Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/22—Carbohydrates or derivatives thereof
  • C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
  • C11D3/225—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
• • 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

Definitions

• the present invention relates to detergent builder granules, more particularly zeolite builder granules.
• the invention also relates to detergent compositions including such granules.
• Zeolites of the molecular sieve type have commonly been employed in cleansers, particularly in laundry detergent compositions, as a builder to provide a water softening function, when the detergent or cleanser is placed in an aqueous solution. Zeolites have more recently been employed to replace phosphate builders.
• zeolites have been found to be relatively difficult to employ in dry-mixed detergent compositions, for a number of reasons. Difficulties arising during manufacture of detergent compositions with zeolite have often been related to the fine particle size of the crystalline zeolites. Typically, zeolites have a particle size of approximately 1-20 ⁇ m. Thus, if the zeolite is used in its normal state with such a particle size, it commonly presents problems with dusting and segregation in the detergent composition.
• EP-A-403,084 discloses a method of forming a zeolite agglomerate, including the steps of blending zeolite particles with a filler and a surfactant, and then agglomerating the thus formed blend in a rotary agglomerator with a zeolite binder.
• the zeolite agglomerate is subsequently combined with other detergent constituents in a second agglomeration step to form a granular detergent product with minimal segregation and dusting.
• Silicate and polyacrylate are mentioned as preferred binding agents.
• EP-A-368,364 and EP-A-279,038 disclose other types of zeolite granules comprising crystalline zeolite material and relatively small amounts of nonionic surfactant and carboxymethyl cellulose.
• zeolite granules of the prior art have generally favourable properties, we have found that their dispersability and dispensability in the wash liquor when applied in a detergent formulation, often leaves to be desired. Consequently, it is an object of the present invention to provide a type of zeolite granules having good dispensability and dispersability characteristics when used in a detergent formulation. It is another object to provide a type of zeolite granule which has a good influence on the dispensing behaviour of the particulate detergent composition in which it is present.
• the present invention provides a builder granule suitable for use in a particulate detergent composition, comprising: 50 - 90% by weight of zeolite material; 0 - 25% by weight of a nonionic surfactant; 1 - 10% by weight of alkalimetal carboxymethyl cellulose, having a purity of more than 80% by weight, up to 20% by weight, preferably 5-12% by weight, of water.
• the present invention provides a particulate detergent composition, comprising one or more nonionic and/or anionic surfactants and builder granules according to the present invention.
• the builder granule of the present invention has an average particle size which is generally in the range of 180-2000 ⁇ m, an average particle size of 200-800 ⁇ m being preferred.
• the binding agent is the binding agent
• Alkalimetal carboxymethyl cellulose preferably sodium carboxymethyl cellulose
• CMC Alkalimetal carboxymethyl cellulose
• the CMC in the builder granule should have a purity of at least 80% by weight, preferably at least 85% by weight. A purity of at least 90% by weight is more preferred, the remainder of the CMC being mainly salts and absorbed water.
• the level at which the CMC is present in the builder granule of the invention is generally 1-10% by weight, whereas a level of 3-5% by weight is preferred.
• the builder granule of the invention further contains a level of up to 25% by weight of a nonionic surfactant. If the builder granule is applied as such, for instance as water softener, then it preferably does not contain any nonionic surfactant. If the builder granule of the invention is applied as a constituent of a particulate detergent formulation, then it contains nonionic surfactant material at a level of preferably 5-25%, more preferably 10-20% by weight. It was found that not only the purity of the CMC but also the type of nonionic surfactant used in the granule according to the present invention affect the desired disintegration and dispersion properties of the granule significantly.
• a low meso-phase forming surfactant is defined as a type of surfactant which does not show substantial gel-formation when diluted with water, whereas a non meso-phase forming surfactant does not show substantial viscosity increase when diluted with water.
• Suitable types of nonionic surfactants for use in the builder granule of the invention are fatty alcohol ethoxylates having an average of 3 - 8 ethylene oxide groups per molecule. Preferred fatty alcohol ethoxylates are non or low meso-phase forming.
• the zeolite material which is present in the builder granule of the invention at a level of 50-90%, preferably 60-90%, more preferably 70-80% by weight, can be a crystalline sodium aluminosilicate detergency builder, as described, for example, in GB 1 429 143 (Procter & Gamble).
