Process for preparing particulate laundry detergent composition

Abstract

The present invention relates to a process for preparing a particulate laundry detergent composition comprising the steps of: (a) contacting water, starch, an acid and a perfume to form a concentrated aqueous acidic mixture wherein the concentrated acidic mixture comprises: (i) from 20% to 60% by weight of starch; (ii) from 10% to 50% by weight of an acid; (iii) from 2% to 20% by weight of a perfume; (iv) from 10% to less than 45% by weight of water; and the concentrated acidic mixture has a pH of less than 4.5; (b) subjecting the concentrated acidic mixture to a perfume emulsification step to emulsify the perfume to form an emulsified perfume mixture in fluid form; and (c) spraying the emulsified perfume mixture in fluid form onto the base detergent particles such that the emulsified perfume mixture at least partially coats the base detergent particles to form the particulate laundry detergent composition wherein the base detergent particles comprise from 4% to 60% by weight of a detersive surfactant.

Description

[0001] This application is a continuation of a PCT International Application having an international filing date of July 2, 2021, a PCT International Application Number of PCT / US2021 / 040221, a national application number of 202180044433.5, and an invention title of “Method for Preparing a Granular Laundry Detergent Composition.” TECHNICAL FIELD

[0002] The present invention provides a method for preparing a granular laundry detergent composition. The method enables the direct incorporation of a starch / fragrance mixture into a laundry powder, thereby providing a convenient and efficient method for producing a laundry detergent powder having good freshness characteristics and good color characteristics (no discoloration). BACKGROUND

[0003] Laundry detergent powders typically contain a fragrance to provide good freshness characteristics. Freshness characteristics need to provide good pure product odor (e.g., odor observed from the product before it is dosed into a wash bath (or an automatic washing machine)), good wet fabric odor (e.g., odor observed from wet fabrics / clothing washed using the product), and good dry fabric odor (e.g., odor observed from dry fabrics after they have been washed using the product).

[0004] Fragrance can be incorporated into laundry powder in a variety of ways: for example, by spraying onto the base particles (so as to at least partially coat the base particles). This spraying step can also be carried out in the presence of other particles (where the fragrance also typically at least partially coats the other particles as well as the base particles).

[0005] Fragrance can also be incorporated into laundry powder by forming fragrance particles and adding these fragrance particles to the detergent base particles (and other particles, if also present). One such fragrance particle is a starch-encapsulated fragrance accord (SEA). These SEAs are typically prepared by forming a mixture of starch and fragrance and spray-drying the mixture to form a spray-dried SEA. The spray-dried SEA is then mixed with the detergent base particles to form the laundry powder.

[0006] The present inventors have attempted to introduce the SEA chemistry (starch and fragrance) directly into a laundry powder (by a spray-on process), which avoids the complexity and energy requirements of having to form spray-dried SEA particles. However, attempts to simply spray a starch / fragrance mixture onto base detergent particles resulted in the laundry powder discoloring after one week (in a common storage stability test). The laundry powder formed yellowish spots throughout the laundry powder.

[0007] The present inventors have found that by adding acid to a starch / fragrance mixture (emulsion) and controlling the pH of the emulsion, starch / fragrance chemistry can be sprayed onto base detergent granules so as to at least partially coat the base detergent granules, and the resulting granular laundry detergent composition does not discolor upon storage. SUMMARY

[0008] The present invention provides a method for making a granular laundry detergent composition, wherein the method comprises the steps of: (a) contacting water, starch, acid, and fragrance to form a concentrated aqueous acidic mixture, wherein the concentrated acidic mixture comprises: (i) from 20 wt% to 60 wt% starch; (ii) from 10 wt% to 50 wt% acid; (ii) from 2 wt% to 20 wt% fragrance; (iv) from 10 wt% to less than 45 wt% water; and wherein the concentrated acidic mixture has a pH of less than 4.5; (b) subjecting the concentrated acidic mixture to a fragrance emulsification step to emulsify the fragrance to form an emulsified fragrance mixture in fluid form; and (c) spraying the emulsified fragrance mixture in fluid form onto base detergent granules, such that the emulsified fragrance mixture at least partially coats the base detergent granules to form the granular laundry detergent composition, wherein the base detergent granules comprise from 4 wt% to 60 wt% detersive surfactant. DETAILED DESCRIPTION

[0009] A process for making a granular laundry detergent composition. The method comprises the steps of: (a) contacting water, starch, acid, and fragrance to form a concentrated aqueous acidic mixture, wherein the concentrated acidic mixture comprises: (i) from 20 wt% to 60 wt% starch; (ii) from 10 wt% to 50 wt% acid; (ii) from 2 wt% to 20 wt% fragrance; (iv) from 10 wt% to less than 45 wt% water; and wherein the concentrated acidic mixture has a pH of less than 4.5; (b) subjecting the concentrated acidic mixture to a fragrance emulsification step to emulsify the fragrance to form an emulsified fragrance mixture in fluid form; and (c) spraying the emulsified fragrance mixture in fluid form onto base detergent granules, such that the emulsified fragrance mixture at least partially coats the base detergent granules to form the granular laundry detergent composition, wherein the base detergent granules comprise from 4 wt% to 60 wt% detersive surfactant.

[0010] Step (a): forming a concentrated aqueous acidic mixture. Step (a): contacting water, starch, acid, and fragrance to form a concentrated aqueous acidic mixture.

[0011] Typically, during step (a), the starch is in the form of a concentrated aqueous starch mixture, wherein the concentrated aqueous starch mixture comprises greater than 50 wt% starch, when the starch is contacted with the perfume.

[0012] Step (b): forming an emulsified perfume mixture. Step (b): subjecting the concentrated acid mixture to a perfume emulsification step to emulsify the perfume to form an emulsified perfume mixture in fluid form.

[0013] Typically, step (b) is carried out in a rotor-stator device which is operated such that the tip speed is greater than 5.0 ms -1 , or greater than 6.0 ms -1 , or even greater than 7.0 ms -1 .

[0014] Any suitable mixing device can be used in step (b). The preferred mixing device is a high shear mixer. Suitable high shear mixers can be dynamic or static mixers. Suitable dynamic mixers can be rotor-stator mixers. The most preferred mixer is a rotor-stator mixer, preferably a rotor-stator mixer operated at a tip speed of greater than 5.0 ms -1 , or greater than 6.0 ms -1 , or even greater than 7.0 ms -1 .

[0015] Suitable high shear mixers are silverstone type rapid mixers or IKA homogenizers. Step (b) can be a batch or continuous process step.

[0016] Preferably, step (b) is carried out at a temperature of from 20°C to 60°C. The emulsion can be at a temperature of from 20°C to 60°C. Preferably, the emulsified perfume mixture in fluid form formed during step (b) has a temperature of from 20°C to 60°C.

[0017] Step (c): spraying the emulsified perfume mixture. Step (c) is spraying the emulsified perfume mixture in fluid form onto the base detergent granules such that the emulsified perfume mixture at least partially coats the base detergent granules to form a granular laundry detergent composition.

