Fragrance-containing particles and methods of making

Abstract

A laundry additive composition is disclosed, the laundry additive composition comprising a plurality of fragrance-containing particles, where each of the fragrance-containing particles comprises: a fragrance ingredient; polyethylene glycol; and an inorganic salt carrier selected from the group consisting of magnesium sulfate, magnesium chloride, and combinations thereof wherein each of the perfume-containing particles has a mass of from 1 mg to 1 g and a maximum size of from 3 mm to 10 mm.

Description

Technical Field

[0001] The present invention relates to fragrance - emitting particles containing magnesium inorganic salts and a method for preparing the same. Background Art

[0002] When consumers do laundry, fragrance is considered a source of pleasure for consumers. Consumers can associate certain fragrances with the performance of laundry products and use them as an indicator of the quality of laundry products. When consumers dispense laundry products, transfer a large amount of wet laundry from the washing machine to the dryer or drying rack or drying line, or when consumers wear clothes, laundry products that provide a pleasant or enhanced fragrance experience meet the needs of the consumers.

[0003] Accordingly, fragrance - containing particles are becoming increasingly popular as laundry fragrance additives. Fragrance - containing particles can be used to impart a new fragrance to the articles being washed or enhance the existing fragrance in the articles being washed.

[0004] Most such fragrance - containing particles contain one or more fragrance components mixed with a carrier material. The fragrance components can be selected from the group consisting of: free fragrances, encapsulated fragrances (also known as perfume microcapsules, PMC), and combinations thereof. The carrier material can be selected from the group consisting of: polymers (e.g., polyethylene glycol, ethylene oxide / propylene oxide block copolymer, polyvinyl alcohol, polyvinyl acetate, and their derivatives), proteins (e.g., gelatin, albumin, casein, etc.), sugars (e.g., dextran, fructose, galactose, glucose, isoglucose, sucrose, etc.), water - soluble or water - dispersible fillers (e.g., zeolite, silica, clay, etc.), and combinations thereof. Some fragrance - containing particles contain only one type of carrier material, while other particles can contain a mixture of two or more different carrier materials.

[0005] There is a continuing need for fragrance - containing particles that provide a long - lasting pleasant fragrance experience to consumers, for example, after drying or even after storage. One approach is to increase the content of perfume microcapsules (PMC), which release fragrance more slowly compared to free fragrances. However, it has been found that fragrance - emitting particles containing too much PMC will cause hardness problems. For example, lower hardness may lead to easy breakage. At the same time, fragrance - emitting particles containing too much PMC will pose challenges to dissolution / solubility. Therefore, there is a need to provide fragrance - emitting particles containing a high content of PMC to provide a pleasant consumer experience and satisfaction while exhibiting the desired hardness and desired dissolution. Summary of the Invention

[0006] The Applicant has surprisingly found that by introducing a filler carrier which is a mixture of polyethylene glycol and certain types of alkaline earth metal inorganic salt carriers, the perfume-containing particles containing a high content of perfume (especially encapsulated perfume) can provide a long-lasting and pleasant fragrance experience. The alkaline earth metal inorganic salt carriers are selected from the group consisting of magnesium sulfate, magnesium chloride, and combinations thereof. Surprisingly and unexpectedly, a certain amount of inorganic salt carriers with a specific particle size not only provides good hardness for the perfume-containing particles, but also provides the required solubility.

[0007] In one aspect, the present invention relates to a composition comprising a plurality of perfume-containing particles, wherein each of the perfume-containing particles in the composition comprises a perfume ingredient; polyethylene glycol; and an alkaline earth metal inorganic salt selected from the group consisting of magnesium sulfate, magnesium chloride, and combinations thereof. Each of the perfume-containing particles has a mass of 1 mg to 1 g and a maximum size of 3 mm to 10 mm. Preferably, each of the particles has a density greater than 1 g / cm 3 、preferably greater than 1.05 g / cm 3 ³.

[0008] Preferably, the perfume ingredient in the composition of the present invention comprises an encapsulated perfume, which is preferably present in fragile perfume microcapsules, and more preferably, the fragile perfume microcapsules are present in an amount in the range of greater than 2% to 30%, preferably greater than 5% to 25%, more preferably greater than 5% to 20%, still more preferably greater than 8% to 16% by weight of each perfume-containing particle.

[0009] Preferably, the perfume ingredient in the composition of the present invention comprises one or more free perfumes, which are preferably present in an amount in the range of 0.1% to 20%, preferably 0.5% to 15%, more preferably 1% to 10% by weight of each perfume-containing particle.

[0010] Preferably, the polyethylene glycol in the composition of the present invention has a weight average molecular weight (Mw) of 2,000 to 30,000 Daltons, preferably 3,000 to 20,000 Daltons, more preferably 4,000 to 15,000 Daltons; and the polyethylene glycol is present in each perfume-containing particle in an amount in the range of 5% to 90%, preferably 40% to 85%, more preferably 50% to 80% by weight of each perfume-containing particle.

[0011] Preferably, each fragrance-containing particle in the fragrance-containing particles of the present invention contains 1% to 40%, preferably 2% to 35%, and more preferably 4% to 32% of alkaline earth metal inorganic salts by weight of each fragrance-containing particle. Preferably, 80% to 100% by weight of the alkaline earth metal inorganic salts are particles characterized by a particle size of less than 600 microns, preferably a particle size of 50 microns to 600 microns, and more preferably a particle size of 50 microns to 420 microns.

