Low moisture composition
A low-moisture composition with a crystalline mesh microstructure from sodium fatty acid carboxylate and polyethylene glycol domains addresses stability and dissolution issues in freshness beads, offering enhanced fragrance delivery and sustainability.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- PROCTER & GAMBLE CO
- Filing Date
- 2023-08-08
- Publication Date
- 2026-05-11
AI Technical Summary
Existing freshness beads face challenges in achieving physical stability, temperature and humidity resistance, and effective dissolution while maintaining low residue, limiting fragrance delivery and sustainability.
A low-moisture composition comprising a crystalline mesh microstructure formed from sodium fatty acid carboxylate and polyethylene glycol domains, with a freshness-enhancing agent, which dissolves during washing, providing improved dissolution rates and stability.
The composition achieves remarkable fragrance delivery, resistance to temperature and humidity, and broader fragrance range, enhancing freshness performance and reducing environmental impact.
Smart Images

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Abstract
Description
[Technical Field]
[0001] Contains a mesh microstructure formed from a dry sodium fatty acid carboxylate compound. water soluble solid Body composition A low-moisture composition comprising a compound (SDC), a polyethylene glycol domain (PEGC), and a freshness-enhancing agent, which dissolves during normal use and delivers remarkable freshness to fabrics. [Background technology]
[0002] Freshness beads are added directly to the washing machine drum to supply freshness to the wash cycle. In the most basic design, the beads consist of a “primary” carrier (e.g., PEG, different molecular weights) and a freshness-enhancing agent (e.g., fragrance capsules, neat fragrance) to deliver the freshness effect. Suitable base compositions are disclosed, for example, in U.S. Patent No. 8,476,219 (B2). In more advanced designs, the beads also consist of one or more “secondary” carriers (often called fillers) dispersed in the primary carrier to fulfill one or more specific functions in the beads. For example, in one disclosure (U.S. Patent No. 9,347,022 (B1)), starch granules are added to the PEG in the beads to reduce the cost of the beads. In another disclosure (International Publication No. 2021 / 170759 (A1)), polymers, inorganic salts, clays, sugars, polysaccharides, glycerol, and fatty alcohols are added to facilitate processing and increase stability. In yet another example, the beads consist of a “primary” carrier comprising salts and sugars, sodium acetate trihydrate, and a block copolymer, as disclosed in U.S. Patent Nos. 11,008,535(B2), 11,220,657(B2), and 10,683,475(B2), respectively.
[0003] Formulating effective solid-soluble compositions presents considerable challenges. The compositions must be physically stable, preferably temperature and humidity resistant, and furthermore, they must be able to dissolve in solution, leaving little to no material residue, thereby performing the desired function. Solid-soluble compositions are well known in the art and are used in several roles, including detergents, oral and body medications, disinfectants, and cleaning compositions.
[0004] It has a mesh microstructure formed from dry sodium fatty acid carboxylate that can contain high concentrations of active substances. water soluble solid Body composition The product (SDC) is readily soluble in water during washing conditions, yet is temperature and humidity resistant, enabling supply chain stability. water soluble solid Body composition The ability to create the product (SDC) is remarkable. Low-moisture compositions containing both PEGC and SDC domains have been found to offer significant advantages over current freshness beads, including improved dissolution rate, sustainability, wider fragrance range, moisture control, broader sourcing opportunities, cost reduction, lighter weight for efficient e-commerce transport, and protection of unsuitable chemicals. [Prior art documents] [Patent Documents]
[0005] [Patent Document 1] U.S. Patent No. 8,476,219(B2) [Patent Document 2] U.S. Patent No. 9347022(B1) [Patent Document 3] International Publication No. 2021 / 170759(A1) [Patent Document 4] U.S. Patent No. 11,008,535(B2) [Patent Document 5] U.S. Patent No. 11,220,657(B2) [Patent Document 6] U.S. Patent No. 10,683,475(B2) [Overview of the Initiative] [Means for solving the problem]
[0006] The low-moisture composition has at least one crystallizer water soluble solid Body composition The product comprises a product (SDC) domain, at least one polyethylene glycol (PEGC) domain, and a freshness-enhancing agent, wherein the crystallizing agent is a sodium salt of a saturated fatty acid having 8 to about 12 carbon atoms, and the freshness-enhancing agent is present in at least one of the SDC or PEGC.
[0007] A low-moisture composition that substantially dissolves during normal use and provides remarkable freshness to the fabric, and is made from a crystallizing agent. water soluble solid Body composition A low-moisture composition is provided, comprising a product (SDC) domain, a polyethylene glycol (PEGC) domain, and water, wherein the crystallizing agent is a sodium fatty acid carboxylate having 8 to about 12 carbon atoms, and the amount of water is less than 10% by weight of the final low-moisture composition, as determined by a moisture content test method.
[0008] A method for producing a low-moisture composition, comprising mixing and heating a crystallizing agent and an aqueous phase until the crystallizing agent is substantially solubilized, Solid soluble composition mixture ( SDCM ) forms, during SDCM Cooling the crystallizing agent to a temperature before significant crystallization, and cooling the solid soluble composition mixture to below the crystallization temperature, and the solid soluble composition mixture to Solid-State Philology composition By crystallizing it, Water-soluble solid composition ( SDC ) To form it into the designed shape and size, and to dry and remove excess water. , By removing approximately 90% to 99% of the water from the ologie solid composition, as determined by the moisture content testing method, water soluble solid Body composition The product (SDC) is produced and has an average solubility percentage of over 5% at 37°C, as determined by a dissolution test method. water soluble solid Body composition generating a product, providing polyethylene glycol (PEG C), and combining SDC and PEG C to generate a low-moisture composition having SDC domains and PEG C domains, wherein a freshness benefit agent is added to at least one of the SDC domains or PEG C domains. A method is provided. BRIEF DESCRIPTION OF THE DRAWINGS
[0009] This specification concludes with claims that particularly and distinctly claim the subject matter regarded as the present disclosure, but it is believed that the present disclosure will be better understood by reading the following description in conjunction with the accompanying drawings. Some of the figures may be simplified by omitting selected elements for the purpose of more clearly showing other elements. The omission of such elements in some of the figures does not necessarily indicate the presence or absence of elements in any of the exemplary embodiments, except as explicitly recited in the corresponding written description. None of the figures necessarily conform to a particular scale. [Figure 1A] Shows a scanning electron microscope (SEM) photograph of crystallizing agent crystals. [Figure 1B] Shows a scanning electron microscope (SEM) photograph of a mesh microstructure made from crystallized crystallizing agent in the SDC domain. [Figure 2A] Shows a scanning electron microscope (SEM) photograph of an executable fragrance capsule (e.g., Red Arrow, top) dispersed in the mesh microstructure of the SDC domain. [Figure 2B] Shows a scanning electron microscope (SEM) photograph of a fragrance capsule dispersed in the mesh microstructure of the SDC domain. [Figure 3] Graph showing the amount of fragrance in the headspace of a dried and rubbed fabric treated with an executable amount of a commercial product (about 1 gram of fragrance capsule, heaped cap) versus the composition of the present invention (about 2.5 grams of fragrance capsule, 1 / 2 cap). The composition of the present invention has a much greater amount of fragrance in the air and much less product added to the wash. [Figure 4A] This shows the dissolution behavior of SDC prepared using different combinations of crystallizing agents in relation to commercially available PEG, as determined by dissolution test methods. [Figure 4B] This shows the dissolution behavior of SDC prepared using different combinations of crystallizing agents in relation to commercially available PEG, as determined by dissolution test methods. [Figure 4C] This shows the dissolution behavior of SDC prepared using different combinations of crystallizing agents in relation to commercially available PEG, as determined by dissolution test methods. [Figure 5] This graph shows the stable temperature of the SDC domain for three compositions of the present invention, using a thermal stability test method. [Figure 6] This graph shows the hydration stability of the SDC domain of the present invention (%dm < 5% at 80% RH) by measuring the moisture uptake at 25°C under different relative humidity conditions using a humidity test method. [Figure 7] This is a diagram of particles in a low-moisture composition, as described in Example 1. [Figure 8] This is a diagram of particles in a low-moisture composition, as described in Example 2. [Figure 9] This is a diagram of particles in a low-moisture composition, as described in Example 3. [Figure 10] This is a diagram of particles in a low-moisture composition, as described in Example 4. [Figure 11A] A representative scanning electron microscope (SEM) image of a comparative composition prepared from potassium palmitate (KC16) and exhibiting small plate-like crystals is shown. [Figure 11B] A representative scanning electron microscope (SEM) image of a comparative composition prepared from triethanolamine palmitate (TEA C16) and exhibiting small plate-like crystals is shown. [Modes for carrying out the invention]
[0010] The present invention includes a low-moisture composition that dissolves substantially or completely during a laundry cycle to provide remarkable freshness to fabrics. The low-moisture composition includes a crystalline mesh. water soluble solid Body composition The present invention comprises at least one domain of a product (SDC), at least one domain of a polyethylene glycol composition (PEGC), and, in embodiments, one or more freshness-enhancing agents, which may be in high concentrations. The crystalline mesh ("mesh") comprises a relatively rigid three-dimensional linked crystalline framework of fibrous crystalline particles formed during treatment with a crystallizing agent. water soluble solid Body composition The resulting product contains a crystallizing agent, low water content, and freshness-enhancing agent, and is readily soluble in water at the target washing temperature.
[0011] The present invention may be more readily understood by referring to the detailed description of the following exemplary compositions. It should be understood that the claims are not limited to the specific products, methods, conditions, apparatus, or parameters described herein, and that the terms used herein are not intended to limit the claimed invention.
[0012] When used in this specification, water soluble solid Body composition The "Product" (SDC) comprises a sodium fatty acid carboxylate crystallizer, an optional freshness enhancer, and 10% by weight or less of water, which, when properly processed, forms an interconnected crystalline mesh of fibers that readily dissolve at the target washing temperature.
[0013] When used herein, “PEG composition” (PEGC) comprises PEG and an optional freshness-enhancing agent.
[0014] As used herein, “domain” means a continuous mass containing substantially the same material. In one embodiment, the domain may include SDC. In another embodiment, the domain may include PEGC.
[0015] As used herein, "low moisture composition" means a freshness composition containing both the SDC domain and the PEGC domain, as well as a freshness beneficial agent, and the low moisture composition has a water content of less than about 10% by weight.
[0016] In this specification, “consumer product” refers to a low-moisture composition purchased for providing freshness to fabrics during a wash cycle, which contains single or numerous particles added to a washing machine drum before or during a rinse or wash cycle to provide excellent freshness to the fabric. Such compositions include, but are not limited to, laundry cleaning compositions and detergents, fabric softening compositions, fabric strengthening compositions, fabric deodorizing compositions, pre-wash cleaning agents, pre-wash treatment agents, laundry additives, spray products, dry cleaning agents or compositions, wash-rinse additives, cleaning additives, post-rinse fabric treatment agents, ironing aids, unit-dose formulations, delayed-delivery formulations, detergents contained on or in porous substrates or nonwoven sheets, and other suitable forms that may be apparent to those skilled in the art in consideration of the teachings herein. Such products may be used as pre-wash and post-wash treatments.
[0017] As used herein, "particles" typically means separate masses (or chunks) in a low-moisture composition, having a mass exceeding approximately 5 mg and a size exceeding 1 mm. Particles may have different shapes, including, but not limited to, hemispheres, spheres, plates, gummy bears, and cashews. Particles may have one or more layers.
[0018] When used herein, the "Solid Solubility Composition Mixture" (SDCM) is defined as the mixture before water removal (e.g., during the mixing or crystallization stage). water soluble solid Body composition Contains the components of the finished product. water soluble solid Body compositionTo produce the product, an intermediate solid-soluble composition mixture containing an aqueous phase with an aqueous carrier is first formed. The aqueous carrier may be distilled water, deionized water, or tap water. The aqueous carrier may be present in an amount of about 65% to 99.5% by weight, or about 65% to 90% by weight, or about 70% to 85% by weight, or about 75% by weight of the SDCM.
