Particulate laundry detergent composition containing pyridinedicarboxylic acid and process for its preparation

Abstract

The present invention relates to a granular laundry detergent composition comprising a surfactant and a pyridinedicarboxylic acid. The composition comprises a first granule characterized in that the first granule comprises the surfactant and the pyridinedicarboxylic acid. The present invention also relates to a consumer product comprising a package and the composition of the present invention. The composition is contained in a compartment of the package. The composition of the present invention can be used to wash fabrics in soft water and hard water. The composition of the present invention can be prepared by mixing a pyridinedicarboxylic acid, a surfactant, and water to produce a slurry; and drying the slurry to obtain the first granule.

Description

Technical Field

[0001] This invention relates to particulate laundry detergent compositions, consumer products, methods for washing fabrics, and methods for preparing them. Background Technology

[0002] It is well known that certain metallic compounds, such as calcium and magnesium, increase water hardness, which can affect negatively charged active detergent materials (such as anionic surfactants), leading to a loss of foaming. Foaming is important for evenly distributing active detergent substances on fabrics and thus improving cleaning performance. Consumers also often use the presence of foam as an indicator of cleaning ability. If foam is not prominent, consumers tend to change the wash water frequently and add more detergent, which is unnecessary and wasteful.

[0003] Furthermore, hard water can readily form scale crusts, for example, when heated, when the pH changes, or when it evaporates. Scale crusts can be seen on fabrics and can be perceived by the wearer as feeling rough to the touch.

[0004] Organic dicarboxylic acids, such as pyridine dicarboxylic acid or its salts, are known as biodegradable chelating agents that can prevent crusting on fabrics. It has also been observed that pyridine dicarboxylic acid coupled with surfactants and magnesium salts in hard surface cleaning detergents maintains foam stability in both soft and hard water.

[0005] While pyridine dicarboxylic acid is known to provide beneficial foaming effects under certain conditions, an object of the present invention is to provide a particulate laundry detergent composition containing pyridine dicarboxylic acid and exhibiting improved foaming compared to other particulate detergent compositions containing pyridine dicarboxylic acid.

[0006] Another object of the present invention is to provide a consumer product comprising the said particulate laundry detergent composition.

[0007] Another object of the present invention is to provide a method for washing fabrics using the granular laundry detergent composition.

[0008] Another object of the present invention is to provide a method for preparing the granular laundry detergent composition. Summary of the Invention

[0009] We were surprised to find that co-formulating a surfactant and pyridine dicarboxylic acid or its salt in a single particle provided enhanced foaming compared to compositions in which the same components were not formulated into the same particle.

[0010] The potential to produce pyridine dicarboxylic acid or its salts through fermentation, combined with its biodegradability, makes it a viable alternative to phosphonate-based chelating agents associated with significant environmental problems.

[0011] In a first aspect, the present invention relates to a particulate laundry detergent composition comprising a surfactant and pyridine dicarboxylic acid or a salt thereof, wherein the composition comprises a first particle, characterized in that the first particle comprises the surfactant and pyridine dicarboxylic acid or a salt thereof.

[0012] In another aspect, the present invention relates to a consumer product comprising packaging and a composition of the first aspect, wherein the packaging comprises at least one compartment in which the composition is contained.

[0013] In another aspect, the present invention relates to a method for washing a fabric, the method comprising the steps of: obtaining at least one fabric to be washed and a washing liquid; and bringing the at least one fabric and the washing liquid into contact with each other, wherein the washing liquid comprises the composition of the first aspect and water, wherein the water has a hardness between 0°D and 28.77°D, preferably between 4.80°D and 19.18°D, more preferably between 6.71°D and 14.39°D.

[0014] In another aspect, the present invention relates to a method for preparing the composition of the first aspect, the method comprising the steps of: mixing pyridine dicarboxylic acid, a surfactant and water to produce a slurry; and drying the slurry to obtain first particles. Detailed Implementation

[0015] The components, compositions, and methods disclosed herein will be described in more detail below.

[0016] As used herein, the articles “a” and “an” when used in a claim are understood to refer to one or more things protected or described in the claim. As used herein, the terms “comprising,” “including,” and “containing” are intended to be non-limiting.

[0017] The term "substantially free" may be used herein. This means that the referred material is present in very small amounts, not intentionally added to the composition to form a portion of the composition, or preferably not at analytically detectable levels. This means that the composition includes the referred material only as an impurity among other intentionally added materials. If present, the referred material may be present at levels of less than 1%, less than 0.1%, less than 0.01%, or even 0% by weight of the composition.

[0018] As used herein, the phrase "granular laundry detergent composition" includes compositions and formulations designed to treat fabrics. Such compositions include, but are not limited to, laundry cleaning compositions and detergents, fabric softening compositions, fabric strengthening compositions, fabric freshening compositions, laundry pre-wash agents, laundry pretreatment agents, laundry additives, spray products, dry cleaning agents or compositions, laundry rinsing additives, washing additives, post-rinse fabric treatment agents, ironing aids, unit-dosage formulations, delayed-delivery formulations, detergents on or incorporated into porous substrates or nonwoven sheets, and other suitable forms that are apparent to those skilled in the art from the teachings herein. Such compositions can be used as laundry pretreatment agents, laundry posttreatment agents, or can be added during rinsing or washing cycles in a laundry operation.

[0019] Unless otherwise specified, all component or composition levels refer to the active portion of the component or composition and do not include impurities, such as residual solvents or byproducts, that may be present in commercially available sources of such components or compositions.

[0020] Unless otherwise specified, all temperatures in this document are in degrees Celsius (°C). Unless otherwise specified, all measurements in this document were taken at 20°C and atmospheric pressure.

[0021] In all embodiments of this disclosure, unless otherwise specified, all percentages are by weight of the total composition. Unless otherwise specified, all ratios are by weight.

[0022] It should be understood that each maximum numerical limit given throughout this specification includes each lower numerical limit, as such lower numerical limits are explicitly stated herein. Each minimum numerical limit given throughout this specification will include each higher numerical limit, as such higher numerical limits are explicitly stated herein. Each numerical range given throughout this specification will include each narrower numerical range falling within such a wider numerical range, as all such narrower numerical ranges are explicitly stated herein.

[0023] Granular laundry detergent composition

[0024] This invention relates to a particulate laundry detergent composition. The particulate laundry detergent composition can be understood as a solid, free-flowing particulate laundry detergent composition, or a particulate laundry detergent composition that can be incorporated into a water-soluble unit dosage product. Those skilled in the art understand the characteristics of solid, free-flowing particulate laundry detergent compositions.

[0025] Typically, water-soluble unit-dosage articles comprise water-soluble nonwoven sheets, wherein: the nonwoven sheet is shaped to create internal compartments in which the particulate laundry detergent composition is contained; or the nonwoven sheet is oriented into layers stacked on top of each other, and the particulate laundry detergent composition is positioned between the layers.

[0026] The water-soluble fiber nonwoven sheet comprises multiple fibers. Preferably, the fibers are entangled fibers in a fibrous structure. The water-soluble fiber nonwoven sheet can be homogeneous or layered. If layered, the water-soluble fiber nonwoven sheet may comprise at least two and / or at least three and / or at least four and / or at least five layers.

[0027] Preferably, the water-soluble fiber nonwoven sheet has a basis weight between 20 gsm and 60 gsm, more preferably between 20 gsm and 55 gsm, more preferably between 25 gsm and 50 gsm, and most preferably between 25 gsm and 45 gsm. Those skilled in the art will know methods for measuring basis weight.

