Liquid treatment composition comprising delivery particles based on vegetable rosin material
The use of vegetable rosin material in treatment compositions addresses the need for sustainable delivery systems by maintaining agent stability and deposition on surfaces despite dilution, enhancing performance and sustainability in fabric care products.
Patent Information
- Application Number
- JP2023532478
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-12-16
- Filing Date
- 2021-12-14
- Publication Date
- 2025-07-23
- Estimated Expiration
- 2041-12-14
AI Technical Summary
Existing treatment compositions that utilize synthetic polymers for delivering beneficial agents face challenges in transitioning to natural and sustainable sources, and these systems are prone to dilution issues that weaken agent performance on target surfaces.
A liquid treatment composition using vegetable rosin material and particles containing beneficial agents, which are stable under dilution and effectively deposit on surfaces like fabrics, utilizing tricyclic diterpene monocarboxylic acids and their derivatives, such as abietic-type acids, to enhance deposition and stability.
The vegetable rosin-based particles maintain the integrity of beneficial agents during washing cycles, ensuring effective deposition and performance on target surfaces by resisting dilution and providing improved stability and deposition efficiency.
Smart Images

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Abstract
Description
Technical Field
[0001] The present disclosure relates to a liquid treatment composition comprising a plant rosin material and particles comprising one or more beneficial agents, and an auxiliary component. The present disclosure also relates to related methods of making and using such compositions.
Background Art
[0002] Treatment compositions such as liquid fabric softeners can utilize various delivery systems to facilitate improved delivery of beneficial agents. Particles are commonly selected as a delivery system, particularly for fragrances.
[0003] For example, a fragrance may be encapsulated in core-shell particles that allow for improved deposition of the fragrance and advantages such as freshness over multiple touch points. Other materials, such as amphiphilic graft copolymers, are disclosed as being capable of forming particles that can bind to beneficial agents and be subsequently deposited onto surfaces such as fabrics.
[0004] However, one drawback of these delivery systems is that while such delivery systems typically require synthetic materials such as synthetic polymers, there is an increasing desire by manufacturers, distributors, and consumers to use materials derived from natural and / or sustainable sources.
[0005] Additionally, or alternatively, some of the materials used to encapsulate or confine beneficial agents are susceptible to the effects of dilution, which results in the release of beneficial agents during the treatment cycle with water. Since the release occurs prior to deposition onto the target surface, the performance of the beneficial agent is weakened at certain touch points such as dry fabrics.
Summary of the Invention
Problems to be Solved by the Invention
[0006] There continues to be a need for treatment compositions that provide an improved delivery mechanism for beneficial agents derived from natural sources.
Means for Solving the Problems
[0007] The present disclosure relates to a liquid treatment composition comprising a vegetable rosin material and particles containing one or more beneficial agents, as well as auxiliary components.
[0008] The present disclosure also relates to a liquid treatment composition comprising a tricyclic diterpene monocarboxylic acid, a derivative thereof, or a mixture thereof, further comprising one or more beneficial agents, preferably wherein the tricyclic diterpene monocarboxylic acid, a derivative thereof, or a mixture thereof comprises a material selected from abietic-type acids, derivatives thereof, pimaric-type acids, derivatives thereof, and mixtures thereof, more preferably wherein the tricyclic diterpene monocarboxylic acid comprises a derivative in ester form, and further comprising auxiliary components.
[0009] The present disclosure also relates to a method of treating a surface, preferably a fabric surface, the method comprising contacting the liquid treatment composition described herein with the surface, optionally in the presence of water. BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The drawings herein are illustrative in nature and are not intended to be limiting.
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[0011] The present disclosure relates to liquid treatment compositions comprising benefit agent delivery particles (or simply "particles" as used herein). The particles of the present disclosure contain one or more benefit agents such as vegetable rosin materials and fragrances. As indicated by the name, vegetable rosin materials are derived from plants, typically pine trees. This makes them attractive as natural or sustainable materials, even if they are later modified or derived.
[0012] Surprisingly, it has been found that the particles containing the vegetable rosin material and the benefit agent of the present disclosure can act as an effective delivery system in the liquid treatment composition. These rosins typically feature, for example, large amounts of abietic acid. Without being bound by theory, it is believed that the structure of the abietic-type acid material results in an interaction with the fragrance raw materials caused by the hydrophobic region. This can lead to the formation of relatively large particles that are relatively stable. The particles are thought to be able to withstand dilution with water. For example, in the case of fabric care products, they can withstand the dilution step during the washing cycle, thus maintaining the bond that promotes the deposition of the benefit agent. Furthermore, the rosin material is thought to be characterized by a relatively high molecular weight that makes it more likely to deposit on the target surface (e.g., fabric) compared to compounds with a relatively low molecular weight.
[0013] The components, compositions, and processes of the present disclosure are described in more detail below.
[0014] As used herein, the articles "a" and "an" as used in the claims are understood to mean one or more of what is claimed or described. As used herein, the terms "include", "includes", and "including" are meant to be non-limiting. The compositions of the present disclosure can comprise, consist essentially of, or consist of the components of the present disclosure.
[0015] In this specification, the terms "substantially free of" or "substantially free from" may be used. This means that the indicated material is in minimal amounts and is not intentionally added to the composition to form part of the composition, or preferably, does not exist at analytically detectable levels. It means that the indicated material is present only as an impurity in one of the other materials that are intentionally included, including the composition. The indicated material, if present, may be present at a level of less than 1% by weight, or less than 0.1% by weight, or less than 0.01% by weight, or even 0% by weight of the composition.
[0016] As used herein, the phrase "fabric care composition" includes compositions and formulations designed to treat fabrics. Such compositions include laundry washing compositions and detergents, fabric softening compositions, fabric strengthening compositions, fabric deodorizing compositions, pre-wash detergents, pre-wash treatment agents, laundry additives, spray products, dry cleaning agents or compositions, post-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 view of the teachings herein, but are not limited thereto. Such compositions can be used as pre-wash treatment agents, post-wash treatment agents, or added during the rinse or wash cycle of a laundry operation.
[0017] Unless otherwise noted, all component or composition levels relate to the active portion of the component or composition, and impurities that may be present in commercial sources of such components or compositions, such as residual solvents or by-products, are excluded.
[0018] All temperatures in this specification are in degrees Celsius (°C) unless otherwise indicated. Unless otherwise stated, all measurements in this specification are performed at 20°C and atmospheric pressure.
[0019] In all embodiments of the present disclosure, all percentages are relative to the weight of the total composition unless otherwise specified. Unless otherwise indicated, all ratios are by weight.
[0020] It should be understood that all upper numerical limits given throughout this specification include all lower numerical limits as if such lower numerical limits were expressly recited herein. All lower numerical limits shown throughout this specification include all higher numerical limitations as if such higher numerical limitations were expressly recited herein. All numerical ranges given throughout this specification include any narrower numerical ranges that fall within such broad numerical ranges as if such narrower numerical ranges were all expressly recited herein.
[0021] Treatment composition The present disclosure relates to a liquid treatment composition comprising particles and auxiliary components.
[0022] The treatment composition may be a consumer product composition. The consumer product composition may be a fabric care composition, a hard surface cleaning composition, a dish care composition, a hair care composition, a body cleansing composition, or a mixture thereof. The consumer product composition may be a conditioning composition such as a liquid fabric softener composition or a hair conditioner composition.
[0023] The treatment composition of the present disclosure may be a fabric care composition. Such a composition can be used as a pre-washing treatment agent, a post-washing treatment agent, or added during the rinsing or washing cycle of a washing operation. The fabric care composition may be a fabric detergent composition, a fabric conditioning composition, or a mixture thereof, preferably a fabric conditioning composition. Examples of fabric conditioning compositions may include liquid fabric softeners and liquid fabric softener compositions.
[0024] The treatment composition may be encapsulated in a water-soluble film so as to be present in the form of a unit-dose article such as a pouch. The water-soluble film may be a polyvinyl alcohol water-soluble film. Suitable films are available from MonoSol, LLC (Indiana, USA). The treatment composition may be encapsulated in a single-compartment pouch or a multi-compartment pouch. The multi-compartment pouch may have at least two, at least three, or at least four compartments. The multi-compartment pouch may include compartments arranged side by side and / or stacked. The composition contained in the pouch or its compartments may be a liquid, a solid (such as a powder), or a combination thereof, and in such cases, at least one encapsulated composition is a liquid composition. Unit-dose articles such as pouches and water-soluble films are described in more detail below.
[0025] The composition may be characterized by its viscosity. The composition may have a viscosity of about 1 to about 1500 centipoise (about 1 to 1500 mPa -1 s) at 20 s * and 21 °C, or about 50 to about 1000 centipoise (about 50 to 1000 mPa * s), or about 100 to 500 centipoise (about 100 to 500 mPa * s), or about 100 to about 200 centipoise (about 100 to 200 mPa * s), as disclosed. The relatively low viscosity improves addition and / or enables reduction of residues in the dispenser drawer. The viscosity is determined according to the method provided in the section on test methods below.
[0026] The treatment composition of the present disclosure may be characterized by a pH of about 2 to about 12, or about 2 to about 8.5, or about 2 to about 7, or about 2 to about 5. The treatment composition of the present disclosure may preferably be in the form of an aqueous liquid and have a pH of about 2 to about 4, preferably about 2 to about 3.7, more preferably about 2 to about 3.5. Such pH levels are thought to promote the stability of certain adjuvants such as conditioning active agents (e.g., ester quats). The pH of the composition is measured by dissolving / dispersing the composition in deionized water to form a 10% concentration solution at about 20°C.
