EP1397475A2 - Poudres compactables - Google Patents

Poudres compactables

Info

Publication number
EP1397475A2
EP1397475A2 EP02735380A EP02735380A EP1397475A2 EP 1397475 A2 EP1397475 A2 EP 1397475A2 EP 02735380 A EP02735380 A EP 02735380A EP 02735380 A EP02735380 A EP 02735380A EP 1397475 A2 EP1397475 A2 EP 1397475A2
Authority
EP
European Patent Office
Prior art keywords
surfactant
solid
powder
particles
less
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Withdrawn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
EP02735380A
Other languages
German (de)
English (en)
Inventor
Hendrick Petrus Frick
Richard Malcolm Clapperton
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.)
Huntsman International LLC
Original Assignee
Huntsman International LLC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from GB0113155A external-priority patent/GB0113155D0/en
Priority claimed from GB0205718A external-priority patent/GB0205718D0/en
Priority claimed from GB0208336A external-priority patent/GB0208336D0/en
Priority claimed from GB0209445A external-priority patent/GB0209445D0/en
Application filed by Huntsman International LLC filed Critical Huntsman International LLC
Publication of EP1397475A2 publication Critical patent/EP1397475A2/fr
Withdrawn legal-status Critical Current

Links

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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/88—Ampholytes; Electroneutral compounds
    • C11D1/94—Mixtures with anionic, cationic or non-ionic 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/88—Ampholytes; Electroneutral 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/88—Ampholytes; Electroneutral compounds
    • C11D1/90—Betaines
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • 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
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • 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
    • C11D3/02—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
    • C11D3/128—Aluminium silicates, e.g. zeolites
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/72—Ethers of polyoxyalkylene glycols