[0019] As used herein, “rheological solid composition” (RSC) describes the solid form of SDCM after crystallization (crystallization stage) before water removal to obtain SDC, where RSC contains more than approximately 65% by weight of water, and the solid form is derived from a linked “structured” mesh (mesh microstructure) of fibrous crystalline particles from the crystallizing agent.
[0020] As used herein, "PEG" comprises polyethylene glycol (PEG) having a molecular weight of about 200 to about 50,000 daltons, most preferably about 6,000 to 10,000 daltons.
[0021] As used herein and as further described below, “freshness beneficial agent” includes materials added to a domain to impart a freshness effect to a fabric through washing. In some embodiments, the freshness beneficial agent may be a neat fragrance. In embodiments, the freshness beneficial agent may be an encapsulated fragrance (fragrance capsule). In embodiments, the freshness beneficial agent may be a mixture of fragrances and / or fragrance capsules.
[0022] As used herein, “crystallization temperature” is used to describe the temperature at which a crystallizing agent (or combination of crystallizing agents) is completely solubilized in SDCM, or, as used herein, to describe the temperature at which a crystallizing agent (or combination of crystallizing agents) exhibits any crystallization in SDCM.
[0023] As used herein, “dissolution temperature” is used to describe the temperature at which a low-water-content composition is completely solubilized in water under normal washing conditions.
[0024] As used herein, “stable temperature” is the temperature at which the SDC and / or PEGC domain material completely melts, such that the composition no longer exhibits a stable solid structure and can be considered a liquid or paste, and the low-moisture composition no longer functions as intended. The stable temperature is the lowest thermal transition temperature determined by a thermal stability test method. In embodiments of the present invention, the stable temperature may be greater than about 40°C, more preferably greater than about 50°C, more preferably greater than about 60°C, and most preferably greater than about 70°C, in order to ensure stability in the supply chain. Those skilled in the art will understand how to measure the lowest thermal transition temperature using differential scanning calorimetry (DSC) equipment.
[0025] As used herein, “humidity stability” is the relative humidity at which a low-moisture composition spontaneously absorbs more than 5% by weight of its original mass in water from the ambient humidity at 25°C. Water absorption may occur in either the SDC domain and / or the PEGC domain. Absorption of small amounts of water when exposed to a humid environment allows for more sustainable packaging. Absorption of large amounts of water risks the composition softening or liquefying and no longer functioning as intended. In embodiments of the present invention, humidity stability may be greater than 70% RH, more preferably greater than 80% RH, more preferably greater than 90% RH, and most preferably greater than 95% RH. Those skilled in the art will understand the method of measuring a 5% weight increase using a dynamic vapor sorption (DVS) apparatus, which is further described in the humidity test method.
[0026] When used herein, “cleaning composition” means, unless otherwise specified, general-purpose or “strong” cleaning agents in the form of granules or powders, in particular cleaning detergents; general-purpose cleaning agents in the form of liquids, gels or pastes, in particular so-called strong liquid types; liquid detergents for delicate fabrics; dishwashing detergents or light dishwashing detergents, in particular highly foaming types; dishwasher detergents, liquid detergents and disinfectants (including antimicrobial handwashing types, cleaning bars, mouthwashes, denture cleaners, toothpastes, car or carpet shampoos, and bathroom cleaners), including various pouches, tablets, granules, liquids and quick-rinsing types for household and commercial use; hair shampoos and hair conditioners; shower gels and foam baths, and metal cleaners; in addition, cleaning aids such as bleaching additives and “stain sticks” or pre-treatment types, dryer additive sheets, dry and wet wipes and pads, nonwoven fabric substrates, and products having substrates such as sponges; in addition, sprays and mists.
[0027] As used herein, “dissolves during normal use” means that a low-water-content composition dissolves completely or substantially during a cleaning cycle. Those skilled in the art will recognize that cleaning cycles have a wide range of conditions (e.g., cycle time, machine type, cleaning solution composition, temperature). A suitable composition dissolves completely or substantially under at least one of these conditions.
[0028] As used herein, the term "bio-based" material refers to renewable materials.
[0029] As used herein, the term “renewable material” refers to a material produced from a renewable material. As used herein, the term “renewable resource” refers to a resource produced by natural processes at a rate comparable to its consumption rate (e.g., within a 100-year timeframe). This resource may be replenished naturally or by agricultural technology. Non-limiting examples of renewable resources include plants (e.g., sugarcane, beets, maize, potatoes, citrus fruits, woody plants, lignocellulose, hemicellulose, and cellulose waste), animals, fish, bacteria, fungi, and forest products. These resources may be naturally occurring, hybridized, or genetically modified organisms. Natural resources such as crude oil, coal, natural gas, and peat, which take more than 100 years to form, are not considered renewable resources. Since at least a portion of the materials of the present invention are derived from renewable resources that can be decarbonized, the use of these materials can reduce the potential for global warming and fossil fuel consumption.
[0030] As used herein, the term “bio-based content” refers to the amount of carbon in a material derived from renewable resources, as a percentage of the weight (mass) of the total organic carbon in the material, determined using ASTM D6866-10, Method B.
[0031] The term "solid" refers to the state of the composition under the expected storage and use conditions for low-moisture compositions.
[0032] When used herein, articles such as "a" and "an" are understood to mean one or more of the claims or descriptions when used in the claims.
[0033] As used herein, the terms “include,” “includes,” and “including” are intended to be non-limiting.
[0034] Unless otherwise noted, all concentrations of components or compositions refer to the active portion of that component or composition, excluding impurities that may be present in the commercially available source of such components or compositions, such as residual solvents or by-products.
[0035] All percentages and ratios are calculated on a weight basis unless otherwise specified. All percentages and ratios are calculated based on the total composition unless otherwise specified.
[0036] It should be understood that all maximum numerical limits given throughout this specification include all lower numerical limits as if they were explicitly stated herein. All minimum numerical limits shown throughout this specification include all higher numerical limits as if they were explicitly stated herein. All numerical ranges given throughout this specification include all narrow numerical ranges that fall within such broad numerical ranges as if they were explicitly stated herein.
[0037] water soluble solid Body composition The composition (SDC) comprises fibrous linked crystals (Figures 1A and 1B) having sufficient crystalline fiber length and concentration to form a mesh microstructure. The mesh allows the SDC to be solid with a relatively small amount of material. The mesh also allows for the capture and protection of particles such as freshness beneficial agents, such as fragrance capsules (Figures 2A and 2B). In embodiments, the active material is discrete particles having a diameter of less than 100 μm, preferably less than 50 μm, and more preferably less than 25 μm. Furthermore, the considerable voids in the mesh microstructure also allow for the inclusion of liquid freshness beneficial agents, such as neat fragrances. In embodiments, up to about 15% by weight of neat fragrance, preferably 13% to 0.5% by weight, preferably 13% to 2% by weight, and most preferably 10% to 2% by weight, can be added. The voids also provide pathways for water to be incorporated into the microstructure during washing to accelerate dissolution compared to a completely solid composition.
[0038] Remarkably, it is possible to prepare SDCs with high dissolution rates, low water content, moisture resistance, and thermal stability. Sodium salts of long-chain fatty acids (i.e., sodium myristate (NaC14) to sodium stearate (NaC18)) can form fibrous crystals. It is generally understood that the crystal growth pattern resulting in fibrous crystallization reflects the hydrophilic (head group) and hydrophobic (hydrocarbon chain) balance of the NaC14-NaC18 molecules. As disclosed in this application, the crystallizers used have the same hydrophilic contribution but exhibit very different hydrophobicity due to the shorter hydrocarbon chain of the fatty acid sodium carboxylate used. In fact, the carbon chain is about half the length of those previously disclosed (U.S. Patent Application Publication 2021 / 0315783(A1)). Furthermore, those skilled in the art will recognize that many surfactants, such as alkyl sulfates, which have the same chain but different head groups, are susceptible to considerable moisture uptake and significant temperature-induced changes. The selected group of crystallizers in the present invention enables all of these useful properties.
[0039] Current water-soluble polymers (e.g., PEG only) limit the use of fragrance capsules as a fragrance enhancer delivery system. The encapsulated fragrance is delivered in an aqueous slurry, with the slurry limited to a maximum of 20-30% by weight of the encapsulated fragrance, and the total amount of encapsulated fragrance limited to approximately 1.2% by weight. Using encapsulated fragrances at concentrations exceeding these limits the solidification of the water-soluble carrier, thereby restricting fragrance delivery. As a result, consumers generally do not fully enjoy the desired amount of freshness due to the limitations on what they can add to their cleaning solutions. This invention addresses this issue. water soluble solid Body composition The composition can construct fragrance capsules of up to 18% by weight, resulting in approximately 15 times greater fragrance delivery compared to current water-soluble polymers. Such high delivery is at least partially enabled by the low water content of the composition, allowing users to experience a significant freshness upgrade compared to current commercially available fabric freshness beads (Figure 3).
[0040] The improved performance of the present invention's compositions compared to current freshness laundry beads is thought to be related to the dissolution rate of the composition's matrix. While not limited to theory, it is considered likely that if the composition dissolves later in the wash cycle, the encapsulated fragrance will deposit on the fabric throughout the wash (TTW), enhancing freshness performance. Current water-soluble polymers used in commercially available fabric freshness beads have a limited dissolution rate, set by the limited molecular weight (MW) range of polyethylene glycol (PEG) used as the dissolution matrix. As a result, single PEG beads must function under a certain range of machine and wash conditions, limiting their performance. In contrast, the dissolution rate of the present composition can be adjusted to suit a range of machine and wash conditions by adjusting the ratio of the composition components (e.g., sodium laurate (NaL) to sodium decanoate (NaD) ratio) (Figures 4A-4C). This allows for the creation of a wide range of compositions useful under many different wash conditions, where the SDC domains can release freshness beneficial agents at different times during the wash cycle.
[0041] The main commercially available fabric freshness bead manufacturing processes limit the selection of freshness beneficial agents. Alternatively, SDC domains can be processed and added to low-moisture compositions. PEG, used to form most currently commercially available beads, must be processed at temperatures between 70°C and 80°C, above the melting point of PEG. Preparing SDC domains at room temperature allows for a wider variety of freshness technologies. In practical processes, the melting point of PEG must be maintained for several hours, and some fragrance ingredients are highly volatile and evaporate during processing. Inclusion of fragrance oils for SDC is performed at around 25°C, opening up a wide range of neatly added fragrances. Furthermore, many fragrance capsule wall structures cease to function at higher process temperatures, releasing the encapsulated fragrances and rendering them inactive in low-moisture compositions. Processing fragrance capsules at lower temperatures allows for a wider range of capsules.
[0042] Controlling water migration in mixed bead compositions (e.g., low-water-content and high-water-content beads) is difficult with current water-soluble polymers because water migrates to the surface of the high-water-content beads. Since beads are often packaged in encapsulated packages to minimize moisture permeation to and from the package, moisture trapped on the surface of the high-water-content beads comes into contact with the surface of the low-water-content beads, leading to bead aggregation and product distribution problems. In contrast, water soluble solid Body composition The structure of the material prevents water movement and therefore allows the use of materials sensitive to water absorption (e.g., cationic polymers, bleaches).
[0043] As mentioned above, current bead formulations using PEG (and other structured materials) are prone to degradation when exposed to heat and / or humidity during transport. Therefore, special transport conditions and / or packaging are often required to mitigate such degradation. The SDC of the present invention contains a crystalline structure that is stable within a range of temperature and humidity conditions. The SDC domain exhibits %dm of less than 5% at 70% RH, more preferably less than 5% at 80% RH, and most preferably less than 5% at 90% RH, as determined by a humidity test method (Figure 5), and does not exhibit an intrinsic melt transition below 50°C, as determined by a thermal stability test method (Figure 6). As a result, no additional resources are required for refrigeration and plastic packaging during transport to prevent moisture migration. Including the SDC domain in a low-moisture composition allows for robust protection of freshness beneficial agents.