[0027] Delivery particles (or "particles") The present disclosure also relates to delivery particles, and in the present disclosure simply referred to as "particles". The particles contain a vegetable rosin material and one or more beneficial agents.
[0028] One or more beneficial agents may be encapsulated within and / or embedded within the vegetable rosin material. The composition of the present disclosure may contain the particles described herein.
[0029] The particles of the present disclosure may be present in a population that may have a volume weighted median diameter (or "diameter" as used herein). The volume weighted median diameter is determined according to the method provided in the section on test methods below. The particles may have a volume weighted median diameter of from about 10 microns to about 400 microns. Without being bound by theory, smaller particles are said to be less effective as delivery particles, and larger particles are thought to be visible in the final product and / or may cause undesirable spots on the targeted surface. Since larger particles tend to contain a relatively high proportion of rosin material relative to the fragrance, the particles at the lower limit of the range may be preferred for enhancing the efficiency of fragrance delivery. The particles may be characterized by a volume weighted median particle diameter of from about 10 microns to about 400 microns, or from about 15 microns to about 300 microns, or from about 20 microns to about 250 microns, or from about 25 microns to about 200 microns, or from about 30 microns to about 150 microns, or from about 35 microns to about 125 microns, preferably from about 40 to about 100 microns, more preferably from about 50 to about 90 microns.
[0030] One or more particles of the present disclosure may include at least one region containing a beneficial agent such as a fragrance ingredient or an enzyme. This region may contain a beneficial agent such as a fragrance ingredient or an enzyme that is surrounded by or encapsulated within the vegetable rosin material. This region may be embedded within the vegetable rosin material and may contain a beneficial agent such as a fragrance ingredient or an enzyme that is, for example, partially embedded.
[0031] One or more particles of the present disclosure may have a structure selected from the group consisting of: (a) a particle comprising a single region having a beneficial agent embedded in a vegetable rosin material; (b) a particle comprising at least two regions having a beneficial agent embedded in a vegetable rosin material; (c) a particle comprising at least one region having a beneficial agent at least partially embedded on the surface of a vegetable rosin material; (d) a particle comprising a single region having a beneficial agent embedded in a vegetable rosin material and at least one region having a beneficial agent at least partially embedded on the surface of the vegetable rosin material; and (e) a particle comprising at least two regions having a beneficial agent embedded in a vegetable rosin material and at least one region having a beneficial agent at least partially embedded on the surface of the vegetable rosin material. The composition of the present disclosure may comprise one or more particles having the structure described in (a)-(e) or a mixture thereof.
[0032] The particles may be characterized by the weight ratio of the vegetable rosin material to the beneficial agent (e.g., preferably a fragrance). The vegetable rosin material and the one or more beneficial agents may be present in the particles in a weight ratio of about 5:95 to about 95:5, preferably about 20:80 to about 80:20, more preferably about 30:70 to about 70:30, even more preferably about 40:60 to about 60:40. The weight ratio may be about 50:50 to about 80:20, or about 50:50 to about 70:30. In order to obtain a relatively good balance between performance and ease of processing, it may be preferable for the weight ratio of rosin material to beneficial agent to be close to 50:50, and a relatively higher ratio than 50:50 may result in an improvement in performance when the beneficial agent is added / present at a certain level.
[0033] The treatment composition of the present disclosure may comprise about 0.01 wt% to about 10 wt%, or about 0.05 wt% to about 7 wt%, or about 0.1 wt% to about 5 wt%, more preferably 0.8 wt% to 4 wt%, or about 1 wt% to about 3 wt% of rosin-based particles of the treatment composition. Such particles may comprise a weight ratio of the rosin material to the beneficial agent (preferably a fragrance raw material) of 70:30 to 50:50.
[0034] The plant rosin materials and beneficial agents of the particles are described in more detail below.
[0035] a. Plant rosin materials The compositions, particles and processes described herein contain plant rosin materials. As used herein, "plant rosin materials" may include plant rosins (including resin acids), plant rosin derivatives or mixtures thereof. The plant rosin materials of the present compositions, particles and processes may provide performance advantages, for example, by improving deposition and / or promoting the stability of beneficial agents. Such materials may be derived from natural and / or sustainable sources, and may in some cases be more preferred than known alternatives to the compositions and processes disclosed herein.
[0036] As described in more detail below, plant rosins are typically derived from conifers (class: Pinopsida), usually pine trees (genus: Pinus). Plant rosin, also called "colophony", is a solid material produced by heating liquid resin to vaporize the terpene components that are volatile liquids. Plant rosins typically consist of compounds related to resin acids such as abietic acid. Plant rosins may be further derived, for example, by esterification and / or hydrogenation.
[0037] The compositions of the present disclosure may include from about 0.01 wt% to about 10 wt% of plant rosin material, based on the weight of the composition. The compositions may include from about 0.01 wt% to about 5 wt%, or from about 0.05 wt% to about 3 wt%, or from about 0.1 wt% to about 1 wt% of plant rosin material, based on the weight of the composition.
[0038] Plant rosin materials may be characterized by a softening point. Plant rosin materials are typically solids at room temperature, but the softening point is a measure of the glass transition temperature associated with these materials. The softening point of plant rosin materials is determined according to the method provided in the section on test methods below.
[0039] The vegetable rosin material may be characterized by a softening point of about 50°C to about 175°C, or about 60°C to about 150°C, or about 75°C to about 125°C. The rosin may need to be softened by heating for introduction into consumer products. Thus, for ease of processing and / or energy savings, vegetable rosin materials having a relatively low softening point (e.g., less than 125°C) may be preferred for the compositions and processes of the present disclosure. A lower softening point may also be effective in improving the deposition aid performance of the vegetable rosin material.
[0040] The vegetable rosin material may be characterized by an acid value (sometimes referred to as "acid value"). The acid value of the vegetable rosin material is related to the total content of free acid in these products. The acid value of the vegetable rosin material is determined according to the method provided in the section of the test method below.
[0041] The vegetable rosin material may be characterized by an acid value of less than about 175, such as about 0 to about 175. For the particles, compositions and processes of the present disclosure, in order to minimize the impact on the final pH of the treatment composition, it is preferably to use a vegetable rosin material having a relatively low acid value, such as less than about 125, preferably less than about 100, more preferably less than about 75, even more preferably less than about 50, and still more preferably less than about 25. Without being bound by theory, it is believed that vegetable rosin materials having a relatively low acid value are also more easily dispersible in the treatment compositions of the present disclosure.
[0042] The color of the vegetable rosin material can be graded based on the Gardner color standard number in the range of 1 to 18. To minimize the impact on the final color of the treatment composition, the vegetable rosin material of the present disclosure may preferably have a color grade of about 1 to about 10, preferably about 1 to about 8. The color grade of the vegetable rosin material is determined according to the method provided in the section of the test method below.
[0043] Vegetable rosin materials may have an odor. Naturally derived resins have a large amount of terpene compounds. For the compositions and processes of the present disclosure, it may be preferable to select relatively small amounts of terpene structures and / or odoriferous compounds such that the naturally derived resins do not inhibit the overall perception. On the other hand, when an aromaticity such as that of pine trees is desired, the presence of terpene structures may be preferred.
[0044] For example, tall oil rosin may contain sulfur contaminants that have an adverse effect on the odor, so gum rosin may be preferred over tall oil rosin. On the other hand, since a "piney" scent associated with rosin materials may be normal or desirable in certain product compositions, it may be desirable for the vegetable rosin materials to have a detectable odor.
[0045] Vegetable rosin materials are typically relatively insoluble in water. For example, the plant resin materials described in the present disclosure may be characterized by a solubility of less than 1 g / L, or less than 100 g / L, or less than 1 g / L, or less than 0.1 g / L, or less than about 0.01 g / L in deionized water at 22 °C. Without wishing to be bound by theory, the relatively insoluble nature of the vegetable rosin materials of the present disclosure is thought to contribute to the deposition efficiency and performance of the associated beneficial agents. For example, compared to particles containing a PEG / vinyl acetate graft copolymer, the rosin-based particles of the present disclosure are less likely to dissolve or disassemble when the treatment composition is diluted during a treatment process such as a wash cycle or a rinse cycle in an automatic washing machine, thereby resulting in improved deposition and performance.
[0046] Vegetable rosin materials may be characterized by a density. Typically, vegetable rosin materials have a density greater than 1.0 kg / dm 3 at 25 °C, preferably at least 1.1 kg / dm 3 and are so characterized.
[0047] Vegetable rosin materials are typically combustible. For the particles, compositions, and processes of the present disclosure, it may be preferable to use vegetable rosin materials having a relatively high flash point, such as higher than 190 °C, to facilitate easier and safer processing. The flash point of the vegetable rosin material is determined according to the method provided in the section on test methods below.
[0048] The treatment compositions of the present disclosure may include particles containing a vegetable rosin material, and the vegetable rosin material may be a material selected from the group consisting of gum rosin, wood rosin, tall oil rosin, their derivatives, and mixtures thereof; preferably gum rosin, its derivatives, and mixtures thereof; more preferably a gum rosin ester. The vegetable rosin material may be an ester of a vegetable rosin, preferably an ester formed from an alcohol having two or more carbon atoms, and more preferably the alcohol may be glycerol, pentaerythritol, or a mixture thereof. The vegetable rosin material may be at least partially hydrogenated, and preferably may be fully hydrogenated. The vegetable rosin material may contain at least 50 wt%, more preferably at least 60 wt%, more preferably at least 70 wt%, more preferably at least 80 wt%, more preferably at least 85 wt% of abietic-type acids, derivatives of abietic-type acids, or mixtures thereof.
