Fragrance-containing granules
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-03-07
- Publication Date
- 2026-03-06
AI Technical Summary
Existing fragrance particles for aroma boosters have low fragrance filling, high carbon footprints, and poor water solubility, leading to inefficient fragrance release and environmental concerns.
Development of fragrance-containing granules with high fragrance filling (>40% by weight), made from biobased materials with a higher melting point, and characterized by a larger size (1-5 mm) and fast dissolution rate (<5 minutes) in water.
The granules provide improved fragrance release and retention, reduced carbon footprint, and enhanced handling and safety compared to conventional particles, while maintaining physical stability for transport at high temperatures.
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Abstract
Description
[Technical field]
[0001] The present disclosure relates to highly loaded, flavor-containing granules with improved performance and / or flavor benefits, especially compared to granules made from existing technologies (e.g., melt pastillation, spray dried granules) and / or materials (e.g., PEG). The present disclosure also relates to methods of making such granules, consumer products containing such granules, and methods of use thereof. [Background technology]
[0002] Perfumes play an important role in influencing consumer enjoyment of a product (e.g., fresh scent) and / or aiding in the perception of product performance (e.g., cleaning power). As a result, perfumes often serve as key elements that help promote the sale of a given consumer product. Furthermore, consumers are becoming more demanding in perfume performance in products. For example, some consumers are seeking products that can deliver strong perfume properties on substrates (e.g., fabrics, hard surfaces, skin), especially from properties that result from highly volatile perfume materials (i.e., top notes). Other consumers are seeking more sustainable and / or biodegradable products with minimal environmental impact, with no or minimal trade-offs in perfume performance and / or sensory benefits.
[0003] Most dry / anhydrous applications, including scent boosters, contain solid particles that can act as carriers for perfume materials and are commonly manufactured using hot melt pastillation processes as the preferred delivery system. As the name suggests, scent boosters are used to provide intense fragrance to laundry. They are intended to be added during the wash cycle in addition to laundry detergents and / or fabric conditioners / enhancers and deposited on washed clothing to release the perfume material at a later touch point. In current hot melt process technology, perfume ingredients are typically incorporated at relatively low levels (i.e., 10% or less), with the other 90% or more being carriers that typically contain materials derived from petrochemicals (e.g., polyethylene glycol). As one can imagine, there are several drawbacks to this approach. First, the perfume loading is low, which increases the cost of manufacturing, packaging and / or transporting these scent particles. Second, there is a large carbon footprint associated with these scent particles, as they carry a disproportionately small amount of perfume material to provide the intended perfume benefit to the consumer. Third, they are not particularly water soluble / dispersible and often take longer than the original wash cycle length to properly dissolve / disperse, which can leave residues on clothing, especially in low temperature wash cycles which are becoming more common as detergents allow for low temperature washes and energy costs and environmental awareness increase.
[0004] Spray-dried powders can have high perfume loading. However, they are fine powders that make them difficult to pour or handle, dusty, a respiratory hazard, and once airborne, they can be an explosion hazard with low ignition energy requirements. This makes them unsuitable as consumer products for fragrance booster applications, and is the reason why this very well-known technology has not been commercialized for said purposes. Summary of the Invention [Means for solving the problem]
[0005] The granules of the present disclosure are based, inter alia, on the discovery of new perfume-containing granules having a particular combination of parameters that enable them to deliver specific benefits including, by way of non-limiting example, high perfume loading, substantivity associated with a low carbon footprint, and / or improved perfume characteristics, particularly the characteristic intensity derived from highly volatile perfume materials (i.e., top notes).
[0006] In a first aspect, the present disclosure relates to a flavor-containing granule comprising: (a) a flavor material comprising a neat flavor and an encapsulated flavor; and (b) a carbohydrate carrier, wherein the amount of flavor material is greater than 40%, 45%, 50%, 55%, or 60% by weight based on the weight of the granule, the weight ratio of the neat flavor to the encapsulated flavor is from 10:1 to 1:1, and the granule has a skeletal density of greater than 1.00 g / mL or 1.05 g / mL.
[0007] In another aspect, the present disclosure provides a process for treating laundry comprising the step of dispensing 1 g to 30 g, preferably 3 g to 20 g, of the granules of the present disclosure into the laundry in a washing machine or basin.
[0008] In yet another aspect, the present disclosure provides a consumer product comprising the granules of the present disclosure, preferably the consumer product is a fragrance booster, fabric refresher, detergent (powder), fabric softener, rinse aid, water softener, bleach booster, disinfectant, unit dose laundry detergent, powder, detergent granule, detergent tablet, laundry bag or cleaning composition.
[0009] An advantage of the present disclosure is to provide new perfume-containing granules that can provide one or more performance and / or sensory benefits. In particular, the granules of the present disclosure have the advantage of having a larger size (1-5 mm) than conventional spray-dried particles (approximately 50 micrometers). The larger size granules according to the present disclosure have multiple advantages. First, the larger size allows for a more controlled release of perfume material (neat and / or encapsulated) during the wash cycle, resulting in a more uniform distribution of perfume on the washed clothes. Second, the larger size granules are easier to handle, generate less dust during handling, and / or reduce the risk of explosion. Third, the larger size also provides less surface area for the perfume material to spread over during storage, resulting in improved perfume quality retention over time.
[0010] Yet another advantage of the present disclosure is that it provides granules with high perfume payload. A sampling of currently commercially available PEG (polyethylene glycol)-based scent booster particles (e.g., P&G Unstopables®) shows an upper perfume loading limit of about 12% by weight of the particle. This low maximum loading is due to the low melting point (i.e., about 59°C) of the PEG-based particles and the resulting consumer product. If more perfume material or other additives are added, the melting point of the PEG-based scent particles becomes too low (i.e., below 59°C) for the consumer product to be reasonably shipped, especially during the summer months when shipping temperatures can easily exceed 60°C or 70°C.
[0011] In contrast, the perfume-containing granules of the present disclosure are formed from bio-based materials that have a higher melting point, preferably greater than 60° C., 70° C., 80° C., 90° C. or 100° C. This means that the perfume-containing granules of the present disclosure can have additional perfume substances and / or other active substances without compromising the melting point of the granule. Thus, the granules of the present disclosure can have a high perfume loading while remaining physically stable to transportation at temperatures above 60° C., 80° C. or 100° C.
[0012] All parts, percentages and proportions referred to in this specification and claims are by weight unless otherwise indicated.
[0013] The values and dimensions disclosed herein should not be understood to be strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such value is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a value disclosed as "50%" is intended to mean "about 50%."
[0014] To facilitate an understanding of the concepts presented herein, embodiments are illustrated in the accompanying drawings. [Brief description of the drawings]
[0015] [Figure 1] FIG. 1 illustrates a process scheme for the manufacture of one embodiment of a flavored granule of the present disclosure. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] The foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as defined in the appended claims. Other features and advantages of any one or more of the embodiments will become apparent from the following detailed description and claims.
[0017] As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, are intended to cover non-exclusive inclusions. For example, a process, method, article, or apparatus that includes a list of elements is not necessarily limited to only those elements, but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Furthermore, unless expressly stated otherwise, "or" means an inclusive or, not an exclusive or. For example, the condition "A or B" is satisfied by any one of the following: A is true (or exists) and B is false (or does not exist), A is false (or does not exist) and B is true (or exists), and A and B are both true (or exist).
[0018] Additionally, the use of "a" or "an" is employed to describe elements and components described herein. This is done merely for convenience and to give a general sense of the scope of the invention. This description should be interpreted to include one or at least one, and the singular also includes the plural unless it is clear that it has a different meaning.
[0019] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present invention, suitable methods and materials are described below. In addition, the materials, methods, and examples are illustrative only and are not intended to be limiting.
[0020] When an amount, concentration, or other value or parameter is given as either a range, a preferred range, or a list of upper and / or lower preferred values, this should be understood to specifically disclose any range formed from any pairing of any upper or preferred value of the range with any lower or preferred value of the range, regardless of whether the range is separately disclosed. When a range of numerical values is recited herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range. For example, if a range of "1-10" is recited, the recited range should be interpreted as including the ranges "1-8", "3-10", "2-7", "1.5-6", "3.4-7.8", "1-2 and 7-10", "2-4 and 6-9", "1-3.6 and 7.2-8.9", "1-5 and 10", "2 and 8-10", "1.5-4 and 8" and the like.