[0044] Finally, although I don't want to limit myself to theory, water soluble solid Body composition The high dissolution rate of the product is thought to be at least partially provided by the mesh microstructure. This is considered important because this porous structure provides the product with both "lightness" and the ability to dissolve rapidly compared to compressed tablets, which allows for easy delivery of the active substance during use. A single crystallizing agent (or in combination with other crystallizing agents) water soluble solid Body compositionIt is considered important to form fibers in the manufacturing process. Fiber formation allows for the retention of active substances without requiring compression that could break microencapsulation. water soluble solid Body composition Making finished products possible.
[0045] In the embodiment, the fibrous crystals may have a minimum length of 10 μm and a thickness of 2 μm, as determined by a fiber testing method. Non-limiting examples of particles are shown in Figures 7, 8, 9, and 10.
[0046] In the embodiment, the active substance may take the form of particles, which may be a) uniformly dispersed within a mesh microstructure, b) coated on the surface of a mesh microstructure, or c) some of the particles may be dispersed within the mesh microstructure and some of the particles may be coated on the surface of a mesh microstructure. In the embodiment, the active substance may be a) in the form of a soluble film on the upper surface of a mesh microstructure, b) in the form of a soluble film on the bottom surface of a mesh microstructure, or c) in the form of a soluble film on both the bottom and top surfaces of a mesh. The active substance may exist as a combination of a soluble film and particles.
[0047] Crystallizing agent The crystallizing agent is selected for its ability to impart different properties to the SDC domain. The crystallizing agent is selected from a small group of sodium fatty acid carboxylates having saturated chains and chain lengths in the range of C8-C12. Within this compositional range, using the preparation method described, such sodium fatty acid carboxylates provide a fibrous mesh microstructure, an ideal solubilization temperature for dissolution during preparation and use, and can be obtained by appropriate blending. water soluble solid Body composition The finished product's properties can be adjusted to suit various applications and conditions.
[0048] The crystallizing agent may be present in the solid soluble composition mixture used to produce the SDC domain in amounts of about 5% to about 35% by weight, about 10% to about 35% by weight, and about 15% to about 35% by weight. The crystallizing agent may be present in the solid soluble composition in amounts of about 50% to about 99% by weight, about 60% to about 95% by weight, and about 70% to about 90% by weight. The crystallizing agent may be present in the low moisture composition in amounts of about 5% to about 60% by weight, about 10% to about 50% by weight, and about 15% to about 40% by weight.
[0049] Suitable crystallizing agents include sodium octanoate (NaC8), sodium decanoate (NaC10), sodium dodecanoate, or sodium laurate (NaC12), and combinations thereof.
[0050] Capsule materials The capsule may include a wall material that encloses the beneficial agent (beneficial agent delivery capsule or simply “capsule”). The beneficial agent may be referred to herein as “beneficial agent” or “encapsulated beneficial agent”. The encapsulated beneficial agent is enclosed within a core. The beneficial agent may be at least one of a fragrance mixture, an odor neutralizer, or a combination thereof. In one embodiment, the fragrance delivery technology may include beneficial agent delivery particles formed by at least partially encapsulating the beneficial agent with a wall material. The beneficial agents are 3-(4-t-butylphenyl)-2-methylpropanal, 3-(4-t-butylphenyl)-propanal, 3-(4-isopropylphenyl)-2-methylpropanal, 3-(3,4-methylenedioxyphenyl)-2-methylpropanal, and 2,6-dimethyl-5-heptenal, α-damascone, β-damascone, γ-damascone, β-damascenone, 6,7-dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanone, methyl-7,3-dihydro-2H-1,5-benzodioxepin-3-one, and 2-[2-(4-methyl-3-cyclohexenyl-1-yl)propyl]cyclopenta Materials may be selected from the group consisting of fragrance raw materials such as n-2-one, 2-sec-butylcyclohexanone, and β-dihydroionone, linalool, ethyllinalool, tetrahydrolinalool, and dihydromyrcenolate; waxes such as silicone oil and polyethylene wax; essential oils such as fish oil, jasmine, camphor, and lavender; skin cooling agents such as menthol and methyl lactate; vitamins such as vitamins A and E; sunscreens; glycerin; catalysts such as manganese catalysts or bleaching catalysts; bleaching particles such as perborates; silicon dioxide particles; antiperspirant active substances; cationic polymers, and mixtures thereof. Suitable beneficial agents can be obtained from Givaudan Corp. (Mount Olive, New Jersey, USA), International Flavors & Fragrances Corp. (South Brunswick, New Jersey, USA), Firmenich Company (Geneva, Switzerland), or Encapsys Company (Wisconsin, USA).As used herein, “Fragrance material” means one or more of the following: aromatic essential oils; aromatic compounds; materials supplied with aromatic essential oils, aromatic compounds, stabilizers, diluents, processing agents, and admixtures; and any materials commonly associated with aromatic essential oils and aromatic compounds.
[0051] The wall (or shell) material of the beneficial agent delivery capsule may include melamine, polyacrylamide, silicone, silica, polystyrene, polyurea, polyurethane, polyacrylate-based materials, polyacrylic acid ester-based materials, gelatin, styrene-malic anhydride, polyamide, aromatic alcohol, polyvinyl alcohol, and mixtures thereof. Melamine wall materials may include melamine crosslinked with formaldehyde, melamine-dimethoxyethanol crosslinked with formaldehyde, and mixtures thereof. Polystyrene wall materials may include polystyrene crosslinked with divinylbenzene. Polyurea wall materials may include urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, polyisocyanates reacted with polyamide, polyamines reacted with aldehyde, and mixtures thereof. Polyacrylate-based wall materials may include polyacrylates formed from methyl methacrylate / dimethylaminomethyl methacrylate, amine acrylates and / or methacrylates, polyacrylates formed from strong acids, carboxylic acid acrylates and / or methacrylate monomers, polyacrylates formed from strong bases, amine acrylates and / or methacrylate monomers, polyacrylates formed from carboxylic acid acrylates and / or carboxylic acid methacrylate monomers, and mixtures thereof.
[0052] The composition may contain beneficial agent delivery capsules in an amount of about 0.05% to about 20% by weight, or about 0.05% to about 10% by weight, or about 0.1% to about 5% by weight, or about 0.2% to about 2% by weight of the composition. The composition may contain a sufficient amount of beneficial agent delivery capsules to provide the composition with an enclosed beneficial agent, preferably a fragrance ingredient, in an amount of about 0.05% to about 10% by weight, or about 0.1% to about 5% by weight, or about 0.1% to about 2% by weight of the composition. Where used herein, the amount or weight percentage of beneficial agent delivery capsules refers to the total of the wall material and the core material.
[0053] The group of beneficial agent delivery capsules according to this disclosure can be characterized by a volume-weighted median particle size of about 1 to about 100 μm, preferably about 10 to about 100 μm, preferably about 15 to about 50 μm, more preferably about 20 to about 40 μm, and even more preferably about 20 to about 30 μm. Different particle sizes can be obtained by controlling the droplet size during emulsification.
[0054] The beneficial drug delivery capsule may feature a core-to-shell ratio of up to 99:1, or even 99.5:1, based on weight.
[0055] Polyacrylic acid ester-based wall materials may include polyacrylic acid esters formed by alkyl and / or glycidyl esters of acrylic acid and / or methacrylic acid, polyacrylic acid esters formed by acrylic acid esters and / or methacrylic acid esters having a hydroxyl group and / or a carboxyl group and an allyl gluconamide, and mixtures thereof.
[0056] Aromatic alcohol-based wall materials may include aryloxyalkanols, arylalkanols, and oligoalkanol aryl ethers. They may also include aromatic compounds having at least one free hydroxyl group, and particularly preferably at least two directly aromatically bonded free hydroxyl groups, where the at least two free hydroxyl groups are preferably directly bonded to the aromatic ring, and more preferably at the meta position relative to each other. The aromatic alcohol is preferably selected from phenol, cresol (o-, m-, and p-cresol), naphthol (alpha- and beta-naphthol), and thymol, as well as ethylphenol, propylphenol, fluorophenol, and methoxyphenol.
[0057] The polyurea wall material may also contain polyisocyanate.
[0058] The polyvinyl alcohol-based wall material may contain crosslinked, hydrophobically modified polyvinyl alcohol, which contains a crosslinking agent comprising i) a first dextranaldehyde having a molecular weight of 2,000 to 50,000 Da, and ii) a second dextranaldehyde having a molecular weight of more than 50,000 to 2,000,000 Da.
[0059] The core of the beneficial agent delivery capsule of this disclosure may contain a partition modifier that can promote more robust shell formation. The partition modifier may be combined with the oleopropyl material of the core before the incorporation of the wall-forming monomer. The partition modifier may be present in the core at a concentration of about 5% to about 55% by weight, preferably about 10% to about 50% by weight, and more preferably about 25% to about 50% by weight of the core.
[0060] The partitioning modifier may include materials selected from the group consisting of vegetable oils, modified vegetable oils, mono-, di-, and tri-esters of C4-C24 fatty acids, isopropyl myristate, dodecanophenone, lauryl laurate, methyl behenate, methyl laurate, methyl palmitate, methyl stearate, and mixtures thereof. The partitioning modifier may preferably include isopropyl myristate, or more preferably consist of isopropyl myristate. The modified vegetable oil may be esterified and / or brominated. The modified vegetable oil may preferably include castor oil and / or soybean oil. U.S. Patent Application Publication No. 20110268802, incorporated herein by reference, describes other partitioning modifiers that may be useful in the beneficial agent delivery capsules described herein.
[0061] The fragrance delivery capsules may be coated with an adhesion aid, a cationic polymer, a nonionic polymer, anionic polymer, or a mixture thereof. Suitable polymers may be selected from the group consisting of polyvinyl formaldehyde, partially hydroxylated polyvinyl formaldehyde, polyvinylamine, polyethyleneimine, ethoxylated polyethyleneimine, polyvinyl alcohol, polyacrylate, and combinations thereof. The freshening composition may include beneficial agent delivery particles, one or more types of beneficial agent delivery capsules, for example, two types of beneficial agent delivery capsules, wherein one of the first or second beneficial agent delivery capsules has a wall made of a different wall material than the other; (b) a wall containing a different amount of wall material or monomer than the other; or (c) a different amount of fragrance oil component than the other; (d) a different fragrance oil; (e) a wall portion that is cured at a different temperature; (f) a fragrance oil having a different cLogP value; (g) a fragrance oil having a different volatility; (h) a fragrance oil having a different boiling point; (i) a wall portion made of a different weight ratio of wall material; (j) a wall portion that is cured at a different curing time; and (k) a wall portion that is heated at a different rate.
[0062] Preferably, the fragrance delivery capsule has a wall material containing an acrylic acid polymer or a derivative thereof, and a beneficial agent containing a fragrance mixture.
[0063] More preferably, the fragrance delivery capsule comprises a silica-containing wall material, such as the delivery capsule disclosed in U.S. Patent Application Publication No. 2020 / 0330949(A1), and a beneficial agent containing a fragrance mixture.
[0064] Neat fragrance ingredients water soluble solid Body composition The product may contain unencapsulated fragrances, each containing one or more fragrance ingredients that provide only a pleasurable effect (i.e., they do not neutralize malodors but provide a pleasant scent). Suitable fragrances are disclosed in U.S. Patent No. 6,248,135. For example, water soluble solid Body composition The product may contain a mixture of volatile aldehydes to neutralize malodors and fragrance aldehydes to produce pleasure.
[0065] aqueous phase Solid soluble composition mixture and water soluble solid Body composition The aqueous phase present in the product consists of an aqueous support made of water and other trace components, optionally including sodium chloride.
[0066] The aqueous phase may be present in the solid soluble composition mixture in an amount of about 65% to 95% by weight, about 65% to about 90% by weight, or about 65% to about 85% by weight of the rheological solid formed as an intermediate composition after the crystallization of the solid soluble composition mixture. The aqueous phase may be present in the solid soluble composition in an amount of 0% to about 10% by weight, 0% to about 9% by weight, 0% to about 8% by weight, or about 5% by weight of the intermediate rheological solid.