Definitions

  • the invention relates to compactable powders suitable for making tablets, e.g. laundry- tablets, or bath bombs, which comprise surfactant and a particulate solid, and which can be added to aqueous systems, for example, washing machines, dishwashers, or bath- or other wash water, as a unit dose, and to tablets prepared by compacting such powders. It is especially applicable to laundry tablets. It is also useful for formulating, pesticide unit dose tablets, e.g. for horticultural applications, or sterilising tablets.
  • Laundry tablets typically comprise as their main ingredients a surfactant mixture and a solid builder.
  • the surfactant mixture typically comprises an anionic surfactant, often with a minor proportion of nonionic, and the builder is usually sodium tripolyphosphate, or less commonly, zeolite.
  • the problem has been met mainly by controlling particle size, by including rapidly soluble particles, such as phase 1 sodium tripolyphosphate, by choice of surfactant/solid ratio and by adding water swellable polymers.
  • Tablets are usually made from a base powder which is a spray dried or fluid-bed granulated mixture of those components of the tablet which are stable and compatible with water and with one another, under the conditions of spray drying or granulation.
  • the powder is blended with the remaining components, e.g. those which are sensitive to water, and the blend is then compressed into a tablet.
  • the tablets comprise a substantially higher concentration of wash-functional components than conventional powders because there is relatively little need for diluents, such as sodium sulphate, needed to make powders free flowing.
  • the compaction pressure is adjusted to give a specified compression-fracture-strength (e.g. 70-80N).
  • Sodium tripolyphosphate may exist in any one of three forms: phase 1 anhydrous; phase 2 anhydrous; and hexahydrate. Commercial products often comprise a mixture of two or more of these phases. Spray dried powders contain only the hexahydrate. In general products containing relatively high proportions of phase 1 anhydrous tripolyphosphate dissolve more rapidly than either phase 2 or hexahydrate. However pure phase 1 crystals, on immersion, form a cement like composition which inhibits the disintegration of the tablet. This can be avoided if a small amount, e.g. 2 to 6% by weight of moisture is present in the crystal.
  • a substantial proportion of any tripolyphosphate in a laundry tablet is therefore usually present as crystals, containing low proportions of phase 2, high proportions of phase 1 and a small amount of moisture, which are blended with the base powder.
  • Other rapidly dissolving solids may be incorporated in the tablet as may water swellable polymers or effervescent mixtures such as citric acid and sodium bicarbonate, which aid disintegration.
  • the size of the laundry tablet has been largely fixed by the optimum dose of wash- functional laundry solids required for an average wash load, which is about 80g. To provide flexibility to cope with very light or extra heavy loads the standard tablet is half this amount (i.e. 40g) thereby enabling 40, 80 or 120g dosages to be achieved by the use of one or more tablets.
  • the invention is also applicable to bath bombs.
  • the latter conventionally comprise a source of effervescence, e.g. a mixture of a salt of carbonic acid (typically sodium bicarbonate) with a water-soluble acid (typically citric acid).
  • a source of effervescence e.g. a mixture of a salt of carbonic acid (typically sodium bicarbonate) with a water-soluble acid (typically citric acid).
  • the mixture is compacted into a tablet, which disintegrates in a burst of effervescence on addition to bath water.
  • the latter is softened by the dissolved components.
  • laundry tablets wherein the surfactant consists essentially of nonionic and amphoteric surfactants, give superior performance in soil removal compared to tablets containing anionic and non-ionic surfactants.
  • amphoteric surfactant is used herein to include those surfactants, which are more accurately described as zwitterionic.
  • amphoteric surfactants are those of the betaine type, which are made commercially by reacting sodium chloroacetate with an amine, e.g. a tertiary amine comprising at least one long chain alkyl group, an imidazoline or amido amine. Sulphobetaines and phosphobetaines are made by analogous methods. The products are usually prepared at a concentration of about 31-35% surfactant. Attempts to concentrate these products above 36 or 37% have resulted in phase separation or given rise to intractable mesophases. Spray-drying amphoteric surfactants normally gives rise to hygroscopic solids.
  • amphoteric surfactants normally contain from 16 to 20% by weight of sodium chloride, based on the total weight of amphoteric surfactant. This typically corresponds to about 6 to 10% of inorganic salts, by weight, based on the total weight of aqueous surfactant.
  • various methods have been proposed for removing salt from imidazolines, including membrane filtration and electroosmosis. Imidazolines containing low concentrations of inorganic salts, e.g. below 3% and even below 1% down to 0.1 or less, are available commercially for special uses. Such products are also normally available only as relatively dilute solutions or as hygroscopic solids.
  • amphoteric surfactants derived from feedstocks with a narrow range of homologues when desalted form a non-hygroscopic solid phase.