[0021] The present disclosure illustratively described herein can be suitably practiced in the absence of any element or elements, or limitation or limitations not specifically disclosed herein. Although compositions and methods are described herein in terms of "comprising" various components or steps, unless otherwise indicated, the compositions and methods can also "consist essentially of" or "consist of" the various components or steps.
[0022] Before addressing the details of the embodiments described below, some terms will be defined or clarified.
[0023] As used herein, the term "wt. %" means percentage by weight.
[0024] As used herein, the term "average granule weight" means a value calculated by taking the total weight (in mg) of 3000 granules and then dividing this by 3000 to get the approximate weight of each granule in mg.
[0025] As used herein, the term "average median diameter" refers to a value calculated using image analysis software (e.g., ImageJ Image Analysis Software, Ver. 1.53o (January 2022), available from NIH; MIPAR Image Analysis Software, Ver. 3.4, available from MIPAR Image Analysis, Columbus, Ohio; or Pax-It Image Management System, Ver. 1.3, available from Pax-It!™). A digital photograph of the granules is taken using a photographic size standard. The image analysis software then measures the diameter of the granules (e.g., several hundred). The average median diameter is then calculated along with the standard deviation.
[0026] The terms "obtainable" and "obtained" can be used interchangeably in the present disclosure and are not meant to indicate that a product must be obtained, for example, by a series of steps following the term "obtained", although such a limited understanding is always included in the term as a preferred embodiment of the present disclosure.
[0027] As used herein, the term "bio-based" refers to atoms or molecules obtained from biomass, e.g., from materials containing organic carbon of renewable origin. Such carbon sources can be derived from agricultural, plant, animal, fungal, microbial, marine, or forestry materials.
[0028] The term "biodegradable" as used herein with respect to materials such as microcapsule shells and / or fragrances means that the material is capable of and / or undergoes physical, chemical, thermal, microbial and / or biological degradation without any actual or perceived health and / or environmental problems. Ideally, the microcapsule shell and / or perfume is considered "biodegradable" if it passes one or more of the following tests: Respiratory biodegradation methods in aqueous media available from the Organization for Economic Cooperation and Development (OECD), the International Organization for Standardization (ISO), and the American Society for Testing and Materials (ASTM) tests, including but not limited to OECD301F or 310 (Ready biodegradation), OECD302 (Intrinsic biodegradation), ISO17556 (Solid irritation test), ISO14851 (Freshwater irritation test), ISO18830 (Marine sediment irritation test), OECD307 (Soil irritation test), OECD308 (Sediment irritation test), and OECD309 (Water irritation test). Preferably, the microcapsule shell and / or perfume is readily biodegradable as determined using the respiratory biodegradation methods in aqueous media, OECD301F or OECD310 tests. More preferably, the microcapsule shell and / or fragrance is biodegradable if the shell and / or fragrance has a biodegradation rate of at least 20%, 30%, 40%, 50%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 98% based on the weight of the shell and / or fragrance within 60 days according to the OECD 301F or OECD 310 test, or most preferably at least 60% biodegradability within 60 days according to the OECD 301F test.
[0029] As used herein, the term "bulk density" refers to the mass of a number of perfume-containing granules divided by the total volume they occupy. The total volume includes the granule volume, the intergranular void volume, and the intragranular void volume. Bulk density differs from skeletal density in that it includes both the intragranular void volume and the intergranular void volume. Bulk density is determined by measuring the volume of 100 g of granules in a 250 mL graduated cylinder after compression by standardized tapping. Tapped bulk density is calculated by dividing the mass (100 g) by the volume.
[0030] As used herein, the term "consumer" refers to both the user of the composition and observers near or around the user.
[0031] The terms "perfume ingredient", "perfume substance" and "perfume material" are used interchangeably and refer to a composition of perfume compounds for the purpose of delivering a specific and / or pleasing perfume profile to promote consumer enjoyment or acceptance of a consumer product and / or perfume composition. "Perfume substance" means a perfume raw material ("PRM") or a mixture of perfume raw materials ("PRMs") used to impart an overall pleasant odor or perfume profile to a composition. "Perfume substance" can encompass any suitable perfume raw material for perfumery use, including materials such as alcohols, aldehydes, ketones, esters, ethers, acetates, nitriles, terpene hydrocarbons, nitrogen or sulfite heterocyclic compounds and essential oils. However, natural vegetable and animal oils and exudates, which contain complex mixtures of various chemical components, are also known for use as "perfume substances". Individual perfume raw materials, including known natural oils, are described by reference to journals commonly used by those skilled in the art, such as "Perfume and Flavourist" or "Journal of Essential Oil Research", or in reference texts such as books by S. Arctander, Perfume and Flavor Chemicals, 1969, Montclair, New Jersey, USA, and more recently republished by Allured Publishing Corporation Illinois (1994). Additionally, some perfume raw materials are supplied by perfume companies (Firmenich, International Flavors & Fragrances, Givaudan, Symrise) as mixtures in the form of their own specialty accords.
[0032] As used herein, the term "perfume profile" refers to a description of how a perfume is perceived by the human nose at any given moment. A perfume profile can change over time. It is the result of a combination of the base, heart, and top notes of a perfume, if present. Base notes provide animalic, woody, sweet, amber or musky characteristics and are characterized as not being very volatile. Heart notes are associated with desirable characteristics such as floral characteristics (e.g., jasmine, rose), fruity, marine, aromatic or spicy characteristics. "Top or head notes" provide citrus, green, light, or fresh characteristics and tend to evaporate quickly due to their high volatility. A perfume profile is composed of two characteristics: "intensity" and "characteristics". "Intensity" relates to the perceived intensity and "characteristics" refers to the odor impression or quality of the perfume, i.e. fresh, clean, etc.
[0033] As used herein, the term "granule" refers to a particle that contains a core (typically a small core particle) and an active agent (typically a perfume). The term "granule" can also refer to fibers, flakes, spheres, powders, platelets, and other shapes and forms.
[0034] As used herein, the terms "Particle Size Dispersity Index (PSDI)" and "Polydispersity Index" are used interchangeably and refer to the distribution of size populations within a granule sample. In this disclosure, the Particle Size Dispersity Index (PSDI) is calculated as the standard deviation divided by the average granule diameter.
[0035] As used herein, the term "substantially free" with respect to a material means that the indicated material is present in an amount of 0% to about 1% by weight, preferably 0% to about 0.5% by weight, or more preferably 0% to 0.2% by weight. The term "essentially free" means that the indicated material is present in an amount of 0% to about 0.1% by weight, preferably 0% to about 0.01% by weight, or more preferably is not present at analytically detectable levels.
[0036] As used herein, the term "skeletal density" is the ratio of the mass of solid material contained within a granule to the sum of the volume of the solid material and the closed (or blind) pores within the granule. Skeletal density in this disclosure is determined by the method described in Skeletal Density Test.
[0037] As used herein with respect to a material (e.g., a granule), “water activity (a w The term "partial vapor pressure of water in a material at a given temperature divided by the partial vapor pressure of pure water at the same temperature."
[0038] As used herein, the terms "g," "mg," and "μg" refer to "grams," "milligrams," and "micrograms," respectively. The terms "L" and "mL" refer to "liters" and "milliliters," respectively.
[0039] It is understood that the test methods disclosed in the Test Methods section of this application must be used to determine the values of each of the parameters of Applicant's inventions described and claimed herein.
[0040] Flavor-containing granules WO 2016 / 205587 (Procter & Gamble) discloses perfume particles made from a hot melt pastillation system that uses an oil-derived PEG (polyethylene glycol) base to form hemispherical granules. These particles have a low perfume loading (20% or less by weight of the particle of encapsulated perfume). The particles also have a closed occlusion of gas (i.e., trapped air) added during the formation process, with a maximum of 0.95 g / cm. 3This results in particles with a density of less than 1000 nm, which allows the particles to suspend in the wash liquor and release perfume directly into the headspace above the wash liquor during use. WO 2018 / 172514 (Firmenich) discloses a solid fragrance booster composition comprising a solid carrier (e.g., sodium chloride, sodium acetate, urea, clay, PEG or mixtures thereof) and a granular powder comprising particles with low perfume loading (≦30% by weight of encapsulated perfume oil). WO 2006 / 056093 (Givaudan SA) teaches how to make water-soluble granules with high perfume loading of over 80% using hydroxypropyl methylcellulose (HPMC). However, it only uses microencapsulated perfume, since adding any significant level of neat perfume oil to HPMC creates a non-granular, heterogeneous mass that cannot be used as a consumer product. Granules made from HPMC and perfume microcapsules are used to load the microcapsules into powdered or granular consumer products, such as laundry detergent powders. The granules are not suitable for scent booster type applications because they cannot contain enough neat oil to impart a consumer acceptable level of perfume to the wet laundry coming out of the washer. Microcapsules are added to deposit the perfume on the fabric and delay release until the clothes are dried.