[0067] Sodium chloride in the aqueous phase solid solubility composition mixture may be present in amounts of 0% to about 10% by weight, 0% to about 5% by weight, and 0% to about 1% by weight. Sodium chloride in the aqueous phase solid solubility composition mixture may be present in amounts of 0% to about 50% by weight, 0% to about 25% by weight, and 0% to about 5% by weight. In embodiments, SDC may contain less than 2% by weight of sodium chloride to ensure humidity stability.
[0068] SDC Domain water soluble solid Body composition The product domain is as described herein. water soluble solid Body composition It is mainly composed of finished products.
[0069] In one embodiment, the SDC domain is present in less than about 13% by weight. In another embodiment, the SDC domain is present in about 10% by weight and less than 1% by weight of neat fragrance. In yet another embodiment, the SDC domain is present in about 8% to 2% by weight of neat fragrance, as exemplified in the examples as “beneficial agent% (dry)”.
[0070] In one embodiment, the SDC domain contains less than about 16% by weight. In another embodiment, the SDC domain contains about 15% by weight and less than 1% by weight of pigment capsules. In yet another embodiment, the SDC domain contains about 15% by weight and less than 2% by weight of fragrance. In yet another embodiment, the SDC domain contains about 15% to 5% by weight of fragrance capsules, as exemplified in the examples as "Freshness agent % (dry)".
[0071] PEGC domain Polyethylene glycol (PEG) material is a preferred carrier material for the non-porous soluble solid structure domain of the present invention. PEG material is generally relatively inexpensive, can be formed into many different shapes and sizes, is readily soluble in water, and liquefies at high temperatures. PEG material has a variety of molecular weights. In the consumer product compositions of the present invention, the PEG carrier material has a molecular weight of about 200 to about 50,000 daltons, preferably about 500 to about 20,000 daltons, preferably about 1,000 to about 15,000 daltons, preferably about 1,500 to about 12,000 daltons, or about 6,000 to about 10,000 daltons, and combinations thereof. Suitable PEG carrier materials include materials with a molecular weight of about 8,000 daltons, PEG materials with a molecular weight of about 400 daltons, PEG materials with a molecular weight of about 20,000 daltons, or mixtures thereof. Suitable PEG carrier materials are commercially available from BASF under the trade name PLURIOL, such as PLURIOL E 8000.
[0072] In one embodiment, PEGC is present in less than about 30% by weight. In another embodiment, the PEGC domain contains 15% to less than 1% by weight of neat fragrance. In another embodiment, the PEGC domain contains 12% to less than 2% by weight of neat fragrance. In yet another embodiment, the PEGC domain contains 12% to less than 5% by weight of neat fragrance. In yet another embodiment, the PEGC domain contains 10% to 2% by weight of neat fragrance, as exemplified in the examples as "freshness agent %".
[0073] In one embodiment, the PEGC domain contains less than about 2% by weight. In another embodiment, the PEGC domain contains 1.5% to 0.1% by weight of fragrance capsules. In yet another embodiment, the PEGC domain contains 1.25% to 0.2% by weight of fragrance capsules. In yet another embodiment, the PEGC domain contains 1.25% to 0.5% by weight of fragrance capsules, as exemplified in the examples as "freshness agent %".
[0074] particle The particle composition can be modified according to the need for a low-moisture composition.
[0075] As a non-limiting example, the particles consist of substantially one domain. In one embodiment, the freshness beneficial agent is a fragrance capsule dispersed in particles mainly composed of SDC. In another embodiment, the freshness beneficial agent is a neat fragrance dispersed in particles mainly composed of SDC. In one embodiment, the freshness beneficial agent is a fragrance capsule dispersed in particles mainly composed of PEGC. In another embodiment, the freshness beneficial agent is a neat fragrance dispersed in particles mainly composed of PEGC. In one embodiment, the freshness beneficial agent includes a fragrance capsule dispersed in particles mainly composed of SDC and a neat fragrance. In one embodiment, the freshness beneficial agent is a fragrance capsule dispersed in particles mainly composed of PEGC and a neat fragrance.
[0076] As a non-limiting example, particles consist of two or more domains. In these cases, the SDCs are small and completely encapsulated within the PEGC domains. In one embodiment, the freshness enhancer is a fragrance capsule dispersed in particles consisting mainly of SDC domains, dispersed in PEGC domains (Figure 7, Example 1). In another embodiment, the freshness enhancer is a fragrance capsule dispersed in particles consisting mainly of SDC domains, dispersed in PEGC domains containing neat fragrance. In yet another embodiment, the freshness enhancer is a neat fragrance dispersed in particles consisting mainly of SDC domains, dispersed in PEGC domains containing fragrance capsules. Typical particles contain less than about 50% by weight of SDC domains, in another embodiment about 45% to 10% by weight of SDC domains, in yet another embodiment about 40% to 15% by weight of SDC domains, and in yet another embodiment about 35% to 20% by weight of SDC domains.
[0077] As a non-limiting example, particles consist of two or more domains. In these cases, the particles have a core of a single SDC domain that is coated with a coating of PEGC domains and completely encapsulated. In one embodiment, the freshness enhancer is a fragrance capsule dispersed in particles consisting mainly of SDC domains, dispersed in PEGC domains (Figure 8, Example 2). In another embodiment, the freshness enhancer is a fragrance capsule dispersed in particles consisting mainly of SDC domains, dispersed in PEGC domains containing neat fragrance. In yet another embodiment, the freshness enhancer is a neat fragrance dispersed in particles consisting mainly of SDC domains, dispersed in PEGC domains containing fragrance capsules. Typical particles contain less than about 90% by weight of SDC domains, in another embodiment about 80% to 40% by weight of SDC domains, in yet another embodiment about 80% to 50% by weight of SDC domains, and in yet another embodiment about 50% to 35% by weight of SDC domains.
[0078] As a non-limiting example, particles are composed of two or more domains. In these cases, the particles have a core of PEGC domains with scattered SDC domains. In one embodiment, the freshness enhancer is a fragrance capsule dispersed in particles composed mainly of SDC domains, dispersed in PEGC domains (Figure 9, Example 3). In another embodiment, the freshness enhancer is a fragrance capsule dispersed in particles composed mainly of SDC domains, dispersed in PEGC domains containing neat fragrance. In yet another embodiment, the freshness enhancer is a neat fragrance dispersed in particles composed mainly of SDC domains, dispersed in PEGC domains containing fragrance capsules. Typical particles contain less than 25% by weight of SDC domains, in another embodiment about 20% to 2% by weight, and in yet another embodiment about 15% to 5% by weight of SDC domains.
[0079] As a non-limiting example, particles are composed of two or more domains. In these cases, the particles have one side containing PEGC domains and one side containing SDC domains. In one embodiment, the freshness enhancer is a fragrance capsule dispersed in particles mainly composed of SDC domains, dispersed in PEGC domains (Figure 10, Example 4). In another embodiment, the freshness enhancer is a fragrance capsule dispersed in particles mainly composed of SDC domains, dispersed in PEGC domains containing neat fragrance. In yet another embodiment, the freshness enhancer is a neat fragrance dispersed in particles mainly composed of SDC domains, dispersed in PEGC domains containing fragrance capsules. Typical particles contain about 75% to 25% by weight of SDC domains, in another embodiment 70% to 30% by weight of SDC domains, and in yet another embodiment 60% to 40% by weight of SDC domains.
[0080] In some embodiments, the particles of the low-moisture composition may have shapes including hemispheres, plates, cubes, cashews, gummy bears, tubes, and spheres. In another embodiment, the particles have a maximum dimension of 3 cm. In yet another embodiment, the particles have average weights of less than about 1,000 mg, about 750 mg to 1 mg, and about 500 mg to 5 mg.
[0081] low moisture composition The low-moisture composition consists of one or more particles and contains at least one SDC domain and at least one PEGC (Example 5).
[0082] When totaled across all particles, the SDC domains may represent approximately 10% to 90% by weight, or approximately 10% to 70% by weight, or approximately 30% to 90% by weight, or approximately 40% to 60% by weight of the low-moisture composition.
[0083] When totaled across all particles, the PEGC domains may amount to approximately 10% to 90% by weight, or approximately 10% to 70% by weight, or approximately 30% to 90% by weight, or approximately 40% to 60% by weight of the low-moisture composition.
[0084] consumer product compositions In one embodiment, the consumer product is added directly to the wash drum at the start of the wash cycle. In another embodiment, the consumer product is added to a fabric conditioner cup inside the washing machine. In yet another embodiment, the consumer product is added at the start of the wash cycle. In yet another embodiment, the consumer product is added during the wash cycle.
[0085] In one embodiment, the consumer product is sold in paper packaging for hydration and temperature stability of the composition. In one embodiment, the consumer product is sold in unit dose packaging. In one embodiment, the consumer product is sold in particles of different colors. In one embodiment, the consumer product is sold in small pouches. In one embodiment, the consumer product is sold in particles of different colors. In one embodiment, the consumer product is sold in a recyclable container.
[0086] Dissolution test method All samples and procedures are maintained at room temperature (25±3°C) before testing and placed in a desiccant chamber (0%RH) for 24 hours or until a constant weight is reached.
[0087] All dissolution measurements are performed at a controlled temperature and a constant stirring rate. A 600 mL jacketed beaker (Cole-Palmer, catalog no. UX-03773-30, or equivalent) is mounted and cooled to the desired temperature by circulating water through the jacketed beaker using a water circulator (Fisherbrand Isotemp 4100, or equivalent) set to the desired temperature. The jacketed beaker is placed in the center of the stirring element of a VWR Multi-Position Stirrer (VWR North American, West Chester, PA, USA catalog no. 12621-046). 100 mL of deionized water (MODEL 18MΩ, or equivalent) and a stirring rod (VWR, Spinbar, catalog no. 58947-106, or equivalent) are added to a second 150 mL beaker (VWR North American, West Chester, PA, USA catalog no. 58948-138, or equivalent). Place the second beaker into the jacketed beaker. Add enough Millipore water to the jacketed beaker so that the water level in the jacketed beaker is higher than that in the second beaker, taking great care to prevent the water in the jacketed beaker from mixing with the water in the second beaker. Set the stirring rod speed to 200 RPM, sufficient to generate a gentle vortex. The temperature is set to reach 25°C or 37°C in the second beaker using the flow from the water circulator, and the relevant temperature is reported in the example. Before conducting the dissolution experiment, measure the temperature in the second beaker with a thermometer.
[0088] All samples were sealed in a desiccator prepared with a fresh desiccant (VWR, Desiccant-Anhydrous Indicating Drierite, stock number 23001, or equivalent) until a certain weight was reached. All test samples had a mass of less than 15 mg.
[0089] A single dissolution experiment is performed by removing a single sample from the desiccator. The sample is weighed within one minute of being removed from the desiccator, and its initial mass (M I) is measured. The sample is dropped into the second beaker while stirring the sample. The sample is dissolved for 1 minute. At the end of 1 minute, the sample is carefully removed from the deionized water. The sample is placed back in the desiccator until a constant final mass is reached. The percentage of mass loss of the sample in a single experiment is M L = 100 * (M I - M F ) / M I and is calculated as follows.
[0090] Nine additional dissolution experiments are performed by first replacing 100 ml of water with fresh deionized water, adding a new sample from the desiccator for each experiment, and repeating the dissolution experiment described in the previous paragraph.
[0091] The average percent mass loss (M A ) for the test is calculated as the average percent mass loss for the 10 experiments, and the average standard deviation of the mass loss (SD A ) is the standard deviation of the average percent mass loss for the 10 experiments.
[0092] This method returns three values: 1) the average mass of the sample (M S ), 2) the temperature (T) at which the sample is dissolved, and 3) the average percent mass loss (M A ). If the method is not run on a sample, the method returns "NM" for all values. The average percent mass loss (M A ) and the average standard deviation of the average percent mass loss (SD A ) are used to plot the dissolution curves shared in Figures 4A, 4B, and 4C. [[ID=3&6]]
[0093] Humidity Test Method Using the humidity test method, the amount of water vapor sorption occurring in the composition is determined between drying at 0% RH and drying at various RHs at 25°C. In this method, a 10 - 60 mg sample is weighed, and the mass changes associated with being conditioned in different environmental states are captured with a dynamic vapor sorption instrument. The resulting mass gain is expressed as the percent change in mass per dry sample mass recorded at 0% RH.