  • tripolyphosphate builder in conventional laundry tablets is substantially in excess of that required for optimum wash performance. The excess is necessary to obtain sufficiently rapid dispersion of the surfactant.
  • reducing the amount of surfactant allows the tripolyphosphate to be reduced proportionately. Since tripolyphosphate is the largest single component, amounting to nearly half the weight of a conventional tablet, this permits the preparation of substantially smaller and more compact tablets.
  • non-ionic / amphoteric based tablets wherein at least part of the amphoteric surfactant is blended with the other solid components in the form of a substantially anhydrous solid, which is preferably a low salt, non-hygrosopic solid, exhibit a desirable combination of strength, solubility and storage stability.
  • effervescable solid mixtures can be blended with substantially anhydrous amphoteric surfactants to form commercially acceptable foaming bath bombs.
  • the strength of the tablet is increased, if at least part of the non-ionic surfactant is adsorbed onto or absorbed in a solid particulate substrate, such as bentonite, prior to incorporation into the powder.
  • a solid particulate substrate such as bentonite
  • the invention provides a powder capable of compaction into tablets, which is formed by blending a solid surfactant with water-swellable and/or water soluble particles comprising inorganic solids and/or polymers, characterised in that the solid surfactant comprises particles consisting essentially of amphoteric surfactant.
  • the particles of amphoteric surfactant preferably contain less than 12%, more preferably, less than 10%, most preferably less than 8%, based on the weight of amphoteric surfactant, of moisture.
  • the solid surfactant consists essentially of amphoteric surfactant and is a substantially non-hygroscopic solid containing less than 12% of sodium chloride, based on the weight of amphoteric surfactant.
  • the mean particle size, and preferably the size of at least the majority of particles, of the amphoteric surfactant is preferably greater than 300 ⁇ , more preferably greater than 500 ⁇ , most preferably greater than 700 ⁇ , usually greater than 750 ⁇ , especially greater than lOOO ⁇ . It is preferred that the mean particle size, and preferably also the major proportion by weight, of the amphoteric surfactant particles, is less than 4mm, more preferably less than 3 mm, most preferably less than 2mm, especially less than 1.5mm.
  • the proportion, by weight, of the solid amphoteric surfactant, which is less than 250 ⁇ , is preferably less than 10%, more preferably less than 5%, most preferably less than 2%, especially less than 1%.
  • references herein to particles of greater than or less than a given size are to be construed in its normal sense as referring to particles respectively retained by, or passing through, a sieve of the appropriate pore size, where the particles are approximately spheroidal, e.g. where the ratio of the biggest dimension to the smallest is less than about 1.5.
  • particle size refers to the longest dimension, whereas sieves tend to segregate needles according to their shortest dimension.
  • the particles comprising inorganic solid preferably comprise a builder, an effervescible mixture, a pesticide or a sterilant.
  • the surfactant preferably consists essentially of non-ionic and amphoteric surfactant.
  • the powder preferably comprises a mixture of surfactants consisting essentially of amphoteric and non-ionic surfactants.
  • the invention provides a powder comprising a solid particulate mixture, which is capable of effervescing on contact with water, and a solid, amphoteric surfactant said surfactant containing less than 10% of moisture, based on the weight of said surfactant, and preferably less than 12% sodium chloride.
  • the solid particulate mixture which is capable of effervescing in water, is preferably a mixture of sodium bicarbonate and citric acid.
  • the invention provides a powder comprising: (A) non-hygroscopic particles consisting of at least 80%, preferably at least 90%, by weight of amphoteric surfactant; and (B) water soluble and/or water swellable particles comprising inorganic solids and/or polymers; all said particles, preferably, having a mean particle size between 400 ⁇ and 4mm,and less than 5% by weight passing a 250 ⁇ sieve.
  • the invention provides a powder comprising a non-ionic surfactant and a solid, particulate builder characterised in that said powder additionally comprises a solid, particulate amphoteric surfactant and a smectite clay.
  • the invention provides a powder comprising a solid amphoteric surfactant, a liquid non-ionic surfactant and inorganic solid particles, capable of adsorbing or absorbing at least part of said non-ionic surfactant, characterised in that at least part of said non-ionic surfactant is premixed with at least part of said solid particles.
  • the invention provides a tablet, or region of a tablet, made by compacting a powder of the invention.
  • amphoteric surfactants it is possible to include all the amphoteric surfactant in the binder and even to dry mix all the ingredients, saving on drying costs. We strongly prefer to manufacture by dry- mixing.
  • a seventh embodiment of our invention therefore provides a method of preparing a laundry detergent which comprises blending together particles of a solid amphoteric surfactant containing less than 12% moisture based on the weight thereof and solid particles of builder and preferably compacting the blend to form a tablet.