[0012] Preferably, each fragrance-containing particle in the fragrance-containing particles further contains one or more other components selected from the group consisting of colorants, solvents, and combinations thereof, and wherein the one or more other components are present in an amount ranging from 0.01% to 10%, preferably 0.02% to 8%, and more preferably 0.1% to 5% by weight of each fragrance-containing particle.

[0013] Preferably, each particle in the particles has a hemispherical shape, a compressed hemispherical shape, or a semi-ellipsoidal shape. Preferably, each particle in the particles has a mass of 5 mg to 1 g, preferably 10 mg to 500 mg, and / or has a maximum dimension of 4 mm to 9 mm.

[0014] Another aspect of the present invention relates to a method for preparing fragrance-containing particles, the method comprising the following steps:

[0015] a) forming a viscous slurry by mixing a fragrance component, molten polyethylene glycol, inorganic salt filler particles, and optionally one or more other components, wherein the inorganic salt filler particles can pass through a sieve characterized by a mesh size of 600 μm; and

[0016] b) forming fragrance-containing particles from the viscous slurry, wherein each fragrance-containing particle formed in this way has a mass of 1 mg to 1 g and a maximum dimension of 3 mm to 10 mm;

[0017] wherein the inorganic salt filler particles contain a filler material selected from the group consisting of:

[0018] magnesium sulfate, magnesium chloride, and combinations thereof.

[0019] Preferably, the inorganic salt filler particles can pass through a sieve characterized by a mesh size of 400 μm, and more preferably can pass through a sieve characterized by a mesh size of 150 μm.

[0020] Each of the flavor particles in the flavor-containing particles may comprise one or more flavor components selected from the group consisting of free flavors, encapsulated flavors, and combinations thereof. In a specific embodiment, the flavor-containing particles comprise one or more free flavors, which are preferably present in an amount ranging from about 0.1% to about 25%, or about 0.2% to about 20%, preferably about 0.5% to about 15%, more preferably about 1% to about 10% by weight of the total weight of each flavor-containing particle. In addition, the flavor-containing particles comprise either separate encapsulated flavors or encapsulated flavors in combination with free flavors. Preferably, the encapsulated flavors are present in fragile flavor microcapsules, and the fragile flavor microcapsules are preferably present in an amount ranging from greater than 2% to 30%, preferably greater than 5% to 25%, more preferably greater than 5% to 20% by weight of each flavor-containing particle. In an exemplary embodiment, the flavor-containing particles comprise 8% to 16% of fragile flavor microcapsules by weight of each flavor-containing particle.

[0021] Optionally, the flavor-containing particles of the present invention may further comprise one or more other components selected from the group consisting of colorants, solvents, and combinations thereof. In some examples, the one or more components are present in an amount ranging from 0.01% to 10%, preferably 0.02% to 8%, more preferably 0.1% to 5% by weight of the total weight of each flavor-containing particle.

[0022] These and other aspects of the present invention will become more apparent when reading the following detailed description of the present invention. Detailed Description

[0023] The features and advantages of various embodiments of the present invention will become apparent from the following description, which includes examples of specific embodiments intended to give a broad representation of the present invention. From this description and from the practice of the present invention, various modifications will be apparent to those skilled in the art. The scope of the present invention is not intended to be limited to the specific forms disclosed, and the present invention encompasses all modifications, equivalents, and alternative alternatives that fall within the spirit and scope of the present invention as defined by the claims.

[0024] The dimensions and values disclosed herein should not be construed as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to represent the recited value and a range functionally equivalent around that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".

[0025] As used herein, when used in the claims, terms such as "a" and "an" are understood to mean one or more of the substances claimed or described. The terms "comprising", "containing", "including" all mean non-limiting.

[0026] The term "perfume-containing particle" or "fragrance-releasing particle" refers to a particle containing one or more perfume ingredients, such as free perfume, pre-perfume, encapsulated perfume (including perfume microcapsules), etc. Preferably, such perfume-containing particles contain perfume encapsulated in perfume microcapsules, especially fragile perfume microcapsules.

[0027] The term "aspect ratio" refers to the ratio of the longest dimension to the shortest dimension of the perfume-containing particle. For example, when such perfume-containing particles have a hemispherical shape, a compressed hemispherical shape, or a semi-ellipsoidal shape, the aspect ratio is the ratio between the bottom (longest) diameter and the height of the perfume-containing particle.

[0028] The term "consisting essentially of" means that the composition contains less than about 1%, preferably less than about 0.5%, of ingredients other than those listed.

[0029] In addition, the term "substantially free of" means that the indicated material is present in an amount from 0 wt% to about 1 wt%, preferably from 0 wt% to about 0.5 wt%, more preferably from 0 wt% to about 0.2 wt%. The term "essentially free of" means that the indicated material is present in an amount from 0 wt% to about 0.1 wt%, preferably from 0 wt% to about 0.01 wt%, and more preferably it is not present at an analytically detectable level.

[0030] As used herein, unless otherwise specified, all concentrations and ratios are by weight. Unless otherwise specified, all temperatures herein are in degrees Celsius (°C). Unless otherwise specifically stated, all conditions herein are at 20 °C and atmospheric pressure. Unless otherwise specifically specified, all polymer molecular weights are determined as weight-average molecular weights.

[0031] Fragrance-containing particles

[0032] The present invention relates to perfume-containing particles and methods for their preparation. The perfume-containing particles of the present invention can each have a specific shape, size, mass, and / or density. The perfume-containing particles of the present invention can have a longest dimension of from about 3 mm to about 10 mm, preferably from about 4 mm to about 9 mm, more preferably from about 5 mm to about 8 mm. Preferably, each perfume-containing particle among such perfume-containing particles can have an aspect ratio of no more than about 5, such as from about 1 to about 5, preferably from about 1.5 to about 4, more preferably from about 2 to about 4.