[0028] In this document, "fiber" refers to an elongated element whose length exceeds its average diameter, preferably with a length-to-average diameter ratio of at least about 10. Preferably, each fiber may have a length greater than or equal to 5.08 cm, greater than or equal to 7.62 cm, greater than or equal to 10.16 cm, greater than or equal to 15.24 cm, or a combination thereof. Alternatively, each fiber may have a length less than 5.08 cm, less than 3.81 cm, less than 2.54 cm, or a combination thereof. Each fiber may have a width less than 100 µm, less than 75 µm, less than 50 µm, less than 25 µm, less than 10 µm, less than 5 µm, less than 1 µm, or a combination thereof. Those skilled in the art will know standard methods and techniques for measuring width. Preferred methods include scanning electron microscopy (SEM) or optical microscopy and image analysis software.

[0029] The water-soluble fiber nonwoven sheet may comprise multiple fibers that are identical or substantially identical in composition. Alternatively, the water-soluble fiber nonwoven sheet may comprise two or more different fibers. Non-limiting examples of fiber differences may include physical differences, such as differences in diameter, length, texture, shape, hardness, elasticity, etc.; and chemical differences, such as crosslinking level, solubility, melting point, Tg, and surfactants. Preferably, the water-soluble fiber nonwoven sheet contains fibers comprising between 80% and 95% by weight, more preferably between 85% and 93%, and more preferably between 87% and 90%.

[0030] Water-soluble fiber nonwoven sheets can exhibit different regions, such as regions with different basis weights, densities, and / or thicknesses. Water-soluble fiber nonwoven sheets may contain textures on one or more of their surfaces. The surfaces of water-soluble fiber nonwoven sheets may contain patterns, such as non-random repeating patterns. Water-soluble fiber nonwoven sheets may have a thickness between 0.01 mm and 100 mm, preferably between 0.05 mm and 50 mm, more preferably between 0.1 mm and 20 mm, even more preferably between 0.1 mm and 10 mm, even more preferably between 0.1 mm and 5 mm, even more preferably between 0.1 mm and 2 mm, even more preferably between 0.1 mm and 0.5 mm, and most preferably between 0.1 mm and 0.3 mm. Those skilled in the art will know standard methods for measuring thickness.

[0031] The fiber may contain a polyvinyl alcohol polymer. Preferably, the fiber contains between 50% and 98% polyvinyl alcohol by weight of the fiber, more preferably between 65% and 97%, more preferably between 80% and 96%, and even more preferably between 88% and 96%.

[0032] Polyvinyl alcohol polymers may have a weight-average molecular weight between 50 kDa and 150 kDa, preferably between 75 kDa and 140 kDa, and more preferably between 100 kDa and 130 kDa. As used herein, “weight-average molecular weight” refers to the weight-average molecular weight as determined using gel permeation chromatography. Other known techniques for determining weight-average molecular weight (MW) will be known to those skilled in the art.

[0033] Preferably, the polyvinyl alcohol polymer is a polyvinyl alcohol homopolymer. Preferably, the polyvinyl alcohol homopolymer has an average degree of hydrolysis percentage of 75% to 100%, more preferably 80% to 95%, and most preferably 85% to 90%. Preferably, the polyvinyl alcohol homopolymer has an average viscosity of 1 mPas to 30 mPas, more preferably 5 mPas to 25 mPas, and most preferably 10 mPas to 20 mPas, wherein this viscosity is measured at 20°C with a 4% aqueous solution in demineralized water.

[0034] The fiber preferably contains between 0.1% and 15% by weight of the fiber of a breaker, wherein the breaker is selected from polyols, sugar alcohols, amines, amides, carbohydrates, polyvalent cations, or mixtures thereof, preferably from polyols, sugar alcohols, or mixtures thereof. Preferably, the fiber contains between 1% and 12% by weight of the fiber, more preferably between 2% and 10%.

[0035] Typically, granular laundry detergent compositions are the full formulation of a laundry detergent composition, rather than a part of it (such as spray-dried, extruded, or agglomerated granules that form only a part of the laundry detergent composition). Typically, granular laundry detergent compositions contain a variety of chemically distinct particles, such as spray-dried base detergent particles and / or agglomerated base detergent particles and / or extruded base detergent particles; combinations of one or more, usually two or more, or five or more, or even ten or more types of particles, selected from: surfactant particles, including surfactant agglomerates, surfactant extruders, surfactant needles, surfactant flakes; 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 colored stripes, needles, layered particles, and ring particles; enzyme particles, such as protease particles, amylase particles, lipase particles, cellulase particles, mannanase particles, pectinase lyase particles, xyloglucanase particles, bleaching enzyme particles, and other enzymes. Any of the following co-particles, preferably these enzyme particles contain sodium sulfate; bleaching agent particles, such as percarbonate particles, especially coated percarbonate particles, such as percarbonate coated with carbonate, sulfate, silicate, borosilicate, or any combination thereof, perborate particles, bleaching activator particles such as tetraacetylethylenediamine particles and / or alkyloxybenzene sulfonate particles, bleaching catalyst particles such as transition metal catalyst particles, and / or isoquinoline onion bleaching catalyst particles, pre-formed peracid particles, especially coated pre-formed Overacid particles; filler particles, such as sulfate particles and chloride particles; clay particles, such as montmorillonite particles and clay with siloxane particles; flocculant particles, such as polyethylene oxide particles; wax particles, such as wax agglomerates; siloxane particles, whitening agent particles; dye transfer inhibitor particles; dye fixative particles; fragrance particles, such as fragrance microcapsules and starch-encapsulated fragrance blends, and pre-fragrance particles, such as Schiff base reaction product particles; tinting dye particles; chelating agent particles, such as chelating agent agglomerates; and any combination thereof.

[0036] Suitable laundry detergent compositions contain detergent ingredients selected from the following: detergency surfactants, such as anionic, nonionic, cationic, amphoteric, and ampholytic surfactants; polymers, such as carboxylate polymers, detergency polymers, anti-redeposition polymers, cellulose polymers, and conditioning polymers; bleaches, such as hydrogen peroxide sources, bleaching activators, bleaching catalysts, and pre-formed peracids; photobleaching agents, such as zinc phthalocyanine sulfonate and / or aluminum phthalocyanine sulfonate; enzymes, such as proteases, amylases, cellulases, and lipases; zeolite builders; phosphate builders; auxiliary builders, such as citric acid and citrate; carbonates, such as sodium carbonate and sodium bicarbonate; sulfates, such as sodium sulfate; silicates, such as sodium silicate; chloride salts, such as sodium chloride; brighteners; chelating agents; toning agents; dye transfer inhibitors; dye fixatives; fragrances; siloxanes; fabric softeners, such as clay; flocculants, such as polyethylene oxide; defoamers; and any combination thereof.

[0037] In a first aspect of the invention, the particulate laundry detergent composition comprises a surfactant and pyridine dicarboxylic acid or a salt thereof, wherein the composition comprises a first particle, characterized in that the first particle comprises the surfactant and the pyridine dicarboxylic acid or a salt thereof.

[0038] Laundry detergent compositions produce a certain amount of foam, which can be used to evenly distribute the product onto the fabric to be washed. The amount of foam is generally limited by the amount of anionic surfactant that can be safely and practically added to the composition.

[0039] Surprisingly, it was found that co-formulating pyridine dicarboxylic acid with surfactants into individual particles provided enhanced foaming effects compared to dry-mixing pyridine dicarboxylic acid powder into surfactant particles.

[0040] Unbound by theory, the beneficial foaming effect provided by the co-formulation of surfactant and pyridine dicarboxylic acid is due to the maximized surface contact and excellent mixing and dissolution of the two components before co-granulation. Another important factor may be the optimized rate of release of pyridine dicarboxylic acid from the aforementioned particles compared to the rate of release from the pyridine dicarboxylic acid powder.

[0041] In a preferred aspect of the invention, the particulate laundry detergent composition may have a pH of at least 9, preferably between 10 and 10.5, in use, wherein the pH of the composition in use is measured at a temperature of 20°C and a concentration of 1 g / L in deionized water. Those skilled in the art will know how to use a pH meter to measure the pH of a solution. Without being bound by theory, a pH of at least 9 will allow for effective activity of the bleach (a common component of particulate laundry detergent compositions), thereby enhancing the whitening and detergency of the composition.