  • the invention provides a method of making a unit dose cleaning tablet comprising surfactant, which comprises the steps of (1) blending a spray dried or granulated base powder comprising at least sufficient inorganic solids to provide a free flowing powder, and optionally part of said surfactant, with a binder comprising at least part of said surfactant, to form a substantially solid blend and (2) compacting said blend to form said tablet, characterised in that said surfactant consists essentially of non-ionic and amphoteric surfactant and that said binder comprises at least part of said amphoteric surfactant, said part of said amphoteric surfactant preferably containing less than 10% moisture and, preferably, less than 12% of sodium chloride, based on the weight thereof.
  • the invention provides a method of preparing a detergent powder, which comprises mixing together: a solid, amphoteric surfactant; a liquid, non-ionic surfactant; and a particulate, inorganic solid, capable of absorbing or adsorbing at least part of said non-ionic surfactant; characterised in that, from 20 to 95% of the total weight of said liquid non-ionic surfactant is premixed with said inorganic solid to form a solid, particulate premix comprising particles of said inorganic solid having said non-ionic surfactant adsorbed thereon or absorbed therein, said premix is mixed with said solid amphoteric surfactant to form a mixture, and from 5 to 80% of the total weight of said non-ionic surfactant is added to said mixture as a liquid.
  • premix comprises particles of clay.
  • mixture contains particles comprising builders, diluents, water-swellable polymers and/or wash adjuvants.
  • the premixed non-ionic surfactant, and any non-ionic surfactant added subsequently to the mixture, may be the same or different.
  • the surfactant consists essentially of amphoteric and non-ionic surfactants.
  • anionic and cationic surfactants which tend to reduce the soil removing effectiveness of amphoteric / non-ionic mixtures, are substantially absent, i.e. not present in amounts sufficient, materially, to affect the soil removing performance of the surfactant mixture.
  • anionic and cationic surfactants being present in laundry detergents of the invention in amounts less than 10% by weight of the total surfactant, preferably less than 5%, usually less than 2%, often less than 1%, ideally less than 0.5%.
  • the builder for use according to our invention preferably comprises sodium tripolyphosphate, and most preferably sodium tripolyphosphate crystals containing more than 60% by weight thereof of phase I, and 1 to 10%, more preferably 2 to 6%, by weight, of moisture.
  • the builder may, for example, comprise zeolite, sodium or potassium carbonate, sodium or potassium citrate, sodium silicate, potassium pyrophosphate, sodium or potassium ethylenediamine tetracetate, sodium or potassium nitrilo triacetate, or a polycarboxylate.
  • the diluent typically comprises sodium sulphate, although any inert particulate solid could be used.
  • Wash adjuvants may, for example, include: bleach, such as sodium perborate or sodium percarbonate; bleach activators, such as tetraacetyl ethylenediamine; enzymes, such as proteases, Upases and/or cellulases; phosphonates, such as amino tris (methylene phosphonates), ethylene diamine tetrakis (methylene phosphonates) and diethylenetriamine pentakis (methylene phosphonates); antifoams, such as silicone antifoams or mineral oils; antiredeposition agents, such as sodium carboxymethylcellulose; optical brighteners; alkalis; fabric conditioners, such as bentonite or ditallowyl betaines; perfumes; preservatives; pigments; dyes and/or polymers.
  • bleach such as sodium perborate or sodium percarbonate
  • bleach activators such as tetraacetyl ethylenediamine
  • enzymes such as proteases, Upases and/or cellulases
  • the surfactant may be as little as 0.25%, preferably more than 0.5%, most preferably more than 1% of the total weight of the tablet. It is preferably less than 5%, more preferably less than 3%, most preferably less than 2%, by weight, of the bath bomb. However for most other applications the surfactant generally constitutes more than 2%, preferably more than 5%, more preferably more than 9%, most preferably more than 10%, sometimes more than 20% and in certain cases more than 30%, or even more than 40%, of the total weight of the tablet. Usually the total proportion of surfactant is less than 60%, generally less than 50%, and for most purposes less than 40%, preferably less than 30%, more preferably less than 20%, often less than 15%, based on the total weight of the tablet.
  • the surfactant preferably comprises non-ionic surfactant, and in particular, non-ionic polyethoxylates, most preferably alkyl polyethoxylates having straight chain or branched alkyl or alkenyl groups with from 8 to 25, preferably 10 to 20 carbon atoms and an average of 1 to 60, e.g. 2 to 50, especially 3 to 10, ethylenoxy groups.
  • HLB of the non-ionic surfactant, or mean HLB of the mixture of non-ionic surfactants is greater than 8, preferably greater than 9, more preferably greater than 10, most preferably greater than 10.5, usually greater than 10.5, e.g. greater than 11, but less thanl ⁇ , preferably less than 15, more preferably less than 14, e.g. less than 13.