[0049] Vegetable rosins and vegetable rosin derivatives and premixes containing such substances are described in more detail below.
[0050] 1. Vegetable Rosin The vegetable rosin materials of the present disclosure may include vegetable rosin. Vegetable rosin is typically obtainable from the oleoresin of plants, which may exude from pine trees or otherwise be derived from pine trees. The oleoresin may be distilled to remove volatile terpenes, and the remaining solid material is the vegetable rosin.
[0051] Vegetable rosin can be solid at room temperature. The solid rosin may be relatively translucent and / or glassy. The vegetable rosin material may have a color ranging, for example, from light yellow to dark brown, or black.
[0052] Vegetable rosin is typically a mixture of compounds and is mainly composed of resin acids (also called rosin acids). Vegetable rosin may contain at least about 75 wt%, or at least about 80 wt%, or at least about 85 wt%, or at least about 90 wt%, or at least about 95 wt% of resin acids based on the weight of the vegetable rosin. Vegetable rosin may contain from about 75 wt% to about 97 wt%, or from about 80 wt% to about 96 wt%, or from about 85 wt% to about 95 wt%, or from about 90 wt% to about 95 wt% of resin acids based on the weight of the vegetable rosin. The remaining material may be a non-acidic material.
[0053] Resin acids are typically monocarboxylic acids having three condensed rings. Resin acids may be tricyclic diterpene monocarboxylic acids having a molecular formula such as C 19 H 29 COOH. Examples of resin acids include abietic-type acids, pimaric-type acids, preisalic acid, or mixtures thereof. The double bonds of abietic-type acids are typically conjugated, while the double bonds of pimaric-type acids are typically not conjugated.
[0054] Examples of abietic-type acids may include abietic acid, neoabietic acid, dehydroabietic acid, pultrinic acid, levopimaric acid, or mixtures thereof. Examples of pimaric-type acids may include pimaric acid, isopimaric acid, sandaracopimaric acid, or mixtures thereof. The structures of these exemplary resin acids are provided in Table A below.
[0055]
Table 1
[0056] Vegetable rosin may contain abietic-type acids, preferably abietic acid. Abietic acid has the empirical formula C 19 H 29 COOH and is also known as abietinic acid or sylvic acid. Abietic-type acids are typically the main components of vegetable rosin. Vegetable rosin may contain at least 50 wt%, or at least 60 wt%, or at least 70 wt%, or at least 80 wt%, or at least 85 wt% of abietic-type acids, preferably abietic acid.
[0057] Vegetable rosin may be classified according to the source from which it is obtained. For example, the vegetable rosin of the present disclosure may be classified as (and include) gum rosin, wood rosin, tall oil rosin, or mixtures thereof. Gum rosin is derived from the resin exudate of a tree or other plant and may be collected by taking sap from the tree, or by wounding the tree and collecting and processing the exudate. Wood rosin may be derived from materials collected from stumps of pine trees, for example, by solvent extraction and / or distillation. Tall oil rosin is a by-product obtained when crude tall oil is distilled during the kraft process of wood pulp production when pine trees are pulped.
[0058] Suitable vegetable rosins may be obtained from various pine species such as Pinus massoniana (Masson pine), Pinus elliottii (slash pine), Pinus palustris (longleaf pine), Pinus taeda (loblolly pine), Pinus oocarpa (Mexican yellow pine), Pinus leiophylla (Chihuahua pine), Pinus devoniana (Pino lacio or Michoacán pine), Pinus montezumae (Montezuma pine), Pinus pinaster (maritime pine), Pinus sylvestris (Scots pine), Pinus halepensis (Aleppo pine), Pinus insularis (Benguet pine), Pinus kesiya (Kesya pine), Pinus strobus (Eastern white pine) or mixtures thereof.
[0059] 2. Vegetable rosin derivatives The vegetable rosin material of the present disclosure may include vegetable rosin derivatives. Vegetable rosin derivatives may be produced by chemically modifying vegetable rosin materials such as rosin acids such as abietic acid. Such derivatives may be produced by esterification, hydrogenation, dimerization, polymerization, saponification or mixing thereof. Accordingly, vegetable rosin derivatives may include rosin esters, hydrogenated rosins, hydrogenated rosin esters, dimerized rosins, polymerized rosins or mixtures thereof.
[0060] The vegetable rosin material may be an ester of a vegetable rosin. The ester of a vegetable rosin may be a reaction product of a vegetable rosin (e.g., rosin acid) and an alcohol. A condensation reaction of a sample between three abietic acid molecules and one glycerol molecule is shown below, which results in a rosin ester.
[0061]
Chem.
[0062] The alcohol in the esterification reaction may be a monoalcohol, a diol or a polyol, preferably a diol or a polyol. Suitable monoalcohols include methanol, which can form rosin methyl ester when reacted with rosin acid. Suitable diols containing two hydroxyl groups include triethylene glycol. The alcohol may also be a polyol containing three or more hydroxyl groups. Suitable polyols may contain a total of three hydroxyl groups (e.g., glycerol), a total of four hydroxyl groups (e.g., pentaerythritol), or a total of six hydroxyl groups (e.g., sorbitol or mannitol). Preferred polyols include glycerol, pentaerythritol and mixtures thereof.
[0063] The alcohol in the esterification reaction may contain from 1 to 10 carbon atoms, preferably from 1 to 7, more preferably from 1 to 6, even more preferably from 1 to 5, and even more preferably from 3 to 5 carbon atoms. The alcohol in the esterification reaction may preferably contain at least 2 carbon atoms, preferably from 2 to 10, more preferably from 2 to 6, and even more preferably from 2 to 5 carbon atoms. In some cases, it may be preferred that the rosin ester is not a methyl ester.
[0064] The alcohol used in the esterification reaction may have a relatively low molecular weight. For example, the alcohol may have a molecular weight of from about 32 Daltons to about 300 Daltons, preferably from about 32 Daltons to about 200 Daltons, more preferably from about 32 Daltons to about 150 Daltons, and even more preferably from about 90 Daltons to about 150 Daltons. Without wishing to be bound by theory, rosin esters formed from low molecular weight alcohols may be characterized by a relatively low softening point and / or a low acid value compared to rosin esters formed from relatively high molecular weight alcohols, which is believed to result in better processability and / or performance.
[0065] The alcohol used in the esterification reaction may be glycerol or pentaerythritol. Thus, the vegetable rosin derivative may be glyceryl rosin ester, pentaerythrityl rosin ester, or a mixture thereof.
[0066] The vegetable rosin derivative may be hydrogenated rosin. Considering that many vegetable rosin compounds (e.g., rosin acid) are unsaturated, they tend to be oxidatively unstable and may change color during storage. Hydrogenation can help stabilize the rosin and reduce undesirable color changes. Furthermore, hydrogenated rosin tends to have a lighter color than the parent rosin, which provides more formulation and aesthetic flexibility.
[0067] The vegetable rosin and / or rosin acid may be partially or fully hydrogenated. The following are sample reactions for the partial and full hydrogenation of abietic acid.
[0068]
Chemical formula
[0069] The treatment composition may include a vegetable rosin material that is at least partially hydrogenated, preferably fully hydrogenated.
[0070] The vegetable rosin derivative may be hydrogenated or esterified. For example, the vegetable rosin derivative may be a hydrogenated methyl ester or a hydrogenated glyceryl ester.
[0071] The vegetable rosin derivative may be a dimerized vegetable rosin. Dimerization may be useful for increasing the softening point and / or stability of rosin acid. A sample dimerization reaction of abietic acid is shown below.
[0072]
Chemical formula
[0073] Since it is difficult or even impossible to completely dimerize a sample of rosin, rosin dimers often exist together with non-dimerized rosin acid. The dimerized rosin acid may be further esterified.
[0074] The vegetable rosin derivative may be dimerized by ions such as 2+ or Ca 2+ For example, zinc resinate is a vegetable rosin derivative in which two abietic acid compounds are bound to zinc ions.
[0075] The vegetable rosin derivative may be a rosin-based polymer. As used herein, a rosin-based polymer is intended to include compounds including rosin-based oligomers containing three or more monomer units derived from rosin acid. The polymer may be a main-chain polymer or a side-chain polymer.
[0076] The vegetable rosin derivative may be a rosin soap in which rosin acid reacts with an alkali metal hydroxide (e.g., NaOH or KOH) or an alkaline earth metal hydroxide (e.g., Ca(OH)2). More broadly, the vegetable rosin derivative may be a salt of rosin acid.
[0077] The plant rosin derivative may be a functionalized plant rosin. In other words, the plant rosin may be functionalized, and one or more functional groups are added to the plant rosin.
[0078] Examples of the plant rosin derivative may include the product of a Diels-Alder reaction such as the reaction product of rosin acid and maleic anhydride, and such a reaction product may be polymerized.
[0079] Examples of the plant rosin derivative may include a rosin-modified phenolic resin in which rosin reacts with phenol. The plant rosin derivative may contain rosin alcohol in which one or more of the carboxyl groups of rosin acid are converted to hydroxyl groups.