[0042] It is known that in hard surface cleaning detergents, pyridine dicarboxylic acid maintains foam stability in both soft and hard water when combined with surfactants and 0.5% to 30% magnesium salts. Surprisingly, it has been found that with less than 0.5% magnesium salt, the present invention provides beneficial foaming effects.

[0043] In one aspect of the invention, the particulate laundry detergent composition may contain between 0% and 20% by weight of the composition, or even between 0% and 2%, or even between 0% and 0.5%. The composition may even be substantially free of magnesium salts.

[0044] Suitable magnesium salts can have a content of at least 5 × 10⁻⁶. -5 The solubility product of inorganic and / or organic magnesium salts. Suitable examples of inorganic magnesium salts are magnesium sulfate, magnesium chloride, magnesium bromide, magnesium iodide and magnesium nitrate, and suitable examples of organic magnesium salts are magnesium citrate and magnesium tartrate and magnesium salts of EDTA.

[0045] In a preferred aspect of the invention, the particulate laundry detergent composition may contain between 0.01% and 4% water by weight of the composition. Without being bound by theory, a higher weight percentage of water will increase the viscosity of the particulate laundry detergent composition, leading to clumping and agglomeration in the manufacturing machine piping. This phenomenon will affect the handling and processability of the particulate laundry detergent composition during manufacturing. Furthermore, the presence of excessive water may promote the growth of microorganisms within the composition, thereby affecting shelf life and long-term stability.

[0046] In a preferred aspect of the invention, the particulate laundry detergent composition further comprises an auxiliary ingredient selected from the group consisting of amines, surfactant systems, water-binding agents, sulfites, fatty acids and / or their salts, enzymes, encapsulated beneficial agents, detergent polymers, toning agents, washing aids, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalysts, bleaching agents, bleaching catalysts, bleaching activators, dirt removers / anti-redeposition agents, polymer dispersants, polymer grease cleaners, brighteners, defoamers, dyes, fragrances, encapsulated fragrances, fragrance delivery systems, structural elasticizers, fabric softeners, carriers, fillers, water-soluble additives, organic solvents, antimicrobial agents and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, rheology modifiers or structural agents, opacifiers, pearlescent agents, pigments, corrosion inhibitors and / or rust inhibitors, and mixtures thereof.

[0047] Suitable enzymes include lipases, proteases, cellulases, amylases, and any combination thereof.

[0048] Suitable proteases include metalloproteinases and / or serine proteases. Examples of suitable neutral or basic proteases include: subtilisin (EC 3.4.21.62); trypsin-type or chymotrypsin-type proteases; and metalloproteinases. Suitable proteases include chemically modified or genetically modified mutants of the aforementioned suitable proteases.

[0049] Suitable amylases are derived from AA560α amylase, which is endogenous to Bacillus spp. DSM 12649, and preferably have the following mutations: R118K, D183*, G184*, N195F, R320K and / or R458K.

[0050] Suitable cellulases include those derived from bacteria or fungi. 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*, *Myceliophthorathermophila*, and *Fusarium oxysporum*.

[0051] 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*).

[0052] In one aspect, the lipase is a first washing lipase, preferably a variant of the wild-type lipase from *Thermophilus spp.* containing the T231R and / or N233R mutations.

[0053] Other suitable enzymes are bleaching enzymes, such as peroxidases / oxidases, including those of plant, bacterial, or fungal origin and their variants. Other suitable enzymes include pectic acid lyases.

[0054] Suitable detergency polymers have structures as defined by one of the following structures (I), (II), or (III):

[0055] (I)-[(OCHR 1 -CHR 2 ) a-O-OC-Ar-CO-] d

[0056] (II)-[(OCHR 3 -CHR 4 ) b -O-OC-sAr-CO-] e

[0057] (III)-[(OCHR 5 -CHR 6 ) c -OR 7 ] f

[0058] in:

[0059] a, b, and c are 1 to 200; d, e, and f are 1 to 50; Ar is a 1,4-substituted phenylene;

[0060] sAr is a 1,3-substituted phenylene group substituted at position 5 by SO3Me; Me is Li, K, Mg / 2, Ca / 2, Al / 3, ammonium, monoalkylammonium, dialkylammonium, trialkylammonium, or tetraalkylammonium, wherein the alkyl group is C1-C. 18 Alkyl or C2-C 10 hydroxyalkyl groups or mixtures thereof; R 1 R 2 R 3 R 4 R 5 and R 6 Independently selected from H or C1-C 18 n-alkyl or C1-C 18 isoalkyl; and R 7 C1-C, whether straight or branched 18 Alkyl groups, or straight-chain or branched C2-C 30 Alkenyl, or a cycloalkyl group having 5 to 9 carbon atoms, or C8-C 30 aryl group, or C6-C 30 Arylalkyl group. Suitable detergency polymers are produced by Clariant with TexCare. ® A range of polymers are available for sale, such as TexCare. ® SRN240 and TexCare ® SRA300. Other suitable detergency polymers are available from Solvay with Repel-o-Tex. ® A range of polymers are available, such as Repel-o-Tex. ® SF2 and Repel-o-Tex ® Crystal.

[0061] Suitable toners include small molecule dyes, typically belonging to the color index (CI) classifications of acidic, direct, basic, reactive (including their hydrolyzed forms), or solvent or disperse dyes, such as dyes classified as blue, violet, red, green, or black, and providing the desired hue alone or in combination. Preferred toners of this type include Acid Violet 50, Direct Violet 9, 66, and 99, Solvent Violet 13, and any combinations thereof.

[0062] Many toners applicable to this invention are known and described in the art, such as toners.

[0063] Suitable toners include phthalocyanine and azo dye conjugates.

[0064] Suitable toners can be alkoxylated. Such alkoxylated compounds can be produced through organic synthesis, which yields mixtures of molecules with different degrees of alkoxylation. These mixtures can be used directly as toners or undergo purification steps to increase the proportion of the target molecule. Suitable toners include alkoxylated diazo dyes and / or alkoxylated thiophene azo dyes.

[0065] Toners can be incorporated as part of a reaction mixture resulting from the organic synthesis of dye molecules via one or more optional purification steps. Such reaction mixtures generally contain the dye molecules themselves and may also contain unreacted starting materials and / or byproducts of the organic synthesis pathway. Suitable toners can be incorporated into the toner particles.

[0066] Suitable bleaching agents include hydrogen peroxide sources, bleaching activators, bleaching catalysts, pre-formed peracids, and any combination thereof. Particularly suitable bleaching agents include combinations of hydrogen peroxide sources with bleaching activators and / or bleaching catalysts.

[0067] Suitable sources of hydrogen peroxide include sodium perborate and / or sodium percarbonate.

[0068] Suitable bleaching activators include tetraacetylethylenediamine and / or alkylphenol sulfonates.

[0069] The composition may contain a bleaching catalyst. Suitable bleaching catalysts include peroxyimine cation bleaching catalysts, transition metal bleaching catalysts, and especially manganese and iron bleaching catalysts. Suitable bleaching catalysts have a structure conforming to the following general formula:

[0070]

[0071] Where R 13Choose from the group consisting of: 2-ethylhexyl, 2-propylheptyl, 2-butyloctyl, 2-pentylnonyl, 2-hexyldecyl, n-dodecyl, n-tetradecyl, n-hexadecyl, n-octadecyl, isononyl, isodecyl, isothidecyl, isotriadecyl and isopentadecyl.

[0072] Suitable anti-redeposition polymers include polyethylene glycol polymers and / or polyethyleneimine polymers.