  • the non-ionic surfactant may optionally comprise, in addition to or instead of alkyl ethoxylates, other ethoxylates including fatty acid ethoxylate, fatty ester ethoxylate, e.g. sorbitan or glyceryl ester ethoxylates, amine ethoxylate, alkyl phenyl ethoxylates, polyoxypropylene ethoxylates, ethoxylated alkanolamides and ethoxylated phosphate esters.
  • alkyl ethoxylates other ethoxylates including fatty acid ethoxylate, fatty ester ethoxylate, e.g. sorbitan or glyceryl ester ethoxylates, amine ethoxylate, alkyl phenyl ethoxylates, polyoxypropylene ethoxylates, ethoxylated alkanolamides and ethoxylated
  • the product may contain alkyl polyglycosides.
  • the product may also contain sugar esters, alkanolamides, and/or amine oxides. The last are considered to be non-ionic surfactants for the purpose of this specification, notwithstanding the fact that they are sometimes classified separately in the literature.
  • the non-ionic surfactant preferably constitutes more than 20%, more preferably more than 30%, most preferably more than 40%, typically more than 50%, often more than 60% and sometimes more than 70%, by weight of the total surfactant.
  • the non-ionic surfactant constitutes less than 90%, more preferably less than 80%, most preferably less than 70% of the total weight of surfactant.
  • the amphoteric surfactant may comprise a betaine, e.g. a betaine of the general formula: Pv 1 2 N + CH 2 COO " , wherein R is an aliphatic hydrocarbyl, hydrocarbyl amido alkyl or hydrocarbyl ether group having an average of from 8 to 30, e.g. 10 to 25, especially 15 to 25 aliphatic carbon atoms and R 1 is an alkyl or hydroxy alkyl group having an average of from 1 to 4 carbon atoms. Particularly preferred are the alkylamido betaines, e.g.
  • R 2 CONH(CH 2 ) n .(R 1 ) 2 N + CH 2 COO " ;
  • R 2 is a C 8 -25 , preferably C 12-2 o, alkyl group, n is from 2 to 4, and R 1 has the same significance as before.
  • C 8 -25 alkyl amido propyl betaines such as coconut amido propyl betaine (CAPB) or any of the corresponding alkyl and alkenyl amido propyl betaines derived from natural palm or coconut fatty acids or from synthetic carboxylic acids having a similar alkyl chain distribution often loosely referred to as CAPB, including hardened and unhardened full or cut oils.
  • lauryl amido propyl betaine and other narrow cut alkyl amido propyl betaines such as stearyl.
  • R is an aliphatic group having from 8 to 25 carbon and R 1 is an alkyl or hydroxyalkyl group with from 1 to 4 carbon atoms.
  • Other amphoteric surfactants for use according to our invention include alkyl amino propionates, alkylamine polyalkoxy sulphates, sulphobetaines, amido sulphobetaines, phosphobetaines and other quaternary amine or quaternised imidazoline sulphonic acids and their salts, and zwitterionic surfactants, e.g.
  • N-alkyl taurines N-alkyl sarcosines, carboxylated amido amines such as RCONH(CH 2 ) n N + where n is 2 to 4, and amino acids having, in each case, at least one aliphatic group having from 8 to 25 carbon atoms.
  • the sodium chloride content of the solid amphoteric surfactant is preferably less than 12% by weight of said amphoteric surfactant, usually less than 10%, more preferably less than 8%, most preferably less than 5%, especially less than 3%, e.g. less than 1%.
  • the total inorganic salt content of the solid amphoteric surfactant is less than 15%, more preferably less than 10% most preferably less than 5%.
  • the solid amphoteric surfactant is preferably substantially anhydrous. By this is meant a moisture content less than 12% more preferably less than 10%, most preferably less than 8%, e.g. 1 to 6% by weight of said amphoteric surfactant.
  • the solid amphoteric surfactant preferably comprises and most preferably consists of a CAPB derivative and in particular of laurylamidopropyl betaine.
  • the solid amphoteric surfactant is based on a narrow cut alkyl feedstock, e.g. comprising more than 70% more preferably more than 80% most preferably more than 90% especially more than 95% of a single homologue.
  • Said single homologue is preferably a betaine of the aforesaid general formula, wherein R has at least 15 aliphatic carbon atoms.
  • the feedstock may be a narrow cut and/or hardened (i.e. hydrogenated) coconut or palm oil, or synthetic equivalent.
  • the solid amphoteric is preferably substantially non-hygroscopic i.e. it does not form a liquid or mesophase on standing in humid air. Preferably it has an equilibrium water content less than 10%, more preferably less than 8% at 40°C in an atmosphere having 65% humidity.
  • amphoteric sufactant constitute at least 0.25%, by weight of the composition, more preferably more than 0.5%, most preferably more than 1%, often more than 2%., but is usually less than 50%, desirably less than 40%, more desirably less than 30%, most desirably less than 20%, typically less than 10%, e.g. less than 5%.
  • the proportion of the total amphoteric surfactant in the laundry tablet which is added separately from the base powder is preferably at least 20% by weight, more preferably at least 30%, most preferably at least 40%, usually at least 50%, desirably at least 60% more desirably at least 70%, most desirably at least 80%, e.g. more than 90%.
  • the solid amphoteric surfactant is preferably added in particulate form, e.g. as powder, granules or needles.
  • amphoteric surfactant may be used in conjunction with anionic surfactants and in particular high foaming anionic surfactants such alkyl sulphates or alkyl ether sulphates.