[0033] The flavor-containing particles of the present invention can have any shape selected from the group consisting of: spherical, hemispherical, compressed hemispherical, semi-ellipsoidal, cylindrical, disc-shaped, circular, lentil-shaped, oval, cubic, rectangular, star-shaped, flower-shaped, and any combination thereof. Lentil-shaped refers to the shape of a lentil. Compressed hemispherical refers to a shape corresponding to a hemisphere that is at least partially flattened such that the average curvature of the curved surface is less than the curvature of a hemisphere with the same radius. The compressed hemispherical particles can have an aspect ratio (i.e., the ratio of its bottom diameter to its height orthogonal to the bottom) of from about 2.0 to about 5, or from about 2.1 to about 4.5, or from about 2.2 to about 4. Oval particles refer to particles having a largest dimension and a second dimension orthogonal to the largest dimension, wherein the ratio of the largest dimension to the second dimension is greater than about 1.2, preferably greater than about 1.5, more preferably greater than about 2. Semi-ellipsoidal particles refer to a shape corresponding to half of an ellipsoidal or oval shape, wherein the flat bottom has a major axis and a minor axis, and the semi-ellipsoidal particles can have an aspect ratio (i.e., the ratio of its major axis to its height orthogonal to the flat bottom) of from about 2 to about 5, or from about 2.1 to about 4.5, or from about 2.2 to about 4.

[0034] Preferably, the flavor-containing particles of the present invention have a hemispherical shape, a compressed hemispherical shape, or a semi-ellipsoidal shape.

[0035] Individual flavor-containing particles can have a volume of from about 0.003 cm 3 to about 0.15 cm 3 and preferably from about 0.005 cm 3 to about 0.12 cm 3 In addition, individual flavor-containing particles of the present invention can each have a mass of from about 0.1 mg to about 5 g, preferably from about 1 mg to about 1 g, more preferably from about 5 mg to about 500 mg, still more preferably from about 10 mg to about 250 mg, still more preferably from about 15 mg to about 125 mg, alternatively their combinations, and any mg integer or mg integer range within any of the foregoing ranges.

[0036] In a preferred embodiment, the flavor-containing particles of the present invention have a density higher than that of water, i.e., greater than 1.0 g / cm 3 . For example, such flavor-containing particles can have a density in the range of from about 1.0 g / cm 3 to about 1.4 g / cm 3 and preferably from about 1.05 g / cm 3 to about 1.25 g / cm 3 .

[0037] In an alternative embodiment of the present invention, the flavor-containing particles of the present invention can have a density lower than that of water such that they can float on water, for example, a density of 0.7 g / cm 3to 0.95 g / cm 3 、or 0.8 g / cm 3 to 0.9 g / cm 3 。

[0038] The fragrance-containing particles of the present invention comprise: a fragrance component; polyethylene glycol; an inorganic carrier, characterized by a specific particle size distribution; and optionally one or more auxiliary components, as detailed below. Preferably, the inorganic salt carrier is a filler particle selected from the group consisting of magnesium sulfate, magnesium chloride, and combinations thereof.

[0039] Fragrance component

[0040] The fragrance-containing particles of the present invention may comprise one or more fragrance components selected from the group consisting of free fragrance, encapsulated fragrance, and combinations thereof.

[0041] In one specific embodiment, the fragrance-containing particles comprise one or more free fragrances, which are preferably present in an amount in the range of about 0.1% to about 25%, or about 0.2% to about 20%, preferably about 0.5% to about 15%, more preferably about 1% to about 10%, based on the total weight of each fragrance-containing particle.

[0042] In addition, the fragrance-containing particles comprise either a separate encapsulated fragrance or an encapsulated fragrance in combination with a free fragrance. Preferably, the fragrance-containing particles comprise a fragrance oil encapsulated in a fragrance microcapsule (PMC), which is preferably fragile (relative to, for example, moisture-activated PMC), but may also be moisture-activated. For the purposes of the present invention, the term "fragrance microcapsule" or "PMC" describes both fragrance microcapsules and fragrance nanocapsules. Preferably, the PMC is preferably present in an amount in the range of greater than 2% to 30%, preferably greater than 5% to 25%, more preferably greater than 5% to 20%, based on the weight of each fragrance-containing particle. For example, the fragrance-containing particles may comprise about 3%, or about 4%, or about 5%, or about 6%, or about 8%, or about 9%, or about 10%, or about 11%, or about 12%, or about 13%, or about 14%, or about 15%, or about 16%, or about 17%, or about 18%, or about 19%, or about 20%, and any integer or integer range within any of the foregoing ranges.

[0043] In another embodiment, each fragrance-containing particle in the fragrance-containing particles comprises both a free fragrance and an encapsulated fragrance (preferably in the form of a fragrance microcapsule and more preferably in the form of a fragile fragrance microcapsule) in a weight ratio in the range of about 1:20 to about 5:1, or about 1:10 to about 2:1, or about 1:8 to about 1:1.

[0044] In one embodiment, the PMC comprises a melamine / formaldehyde shell, which is commercially available from Appleton, Quest International, International Flavor & Fragrances or other suitable sources. In a preferred embodiment, the shell of the PMC is coated with a polymer to enhance the ability of the PMC to adhere to the fabric.