• Suitable sodium aluminosilicates of this type are the well-known commercially available zeolites A and X, and mixtures thereof.
• the zeolite may be the commercially available zeolite 4A now widely used in laundry detergent powders.
• the zeolite material incorporated in the builder granule of the invention is maximum aluminium zeolite P (zeolite MAP), as described and claimed in EP-A-384,070 (Unilever).
• Zeolite MAP is defined as an alkalimetal aluminosilicate of the zeolite P type having a silicon to aluminium ratio not exceeding 1.33, preferably within the range of from 0.90 to 1.33, and more preferably within the range of from 0.90 to 1.20.
• zeolite MAP having a silicon to aluminium ratio not exceeding 1.07, more preferably about 1.00.
• the calcium binding capacity of zeolite MAP is generally at least 150 mg CaO per gram of anhydrous material, as measured according to method 1 as disclosed in EP-A-384,070.
• zeolite MAP is most preferred for use in the builder granules of the present invention. Because of the superior dispersion properties of zeolite MAP, an even lower residue was observed to be obtainable with builder granules including zeolite MAP than with zeolite 4A granules. As a consequence, the risk that detergent residue remains on the fabric after the wash, is considerably reduced when applying builder granules of the invention including zeolite MAP as a constituent of a detergent formulation. Furthermore, zeolite MAP has a lower water content than commercially available zeolite 4A; zeolite MAP has a water level below 18%, whereas zeolite 4A has a water level above 18%.
• the water vapour pressure of zeolite MAP is clearly lower than of zeolite 4A. Because of this lower water content and lower water vapour pressure, the storage stability of bleaches, bleach precursors and enzymes present in detergent formulations also containing zeolite MAP granules of the invention, can be improved. Zeolite MAP granules have lower friability values than zeolite 4A granules, indicating that zeolite MAP is a stronger type of zeolite. Therefore, detergent formulations including builder granules of the invention containing zeolite MAP have improved properties such as dynamic flow rate and compressibility. Furthermore, the particle size distribution of said formulations may be more uniform and therefore less sensitive to powder segregation, than with builder granules containing zeolite 4A.
• the liquid carrying capacity of builder granules including zeolite MAP is relatively high, as compared to builder granules including zeolite 4A. Therefore, detergent formulations with high liquid surfactant percentages can be made via simple dry-mixing, when applying zeolite MAP in the builder granules of the invention.
• the builder granules of the invention are effectively produced by granulating zeolite material with the other constituents of the granules in a low speed mixer/granulator such as a V-blender, a PK Niro Zigzag(TM) granulator or a rotating drum.
• a low speed mixer/granulator such as a V-blender, a PK Niro Zigzag(TM) granulator or a rotating drum.
• this granulation process is carried out in a high speed mixer/granulator such as a FUKAE(TM) mixer, a VOMM turbo(TM) granulator, a Schugi Flexomix(TM) or a Lödige ploughshare mixer.
• the thus formed granules are dried in a fluid bed and sieved to obtain the required particle size distribution.
• the bulk density of the builder granules of the invention is typically in the range of 300-800 g/l, more preferably in the range of 400-700 g/l.
• the bulk density of the produced builder granules could be effectively controlled by incorporating therein a spray-dried amorphous alkalimetal silicate (desirably having a density of 50-600 g/l) at a level of 0.5-25%, more preferably 0,5-10% by weight.
• Preferred spraydried amorphous alkalimetal silicates are sodium silicates having a SiO 2 to Na 2 O mol ratio being in the range of 1.7 - 3.4, sodium silicates having a SiO 2 to Na 2 O mol ratio in the range of 1.7 to 2.4 being most preferred.
• the builder granules may be used for producing a wide range of particulate detergent formulations, via the dry-mixing route.
• the detergent formulation of the invention desirably comprises a peroxy bleach and one or more anionic and/or nonionic surfactants, in addition to the builder granules of the invention. These builder granules are preferably present in said formulation at a level of 20-80% by weight.
• the detergent composition of the invention preferably contains one or more nonionic surfactants.
• Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C 12 -C 15 primary and secondary alcohols ethoxylated with an average of from 3 to 20 moles of ethylene oxide per mole of alcohol.