  • the proportion of amphoteric surfactant may be from 20 to 100% preferably 30 to 70% by weight of the total surfactant.
  • the base powder preferably comprises a builder, which may for example comprise sodium tripolyphosphate, zeolite, sodium carbonate, sodium silicate, potassium pyrophosphate and/or sodium citrate. It preferably comprises conventional components of spray dried laundry detergent powders e.g. stain removers such as aminomethylene phosphonates, enzymes or oxidising bleaches, antiredeposition agents such as sodium carboxymethyl cellulose, optical brightening agents, perfume and colouring.
  • a builder which may for example comprise sodium tripolyphosphate, zeolite, sodium carbonate, sodium silicate, potassium pyrophosphate and/or sodium citrate.
  • spray dried laundry detergent powders e.g. stain removers such as aminomethylene phosphonates, enzymes or oxidising bleaches, antiredeposition agents such as sodium carboxymethyl cellulose, optical brightening agents, perfume and colouring.
  • the inorganic content of the base powder is preferably at least 30% based on the total weight thereof, more preferably at least 40% most preferably at least 50%, e.g. 60 to 90%.
  • the blended solids may comprise, in addition to the solid amphoteric surfactant, and any base powder, builders such as tetra potassium pyrophosphate, high phase 1 sodium tripolyphosphate, or zeolite, water-swellable polymers, such as water- swellable polyacrylates and any of the conventional wash adjuvants, all of which may be included in proportions conventional for laundry tablets.
  • builders such as tetra potassium pyrophosphate, high phase 1 sodium tripolyphosphate, or zeolite
  • water-swellable polymers such as water- swellable polyacrylates and any of the conventional wash adjuvants, all of which may be included in proportions conventional for laundry tablets.
  • the total proportion of builder in the powder, or in the laundry tablet, for example, may be greater than 10%, preferably greater than 15%, more preferably greater than 20%, most preferably greater than 30%, usually greater than 40%, sometimes greater than 45%, e.g. greater than 50%, by weight based on the weight of the powder or tablet.
  • the proportion of builder is less than 90%, preferably less than 80%, more preferably less than 70%, e.g. less than less than 60%, by weight based on the weight of the powder or tablet.
  • the tablet may comprise binders in addition to the solid amphoteric surfactant.
  • any surfactant in the base powder will contribute to the binding effect, as will any citric acid / bicarbonate mixtures.
  • the latter are conventionally compacted with a small amount of water, which gives a cementing effect.
  • Any liquid ingredients such as non-ionic surfactant may be sprayed on to the tablet or the mixture from which it is compacted, or onto porous particles added to the mixture
  • smectite clays such as bentonite or montmorillonite
  • the clay, and also, desirably the other components of the tablet should have a mean particle size, and preferably also at least the majority of particles, greater than 250 ⁇ , e.g. greater than 300 ⁇ , more preferably greater than 350 ⁇ , most preferably greater than 400 ⁇ , typically greater than 450 ⁇ , especially greater than 500 ⁇ .
  • the mean particle size of the clay and preferably also the size of at least the majority of the particles in the composition, be less than 2 mm, more preferably less than 1.5 mm, most preferably less than 1mm.
  • the clay, and preferably the powder composition as a whole should contain less than 10%, by weight, more preferably less than 5%, by weight, most preferably less than 3%, by weight, especially less than 2%, by weight, most desirably less than 1%, by weight, of particles smaller than 250 ⁇
  • the clay be used as the carrier for at least part of the non-ionic surfactant, and more preferably, at least the major part.
  • the non-ionic surfactant is preferably sprayed onto the clay to form a premix prior to blending with the other components.
  • the clay may be present in a proportion of greater than 2%, preferably greater than 5%, more preferably greater than 6%, most preferably greater than 7%, especially greater than 8%, e.g. greater than 9%, by weight based on the total weight of the powder.
  • the clay may typically constitute up to 25%, preferably less than 20%, more preferably less than 18%, most preferably less than 16%, e.g. less than 15%, by weight based on the total weight of the powder.
  • the proportion of non-ionic surfactant used to make the premix is preferably at least 30%, more preferably at least 40%, most preferably at least 50%, desirably at least 60%, more desirably at least 70%, most desirably over 75%, e.g. over 80%, of the total non-ionic surfactant in the powder. If all the non-ionic surfactant is added in the premix there is a tendency for the components of the powder to segregate, in the course of transport, handling or storage after the powder has been blended, and prior to compaction into a tablet. This can be reduced or avoided by adding a small amount of liquid non-ionic to the final formulation after mixing. The added surfactant may, for example, be sprayed onto the powder.
  • the proportion post-added in this way is chosen to give whatever balance between the physical stability of the powder and the compression strength of the compacted tablet, the user may require.