[0045] In another embodiment, the fragrance-containing particles may comprise a formaldehyde scavenger. In another embodiment, the fragrance of the fragrance-containing particles is coordinated with the fragrances of other fabric care products (such as laundry detergents). Thus, consumers who like the APRIL FRESH fragrance can use a composition packaged with multiple fragrance-containing particles having the APRIL FRESH fragrance, thereby coordinating the fragrance experience of washing their laundry with the fragrance experience when using APRIL FRESH. The fragrance-containing particles of the present invention can be sold as a product line with coordinated fragrances (along with laundry detergents).

[0046] Polyethylene glycol (PEG)

[0047] The fragrance-containing particles of the present invention comprise polyethylene glycol (PEG) as a first carrier. PEG has a low cost, can be formed into many different shapes and sizes, minimizes the diffusion of free fragrance, and is highly soluble in water. As used herein, the term "polyethylene glycol" or "PEG" includes homopolymers comprising repeating units of ethylene oxide, random copolymers comprising repeating units of ethylene oxide and propylene oxide, block copolymers comprising blocks of poly(ethylene oxide) and poly(propylene oxide), and combinations thereof.

[0048] Preferably, each of the fragrance-containing particles in the fragrance-containing particles comprises from about 5 wt% to about 90 wt%, preferably from about 40 wt% to about 85 wt%, more preferably from about 41 wt% to about 80 wt% of PEG, and more preferably such PEG is characterized by a weight average molecular weight (Mw) in the range of from about 2,000 daltons to about 30,000 daltons, preferably from about 3,000 daltons to about 20,000 daltons, more preferably from about 4,000 daltons to about 15,000 daltons. Suitable PEGs include homopolymers that can be commercially obtained from BASF under the trade name E 8000.

[0049] Particularly preferred PEGs in the context of the present invention are ethylene oxide - propylene oxide - ethylene oxide (EOx1POyEOx2) triblock copolymers which preferably have an average ethylene oxide chain length of from about 2 to about 90, preferably from about 3 to about 50, more preferably from about 4 to about 20 ethylene oxide units, and an average propylene oxide chain length of from 20 to 70, preferably from 30 to 60, more preferably from 45 to 55 propylene oxide units. More preferably, the ethylene oxide - propylene oxide - ethylene oxide (EOx1POyEOx2) triblock copolymer has a molecular weight of from about 2000 daltons to about 30,000 daltons, preferably from about 3000 daltons to about 20,000 daltons, more preferably from about 4000 daltons to about 15,000 daltons.

[0050] Preferably, the copolymer comprises from 10% to 90%, preferably from 15% to 50%, most preferably from 15% to 25% by weight of the copolymer of a combination of ethylene oxide blocks. Most preferably, the total ethylene oxide content is equally divided over the two ethylene oxide blocks. By equally divided herein is meant that each ethylene oxide block on average contains from 40% to 60%, preferably from 45% to 55%, even more preferably from 48% to 52%, most preferably 50% of the total number of ethylene oxide units, the % of the two ethylene oxide blocks totalling 100%. Some ethylene oxide - propylene oxide - ethylene oxide (EOx1POyEOx2) triblock copolymers improve cleaning.

[0051] Suitable ethylene oxide - propylene oxide - ethylene oxide triblock copolymers are commercially available under the trade name Pluronic series from BASF Corporation, or under the Tergitol L series from Dow Chemical Company. Particularly suitable materials are PE 9200. Other suitable materials include F38, F68 and F108.

[0052] Alkaline earth metal inorganic salt filler

[0053] In addition to the above-mentioned perfume ingredients and PEGs, the perfume-containing particles of the present invention further comprise a water-soluble inorganic salt filler material in particulate form as a second carrier.

[0054] The filler material may be or comprise a water-soluble alkaline earth metal salt. Specifically, the filler material may be or comprise a water-soluble material selected from the group consisting of magnesium sulfate, magnesium chloride and combinations thereof.

[0055] Among all alkali metal salts and alkaline earth metal salts, the applicant surprisingly found that certain salts (such as magnesium sulfate, magnesium chloride) can provide stable fragrance-containing particles with a high content of PMC. In a preferred embodiment, the inorganic salt filling material is magnesium sulfate. In another preferred embodiment, the inorganic salt filling material is magnesium chloride.

[0056] Preferably, each fragrance-containing particle in the fragrance-containing particles contains about 1 wt% to about 40 wt%, preferably about 2 wt% to about 35 wt%, more preferably about 4 wt% to about 32 wt% of the inorganic salt based on the weight of each fragrance-containing particle.

[0057] Preferably, 80 wt% to 100 wt% of the inorganic salt filling material present in the fragrance-containing particles is characterized by a particle size of less than 600 microns, preferably 50 microns to 600 microns, more preferably 50 microns to 500 microns.

[0058] The alkaline earth metal inorganic salt filling material is present in the fragrance-containing particles in particulate form, i.e., as discrete particles with a specific particle size distribution. Without being bound by any theory, the alkaline earth metal inorganic salt is an anhydrous salt, which can form a hydrate and disperse in the melt when introduced into the melt, thus stabilizing the beads even in the case of high PMC (where water is introduced).

[0059] In some examples, about 80 wt% to 100 wt%, preferably about 85 wt% to 100 wt%, more preferably about 90 wt% to 100 wt%, still more preferably about 95 wt% to 100 wt%, still more preferably about 98 wt% to 100 wt%, and most preferably about 99 wt% to 100 wt% of such discrete particles have a particle size of about 400 microns to about 600 microns. Preferably, about 80 wt% to 100 wt% of such discrete particles have a particle size of about 400 microns to about 550 microns.