[0041] There are several drawbacks. First, the disclosed scented particles have low perfume loading and / or cannot carry much in the form of additional actives. This means that these products require a relatively large amount of packaging, storage space, and / or higher shipping costs. Second, the disclosed scented particles are made from materials that are not environmentally friendly for the carrier. This is problematic because consumers and / or regulators are demanding / needing sustainable products that can be more renewably sourced. Third, these approaches do not teach how to improve the perfume profile, more specifically how to selectively increase and / or extend the intensity of the more desirable characteristics (i.e., top notes) that result from high volatility perfume materials. Finally, the intended perfume release based on the scented granules disclosed in WO2016 / 205587 occurs during exposure to the wash liquor while washing the clothes, which is not the desired touch point for delivering the scent of the scent booster product while the consumer is wearing the washed clothes.
[0042] Therefore, existing solutions still have limitations and do not adequately teach how to overcome these problems.Therefore, there is still a need to develop new scented granules with high perfume loading.There is also a need for these scented granules to be sustainable, regeneratively sourced, and / or have significantly reduced transport, packaging, and / or carbon usage.It is also desirable that the scented granules are useful for improving perfume profile, especially the intensity of perfumes (i.e., top notes) that originate from highly volatile perfume materials.
[0043] The inventors have surprisingly discovered new perfume-containing granules that have a specific combination of parameters that allow them to deliver specific benefits, including, but not limited to, high perfume loading, substantivity associated with a low carbon footprint, and / or improved perfume profile, especially the characteristic intensity (i.e., top note) that comes from highly volatile perfume materials. As used herein, the term "highly volatile perfume material" refers to a perfume material that has a vapor pressure of more than 0.1 Torr (0.0133 kPa) at 25°C (i.e., top note). The vapor pressure is determined according to Test Method 1 (Determination of Vapor Pressure) of WO 2016 / 200761, the contents of which are incorporated herein by reference.
[0044] Specifically, in one embodiment, the present disclosure provides a flavor-containing granule comprising (a) a flavoring material including a neat flavoring and an encapsulated flavoring, and (b) a carbohydrate carrier, wherein the amount of the flavoring material is greater than 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 70 wt%, 80 wt%, or 90 wt%, based on the weight of the granule, and the weight ratio of the neat flavoring to the encapsulated flavoring is 10:1 to 1:1, and the granule has a skeletal density greater than 1.00 g / mL, 1.05 g / mL, 1.10 g / mL, or 1.15 g / mL, preferably greater than 1.00 g / mL. Preferably, the flavoring material is present in an amount greater than 40 wt%, 45 wt%, 50 wt%, 55 wt%, or 60 wt%, based on the weight of the granule.
[0045] Unlike other scented particles designed to float in liquid to provide enhanced perfume bloom benefits during the wash cycle (see WO 2016 / 205587), the perfume-containing granules of the present disclosure generally do not float in the wash liquor or do not float in the wash liquor for any significant time. Instead, the granules of the present disclosure tend to dissolve relatively quickly when added to the wash liquor to release the perfume material and, if present, other beneficial ingredients. Preferably, the granules of the present disclosure are characterized by a dissolution rate of about 5 minutes, 4 minutes, 3 minutes, 2 minutes, 1 minute, or 30 seconds or less, measured in deionized water at 25° C. using the dissolution rate test described in this disclosure. In some embodiments, the dissolution rate is about 30 seconds to 1 minute, about 1 minute to 5 minutes, about 30 seconds to 3 minutes, or about 30 seconds to 2 minutes. In some embodiments, the dissolution rate is about 1 minute or less.
[0046] By having a fast dissolution rate, the perfume-containing granules dissolve in the wash liquor and release the perfume material, if present, and other beneficial ingredients, if present. In some embodiments, most or substantially all of the perfume-containing granules dissolve in the wash liquor in 1 to 5 minutes, preferably less than about 1 minute, when added to the wash liquor. It is believed that successful incorporation of perfume-containing granules into granular laundry detergent products requires rapid dissolution in water at about 25°C, within about 5 minutes, preferably within about 1 minute. This fast dissolution rate has an additional advantage over PEG-based scent boosters in that it dissolves in the fabric conditioner dispenser of an automatic washing machine, allowing less product to be added for the same or higher level of perfume performance on dry clothes. This is because the fabric conditioner dispenser is dispensed in the final rinse of the wash cycle, which means that most of the perfume or perfumed microcapsules are not rinsed down the drain, which unfortunately happens to be more than half of the perfume added when the scent booster is added at the beginning of the wash cycle, when the machine program can include 3 or 4 rinse cycles (minimum 2 rinse cycles).
[0047] As used herein, the term "particulate laundry detergent" refers to a solid powder or granular laundry detergent composition, such as general-purpose or heavy-duty laundry detergent for fabrics.The particulate laundry detergent is preferably a flowable powder or granular detergent composition.In other words, perfume-containing granules should dissolve or disperse or disintegrate in water at the same or similar rate as the base particles of such granular laundry detergent product.Therefore, the perfume-containing granules of the present disclosure that have a fast dissolution rate are suitable for incorporation into such particulate laundry detergent products, otherwise they may have a negative impact on the overall consumer perception and acceptance of particulate laundry detergent products.
[0048] Moreover, consumers typically dislike the appearance of undissolved perfume-containing granules during the washing process and tend to view their presence as an indication of poor and / or unacceptable performance of such products.In fact, such undissolved perfume-containing granules may deposit residue on fabrics during washing, which consumers may consider as a product defect.As used herein, the term "residue" refers to the mass of material from the granules that is retained on fabrics or materials after use.In some embodiments, the perfume-containing granules of the present disclosure have a dispersion profile with less than 5% or less than 2% or less than 1% of residue associated with the granules.
[0049] Essentially, the solution is to print granules using primarily water-soluble or water-dispersible bio-based materials in combination with fragrance oils to create an oil-in-water emulsion that is deposited as "dots" or "droplets" on the belt. The droplets are then dried to remove all or substantially all of the water to form new fragrance-containing granules. According to some embodiments, the granules of the present disclosure are formed from droplets resulting from a deposition process that includes depositing a semi-viscous slurry on a belt. In certain embodiments, the slurry has a viscosity at room temperature of 1,000 m·Pas to 20,000 m·Pas, preferably 2,000 m·Pas to 10,000 m·Pas. Without wishing to be bound by theory, it is important to form the granules from a semi-viscous slurry because too much water results in a low viscosity slurry that cannot be deposited as discrete "dots" or "droplets" on the belt. However, too little water results in a high viscosity slurry that is difficult to pump and deposit on the belt. Applicants have found a sweet spot in terms of viscosity range so that slurries can be formulated with as little water as possible and still be functional for the printing process, with less water to evaporate, thus making these particles more efficient and / or more sustainable.
[0050] In some embodiments, the perfume-containing granules of the present disclosure contain a plurality of intragranular voids (i.e., voids within the granules) formed from heating the granules to evaporate water. Preferably, the granules contain less than 20%, 15%, 10%, 5% or 1% water by weight based on the weight of the granule. In some embodiments, the granules are essentially free of water. As used herein, the term "voids" refers to voids within the granules of porous or hollow morphology that are preferably not filled with other impurities and remain continuous after the granules are formed. As the name suggests, the voids are filled with air and not with other gases. The granules of the present disclosure have voids that may have asymmetric or irregular shapes with curved contours, or spherical or irregular spherical shapes (e.g., ellipsoidal, crescent, etc.). No observable differences in key performance criteria (e.g., dissolution rate, etc.) are expected between spherical voids versus non-spherical voids. Thus, in certain embodiments of the present disclosure, "air voids" can include a combination of spherical and non-spherical air voids.