[0080] Examples of commercially available plant rosin derivatives suitable for the compositions and processes disclosed herein may include those disclosed in Example 1 in the Examples section below.
[0081] b. Beneficial agent The particles of the present disclosure contain one or more beneficial agents. As described above, it is believed that the beneficial agent is embedded and / or encapsulated in the plant rosin material when the particles are formed. Therefore, the formation of the particles can lead to an improvement in the stability, delivery, and / or performance of the beneficial agent on a target surface such as a fabric or a hard surface. For example, such embedding and / or encapsulation of the beneficial agent can prevent the decomposition of the beneficial agent and / or undesirable interactions with other components of the liquid consumer product.
[0082] The composition of the present disclosure may contain a beneficial agent and / or particles containing a beneficial component at a level that provides the beneficial component as intended when the composition is used. For example, the beneficial agent in the particles may be present at a level of about 0.05 wt% to about 10 wt%, or about 0.05 wt% to about 5 wt%, or about 0.1 wt% to about 4 wt% of the composition.
[0083] Beneficial agents may be selected from the group consisting of fragrance materials, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, skin coolants, vitamins, sunscreens, antioxidants, glycerin, malodor reducing agents, odor control substances, antistatic agents, softeners, insect and moth repellents, colorants, fluorescent brighteners, whiteners, defoamers, anti-foaming agents, UV protectants for fabrics and skin, sunlight fading inhibitors, anti-allergy agents, waterproofing agents, skin care agents, glycerin, natural actives, aloe vera, vitamin E, shea butter, cocoa butter, brighteners, antiperspirant actives, skin softeners, skin sensates, and mixtures thereof. Particularly preferred beneficial agents for the particles include fragrance materials.
[0084] The delivery efficiency of the beneficial agent can be most effective when the beneficial agent is relatively hydrophobic.
[0085] The beneficial agent of the particles may include a fragrance material that may contain one or more perfume raw materials. The term "perfume raw material" (or perfume raw material, "PRM") as used herein means a compound having a molecular weight of at least about 100 g / mol and useful for imparting odor, fragrance, essence, or scent, either alone or in combination with other perfume raw materials. Typical PRMs include, in particular, alkenes such as alcohols, ketones, aldehydes, esters, ethers, nitrites, and terpenes. Lists of common PRMs can be found in various references such as "Perfume and Flavor Chemicals", Volumes I and II; Steffen Arctander Allured Pub. Co. (1994) and "Perfumes: Art, Science and Technology", Miller, P.M. and Lamparsky, D., Blackie Academic and Professional (1994).
[0086] Suitable perfume raw materials may include materials such as geraniol, linalool, linalyl acetate, pyranol, geranyl acetate, anisaldehyde, citral, citronellal, lysmeral, citronellol, rose oxide, tetrahydrolinalool, hydroxycitronellal, β-ionone, menthol, cinnamaldehyde, anethole, vanillin, ethylvanillin, eugenol, clove oil, carvone, piperonal, and mixtures thereof. The perfume raw materials may include naturally derived materials such as essential oils.
[0087] The PRM may be characterized by their boiling point (B.P.) measured at normal pressure (760 mmHg) and the octanol / water partition coefficient (P) that can be described with respect to logP determined according to the following test method. As described in more detail below, based on these characteristics, the PRM may be classified as a perfume in the first quadrant, the second quadrant, the third quadrant, or the fourth quadrant. Perfumes having various PRMs from different quadrants may, for example, desirably provide aromatic effects at different touch points during normal use.
[0088] The perfume raw material may include a perfume raw material selected from the group consisting of a perfume raw material having a boiling point (B.P.) lower than about 250 °C and a logP lower than about 3, a perfume raw material having a B.P. higher than about 250 °C and a logP higher than about 3, a perfume raw material having a B.P. higher than about 250 °C and a logP lower than about 3, a perfume raw material having a B.P. lower than about 250 °C and a logP higher than about 3, and mixtures thereof. The perfume raw material having a B.P. lower than about 250 °C and a logP lower than about 3 is known as a perfume raw material in the first quadrant. The perfume raw material in the first quadrant is preferably limited to less than 30% of the perfume composition. The perfume raw material having a B.P. higher than about 250 °C and a logP higher than about 3 is known as a perfume raw material in the fourth quadrant, the perfume raw material having a B.P. higher than about 250 °C and a logP lower than about 3 is known as a perfume raw material in the second quadrant, and the perfume raw material having a B.P. lower than about 250 °C and a logP higher than about 3 is known as a perfume raw material in the third quadrant. Suitable perfume raw materials in the first, second, third, and fourth quadrants are disclosed in U.S. Patent No. 6,869,923 (B1).
[0089] The treatment composition may include particles in which the beneficial agent is an aromatic material, the aromatic material including a perfume raw material in the first quadrant of about 1 wt% to about 40 wt% of the aromatic material and / or a non-first quadrant perfume raw material of about 60 wt% to about 99 wt% of the aromatic material.
[0090] The particles of the present disclosure can be particularly useful for effectively solubilizing certain fragrance ingredients present in aqueous consumer product compositions, especially those that are relatively low in surfactants, thereby being useful for avoiding emulsifiers and other processing steps. In particular, the delivery particles of the present disclosure are useful when the beneficial agent of the particles contains a hydrophobic fragrance ingredient. The hydrophobic fragrance ingredient may be characterized by a relatively high logP value, such as a logP greater than about 3.0, and may include those described above such as PRM in the third quadrant, PRM in the fourth quadrant, or mixtures thereof. The beneficial agent of the particles may include at least about 50 wt%, or at least about 60 wt%, or at least about 70 wt%, or at least about 80 wt%, or at least about 90 wt%, or about 100 wt% of PRM in the third quadrant, PRM in the fourth quadrant, or mixtures thereof. Compositions containing such levels of PRM in the third and / or fourth quadrants as the beneficial agent of the particles may be aqueous, and at least 60 wt%, or at least 70 wt%, or at least 80 wt%, or at least 90 wt%, or at least 95 wt%, or at least 97 wt% of the composition may be water and / or less than 10 wt%, or less than 5 wt%, or less than 3 wt% of surfactant.
[0091] Non-limiting examples of PRM in the third quadrant include isobornyl acetate, carvone, α-citronellol, paracymene, dihydromyrcenol, geranyl acetate, d-limonene, linalyl acetate, vertenex, and mixtures thereof.
[0092] Non-limiting examples of quadrant 4 (or persistent) PRMs include allylcyclohexanepropionate, ambroxide, amyl benzoate, amyl cinnamate, amyl cinnamate aldehyde, amyl cinnamate aldehyde dimethyl acetal, isoamyl salicylate, hydroxycitronellal-methyl anthranilate (known as aurantiol®), benzophenone, benzyl salicylate, p-tert-butylcyclohexyl acetate, isobutylquinoline, β-caryophyllene, cadinene, cedrol, cedryl acetate, cedryl formate, cinnamyl cinnamate, cyclohexyl salicylate, cyclamen aldehyde, dihydroisojasmoneate, diphenylmethane, diphenyloxide, dodecalactone, 1-(1,2,3,4,5,6,7,8-octahydro-2,3,8,8-tetramethyl-2-naphthalenyl)-ethanone (known as iso E super®), ethylene brassylate, methylphenyl glycidate, ethyl undecylenate, 15-hydroxypentadecanoic acid lactone (known as exaltolide®), 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethyl-cyclopenta-γ-2-benzopyran (known as galaxolide®), geranyl anthranilate, geranyl phenylacetate, hexadecanolide, hexenyl salicylate, hexyl cinnamic aldehyde, hexyl salicylate, α-ionone, γ-ionone, γ-n-methyl ionone, p-tert-butyl-α-methylhydrocinnamaldehyde (known as lilial®), lilial (p-t-bucinal)®, linalyl benzoate, 2-methoxynaphthalene, methyl dihydrojasmonate, jakou indanone, jakou ketone, jakou tibetine, myristicin, oxahexadecanolide-10, oxahexadecanolide-11, patchouli alcohol, 5-acetyl-1,1,2,3,3,6-Hexamethylindane (known as phantolide®), phenylethyl benzoate, phenylethyl phenyl acetate, phenylheptanol, phenylhexanol, α-santalol, δ-undecalactone, γ-undecalactone, vetiveryl acetate, yara-yara, ylangene, and mixtures thereof may be mentioned.,
[0093] c. Premix The vegetable rosin material may be combined with one or more beneficial agents in the premix. The premix is added to a base composition that may contain auxiliary components to form a treatment composition. The treatment composition of the present disclosure may include a premix containing a vegetable rosin material and one or more beneficial agents, as described in more detail below.,
[0094] The premix may contain from about 1% to about 99% by weight of the vegetable rosin material of the premix. The premix may contain from about 1% to about 99% by weight of the beneficial agent of the premix. The premix may contain the weight ratio of the vegetable rosin material to the beneficial agent from about 1:99 to about 99:1, preferably from about 5:95 to about 95:5, more preferably from about 10:90 to about 90:10, more preferably from about 20:80 to about 80:20, more preferably from about 30:70 to about 80:20, more preferably from about 40:60 to about 80:20. It is considered that the performance advantages increase as the weight ratio of the vegetable rosin to the beneficial agent increases.,
[0095] The premix may contain an emulsifier. The premix may contain from about 1% to about 95% by weight, or from about 5% to about 95% by weight, preferably from about 5% to about 40% by weight of the emulsifier of the premix. The premix may contain the weight ratio of the vegetable rosin material to the emulsifier from about 5:95 to about 95:5. The premix may contain the weight ratio of the beneficial agent to the emulsifier from about 5;95 to about 95:5. Suitable emulsifiers may include surfactants, amphiphilic polymers, or mixtures thereof.,
[0096] Suitable surfactants may include nonionic surfactants, anionic surfactants, or mixtures thereof, preferably nonionic surfactants. Suitable nonionic surfactants may include alkoxylated surfactants, pyrrolidone-based surfactants (including alkyl pyrrolidones, preferably C12 alkyl pyrrolidones), alkyl polyglycosides, and mixtures thereof. The preferred HLB value of the nonionic surfactant is 3 to 12.5. Suitable commercially available nonionic surfactants may include Lutensol™ XP 40 (formerly BASF), Lutensol™ XP 70 (formerly BASF), Plurafac™ LF 224 (BASF), Plurafac™ LF 401 (BASF), Ecosurf™ EH 9 (DOW), Neodol™ surfactants (SHELL), Dobanol™ surfactants (SHELL), Surfadone™ LP-300 (ASHLAND), Planteren™ APG 600, or mixtures thereof.