[0060] In some alternative and preferred examples, about 80 wt% to 100 wt%, preferably about 85 wt% to 100 wt%, more preferably about 90 wt% to 100 wt%, still more preferably about 95 wt% to 100 wt%, still more preferably about 98 wt% to 100 wt%, and most preferably about 99 wt% to 100 wt% of such discrete particles have a particle size not exceeding 150 microns. Preferably, about 80 wt% to about 100 wt% of such discrete particles have a particle size of about 5 microns to about 150 microns, preferably about 10 microns to about 125 microns, more preferably about 10 microns to about 105 microns, most preferably about 10 microns to about 90 microns.

[0061] In addition to magnesium sulfate and magnesium chloride, the filler material may further include additional water-dispersible materials selected from the group consisting of: other inorganic alkali metal salts, organic alkali metal salts, inorganic alkaline earth metal salts, organic alkaline earth metal salts, starch (including modified starch), cellulose (including modified cellulose), zeolite, silica, clay, and combinations thereof. For example, in one embodiment, the fragrance-containing particles of the present invention may include magnetic sulfate and sodium sulfate.

[0062] Optional component / auxiliary component

[0063] The fragrance-containing particles of the present invention may optionally contain one or more optional components / auxiliary components in an amount in the range of about 0.01% to 10%, preferably 0.02% to 8%, more preferably 0.1% to 5%, including colorants, solvents, antimicrobial materials, acaricidal materials, dye transfer inhibitors, and combinations thereof.

[0064] The colorant may impart a color to the fragrance-containing particles, and the color is selected from the group consisting of: blue, green, yellow, orange, pink, red, purple, gray, etc. The colorant may be selected from the group consisting of: dyes, pigments, and combinations thereof. Preferably, the colorant includes at least one dye selected from those commonly used in laundry detergents. Examples of suitable dyes include, but are not limited to, LIQUITINT BLUE BL, LIQUITINTPINK AM, AQUA AS CYAN 15, and VIOLET FL purchased from Milliken Chemical. If a dye is used, the fragrance-containing particles may contain such a dye in an amount less than about 0.1%, or about 0.001% to about 0.1%, or about 0.01% to about 0.02%, or a combination thereof, based on the weight of the particles.

[0065] The fragrance-containing particles of the present invention may be substantially free of laundry detergent active substances. To reduce costs and avoid formulation capacity problems, one aspect of the present invention may include fragrance-containing particles that are substantially free or completely free of laundry detergent active substances. In one embodiment, each fragrance-containing particle in the fragrance-containing particles contains less than about 3%, or less than about 2%, or less than about 1%, or less than about 0.1% of laundry detergent based on the weight of the fragrance-containing particle. Laundry detergent active substances may include: detergent surfactants, detergent builders, bleaches, enzymes, mixtures thereof, etc. Particularly preferably, the fragrance particles of the present invention are substantially free or substantially free of surfactants, because the presence of such surfactants can accelerate the dissolution of the fragrance particles in water, which is undesirable in the context of the present invention. It should be understood that non-detergent levels of surfactants may be used to assist in dissolving the fragrance contained in the composition. More preferably, the fragrance particles of the present invention are substantially free or substantially free of any detergent active substances.

[0066] Depending on the application, the flavored particles of the present invention may contain a solvent selected from the group consisting of glycerin, polypropylene glycol, isopropyl myristate, dipropylene glycol, 1,2 - propylene glycol, and PEG with a weight average molecular weight of less than 2,000, and mixtures thereof.

[0067] The flavored particles may also contain an antioxidant. The antioxidant may help promote the stability of the color and / or odor of the particles over time between production and use. The flavored particles may contain such an antioxidant in an amount between about 0.001% and about 2% by weight, preferably between 0.01% and about 1% by weight, more preferably between about 0.05% and about 0.5% by weight. The antioxidant may be butylated hydroxytoluene.

[0068] Method for preparing fragrance-containing particles

[0069] The flavored particles of the present invention can be formed by those methods known in the art for preparing lozenges. The flavored particles of the present invention can be prepared in a batch mode or a continuous mode. In the batch mode, molten PEG is loaded into a mixing vessel with temperature control. Then, flavor components (such as free flavor and / or PMC), water - soluble inorganic salt filler particles (such as magnesium chloride particles, magnesium sulfate particles, etc.), and optional components (such as dyes, pigments, solvents, etc.) are added and mixed with the molten PEG until homogeneous. In the continuous mode, molten PEG is mixed with the above - mentioned flavor components, filler particles, and optional components in a liquid continuous stirrer (in - line mixer) such as a static mixer or a high - shear mixer, and then the resulting homogeneous mixture is used for lozenge formation. The flavor components, filler particles, and optional components can be added to the molten PEG in any order or simultaneously in a step before lozenge formation.

[0070] The flavored particles can be obtained by a lozenge - forming method. A desired formulation containing the above - mentioned molten PEG, flavor components, filler particles, and optional components is provided as a viscous slurry. The viscous slurry can be provided at a processing temperature less than about 20 degrees Celsius higher than the starting solidification temperature of the PEG material, as determined by differential scanning calorimetry. In one embodiment, PMC can be added to the molten PEG and free flavor in the form of a slurry to form a viscous slurry. PMC can also be added to the molten PEG and free flavor in powder form to form a viscous slurry.

[0071] In a particularly preferred embodiment of the present invention, a gas or gas - generating component can be added to the viscous slurry to form an aerated viscous slurry.