[0051] The voids may have a variety of dimensions, for example, as measured longitudinally, in non-limiting examples, anywhere from about 1 micrometer to about 3000 micrometers. Without wishing to be bound by theory, it is believed that smaller air voids (e.g., less than about 1000, 500, 400, 300, 200, or 100 micrometers, or any units in between) can merge with other air voids to form larger air voids during the drying process. The resulting larger voids (e.g., 100 micrometers or more, 200 micrometers or more, 300 micrometers or more, 400 micrometers or more, 500 micrometers or more, 600 micrometers or more, 700 micrometers or more, 800 micrometers or more, 900 micrometers or more, or 1000 micrometers or more) are more desirable than small voids for facilitating dissolution rates. Alternatively, the voids of the present disclosure may include any combination of smaller and larger voids, so long as they result in granules having the desired dissolution rates described herein. In some embodiments, the perfume-containing granules of the present disclosure comprise a plurality of intragranular voids having a longitudinal dimension of at least 1 micrometer, at least 10 micrometers, at least 50 micrometers, at least 100 micrometers, at least 200 micrometers, at least 300 micrometers, at least 400 micrometers, or at least 500 micrometers. In some embodiments, the perfume-containing granules of the present disclosure comprise a plurality of intragranular voids having a longitudinal dimension of 3000 micrometers or less, 2500 micrometers or less, 2000 micrometers or less, or 1500 micrometers or less.
[0052] In some embodiments, the total volume of voids within the perfume-containing granule (i.e., intragranular voids) is at least 10%, at least 15%, at least 20%, at least 25%, or at least 30%, based on the volume of the granule. In some embodiments, the total volume of voids within the granule is 70% or less, 65% or less, 60% or less, 55% or less, or 50% or less, based on the volume of the granule. In some embodiments, the total volume of voids within the granule is in the range of 15%-70%, 20%-60%, or 35%-55%, based on the volume of the granule. Without wishing to be bound by theory, it is believed that the intragranular voids can increase the dissolution rate of the granule during its use in a wash cycle.
[0053] It is important to note that in any process used to create the air voids that entrap the air in the perfume-containing granules of the present disclosure, no air or other gases are intentionally added to the precursor material. Furthermore, as mentioned above, the voids found in the perfume-containing granules are formed from water evaporation during the heating process, and not as a result of any crushing during the cooling process of the precursor material from which the granules are made. The combination of these different factors results in the granules of the present disclosure having voids with significantly different properties to any currently known scented particles.
[0054] In some embodiments, the carbohydrate carrier is water-soluble or water-dispersible. In some embodiments, the carbohydrate carrier has a melting point temperature of at least 70°C, at least 80°C, at least 90°C, or at least 100°C. The flavor loading of current benchmark PEG-based granules is limited to a maximum of 12% by weight of the granule. The melting point temperature of PEG is about 60°C to 62°C. Due to its low melting point, adding more flavoring substances or other additives to the PEG-based granules would make the melting point temperature of the granules too low for transportation, as the temperature can often exceed 60°C. Thus, formulation flexibility is limited with PEG-based granules. In contrast, the flavor-containing granules of the present disclosure are made from carbohydrate carriers with higher melting point temperatures, so that more flavoring substances or other additives can be added while still maintaining compatibility for transportation (and storage) at high temperatures (e.g., >80°C, >90°C, or >100°C).
[0055] In some embodiments, the flavor-containing granules of the present disclosure have an average median diameter ranging from 1 mm to 20 mm, or 1 mm to 15 mm, or 1 mm to 10 mm, or 1 mm to 5 mm, or 2 mm to 3 mm. In some embodiments, the granules have an average median diameter of at least 0.5 mm, at least 1 mm, at least 1.5 mm, or at least 2 mm. In some embodiments, the granules have an average median diameter of 20 mm or less, 18 mm or less, 15 mm or less, 12 mm or less, 10 mm or less, 8 mm or less, 5 mm or less, or 3 mm or less. The average median diameter of the granules can be determined by measuring the diameter distribution of the granules using image analysis software described in this disclosure.
[0056] In some embodiments, the flavor-containing granules of the present disclosure have the following characteristics: (i) a water activity (a) of less than 0.6 at 25°C w ), and / or (ii) an average granule weight of from 1 mg to 10 mg, or from 3 mg to 7 mg, and / or (iii) Bulk density of 0.1 g / mL to 1 g / mL, or 0.2 g / mL to 0.6 g / mL It is characterized by:
[0057] In some embodiments, the flavor-containing granules have all three of the above characteristics. w ), average granule weight and bulk density may provide a significant improvement over existing scent particles. Without wishing to be bound by theory, a perfume-containing granule with these characteristics is a dry flowable, high perfume loading powder / granule that provides protection from air and evaporation, and long-lasting performance in a convenient and safe manner that avoids unintentional ignition of perfume vapors.
[0058] In some embodiments, the perfume-containing granules of the present disclosure have a particle size dispersity index (PSDI) of less than 0.2 (standard deviation / average). PSDI can be measured using a Malvern Nano-S, further details of the method are given in<https: / / www.ncbi.nlm.nih.gov / pmc / articles / PMC5035303 / > and the contents of which are incorporated herein by reference. It is yet another advantage that the granules of the present disclosure exhibit a polydispersity index of less than 0.2 (standard deviation / average). This means that the granules of the present disclosure have a more monodisperse particle size distribution than conventional spray-dried particles, which tend to have a polydisperse particle size distribution. Without wishing to be bound by theory, it is believed that the more monodisperse particle size distribution of the granules, as well as the ability to adjust the particle size, results in a more favorable uniform distribution of the granules when blended with other dry products. As a result, during use, the perfume-containing granules of the present disclosure exhibit a more uniform distribution on washed clothes.
[0059] In some embodiments, the perfume-containing granules of the present disclosure have a weight ratio of perfume material to carbohydrate carrier of about 9:1 to about 1:1.5, or about 9:1 to about 1:1. In other words, the granules of the present disclosure have a high perfume loading. In certain embodiments, consumer products (e.g., scent boosters) formulated with the granules of the present disclosure have a weight ratio of perfume material to carbohydrate carrier of 50 / 50, which is significantly higher than the current level of 10 / 90 perfume material to carrier of the current benchmark PEG-based scent booster. In fact, the granules of the present disclosure provide a scent booster product that can be dosed into a washing machine (or sink) at one-fifth the current dosage while providing the benefits of parity and / or improved perfume profile. Furthermore, this high perfume loading property of the granules significantly reduces packaging size (e.g., less plastic or cardboard), requires significantly less storage and warehouse space, and / or minimizes transportation costs and associated carbon footprint.
[0060] Another aspect of the present disclosure is the desire to transition to the use of granules and / or their ingredients (e.g., fragrance materials, microcapsules, etc.) derived from "Green Chemistry" principles. Green Chemistry focuses on the design of products and processes that minimize environmental impact, particularly by using renewable feedstocks, reused and / or upcycled carbon resources that can be replenished to replace parts that are depleted by use and / or consumption, either by natural regeneration or other recurring processes within a finite time (such as within a human lifespan). In other words, the raw materials or feedstocks used to manufacture the granules and / or their ingredients should be renewable, reused and / or upcycled carbon resources, rather than depleted whenever technically and economically feasible. As used herein, "BRC" refers to carbon and non-fossil carbon that is part of the Earth's natural environment. BRC is a naturally occurring renewable, reused and / or upcycled carbon resource that can be replenished to replace parts that are depleted by use and consumption, either by natural regeneration or other recurring processes within a finite time (such as within a human lifespan). BRC excludes carbon derived from virgin crude oil. In some embodiments, the perfume-containing granules of the present disclosure have a bio-renewable carbon (BRC) content of at least 25%, at least 30%, at least 35%, at least 40%, at least 45%, at least 50%, at least 55%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, or at least 95% based on the weight of the granule.
[0061] In some embodiments, the flavor-containing granules may be formed into spheres, hemispheres, and the like. The granules may have any shape selected from the group consisting of spheres, hemispheres, compressed hemispheres, disks, circles, lenticular shapes, rectangles, and combinations thereof, preferably hemispheres or compressed hemispheres. As used herein, "lenticular shape" refers to the shape of a lentil, and "compressed hemisphere" refers to a shape corresponding to an at least partially or substantially flattened hemisphere such that the surface of curvature is, on average, less than the curvature of a hemisphere having the same radius. Compressed hemispherical particles can have an aspect ratio (i.e., the ratio of the diameter of the base to the height of the base perpendicular to the base) of about 2.0 to about 5, alternatively about 2.1 to about 4.5, alternatively about 2.2 to about 4. "Rectangular shaped" granules refer to particles having a maximum dimension and a secondary dimension perpendicular to the maximum dimension, the ratio of the maximum dimension to the secondary dimension being greater than about 1.2, preferably greater than about 1.5, and more preferably greater than about 2. Additionally, the granules of the present disclosure may be broken and deformed during the drying step of the manufacturing process, resulting in granules having irregularly shaped hemispheres or compressed hemispheres.