[0018] Typically, step (c) is carried out in a mixer, wherein the weight ratio of the emulsified perfume mixture in fluid form dosed into the mixer to the base detergent granules is in the range of from 0.002:1 to 0.15:1.

[0019] Suitable mixers are rotating mixing drums.

[0020] A suitable way to spray the emulsified perfume mixture onto the base detergent granules is a spray nozzle. The spray nozzle typically atomizes the emulsified perfume mixture into droplets. A suitable spray nozzle can be a pressure nozzle or a multi-phase nozzle.

[0021] A powder mixer can be used to ensure that the emulsified perfume mixture is adequately dispersed onto the base detergent granules. A suitable powder mixer is a paddle mixer.

[0022] Other detergent granules can be present during step (c) and typically, the emulsified perfume mixture at least partially coats the other detergent granules as well as at least partially coating the detergent base granules.

[0023] Perfume: Any perfume raw material (PRM) is suitable. Suitable PRMs include those selected from the group consisting of 3-(4-tert-butylphenyl)-2-methylpropanal, 3-(4-tert- butylphenyl)-propanal, 3-(4-isopropylphenyl)-2-methylpropanal, 3-(3,4- methylenedioxyphenyl)-2-methylpropanal, 2,6-dimethyl-5-heptenal, damascone, 6,7- dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanone, methyl-7,3-dihydro-2H-1,5- benzodioxepin-3-one, 2-[2-(4-methyl-3-cyclohexenyl-1 -yl)propyl]cyclopentan-2-one, 2- sec-butylcyclohexanone, dihydroionone, linalool, ethyllinalool, tetrahydrolinalool, dihydromyrcenol, and any combination thereof.

[0024] Other examples of suitable perfume raw materials are described in WO 99 / 55819.

[0025] Especially preferred perfume raw materials include high impact accords (HIA) perfume raw materials, especially those PRMs having a boiling point of 275°C or less, an octanol / water partition coefficient P of about 2000 or greater, and an odor detection threshold of less than or equal to 50 parts per billion (ppb) as determined at about 760 mm Hg normal standard pressure.

[0026] Preferred perfume raw materials can have a log P of 2.0 or greater.

[0027] Acid: Preferably, the acid is an organic acid. Preferred acids are selected from carboxylic acids. Highly preferred acids are citric acid.

[0028] Preferred acids are C1-C 12 carboxylic acids. The term C1-C 12 carboxylic acids refers to carboxylic acids having from 1 to 12 carbon atoms, including the C atom of the carboxyl group. The carboxylic acid can be a saturated hydrocarbon. Alternatively, the carboxylic acid can be an unsaturated hydrocarbon.

[0029] The carboxylic acid can be a cyclic carboxylic acid. An example of a cyclic carboxylic acid is a lactone, for example ascorbic acid.

[0030] The carboxylic acid can be an aromatic carboxylic acid. An example of an aromatic carboxylic acid is salicylic acid.

[0031] Preferably, the carboxylic acid is at least a di-carboxylic acid. More preferably, it is at least a tri-carboxylic acid. By at least a tri-carboxylic acid is meant that it carries at least three carboxylic acid groups.

[0032] Preferably, the carboxylic acid is a C4-C8 carboxylic acid. In a preferred embodiment of the application, the carboxylic acid is selected from C2-C6 carboxylic acids.

[0033] Preferably, the carboxylic acid is selected from acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic acid, citric acid, succinic acid, hydroxysuccinic acid, maleic acid, fumaric acid, mesotartaric acid, glyoxylic acid, adipic acid, lactic acid, lactic acid, tartaric acid, salicylic acid, ascorbic acid, potassium, calcium and / or sodium salts of any of the foregoing acids, and mixtures of any of these.

[0034] The acid, especially the carboxylic acid such as citric acid, can be in the form of a salt. Preferably, the salt of the acid is a potassium salt and / or a sodium salt. More preferably, the acid is a tri-potassium salt and / or a tri-sodium salt of a tri-carboxylic acid. Most preferably, the acid is a tri-potassium salt and / or a tri-sodium salt of citric acid.

[0035] The above-mentioned acids and their salts are commercially available and their synthesis or isolation from raw materials is known to the person skilled in the art.

[0036] Starch: Typically, during step (a), when the starch is contacted with the flavour, the starch is in the form of a concentrated aqueous starch mixture, wherein the concentrated aqueous starch mixture comprises more than 50 wt.% of starch.

[0037] Preferably, the starch is selected from octenyl succinic anhydride starch.

[0038] Suitable starches can be made from raw starch, pregelatinized starch, modified starches derived from tubers, legumes, cereal plants and grains, for example corn starch, wheat starch, rice starch, waxy corn starch, oat starch, tapioca modified starch, waxy barley starch, waxy rice starch, waxy rice starch, waxy maize starch, amylopectin starch, potato starch, tapioca starch, oat starch, tapioca modified starch, and any combination thereof.

[0039] Suitable modified starches include hydrolyzed starch, acid-thinned starch, starch esters of short and long chain hydrocarbons, for example, acetic acid starch, octenyl succinic anhydride starch, dodecenyl succinic anhydride starch, and any combination thereof.

[0040] The term "hydrolyzed starch" refers to an oligosaccharide type material typically obtained by acid hydrolysis and / or enzymatic hydrolysis of starch, preferably corn starch. Suitable hydrolyzed starches include maltodextrin and corn syrup solids.

[0041] Suitable hydrolyzed starches typically have a dextrose equivalent (DE) value of 10 to 36 DE. The DE value is a measure of the reducing equivalents of hydrolyzed starch, expressed as a percentage (on a dry basis), based on dextrose. The higher the DE value, the more reducing sugars are present. The method for determining DE values can be found in Standard Analytical Methods of the Member Companies of Corn Industries Research Foundation, 6th Edition, Corn Refineries Association, Inc. Washington, DC 1980, D-52.

[0042] Suitable starch esters have a degree of substitution of 0.01% to 10.0%. The hydrocarbon portion of the modified ester is typically a C2to C 16 Suitable starches include various types of octenyl succinic anhydride (OSA) substituted waxy corn starches such as: (i) waxy starch: acid hydrolysis and OSA substitution; (ii) blend of corn syrup solids: waxy starch, OSA substitution and dextrinization; (iii) waxy starch: OSA substitution and dextrinization; (iv) blend of corn syrup solids or maltodextrin with waxy starch: acid hydrolysis, OSA substitution, then cooking and spray drying; (v) waxy starch: acid hydrolysis and OSA substitution, then cooking and spray drying; and (vi) above modifications of high and low viscosity (based on level of acid treatment).

[0043] Suitable modified starches typically have emulsification and emulsion stabilization capabilities, such as octenyl succinic acid starch, in order to have the ability to entrain perfume oil droplets in the emulsion due to the hydrophobic nature of the starch modifier. Typically, the perfume oil remains entrained in the modified starch until solubilized in the wash solution.