  • compositions of our invention preferably contain at least 5%, more preferably at least 10%, most preferably at least 15%, optionally more than 20%, sometimes more than 30%, occasionally more than 40% of amphoteric surfactant, based on the total weight of the surfactant.
  • the amphoteric surfactant usually constitutes less than 70%, preferably less than 60%, typically less than 50% of the total weight of the surfactant.
  • the compacted blend of solid amphoteric surfactant and solid particles may constitute the whole, or only a region or part of the total tablet.
  • the tablet may comprise two or more layers of which at least one may consist of ingredients other than the amphoteric surfactant.
  • the tablet may be any convenient shape such as cuboid, disc or spheroid. It may be designed for direct addition to the drum or, if sufficiently soluble, to the drawer of a washing machine.
  • the invention has been described primarily in relation to cleaning compositions, but is useful for a variety of applications, in which an active ingredient needs to be dissolved rapidly in water, in conjunction with a surfactant.
  • biocides including sterilants for clinics or hospitals, disinfectants for domestic, institutional, industrial or agricultural applications, or herbicides or pesticides for agricultural or horticultural use, may be formulated, together with wetting agents, as rapidly dissolving tablets in accordance with the teaching herein.
  • glyphosate An example of a herbicide that can, advantageously, be incorporated into a tablet according to the present invention is glyphosate.
  • mixtures of glyphosate with dry, desalted laurylamidopropyl betaine may be so formulated, optionally together with auxiliary wetting agents, such as ether carboxylates or amine oxides and/or binders, such as bentonite, and/or disintegrants, such as a mixture of citric acid and sodium carbonate, or a water swellable polymer.
  • auxiliary wetting agents such as ether carboxylates or amine oxides and/or binders, such as bentonite
  • disintegrants such as a mixture of citric acid and sodium carbonate, or a water swellable polymer.
  • the invention is especially useful for active ingredients that are too water sensitive to be stored for extended periods in aqueous solutions, suspensions or emulsions.
  • compositions described herein are envisaged primarily as being for use in the form of tablets.
  • powder compositions of the invention are capable of being used as such, and are not excluded from the scope of the invention when so used.
  • amphoteric surfactant had a mean particle size of 1.3 mm and the other solid components had a mean particle size between 600 and 700 ⁇ , and less than 1% by weight smaller than 250 ⁇ , unless the contrary is indicated.
  • a base powder was prepared by spray drying an aqueous slurry.
  • the base powder consisted of :- wt %
  • C12 alkyl amidopropyl betaine 2.5
  • the three amidopropyl betaines were all prepared from narrow cut (>80% C12), hardened, coconut feedstocks and had the following characteristics :
  • the samples were compacted into tablets each weighting 35g by applying a pressure of 15kN.
  • the tablets all had a compression strength of 41+4N.
  • a conventional (comparative) anionic tablet had the following composition: wt %
  • the surfactant comprised :- wt % Sodium Ci 0 .i 2 linear alkyl benzene sulphonate 9
  • a formulation according to the invention was prepared comprising the same ingredients in the same relative proportions, but replacing the 15% anionic/non-ionic surfactant with 10.15% of nonionic/amphoteric surfactant having the composition in % by weight based on the total composition of
  • Example 2 40g 56.3 55.0 73.5 58.8
  • the non-ionic / amphoteric tablet of the invention out-performed the conventional anionic/nonionic tablet at all doses.
  • the 30g tablet of the invention out-performed the 40g conventional tablet.
  • a bath bomb was prepared from a mixture of equal weights of citric acid and sodium bicarbonate. The mixture was added to the tableting press in three equal layers. The mixture used to make the middle layer contained 2%, by weight of the mixture, of the surfactant C from Example 1 and 2% of sodium lauryl sulphate.
  • the following powder formulation was prepared by mixing the solid components and spraying the non-ionic surfactant onto the mixed solids:
  • a 35 g tablet compressed under 30kN pressure had a compression-strength of 24N and a disintegration time of 30 seconds.
  • Example 6 The process of Example 4 was repeated substituting 9.4% of bentonite, based on the total weight of powder for an equal weight of the sodium sulphate, and premixing the non-ionic surfactant with the bentonite. The resulting tablet had a compression- strength of 107N and a disintegration time of 26 seconds.
  • Example 6
  • Example 5 The powder of Example 5 tended to segregate. Example 5 was repeated, premixing 4% of the non-ionic surfactant, based on the total weight of the powder, and post- adding the remaining 1.4%. No segregation was observed and the compacted tablet had a compression-strength of 40N and disintegration time of 25 seconds.
  • a herbicidal composition was prepared by blending 70%, by weight, of the isopropylamine salt of glyphosate, 10%, by weight, of a dried and desalted lauryl amidopropyl betaine, 10%, by weight, of sodium capryl (6 mole ethoxy) methyl carboxylate and 10%, by weight, of bentonite. The powder was compressed to form a strong, rapidly soluble tablet.
  • a laundry detergent tablet was prepared by compacting a powder consisting of:

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Abstract

La présente invention concerne des compositions pulvérulentes, qui peuvent être compactées en pastilles solides, hydrosolubles, telles que des pastilles de détergent de lavage ou des sels de bain, sont fabriquées par mélange de tensio-actif solide, particulaire, de préférence dessalé, amphotère, par exemple, de la bétaïne de laurylamidopropyle séchée, avec des particules hydrosolubles et/ou gonflables dans l'eau, inorganiques et/ou polymères, telles que de la bentonite. Une pastille de blanchisserie classique comprend une bétaïne amidopropyle solide, non hygroscopique, un tensio-actif non ionique, de la bentonite, des adjuvants et des adjuvants de lavage.
EP02735380A 2001-05-31 2002-05-24 Poudres compactables Withdrawn EP1397475A2 (fr)

Applications Claiming Priority (9)

Application Number Priority Date Filing Date Title
GB0113155 2001-05-31
GB0113155A GB0113155D0 (en) 2001-05-31 2001-05-31 Compacted cleaning compositions
GB0205718 2002-03-12
GB0205718A GB0205718D0 (en) 2002-03-12 2002-03-12 Compacted cleaning compositions
GB0208336A GB0208336D0 (en) 2002-04-11 2002-04-11 Compacted cleaning compositons
GB0208336 2002-04-11
GB0209445 2002-04-25
GB0209445A GB0209445D0 (en) 2002-04-25 2002-04-25 Compacted cleaning compositions
PCT/EP2002/005690 WO2002102948A2 (fr) 2001-05-31 2002-05-24 Poudres compactables

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EP1397475A2 true EP1397475A2 (fr) 2004-03-17

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EP02735380A Withdrawn EP1397475A2 (fr) 2001-05-31 2002-05-24 Poudres compactables

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EP (1) EP1397475A2 (fr)
AU (1) AU2002310836A1 (fr)
WO (1) WO2002102948A2 (fr)

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Publication number Priority date Publication date Assignee Title
ES2379917B1 (es) * 2010-10-06 2012-12-26 Jordi Caparros Casco Composiciones detergentes.
US8481474B1 (en) 2012-05-15 2013-07-09 Ecolab Usa Inc. Quaternized alkyl imidazoline ionic liquids used for enhanced food soil removal
US8716207B2 (en) 2012-06-05 2014-05-06 Ecolab Usa Inc. Solidification mechanism incorporating ionic liquids
DE202013001148U1 (de) * 2013-02-06 2014-05-07 Wetrok Ag Reinigungsmittel
CN105238604A (zh) * 2015-11-09 2016-01-13 云南健牛生物科技有限公司 一种高稳定的含盐洗衣泡腾片及其制备方法
EP4117792A4 (fr) 2020-03-10 2024-01-24 Soakness LLC Formulation de produit de bain à dissolution de percarbonate de sodium

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US4083813A (en) * 1976-10-01 1978-04-11 The Procter & Gamble Company Process for making granular detergent composition
DE2918363A1 (de) * 1979-05-07 1980-11-27 Henkel Kgaa Waschmittel fuer textilien
GB2207144B (en) * 1987-06-23 1991-07-31 Camille Simon Limited Detergent compositions
SE468013B (sv) * 1991-08-16 1992-10-19 Kommentus Ecogreen Ab Maskindiskmedel och dess framstaellning
DK173111B1 (da) * 1996-04-03 2000-01-31 Cleantabs As Tøjvasketabletter
US5885949A (en) * 1996-06-05 1999-03-23 Amway Corporation Tableted household cleaner comprising carboxylic acid, BI carbonate and polyvinyl alcohol
GB9723810D0 (en) * 1997-11-12 1998-01-07 Mcbride Robert Ltd Fabric softening co-granules
US6080714A (en) * 1997-11-20 2000-06-27 Akzo Nobel Nv Solid composition comprising an amphoteric surfactant, a process for its preparation, and the use thereof
DE19948668A1 (de) * 1999-10-08 2001-04-19 Cognis Deutschland Gmbh Waschmitteltabletten

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WO2002102948A2 (fr) 2002-12-27
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