[0062] In some embodiments, the perfume-containing granules of the present disclosure may have different shapes, sizes, and / or skeletal densities. In some embodiments, the perfume-containing granules are added as ingredients in other products. For example, the granules may be added to a powder laundry detergent. Given that the perfume-containing granules are different shapes and / or sizes from the detergent particles, they are more likely to separate from the detergent particles during transportation and storage. Such separation may result in significant dose-to-dose variation in the amount of perfume-containing granules in the particulate laundry detergent composition. It has been discovered that such hemispherical or compressed hemispherical shapes help to significantly reduce the separation of perfume-containing granules in a powder laundry detergent composition, for example, by at least 20%, 30%, 40%, 50%, 60%, 70%, or 80%, compared to perfume-containing granules having other shapes.
[0063] fragrance As used herein, the term "neat fragrance" refers to a fragrance ingredient that is free of exogenous substances and that is not encapsulated and / or bound to other compounds that cause a delay in the release of the fragrance ingredient. In some embodiments, the fragrance material comprises a neat fragrance, and the neat fragrance is present in an amount of >30 wt%, >40 wt%, >50 wt%, >60 wt%, >70 wt%, >80 wt%, or >90 wt%, based on the total weight of the granule. In some embodiments, the granules of the present disclosure comprise a neat fragrance in an amount of 30 wt% to 45 wt%, or 25 wt% to 42.5 wt%, based on the total weight of the granule.
[0064] As used herein, the term "encapsulated perfume" refers to perfume ingredients that are encapsulated in microcapsules (to stabilize the odor impression over an extended period of time). Microcapsules are used to deliver perfume to a target area in a time-delayed or controlled manner. In some embodiments, the microcapsules have an average particle size of 1 to 100 micrometers, preferably 1 to 50 micrometers, or more preferably 1 to 20 micrometers. Microcapsules can be prepared from natural materials such as fungal chitosan (WO 2016 / 185171), silk fibroin particles (US 2015 / 0164117), and biomolecules used as emulsifiers in microcapsule preparation (WO 2016 / 193435, WO 2017 / 102812, US 2018 / 0078468, WO 2018 / 019894, WO 2018 / 019896, and WO 2017 / 102812). Microcapsules comprising multi-layered coacervates between gelatin and gum arabic can be used in the present disclosure (U.S. Pat. No. 4,946,624, WO 2012 / 001604, U.S. Pat. Appl. Pub. No. 2015 / 0250689, and WO 2018 / 002214). Protein microcapsules are also useful within the scope of the present disclosure (U.S. Pat. Appl. Pub. No. 2017 / 0189283). In some embodiments, environmentally friendly microcapsules are also within the scope of the present disclosure, in which the shell is at least 60% biodegradable within 60 days according to OECD 301F (WO 2021 / 122633).
[0065] In some embodiments, the encapsulated perfume is encapsulated by a biodegradable microcapsule shell. Preferably, the biodegradable microcapsule shell has a biodegradation rate of at least 20%, at least 30%, at least 40%, at least 50%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 95%, or at least 98% within 60 days according to OECD301F or OECD310 based on the weight of the microcapsule shell, preferably 60% within 60 days according to OECD301F based on the weight of the microcapsule shell. As used herein, the terms "wall" and "shell" are used interchangeably to refer to the structure formed by the microencapsulating polymer that surrounds the active material (e.g., perfume) core that is microencapsulated.
[0066] Other suitable non-limiting examples of microcapsules within the scope of the present disclosure include: (i) microcapsules having a biodegradable microcapsule shell comprising at least one bio-based epoxide selected from diglycidyl ether diphenol ester, preferably the bio-based epoxide is selected from diglycidyl ether diphenol methyl ester; diglycidyl ether diphenol ethyl ester; diglycidyl ether diphenol butyl ester; diglycidyl ether diphenol pentyl ester; or diglycidyl ether diphenol methoxy PEG, PEG being any one of PEG1 to PEG10, preferably diglycidyl ether diphenol methoxy PEG1, and the bio-based epoxide is polymerized by interfacial polymerization with a polyamine selected from hexamethylenediamine (HMDA), ethylenediamine (EDA), diethylenetriamine (DETA), dipropylenetriamine (norspermidine), triethylenetetramine (TETA), tetraethylenepentamine (TEPA), chitosan oligosaccharide (COS), guanidine carbonate, polylysine or lysine-containing protein, gelatin, or a combination thereof; and / or (ii) microcapsules having a biodegradable microcapsule shell comprising an isocyanate-biodegradable polymer shell comprising the reaction product of a biodegradable isocyanate-terminated prepolymer with a crosslinker and optionally a polyelectrolyte emulsifier under aqueous conditions, wherein the biodegradable isocyanate-terminated prepolymer comprises gelatin, collagen, chitosan, modified guar, modified glucan, gum arabic, protein, hydrolyzed protein, fermented protein, hydrophobin, enzyme, partially neutralized citrate ester, alginate, carrageenan, pectin, modified starch, or modified cellulose, and the crosslinker comprises an oxidized sugar (EP 21198609.6); and / or (iii) microcapsules having a biodegradable microcapsule shell comprising chitosan crosslinked with a multifunctional isocyanate having at least two isocyanate functional groups and tannic acid, the tannic acid being hydrolyzed tannic acid, non-hydrolyzed tannic acid, or a combination thereof, the shell further comprising carrageenan, gum arabic, or a combination thereof, and the multifunctional isocyanate being a biuret, an isocyanurate, an allophanate, a uretdione, an oligomeric hexamethylene diisocyanate, or a combination thereof (EP 22150553.0); and / or (iv) microcapsules having a biodegradable microcapsule shell comprising the reaction product of a biodegradable isocyanate-terminated prepolymer with a crosslinker and optionally a polyelectrolyte emulsifier under aqueous conditions (EP 22151570.3); and / or (v) microcapsules having a biodegradable microcapsule shell comprising a trimethylolpropane adduct of xylylene diisocyanate, a dispersant comprising modified pea protein, and a hydrocolloid comprising gum arabic; and / or (vi) Microcapsules having a biodegradable microcapsule shell comprising a biopolymer crosslinked with one or more crosslinking agents, wherein the biopolymer is whey protein or modified whey protein.
[0067] In some embodiments, the materials used to form the walls of the biodegradable microcapsules of the present disclosure preferably do not form a blend of biodegradable and non-biodegradable materials. In some embodiments, the materials used to form the walls of the microcapsules form a blend of biodegradable and non-biodegradable materials, and the level of non-biodegradable material is less than 10%, less than 5%, less than 3%, less than 1%, or less than 0.5% by weight of the microcapsule. In some embodiments, the materials used to form the walls of the microcapsules form a blend of biodegradable and non-biodegradable materials, and the biodegradation rate of all components of the blend is at least 20%, 30%, 40%, 50%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, or 98% based on the total weight of the blend within 60 days according to OECD301F or OECD310.
[0068] In some embodiments, the perfume material comprises an encapsulated perfume, and the encapsulated perfume is present in an amount of >5%, >10%, >15%, >20%, >25%, or >30% based on the total weight of the granule. In some embodiments, when containing these levels of encapsulated perfume, the neat oil equivalent (NOE) in the solid form fabric conditioner (including the granules of the present disclosure) is 1-10%. In some embodiments, the granules of the present disclosure contain encapsulated perfume in an amount of 5%-20% or 7.5%-15% by weight based on the total weight of the granule.
[0069] In some embodiments, the perfume material comprises a neat perfume and an encapsulated perfume, and the total amount of the neat perfume and the encapsulated perfume is at least 40% by weight, at least 50% by weight, at least 60% by weight, at least 70% by weight, at least 80% by weight, or at least 90% by weight based on the total weight of the granule. In some embodiments, the weight ratio of the neat perfume to the encapsulated perfume is 10:1 to 1:1. In some embodiments, the weight ratio of the neat perfume to the encapsulated perfume is 8:1 to 2:1, or 7:1 to 2:1, or 6:1 to 3:1, or 5:1 to 3:1. In some embodiments, the weight ratio of the neat perfume to the encapsulated perfume is at least 0.5:1, or at least 0.8:1, or at least 1:1, or at least 2:1, or at least 3:1. In some embodiments, the weight ratio of neat perfume to encapsulated perfume is 15:1 or less, or 12:1 or less, or 11:1 or less, or 10:1 or less, or 9:1 or less, or 8:1 or less, or 7:1 or less, or 6:1 or less, or 5:1 or less.