[0044] Concentrated aqueous acidic mixture: The concentrated acidic mixture comprises: (i) 20% to 60% by weight starch; (ii) 10% to 50% by weight perfume; (ii) 2% to 20% by weight acid; (iv) 10% to less than 45% by weight water; and wherein the concentrated acidic mixture has a pH of less than 4.5.

[0045] Preferably, the concentrated acidic mixture has a pH of less than 4.0.

[0046] Typically, when the concentrated acidic mixture is diluted in 10 seconds -1The concentrated aqueous acidic mixture has a viscosity in the range of 0.1 to 3.0 Pa.s when measured at a shear rate of 40 s"1and a temperature of 40°C. The method for measuring the viscosity of the concentrated aqueous acidic mixture is described in more detail below.

[0047] Emulsified perfume mixture: The emulsified perfume mixture is in the form of a fluid. Typically, the emulsified perfume mixture is in the form of a liquid suspension.

[0048] Preferably, the emulsified perfume mixture comprises perfume oil droplets having a size of less than 20 pm, preferably less than 15 pm, more preferably less than 5.0 pm, and most preferably less than 2.5 pm, preferably from 0.5 pm to 5.0 pm. The method for measuring the size of the perfume oil droplets within the emulsified perfume mixture is described in more detail below.

[0049] Preferably, the emulsified perfume mixture comprises greater than 10 wt%, preferably greater than 30 wt%, more preferably greater than 40 wt%, and most preferably greater than 50 wt% of perfume.

[0050] Typically, the emulsified perfume mixture is not subjected to a spray-drying step.

[0051] Base detergent granule: The base detergent particle comprises from 4 wt% to 60 wt% of detersive surfactant.

[0052] Typically, the base detergent particle comprises: (a) from 4 wt% to 35 wt% of detersive surfactant; and (b) from 5 wt% to 91 wt% of carrier material.

[0053] Typically, the base detergent particle is alkaline. Typically, the base detergent particle has a pH of greater than 7.5, or greater than 8.0, or greater than 9.0, or greater than 10.0 when dissolved in deionized water at a concentration of 1 g / L at 20°C.

[0054] The base detergent particle can be in the form of an agglomerate, an extrudate, a lens, a bead, or a spray-dried particle. The base detergent particle can be in the form of an agglomerate. The base detergent particle can be in the form of a spray-dried particle.

[0055] Preferably, the detersive surfactant is an anionic detersive surfactant. Suitable detersive surfactants and anionic detersive surfactants are described in more detail below.

[0056] Granular laundry detergent composition:Typically, the granular laundry detergent composition is a fully formulated laundry detergent composition, not just a part thereof (such as a spray-dried, extruded or agglomerated particle that forms only a part of the laundry detergent composition). Typically, the solid composition comprises a plurality of chemically distinct particles, such as spray-dried base detergent particles and / or agglomerated base detergent particles and / or extruded base detergent particles; combined with one or more, typically two or more, or five or more, or even ten or more particles selected from: surfactant particles, including surfactant agglomerates, surfactant extrudates, surfactant needles, surfactant sheets, surfactant tablets; phosphate particles; zeolite particles; silicate particles, especially sodium silicate particles; carbonate particles, especially sodium carbonate particles; polymer particles, such as carboxylate polymer particles, cellulose polymer particles, starch particles, polyester particles, polyamine particles, terephthalic acid polymer particles, polyethylene glycol particles; aesthetic particles, such as coloured noodles, needles, lamellae and ring particles; enzyme particles, such as protease particles, amylase particles, lipase particles, cellulase particles, mannanase particles, pectate lyase particles, xyloglucanase particles, bleach particles, such as percarbonate particles, especially coated percarbonate particles, such as percarbonate coated with carbonate, sulfate, silicate, borosilicate, or any combination thereof, perborate particles, bleach activator particles such as tetraacetyl ethylene diamine particles and / or alkyl oxybenzene sulfonate particles, bleach catalyst particles such as transition metal catalyst particles, and / or isoquinolinium bleach catalyst particles, pre-formed peracid particles, especially coated pre-formed peracid particles; filler particles, such as sulfate particles and chloride particles; clay particles, such as montmorillonite particles and clay and siloxane particles; flocculant particles, such as polyethylene oxide particles; wax particles, such as wax agglomerates; siloxane particles, brightener particles; dye transfer inhibitor particles; dye fixative particles; perfume particles, such as perfume microcapsules and starch encapsulated perfume accord particles, and pro-perfume particles, such as Schiff base reaction product particles; hueing dye particles; chelant particles, such as chelant agglomerates; and any combination thereof.

[0057] Suitable laundry detergent compositions comprise a detergent ingredient selected from the group consisting of detersive surfactants such as anionic detersive surfactants, nonionic detersive surfactants, cationic detersive surfactants, zwitterionic detersive surfactants, and amphoteric detersive surfactants; polymers such as carboxylate polymers, soil release polymers, anti-redeposition polymers, cellulosic polymers, and care polymers; bleaching agents such as sources of hydrogen peroxide, bleach activators, bleach catalysts, and preformed peracids; photobleaches such as sulfonated zinc phthalocyanines and / or sulfonated aluminum phthalocyanines; enzymes such as proteases, amylases, cellulases, lipases; zeolite builders; phosphate builders; auxiliary builders such as citric acid and citrate salts; carbonate salts such as sodium carbonate and sodium bicarbonate; sulfate salts such as sodium sulfate; silicate salts such as sodium silicate; chloride salts such as sodium chloride; brighteners; chelants; hueing agents; dye transfer inhibitors; dye fixatives; perfumes; silicones; fabric softeners such as clays; flocculants such as polyethylene oxide; suds suppressors; and any combination thereof.

[0058] Suitable laundry detergent compositions can have a low buffering capacity. Such laundry detergent compositions typically have a reserve alkalinity of less than 5.0 g NaOH / 100 g to pH 9.5. These low buffering laundry detergent compositions typically comprise a low level of carbonate salts.

[0059] Detersive surfactant: Suitable detersive surfactants include anionic detersive surfactants, nonionic detersive surfactants, cationic detersive surfactants, zwitterionic detersive surfactants, and amphoteric detersive surfactants. Suitable detersive surfactants can be linear or branched, substituted or unsubstituted, and can be derived from petrochemical or biological materials.

[0060] Anionic detersive surfactant: Suitable anionic detersive surfactants include sulfonate detersive surfactants and sulfate detersive surfactants.

[0061] Suitable sulfonate detersive surfactants include methyl sulfonate, alpha olefin sulfonate, alkyl benzene sulfonate, especially alkyl benzene sulfonate, preferably C 10-13 alkyl benzene sulfonate. Suitable alkyl benzene sulfonate (LAS) is available, preferably obtained by sulfonating commercially available linear alkyl benzene (LAB); suitable LAB includes lower 2-phenyl LAB, other suitable LAB includes higher 2-phenyl LAB such as those available under the tradename those supplied by Sasol.