[0097] Suitable amphiphilic polymers may include graft copolymers such as poly(ethylene glycol)-poly(vinyl acetate) graft copolymers, polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol graft copolymers, or mixtures thereof. Commercially available graft copolymers may include Sokalon® HP 22 or Soluplus® (both available from BASF).
[0098] The premix can be prepared by heating a vegetable rosin material. The vegetable rosin material can be heated to a temperature above the softening point of the vegetable rosin material. The premix may also be prepared by combining and mixing the heated vegetable rosin material with a beneficial agent.
[0099] For the sake of the homogeneity of the premix, the mixing may be carried out in a heated oil bath set at the same temperature as the softening point of the vegetable rosin material. As the sample becomes homogeneous, the temperature can be gradually decreased. This promotes a reduction in the risk of loss of volatile materials (e.g., evaporation of volatile PRM).
[0100] Processing aids (e.g., the above emulsifier) can be added at any suitable time. Preferably, the emulsifier is combined with the vegetable rosin material before being added to the beneficial agent (e.g., fragrance), if present. The order of addition is thought to improve the ease of homogenization of the mixture.
[0101] As an additional or alternative step of heating, the vegetable rosin material may be ground into small particles and mixed with the beneficial agent.
[0102] Once prepared, the premix may be stored at ambient temperature. That being said, when using the premix to make the final product composition, the premix may be heated, for example to about 60 °C, before being poured into the final product or combined with the base composition otherwise. This heating step is most likely to be useful when the premix is characterized by a relatively high weight ratio of rosin to beneficial agent (e.g., exceeding 50:50). If the premix contains, for example, a nonionic surfactant as an emulsifier, the heating step may not be required.
[0103] Water The liquid treatment composition of the present disclosure may contain water. The liquid treatment composition described in the present disclosure may contain at least 8% by weight of water, preferably at least 25% by weight of water, more preferably at least 50% by weight of water, more preferably at least 60% by weight of water, more preferably at least 70% by weight of water, more preferably at least 75% by weight of water, more preferably at least 80% by weight of water, more preferably at least 90% by weight of water, based on the treatment composition.
[0104] The liquid treatment composition described in the present disclosure may contain from about 1% to about 99% by weight, or from 10% to 99% by weight, or from about 10% to about 96% by weight, or from about 12% to about 90% by weight, or from about 20% to about 80% by weight, or from about 40% to about 80% by weight of water, based on the composition.
[0105] The liquid consumer product composition of the present disclosure may contain a relatively large amount of water, such as more than 50%, or more than 60%, or more than 70%, or more than 80%, or more than 90% of water. In particular, liquid compositions such as strong laundry detergents, liquid fabric conditioners (e.g., softeners) and liquid hard surface cleaners may advantageously be formulated with a large amount of water, for example to enhance fluidity or dispersibility.
[0106] The composition of the present disclosure may contain less than 50% by weight, or less than 40% by weight, or less than 30% by weight, or less than 20% by weight, or less than 15% by weight, or less than 12% by weight, or less than 10% by weight of water, based on the composition.
[0107] The liquid composition of the present disclosure may be substantially a non-aqueous composition and may contain less than 10% by weight, or less than 5% by weight, or less than 3% by weight, or less than 1% by weight, or less than 0.1% by weight, or even less than 0% by weight of water, based on the composition.
[0108] The water level may depend on the form and / or intended use of the composition. The amount of water may vary according to the form and / or intended use of the composition. For example, the composition may be in the form of a unit dose composition (e.g., a liquid composition encapsulated by a water-soluble film), and water may be present in an amount of about 1% to about 20%, or about 5% to about 15%. When the composition is in the form of a compact liquid laundry detergent, water may be present in an amount of about 10% to about 50% or about 20% to about 40%.
[0109] Auxiliary components The treatment composition of the present disclosure may further include auxiliary components in addition to the particles of the present disclosure. The auxiliary agent may be suitable for delivering a treatment effect to a target surface such as a fabric or other textile. As used herein, the auxiliary components may also include agents that promote chemical or physical stability in the treatment composition, such as buffers, structuring agents / thickeners, and / or carriers.
[0110] The auxiliary components may be present in the composition in an amount suitable for the intended use of the composition. Typical use concentrations range from a low concentration of 0.001% by weight of the composition for auxiliary agents such as optical brighteners to 50% by weight of the composition for builders.
[0111] Auxiliary components may include amines, surfactant systems, water-binding agents, sulfites, fatty acids and / or their salts, enzymes, encapsulated beneficial agents, soil release polymers, colorants, builders, chelating agents, migration inhibitors, dispersants, enzyme stabilizers, catalyst substances, bleaching agents, bleaching catalysts, bleach activators, polymer dispersants, soil removal / redeposition inhibitors, polymer dispersants, polymer fabric detergents, optical brighteners, antifoaming agents, dyes, colorants, free perfumes, perfume delivery systems, structure elasticizing agents, fabric softeners, carriers, fillers, hydrotropes, organic solvents, antibacterial and / or preservative agents, neutralizing and / or pH adjusting agents, processing aids, fillers, rheology modifiers or structuring agents, opacifying agents, pearl essence agents, pigments, anti-corrosion and / or anti-discoloration agents, and mixtures thereof. The compositions of the present disclosure may include, among other things, amines, surfactant systems, conditioning agents, water-binding agents, sulfite agents, structuring agents, organic solvents, free perfumes, perfume delivery systems, or mixtures thereof. Some of these auxiliary agents are described in more detail below.
[0112] Consumer product aids may include a surfactant system, a conditioning active substance, or a combination thereof. Preferably, the surfactant system includes anionic surfactants, nonionic surfactants, cationic surfactants, and / or zwitterionic surfactants. Preferably, the fabric softener includes a quaternary ammonium compound, a silicone compound, or both.
[0113] The liquid consumer product compositions described in the present disclosure may include a surfactant system. The surfactant system may consist of one surfactant. The surfactant system may include a plurality of surfactants.
[0114] The compositions of the present disclosure may include a surfactant system in an amount of about 20 wt% to about 75 wt%, or about 25 wt% to about 70 wt%, or about 30 wt% to about 50 wt% of the composition. The compositions of the present disclosure may include a surfactant system in an amount less than 20 wt%, or less than 10 wt%, or less than 5 wt%, or less than 3 wt% of the composition.
[0115] The surfactant system may include an anionic surfactant, a nonionic surfactant, an amphoteric surfactant, a cationic surfactant, an ampholytic surfactant, or a combination thereof. The surfactant system may include a linear alkylbenzene sulfonate, an alkyl ethoxylated sulfate, an alkyl sulfate, a nonionic surfactant such as an ethoxylated alcohol, an amine oxide, or a mixture thereof. The surfactant may at least partially be derived from natural resources such as natural feedstock alcohols.
[0116] Suitable anionic surfactants may include any conventional anionic surfactant. These may include, for example, sulfate detergency surfactants for alkoxylated and / or non-alkoxylated alkyl sulfate materials, and / or sulfonic acid-based detergency surfactants such as alkylbenzene sulfonate. The anionic surfactant may be linear, branched, or a combination thereof. Preferred surfactants include linear alkylbenzene sulfonate (LAS), alkyl ethoxylated sulfate (AES) including sodium lauryl ether sulfate (SLES), alkyl sulfate (AS) including sodium lauryl sulfate (SLS), or mixtures thereof. Other suitable anionic surfactants include modified alkyl benzene sulfonate (MLAS), methyl ester sulfonate (MES), and / or alkyl ethoxylated carboxylate (AEC). The anionic surfactant may be present in acid form, salt form, or mixtures thereof. The anionic surfactant may be partially or fully neutralized, for example, by an alkali metal (e.g., sodium) or an amine (e.g., monoethanolamine). In certain treatment compositions, such as those containing cationic materials like fabric conditioning agents, it may be desirable to limit the amount of anionic surfactant present. For example, the treatment composition may contain less than 5 wt%, or less than 3 wt%, or less than 1 wt%, or less than 0.1 wt%, or even 0 wt% of anionic surfactant.