[0072] Then, an inflated or non-inflated viscous slurry can be made into flavored particles (especially in the form of lozenges) by a ROTOFORMER purchased from Sandvik Materials Technology. Specifically, the viscous slurry can be distributed to the stator through a feed pipe. A cylinder is provided for rotating around the stator along the longitudinal axis L of this cylinder, where the cylinder has a periphery, and a plurality of perforations are arranged around the periphery. Then, the viscous slurry is made to pass through the perforations of the cylinder onto a moving conveyor device below the cylinder to form droplets of this viscous slurry. The droplets of such viscous slurry are cooled to below the glass transition temperature of the PEG material on the moving conveyor device, thereby forming a plurality of lozenges having a hemispherical shape or a compressed hemispherical shape (depending on the viscosity of the slurry). This method can be implemented using any device disclosed herein.

[0073] In order to control the particle size distribution of the water-soluble or water-dispersible filler particles added to the molten PEG to reduce the compositional variation of the flavored particles thus formed, the present invention can select filler particles that already have the desired particle size distribution as described above, or process the filler particles (e.g., by grinding and screening) to achieve the desired particle size distribution.

[0074] For example, larger alkaline earth metal inorganic salt filler particles can be ground and / or screened to provide filler particles with a smaller particle size. The following sieves can be easily used for this purpose:

[0075] · Sieve # Tyler Standard Screen No. 100 (having a mesh size of 150 microns)

[0076] · Sieve # Tyler Standard Screen No. 115 (having a mesh size of 125 microns)

[0077] · Sieve # Tyler Standard Screen No. 150 (having a mesh size of 106 microns)

[0078] · Sieve # Tyler Standard Screen No. 170 (having a mesh size of 90 microns)

[0079] · Sieve # Tyler Standard Screen No. 200 (having a mesh size of 75 microns)

[0080] In addition, smaller inorganic salt filler particles can be screened out to provide the desired particle size distribution. The following sieves can be easily used for this purpose:

[0081] · Sieve # Tyler Standard Screen No. 325 (having a mesh size of 45 microns)

[0082] · Sieve # Tyler Standard Screen No. 400 (having a mesh size of 38 microns)

[0083] · Sieve # Tyler Standard Screen No. 625 (having a mesh size of 20 microns)

[0084] ·Sieve#Tyler Standard Sieve Size 800 (with a mesh size of 15 microns)

[0085] ·Sieve#Tyler Standard Sieve Size 1250 (with a mesh size of 10 microns)

[0086] ·Sieve#Tyler Standard Sieve Size 2500 (with a mesh size of 5 microns)

[0087] For example, the raw material containing inorganic salt filler particles may or may not be ground first and screened through a sieve (i.e., Sieve#Tyler Standard Sieve Size 100 with a mesh size of 150 microns). Accordingly, all the filler particles passing through this first sieve will have a particle size not exceeding approximately 150 microns. Alternatively, the raw material of the filler particles can be screened through Sieve#Standard Tyler Sieve Size 115 (with a mesh size of 125 microns), so that all the filler particles passing through this sieve will have a particle size not exceeding approximately 125 microns. Alternatively, the raw material of the filler particles can be screened through Sieve#Standard Tyler Sieve Size 150 (with a mesh size of 106 microns), so that all the filler particles passing through this sieve will have a particle size not exceeding approximately 106 microns.

[0088] In addition, the raw material of the filler particles can also be screened through Sieve#Tyler Standard Sieve Size 2500 (with a mesh size of 5 microns). Since all the particles passing through this sieve will have a particle size not exceeding approximately 5 microns, the passing particles can be removed, and the non-passing particles can be retained to ensure that the filler particles used have a main particle size of at least 5 microns. Similarly, the raw material of the filler particles can be further screened through Sieve#Tyler Standard Sieve Size 1250 (with a mesh size of 10 microns), and the passing particles can be removed to ensure that the retained particles (i.e., the non-passing particles) have a main particle size of at least 10 microns.

[0089] Packaged composition

[0090] The unit dose or multiple such unit doses of the fragrance-containing particles made by the method of the present invention can be accommodated in a package to form a packaged composition. The package can be a bottle, a bag, or other containers. In one embodiment, the package is a bottle, preferably a PET bottle including a translucent part, to display the fragrance-containing particles to the observing consumer. In one embodiment, the package includes a single unit dose (e.g., a trial-size sachet), or multiple unit doses (e.g., from about 15 unit doses to about 30 unit doses).

[0091] Dispensing

[0092] Multiple fragrance-containing particles can together form a unit dose for dispensing into a laundry washing machine or a laundry tub for hand washing. A single unit dose tablet can contain from about 13 g to about 27 g, or from about 14 g to about 20 g, or from about 15 g to about 19 g, or from about 16 g to about 18 g, or combinations thereof.

[0093] The aforementioned package can include a dispensing device for dispensing the fragrance-containing particles from the package into a laundry washing machine (or a laundry tub in a hand washing application). The user can use the dispensing device to meter the recommended amount of the unit dose, or simply use the dispensing device to meter the fragrance-containing particles according to the user's own fragrance preference. Examples of the dispensing device can be a dispensing top cover, a dome, etc. that are functionally attached to the package. The dispensing device can be releasably separable from the package and capable of being reattached to the package, such as, for example, a cup that can be mounted on the package. The dispensing device can be tethered (e.g., by a hinge or wire) to the remainder of the package (or alternatively not tethered). The dispensing device can have one or more demarcation lines (e.g., fill lines) to indicate the amount of the recommended unit dose. The package can include a removable opening for guiding the user to open the package and usage instructions for dispensing (e.g., pouring) the fragrance-containing particles contained in the package into the dispensing device. Thereafter, the user can be guided to dispense the fragrance-containing particles in the dispensing device into a laundry washing machine or a laundry tub. The fragrance-containing particles of the present invention can be used to increase the freshness of laundered items. The package including the dispensing device can be made of plastic.