[0062] Suitable sulfate detersive surfactants include alkyl sulfate, preferably C 8-18 alkyl sulfate, or predominantly C 12 alkyl sulfate.

[0063] Preferred sulphate detersive surfactants are alkyl alkoxylated sulphates, preferably alkyl ethoxylated sulphates, preferably C 8-18 alkyl alkoxylated sulphates, preferably C 8-18 alkyl ethoxylated sulphates, preferably alkyl alkoxylated sulphates have an average degree of alkoxylation of from 0.5 to 20, preferably from 0.5 to 10, preferably the alkyl alkoxylated sulphates are C 8-18 alkyl ethoxylated sulphates having an average degree of ethoxylation of from 0.5 to 10, preferably from 0.5 to 5, more preferably from 0.5 to 3, and most preferably from 0.5 to 1.5.

[0064] The alkyl sulphates, alkyl alkoxylated sulphates and alkyl benzene sulphonates can be linear or branched, substituted or unsubstituted, and can be derived from petrochemical or biological materials.

[0065] Other suitable anionic detersive surfactants include alkyl ether carboxylates.

[0066] Suitable anionic detersive surfactants can be in the form of a salt, suitable counterions include sodium, calcium, magnesium, amino alcohols, and any combination thereof. The preferred counterion is sodium.

[0067] Nonionic detersive surfactant: Suitable nonionic detersive surfactants are selected from: C8-C 18 alkyl ethoxylates, such as nonionic surfactants; C6-C 12 alkyl phenol alkoxylates, wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units, or mixtures thereof; C 12 -C 18 alcohols and C6-C 12 condensates of alkyl phenols with ethylene oxide / propylene oxide block polymers, such as alkyl polysaccharides, preferably alkyl polyglycosides; methyl ester ethoxylates; polyhydroxy fatty acid amides; ether capped poly(alkoxylated) alcohol surfactants; and mixtures thereof.

[0068] Suitable nonionic detersive surfactants are alkyl polyglucosides and / or alkyl alkoxylated alcohols.

[0069] Suitable nonionic detersive surfactants include alkyl alkoxylated alcohols, preferably C 8-18 alkyl alkoxylated alcohols, preferably C 8-18 alkyl ethoxylated alcohols, preferably the alkyl alkoxylated alcohols have an average degree of alkoxylation of from 1 to 50, preferably from 1 to 30, or from 1 to 20, or from 1 to 10, preferably the alkyl alkoxylated alcohols are C8-18 alkyl ethoxylated alcohols having an average degree of ethoxylation of 1 to 10, preferably 1 to 7, more preferably 1 to 5, and most preferably 3 to 7. The alkyl alkoxylated alcohols can be linear or branched, and substituted or unsubstituted.

[0070] Suitable nonionic detersive surfactants include secondary alcohol based detersive surfactants.

[0071] Cationic detersive surfactant: Suitable cationic detersive surfactants include alkyl pyridinium compounds, alkyl quaternary ammonium compounds, alkyl quaternary phosphonium compounds, alkyl ternary sulfonium compounds, and mixtures thereof.

[0072] A preferred cationic detersive surfactant is a quaternary ammonium compound having the general formula:

[0073] (R)(R1)(R2)(R3)N + X -

[0074] wherein R is a linear or branched, substituted or unsubstituted C 6-18 alkyl or alkenyl moiety, R1and R2are independently selected from a methyl or ethyl moiety, R3is a hydroxyl, hydroxymethyl, or hydroxyethyl moiety, and X is an anion that provides charge neutrality, preferred anions include: halide, preferably chloride; sulfate; and sulfonate.

[0075] Zwitterionic detersive surfactant: Suitable zwitterionic detersive surfactants include amine oxides and / or betaines.

[0076] Polymer: Suitable polymers include carboxylate polymers, soil release polymers, anti-redeposition polymers, cellulosic polymers, care polymers, and any combination thereof.

[0077] Carboxylate polymer: The composition can comprise a carboxylate polymer, such as a maleate / acrylate random copolymer or a polyacrylate homopolymer. Suitable carboxylate polymers include: a polyacrylate homopolymer having a molecular weight of 4,000 Da to 9,000 Da; a maleate / acrylate random copolymer having a molecular weight of 50,000 Da to 100,000 Da, or 60,000 Da to 80,000 Da.

[0078] Another suitable carboxylate polymer is a copolymer comprising: (i) from 50 wt% to less than 98 wt% of structural units derived from one or more monomers comprising carboxyl groups; (ii) from 1 wt% to less than 49 wt% of structural units derived from one or more monomers comprising sulfonate moieties; and (iii) from 1 wt% to 49 wt% of structural units derived from one or more monomers selected from ether bond-containing monomers represented by formulae (I) and (II):

[0079]

[0080] wherein in formula (I), R0represents a hydrogen atom or a CH3group, R represents a CH2group, a CH2CH2group or a single bond, X represents a number from 0 to 5, provided that when R is a single bond X represents a number from 1 to 5, and R1is a hydrogen atom or a C1to C4alkyl group; 20 an organic group;

[0081]

[0082] wherein in formula (II), R0represents a hydrogen atom or a CH3group, R represents a CH2group, a CH2CH2group or a single bond, X represents a number from 0 to 5, and R1is a hydrogen atom or a C1to C4alkyl group; 20 an organic group.

[0083] It can be preferred that the polymer has a weight average molecular weight of at least 50 kDa or even at least 70 kDa.

[0084] Soil release polymer: The composition can comprise a soil release polymer. Suitable soil release polymers have a structure as defined by one of the following structures (I), (II) or (III):

[0085] (I) - [(OCHR 1 - CHR 2 ) a - O-OC-Ar-CO- d

[0086] (II) - [(OCHR 3 - CHR 4 ) b - O-OC-sAr-CO- e

[0087] (III) - [(OCHR 5 - CHR 6 ) c - OR 7 ] f

[0088] wherein:

[0089] a, b and c are from 1 to 200;

[0090] d, e and f are from 1 to 50;

[0091] Ar is a 1,4-substituted phenylene;

[0092] sAr is a 1,3-substituted phenylene substituted at position 5 with SO3Me;

[0093] Me is Li, K, Mg / 2, Ca / 2, Al / 3, ammonium, mono-, di-, tri-, or tetra-alkylammonium, wherein alkyl is C1-C 18 alkyl or C2-C 10 hydroxyalkyl or mixtures thereof;

[0094] R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are independently selected from H or C1-C 18 n-alkyl or C1-C 18 iso-alkyl; and

[0095] R 7 is a linear or branched C1-C 18 alkyl, or a linear or branched C2-C 30 alkenyl, or a cycloalkyl group having from 5 to 9 carbon atoms, or a C8-C 30 aryl group, or a C6-C 30 aralkyl group.

