EP19900304333 1989-04-24 1990-04-23 Compositions détergentes Ceased EP0395333A3 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP99122669A EP0987320A3 (fr) 1989-04-24 1990-04-23 Compositions détergentes

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB8909254 1989-04-24
GB898909254A GB8909254D0 (en) 1989-04-24 1989-04-24 Detergent compositions
GB9007271 1990-03-30
GB9007271A GB2240110B (en) 1989-04-24 1990-03-30 Detergent tablets

Related Child Applications (1)

Application Number Title Priority Date Filing Date
EP99122669A Division EP0987320A3 (fr) 1989-04-24 1990-04-23 Compositions détergentes

Publications (2)

Publication Number Publication Date
EP0395333A2 true EP0395333A2 (fr) 1990-10-31
EP0395333A3 EP0395333A3 (fr) 1991-03-20

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EP19900304333 Ceased EP0395333A3 (fr) 1989-04-24 1990-04-23 Compositions détergentes

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Country Link
EP (1) EP0395333A3 (fr)
JP (1) JPH0747760B2 (fr)
AU (1) AU647736B2 (fr)
BR (1) BR9001903A (fr)
MY (1) MY105883A (fr)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0466485A3 (en) * 1990-07-13 1992-03-04 Unilever Plc Detergent compositions
WO1992018604A1 (fr) * 1991-04-12 1992-10-29 Henkel Kommanditgesellschaft Auf Aktien Procede de production de pastilles de detergent pour machines a laver la vaisselle
WO1993000419A1 (fr) * 1991-06-27 1993-01-07 Henkel Kommanditgesellschaft Auf Aktien Procede de fabrication de produits de lavage en comprimes pour le lavage de la vaisselle en machine
EP0724012A1 (fr) * 1995-01-27 1996-07-31 The Procter & Gamble Company Composition détergente contenant un agent de blanchiment et un agent d'azurage
EP0622450A3 (fr) * 1993-04-29 1997-02-19 Amway Corp Compositions détergentes et méthodes pour leur fabrication.
US5658874A (en) * 1994-11-14 1997-08-19 Lever Brothers Company, Division Of Conopco, Inc. Production of detergent tablet compositions
US5916866A (en) * 1994-11-14 1999-06-29 Lever Brothers Company, Division Of Conopco, Inc. Preparation of laundry detergent tablets
WO1999041350A1 (fr) * 1998-02-16 1999-08-19 Henkel Kommanditgesellschaft Auf Aktien Corps moules a plusieurs phases presentant une division de phases optimisee
WO2000050557A1 (fr) * 1999-02-25 2000-08-31 Henkel Kommanditgesellschaft Auf Aktien Corps moules de produits de lavage et de nettoyage stables au stockage
GB2335435B (en) * 1997-03-24 2000-11-08 Unilever Plc Detergent compositions
WO2000071666A1 (fr) * 1999-05-21 2000-11-30 Unilever Plc Compositions de detergent
WO2001034759A1 (fr) * 1999-11-11 2001-05-17 The Procter & Gamble Company Pastilles detergentes contenant un agent de blanchiment
US6313080B1 (en) 1998-02-04 2001-11-06 Unilever Home & Personal Care, Usa Division Of Conopco, Inc. Detergent compositions
US20080045593A1 (en) * 2006-08-15 2008-02-21 Steris Inc. One part, solids containing decontamination blend composition
US20080176943A1 (en) * 2006-08-15 2008-07-24 Kaiser Herbert J One part, solids containing decontamination blend composition
WO2009040175A1 (fr) * 2007-09-24 2009-04-02 Unilever Plc Améliorations relatives à des compositions de traitement des tissus comprenant des séquestrants et des dispersants

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2053433C (fr) * 1990-10-19 1997-03-25 Michael Joseph Garvey Compositions de detergents
CA2083331C (fr) * 1991-11-26 1998-08-11 Johannes H. M. Akkermans Compositions pour detergent

Citations (4)

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DE1467595A1 (de) * 1963-05-02 1969-01-09 Henkel & Cie Gmbh Waschmitteltabletten und Verfahren zu deren Herstellung
DE3535516A1 (de) * 1985-10-04 1987-04-09 Fritz Buchner Tablettenfoermiges wasch- und reinigungsmittel, verfahren zu seiner herstellung und seine verwendung
EP0253772A2 (fr) * 1986-07-15 1988-01-20 Warner-Lambert Company Compositions contenant un agent blanchissant pour le nettoyage et/ou le lavage des dentiers
WO1990002165A1 (fr) * 1988-08-17 1990-03-08 Henkel Kommanditgesellschaft Auf Aktien Procede de preparation de tablettes de produit a lessive a teneur reduite en phosphates