[0094] In one embodiment, the fragrance-containing particles of the present invention can be applied to a laundry washing machine, such as used during the "wash cycle" of a washing machine (but the "rinse cycle" can also be used). In another embodiment, during the washing and / or rinsing of laundry, the fragrance-containing particles of the present invention are applied in a laundry tub for hand washing. In a hand washing application of laundry, the fragrance-containing particles can also contain an "antifoaming agent", such as those purchased from Wacker.

[0095] Example

[0096] Example 1: Fragrance-containing beads of the present invention

[0097] Examples 1 to 7 of the present invention of the fragrance-containing bead samples were prepared by the following method.

[0098] First, the PEG8000 raw material was heated overnight in an oven at 75 °C to form a molten PEG slurry.

[0099] Secondly, measure appropriate amounts of molten PEG slurry, different contents of inorganic salt filler particles with different particle size distributions (magnesium sulfate and magnesium chloride respectively), fragrance microcapsules, and free fragrance, and mix them to form corresponding fragrance-containing compositions, the specific compositions of which are decomposed as shown in Table 1 below. Manually mix the mixture for about 10 minutes to form a viscous and homogeneous slurry (this can also be done with a motor-driven stirrer), while placing the beaker on a heater to maintain the mixture at a temperature of about 75 °C.

[0100] Then, at about 30 seconds after the mixing step is completed, pour the viscous slurry into a mold with a bead-shaped cavity. Allow the viscous slurry to cool to ambient temperature in the mold, thereby forming solidified bead-shaped fragrance-containing particles.

[0101] Table 1: Examples and comparative examples of the present invention of fragrance-containing particles

[0102]

[0103] ~PEG8000 commercially available from BASF

[0104] *Weight average particle size D[4,3] = 62 μm

[0105] #Weight average particle size D[4,3] = 498 μm

[0106] ##Weight average particle size D[4,3] = 60 μm

[0107] Grind and / or screen the filler materials (magnesium sulfate and magnesium chloride in the examples of Table 1) in the fragrance-containing particles through a sieve #Taylor standard sieve as described above to obtain filler materials with the desired mesh size. The weight average particle size can be measured.

[0108] Comparative Example A and Comparative Example B were prepared by a similar method, except that Comparative Example A contained a low content of PMC and no inorganic salt, while Comparative Example B contained a high content of PMC and no inorganic salt.

[0109] Example 2: Densities of examples and comparative examples of the present invention

[0110] The density was measured by repeating the test 3 times by the method shown below. The densities of the examples and comparative examples of the present invention are listed in Table 2 below.

[0111] 1. For each measurement, collect 5 beads from the sample.

[0112] 2. Handle the beads gently to avoid damaging the beads (causing dents, chips, etc.), which may lead to inaccurate results.

[0113] 3. Ensure sufficient ethanol (or hexane for beads with a density < 500 g / L) in the beaker such that the beads will be covered by at least 10 mm of liquid after immersion when placed in the upper cup of the universal basket.

[0114] 4. Suspend the universal basket from the bracket. Ensure that no air bubbles adhere to the immersed part of the bracket.

[0115] 5. Close the ventilation shield door and zero the tare balance reading precisely.

[0116] 6. Place 5 beads in the upper cup of the universal basket. Record the weight shown on the balance.

[0117] This is Weight A.

[0118] 7. Remove the 5 beads from the upper cup of the universal basket using forceps, handling the beads carefully and gently to avoid damaging them.

[0119] 8. Close the ventilation shield door and zero the tare balance reading precisely.

[0120] 9. Place the same 5 beads in the lower cup of the universal basket. Ensure that no air bubbles adhere to the immersed part of the bracket.

[0121] 10. Wait until the balance stabilizes and record the weight shown. This is Weight B.

[0122] 11. Determine the density of the sample.

[0123]

[0124] ρ B = bead density

[0125] ρ0 = density of the liquid

[0126] ρ L = density of air (0.0012 g / cm 3 )

[0127] Table 2: Densities of examples and comparative examples of the present invention

[0128]

[0129] Example 3: Hardness test of examples and comparative examples of the present invention

[0130] Use an Instron compressor (Model 3369 bench-top materials testing system, capacity 50 kN, from Instron) to test the hardness of the examples and comparative examples of the present invention using the following test method.

[0131] 1. After production, store the beads in a sealed container and place them at 22°C - 25°C,

[0132] in an environment of 30RH%-50RH% for at least 24 hours.

[0133] 2. Place a bead on the bottom measuring plate with the flat side of the bottom facing down. Balance the load.

[0134] 3. In the Instron compression mode, set the extension to the control mode and the compression speed to 8 mm / min. Start the program.

[0135] 4. After the top plate contacts the bead, when a decrease in the force value is detected on the result graph, regard the load drop point as a valid hardness data and stop the machine.

[0136] Table 3: Hardness of examples and comparative examples of the present invention

[0137]

[0138] Table 3 shows the hardness comparison between the examples of the present invention and Comparative Example 1. It can be seen from the data shown in Table 3 that when the PMC content increases (from 3% in Comparative Example A to 14.4% in Comparative Example B), the hardness decreases significantly (-57%). However, interestingly, compared with Comparative Example B, Examples 1 to 5 of the present invention containing the same high content of PMC and adding inorganic salts of magnesium sulfate or magnesium chloride show a significantly increased hardness. In addition, Example 1 of the present invention containing magnesium sulfate with a particle size less than 150 microns shows a higher hardness than Example 3 of the present invention in which the particle size of magnesium sulfate is between 425 microns and 600 microns.