• Primary and secondary alcohol alkoxylates also containing propylene oxide groups and/or butylene oxide groups as well as end-capped alkoxylates may also be used as a constituent of the detergent composition of the invention.
• anionic surfactants may be present at a level of up to 20% by weight, said level being desirably in the range of from 1 to 10% by weight, these figures being based on a fully formulated detergent composition.
• 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 C 8 -C 15 ; primary and secondary alkyl sulphates, particularly sodium C 12 -C 15 primary alcohol sulphates; olefin sulphonates; alkane sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates.
• the detergent composition of the invention may also comprise a bleach component, encapsulated or not, in an amount of up to 30% by weight.
• Said bleach component may be a hypohalite bleach such as NaDCCA, or a peroxygen compound, i.e. a compound capable of yielding hydrogen peroxide in aqueous solution.
• a peroxygen compound selected from alkali metal peroxides, organic peroxides, such as urea peroxide, and inorganic persalts such as the alkali metal perborates, percarbonates, perphosphates, persilicates and persulphates, is preferably used. Mixtures of two or more of such compounds may also be suitable.
• sodium perborate tetrahydrate and, especially, sodium perborate monohydrate are particularly preferred.
• Sodium perborate monohydrate is preferred because of its high active oxygen content.
• Sodium percarbonate may also be preferred for environmental reasons.
• the peroxygen bleach compound is suitably present in the detergent composition of the invention at a level of up to 25% by weight, preferably of from 5 to 20% by weight.
• the hypohalite bleach may be suitably used in an amount of up to 10%, preferably 1-5% by weight, as active chlorine.
• Organic peroxyacids may also be suitable as peroxygen bleaching agent.
• Such materials normally have the general formula: wherein R is an alkylene or substituted alkylene group containing from 1 to about 20 carbon atoms, optionally having an internal amide linkage; or a phenylene or substituted phenylene group; and Y is hydrogen, halogen, alkyl, aryl, an imido-aromatic or non-aromatic group, a C00H or group or a quaternary ammonium group.
• Typical monoperoxy acids useful herein include, for example:
• inorganic peroxyacid compounds are suitable, such as for example potassium monopersulphate (MPS). If organic or inorganic peroxyacids are used as the peroxygen compound, the amount thereof will normally be within the range of about 2-10 % by weight, preferably from 4-8 % by weight.
• MPS potassium monopersulphate
• All these peroxide compounds may be utilized alone or in conjunction with a peroxyacid bleach precursor.
• Peroxyacid bleach precursors are known and amply described in literature, such as in the British Patents 836988; 864,798; 907,356; 1,003,310 and 1,519,351; German Patent 3,337,921; EP-A-0185522; EP-A-0174132; EP-A-0120591; and US Patents 1,246,339; 3,332,882; 4,128,494; 4,412,934 and 4,675,393.
• peroxyacid bleach precursors are those of the cationic i.e. quaternary ammonium substituted peroxyacid precursors as disclosed in US Patent 4,751,015 and 4,397,757, in EP-A0284292 and EP-A-331,229.
• peroxyacid bleach precursors of this class are:
• a further special class of bleach precursors is formed by the cationic nitriles as disclosed in EP-A-303,520 and in European Patent Specification No.'s 458,396 and 464,880.
• any one of these peroxyacid bleach precursors can be used in the present invention, though some may be more preferred than others.
• the preferred classes are the esters, including acyl phenol sulphonates and acyl alkyl phenol sulphonates; the acyl-amides; and the quaternary ammonium substituted peroxyacid precursors including the cationic nitriles.
• Examples of said preferred peroxyacid bleach precursors or activators are sodium-4-benzoyloxy benzene sulphonate (SBOBS); N,N,N'N'-tetraacetyl ethylene diamine (TAED); sodium-1-methyl-2-benzoyloxy benzene-4-sulphonate; sodium-4-methyl-3-benzoloxy benzoate; SPCC; trimethyl ammonium toluyloxy-benzene sulphonate; sodium nonanoyloxybenzene sulphonate (SNOBS); sodium 3,5,5-trimethyl hexanoyloxybenzene sulphonate (STHOBS); and the substituted cationic nitriles.