[0073] 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 the group consisting of: C4-C 25 Alkyl groups, polypropylene, polybutylene, vinyl esters of saturated C1-C6 monocarboxylic acids, C1-C6 alkyl esters of acrylic acid or methacrylic acid, and mixtures thereof. Suitable polyethylene glycol polymers have a polyethylene glycol backbone with randomly grafted polyvinyl acetate side chains. 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 grafting sites per ethylene oxide unit can be less than 0.02, or less than 0.016, and the average number of grafting sites per ethylene oxide unit can range from 0.010 to 0.018, or the average number of grafting sites per ethylene oxide unit can be less than 0.010, or in the range of 0.004 to 0.008. A suitable polyethylene glycol polymer is Sokalan HP22.

[0074] Suitable flavorings include flavoring materials selected from the group consisting of: (a) flavoring materials having a ClogP of less than 3.0 and a boiling point of less than 250°C (Quadrant 1 flavoring materials); (b) flavoring materials having a ClogP of less than 3.0 and a boiling point of 250°C or greater (Quadrant 2 flavoring materials); (c) flavoring materials having a ClogP of 3.0 or greater and a boiling point of less than 250°C (Quadrant 3 flavoring materials); (d) flavoring materials having a ClogP of 3.0 or greater and a boiling point of 250°C or greater (Quadrant 4 flavoring materials); and (e) mixtures thereof.

[0075] For fragrances, a preferred form is fragrance delivery technology. Such delivery technologies also stabilize and enhance the release of deposited fragrance materials from washed fabrics. These fragrance delivery technologies can also be used to further increase the persistence of fragrance release from washed fabrics. Suitable fragrance delivery technologies include: fragrance microcapsules, pre-fragrances, polymer-assisted delivery, molecular-assisted delivery, fiber-assisted delivery, amine-assisted delivery, cyclodextrins, starch-encapsulated blends, zeolites and other inorganic carriers, and any mixtures thereof.

[0076] Suitable encapsulating flavorings may contain materials selected from the group consisting of flavoring ingredients and / or optionally materials selected from the group consisting of: vegetable oils (including pure vegetable oils and / or blended vegetable oils), including castor oil, coconut oil, cottonseed oil, grape oil, rapeseed oil, soybean oil, corn oil, palm oil, flaxseed oil, safflower oil, olive oil, peanut oil, coconut oil, palm kernel oil, castor oil, lemon oil, and mixtures thereof; esters of vegetable oils, including dibutyl adipate, dibutyl phthalate, and butyl acetate. Benzyl butyl adipic acid, octyl benzyl adipate, tricresyl phosphate, trioctyl phosphate, and mixtures thereof; straight-chain or branched hydrocarbons, including those having a boiling point greater than about 80°C; partially hydrogenated terphenyl, phthalates, alkyl biphenyls (including monoisopropyl biphenyl), alkylated naphthalenes (including dipropyl naphthalene), petroleum solvents (including kerosene), mineral oils, and mixtures thereof; aromatic solvents, including benzene, toluene, and mixtures thereof; silicone oils; and mixtures thereof.

[0077] Suitable fragrance delivery systems may take the form of polymer-assisted delivery systems. Such fragrance delivery systems may take the form of encapsulations, such as core-shell encapsulations, where the core contains the fragrance ingredient and is surrounded by a polymer shell. The polymer shell may comprise polymeric materials derived from polyacrylates, polyureas, polyurethanes, polysaccharides, polyvinyl alcohol, melamine, their derivatives, or combinations thereof. Additionally or alternatively, suitable fragrance delivery systems may include known fragrance precursor / aromatic agent precursor materials.

[0078] Pyridine dicarboxylic acid

[0079] Pyridine dicarboxylic acids (pyridine-2,6-dicarboxylic acids or PDC and DPA) have the following formula:

[0080]

[0081] Pyridine dicarboxylic acids can exist in different forms depending on the dissociation state of their carboxylic acid groups: fully protonated, partially protonated (one negative charge), or fully unprotonated (two negative charges), as shown above. Salts of pyridine dicarboxylic acids (also known as dipicolinates) can be formed by coordination between the negative charge of the unprotonated carboxylic acid and a positively charged counterion. Suitable positively charged counterions are selected from sodium, potassium, calcium, magnesium, hydrochloride, or mixtures thereof, preferably sodium. Other suitable positively charged counterions will be known to those skilled in the art.

[0082] The term pyridine dicarboxylic acid is not limited to the acid (protonated) form, but should be extended in its interpretation to include pyridine dicarboxylic acid in the acid (protonated) form, pyridine dicarboxylic acid in the partially and / or completely unprotonated form, salts of pyridine dicarboxylic acid, or mixtures thereof.

[0083] In a preferred aspect of the invention, pyridine dicarboxylic acid or its salt may be present at a concentration between 0.5% and 90%, preferably between 0.5% and 31%, and more preferably between 1% and 5% based on the weight of the first particle. Even pyridine dicarboxylic acid may be present at a concentration between 0.5% and 5% based on the weight of the first particle, or even between 0.5% and less than 3%.

[0084] Unbound by theory, the close contact and mixing of pyridine dicarboxylic acid with surfactants to form the first particles allows low concentrations of pyridine dicarboxylic acid to produce the desired effect. Low concentrations of pyridine dicarboxylic acid (between 1% and 5% by particle weight) may be superior to high concentrations (up to 90% by particle weight) because it leaves greater flexibility for adding other active ingredients as part of the particles, potentially producing additional beneficial effects.

[0085] The composition may contain pyridine dicarboxylic acid at a weight of between 0.1% and 40%, preferably between 0.5% and 20%, more preferably between 0.5% and 10%, and most preferably between 1% and 5%.

[0086] surfactants

[0087] Surfactants should be understood as detergency surfactants. Suitable detergency surfactants include anionic, nonionic, cationic, amphoteric, and amphoteric surfactants. Suitable detergency surfactants can be linear or branched, substituted or unsubstituted, and can be derived from petrochemical or biological materials. Suitable and preferred surfactants will be discussed in more detail below.

[0088] Suitable anionic detergency surfactants include sulfonate detergency surfactants and sulfate detergency surfactants.

[0089] Suitable sulfonate detergency surfactants include methyl ester sulfonates, α-olefin sulfonates, alkylbenzene sulfonates, especially alkylbenzene sulfonates, preferably C 10-13 Alkylbenzene sulfonates. Suitable alkylbenzene sulfonates (LAS) are available, preferably obtained by sulfonating commercially available linear alkylbenzenes (LABs); suitable LABs include lower 2-phenyl LABs, and other suitable LABs include higher 2-phenyl LABs, such as those marketed under the trade name Hyblene. ® Those supplied by Sasol.

[0090] Suitable sulfate detergency surfactants include alkyl sulfates, preferably C 8-18 Alkyl sulfates, or mainly C 12 Alkyl sulfates.

[0091] Preferred sulfate detergency surfactants are alkylalkoxylated sulfates, preferably alkylethoxylated sulfates, and preferably C 8-18 Alkyl alkoxylated sulfates, preferably C 8-18 Alkyl ethoxylated sulfates, preferably alkyl alkoxylated sulfates, have an average degree of alkoxylation of 0.5 to 20, preferably 0.5 to 10, and preferably alkyl alkoxylated sulfates are C 8-18 Alkyl ethoxylated sulfate having an average degree of ethoxylation of 0.5 to 10, preferably 0.5 to 5, more preferably 0.5 to 3, and most preferably 0.5 to 1.5.

[0092] Alkyl sulfates, alkylalkoxylated sulfates, and alkylbenzene sulfonates can be linear or branched, substituted or unsubstituted, and can be derived from petrochemical or biological materials. Other suitable anionic detergency surfactants include alkyl ether carboxylates.

[0093] Suitable anionic detergency surfactants can be in the form of salts, and suitable counterions include sodium, calcium, magnesium, amino alcohols, and any combination thereof. Sodium is the preferred counterion.