[0139] Example 4: Dissolution / solubility of examples and comparative examples of the present invention

[0140] The dissolution of the examples and comparative examples of the present invention was tested as follows.

[0141] 1. Select 5 conventional fragrance bead samples and record the weight x;

[0142] 2. Take 500 ml of water in a beaker, place the rotor in the beaker, adjust the stirrer so that the water in the beaker forms a vortex and ensure that the height of the vortex is half of the height of the water;

[0143] 3. Take a photo at regular intervals and adjust the height of the camera, then pour the bead sample into the beaker and record the dissolution time of the beads with the camera. Set the dissolution time to y.

[0144] 4. To better compare different formulations, standardize the measured bead weight to 0.19 g,

[0145] which means dissolution time = y * 0.19 / x.

[0146] Table 4: Dissolution of examples and comparative examples of the present invention

[0147]

[0148] Ratio = (dissolution time of Comparative Example A - dissolution time of the present invention) / dissolution time of Comparative Example A

[0149] As can be seen from Table 4, the embodiments of the present invention containing the required inorganic salts with the required particle size have a shorter dissolution time than Comparative Example A and Comparative Example B containing PEG and fragrance and no inorganic salts.

[0150] Unless expressly excluded or otherwise limited, each document cited herein, including any cross-referenced or related patent or patent application and any patent application or patent to which this application claims priority or the benefit of its advantageous effects, is hereby incorporated by reference in its entirety. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein, or an admission that it alone, or in any combination with any one or more other references, makes, suggests, or discloses any such invention. Further, when any meaning or definition of a term in this invention conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to the term in this invention shall govern.

[0151] Although specific embodiments of the invention have been illustrated and described, it will be apparent to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. Accordingly, it is intended that all such changes and modifications that fall within the scope of the invention be covered by the appended claims.

Claims

1. A composition comprising a plurality of perfumed particles, wherein each of the perfumed particles comprises: Fragrance ingredients; Polyethylene glycol; and an alkaline earth metal inorganic salt selected from the group consisting of magnesium sulfate, magnesium chloride, and combinations thereof, Each of the fragrance-containing particles has a mass of 1 mg to 1 g and a maximum dimension of 3 mm to 10 mm.

2. The composition according to claim 1, wherein each of the particles has a particle size greater than 1 g / cm 3 , preferably greater than 1.05 g / cm 3 density.

3. A composition according to claim 1 or 2, wherein the fragrance ingredient comprises encapsulated fragrance, preferably present in breakable fragrance microcapsules, and wherein more preferably the breakable fragrance microcapsules are present in an amount ranging from greater than 2% to 30%, preferably greater than 5% to 25%, more preferably greater than 5% to 20%, still more preferably greater than 8% to 16% by weight per fragrance-containing particle.

4. A composition according to any one of the preceding claims, wherein the perfume ingredient comprises one or more free perfumes, preferably present in an amount ranging from 0.1% to 20%, preferably from 0.5% to 15%, more preferably from 1% to 10% by weight per perfume-containing particle.

5. A composition according to any one of the preceding claims, wherein the polyethylene glycol has a weight average molecular weight (Mw) of 2,000 to 30,000 daltons, preferably 3,000 to 20,000 daltons, more preferably 4,000 to 15,000 daltons; wherein The polyethylene glycol is present in each perfume-containing particle in an amount ranging from 5% to 90%, preferably from 40% to 85%, more preferably from 50% to 80% by weight of each perfume-containing particle.

6. A composition according to any one of the preceding claims, wherein each of the perfume-containing particles comprises from 1% to 40%, preferably from 2% to 35%, and more preferably from 4% to 32% of the alkaline earth metal inorganic salt by weight of each perfume-containing particle.

7. A composition according to any one of the preceding claims, wherein 80% to 100% by weight of the alkaline earth metal inorganic salt is particles characterized by a particle size of less than 600 microns, preferably a particle size of 50 to 600 microns, more preferably a particle size of 50 to 420 microns.

8. A composition according to any one of the preceding claims, wherein each of the fragrance-containing particles further comprises one or more other ingredients selected from the group consisting of: a colorant, a solvent, and combinations thereof, and wherein the one or more other ingredients are present in an amount ranging from 0.01% to 10%, preferably from 0.02% to 8%, more preferably from 0.1% to 5% by weight of each fragrance-containing particle.

9. The composition according to any one of the preceding claims, wherein each of the particles has a hemispherical shape, a compressed hemispherical shape, or a hemispherical shape.

10. A composition according to any preceding claim, wherein each of the particles has a mass of 5 mg to 1 g, preferably 10 mg to 500 mg, and / or has a maximum dimension of 4 mm to 9 mm.

11. A method for preparing a flavored particle, the method comprising the steps of: a) forming a viscous slurry by mixing a flavor ingredient, molten polyethylene glycol, inorganic salt filler particles, and optionally one or more other ingredients, wherein the inorganic salt filler particles are capable of passing through a screen characterized by a mesh size of 600 μm; and b) forming flavor-containing particles from said viscous slurry, wherein each flavor-containing particle of said flavor-containing particles so formed has a mass of from 1 mg to 1 g and a maximum dimension of from 3 mm to 10 mm; The inorganic salt filler particles include a filler material selected from the group consisting of magnesium sulfate, magnesium chloride, and combinations thereof.

12. The method according to claim 11, wherein the inorganic salt filler particles are capable of passing through a sieve characterized by a mesh size of 400 μm, more preferably capable of passing through a sieve characterized by a mesh size of 150 μm.

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