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DE3169751D1 (en) * 1980-12-09 1985-05-09 Unilever Nv Bleach activator granules
JPS57142910A (en) * 1981-02-28 1982-09-03 Sankin Kogyo Kk Water-soluble solid agent for cleaning artificial denture
DE3812693A1 (de) * 1988-03-19 1989-09-28 Reckitt Gmbh Reinigungstablette fuer zahnprothesen
GB8810954D0 (en) * 1988-05-09 1988-06-15 Unilever Plc Enzymatic detergent & bleaching composition
GB8824108D0 (en) * 1988-10-14 1988-11-23 Unilever Plc Bleaching & detergent compositions

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1467595A1 (de) * 1963-05-02 1969-01-09 Henkel & Cie Gmbh Waschmitteltabletten und Verfahren zu deren Herstellung
DE3535516A1 (de) * 1985-10-04 1987-04-09 Fritz Buchner Tablettenfoermiges wasch- und reinigungsmittel, verfahren zu seiner herstellung und seine verwendung
EP0253772A2 (fr) * 1986-07-15 1988-01-20 Warner-Lambert Company Compositions contenant un agent blanchissant pour le nettoyage et/ou le lavage des dentiers
WO1990002165A1 (fr) * 1988-08-17 1990-03-08 Henkel Kommanditgesellschaft Auf Aktien Procede de preparation de tablettes de produit a lessive a teneur reduite en phosphates

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H. STACHE, H. GROSSMANN: "WASCHMITTEL", SPRINGER, BERLIN *

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0466485A3 (en) * 1990-07-13 1992-03-04 Unilever Plc Detergent compositions
US5225100A (en) * 1990-07-13 1993-07-06 Lever Brothers Company, Division Of Conopco, Inc. Detergent compositions
WO1992018604A1 (fr) * 1991-04-12 1992-10-29 Henkel Kommanditgesellschaft Auf Aktien Procede de production de pastilles de detergent pour machines a laver la vaisselle
US5358655A (en) * 1991-04-12 1994-10-25 Henkel Kommanditgesellschaft Auf Aktien Process for the production of detergent tablets for dishwashing machines
WO1993000419A1 (fr) * 1991-06-27 1993-01-07 Henkel Kommanditgesellschaft Auf Aktien Procede de fabrication de produits de lavage en comprimes pour le lavage de la vaisselle en machine
EP0622450A3 (fr) * 1993-04-29 1997-02-19 Amway Corp Compositions détergentes et méthodes pour leur fabrication.
US5658874A (en) * 1994-11-14 1997-08-19 Lever Brothers Company, Division Of Conopco, Inc. Production of detergent tablet compositions
US5916866A (en) * 1994-11-14 1999-06-29 Lever Brothers Company, Division Of Conopco, Inc. Preparation of laundry detergent tablets
EP0724012A1 (fr) * 1995-01-27 1996-07-31 The Procter & Gamble Company Composition détergente contenant un agent de blanchiment et un agent d'azurage
EP0956332B1 (fr) * 1997-03-24 2002-02-13 Unilever Plc Compositions detergentes
GB2335435B (en) * 1997-03-24 2000-11-08 Unilever Plc Detergent compositions
US6313080B1 (en) 1998-02-04 2001-11-06 Unilever Home & Personal Care, Usa Division Of Conopco, Inc. Detergent compositions
WO1999041350A1 (fr) * 1998-02-16 1999-08-19 Henkel Kommanditgesellschaft Auf Aktien Corps moules a plusieurs phases presentant une division de phases optimisee
WO2000050557A1 (fr) * 1999-02-25 2000-08-31 Henkel Kommanditgesellschaft Auf Aktien Corps moules de produits de lavage et de nettoyage stables au stockage
WO2000071666A1 (fr) * 1999-05-21 2000-11-30 Unilever Plc Compositions de detergent
US6387861B1 (en) 1999-05-21 2002-05-14 Unilever Home & Personal Care Usa Division Of Conopco, Inc. Detergent compositions
WO2001034759A1 (fr) * 1999-11-11 2001-05-17 The Procter & Gamble Company Pastilles detergentes contenant un agent de blanchiment
US20080045593A1 (en) * 2006-08-15 2008-02-21 Steris Inc. One part, solids containing decontamination blend composition
US20080176943A1 (en) * 2006-08-15 2008-07-24 Kaiser Herbert J One part, solids containing decontamination blend composition
US9700644B2 (en) * 2006-08-15 2017-07-11 American Sterilizer Company One part, solids containing decontamination blend composition
US9724550B2 (en) * 2006-08-15 2017-08-08 American Sterilizer Company One part, solids containing decontamination blend composition
WO2009040175A1 (fr) * 2007-09-24 2009-04-02 Unilever Plc Améliorations relatives à des compositions de traitement des tissus comprenant des séquestrants et des dispersants

Also Published As

Publication number Publication date
EP0395333A3 (fr) 1991-03-20
JPH0317199A (ja) 1991-01-25
AU5376490A (en) 1990-10-25
JPH0747760B2 (ja) 1995-05-24
AU647736B2 (en) 1994-03-31
BR9001903A (pt) 1991-07-30
MY105883A (en) 1995-02-28

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