[0094] This method utilizes an SPSx Vapor Sorption Analyzer (ProUmid GmbH&Co.KG, Ulm, Germany) with a resolution of 1 μg, or an equivalent dynamic vapor sorbent (DVS) instrument capable of controlling relative humidity (%RH) to within ±3%, temperature to within ±2°C, and measuring mass with an accuracy of ±0.001 mg.
[0095] Disperse 10-60 mg of the raw material or composition sample uniformly in a tare-filled 1-inch diameter aluminum pan. Place the aluminum pan containing the dispersed raw material or composition sample into a DVS instrument, set the DVS instrument to 25°C and 0%RH, and record the mass at that point with an accuracy of 0.001 mg or better every 15 minutes. After the sample has been in the DVS for at least 12 hours under these conditions and a constant weight has been achieved, record the mass of the sample m d The amount is recorded with an accuracy of 0.01 mg or higher. Once this step is complete, the instrument is advanced in 10% RH increments up to 90% RH. The sample is held in DVS for a minimum of 12 hours at each step, and the mass of the sample is measured m until a constant weight is reached. n The data is recorded with an accuracy of 0.001 mg or higher at each stage.
[0096] For a specific sample, constant weight can be defined as the change in continuous mass weighing that does not differ by more than 0.004%. For a specific sample, the change in mass % (%dm) per unit of dry sample mass is defined as follows:
[0097]
number
[0098] The percentage change in mass per unit of dry sample mass is reported in units of 0.01%.
[0099] Humidity stability at 80%RH means that the humidity level fluctuates by 5% or less at 80%RH. Lack of humidity stability at 80%RH means that the humidity level fluctuates by more than 5% at 80%.
[0100] Thermal stability test method All samples and procedures are maintained at room temperature (25±3°C) and at a relative humidity of 40±10% for 24 hours prior to testing.
[0101] In the thermal stability test method, differential scanning calorimetry (DSC) is performed on a 20 mg ± 10 mg sample of the sample composition. Simple scanning is performed between 25°C and 90°C, and the temperature at which the maximum peak is observed is considered the stable temperature and reported in the nearest °C.
[0102] The sample is filled into the DSC dish. All measurements are performed using a high-volume stainless steel dish set (TA part number 900825.902). The dish, lid, and gasket are weighed using a Mettler Toledo MT5 analytical microbalance (or equivalent, Mettler Toledo, LLC., Columbus, OH) to determine the tare weight. The sample is filled into the dish to a target weight of 20 mg (+ / - 10 mg) according to the manufacturer's specifications, taking care to ensure that the sample is in contact with the bottom of the dish. The dish is then sealed with a TA High Volume Die Set (TA part number 901608.905). The final assembly is weighed to obtain the weight of the sample. The sample is filled into a TA Q Series DSC (TA Instruments, New Castle, DE) according to the manufacturer's instructions. The DSC procedure uses the following settings: 1) Equilibrate at 25°C; 2) Mark the end of cycle 1; 3) Increase temperature to 90.00°C at 1.00°C / min; 4) Mark the end of cycle 3; then 5) End method; press Run.
[0103] Moisture Test Method All samples and procedures are maintained at room temperature (25±3°C) and at a relative humidity of 40±10% for 24 hours prior to testing.
[0104] The moisture content test method is used to quantify the weight percentage of water in a composition. In this method, Karl Fischer (KF) titration is performed on each of three similar samples of the sample composition. The titration is performed using a volumetric KF titrator and a one-component solvent system. The sample is 0.3 ± 0.05 g in mass and is dissolved in the titration vessel for 2.5 minutes before titration. The average (arithmetic mean) moisture content of the three test specimen replicas is reported in units of 0.1 wt% of the sample composition.
[0105] To measure the water content of the sample, a Mettler Toledo V30S Volumetric KF Titrator is used. The instrument is equipped with Honeywell Fluka Hydraanal Solvent (catalog no. 34800-1L-US) for dissolving the sample, Honeywell Fluka Hydraanal Titrant-5 (catalog no. 34801-1L-US) for titrating the sample, and three drying tubes (titration bottle, solvent bottle, and waste bottle) filled with Honeywell Fluka Hydraanal Molecular sieve 3nm (catalog no. 34241-250g) to preserve the effectiveness of the anhydrous material.
[0106] The method used to measure the samples was type "KF vol", ID "U8000", and title "KFVol 2-comp 5", each having eight lines in which the method functions.
[0107] Line 1 title has the following selected elements: Type is set to Karl Fischer Titration Vol.; Compatibility is set to V10S / V20S / V30S / T5 / T7 / T9; ID is set to U8000; Title is set to KFVol 2-comp 5; Author is set to Administrator; Date and time are defined along with Modified on and Modified by when the method was created; Protection is set to no and SOP is set to None.
[0108] Line 2 samples have two options: sample and concentration. When the sample option is selected, the following fields are defined as follows: Set the number of IDs to 1. Set ID1 to -- and select entry type as weight. Set the lower limit to 0.0 g. Set the upper limit to 5.0 g. Set the density to 1.0 g / mL. Set the correction factor to 1.0. Set the temperature to 25.0 °C. Select auto start and set entry as after addition. When the concentration option is selected, the following fields are defined as follows: Select titrator to KF 2-comp 5. Set nominal concentration to 5 mg / mL. Select standard to water-standard 10.0. Select entry type as weight. Set the lower limit to 0.0 g. Set the upper limit to 2.0 g. Set the temperature to 25.0 °C. Set the mixing time to 10 seconds. Auto start is selected. Select entry as after addition. The lower limit of the concentration is set at 4.5 mg / mL, and the upper limit of the concentration is set at 5.6 mg / mL.
[0109] Line 3, the titration stand (KF stand), has fields defined as follows: Set the type to KF stand. Select the titration stand to KF stand. Select the drift source to online. Set the maximum starting drift to 25.0 μg / min.
[0110] Line 4 mixing time has a field defined as follows: set the duration to 150 seconds.
[0111] Line 5 titration (KF volume)[1] has six options: titrant, sensor, agitation, pre-distribution, control, and termination. When the titrant option is selected, the following fields are defined as follows: Select titrant to KF 2-comp 5. Set nominal concentration to 5 mg / mL and reagent type to 2-comp. When the sensor option is selected, the following fields are defined as follows: Set type to polarized. Select sensor to DM143-SC. Set unit to mV. Set indication to voltammetry and Ipol to 24.0 μA. When the agitation option is selected, the following fields are defined as follows: Set speed to 50%. When the pre-distribution option is selected, the following fields are defined as follows: Select mode to None. Set wait time to 0 seconds. When the control option is selected, the following fields are defined as follows: Set endpoint to 100.00 mV. Set control band to 400.00 mV. Set the maximum infusion rate to 3 mL / min. Set the infusion rate (minutes) to 100 μL / min and select Start successfully. When the End option is selected, the following fields are defined as follows: Select Type as Drift Stop Relative. Set Drift to 15.0 μg / min. Vmax is 15 mL; Minimum time is set to 0 seconds and maximum time is set to ∞ seconds.
[0112] The calculation on line 6 has fields defined as follows: The result type is selected as predefined. Set the result to content. Set the result unit to %. Set the expression to R1=(VEQ * CONC-TIME * Set D...). Set the constant C to 0.1. Set the decimal part to 2. Do not select result limits. Select record statistics. Do not select extra statistical functions.
[0113] Line 7 recording has fields defined as follows: Select Result No. Select Raw Result No. Select Table of Measurements No. Select Sample Data No. Select Resource Data No. Select EV No. Select Et No. Select Vt No. Select H2O-t No. Select Drift-t No. Select H2O-t&Drift-t No. Select Vt&Drift-t No. Select Method No., Select Series Data No.
[0114] The end of line 8 of the sample has a field defined as follows: Select Open Series.
[0115] Once a method is selected, pressing Start defines the following fields: Set Type to Method. Set Method ID to U8000. Set Sample Quantity to 1. Set ID1 to -- and Sample Size to 0g. Press the Start option again. The instrument measures the maximum drift and, once steady state is reached, allows the user to select sample addition. At this point, the user adds the 3-hole adapter, removes the stopper, places the sample in the titration beaker, replaces the 3-hole adapter and stopper, and enters the sample mass in grams on the touchscreen. The reported value is the weight percentage of water in the sample. Repeat this measurement three times for each sample and report the average of the three measurements.
[0116] Fiber testing methods The fiber testing method is: water soluble solid Body composition This is used to determine whether the product crystallizes under process conditions and whether it contains fibrous crystals. A simple definition of a fiber is "a thread or a thread-like structure or object." Fibers have a long length in only one direction (e.g., Figures 1A and 1B). This is different from other crystalline forms such as plates or lamellae that have long lengths in two or more directions (Figures 11A and 11B). Having DCS as a fiber. water soluble solid Body composition Only the finished product is within the scope of this invention. Those skilled in the art will know that if present in the same particles, water soluble solid Body composition Recognizes SDC domains from PEGC domains in the finished product.
[0117] A sample approximately 4 mm in diameter is placed on an SEM sample shuttle and stub (Quorum Technologies, AL200077B and E7406) having a pre-coated slit containing a 1:1 mixture of Scigen Tissue Plus optimal cutting temperature (OCT) compound (Scigen 4586) and colloidal graphite (agar scientific G303E). The placed sample is plunge-frozen in a liquid nitrogen slush bath. Next, the frozen sample is inserted into a Quorum PP 3010 Tcryo prep chamber (Quorum Technologies PP3010T) or equivalent and equilibrated to -120°C before freeze-fracturing. Freeze-fracturing is performed by cutting off the top of the vitreous sample using a cryogenic built-in knife in the cryoprep chamber. Additional sublimation is performed at -90°C for 5 minutes to remove any residual ice on the sample surface. The sample is further cooled to -150°C and sputter-coated with a Pt layer that is present in the cryo-prep chamber for 60 seconds to reduce static charge.
[0118] High-resolution imaging is performed using a Hitachi Ethos NX5000 FIB-SEM (Hitachi NX5000) or an equivalent device.
[0119] To determine the fibrous morphology of the sample, imaging is performed at a magnification of 20,000x. At this magnification, individual crystals of the crystallizing agent can be observed. The magnification may be slightly adjusted to a lower or higher value until individual crystals are observed. Those skilled in the art can evaluate the longest dimension of a representative crystal in the image. If this longest dimension is about 10 times or more the other orthogonal dimensions of the crystal, these crystals are considered fibers and are within the scope of the present invention. [Examples]
[0120] These examples have a mesh microstructure formed from a dry sodium fatty acid carboxylate formulation. water solublesolid Body composition This provides non-limiting examples of low-moisture compositions comprising a product (SDC) domain, a polyethylene glycol (PEGC) domain, and activators dispersed within these domains, such as freshness-enhancing agents that deliver exceptional freshness to fabrics.
[0121] The composition of the present invention represents particles containing an SDC domain that, when properly processed, forms a fibrous mesh that dissolves completely within a washing cycle, and which contains a crystallizing agent. The composition of the present invention also represents a PEGC domain that, when used in combination with the SDC domain, creates a unique low-moisture composition that is easy to process and provides distinctive aesthetic properties and improved freshness performance.
[0122] The freshness enhancer takes the form of a fragrance capsule and / or neat fragrance distributed to different domains. Example 1 demonstrates a particle consisting of two or more domains in which the SDC domain is small and completely encapsulated within a single PEGC domain (Figure 7). Example 2 demonstrates a particle consisting of two or more domains in which a single SDC domain is coated and completely encapsulated within the coating of the PEGC domain (Figure 8). Example 3 shows a particle consisting of two or more domains in which the particle has a PEGC domain core and SDC domains are scattered (Figure 9). Example 4 demonstrates a particle consisting of two or more domains in which the particle has one side containing a PEGC domain and one side containing an SDC domain (Figure 10). Example 5 proposes a low-moisture composition consisting of a physical mixture of two or more different types of particles and a freshness enhancer, wherein some of the particles are structured as described in Examples 1-4. Example 6 is neutralized and blended with PEGC water soluble solid Body composition This suggests specific blends of fatty acid materials used to manufacture the product, and compositions prepared from fragrance capsules having different wall structures.