[0094] Suitable nonionic detergency surfactants are selected from the group consisting of: C8-C 18 Alkyl ethoxylates, such as NEODOL from Shell ® Nonionic surfactant; C6-C 12 Alkylphenol alkoxylates, wherein preferably the alkoxyl unit is an ethyleneoxy unit, an propyleneoxy unit, or a mixture thereof; C 12 -C 18 Alcohols and C6-C 12 Condensations of alkylphenols with ethylene oxide / propylene oxide block polymers, such as Pluronic from BASF.® Alkyl polysaccharides, preferably alkyl polyglycosides; methyl ester ethoxylates; polyhydroxy fatty acid amides; ether-terminated poly(alkoxylated) alcohol surfactants; and mixtures thereof.

[0095] Suitable nonionic detergency surfactants are alkyl polyglucosides and / or alkyl alkoxylated alcohols.

[0096] Suitable nonionic detergency surfactants include alkylalkoxylated alcohols, preferably C 8-18 Alkyl alkoxylated alcohols, preferably C 8-18 Alkyl ethoxylated alcohols, preferably alkyl alkoxylated alcohols, have an average degree of alkoxylation of 1 to 50, preferably 1 to 30, or 1 to 20, or 1 to 10, and preferably alkyl alkoxylated alcohols are C10 and C20. 8-18 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. Alkyl alkoxylated alcohols can be straight-chain or branched, and substituted or unsubstituted.

[0097] Suitable nonionic detergency surfactants include detergency surfactants based on secondary alcohols.

[0098] Suitable cationic detergency surfactants include alkylpyridinium compounds, alkyl quaternary ammonium compounds, alkyl quaternary phosphonium compounds, alkyl ternary sulfonium compounds, and mixtures thereof.

[0099] Preferred cationic detergency surfactants are quaternary ammonium compounds having the following general formula:

[0100] (R)(R1)(R2)(R3)N + X -

[0101] Where R is a straight or branched chain, substituted or unsubstituted C. 6-18 The alkyl or alkenyl moiety, R1 and R2 are independently selected from the methyl or ethyl moiety, R3 is the hydroxyl, hydroxymethyl or hydroxyethyl moiety, and X is an anion that provides electroneutrality, preferably including: halide ions, preferably chloride ions; sulfate ions; and sulfonate ions.

[0102] Suitable amphoteric detergency surfactants include amine oxides and / or betaine.

[0103] In a preferred aspect of the invention, a surfactant may be present in an amount between 5% and 99% by weight of the first particle, preferably between 5% and less than 50%, and more preferably between 8% and 25%.

[0104] In a preferred aspect of the invention, the surfactant may be selected from anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, or mixtures thereof, preferably wherein the surfactant is anionic. Not bound by theory, the invention can be used with different types of surfactants; however, the presence of anionic surfactants and pyridine dicarboxylic acids in the co-formulation increases the foaming properties of the formulation.

[0105] The anionic surfactant is selected from linear alkyl sulfates, branched alkyl sulfates, alkoxylated alkyl sulfates, methyl ester sulfonates, linear alkylbenzene sulfonates, or mixtures thereof, preferably linear alkylbenzene sulfonates.

[0106] Suitable straight-chain alkyl sulfates can be C8-18 straight-chain alkyl sulfates, preferably C12-14 straight-chain alkyl sulfates.

[0107] Suitable branched alkyl sulfates can have the following formula:

[0108]

[0109] Where X is a sulfate group, m is greater than or equal to 0 and n is less than or equal to 16, preferably where m is between 6 and 11 and n is between 0 and 5.

[0110] Suitable alkoxylated alkyl sulfates can be C12-18 alkoxylated alkyl sulfates, more preferably C12-15 alkoxylated alkyl sulfates.

[0111] The methyl ester sulfonate is preferably a C16-18 methyl ester sulfonate.

[0112] The linear alkylbenzene sulfonate is preferably a C10-13 linear alkylbenzene sulfonate.

[0113] Particles

[0114] The presence of a first particle in a particulate laundry detergent composition means that a second, third, or even more particles may be present, as long as the first particle contains a surfactant and pyridine dicarboxylic acid or a salt thereof.

[0115] The first particles may be present in amounts between 1% and 99% by weight of the composition.

[0116] In a preferred aspect of the invention, a first particle may be present in a weight of 40% to 80%, more preferably between 40% and 60%, based on the composition.

[0117] In a preferred aspect of the invention, the first particle may have a density between 0.1 g / cm³ and 1.5 g / cm³, most preferably between 0.3 g / cm³ and 0.9 g / cm³. Those skilled in the art will know common methods for measuring the density of said particle. The first particle may be selected from the group consisting of blown powders, agglomerates, extrudates, encapsulants, flakes, pellets, granules, and mixtures thereof, more preferably agglomerates, blown powders, and mixtures thereof, and most preferably blown powders. Those skilled in the art will know common methods for producing these types of particles. Exemplary versions will be described later in the specification.

[0118] Unbound by theory, the first particle, in the form of blown powder, possesses the best physicochemical properties that provide optimal results in foam formation.

[0119] In another preferred aspect of the invention, the composition may contain water at a concentration between 0.1% and 4%, preferably between 1% and 4%, based on the weight of the first particles. Without being bound by theory, a higher weight percentage of water will increase the viscosity of the particles, leading to clumping and agglomeration in the mechanical tube. This phenomenon will affect the handling and processability of the particles during manufacturing. Furthermore, excessive water in the particles may promote microbial growth, thereby affecting the shelf life and long-term stability of the composition.

[0120] In another aspect of the invention, the first particle may comprise at least one inorganic material selected from carbonates, sulfates, chlorides, silicates, or mixtures thereof, preferably wherein the at least one inorganic material comprises at least one counterion, more preferably wherein the at least one counterion is selected from the group consisting of alkali metals or alkaline earth metals.

[0121] Preferably, the first particle contains inorganic material comprising between 1% and 90%, more preferably between 20% and 60%.

[0122] Suitable carbonates may include carbonate salts. The first particle may contain 0% to 70% by weight of carbonate, or 5% to 30% by weight of carbonate. The first particle may even be substantially free of carbonate; substantially free of carbonate means "without intentional addition". Suitable carbonates include sodium carbonate and sodium bicarbonate. The preferred carbonate is sodium bicarbonate.

[0123] Suitable silicates may include silicate salts. The first particle may contain 0% to 20% by weight of silicate, or 4% to 15% by weight of silicate. The first particle may even be substantially free of silicate; substantially free of means "without intentional addition". Preferred silicate is sodium silicate, particularly preferred is sodium silicate having a Na₂O:SiO₂ weight ratio of 1.0 to 2.8, preferably 1.6 to 2.35.

[0124] Suitable sulfates may include sulfate salts. The first granule may contain 0% to 80% by weight of sulfate, or 30% to 50% by weight of sulfate. The first granule may even be substantially sulfate-free; substantially sulfate-free means "without intentional addition". The preferred sulfate is sodium sulfate.

[0125] Suitable chlorides may include chloride salts. The first particle may contain 0% to 80% by weight of chloride salt, or 30% to 50% by weight of chloride salt. The first particle may even be substantially free of chloride salt; substantially free of means "without intentional addition". The preferred chloride salt is sodium chloride.

[0126] Alkali metals are elements in Group 1 of the periodic table, such as Li, Na, K, Rb, Cs, and Fr.

[0127] Alkaline earth metals are elements in Group 2 of the periodic table, such as Be, Mg, Ca, Sr, Ba, and Ra.

[0128] Counterions can preferably be selected from Na, K, Mg or Ca.

[0129] It should be understood that counterions can also be ammonium ions or any other ions that the technician deems suitable as part of an inorganic material.

[0130] The term coordination refers to the ionic bond between a negative charge and a positive charge. In this respect, the negative charge is carried by the dissociated form of carbonates, sulfates, chlorides, silicates, or mixtures thereof, and the positive charge is carried by counter ions.

[0131] Consumer products

[0132] In a second aspect, the present invention relates to a consumer product comprising packaging and a composition according to the first aspect, wherein the packaging comprises at least one compartment in which the composition is contained.