[0070] In some embodiments, the neat perfume and / or encapsulated perfume comprises perfume materials having a logP value (partition coefficient) of less than 2. In some embodiments, the neat perfume and / or encapsulated perfume comprises at least 1, at least 2, at least 3, at least 4, at least 5, at least 6, at least 7, at least 8, at least 9, or at least 10 high performance perfume ingredients selected from the group consisting of ultra-high impact perfume materials as listed in Table 1 and high impact perfume materials as listed in Table 2.
[0071] [Table 1]
[0072] [Table 2]
[0073] [Table 3]
[0074] [Table 4]
[0075] [Table 5]
[0076] In some embodiments, the neat perfume and / or the encapsulated perfume may further comprise at least one additional perfume material. In some embodiments, the neat perfume and / or the encapsulated perfume may further comprise 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, 25, 30, 35, 40 or more additional perfume materials. Non-limiting examples of such additional perfume materials include those described in US Patent Application Publication No. 2018 / 0325786, US Pat. No. 4,534,891, US Pat. No. 5,112,688, and US Pat. No. 5,145,842, the contents of each of which are incorporated herein by reference. In some embodiments, the additional perfume material, when combined with one or more perfume materials in Tables 1 and 2, constitutes the total perfume material composition present in the granules of the present disclosure.
[0077] In some embodiments, the carbohydrate carrier is selected from the group consisting of starch, modified starch, polysaccharides (e.g., gum arabic), cellulose, pectin, and mixtures thereof. In some embodiments, the carbohydrate carrier comprises a starch selected from the group consisting of corn starch, potato starch, rice starch, tapioca starch, and mixtures thereof. In some embodiments, these starches can be chemically modified (i.e., modified starches). The starches of the present disclosure can be obtained from seeds, roots, or tubers. The starches can be obtained by wet milling, washing, sieving, and drying. The starches are obtained primarily from corn, wheat, and potato, and to a lesser extent from sources such as rice, sweet potato, sago, and mung bean. The starches can be unmodified or chemically modified (i.e., modified starches) to enable the starches to function under conditions frequently encountered during processing or storage, such as high heat, high shear, low pH, oxidation, freezing / thawing, and / or cooling. Such modifications include, but are not limited to, acid treatment, alkali treatment, bleaching, oxidation, enzyme treatment, acetylation, phosphorylation, or combinations thereof. In some embodiments, the carbohydrate carrier comprises or is a modified starch. In some embodiments, the modified starch is selected from the group consisting of cationic starch, hydroxyethyl starch, carboxymethylated starch, and combinations thereof. In some embodiments, the modified starch is an octenylsuccinic anhydride (OSA) modified starch. In some embodiments, the modified starch is starch sodium octenyl succinate (E1450). Other types of modifications known to those skilled in the art are also considered to be within the scope of this disclosure. Suitable examples of modified starches include, but are not limited to, CAPSUL®, CAPSUL® FP, HI-CAP® IMF, HI-CAP® 100 (starch sodium octenyl succinate), and the like (available from Ingredion, Westchester, IL, USA). In some embodiments, the aqueous (modified) starch solution may contain maltose, sucrose, maltodextrin, or combinations thereof.In some embodiments, the aqueous (modified) starch solution may include a cellulose ether.
[0078] In some embodiments, the carbohydrate carrier comprises modified and unmodified starch. As used herein, the term "unmodified starch" means that the starch is not chemically modified. In some embodiments, the carbohydrate carrier comprises gum arabic. In some embodiments, the carbohydrate carrier is present in the granule in an amount of 10% to 50% by weight, preferably 20% to 40% by weight, based on the total weight of the granule. In some embodiments, the flavoring material is adsorbed or absorbed onto the carbohydrate carrier.
[0079] In some embodiments, the flavor-containing granules of the present disclosure may further comprise additional ingredients such as a friability reducing agent selected from the group consisting of glycerin, corn syrup, gelatin, polyvinylpyrrolidone, polyvinyl alcohol, and combinations thereof. The friability reducing agent may reduce the friability of the granule. In some embodiments, the friability reducing agent comprises or is glycerin. In some embodiments, the amount of friability reducing agent present in the granule is 1% to 10%, 2% to 8%, or 3% to 7% by weight based on the weight of the granule. In some embodiments, the amount of friability reducing agent present in the granule is at least 0.5%, or at least 1%, or at least 2%, or at least 3%, or at least 4%, or at least 5% by weight based on the weight of the granule. In some embodiments, the amount of friability reducing agent present in the granule is 12% or less, or 11% or less, or 10% or less, or 9% or less, or 8% or less, or 7% or less by weight based on the weight of the granule.
[0080] In some embodiments, the perfume-containing granules of the present disclosure may further comprise one or more additional ingredients selected from the group consisting of surfactants, enzymes, antimicrobial agents, odor control agents, soil removal polymers, anti-redeposition polymers, probiotics, softeners, chelating agents, antistatic agents, and combinations thereof. In some embodiments, this may result in a single granule that combines several active ingredients to create a finished laundry or cleaning product without the need for subsequent dosing or blending of the product.
[0081] Process for preparing granules In some embodiments, the flavor-containing granules of the present disclosure can be prepared according to the following method. There are alternatives to this method, so there is no limitation on the method of obtaining the granules, provided that a high flavor loading can be obtained. Thus, according to one embodiment, the flavor-containing granules are obtained by a process as shown in Figure 1. With reference to Figure 1, the process includes the following steps: (i) preparing an aqueous phase having a high solids content (e.g., 68-70% by weight) and high viscosity (5,000-10,000 cP) by dissolving and / or dispersing a carbohydrate carrier in water; (ii) preparing an oil phase (neat and encapsulated) containing a perfume material and mixing the oil phase with the water phase of step (i) to obtain an oil-in-water emulsion (feed slurry in FIG. 1); (iii) mixing the emulsion of step (ii) with a high shear disperser (IKA T50 Ultra-Turrax) to subject it to high shear mixing (e.g., 13500 RPM) to reduce the oil droplet size to <5 micrometers; (iv) dispensing 3 mm diameter droplets or dots of the emulsion feed of step (iii) onto a conveyor belt (using the depositor of FIG. 1) at a belt speed of 10 meters per minute; (v) drying the dots by applying heat to the dots as they move along the conveyor belt to obtain the perfume-containing granules of the present disclosure; Other drying methods such as fluidized bed or even room temperature drying may be suitable.
[0082] consumer products In another aspect, the present disclosure relates to a consumer product comprising the perfume-containing granules of the present disclosure. In some embodiments, the consumer product is a particulate laundry detergent comprising a majority of detergent particles and a minor portion of perfume-containing granules (e.g., in an amount ranging from about 0.1% to about 30%, preferably from about 0.5% to about 20%, or more preferably from about 1% to about 15%, based on the total weight of such particulate laundry detergent). In some embodiments, the consumer product comprises the perfume-containing granules. In some embodiments, the consumer product is a scent booster, fabric refresher, laundry detergent (powder), fabric softener, rinse aid, water softener, bleach booster, disinfectant, unit dose laundry detergent, detergent granules, detergent tablets, laundry bags, or cleaning compositions. Preferably, the consumer product is a scent booster. The scent booster provides a strong scent to the laundry and can be used with other laundry additives such as detergents or fabric softeners. Thus, another object of the present disclosure is a laundry composition comprising a scent booster and a laundry additive selected from a detergent, a fabric softener, a rinse aid, or a bleach booster product. Another object of the present disclosure is the use of the scent booster in the wash to provide perfume to fabrics.
[0083] In yet another aspect, the present disclosure relates to the use of the above-mentioned consumer product for hand-washing fabrics. According to a particular embodiment, the present disclosure relates to a method of using a laundry composition for hand-washing fabrics, comprising: (a) providing such a laundry composition; (b) forming a laundry liquor by diluting the laundry composition with water in a weight ratio of about 1:100 to about 1:1000; (c) hand-washing fabrics in the laundry liquor; and (d) rinsing the fabrics with water. In another embodiment, the present disclosure relates to the use of the above-mentioned laundry composition for washing machine fabrics.