[0096] Suitable soil release polymers are sold by Clariant under the series of polymers, for example SRN240 and SRA300. Other suitable soil release polymers are sold by Solvay under the series of polymers, for example SF2 and Crystal.

[0097] Anti-redeposition polymer: Suitable anti-redeposition polymers include polyethylene glycol polymers and / or polyethylene imine polymers.

[0098] Suitable polyethylene glycol polymers include random graft copolymers comprising: (i) a hydrophilic backbone comprising polyethylene glycol; and (ii) one or more hydrophobic side chains selected from: C4-C 25alkyl groups, polypropylene, polybutylene, vinyl esters of saturated C1-C6 monocarboxylic acids, C1-C6 alkyl esters of acrylic or methacrylic acid, and mixtures thereof. Suitable polyethylene glycol polymers have a polyethylene glycol backbone with polyvinyl acetate side chains grafted randomly. The average molecular weight of the polyethylene glycol backbone can range from 2,000 Da to 20,000 Da, or from 4,000 Da to 8,000 Da. The molecular weight ratio of the polyethylene glycol backbone to the polyvinyl acetate side chains can range from 1 : 1 to 1 :5, or from 1 : 1.2 to 1 :2. The average number of graft sites per ethylene oxide unit can be less than 0.02, or less than 0.016, the average number of graft sites per ethylene oxide unit can range from 0.010 to 0.018, or the average number of graft sites per ethylene oxide unit can be less than 0.010, or range from 0.004 to 0.008.

[0099] Suitable polyethylene glycol polymers are described in WO08 / 007320.

[0100] Suitable polyethylene glycol polymers are Sokalan HP22.

[0101] Cellulosic polymer: Suitable cellulose polymers are selected from alkyl celluloses, alkyl alkoxy alkyl celluloses, carboxy alkyl celluloses, alkyl carboxy alkyl celluloses, sulfonic acid alkyl celluloses, more preferably from carboxymethyl cellulose, methyl cellulose, methyl hydroxyethyl cellulose, methyl carboxymethyl cellulose, and mixtures thereof.

[0102] Suitable carboxymethyl cellulose has a degree of carboxymethyl substitution of from 0.5 to 0.9 and a molecular weight of from 100,000 Da to 300,000 Da.

[0103] Suitable carboxymethyl cellulose has a degree of substitution greater than 0.65 and a degree of blockiness greater than 0.45, for example as described in WO09 / 154933.

[0104] Care polymer: Suitable care polymers include cationically modified or hydrophobically modified cellulose polymers. Such modified cellulose polymers can provide an anti-abrasion benefit and a dye lock benefit to fabrics during a wash cycle. Suitable cellulose polymers include cationically modified hydroxyethyl cellulose.

[0105] Other suitable care polymers include dye lock polymers, for example condensation oligomers produced by condensation of imidazole and epichlorohydrin, preferably in a 1 :4: 1 ratio. A suitable commercially available dye lock polymer is FDI (Cognis).

[0106] Other suitable care polymers include amino-silicones, which can provide fabric feel benefits and fabric shape retention benefits.

[0107] Bleach: Suitable bleaching agents include sources of hydrogen peroxide, bleach activators, bleach catalysts, preformed peracids, and any combination thereof. Especially suitable bleaching agents include combinations of sources of hydrogen peroxide with bleach activators and / or bleach catalysts.

[0108] Hydrogen peroxide source: Suitable sources of hydrogen peroxide include sodium perborate and / or sodium percarbonate.

[0109] Bleach activator: Suitable bleach activators include tetraacetyl ethylene diamine and / or alkyl phenol sulfonate.

[0110] Bleach catalyst: The composition can comprise a bleach catalyst. Suitable bleach catalysts include bleach catalysts of the peroxyimidazolium cation, transition metal bleach catalysts, especially manganese and iron bleach catalysts. Suitable bleach catalysts have a structure according to the general formula:

[0111]

[0112] wherein R 13 is selected from the group consisting of 2-ethylhexyl, 2-propylheptyl, 2-butyloctyl, 2- amyl nonyl, 2-hexyldecyl, n-dodecyl, n-tetradecyl, n-hexadecyl, n-octadecyl, isononyl, isodecyl, isotridecyl, and isopentadecyl.

[0113] Preformed peracid: Suitable preformed peracids include phthalimido-peroxy hexanoic acid.

[0114] Enzyme: Suitable enzymes include lipases, proteases, cellulases, amylases, and any combination thereof.

[0115] Protease: Suitable proteases include metalloproteases and serine proteases. Examples of suitable neutral or alkaline proteases include: subtilisins (EC 3.4.21.62); trypsin-like or chymotrypsin-like proteases; and metalloproteases. Suitable proteases include chemically or genetically modified mutants of the foregoing suitable proteases.

[0116] Suitable commercially available proteases include those sold under the trade names Liquanase Savinase and those sold under the tradename Preferenz Protease series, including P280, P281, P2018-C, P2081-WE, P2082-EE and P2083-A / J, Purafect Purafect and Purafect those sold under the tradename and those sold under the tradename BLAP by Solvay Enzymes; those available from Henkel / Kemira, i.e. BLAP (sequence shown in Figure 29 of US 5,352,604 with the following mutations: S99D + S101 R + S103A + V104I + G159S, hereinafter referred to as BLAP); BLAP R (BLAP with S3T + V4I + V199M + V205I + L217D), BLAP X (BLAP with S3T + V4I + V205I) and BLAP F49 (BLAP with S3T + V4I + A194P + V199M + V205I + L217D), all from Henkel / Kemira; and KAP from Kao (Bacillus alkalophilus subtilisin with mutations A230V + S256G + S259N).

[0117] Suitable proteases are described in WO 11 / 140316 and WO 11 / 072117.

[0118] Amylase: Suitable amylases are derived from AA560 alpha amylase endogenous to Bacillus sp. DSM 12649, preferably having the following mutations: R118K, D183*, G184*, N195F, R320K and / or R458K. Suitable commercially available amylases include Natalase, Ultra, SZ, (both from Novozymes) and AA, Preferenz series amylases, and Ox Am、 HT Plus (both from DuPont).

[0119] The appropriate amylase is described in WO06 / 002643.

[0120] Cellulase: Suitable cellulases include those of bacterial or fungal origin. Chemically modified or protein-engineered mutants are also suitable. Suitable cellulases include those from the genera *Bacillus*, *Pseudomonas*, *Humicola*, *Fusarium*, *Thielavia*, and *Acremonium*, such as fungal cellulases produced by *Humicola insolens*, *Myceliophthora thermophila*, and *Fusarium oxysporum*.

[0121] Commercially available cellulases include and Premium Know (Novozymes A / S) Series of enzymes (DuPont), and AB enzyme series. Suitable commercially available cellulases include... Premium Classic. Suitable proteases are described in WO07 / 144857 and WO10 / 056652.