[0123] The data in Tables 1 to 8 provides parameters related to the particles in the following manner. Preparation of SDC Domains - All weights listed in this part of the table correspond to the amounts added to prepare the solid soluble composition mixture (SDCM). "Freshness Agent % (Dry)" is the weight percentage of freshness agent remaining in the SDC after drying, assuming no residual water as determined by the moisture content test method. "Retardant CA %" is the weight percentage of NaC12 (slow dissolution) in a mixture of NaC12 and NaC10 and NaC8 (fast dissolution).
[0124] All SDC domains are prepared through three fabrication steps to ensure the formation of a fibrous mesh within the domain. 1. Mix the crystallizing agents completely in water to form SDCM, and optionally add the activator. 2. Formation - The composition from the mixing step is formed to the desired SDC size and dimensions by techniques including crystallization. 3. Drying - The amount of water is reduced to ensure desired performance, including solubility, hydration, and thermal stability, and an activator is optionally added.
[0125] Preparation of PEGC Domains - All weights listed in this part of the table correspond to the amounts of PEG and freshness agent added to prepare the PEGCs. Any water added to the domains by inclusion in the flavor capsule slurry is not removed and remains as part of the domains when combined to form a low-moisture composition.
[0126] Low Moisture Compositions - All weights listed in this section correspond to the amounts of SDC and PEGC combined to produce low moisture composition particles. For clarity, the percentages of the components of the low moisture composition are given as follows: "CA%" = crystallizer from SDC in the final low moisture composition, "Fragrance Capsules%" = fragrance capsules in the final low moisture composition, "Fragrance%" = neat fragrance in the low moisture composition, "PEG%" = PEG in the low moisture composition, and "Water%" = water in the low moisture composition, including water not removed from PEGC. Finally, "Average Mass" = the average mass of particles produced as described in each example of the low moisture composition.
[0127] The data in Tables 9-10 provide predictive particles composed solely of SDC and PEGC domains, the former having different blends of crystallizers and freshness enhancers, and the latter having PEG and freshness enhancers of different molecular weights.
[0128] The data in Tables 11-12 provide predictive low-moisture compositions containing a physical mixture of particles having SDC domains, PEGC domains, and freshness-enhancing agents. The "Amount of Fragrance Capsules During Washing" is the amount of fragrance capsules during washing to deliver the desired dry fabric feel effect to the consumer. The "Amount of Neat Capsules During Washing" is the amount of neat fragrance during washing to deliver the desired wet fabric feel effect to the consumer. The @ symbol displayed with the particles identifies the mass of the particles in the low-moisture composition. "Amount of Composition" is the total amount of all particles in the low-moisture composition, which the consumer adds to the washing solution.
[0129] The data in Table 13 provide a predictive low-moisture composition comprising an SDC domain prepared from a mixture of C8, C10, and C12 long-chain fatty acids that are neutralized to produce an SDC domain, and then combined with a PEGC domain and a flavor capsule having a different wall structure.
[0130] material (1) Water: Millipore, Burlington, MA (18m-ohm resistance) (2) Capri Ru Sodium octanoate (NaC8): TCI Chemicals, catalog number 00034 (3) Sodium caprate (sodium decanoate, NaC10): TCI Chemicals, catalog number D0024 (4) Sodium laurate (sodium dodecanoate, NaC12): TCI Chemicals, catalog number L0016 (5) Fragrance capsule slurry: Encapsys, enclosed fragrance #1, melamine formaldehyde wall chemical reaction (31% activity) (6) Fragrance capsule slurry: Encapssys, encapsulated fragrance #2, urea wall chemical action, (21% activity) (7) PEG-6000gmol -1 Alfa Aesar, product code A17541.30. (8) PEG-8000gmol -1 Alpha Aesar, product code 43443. (9) PEG-9000 gmol -1 Dow Chemical, product code C4633240. (10) PEG-10,000 gmol -1 Alfa Aesar, product code B21955.30. (11) Neat Fragrance: International Flavors and Fragrances, Neat Fragrance Oil #1 (12) Fatty acid blend: C810L, Procter & Gamble Chemicals, Sample code: SR26399 (13) Lauric acid: Peter Cremer, Catalog No. FA-1299, Lauric acid (14) Sodium hydroxide (50% by weight solution): Fisher Scientific, catalog number SS254-4 (15) Fragrance capsule slurry: Encapssys, encapsulated fragrance #3, polyacrylate wall chemical action, 21% by weight active (16) Fragrance capsule slurry: Encapssys, encapsulated fragrance #4, high core-to-wall ratio, polyacrylate wall chemical action (17) Encapsulated fragrance #5, polyurea wall chemical action, 32% by weight active (18) Fragrance capsule slurry: Encapssys, encapsulated fragrance #6, polyacrylate wall chemistry, 6.2% by weight activity
[0131] (Example 1) Example 1 demonstrates a particle composed of two or more domains in which the SDC domain is completely encapsulated within a single PEGC domain (Figure 7).
[0132] This embodiment demonstrates a composition that allows for the adjustment of the amount and distribution of different freshness beneficial agents using different domains within a single particle. In this non-limiting example, SDC domains are dispersed within a continuous domain of PEGC. This offers several advantages. First, SDC domains offer the opportunity to increase the amount of fragrance capsules in the particle (e.g., about 18% by weight) compared to a single PEGC domain (e.g., about 1.2% by weight). Second, these particles improve the aesthetics of the particles by maintaining the "smooth" appearance from PEGC. Third, such compositions offer advantages in manufacturing, as the flow properties of the "molten" composition are similar to those of the whole PEG composition, and these composite compositions offer the possibility of being prepared using existing commercially available equipment. Samples AA to AI are non-limiting examples of possible different domain compositions and weight ratios in the resulting particles that can be used as low-moisture compositions.
[0133] Preparation of the SDC domain Mixing - A 250 ml stainless steel beaker (Thermo Fisher Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7CER Hotplate, catalog number NO97042-690). Water (Milli-Q Academic) and a crystallizing agent were added to the beaker. A temperature probe was placed in the composition. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled and adjusted. Made An impeller was placed in the material. The heater was set to 80°C and the impeller was set to rotate at 250 rpm, and the composition was heated to 80°C until all the crystallizing agent was solubilized and the composition became transparent. Then, MadeThe mixture was poured into a Max100 Mid Cup (Speed Mixer), covered, and allowed to cool to 25°C. As specified in the table, the freshness enhancer was added by mixing the prepared mixture in a Speedmixer (Flack Tek.Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes.
[0134] Formation - The preparation was poured onto aluminum foil to a uniform thickness of approximately 1 mm. The preparation was then placed in a refrigerator (VWR Door Solid Lock F Refrigerator 115V, 76300-508, or equivalent) equilibrated at 4°C for 8 hours to allow the crystallizing agent to crystallize.
[0135] Drying - The compositions were dried for an additional 8 hours in a convection oven (Yamato, DKN400, or equivalent) set to 25°C, passing a steady flow of air through them. The final SDC was confirmed to have a moisture content of less than 10% by a moisture content test method. The domains were either in the shape of a mold or flat sheets were crushed into coarse pieces approximately 1 mm x 1 mm in size.
[0136] Preparation of PEGC domains Separately, a 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7CER Hotplate, catalog number NO97042-690). PEG (materials 8-11) was added to the beaker. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. A temperature probe was also placed in the preparation. The impeller was set to rotate at 250 rpm. The preparation was heated to 100°C until the PEG was completely melted. As specified in the table, a freshness enhancer was added by placing the preparation in a Speedmixer (Flack Tek. Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes. Using this preparation, a low-moisture composition was prepared within 5 minutes of reaching the final temperature.
[0137] Preparation of low-moisture compositions A 60 ml Speed Mixer cup and cap were weighed. The cap was removed, and the SDC domain was added to the cup. The cup was resealed with the cap and weighed again. The mass of the SDC domain in the preparation was the difference in weight.
[0138] A second 60 ml Speed Mixer cup and cap were weighed. The cap was removed, and the freshness enhancer was added to the cup. The cup was resealed with the cap and weighed again, where the mass of the freshness enhancer in the preparation is the difference in weight. The cap was removed from the cup once more.
[0139] Less than 30 seconds later, PEGC was added to the cup, the cap was replaced, and the entire preparation was reweighed. The mass of PEGC in the preparation was the difference in weight. The cup was placed in a Speedmixer, started, and the preparation was mixed at 3000 RPM for 1 minute. Less than 30 seconds after mixing (and before crystallization), the preparation was transferred to a polymer mold patterned with 5 mm diameter hemispheres. The preparation was cooled at 25°C for at least 30 minutes. A diagram of the particle structure in this low-moisture composition is shown in Figure 7.
[0140] [Table 1]
[0141] [Table 2]
[0142] [Table 3]
[0143] (Example 2) Example 2 demonstrates particles consisting of two or more domains, each coated with a single SDC domain and completely encapsulated within a PEGC domain coating (Figure 8).
[0144] This embodiment demonstrates that the composition has particles having an SDC domain core and a PEGC coating. In this non-limiting example, a single SDC domain is encapsulated within a continuous domain of PEGC. This offers several advantages. These particles offer the opportunity to increase the amount of fragrance capsules in the SDC domain (e.g., about 18% by weight) compared to the amount in the SDC domain (e.g., about 1.3% by weight). The particles increase the freshness beneficial agent capacity by about 10 times. The SDC domain is also about 50-70% lower in density, making the particles (and the resulting low-moisture composition) more favorable for different commercial methods such as e-commerce, making them more sustainable with less carrier than required for unit freshness, and sustainably replacing petroleum-based PEG with a natural crystallizer. Furthermore, the use of the PEGC coating allows the particles to maintain the "smooth" or glossy appearance of the PEGC domain, which is appreciated by many consumers. Samples BA-BI are non-limiting examples of possible different domain compositions and weight ratios in the resulting particles.
[0145] Preparation of the SDC domain Mixing - A 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7 CER Hotplate, catalog number NO97042-690). Water (Milli-Q Academic) and crystallizer were added to the beaker. A temperature probe was placed in the composition. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. The heater was set to 80°C and the impeller was set to rotate at 250 rpm, and the composition was heated to 80°C until all the crystallizer was solubilized and the composition became clear. The mixture was then poured into a Max100 Mid Cup (Speed Mixer), covered, and allowed to cool to 25°C. As specified in the table, the freshness-enhancing agent was added by placing the preparation in a Speedmixer (Flack Tek.Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes.
[0146] Formed - The prepared material was transferred to a polymer mold patterned with hemispheres 5 mm in diameter. The mold was then placed in a refrigerator (VWR Door Solid Lock F Refrigerator 115V, 76300-508, or equivalent) equilibrated at 4°C for 8 hours to allow the crystallizing agent to crystallize.
[0147] Drying - The compositions were dried for an additional 8 hours in a convection oven (Yamato, DKN400, or equivalent) set to 25°C, passing a steady flow of air through them. The final SDC was confirmed to have a moisture content of less than 10% by a moisture content test method.
[0148] Preparation of PEGC domains Separately, a 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7 CER Hotplate, catalog number NO97042-690). PEG (materials 8-11) was added to the beaker. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. A temperature probe was also placed in the preparation. The impeller was set to rotate at 250 rpm. The preparation was heated to 100°C until the PEG was completely melted. As specified in the table, a freshness enhancer was added by placing the preparation in a Speedmixer (Flack Tek. Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes. Using this preparation, a low-moisture composition was prepared within 5 minutes of reaching the final temperature.