[0117] The surfactant system may contain a nonionic surfactant. Suitable nonionic surfactants include alkoxylated fatty alcohols such as ethoxylated fatty alcohols. Other suitable nonionic surfactants include alkoxylated alkylphenols, alkylphenol condensates, medium-chain branched alcohols, medium-chain branched alkyl alkoxylates, alkyl polysaccharides (e.g., alkyl polyglycosides), polyhydroxy fatty acid amides, ether-capped poly(oxyalkylated) alcohol surfactants, and mixtures thereof. The alkoxylate units may be ethyleneoxy units, propyleneoxy units, or mixtures thereof. The nonionic surfactant may be linear, branched (e.g., medium-chain branched), or a combination thereof. Certain nonionic surfactants may include alcohols having an average of about 12 to about 16 carbons and an average of about 3 to about 9 ethoxy groups, such as a C12-C14 EO7 nonionic surfactant.
[0118] Suitable zwitterionic surfactants include betaines such as alkyldimethylbetaine and cocodimethylamidopropylbetaine, C8-C 18 (e.g., C 12 -C 18 ) amine oxides (e.g., C 12 - 14 dimethylamine oxide), and / or N-alkyl-N,N-dimethylamino-1-propanesulfonate (where the alkyl group may be C8-C 18 or C 10 -C 14 ) and other conventional zwitterionic surfactants such as sulfobetaines and hydroxybetaines. The zwitterionic surfactant may include an amine oxide.
[0119] The compositions of the present disclosure may contain conditioning actives. Compositions containing conditioning actives may provide benefits related to softness, anti-wrinkle, anti-static, conditioning, anti-stretching, color, and / or appearance. Suitable conditioning actives for the compositions of the present disclosure include quaternary ammonium ester compounds, silicones, non-ester quaternary ammonium compounds, amines, fatty acid esters, sucrose esters, silicones, dispersible polyolefins, polysaccharides, fatty acids, softening or conditioning oils, polymer latexes, or combinations thereof. Preferably, the treatment composition contains a conditioning active including a quaternary ammonium ester compound, more preferably a quaternary ammonium ester compound combined with a silicone.
[0120] The conditioning active may be present at a level of about 1 wt% to about 99 wt% of the composition. The composition may contain from about 1 wt%, or from about 2 wt%, or from about 3 wt% to about 99 wt%, or to about 75 wt%, or to about 50 wt%, or to about 40 wt%, or to about 35 wt%, or to about 30 wt%, or to about 25 wt%, or to about 20 wt%, or to about 15 wt%, or to about 10 wt% of the conditioning active. The composition may contain from about 5 wt% to about 30 wt% of the conditioning active.
[0121] The liquid treatment compositions described in the present disclosure may contain an external structuring agent. The external structuring agent can provide physical stability to the liquid compositions described in the present disclosure, for example, by helping to suspend the delivery particles. When present, the structuring agent is preferably present in an effective amount capable of suspending the particles in the treatment composition. The external structuring agent may include a non-polymeric crystalline hydroxyl-functional structuring agent and / or a polymeric structuring agent.
[0122] The non-polymeric crystalline hydroxyl-functional structurant may contain crystallizable glycerides that can be pre-emulsified to assist in dispersion into the final detergent composition. Suitable crystallizable glycerides include hydrogenated castor oil, i.e., "HCO", or derivatives thereof, provided that they can crystallize within the liquid detergent composition.
[0123] The polymeric structurant may include structurants of natural origin and / or synthetic structurants. Natural origin polymeric structurants include hydroxyethyl cellulose, hydrophobically modified hydroxyethyl cellulose, carboxymethyl cellulose, polysaccharide derivatives, and mixtures thereof. Suitable polysaccharide derivatives include pectin, alginate, arabinogalactan (gum arabic), carrageenan, gellan gum, xanthan gum, guar gum, and mixtures thereof. The structurant may include cellulose fibers, for example, in the form of microfibrillated cellulose. The cellulose may be derived from bacteria, wood, or other plants such as fruits or sugar beets.
[0124] Synthetic polymeric structurants include polycarboxylates, polyacrylates, hydrophobically modified ethoxylated urethanes, hydrophobically modified nonionic polyols, and mixtures thereof. The polycarboxylate polymer may be a polyacrylate, polymethacrylate, or a mixture thereof. The polyacrylate may be a copolymer of an unsaturated mono- or di-carbonic acid and a C1-C alkyl ester of (meth)acrylic acid. 30 Such a copolymer is available from Lubrizol Corp. under the trade name Carbopol® Aqua 30.
[0125] The compositions of the present disclosure may include a solvent, preferably an organic solvent such as a non-amino functional organic solvent. Suitable organic solvents include glycerol, ethylene glycol, 1,3-propanediol, 1,2-propanediol, tetramethylene glycol, pentamethylene glycol, hexamethylene glycol, 2,3-butanediol, 1,3-butanediol, diethylene glycol, triethylene glycol, polyethylene glycol, glycerol formal dipropylene glycol, polypropylene glycol, dipropylene glycol n-butyl ether, and mixtures thereof. The organic solvent can provide a physical stability effect, particularly in compact formulations having a relatively low water content. The compositions of the present disclosure may include from about 5 wt% to about 80 wt%, or from about 10 wt% to about 50 wt% of the organic solvent in the composition.
[0126] The compositions of the present disclosure may include additional aesthetic agents such as those selected from dyes, opacifiers, pearl essence agents, or mixtures thereof.
[0127] The liquid consumer product compositions described in the present disclosure may include a fragrance delivery system. Suitable fragrance delivery systems may include core-shell capsule agents, pro-fragrances (amine-based and / or silicone-based pro-fragrances), and mixtures thereof. The core-shell capsule agent may include a core and a shell surrounding the core. The core may include a beneficial agent such as a fragrance, and optionally a partitioning regulator such as isopropyl myristate. The shell may include a polymer, such as melamine formaldehyde, polyurea, polyvinyl alcohol, polyacrylate, polysaccharide. Suitable capsule agents may be characterized by a volume-weighted median particle diameter of from about 10 microns to about 100 microns, or from about 10 microns to about 50 microns, or from about 15 microns to about 40 microns. The fragrance delivery system can provide effects such as improved fragrance stability, deposition, and / or longevity, and may be particularly useful for fragrance raw materials that do not bind well to the plant rosin materials of the present disclosure.
[0128] When the consumer product composition is in the form of a unit dose article such as a pouch or sachet, the composition may be enclosed by a water-soluble film. The water-soluble unit dose article may include at least one water-soluble film shaped such that the unit dose article includes at least one internal compartment surrounded by the water-soluble film. At least one compartment contains a detergent composition.
[0129] The unit dose article may include more than one compartment, or even at least two compartments, or even at least three compartments, or even at least four compartments, or even at least five compartments. The compartments may be arranged in an overlapping orientation, i.e., one on top of the other. Alternatively, the compartments may be arranged in an adjacent orientation, i.e., positioned adjacent to one another. The compartments may be further oriented in a "tire and rim" arrangement. That is, a first compartment is positioned adjacent to a second compartment, but the first compartment at least partially surrounds the second compartment without completely enclosing the second compartment. Alternatively, one compartment may be completely enclosed within another compartment. If one compartment contains the liquid composition described in the present disclosure, another compartment may contain a solid, a liquid, or a mixture thereof.
[0130] The film of the present invention may be water-soluble or water-dispersible (e.g., in water at 20 °C). Preferred film materials include polymer materials. The film material can be obtained by casting, blow molding, extrusion molding, or blow extrusion molding of polymer materials, which are well-known in the art. Preferably, the water-soluble film comprises a polyvinyl alcohol polymer or copolymer, preferably a blend of a polyvinyl alcohol polymer and / or a polyvinyl alcohol copolymer, preferably selected from sulfonated and carboxylated anionic polyvinyl alcohol copolymers, particularly carboxylated anionic polyvinyl alcohol copolymers, and most preferably comprises a blend of a polyvinyl alcohol homopolymer and a carboxylated anionic polyvinyl alcohol copolymer. Suitable films include those supplied by MonoSol, LLC (Indiana) under product reference numbers M8630, M8900, M8779, and / or M8310. The film may contain an aversion agent, such as a bittering agent. Before being formed into unit dose articles, the thickness of the water-soluble film is preferably 20 to 150 microns, preferably 35 to 125 microns, more preferably 50 to 110 microns, and most preferably about 76 microns.
[0131] Manufacturing process The present disclosure also relates to a process for making a liquid treatment composition. The process for making a liquid treatment composition, which can be a consumer product composition, may include combining the components described herein (e.g., a plant rosin material, one or more beneficial agents, and adjunct materials).
[0132] The process for making the liquid treatment composition described in the present disclosure may include combining a plant rosin material and one or more beneficial agents as individual components with a liquid base composition (e.g., without premixing the plant rosin material and one or more beneficial agents), where the liquid base composition contains adjunct components.
[0133] The process for making the liquid treatment composition described in the present disclosure may include a step of providing a premix. The premix may include a vegetable rosin material and one or more beneficial agents. The premix may be combined with a liquid-based composition. The liquid-based composition may include auxiliary components.
[0134] The liquid treatment composition of the present disclosure can be formulated into any suitable form and can be prepared by any process selected by the formulator. The materials may be combined in a batch process, a circulation loop process, and / or an in-line mixing process. Suitable apparatuses for use in the processes disclosed herein may include continuous stirred tank reactors, homogenizers, turbine stirrers, recirculation pumps, paddle mixers, plow shear mixers, ribbon blenders, vertical axis granulators, and drum mixers (both batch type and, if available, of continuous process configuration), spray dryers, and extruders.