[0122] Lipase: Suitable lipases include those from bacteria, fungi, or synthetic sources, as well as their variants. Chemically modified or protein-engineered mutants are also suitable. Examples of suitable lipases include those from the genus *Thermomyces*, such as those from *H. lanuginosa* (*T. lanuginosus*).

[0123] The lipase may be a "first-cycle lipase," for example, such as those described in WO06 / 090335 and WO13 / 116261. In one aspect, the lipase is a first-wash lipase, preferably a variant of a wild-type lipase from *Thermophilus spp.* containing the T231R and / or N233R mutation. Preferred lipases include those marketed under trade names. and those sold by Novozymes (Bagsvaerd, Denmark).

[0124] Other suitable lipases include Liprl 139, e.g., as described in WO2013 / 171241; and TfuLip2, e.g., as described in WO2011 / 084412 and WO2013 / 033318.

[0125] Other enzyme: Other suitable enzymes are bleaching enzymes, such as peroxidases / oxidases, including those of plant, bacterial, or fungal origin, and variants thereof. Commercially available peroxidases include (Novozymes A / S). Other suitable enzymes include choline oxidase and perhydrolase, such as those used in Gentle Power Bleach TM .

[0126] Other suitable enzymes include pectate lyases sold under the tradename (From Novozymes A / S, Bagsvaerd, Denmark) and (DuPont). Mannanases sold under the tradename (Novozymes A / S, Bagsvaerd, Denmark) and (Du Pont).

[0127] Zeolite builder: The composition can comprise a zeolite builder. The composition can comprise from 0wt% to 5wt% of a zeolite builder, or 3wt% of a zeolite builder. The composition can even be essentially free of a zeolite builder; essentially free is meant "free of intentional addition". Typical zeolite builders include zeolite A, zeolite P, and zeolite MAP.

[0128] Phosphate builder: The composition can comprise a phosphate builder. The composition can comprise from 0wt% to 5wt% of a phosphate builder, or up to 3wt% of a phosphate builder. The composition can even be essentially free of a phosphate builder; essentially free is meant "free of intentional addition". A typical phosphate builder is sodium

[0129] Carbonate: The composition can comprise a carbonate. The composition can comprise from 0wt% to 10wt% of a carbonate, or from 0wt% to 5wt% of a carbonate. The composition can even be essentially free of a carbonate; essentially free is meant "free of intentional addition". Suitable carbonates include sodium carbonate and sodium bicarbonate.

[0130] Silicate:The composition can comprise silicate. The composition can comprise from 0wt% to 10wt% silicate, or from 0wt% to 5wt% silicate. A preferred silicate is sodium silicate, especially preferred is sodium silicate having a Na2O:SiO2 ratio of from 1.0 to 2.8, preferably from 1.6 to 2.0.

[0131] Sulphate: A suitable sulphate is sodium sulphate.

[0132] Brightener: Suitable optical brighteners include: diphenylstyryl biphenyl compounds such as CBS-X, a diaminostilbene disulfonic acid compound such as DMS pure Xtra and HRH, and pyrazoline compounds such as SN and coumarin compounds such as SWN.

[0133] A preferred brightener is: 2(4-styryl-3-sulfophenyl)-2H-napthol[1,2-d]triazole sodium, 4,4' bis{[(4-anilino-6-(N methyl-N-2 hydroxyethyl) amino 1,3,5-triazin-2-yl)] amino} stilbene-2-2' disulfonic acid disodium, 4,4'-bis{[(4-anilino-6-morpholino-1,3,5-triazin-2-yl)] amino} stilbene-2-2'-disulfonic acid disodium, and 4,4'-bis(2-sulfostyryl)biphenyl disodium. A suitable optical brightener is C.I. Fluorescent Brightener 260, which brightener can be used in its beta or alpha crystalline form or a mixture of these crystalline forms.

[0134] Chelant: The composition can also comprise a chelating agent selected from: diethylenetriaminepentaacetate, diethylenetriaminepenta(methyl phosphonic acid), ethylenediamine-N'N'-disuccinic acid, ethylenediaminetetraacetate, ethylenediamine tetra(methylene phosphonic acid), and hydroxyethanedichloromethylene phosphonic acid. A preferred chelating agent is ethylenediamine-N'N'-disuccinic acid (EDDS) and / or hydroxyethanediphosphonic acid (HEDP). The composition preferably comprises ethylenediamine-N'N'-disuccinic acid or a salt thereof. Preferably the ethylenediamine-N'N'-disuccinic acid is in the S,S enantiomeric form. Preferably the composition comprises 4,5-dihydroxy-isophthalic acid disodium salt. Preferred chelating agents can also act as calcium carbonate crystal growth inhibitors such as: 1 -hydroxyethanediphosphonic acid (HEDP) and salts thereof; N,N-dicarboxymethyl-2-aminopentane-1,5-dioic acid and salts thereof; 2-phosphonobutane-1,2,4-tricarboxylic acid and salts thereof; and combinations thereof.

[0135] Shading agent:Suitable shading agents include small molecule dyes, typically falling within the following Colour Index (C.I.) classifications: acid dyes, direct dyes, basic dyes, reactive dyes (including their hydrolysed forms) or solvent dyes or disperse dyes, for example dyes classified as blue, violet, red, green or black, and providing the desired shade, alone or in combination. Preferred such shading agents include acid violet 50, direct violet 9, 66 and 99, solvent violet 13, and any combination thereof.

[0136] Many shading agents suitable for use in the present application are known and described in the art, such as those described in WO2014 / 089386.

[0137] Suitable shading agents include phthalocyanine and azo dye conjugates, such as those described in WO2009 / 069077.

[0138] Suitable shading agents can be alkoxylated. Such alkoxylated compounds can be prepared by organic synthesis, which can result in a mixture of molecules with different degrees of alkoxylation. Such mixtures can be used directly to provide a shading agent, or can be subjected to a purification step to increase the proportion of the target molecule. Suitable shading agents include alkoxylated bis-azo dyes, such as those described in WO2012 / 054835, and / or alkoxylated thio-azo dyes, such as those described in WO2008 / 087497 and WO2012 / 166768.

[0139] Shading agents can be incorporated into the detergent composition as part of a reaction mixture which is the result of organic synthesis of dye molecules, by one or more optional purification steps. Such reaction mixtures generally comprise the dye molecules themselves, and in addition can comprise unreacted starting materials and / or by-products of the organic synthesis route. Suitable shading agents can be incorporated into shading dye particles, such as those described in WO 2009 / 069077.

[0140] Dye transfer inhibitor: Suitable dye transfer inhibitors include polyamine N-oxide polymers, copolymers of N-vinylpyrrolidone and N-vinylimidazole, polyvinylpyrrolidone, polyvinyl oxazolidone, polyvinyl imidazole, and mixtures thereof. Preferred are poly(vinylpyrrolidone), poly(vinylpyridine betaine), poly(vinylpyridine N-oxide), poly(vinylpyrrolidone-vinylimidazole), and mixtures thereof. Suitable commercially available dye transfer inhibitors include PVP-K15 and K30 (Ashland), HP165, HP50, HP53, HP59, HP56K, HP56, HP66 (BASF), S-400, S403E and S-100 (Ashland).