[0149] Preparation of low-moisture compositions The weight of the weighing dish was measured. SDC was placed in the weighing dish, and the weight of the SDC was determined by the difference in mass. The SDC was immersed in PEGC molten material. Excess PEGC was wiped off the surface of the SDC. The preparation was placed in the weighing dish. The preparation was cooled at 25°C for at least 30 minutes. The weight of the weighing dish was measured, and the weight of the fragrance was determined by the difference in weight. A diagram of the particle structure in this low-moisture composition is shown in Figure 8.
[0150] [Table 4]
[0151] [Table 5]
[0152] [Table 6]
[0153] (Example 3) Example 3 shows a particle in which the particle has a PEGC domain core and is composed of two or more domains in which SDC domains are scattered (Figure 9).
[0154] Such particles offer, for example, the opportunity for particles to have significant amounts of PEGC and SDC domains, independent of the solubility characteristics of each domain. In non-limiting samples CA and CB, fragrance capsules are placed in SDC domains and released into a washing cycle at a rate consistent with the composition of the crystallizer blend, while neat fragrance is placed in PEGC domains and released into a washing cycle at a rate consistent with the molecular weight of PEG. The solubility percentage determined by the solubility test method is, here, independent of different domains, in contrast to the particles described in Example 1, for example. Furthermore, such forms are aesthetically advantageous to consumers, as the fixed domains exhibit different functions within the particles. Moreover, such forms are easily commercially prepared, for example, by passing warm PEGC domains through a "spray" of SDC domain particles that can adhere to the surface of the domains.
[0155] Preparation of the SDC domain Mixing - A 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7 CER Hotplate, catalog number NO97042-690). Water (Milli-Q Academic) and crystallizer were added to the beaker. A temperature probe was placed in the composition. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. The heater was set to 80°C and the impeller was set to rotate at 250 rpm, and the composition was heated to 80°C until all the crystallizer was solubilized and the composition became clear. The mixture was then poured into a Max100 Mid Cup (Speed Mixer), covered, and allowed to cool to 25°C. As specified in the table, the freshness-enhancing agent was added by placing the preparation in a Speedmixer (Flack Tek.Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes.
[0156] Formation - The preparation was poured onto aluminum foil to a uniform thickness of approximately 1 mm. The preparation was then placed in a refrigerator (VWR Door Solid Lock F Refrigerator 115V, 76300-508, or equivalent) equilibrated at 4°C for 8 hours to allow the crystallizing agent to crystallize.
[0157] Drying - The compositions were dried for a further 8 hours in a convection oven (Yamato, DKN400, or equivalent) set to 25°C, passing a steady flow of air through them. The final SDC was confirmed to have a moisture content of less than 10% by a moisture content test method. The flat sheets were crushed into coarse pieces approximately 1 mm x 1 mm in size.
[0158] Preparation of PEGC domains Separately, a 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7 CER Hotplate, catalog number NO97042-690). PEG (materials 8-11) was added to the beaker. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. A temperature probe was also placed in the preparation. The impeller was set to rotate at 250 rpm. The preparation was heated to 100°C until the PEG was completely melted. As specified in the table, a freshness enhancer was added by placing the preparation in a Speedmixer (Flack Tek. Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes. Using this preparation, a low-moisture composition was prepared within 5 minutes of reaching the final temperature.
[0159] Preparation of low-moisture compositions A small amount of PEGC was placed in a weighing dish and weighed. A small amount of SDC was gently sprinkled onto the PEGC before significant crystallization occurred (within 30 seconds). Small-sized SDC domains adhered to the surface of the PEGC domains as the material crystallized. The preparation was cooled at 25°C for at least 30 minutes. The resulting particles were removed from the mold and reweighed to determine the aggregated amount of SDC. A diagram of the particle structure in this low-moisture composition is shown in Figure 9.
[0160] [Table 7]
[0161] (Example 4) Example 4 demonstrates a particle composed of two or more domains, with one side containing a PEGC domain and the other side containing an SDC domain (Figure 10).
[0162] Such particles also offer the opportunity to independently possess the solubility properties of each domain, for example, particles having significant amounts of PEGC and SDC domains. In the non-limiting examples of samples DA and DB, the fragrance capsule is placed in the SDC domain and released into a washing cycle at a rate consistent with the composition of the crystallizer blend, and the neat fragrance is placed in the PEGC domain and released into a washing cycle at a rate consistent with the molecular weight of PEG. The solubility percentage determined by the solubility test method is not dependent on different domains, here in contrast to the particles described in Example 1, for example. Furthermore, such a form does not impose limitations on the absolute amount of SDC and PEGC domains in the particles, compared to Example 3.
[0163] Preparation of the SDC domain Mixing - A 250 ml stainless steel beaker (Thermo Fisher Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7CER Hotplate, catalog number NO97042-690). Water (Milli-Q Academic) and a crystallizer were added to the beaker. A temperature probe was placed in the composition. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the preparation. The heater was set to 80°C and the impeller was set to rotate at 250 rpm, and the composition was heated to 80°C until all the crystallizer was solubilized and the composition became clear. The preparation was then poured into a Max100 Mid Cup (Speed Mixer), covered, and allowed to cool to 25°C. As specified in the table, the freshness-enhancing agent was added by placing the preparation in a Speedmixer (Flack Tek.Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes.
[0164] Formed - The prepared material was transferred to a polymer mold patterned with hemispheres 5 mm in diameter. The mold was then placed in a refrigerator (VWR Door Solid Lock F Refrigerator 115V, 76300-508, or equivalent) equilibrated at 4°C for 8 hours to allow the crystallizing agent to crystallize.
[0165] Drying - The compositions were dried for a further 8 hours in a convection oven (Yamato, DKN400, or equivalent) set to 25°C, passing a steady flow of air through them. Once completely dry, the preparations were removed from the molds. The final SDC was confirmed to have a moisture content of less than 10% by a moisture content test method.
[0166] Preparation of PEGC domains Separately, a 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7 CER Hotplate, catalog number NO97042-690). PEG (materials 8-11) was added to the beaker. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. A temperature probe was also placed in the preparation. The impeller was set to rotate at 250 rpm. The preparation was heated to 100°C until the PEG was completely melted. A freshness enhancer was added by placing the preparation in a Speedmixer (Flack Tek. Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes, as specified in the table. Using this preparation, a low-moisture composition was prepared within 5 minutes after reaching the final temperature. The preparation was transferred to a polymer mold patterned with hemispheres 5 mm in diameter.
[0167] Preparation of low-moisture compositions Within 30 seconds of placing the preparation in the mold, the domains of SDC were placed on the liquid PEGC, and the flat surface of SDC was placed on the flat surface of PEGC. The preparation was cooled at 25°C for at least 30 minutes. After complete cooling, the low-moisture composition was removed from the mold. The two domains were fixed, and the resulting particles were spherical as shown in Figure 10.
[0168] [Table 8]
[0169] (Example 5) Example 5 demonstrates a low-moisture composition comprising two or more different particles, the particles may contain a combination of SDC and PEGC domains as described in the previous examples, or they may contain only a single SDC and PEGC domain together with a freshness-enhancing agent. These non-limiting examples describe the latter. However, it is understood that physical blends of such particles for producing a low-moisture composition may also include the former.
[0170] Particle composition samples EA to EH (Tables 9 and 10) represent viable particle compositions containing a single SDC or PEGC domain. Samples EI to EQ (Tables 11 and 12) represent the low-moisture compositions of the present invention, composed of the particle compositions. The type and amount of particles in the low-moisture compositions are expressed as “composition dose,” or a typical amount used by a consumer in a single wash. When determining the dose, many considerations are important, including the amount of “fragrance capsules during washing” and the amount of “neat fragrance during washing” added by the dose. However, other factors, such as the selection of SDC or PEGC domain compositions, are also important in determining the level of freshness benefit. For example, consumers may prefer a very long-lasting freshness on dry fabric, which may require a dose of about 5 to 10 grams of fragrance capsules during washing, or they may prefer only an initial burst of freshness upon friction, which may require a dose of about 0.5 to 2 grams of fragrance capsules during washing. For example, consumers may prefer an extremely "instantaneous" freshness when removing a damp cloth from a detergent solution that may require approximately 5-10 grams of neat fragrance, or they may prefer a subtly pleasant lingering freshness when removing a damp cloth from a detergent solution that may require only approximately 1-2 grams of pure fragrance. These freshness profiles are further influenced by the dissolution rate of the domains containing the freshness-enhancing agents. Finally, the selection of particles constituting a low-moisture composition is also influenced by commercial considerations. Often, it is more commercially viable to produce two types of particles and physically mix them in different ratios, rather than a special process for each consumer, to allow the composition to reach all consumer preferences. This is often referred to as "delayed product differentiation." Some consumers may prefer doses containing a large amount of composition, around 50-100 grams, while some e-consumers or sustainability-conscious consumers may prefer a more concentrated, compact dose of around 10-20 grams. Ultimately, these examples offer a variety of freshness performances and commercial opportunities.
[0171] [Table 9] * Prepared from fragrance capsule slurry materials 5 and 6.
[0172] [Table 10] * Prepared from fragrance capsule slurry materials 5 and 6.
[0173] [Table 11]
[0174] [Table 12]
[0175] (Example 6) Example 6 is neutralized with an SDC composition and blended with a PEGC composition so that the SDC (e.g., Figures 4A, 4B, and 4C) and PEGC domains have different dissolution rate profiles. water soluble solid Body composition We propose that compositions prepared from specific blends of fatty acid materials that produce the product allow for different sequences of active substances within each domain at specific times in the washing cycle. The dissolution rate of SDC is influenced by the percentage of slow crystallizing agent (delayed CA%), with high concentrations of SDC (e.g., sample EU) dissolving more slowly than low concentrations of SDC (e.g., sample ER). The absolute dissolution rates at different temperatures are determined by dissolution test methods. The dissolution rate of PEGC is influenced by the molecular weight of PEG, thereby causing sample ER (e.g., PEG10,000) to dissolve more slowly than sample ES (e.g., PEG8,000), and sample ES to dissolve more slowly than sample ET and sample EU (e.g., PEGPEG 6,000). The absolute dissolution rates at different temperatures are determined by dissolution test methods.
[0176] Preparation of the SDC domain Mixing - A 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7CER Hotplate, catalog number NO97042-690). Water (Milli-Q Academic) and a crystallizer were added to the beaker. A temperature probe was placed in the composition. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. The heater was set to 80°C and the impeller was set to rotate at 250 rpm, and the composition was heated to 80°C until all the crystallizer was solubilized and the composition became clear.
[0177] Formation - The composition was then poured into a Max100 Mid Cup, covered, and allowed to cool to 25°C. A freshness enhancer was added by placing the preparation in a Speedmixer (Flack Tek.Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes, as specified in the table. In non-limiting examples, the preparation was transferred to a polymer mold patterned with hemispheres of 5 mm in diameter. In another non-limiting example, the preparation was sprayed through an orifice to produce small droplets. The size and shape of the DSC domains were formed to satisfy the final structure of the final low-moisture composition (e.g., Figures 7, 8, 9, and 10). The mold was then placed in a refrigerator (VWR Door Solid Lock F Refrigerator 115V, 76300-508, or equivalent) equilibrated at 4°C for 8 hours to crystallize the crystallizer.
[0178] Drying - The prepared material was placed in a convection oven (Yamato, DKN400, or equivalent) set to 25°C for a further 8 hours, passing a steady flow of air through it to dry the composition. Once completely dry, the prepared material was removed from the mold. The final SDC was confirmed to have a moisture content of less than 10% by a moisture content test method.