[0135] The liquid treatment composition may be encapsulated in a water-soluble film according to known methods to form unit dose articles.
[0136] The liquid treatment composition may be placed in an aerosol or other spray container according to known methods.
[0137] Process for treating a surface The present disclosure also relates to a process for treating surfaces such as fabrics, hair, and / or skin. The process may include a step of contacting the surface with the treatment composition described in the present disclosure.
[0138] The contacting step may occur in the presence of water. The process of the present disclosure may include diluting a compact liquid laundry composition with water to form a treatment solvent that can contact the surface to be treated. The compact liquid detergent composition may be diluted 100-fold to 1000-fold, or 200-fold to 900-fold, or 300-fold to 800-fold with water.
[0139] The contacting step may be carried out within the drum of the automatic washing machine. The contacting step may occur as a pretreatment step.
[0140] Combination The specifically contemplated combinations of the present disclosure are described in the following alphabetically labeled paragraphs herein. These combinations are essentially for illustrative purposes and are not intended to be limiting. A. A liquid treatment composition comprising particles and auxiliary components, wherein the particles comprise a vegetable rosin material and one or more beneficial agents. B. The liquid treatment composition according to paragraph A, wherein the particles have a volume-weighted median particle diameter of about 10 microns to about 400 microns, or about 15 microns to about 300 microns, or about 20 microns to about 250 microns, or about 25 microns to about 200 microns, or about 30 microns to about 150 microns, or about 35 microns to about 125 microns, preferably about 40 microns to about 100 microns, more preferably about 50 microns to about 90 microns. C. The liquid treatment composition according to any one of paragraphs A or B, wherein the vegetable rosin material and one or more beneficial agents are present in the particles in a weight ratio of about 5:95 to about 95:5, preferably about 20:80 to about 80:20, more preferably about 30:70 to about 70:30, still more preferably about 40:60 to about 60:40. D. The liquid treatment composition according to any one of paragraphs A to C, wherein the vegetable rosin material is a material selected from the group consisting of gum rosin, wood rosin, tall oil rosin, their derivatives and mixtures thereof, preferably a material selected from the group consisting of gum rosin, its derivatives and mixtures thereof, more preferably comprising a gum rosin ester. E. The liquid treatment composition according to any one of paragraphs A to D, wherein the vegetable rosin material is a vegetable rosin ester, preferably an ester formed from an alcohol having two or more carbon atoms, more preferably the alcohol is glycerol, pentaerythritol or a mixture thereof. F. The liquid treatment composition according to any one of paragraphs A to E, wherein the vegetable rosin material is at least partially hydrogenated, preferably fully hydrogenated. G. The vegetable rosin material contains at least 50% by weight, more preferably at least 60% by weight, more preferably at least 70% by weight, more preferably at least 80% by weight, more preferably at least 85% by weight of abietic acid type acids, derivatives of abietic acid type acids or mixtures thereof, and is the liquid treatment composition according to any one of paragraphs A to F. H. The vegetable rosin material is characterized by a softening point of about 50°C to about 175°C, preferably about 60°C to about 150°C, more preferably about 75°C to about 125°C, and is the liquid treatment composition according to any one of paragraphs A to G. I. The vegetable rosin material is characterized by an acid value of less than about 175, preferably less than about 125, preferably less than about 100, more preferably less than about 75, even more preferably less than about 50, more preferably less than about 25, and is the liquid treatment composition according to any one of paragraphs A to H. J. When the vegetable rosin material is graded according to the Gardner color standard number, it is characterized by a color grade of about 1 to about 10, or about 1 to about 8, and is the liquid treatment composition according to any one of paragraphs A to I. K. The one or more beneficial agents are selected from the group consisting of fragrance materials, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, skin cooling agents, vitamins, sunscreens, antioxidants, glycerin, malodor reducing agents, odor control substances, antistatic agents, softeners, insect and moth repellents, colorants, fluorescent brighteners, whiteners, defoamers, anti-foaming agents, UV protectants for fabrics and skin, sunlight fading inhibitors, anti-allergy agents, waterproof agents, skin care agents, glycerin, natural active agents, aloe vera, vitamin E, shea butter, cocoa butter, whitening agents, antiperspirant active agents, skin softeners, skin sensates, and mixtures thereof, and are preferably selected from fragrance materials, and are the liquid treatment composition according to any one of paragraphs A to J. L. The one or more beneficial agents include a fragrance material, and is the liquid treatment composition according to any one of paragraphs A to K. M. The fragrance material contains about 1% to about 40% by weight of fragrance raw materials in the first quadrant of the fragrance material, and / or about 60% to about 99% by weight of non-first quadrant fragrance raw materials of the fragrance material, and is the liquid treatment composition according to any one of paragraphs A to L. N. The liquid treatment composition according to any one of paragraphs A to M, wherein one or more beneficial agents are encapsulated in and / or partially embedded in the vegetable rosin material. O. The liquid treatment composition according to any one of paragraphs A to N, which is formed by a process including adding a premix to a base composition, the premix containing a vegetable rosin material and one or more beneficial agents. P. The auxiliary component is selected from amines, surfactant systems, water binders, sulfites, fatty acids and / or their salts, enzymes, encapsulated beneficial agents, soil release polymers, colorants, builders, chelating agents, migration inhibitors, dispersants, enzyme stabilizers, catalyst substances, bleaching agents, bleaching catalysts, bleach activators, polymer dispersants, soil removal / redeposition preventers, polymer dispersants, polymer fabric detergents, optical brighteners, foam suppressants, dyes, colorants, free fragrances, fragrance delivery systems, structure elasticizers, fabric softeners, carriers, fillers, hydrotropes, organic solvents, antibacterial agents and / or preservatives, neutralizing agents and / or pH adjusters, processing aids, fillers, rheology modifiers or structuring agents, opacifiers, pearl essence agents, pigments, corrosion and / or discoloration resistant agents, and mixtures thereof. The liquid treatment composition according to any one of paragraphs A to O. Q. The auxiliary component includes a surfactant system, a fabric softener or a combination thereof. Preferably, the surfactant system includes an anionic surfactant, a nonionic surfactant, a cationic surfactant and / or an amphoteric surfactant, and / or preferably the fabric softener includes a quaternary ammonium compound, a silicone compound or both. The liquid treatment composition according to any one of paragraphs A to P. R. The liquid treatment composition further includes an amphiphilic polymer, preferably an amphiphilic graft copolymer, more preferably an amphiphilic graft copolymer including a polyalkylene glycol as a graft base and one or more side chains including a vinyl acetate moiety and optionally an N-vinylcaprolactam moiety. The liquid treatment composition according to any one of paragraphs A to Q. S. The liquid treatment composition is the liquid treatment composition according to any one of paragraphs A to R, comprising at least 8% by weight of water, preferably at least 25% by weight of water, more preferably at least 50% by weight of water, more preferably at least 60% by weight of water, more preferably at least 70% by weight of water, more preferably at least 75% by weight of water, more preferably at least 80% by weight of water, more preferably at least 90% by weight of water, of the liquid treatment composition. T. The liquid treatment composition has a viscosity of 1 to 1500 centipoises (1 to 1500 mPa -1 s) at 20 s * and 21 °C, and is the liquid treatment composition according to any one of paragraphs A to S. U. The liquid treatment composition further comprises a structuring agent present in an effective amount preferably capable of suspending particles in the liquid treatment composition, and is the liquid treatment composition according to any one of paragraphs A to T. V. The liquid treatment composition is a consumer product composition, preferably a fabric care composition, a hard surface cleaning composition, a dish care composition, a hair care composition, a body cleaning composition or a mixture thereof, and preferably the fabric care composition is a fabric detergent composition, a fabric conditioning composition or a mixture thereof, and is the liquid treatment composition according to any one of paragraphs A to U. O. The liquid treatment composition is encapsulated in a water-soluble film, and is the liquid treatment composition according to any one of paragraphs A to V. X. A liquid treatment composition comprising particles and auxiliary components, wherein the particles comprise a tricyclic diterpene monocarboxylic acid, a derivative thereof or a mixture thereof, the particles further comprise one or more beneficial agents, and preferably the tricyclic diterpene monocarboxylic acid, a derivative thereof or a mixture thereof comprises a substance selected from the group consisting of abietic-type acids, derivatives thereof, pimaric-type acids, derivatives thereof and mixtures thereof, and more preferably the tricyclic diterpene monocarboxylic acid comprises a derivative in the form of an ester. Y. A method for treating a surface, preferably a method for treating a fabric, the method comprising the step of contacting the surface with the liquid treatment composition according to any one of paragraphs A to X, optionally in the presence of water.
[0141] Test methods It will be understood that the respective values of the parameters of the subject matter of the invention claimed and described herein are to be determined using the test methods disclosed in the test methods chapter of this application.
[0142] Test method for determining the logarithm of the octanol / water partition coefficient (logP) For each PRM in the flavor mixture to be tested, the log value (logP) of the octanol / water partition coefficient is calculated. The logP value of an individual PRM is calculated using the Consensus logP Computational Model, version 14.02 (Linux®), available from Advanced Chemistry Development Inc. (ACD / Lab) (Toronto, Canada), and a unitless logP value is obtained. The ACD / Labs Consensus logP Computational Model is part of the ACD / Labs model suite.
[0143] Softening point test method If available, the softening point of the vegetable rosin material provided by the manufacturer / supplier must be used.