[0141] Perfume: Suitable perfume include perfume materials selected from the group of: (a) perfume materials having a ClogP of less than 3.0 and a boiling point of less than 250°C (1st quadrant perfume materials); (b) perfume materials having a ClogP of less than 3.0 and a boiling point of 250°C or greater (2nd quadrant perfume materials); (c) perfume materials having a ClogP of 3.0 or greater and a boiling point of less than 250°C (3rd quadrant perfume materials); (d) perfume materials having a ClogP of 3.0 or greater and a boiling point of 250°C or greater (4th quadrant perfume materials); and (e) mixtures thereof.

[0142] It can be preferred for the perfume to be in the form of a perfume delivery technology. Such delivery technologies also stabilize and enhance deposition and release of the perfume material from the laundered fabric. Such perfume delivery technologies can also be used to further increase the longevity of the release of the perfume from the laundered fabric. Suitable perfume delivery technologies include: perfume microcapsules, pro-perfumes, polymer assisted delivery, molecular assisted delivery, fiber assisted delivery, amine assisted delivery, cyclodextrins, starch encapsulated accords, zeolites and other inorganic carriers, and any mixture thereof. Suitable perfume microcapsules are described in WO2009 / 101593.

[0143] Silicone: Suitable silicones include polydimethylsiloxanes and amino-silicones. Suitable silicones are described in WO05075616.

[0144] Process for making detergent granules: Typically, the particles of the composition can be prepared by any suitable method. For example: spray drying, agglomeration, extrusion, and any combination thereof.

[0145] Typically, a suitable spray drying process includes the steps of forming an aqueous slurry mixture, transferring it through at least one pump, preferably two pumps, to a pressure nozzle. The aqueous slurry mixture is atomized into a spray drying tower and the aqueous slurry mixture is dried to form spray dried particles. Preferably, the spray drying tower is a counter-current spray drying tower, although a co-current spray drying tower can also be suitable.

[0146] Typically, the spray dried powder is subjected to cooling, for example air stripping. Typically, the spray dried powder is subjected to particle size classification, for example sieving, to obtain a desired particle size distribution. Preferably, the spray dried powder has a particle size distribution such that the weight average particle size is in the range of 300 microns to 500 microns and less than 10 wt% of the spray dried particles have a particle size greater than 2360 microns.

[0147] It can be preferred to heat the aqueous slurry mixture to raise the temperature prior to atomization into the spray drying tower, such as described in WO 2009 / 158162.

[0148] For anionic surfactants, such as linear alkyl benzene sulfonate, it can be preferred to introduce into the spray drying process after the step of forming the aqueous slurry mixture: for example, after pumping, introducing the acid precursor into the aqueous slurry mixture, such as described in WO 09 / 158449.

[0149] For a gas, such as air, it can be preferred to introduce into the spray drying process after the step of forming the aqueous slurry, such as described in WO 2013 / 181205.

[0150] For any inorganic ingredients, such as sodium sulfate and sodium carbonate, it can be preferred to micronize into small particle sizes if present in the aqueous slurry mixture, such as described in WO 2012 / 134969.

[0151] Generally, suitable agglomeration processes include the step of contacting in a mixer a detersive ingredient, such as a detersive surfactant, for example linear alkyl benzene sulfonate (LAS) and / or alkyl alkoxylated sulfate, with an inorganic material, such as sodium carbonate and / or silica. The agglomeration process can also be an in situ neutralization agglomeration process, wherein an acid precursor of a detersive surfactant, such as LAS, is contacted with a basic material, such as a carbonate and / or sodium hydroxide, in a mixer, and wherein the acid precursor of the detersive surfactant is neutralized by the basic material during the agglomeration process to form the detersive surfactant.

[0152] Other suitable detergent ingredients that can be agglomerated include polymers, chelants, bleach activators, silicones, and any combination thereof.

[0153] The agglomeration process can be a high, medium, or low shear agglomeration process, wherein a high shear, medium shear, or low shear mixer is used, respectively. The agglomeration process can be a multi-step agglomeration process, wherein two or more mixers are used, such as a high shear mixer in combination with a medium or low shear mixer. The agglomeration process can be a continuous process or a batch process.

[0154] It can be preferred for the agglomerates to be subjected to a drying step, for example, to a fluid bed drying step. It can also be preferred for the agglomerates to be subjected to a cooling step, for example, to a fluid bed cooling step.

[0155] Typically, the agglomerates are subjected to particle size fractionation, for example fluid bed elutriation and / or sieving, to obtain a desired particle size distribution. Preferably, the agglomerates have a particle size distribution such that the weight average particle size is in the range from 300 microns to 800 microns, and less than 10 wt% of the agglomerates have a particle size of less than 150 microns, and less than 10 wt% of the agglomerates have a particle size of greater than 1200 microns.

[0156] For fine and oversized agglomerates it can be preferred to recycle back into the agglomeration process. Typically, oversized particles are subjected to a comminution step, such as milling, and recycled back into the agglomeration process at an appropriate location, such as a mixer. Typically, fines are recycled back into the agglomeration process at an appropriate location, such as a mixer.

[0157] For ingredients, such as polymers and / or nonionic soil release surfactants and / or perfume, it can be preferred to spray onto the base detergent particles, such as spray dried base detergent particles and / or agglomerated base detergent particles. Typically, this spray step is carried out in a tumble drum mixer.

[0158] Method of laundering fabric: A method of laundering fabric comprises the steps of contacting the solid composition with water to form a wash liquor, and laundering fabric in said wash liquor. Typically, the wash liquor has a temperature of from above 0°C to 90°C, or to 60°C, or to 40°C, or to 30°C, or to 20°C. The fabric can be contacted with water before, after or simultaneously with contacting the solid composition with water. Typically, the wash liquor is formed by contacting the laundry detergent with water in such an amount that the concentration of the laundry detergent composition in the wash liquor is from 0.2 g / l to 20 g / l, or from 0.5 g / l to 10 g / l, or to 5.0 g / l. The method of laundering fabric can be carried out in a front-loading automatic washing machine, a top-loading automatic washing machine, including a high efficiency automatic washing machine, or a suitable hand-washing vessel. Typically, the wash liquor comprises 90 litres or less, or 60 litres or less, or 15 litres or less, or 10 litres or less of water. Typically, 200 g or less, or 150 g or less, or 100 g or less, or 50 g or less of the laundry detergent composition is contacted with water to form the wash liquor.