[0179] Preparation of PEGC domains Separately, a 250 ml stainless steel beaker (Thermo Fischer Scientific, Waltham, MA) was placed on a hot plate (VWR, Radnor, PA, 7×7 CER Hotplate, catalog number NO97042-690). PEG (materials 8-11) was added to the beaker. An overhead mixer (IKA Works Inc, Wilmington, NC, model RW20 DMZ) and a mixing device including a 3-blade impeller design were assembled, and the impeller was placed in the composition. A temperature probe was also placed in the preparation. The impeller was set to rotate at 250 rpm. The preparation was heated to 100°C until the PEG was completely melted. As specified in the table, a freshness enhancer was added by placing the preparation in a Speedmixer (Flack Tek. Inc, Landrum, SC, model DAC 150.1 FVZ-K) at 3000 rpm for 3 minutes. In non-limiting examples, the preparation was used to produce a low-moisture composition within 5 minutes of reaching the final temperature. In non-limiting examples, the preparation was transferred to a polymer mold patterned with hemispheres of 5 mm in diameter. The size and shape of the DSC domains were formed to satisfy the final structure of the final low-moisture composition (e.g., Figures 7, 8, 9, and 10).
[0180] Preparation of low-moisture compositions Sample ER(5mg)-SDC composition is sprayed as droplets onto a flat sheet, crystallized, and dried. PEGC is sprayed onto a flat sheet and crystallized. Two flat ends are combined to create low-moisture composition particles (e.g., Figure 10). Sample ES(5mg)-SDC composition is sprayed as droplets onto a flat sheet, crystallized, and dried. PEGC is sprayed onto the surface of the SDC composition and crystallized. The low-moisture composition is coated particles (e.g., Figure 8). Sample ET(500mg)-PEGC composition is placed on a flat sheet as a large droplet, crystallized, and dried. SDC is sprayed to generate fine granules, which adhere to the surface of the large droplet. The low-moisture composition is sugar gum droplet-like particles (e.g., Figure 9). Sample EU(500mg)-SDC composition is spray-dried small particles. Small SDC particles are added to the PEGC molten material, and larger droplets are placed on a flat surface to crystallize. The low-moisture composition encapsulates the SDC (e.g., Figure 7).
[0181] In non-limiting cases, the final low-moisture composition for the washing process may contain particles comprising one of the multiple particle combinations described in Sample ER, Sample ES, Sample ET, and Sample EU.
[0182] [Table 13]
[0183] The dimensions and values disclosed herein should not be understood as being strictly limited to the exact numerical values listed. Instead, unless otherwise specified, each such dimension is intended to mean both the listed value and the functionally equivalent range encompassing that value. For example, a dimension disclosed as "40 mm" is intended to mean "approximately 40 mm."
[0184] All documents referenced herein, including any patents or patent applications that are cross-referenced or related, and any patent applications or patents on which this application claims priority or benefit thereof, are incorporated herein by reference in their entirety unless explicitly stated to be excluded or limited. No reference to any document shall be deemed prior art to any invention disclosed or claimed herein, nor shall it be deemed to teach, suggest or disclose any such invention, either alone or in combination with any other reference. Furthermore, if any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in any document incorporated by reference, the meaning or definition given to the term in this document shall apply.
[0185] While specific embodiments of the present 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. Therefore, it is intended that all such changes and modifications within the scope of the invention be covered in the appended claims. [1] A low-moisture composition, 1) At least one solid solubility composition (SDC) domain having a crystallizing agent, 2) At least one polyethylene glycol (PEGC) domain, 3) Contains freshness-enhancing agents, The crystallizing agent is a sodium salt of a saturated fatty acid having 8 to about 12 carbon atoms. A low-moisture composition in which the freshness-enhancing agent is present in at least one of the SDC or PEGC. [2] The low-moisture composition according to [1], wherein the sodium salt of the saturated fatty acid of the crystallizing agent comprises 50% to 70% by weight of C12, 15% to 25% by weight of C10, and 15% to 25% by weight of C8. [3] The low-moisture composition according to [1], wherein the sodium salt of the saturated fatty acid comprises 50% to 70% of a delayed crystallizing agent (delayed CA%). [4] The low-moisture composition according to any one of [1] to [3], wherein the crystallizer in the SDC domain is in the form of a fiber determined by a fiber testing method. [5] A low-moisture composition according to any one of [1] to [4], wherein the amount of water is less than 10% by weight of the final low-moisture composition determined by the moisture content test method. [6] The freshness beneficial agent is at least one of a fragrance or an odor neutralizer, preferably the freshness beneficial agent is a neat fragrance, and more preferably the freshness beneficial agent is 3-(4-t-butylphenyl)-2-methylpropanal, 3-(4-t-butylphenyl)-propanal, 3-(4-isopropylphenyl)-2-methylpropanal, 3-(3,4-methylenedioxyphenyl)-2-methylpropanal, and 2,6-dimethyl-5-heptenal, α-damascone, β-damascone, γ-damascone A low-moisture composition according to any one of [1] to [5], wherein the composition is at least one of the following: β-damascenone, 6,7-dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanone, methyl-7,3-dihydro-2H-1,5-benzodioxepin-3-one, 2-[2-(4-methyl-3-cyclohexenyl-1-yl)propyl]cyclopentan-2-one, 2-sec-butylcyclohexanone, and β-dihydroionone, linalool, ethyllinalool, tetrahydrolinalool, dihydromyrcenol, or a mixture thereof. [7] The low-moisture composition according to [6], wherein the fragrance is enclosed in a capsule having a wall and a core, and preferably the capsule wall comprises at least one of melamine, polyacrylamide, silicone, silica, polystyrene, polyurea, polyurethane, polyacrylate-based material, polyacrylate ester-based material, gelatin, styrene-malic anhydride, polyamide, aromatic alcohol, polyvinyl alcohol, or a mixture thereof. [8] The low-moisture composition according to [7], wherein the freshness beneficial agent is a mixture of neat fragrance and fragrance capsules. [9] The low-moisture composition according to [7], wherein the fragrance capsule is present in an amount of about 0.05% to about 20% by weight of the composition.
[10] The low-moisture composition according to any one of [1] to [9], wherein the sodium salt is at least one of sodium C8, sodium C10, or sodium C12.
[11] The low-moisture composition according to any one of [1] to
[10] , wherein the crystallizer is present in an amount of about 70% to about 95% by weight of the low-moisture composition.
[12] The low-moisture composition according to [8], wherein the neat fragrance constitutes about 0.01% to about 25% by weight, preferably about 0.1% to about 25% by weight, based on the total weight of the low-moisture composition.
[13] The low-moisture composition according to any one of [1] to
[12] , wherein the PEGC comprises PEG having a molecular weight of about 200 to about 50,000 daltons.
[14] The low-moisture composition according to any one of [1] to
[13] , wherein the low-moisture composition is composed of particles, preferably a physical mixture of particles composed of SDC domains and particles composed of PEGC domains.
[15] A method for producing a low-moisture composition, a) Mixing and heating the crystallizing agent and the aqueous phase until the crystallizing agent is substantially solubilized, and then cooling to the temperature before significant crystallization of the crystallizing agent in the form of SDCM, b) Cooling the solid soluble composition mixture to below the crystallization temperature and crystallizing the solid soluble composition mixture into an intermediate rheological solid to form the SDC into the designed shape and size, c) Drying and removing excess water, and removing approximately 90% to approximately 99% of the water determined by the moisture content test method from the intermediate rheological solid composition to produce a solid soluble composition (SDC) having an average solubility percentage of more than 5% at 37°C as determined by the solubility test method, e) To provide polyethylene glycol (PEGC), f) Combining the SDC and the PEGC to produce a low-moisture composition having SDC domains and PEGC domains, A method comprising adding a freshness-enhancing agent to at least one of the SDC domain or the PEGC domain.
Claims
1. A low-moisture composition, 1) A water-soluble solid composition (SDC) domain comprising a crystallizing agent and 10% by weight or less of water, 2) At least one polyethylene glycol (PEGC) domain, 3) Contains freshness-enhancing agents, The low-moisture composition has a water content of less than 10% by weight. The crystallizing agent is a sodium salt of a saturated fatty acid having 8 to 12 carbon atoms. The freshness-enhancing agent is present in at least one of the SDC or PEGC. A low-moisture composition wherein the sodium salt of the saturated fatty acid in the crystallizing agent comprises 50% to 70% by weight of C12, 15% to 25% by weight of C10, and 15% to 25% by weight of C8.
2. The low-moisture composition according to claim 1, wherein the sodium salt of the saturated fatty acid has a delaying CA% of 50% to 70%, and the delaying CA% is the weight percentage of NaC12 in a mixture of NaC12, NaC10, and NaC8.
3. The low-moisture composition according to claim 1 or 2, wherein the crystallizer in the SDC domain is in the form of a fiber determined by a fiber testing method.
4. The low-moisture composition according to claim 1 or 2, wherein the freshness beneficial agent is at least one of a fragrance or an odor neutralizer.
5. The low-moisture composition according to claim 1 or 2, wherein the freshness beneficial agent is a neat fragrance.
6. The freshness beneficial agent is 3-(4-t-butylphenyl)-2-methylpropanal, 3-(4-t-butylphenyl)-propanal, 3-(4-isopropylphenyl)-2-methylpropanal, 3-(3,4-methylenedioxyphenyl)-2-methylpropanal, and 2,6-dimethyl-5-heptenal, α-damascone, β-damascone, γ-damascone, β-damascenone, 6,7-dihydro-1,1,2,3,3-pentamethyl The low-moisture composition according to claim 1 or 2, comprising at least one of the following: -4(5H)-indanone, methyl-7,3-dihydro-2H-1,5-benzodioxepin-3-one, 2-[2-(4-methyl-3-cyclohexenyl-1-yl)propyl]cyclopentan-2-one, 2-sec-butylcyclohexanone, and β-dihydroionone, linalool, ethyllinalool, tetrahydrolinalool, dihydromyrcenol, or a mixture thereof.
7. The low-moisture composition according to claim 4, wherein the fragrance is enclosed in a capsule having a wall and a core.
8. The low-moisture composition according to claim 7, wherein the wall comprises at least one of melamine, polyacrylamide, silicone, silica, polystyrene, polyurea, polyurethane, polyacrylate-based material, polyacrylate ester-based material, gelatin, styrene-malic anhydride, polyamide, aromatic alcohol, polyvinyl alcohol, or a mixture thereof.
9. The low-moisture composition according to claim 1 or 2, wherein the freshness beneficial agent is a mixture of neat fragrance and fragrance capsules.
10. The low-moisture composition according to claim 7, wherein the fragrance capsule is present in an amount of 0.05% to 20% by weight of the composition.
11. The low-moisture composition according to claim 1 or 2, wherein the crystallizing agent is present in an amount of 70% to 95% by weight of the low-moisture composition.
12. The low-moisture composition according to claim 9, wherein the neat fragrance constitutes 0.01% to 25% by weight based on the total weight of the low-moisture composition.
13. The low-moisture composition according to claim 1 or 2, wherein the PEGC comprises a PEG having a molecular weight of 200 to 50,000 daltons.
14. The low-moisture composition according to claim 1 or 2, wherein the low-moisture composition is composed of particles.
15. The low-moisture composition according to claim 14, wherein the particles are a physical mixture of particles composed of SDC domains and particles composed of PEGC domains.
16. A method for producing a low-moisture composition, a) Mixing and heating the crystallizing agent and the aqueous phase until the crystallizing agent is substantially solubilized to form a solid soluble composition mixture (SDCM), and then cooling the SDCM to a temperature before significant crystallization of the crystallizing agent, b) Cooling the solid soluble composition mixture to below the crystallization temperature and crystallizing the solid soluble composition mixture into a rheological solid composition to form a water-soluble solid composition (SDC) in the designed shape and size, c) Drying and removing excess water, and removing 90% to 99% of the water determined by the moisture content test method from the rheological solid composition to produce a water-soluble solid composition (SDC), thereby producing a water-soluble solid composition having an average solubility percentage of more than 5% at 37°C as determined by the dissolution test method, e) To provide polyethylene glycol (PEGC), f) Combining the SDC and PEGC to produce a low-moisture composition having SDC domains and PEGC domains, The crystallizing agent is a sodium salt of a saturated fatty acid having 8 to 12 carbon atoms, and the sodium salt of the saturated fatty acid in the crystallizing agent comprises 50% to 70% by weight of C12, 15% to 25% by weight of C10, and 15% to 25% by weight of C8. A method comprising adding a freshness-enhancing agent to at least one of the SDC domain or the PEGC domain.