[0084] While numerous aspects and embodiments have been described above, these are illustrative and not limiting. After reading this specification, one of ordinary skill in the art will appreciate that other aspects and embodiments are possible without departing from the scope of the invention. All publications cited herein are incorporated by reference in their entirety.
[0085] Test Method In order that the invention described and claimed herein may be more fully understood, the following test methods described should be used.
[0086] Test method 1: Dissolution rate test The Dissolution Rate Test is used to measure the rate at which granules dissolve. This test is performed by adding 99.0 g of deionized water to a 400 mL clear beaker at room temperature (25° C.). The beaker is placed on a stir / hot plate. A conductivity probe (Fisher Conductivity Meter) is placed into the beaker using the clamp. The conductivity meter is turned on and the stir speed is set to 500 RPM. 1.0 g of granules is added to the mix water and the timer is started. When the conductivity meter reading plateaus, the meter will flash a "READY" status and the timer will stop. The elapsed time (i.e., the total time required for the granules to completely dissolve) is recorded as the dissolution rate of the granules.
[0087] Test Method 2: Skeletal Density Test (i.e. Porosity Test) The porosity test is used to measure the relative volume of porosity contained within the internal structure of a granule (i.e., intragranular porosity). The principle of Applicant's porosity test follows the published international standard ISO 15901-01: Evaluation of pore size distribution and porosity of materials by mercury porosimetry and gas adsorption - Part 1: Principles of mercury porosimetry. Porosity is divided into two categories: intergranular (voids between granules) and intragranular porosity (pores within granules). The method is used to measure intragranular porosity. Details of the method adapted for this disclosure are as follows:
[0088] Approximately 2 cm2 with granule sizes of 300 μm to 600 μm by sieve classification 3 A volumetric granule sample is loaded into a hardness tester assembly with appropriate bulb and stem assemblies to ensure greater than 25% and less than 75% stem volume utilization over the pressure range specified in Part 3. The sample assembly is then evacuated to remove gas from the pores.
[0089] Dry nitrogen is introduced in a controlled manner into the evacuated measuring cell and the pressure is increased (by applying pressure stepwise, continuously or stepwise) with the required precision for the specific pore size range of interest, covering up to at least 0.2 MPa, corresponding to a pore size of 6 μm, according to the appropriate equilibrium conditions for the mercury entering the pores. The pressure and the corresponding volume of the invaded mercury can be recorded graphically or via computer. Once the maximum required pressure is reached, the pressure is reduced to ambient and the sample holder is transferred to the high pressure unit.
[0090] In the high pressure unit, the pressure is increased through the intrusion of mercury (as working fluid) by stepwise pressurization according to the appropriate equilibrium conditions of mercury entering the pores, with the precision required for the specific pore size range of interest, covering at least a maximum of 400 MPa, which corresponds to a pore diameter of 3 nm. As a result, mercury is forced into the pore system and the decrease in the length of the mercury column is measured as a function of pressure. The pressure and the corresponding volume of invaded mercury can be recorded via a computer.
[0091] The applied pressure is inversely proportional to the apparent width of the pore entrance. For a cylindrical pore, the Washburn equation describes the relationship between pressure and diameter: p =-4γcosθ / P, where d p is the pore diameter, γ is the surface tension of mercury [Nm -1 ], θ is the contact angle, and P is the penetration pressure. Commonly used values for the surface tension and contact angle of mercury are 480 mN.m -1 and 140°. The Washburn equation is used to convert the pressure readings to pore size. The pore volume distribution is obtained by plotting the intrusion volume related to the sample mass as the vertical axis depending on the pore diameter as the horizontal axis.
[0092] The cumulative pore volume distribution includes both interstitial and intragranular pores. Within the scope of this disclosure, the intragranular pore size threshold has been determined using differential distribution analysis. 30 μm is the cutoff pore size, with pores larger than 30 μm considered intergranular and pores smaller than 30 μm considered intragranular. Intragranular porosity is calculated by dividing the intragranular pore volume by the sum of the intragranular pore volume and the solid volume of the granule sample. The solid volume of the sample is the sample volume minus the total pore volume. EXAMPLES
[0093] The following non-limiting examples are provided to further illustrate the present invention and should not be construed as limitations thereof, since many variations of the present invention are possible without departing from the spirit or scope of the invention.
[0094] Example 1 - Preparation of granules containing both neat and encapsulated flavors The composition of the perfume-containing granules is shown in Table 3 below. In a suitable container, the specified amount of water was added and heated to approximately 60° C. With continuous mixing, sodium sulfate was added and mixed until completely dissolved. Capsul® modified starch was added slowly to minimize clumping and mixing was continued until completely dissolved. The resulting solution was cooled to approximately 30° C. The viscosity of the solution was checked with a Brookfield viscometer at 60 RPM using spindle #7. The viscosity value was high at 30,000 cPs.
[0095] In a separate container, a predetermined amount of neat perfume oil was added. While homogenizer IKA Turrax® T-50 (available from IKA-Werke GmbH & Co. KG, Staufen, Germany) was immersed in the starch and sodium sulfate solution, neat perfume oil was slowly added to the solution until the neat perfume container was empty. Continuous high shear at 13500 RPM for a minimum of 5 minutes. The viscosity of the resulting oil-in-water emulsion was checked with a Brookfield viscometer using spindle #7 at 60 RPM. The viscosity value was high at 30,000 cPs. The size distribution of the oil droplets in the emulsion was also checked. The target mean of less than 10 micrometers and the target mode of less than 3 micrometers were achieved.
[0096] While continuously mixing the emulsion, the microcapsule slurry containing the encapsulated perfume was slowly added into the emulsion in a predetermined amount. In the granules prepared in this Example 1, the weight ratio of neat perfume to encapsulated perfume was 4:1. Again, the viscosity of the resulting emulsion was checked with a Brookfield viscometer using spindle #4 at 60 rpm. The viscosity value was as high as 10,000 cPs.
[0097] Finally, while mixing, rice starch was added to the emulsion in the specified amount to make the emulsion stock (i.e., feed slurry) to be used in the printing process as shown in Figure 1. The viscosity of the resulting emulsion was again checked at 60 rpm using spindle #4. The viscosity value was high at 15,000 cPs.
[0098] As shown in Figure 1, the emulsion raw material (i.e., feed slurry) produced above was deposited on a conveyor belt as droplets or dots with a diameter of 3 mm. The conveyor belt moved at a belt speed of 10 meters per minute. The dots were dried in a drying chamber by infrared light to produce the perfume-containing granules of the present disclosure.
[0099] [Table 6]
[0100] Example 2 (Comparative) - Preparation of Granules Containing Encapsulated Flavor Only Granules were prepared in the same manner as in Example 1, except that the composition of the flavor-containing granules shown in Table 4 below (no neat flavor was used) was used.
[0101] [Table 7]
[0102] Example 3 (Comparative) - Preparation of Spray-Dried Samples The same emulsion (Table 3) prepared in Example 1 was used to prepare spray-dried particles, except that the emulsion was diluted with an additional 680 g of water to reduce the viscosity of the emulsion to a few hundred centipoise suitable for the spray-drying process. The resulting emulsion was spray-dried using well-known spray-drying techniques to produce spray-dried particles (spray-dried sample). In the spray-dried sample, the weight ratio of neat perfume to encapsulated perfume was 4:1.
[0103] Example 4 (Comparative) - Preparation of PEG Beads (i.e., PEG-Based Scent Booster) 85.59 g of Pluriol® E8000 PEG (polyethylene glycol) was added to a 150 mL glass beaker using an IKA Eurostar overhead mixer. The PEG was melted using a 72° C. water bath as the heat source for the beaker. The overhead mixer was turned on midway through the melting process when the PEG material could be stirred freely and set at a low speed (75 rpm). It took approximately 30 minutes for the PEG to completely melt.
[0104] Once the PEG was completely melted, the overhead mixer was set at low speed (75 rpm) and 6.41 g of the microcapsule slurry containing 2.0 g of encapsulated fragrance was slowly added to the molten PEG. While the PEG / microcapsule mixture was continuously mixed at 75 rpm, 8.0 g of neat fragrance oil was added to the mixture and the water bath was reset to 70°C.
[0105] While the PEG / microcapsule / neat flavor molten mixture was continuously mixed, a 5 mL syringe was inserted into the molten mixture and 5 mL of the molten sample was drawn into the syringe. The molten sample was evenly dispensed as small droplets onto a room temperature baking sheet. The droplets were cooled and collected from the baking sheet as PEG beads. The resulting PEG beads contain a 4:1 weight ratio of neat flavor and encapsulated flavor.