[0133] The fact that the packaging includes at least one compartment means that it may contain a second, third, or even more compartments, as long as the at least one compartment can contain the composition of the present invention. Those skilled in the art will know suitable packaging for the compositions of the present invention. Exemplary versions of such packaging are described herein.

[0134] Packaging can be plastic, fiber-based, or a mixture thereof. Fiber-based packaging may include cardboard, corrugated cardboard, or a mixture thereof. When packaging contains both plastic and fiber-based materials, it is preferable that the packaging contains less than 10% by weight, or even less than 5% by weight, of fiber-based material. This ratio of plastic to fiber-based material is preferred because such low plastic content allows the packaging to be placed in paper recycling streams in many countries.

[0135] The packaged product includes packaging. The packaging includes an opening and at least one internal compartment communicating with the opening. A particulate laundry detergent composition is contained within the internal compartment. Preferably, the opening is sized sufficiently to allow a user to pass their hand through the opening and retrieve the particulate laundry detergent composition contained therein.

[0136] The packaging may contain cellulose-containing materials, plastics, or mixtures thereof, preferably wherein the packaging contains at least 50% recycled material by weight of the packaging. Preferably, the cellulose-containing materials include cardboard, corrugated cardboard, paperboard, or mixtures thereof.

[0137] The packaging may have any suitable shape and size. Those skilled in the art will know suitable packaging sizes and dimensions. The packaging may include elements such as a handle and a closure. If the packaging includes a closure, it may be a resealable cap, such as a hinged cap, screw cap, or removable cap. The packaging may include child-proof closures or other latches or locking mechanisms that prevent child access or child-proof opening. Those skilled in the art will know suitable methods.

[0138] The packaging may include a dispensing device for dispensing a particulate laundry detergent composition from the packaging into a laundry washing machine (or a laundry tub in a hand-washing application). The user can use the dispensing device to measure a recommended unit dose, or simply to measure the particulate laundry detergent composition according to their own preference. Examples of the dispensing device may be a dispensing cap, dome, etc., functionally attached to the packaging. The dispensing device may be releasable from and reattachable to the packaging, such as a cup that can be mounted on the packaging. The dispensing device may be fastened (e.g., by a hinge or thread) to the rest of the packaging (or alternatively, not fastened). The dispensing device may have one or more dividing lines (e.g., filler lines) to indicate the recommended unit dose. The packaging may include instructions for instructing the user to open a removable opening in the packaging and to dispense (e.g., pour) the particulate laundry detergent composition contained in the packaging into the dispensing device. The user can then be instructed to dispense the particulate laundry detergent composition from the dispensing device into a laundry washing machine or laundry tub. The granular laundry detergent composition of the present invention can be used to increase the freshness of laundry. The packaging, including the dispensing device, can be made of plastic.

[0139] Methods of washing fabrics

[0140] In a third aspect, the present invention relates to a method for washing a fabric, the method comprising the steps of: A) obtaining at least one fabric to be washed and a washing liquid; and B) bringing the at least one fabric and the washing liquid into contact with each other, wherein the washing liquid comprises a composition according to the first aspect and water, wherein the water has a hardness between 0°D and 28.77°D, preferably between 4.80°D and 19.18°D, more preferably between 6.71°D and 14.39°D.

[0141] Water hardness is measured using the following test method.

[0142] A method for washing fabrics includes contacting a particulate laundry detergent composition with water to form a washing liquid, and washing the fabric in the washing liquid. Typically, the washing liquid has a temperature above 0°C to 90°C, or up to 60°C, or up to 40°C, or up to 30°C, or up to 20°C. The fabric may be in contact with water before, after, or simultaneously with contacting the particulate laundry detergent composition with water. Typically, the washing liquid is formed by contacting the particulate laundry detergent composition with water in an amount such that the concentration of the particulate laundry detergent composition in the washing liquid is from 0.2 g / L to 20 g / L, or from 0.5 g / L to 10 g / L, or up to 5.0 g / L. The method for washing fabrics 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-wash container. Typically, the washing liquid contains 90 liters or less, or 60 liters or less, or 15 liters or less, or 10 liters or less of water. Typically, 200g or less, or 150g or less, or 100g or less, or 50g or less of a particulate laundry detergent composition is brought into contact with water to form a detergent liquid.

[0143] Method for preparing the composition

[0144] In a fourth aspect, the present invention relates to a method for preparing a composition according to the first aspect, the method comprising the steps of: A) mixing pyridine dicarboxylic acid, a surfactant and water to produce a slurry; and B) drying the slurry to obtain first particles.

[0145] Unbound by theory, certain components of particulate laundry detergent compositions, such as surfactants and silicates, absorb moisture from the air (hygrosensitivity), resulting in higher cohesion of the particles and a shift to an amorphous state. This state reduces particle flowability, causing problems during manufacturing, such as clumping and agglomeration in mechanical tubes. Furthermore, reduced efficacy in use can be observed after prolonged storage in humid environments. Particles containing pyridine dicarboxylic acid and surfactants are believed to exhibit surprisingly low hygrosensitivity and potentially beneficial effects in terms of handling, processability, and long-term stability. Unbound by theory, pyridine dicarboxylic acid can create a shield around the particles, preventing ambient water from entering them. Alternatively, pyridine dicarboxylic acid can directly absorb ambient water, preventing it from reaching sensitive components such as surfactants or silicates.

[0146] Unbound by theory, fast-dissolving and low-density concentrated granular laundry detergent compositions typically require a large amount of energy in the form of heat to dry the product during spray drying.

[0147] By adding pyridine dicarboxylic acid along with other surfactants to the spray-dried particles, we surprisingly observed a significant improvement in the drying efficiency of the spray-dried particles, thereby reducing the energy consumption associated with their manufacture.

[0148] Those skilled in the art will know the granulation methods and corresponding processing steps used to produce granular laundry detergent products. An exemplary version is explained here:

[0149] Pyridine dicarboxylic acid can be mixed with linear alkylbenzene sulfonates and inorganic materials such as alkali metal salts. The mixture may contain 0.1% to 20% by weight, most preferably 0.5% to 5% by weight, of pyridine dicarboxylic acid on a dry basis, and 5% to 50% by weight, most preferably 8% to 30% by weight, of linear alkylbenzene sulfonates. Alkali metal salts can be added as filler balancing materials.

[0150] Optionally, additional materials may be added to the blend, including but not limited to: alkali metal silicates, alkali metal hydroxides, maleic acid / acrylates, water, metal carbonates, and / or dyes. The blend may be produced in batch or continuous mixing tanks. Batch mixing tanks are preferred.

[0151] Pyridine dicarboxylic acid can be added to the mixer or agitator immediately after the addition of water but before the addition of metal carbonate. Preferably, the following order of addition is followed: linear alkylbenzene sulfonate, pyridine dicarboxylic acid, remaining liquid feedstock, metal carbonate, and filler balancing material.

[0152] Liquid blends may undergo a curing process. Suitable curing processes include, but are not limited to, spray drying, roller drying, agglomeration, pelletizing, coating, spray freeze-drying, and extrusion. Spray drying is preferred.

[0153] After curing, the material is processed into particles ranging from 50 μm to 1600 μm through size grading, sieving, grinding, crushing, milling, and / or agglomeration. Subsequently, and optionally, the particles can be dry-mixed with powder additives, including but not limited to: enzymes, optical brighteners, polymers, fillers, flow aids, dispensing aids, aesthetic agents, fragrances, and / or other particles containing active substances. Finally, and optionally, the resulting powder mixture can be loaded with small amounts of active substances and / or fragrances in liquid form through a spraying process.