• SBOBS sodium-4-benzoyloxy benzene sulphonate
• TAED N,N,N'N'-tetraacetyl ethylene diamine
• TAED sodium-1-methyl-2-benzoyloxy benzene-4-sulphon
• the precursors may be used in an amount of up to 12 %, preferably from 2-10 % by weight, of the composition.
• the detergent composition of the invention can contain any of the ingredients conventionally present in compositions intended for the washing of fabrics.
• examples of such components include inorganic and organic detergency builders, other inorganic salts such as sodium sulphate, fluorescers, polymers, lather control agents, enzymes and perfumes.
• anti-redeposition agents include anti-redeposition agents, bleach stabilisers, and photobleaches.
• zeolite MAP material as herein defined
• SCMC sodium carboxymethyl cellulose
• the composition of the thus-formed zeolite MAP granules is as follows: Example No. 1 A (%wt) (%wt) zeolite MAP 72.7 72.7 Blanose 7 M1 3.6 - Gabrosa DT 732 - 3.6 Dobanol 25-7 14.5 - Synperonic A7 - 14.5 Water 9.2 9.2 9.2
• the granules of Example 1 contain a CMC compound having a purity according to the present invention whereas the granules of Example A contain a different SCMC compound having a purity below the lower limit of 80% by weight, as specified in the present patent application.
• the zeolite MAP granules of Examples 1 and A were used to prepare particulate detergent formulations, by spraying a surfactant mixture onto said granules and postdosing the other constituents of the formulations.
• the thus-prepared formulations which only differ in respect of the composition of the zeolite MAP granules present therein, have the following composition: Example no.
• a dispensing test was carried out with these compositions, according to the following procedure.
• a Wascator(TM ) dispenser bank with automatic powder dosing was used.
• the water intake temperature was set at a constant temperature of 10°C.
• the water hardness was 6°GH, and the pressure was adjusted at 1.5 bar.
• the automatic feeding unit was adjusted such that it doses 100 gr of the particulate detergent composition in 8 seconds in a wet dispenser. A pre-wetting time of 1 minute was applied; subsequently, 8 litre water was dosed in 1 minute (at a pressure of 1.5 bar) to flush the detergent formulation out of the dispenser. After 7 minutes powder dosing was started again. This was repeated 10 times.
• Dispenser residues were assessed by weighing the detergent residues remaining in the dispenser after the test. These residues were collected in the wet state. The result of each dispensing test being the total amount of residue in the form of wet detergent product collected in the dispenser after the test, was expressed as a percentage of the total amount of dry detergent product dosed during the 10 cycles. Using this method, the following dispensing residue values were obtained.
• Example No 2 B For the composition including granules of Example 1 0.0
• composition of these zeolite granules is as follows: Example No. 3 C (%wt) (%wt) zeolite MAP 76.0 - zeolite 4A - 76.0 Blanose 7 M1 3.9 - Gabrosa DT 732 - 2.0 Marlipal O13/50 11.7 - Ethoxylate 6.5 EO - 2.6 Sodium sulphate - 2.9 NaOH - 0.5 Water 8.4 16.0
• Example no. 3 C Black spot” test result 0.46 2.13 "Insolubles” test result 5.0 50.5

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• 1996
  • 1996-11-07 EP EP96938147A patent/EP0863974B1/en not_active Expired - Lifetime
  • 1996-11-07 JP JP9520103A patent/JP2000500799A/ja active Pending
  • 1996-11-07 BR BR9611645A patent/BR9611645A/pt not_active IP Right Cessation
  • 1996-11-07 WO PCT/EP1996/004886 patent/WO1997020020A1/en active IP Right Grant
  • 1996-11-07 AU AU75679/96A patent/AU701161B2/en not_active Ceased
  • 1996-11-07 CA CA002237575A patent/CA2237575C/en not_active Expired - Fee Related
  • 1996-11-07 DE DE69626302T patent/DE69626302T2/de not_active Expired - Lifetime
  • 1996-11-07 TR TR1998/00973T patent/TR199800973T2/xx unknown
  • 1996-11-07 ES ES96938147T patent/ES2192233T3/es not_active Expired - Lifetime
  • 1996-11-18 ZA ZA9609640A patent/ZA969640B/xx unknown

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