[0106] Example 5 (Comparative) - Preparation of HPMC High Flavor Granules 30 g of Methocel™ K4M HPMC powder was added onto a stainless steel tray to form an HPMC powder bed. Using a pipette, 10 g of the microcapsule slurry (containing 2.8 g of encapsulated fragrance) was deposited onto the HPMC powder bed in the form of droplets. The droplets were deposited onto the powder bed in a pattern or array such that the droplets were evenly distributed and spaced apart. The pipette was then used again to deposit 11.2 g of neat fragrance in the form of droplets onto the HPMC powder bed. The neat fragrance was deposited onto the microcapsule droplet spots and between the microcapsule droplets. The stainless steel tray was then placed into an oven set at 50-200° C. for 30 minutes. The tray was then removed from the oven and allowed to cool to room temperature.
[0107] The product in the tray was screened through a 60 mesh (250 micrometer) screen and the HPMC granule product was collected on the screen. Some HPMC powder passed through the screen. It was found that the HPMC granules (containing neat and encapsulated fragrance) were not of uniform size. Some HPMC granules were clumped and on the order of a few centimeters while some other HPMC granules were significantly smaller. The neat fragrance oil acted as a flocculant for the HPMC powder and some large agglomerates were obtained after drying in the oven. Agglomeration also resulted in inconsistent / uneven distribution of the fragrance material.
[0108] Example 6 - Dissolution and Residue Evaluation A study was conducted to evaluate the dissolution of various scent booster samples (see Table 5 below) in a water temperature controlled wash cycle. Sample amounts were determined to deliver 0.5g of perfume equivalent per wash.
[0109] [Table 8]
[0110] A specified amount of test sample was placed into a black cotton blend drawstring bag (6×8 inches) and washed in a Speed Queen® stackable washer under the conditions listed below: Washing conditions: Wash Cycle - Rapid Wash (30 minute wash cycle) Temperature - low temperature setting Dirt level: Medium Spin Speed - Medium
[0111] Once washing was complete, the washed black cotton blend drawstring bag was turned inside out and inspected. Visual inspection showed that all of the disclosed granules, spray dried particles and HPMC granule samples were completely dissolved under the wash conditions (wash cycle and water temperature) tested. There were no visual signs of sample residue remaining on the black cotton blend drawstring bag after washing with these samples. However, visual inspection showed that a significant amount of PEG bead residue remained on the black cotton blend drawstring bag after washing with the PEG bead sample. This demonstrated that the PEG bead sample was not completely dissolved under the wash conditions tested.
[0112] Example 7 - Fragrance Performance Evaluation To evaluate perfume performance, the perfume intensity of the perfumes contained in the scent booster samples listed in Table 6 below was evaluated by conducting a wash experiment. The sample amounts were determined to deliver 0.5g of perfume equivalent per wash.
[0113] [Table 9]
[0114] The washing experiment was carried out as follows. Washer settings: Permanent Press Temperature: cold Medium speed rotation Dirt level: Medium Dryer settings: 60 minutes (medium) Washing Process: Set the washer to the above settings. Fill the drum with a 4 lbs load of clothing. Add 50 g of unscented Tide® Free and Clear detergent to the detergent drawer. The specified amount of the scent booster sample listed in Table 6 is added directly to the drum. Close the washer door and start the wash. Once the wash is complete, remove the clothes from the washer and place in the dryer on a medium setting for 60 minutes.
[0115] Perfume intensity and performance were evaluated by a group of evaluators at three different stages (wet, pre-rub, and post-rub) and rated on a scale ranging from 0 to 5. A value of 0 indicates that the fabric produced no sign of released perfume, and 5 indicates a very strong odor of released perfume. "Wet" refers to the stage where the clothes have been washed but not dried (i.e., the clothes have been removed from the washing machine but before being placed in the dryer). "Pre-rub" refers to the stage where the clothes have been dried (in the dryer) but before the dried clothes have been folded or rubbed. "Post-rub" refers to the stage where the clothes have been dried (in the dryer) and the dried clothes were rubbed three times between both hands to rupture the microcapsules attached to the clothes.
[0116] At each of the three different stages (wetting, pre-rubbing, and post-rubbing), the evaluators smelled the fabric and rated it for evidence of perfume released from the fabric. The results were recorded and are shown in Table 7 below.
[0117] [Table 10]
[0118] It should be noted that not all of the acts described above in the summary or examples are required, that some of the specific acts may not be required, and that one or more additional acts may be performed in addition to those described. Furthermore, the order in which the acts are listed is not necessarily the order in which the acts are performed.
[0119] In the foregoing specification, the concepts have been described with reference to specific embodiments. However, those skilled in the art will appreciate that various modifications and changes can be made without departing from the scope of the invention as set forth in the following claims. Accordingly, the specification is to be regarded in an illustrative rather than a restrictive sense, and all such modifications are intended to be included within the scope of the present invention.
[0120] Benefits, other advantages, and solutions to problems have been described above with respect to specific embodiments. However, the benefits, advantages, solutions to problems, and any features that may give rise to or make more prominent any benefit, advantage, or solution should not be construed as critical, necessary, or essential features of any or all of the claims.
[0121] It should be understood that certain features that are, for clarity, described herein in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features that are, for brevity, described in the context of a single embodiment, may also be provided separately or in any subcombination.
Claims
1. A flavor-containing granule, (a) fragrance materials, including neat fragrances and encapsulated fragrances; (b) a carbohydrate carrier; and Including, the amount of the flavoring material is greater than 40%, 45%, 50%, 55%, or 60% by weight based on the weight of the granule; the weight ratio of the neat fragrance to the encapsulated fragrance is 10:1 to 1:1; The granules have a skeletal density of greater than 1.00 g / mL or greater than 1.05 g / mL.
2. 10. The granules of claim 1, wherein the granules have an average median diameter in the range of 1 mm to 5 mm, or 2 mm to 3 mm.
3. The granules contain one or more intragranular voids, and the granules have a dissolution rate of 1 minute or 30 seconds or less when measured in deionized water at 25° C. according to the Dissolution Rate Test described herein. Granules according to claim 1 characterized by:
4. The granules are (a) a water activity (aw) of <0.6 at 25°C, and / or (b) an average granule weight of 1 mg to 10 mg, or 3 mg to 7 mg, and / or (c) a bulk density of 0.1 g / mL to 1 g / mL, or 0.2 g / mL to 0.6 g / mL The granule of claim 1 having
5. 2. The granules of claim 1, wherein the granules have a particle size dispersity index (PSDI) of <0.2 (standard deviation / average).
6. 2. The granule of claim 1, wherein the weight ratio of said flavoring substance to said carbohydrate carrier is from 9:1 to 1:
1.
7. 10. The granule of claim 1, wherein the granule has a biologically renewable carbon (BRC) content of at least 50%, at least 55%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, or at least 95%, based on the weight of the granule.
8. The granule of claim 1 , wherein the carbohydrate carrier comprises starch, modified starch, polysaccharide, cellulose, and / or pectin.
9. The granule of claim 8 , wherein the carbohydrate carrier comprises a modified starch.
10. The fragrance material is (i) 30% to 45%, or 25% to 42.5% by weight of a neat flavoring, based on the total weight of the granules; (ii) 5% to 20%, or 7.5% to 15% by weight of an encapsulated flavoring, based on the total weight of the granules; The granule of claim 1 comprising:
11. 2. The granule of claim 1, wherein the encapsulated perfume is encapsulated by a biodegradable microcapsule shell, preferably the biodegradable microcapsule shell having a biodegradation rate of at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 95% or at least 98% based on the weight of the microcapsule shell within 60 days according to OECD 301F.
12. 10. The granule of claim 1, wherein the carbohydrate carrier has a melting point temperature of 70°C or higher, 80°C or higher, 90°C or higher, or 100°C or higher.
13. A process for treating laundry comprising the step of adding 1 g to 30 g, preferably 3 g to 20 g, of granules according to any one of claims 1 to 12 to the laundry in a washing machine or basin.
14. 13. A consumer product comprising a perfume-containing granule according to any one of claims 1 to 12, wherein the consumer product is a scent booster, fabric refresher, detergent (powder), fabric softener, rinse aid, water softener, bleach booster, disinfectant, unit dose laundry detergent, detergent granule, detergent tablet, laundry bag or cleaning composition.