[0159] Method for measuring viscosity of concentrated aqueous acidic mixture: The shear viscosity of the concentrated aqueous mixture of the application is measured using a TA AR2000 rheometer using a cup and bob arrangement. The measurement is carried out using a continuous shear rate ramp from 2000 s -1 to 0.1 s -1 for 390 seconds. The rheometer cup is preheated to a temperature of 40°C for at least 30 minutes before starting the rheology test. The shear viscosity is recorded at a shear rate of 10 s -1 .

[0160] Method for measuring perfume oil droplet size in emulsified perfume mixture: The morphology and particle size distribution of the emulsions were examined using confocal laser scanning microscopy (CLSM) with a 60x oil immersion objective (Leica SP8, Leica, Germany). Two different fluorescent dyes were used to visualize the oil inside the capsules and the thickness of the capsule wall, respectively. The oil inside the capsules was visualized with Nile red, while the starch wall was visualized with Calcofluor White (CFW). (X. Jia et al., Food Hydrocolloids 43 (2015) 275-282; Wei Liu et al., J. Agricultural Food Chemistry 2018 66(35), 9301-9308; L. Bai et al., Biomacromolecules 2018, 19, 1674-1685).

[0161] To image the emulsions, 10 μΐ of a 0.1% w / v solution of Nile red in ethanol and 100 μΐ of a 1% w / v solution of Calcofluor White in water were added to 0.5 ml of the emulsion. After homogenization using a small spatula and equilibration at ambient temperature for at least 10 minutes, 6 μΐ^of the stained sample was placed on a microscope slide and covered with a coverslip. Images were taken confocally. The diameter (d32) of the emulsion was measured by taking the average of at least 100 droplets using Image J (FIJI) software.

[0162] Examples

[0163] A comparison was made between the granular laundry detergent composition prepared according to the process of the application and a comparative granular laundry detergent composition prepared according to a comparative process (without acid and at a higher pH).

[0164] Two fluids were prepared based on the different compositions given in Table 1 (parts by weight) below. All fluids were homogenized by a silverstone type rapid mixer. For fluid A, citric acid was added at 50 °C and dispersed into the aqueous starch before the addition of the perfume oil. Only fluid A had a pH of less than 4, as measured directly into the fluid.

[0165] Table 1

[0166]

[0167] 1 The starch was sourced from Ingredion UK Limited, Manchester M22 5LW, England

[0168] A spray-dried laundry detergent base powder was prepared using standard methods according to the compositions presented in Table 2 (parts by weight).

[0169] Table 2

[0170] LAS 19.6 wt% Polyacrylate polymer 3.5 wt% Sodium carbonate 17.3 wt% Sodium sulphate 44.4 wt% Sodium silicate 11.6 wt% Water 1.5 wt% Miscellaneous Balance to 100 wt%

[0171] The granular laundry detergent powder according to Table 3 (wt%) was prepared by dry mixing with a nonionic surfactant sprayed and dispersed onto the powder in a batch rotary mixer.

[0172] Table 3

[0173] ％ Spray dried base granule according to Table 2 49.4 Aluminosilicate 5.0 Citric acid 1.0 Brightener 0.2 Suds suppressor 0.4 LAS agglomerate 11.6 AES agglomerate 2.9 Carbonate 5.1 Percarbonate 14.5 Bleach activator 3.9 Nonionic surfactant 1.3 Miscellaneous Balance

[0174] Table 4 (wt) granular laundry detergent compositions containing several starch fluid compositions were completed. The starch fluid was sprayed onto the powder and evenly dispersed in the product so that the base granule was at least partially coated by the Kenwood food mixer.

[0175] Table 4

[0176] Powder A Powder B Fluid used according to Table 1 C D Final product according to Table 3 98 98 Fluid 2 2

[0177] Powder discoloured on storage .

[0178] The granular laundry detergent compositions according to Table 4 were sampled and placed on a petri dish. The petri dish samples were placed and stored at 40°C / 30% rH for 1 week. The results (discoloration evaluation) are shown in Table 5.

[0179] Table 5

[0180] Product A Product B 40°C, 1 week No significant discolouration Discoloured with yellow spots in the detergent product.

[0181] Powder A (invention) showed minimal no significant discoloration, while powder B (comparative) showed significant discoloration.

[0182] The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the exact value and a functional equivalent ranging approximately thereabout. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm."

Claims

1. A method for preparing a granular laundry detergent composition, wherein the method comprises the following steps: (a) Contacting water, starch, acid, and flavoring to form a concentrated aqueous acidic mixture, wherein the concentrated acidic mixture comprises: (i) 20% to 60% by weight of starch; (ii) 10% to 50% by weight of spices; (ii) 2% to 20% by weight of acid; (iv) 10% to less than 45% by weight of water; and The concentrated acidic mixture described herein has a pH value equal to or less than 3.4; (b) subjecting the concentrated acidic mixture to a fragrance emulsification step to emulsify the fragrance to form an emulsified fragrance mixture in fluid form; and (c) Spraying the emulsified fragrance mixture in fluid form onto base detergent particles such that the emulsified fragrance mixture at least partially coats the base detergent particles to form the granular laundry detergent composition, wherein the base detergent particles contain 4% to 60% by weight of a detergency surfactant. The emulsified flavoring mixture described herein has not undergone a spray drying step.

2. The method according to claim 1, wherein the emulsified fragrance mixture in fluid form is in the form of a liquid suspension.

3. The method according to any of the preceding claims, wherein during step (a), when the starch is in contact with the flavoring, the starch is in the form of a concentrated aqueous starch mixture, wherein the concentrated aqueous starch mixture contains more than 50% by weight of starch.

4. The method according to any of the preceding claims, wherein step (b) is performed in a rotor-stator assembly, said rotor-stator assembly being operated such that the tip speed is greater than 5 ms. -1 .

5. The method according to any of the preceding claims, wherein step (c) is carried out in a mixer, and wherein the weight ratio of the emulsified fragrance mixture in fluid form dispensed into the mixer to the base detergent particles is in the range of 0.002:1 to 0.15:

1.

6. The method according to any of the preceding claims, wherein the base detergent particles are in the form of an agglomerate.

7. The method according to any one of claims 1 to 5, wherein the base detergent particles are in the form of spray-dried particles.

8. The method according to any preceding claim, wherein the base detergent particles comprise: (a) 4% to 35% by weight of detergency surfactant; and (b) 5% to 91% by weight of carrier material.

9. The method according to any of the preceding claims, wherein when 10s -1 When measured at a shear rate and at a temperature of 40°C, the concentrated aqueous acidic mixture has a viscosity in the range of 0.1 to 3.0 Pa·s.

10. The method according to any of the preceding claims, wherein other detergent particles may be present during step (c), and the emulsified fragrance mixture at least partially coats the other detergent particles and at least partially coats the detergent base particles.

11. The method according to any of the preceding claims, wherein the acid is selected from carboxylic acids.

12. The method according to any of the preceding claims, wherein the detergency surfactant is an anionic detergency surfactant.

13. The method according to any of the preceding claims, wherein the starch is selected from octenyl succinic acid starch.

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