[0154] Typically, suitable agglomeration methods involve contacting detergency components, such as detergency surfactants, such as linear alkylbenzene sulfonates and / or alkylalkoxylated sulfates, with inorganic materials, such as sodium carbonate and / or silica, in a mixer. Agglomeration methods can also be in-situ neutralization agglomeration methods, wherein acidic precursors of detergency surfactants, such as linear alkylbenzene sulfonates, are contacted with alkaline materials, such as carbonates and / or sodium hydroxide, in a mixer, and wherein the acidic precursors of detergency surfactants are neutralized by the alkaline material during the agglomeration process to form the detergency surfactant. Other suitable detergent components that can be agglomerated include polymers, chelating agents, bleach activators, siloxanes, and any combinations thereof.

[0155] The agglomeration method can be a high-, medium-, or low-shear agglomeration method, wherein high-, medium-, or low-shear mixers are used accordingly. The agglomeration method can be a multi-step agglomeration method, wherein two or more mixers are used, such as a combination of a high-shear mixer and a medium- or low-shear mixer. The agglomeration method can be a continuous method or a batch method. It is preferable for the agglomerate to undergo a drying step, for example, a fluidized bed drying step. It is also preferable for the agglomerate to undergo a cooling step, for example, a fluidized bed cooling step.

[0156] Typically, agglomerates undergo particle size classification, such as fluidized bed washing 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 of 300 micrometers to 800 micrometers, and less than 10% by weight of the agglomerates have a particle size of less than 150 micrometers, and less than 10% by weight of the agglomerates have a particle size of greater than 1200 micrometers. For fine and excessively large agglomerates, recycling back into the agglomeration process is preferred. Typically, excessively large particles undergo a pulverizing step, such as grinding, and are recycled back to the appropriate location in the agglomeration process, such as a mixer. Typically, fine powder is recycled back to the appropriate location in the agglomeration process, such as a mixer.

[0157] For the ingredients, such as polymers and / or nonionic detergency surfactants and / or fragrances, it is preferable to spray them onto the base detergent particles, such as spray-dried base detergent particles and / or agglomerated base detergent particles. Typically, this spraying step is carried out in a tumbling drum mixer.

[0158] In a preferred aspect of the invention, mixing can be carried out in a mixer, and drying can be thermal drying, preferably spray drying, wherein spray drying converts the slurry into blown powder, preferably wherein the blown powder has an average particle size between 0.1 mm and 1.8 mm, more preferably between 0.2 mm and 0.8 mm, and most preferably between 0.3 mm and 0.6 mm, and preferably wherein thermal drying is carried out in a heating tower.

[0159] Unbound by theory, spray drying is advantageous compared to other granulation methods because it provides improved physicochemical properties to the granules to deliver the aforementioned beneficial effects.

[0160] Technicians will know how to operate the agitator used to mix the ingredients for making granular laundry detergent compositions.

[0161] Typically, a suitable heating and drying method is the drying method described above, in which heat is used as the form of energy. Those skilled in the art will know suitable heating and drying methods for producing the particles and the operation of the heating tower. Preferably, the heating tower is a spray drying tower.

[0162] Typically, a suitable spray drying method involves forming an aqueous slurry mixture, transferring the aqueous slurry mixture to a pressure nozzle using at least one pump, preferably two pumps, atomizing the aqueous slurry mixture into a spray drying tower, and drying the aqueous slurry mixture to form spray-dried particles. Preferably, the spray drying tower is a counter-current spray drying tower, although a co-current spray drying tower is also suitable.

[0163] Typically, spray-dried powders are cooled, for example, by air stripping. Typically, spray-dried powders are subjected to particle size classification, such as sieving, to obtain a desired particle size distribution. Preferably, the spray-dried powders have a particle size distribution such that the weight-average particle size is in the range of 300 to 500 micrometers, and less than 10% by weight of the spray-dried particles have a particle size greater than 2360 micrometers.

[0164] Preferably, the aqueous slurry mixture is heated to raise the temperature before atomization into the spray drying tower. For anionic surfactants, such as linear alkylbenzene sulfonates, it is preferable to introduce them into the spray drying process after the step of forming the aqueous slurry mixture: for example, the acid precursor is introduced into the aqueous slurry mixture after pumping. For gases, such as air, it is preferable to introduce them into the spray drying process after the step of forming the aqueous slurry. For any inorganic components, such as sodium sulfate and sodium carbonate, it is preferable to micronize them into small particle sizes if they are present in the aqueous slurry mixture.

[0165] Test methods

[0166] Particle density determined

[0167] Those skilled in the art will know common methods for measuring particle density as defined in this patent. Exemplary versions of the test methods used are as follows:

[0168] The particle density as defined in this patent is the apparent volume density. Apparent volume density is defined as the mass of the sample divided by its total volume, which includes the solid material and the void space between the particles. This method can be used for free-flowing materials. The material is poured freely through a funnel into a measuring cup of known volume. The apparent volume density is obtained by weighing the empty and full measuring cups. The steps of this process are as follows:

[0169] Weigh a clean, empty cup to an accuracy of 0.1 g and place the weighed cup under the funnel. Seal the funnel at its bottom opening, keeping the sealing plate gently against the funnel opening. Fill the funnel with the sample up to the upper lip, then quickly open the seal to allow the sample to flow in and overflow the cup. Carefully level the contents of the cup with the straight edge, then gently tap to compact the powder; this helps prevent accidental spillage during weighing. Weigh the cup containing the sample to an accuracy of 0.1 g. Perform a density measurement on the grasped sample. Once the grasped sample is removed from the carton, the carton is no longer representative and cannot be used for quantitative analysis.

[0170] Water hardness measurement

[0171] Technicians will be familiar with common methods for measuring water hardness. An exemplary version of the test method used is as follows:

[0172] The principle of this test method lies in the simple determination of water hardness (based on the presence of magnesium and / or calcium) through reaction with EDTA. The disodium salt of ethylenediaminetetraacetic acid (EDTA) forms stable complexes with calcium and magnesium ions. This property serves as the basis for a simple volumetric determination of water hardness. Calcium / magnesium ions are titrated with EDTA using a hardness indicator, which itself forms a colored metal complex. The volume (ml) of EDTA required to induce this color change is substituted into a standard calculation method, which will give the total (or calcium / magnesium) hardness of the water.

[0173] Take a clean 100mL graduated cylinder and use it to take out 50mL of water sample whose hardness needs to be determined.

[0174] Place the sample in a porcelain mortar and add one total hardness indicator tablet (BDH Laboratory Supplies, Pool BH15 1TD Reagent D Prod 16023 2E), crushing it to ensure complete dissolution. Add 5 drops of undiluted ammonia buffer solution (containing 15% w / v NH3), resulting in a pink / red solution. Titrate the solution with 0.01M EDTA solution (from a burette) until a color change from pink / red to clear blue is observed.

[0175] Record the EDTA titer and apply the following equation:

[0176]

[0177]

[0178] Reference: p779 The Water Encyclopedia Second Edition 1990 Frits van der Leeden

[0179] For a standard 50 mL water sample divided into equal portions, the above equation can be simplified as follows:

[0180]

[0181] Example

[0182] Example 1 .

[0183] Granular laundry detergent powder A is manufactured by spray drying particles having the composition shown in Table 1. This formulation does not contain pyridine dicarboxylic acid.

[0184] Granular laundry detergent composition powder B was prepared separately by spray drying of particles having the composition shown in Table 1. Then, 97 parts of the spray-dried particles were dry-mixed with 3 parts of powdered pyridine dicarboxylic acid.

[0185] Finally, granular laundry detergent composition powder C was prepared by spray drying of particles containing 3% by weight of pyridine dicarboxylic acid. The composition of powder C is shown in Table 1.

[0186] Table 1. Composition of powder A, powder B and powder C

[0187]

[0188] At 25°C, powders A, B, and C were dissolved in 500 ml of water with a hardness of 21.10°D inside a cylindrical container with a height of 29 cm and a diameter of 9 cm to prepare a washing liquid with a concentration equivalent to 378 ppm of linear alkylbenzene sulfonate in all three cases.

[0189] During the time interval, the washing liquid in the cylindrical container swirls at a constant rotational speed of 30 revolutions per minute.

[0190] In the experiment, after 180 seconds, 160 μL of technical scale (a mixture of paraffin oil and fatty acids with the composition shown in Table 2) was added to each washing liquid, followed by tumbling four more times. Finally, after 420 seconds of tumbling, an additional 320 μL of scale was added to each washing liquid, and tumbling was continued for another 10 times. The height of the foam generated inside the cylinder after each time interval was recorded by measuring the distance between the water-foam interface and the lowest point of the concave meniscus formed at the top of the foam inside the cylinder. The height of the foam generated inside the cylinder after each time interval is recorded and shown in Table 3.

[0191] As can be observed in Table 3, powder A achieved the lowest foam height among the three products throughout the experiment. The Δ values ​​in the last two columns of Table 3 represent the increase in foam height when pyridine dicarboxylic acid was co-formulated with the surfactant in the same granules.

[0192] Surprisingly, despite having the same composition, powder C achieved a higher foam height than powder B in the later stages of the test (after dirt was added).

[0193] Table 2 - Composition of Technical Scale

[0194]

[0195] Table 3. Foam measured inside the rolling cylinder at different time intervals before and after the addition of technical fouling. high

[0196]

[0197] Example 2

[0198] Granular laundry detergent powder D is manufactured by spray drying particles having the composition shown in Table 4. This formulation does not contain pyridine dicarboxylic acid.

[0199] Granular laundry detergent powder E was prepared by spray drying of particles containing 3% by weight of pyridine dicarboxylic acid. The composition of powder E is shown in Table 4.

[0200]

[0201] Powder D and powder E were both packed into identical cardboard boxes with a total surface area of ​​1800 cm² and a moisture transfer rate of 50 g / m² / day. The moisture transfer rate of the packaging material was determined by dynamic vapor adsorption. Methods for performing dynamic vapor adsorption on packaging materials are known to those skilled in the art. Each box contained 1500 g of powder. The boxes were then kept inside an oven conditioned at 32°C and 80% relative humidity for up to 7 days. Every 7 hours, one box of powder D and powder E was removed from the oven and allowed to cool and equilibrate with the ambient temperature and humidity for 12 hours. Subsequently, each box was opened, and the flowability of the powder was qualitatively examined according to the grading criteria shown in Table 5. The relative humidity of the powder was also measured. Those skilled in the art know that relative humidity is a technical term describing the free moisture in a powder sample.

[0202] Table 5. Grading scale for powder flowability

[0203]

[0204] At the end of the experiment, graphs were plotted for the flowability grade of powders D and E relative to the relative humidity of the powders. As expected, the flowability of the powders decreased with increasing relative humidity. The relative air humidity of the powders when the flowability was below the threshold grade of 6 was calculated as a measure of humidity sensitivity. These values ​​are recorded in Table 6.

[0205] Table 6. Critical equilibrium relative humidity for powders D and E.

[0206]

[0207] As can be observed in Table 6, the critical equilibrium relative temperature of powder E is significantly higher than that of powder D, indicating that powder E has lower moisture sensitivity.

[0208] The dimensions and values ​​disclosed herein should not be construed as strictly limited to the precise numerical values ​​cited. Rather, unless otherwise specified, each such dimension is intended to represent the stated value and the range surrounding its functional equivalent. For example, a dimension disclosed as “40 mm” is intended to represent “approximately 40 mm”.

Claims

1. A particulate laundry detergent composition, said particulate laundry detergent composition comprising a surfactant and pyridine dicarboxylic acid or a salt thereof, The composition said composition comprises a first particle, Its features are, The first particle contains the surfactant and the pyridine dicarboxylic acid or a salt thereof.

2. The composition according to claim 1, wherein the pyridine dicarboxylic acid or its salt is present in an amount between 0.5% and 90%, preferably between 0.5% and 31%, more preferably between 1% and 5% based on the weight of the first particles.

3. The composition according to claims 1 to 2, wherein the pH of the composition in use is at least 9, preferably between 10 and 10.5, wherein the pH of the composition in use is measured at a temperature of 20°C and a concentration of 1 g / L in deionized water.

4. The composition according to any of the preceding claims, wherein the first particles are present in an amount between 40% and 80%, preferably between 40% and 60%, based on the weight of the composition.

5. The composition according to any of the preceding claims, wherein the surfactant is present in an amount between 5% and 99% by weight of the first particles, preferably between 5% and less than 50%, more preferably between 8% and 25%.

6. The composition according to any preceding claim, wherein the composition comprises water at a concentration between 0.01% and 4% by weight of the composition. Preferably, the composition comprises water at a concentration between 0.1% and 4%, more preferably between 1% and 4%, based on the weight of the first particles.

7. The composition according to any of the preceding claims, wherein the surfactant is selected from anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, or mixtures thereof. Preferably, the surfactant is an anionic surfactant.

8. The composition according to claim 7, wherein the anionic surfactant is selected from linear alkyl sulfates, branched alkyl sulfates, alkoxylated alkyl sulfates, methyl ester sulfonates, linear alkylbenzene sulfonates, or mixtures thereof, preferably linear alkylbenzene sulfonates. Preferably, the linear alkylbenzene sulfonate is a C10-13 linear alkylbenzene sulfonate.

9. The composition according to any preceding claim, wherein the first particle further comprises at least one inorganic material selected from carbonates, sulfates, chlorides, silicates, and mixtures thereof. Preferably, the at least one inorganic material contains at least one counterion; more preferably, the at least one counterion is selected from the group consisting of alkali metals or alkaline earth metals.

10. The composition according to any of the preceding claims, wherein the first particles have a density between 0.1 g / cm³ and 1.5 g / cm³, most preferably between 0.3 g / cm³ and 0.9 g / cm³. Preferably, the first particle is selected from the group consisting of blown powder, agglomerates, extruders, encapsulants, flakes, pellets, granules, and mixtures thereof, more preferably agglomerates, blown powder, and mixtures thereof, and most preferably blown powder.

11. The composition according to any preceding claim, further comprising an auxiliary component, wherein the auxiliary component is selected from the group consisting of amines, surfactant systems, water-binding agents, sulfites, fatty acids and / or their salts, enzymes, encapsulated beneficial agents, detergent polymers, toning agents, washing aids, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalysts, bleaching agents, bleaching catalysts, bleaching activators, dirt removers / anti-redeposition agents, polymer dispersants, polymer grease cleaners, brighteners, defoamers, dyes, fragrances, encapsulated fragrances, fragrance delivery systems, structural elasticizers, fabric softeners, carriers, fillers, water-soluble additives, organic solvents, antimicrobial agents and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, rheology modifiers or structural agents, opacifiers, pearlescent agents, pigments, corrosion inhibitors and / or rust inhibitors, and mixtures thereof.

12. A consumer product comprising packaging and the composition according to claims 1 to 11, wherein the packaging comprises at least one compartment, and wherein the composition is contained in the at least one compartment.

13. A method for washing fabrics, the method comprising the following steps: A) Obtain at least one fabric to be washed and a washing liquid; as well as B) Bring the at least one fabric and the washing liquid into contact with each other. The washing liquid comprises the composition according to claims 1 to 11 and water. The water has a hardness between 0°D and 28.77°D, preferably between 4.80°D and 19.18°D, and more preferably between 6.71°D and 14.39°D.

14. A method for preparing the composition according to claims 1 to 11, the method comprising the following steps: A) Pyridine dicarboxylic acid, a surfactant, and water are mixed to produce a slurry; as well as B) Dry the slurry to obtain the first particles.

15. The method according to claim 14, The mixing is carried out in a mixer. The drying process is heat drying, and preferably the heat drying process is spray drying, wherein the spray drying converts the slurry into blown powder. Preferably, the blown powder has an average particle size between 0.1 mm and 1.8 mm, more preferably between 0.2 mm and 0.8 mm, and most preferably between 0.3 mm and 0.6 mm. Preferably, the heating and drying is carried out in a heating tower.

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