[0144] If not available from the manufacturer / supplier, the softening point is measured in accordance with ASTM E28-18, "Standard Test Methods for Softening Point of Resins Derived from Pine Chemicals", using the version approved on July 1, 2018 and published in July 2018. More specifically, the reference method provided in the above version ("Automated Ring and Ball Softening Point Method") must be followed. The method is summarized here.
[0145] As used herein (and as described in ASTM E28-18), the softening point is defined as the temperature at which a disk of the sample held in a horizontal ring (brass shoulder ring; 19.8 mm inner diameter, 23.0 mm outer diameter as specified in the ASTM method) is pushed downward a distance of 25.4 mm (1 inch) under the weight of a steel ball (9.53 mm diameter; mass 3.45 - 3.55 g) as the sample is heated at 5 °C / min in water, glycerin, silicone oil, ethylene glycol / water, or glycerin / water bath.
[0146] Sample Preparation: Select a representative sample of the rosin material to be tested. The sample shall include freshly fractured chunks free of flakes, chips, or oxidized surfaces and shall avoid containing finely divided material or dust. Melt the sample in a clean container, avoiding overheating and introduction of air bubbles into the sample. The time from start of heating to injection of the sample shall not exceed 15 minutes. Place the ring, bottom down, on a metal surface. The ring may be preheated. Pour the melted rosin sample into the ring such that an excess remains upon cooling. After cooling for at least 30 minutes, remove excess material from around and on top of the ring.
[0147] Bath Liquid: The choice of bath liquid depends on the softening point ("SP") of the rosin material. For SP between 35 °C and 80 °C, use water (distilled or deionized and freshly boiled). For SP between 80 °C and 150 °C, use USP glycerin. For SP above 80 °C, use silicone oil (polydimethylsiloxane - 200 fluid, 50 cSt, manufactured by Dow Corning (Midland, MI)). For SP up to 35 °C, use a 50 / 50 (v / v) mixture of ethylene glycol and distilled water. Cool the bath to -25 °C in a pre-cooled freezer or isopropyl dry ice bath.
[0148] Test: Use a suitable automated ring and ball softening point apparatus equipped with a control unit and calibrate it according to the manufacturer's instructions. Place the stirrer in a 600 mL beaker and fill it with the above bath solution according to the softening point of the rosin material. Set up the apparatus, ring, ball, test insert, and support pins as recommended in the manufacturer's instructions. Confirm that the control unit is set for the correct bath solution.
[0149] Heat the bath so that the temperature of the bath solution rises uniformly at a rate of 5 °C / min. The test is completed when the light beam is blocked by the ball and the material. Record the softening point at the temperature displayed on the unit after the test is completed.
[0150] Acid Value Test Method If available, the acid value of the vegetable rosin material provided by the manufacturer / supplier must be used.
[0151] If not available from the manufacturer / supplier, the acid value is measured according to ASTM D465-15 (re-approved in 2020), "Standard Test Methods for Acid Number of Pine Chemical Products Including Tall Oil and Other Related Products", approved on June 1, 2020 and published in June 2020. More specifically, it must follow the reference method ("potentiometric titration method") provided in the above-mentioned document. The method is summarized here.
[0152] Prepare a sample of freshly shredded rosin material, and it may be further ground to facilitate weighing and dissolution, but small pieces containing oxidized surfaces and existing rosin dust or powder shall not be used. In the case of a heterogeneous liquid, place it in a sealed container equipped with very small air vents or their equivalents and heat it in a warm water bath. The sample may be stirred during heating and used after it has been sufficiently stirred to be homogeneous.
[0153] Based on the following table, transfer a specified amount of the sample to a 400 mL tall beaker. Add an appropriate amount of Solvent I and dissolve it with swirling, and gently heat it if necessary. Add an appropriate amount of Solvent II and cool it to near room temperature if necessary. Immerse each electrode of a glass electrode pH meter (calibrated / standardized according to the manufacturer's instructions) into the solution. Stir with a stir bar.
[0154] Titrate with a standard aqueous alkali solution (0.5 N or 0.1 N KOH solution) and record the burette and pH meter readings. An adequate amount of alkali may be added to bring the pH of the solution to about 8. Add the alkali in 1.0 mL increments until the change in pH per increment of the added amount is about 0.3 pH units. Reduce the addition of the alkali to less than 0.1 mL until passing the endpoint as indicated by a significant decrease in pH units per 0.1 mL added. Continue the titration in 1.0 mL increments until the inflection point is clearly defined.
[0155] Determine the inflection point (the point of maximum change in pH per 1 mL of the alkali solution) to the nearest 0.05 mL by plotting the pH readings against the milliliters of alkali used. (To increase accuracy, the expected pH per 1 mL may be plotted against the pH, and the peak corresponds to the inflection point.) The inflection point is considered the endpoint of the titration.
[0156] The acid value of the sample, expressed as milligrams of KOH per 1 gram of the sample, is as follows: Acid value = (A × N × 56.1) / B where A = the volume of the alkali solution (mL) required for the sample titration; N = the normality of the alkali solution, and B = the sample weight (grams), and round to the nearest integer may be reported.
[0157] Color Grade Test Method (Gardner Color) If available, the color grade (Gardner color) of the vegetable rosin provided by the manufacturer / supplier must be used.
[0158] If not available from the manufacturer / supplier, the color grade (Gardner color) shall be measured in accordance with ASTM D6166-12 (Reapproved 2016), “Standard Test Method for Color of Pine Chemicals and Related Products (Instrumental Determination of Gardner Color),” approved on December 1, 2016 and published in December 2016. The method is summarized here.
[0159] Measure the transmitted color and report the color of the liquid sample using an instrument such as a Gardner Color Comparator L, 115V (e.g., BYK) that can measure and report in Gardner color (or, although less preferably, in a color system convertible to Gardner color by a known method such as those disclosed in ASTM D6166-12). Calibrate the instrument according to the manufacturer's instructions.
[0160] To prepare the rosin material for color analysis, introduce the molten sample of the rosin material into a glass cuvette (10 mm path unless otherwise specified by the instrument manufacturer). If the sample is solid, it shall contain freshly broken chunks and shall not contain dust or finely divided material. The solid shall be melted (e.g., in an oven, sand bath, or oil bath for less than 15 minutes) taking care to avoid overheating and introduction of air bubbles. The measurement shall be made while the sample is still molten after introducing the molten sample into the glass cuvette. If turbidity is observed in the material, it shall be filtered.
[0161] Insert the glass cuvette into the instrument and measure the color according to the manufacturer's instructions.
[0162] Flash Point Test Method If available, the flash point of the vegetable rosin provided by the manufacturer / supplier shall be used.
[0163] If not available from the manufacturer / supplier, the flash point shall be measured in accordance with ASTM D92-18, "Standard Test Methods for Flash and Fire Points by Cleveland Open Cup Tester," approved on July 1, 2018, and published in July 2018.
[0164] Test method for determining the amount of the main rosin acid isomers If available, the amount of the main rosin acid isomers of the vegetable rosin provided by the manufacturer / supplier shall be used.
[0165] If not available from the manufacturer / supplier, the amount of the main rosin acid isomers shall be measured in accordance with ASTM D5974-15, "Standard Test Method for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas Chromatography," approved on July 1, 2015, and published in August 2015. The method is summarized here.
[0166] This method uses gas chromatography to measure, for example, the amount of rosin acid present in a rosin sample. Prior to chromatographic separation, a specific free acid must be converted to a more volatile and more stable methyl ester. For rosin acids, this conversion may be carried out with tetramethylammonium hydroxide (TMAH).
[0167] To prepare the methyl ester, dissolve the rosin sample (if solid, freshly break to avoid oxidation) in 0.5 - 3.0 mL of a 50:50 ether / methanol mixture (and optionally 2 - 3 drops of toluene), and add 2 - 3 drops of phenolphthalein indicator solution. Titrate the mixture to pH 7.9 - 8.1 using a 6% solution of TMAH or until the first persistent pink color. If over-titrated, the mixture may be back-titrated with a 5% acetic acid in methanol solution (v / v). When injecting the solution into the heated injection port of the chromatograph, the tetramethylammonium salt is pyrolyzed to the methyl ester.
[0168] Use a gas chromatograph (GC) equipped with a flame ionization detector (FID) and operate under the following conditions: column temperature (oven temperature) - initial 150 °C; hold for 5 minutes; ramp 5 °C / min; final 250 °C; hold for 10 minutes; injection port temperature 300 °C; injection port liner, glass split; detector temperature 325 °C; carrier gas, helium; gas linear velocity, 19.5 - 20.5 cm / s; split ratio, maximum 100:1; detector (FID); hydrogen, 30 mL / min; air, 400 mL / min; makeup gas, 30 mL / min. Preferably use a high-resolution column with a length of 30 m, an inner diameter of 0.32 mm, and a film thickness of 0.20 μm of a cyanopropylsiloxane type liquid.
[0169] Prepare calibration standards of myristic acid and high-purity standards of rosin acids expected to be present, record the weights and convert to methyl esters as described above. To prepare the test sample, accurately weigh approximately 50 mg of the sample and approximately 15 mg of myristic acid into a suitable vial, record the weights and convert the methyl esters as described above.
[0170] Calibrate the GC using calibration standards (injected at 0.5 - 1.0 μL), record the retention times, and calculate the individual relative response factors. To analyze the test sample, inject 0.5 - 1.0 μL (dilute the sample with additional solvent if necessary), obtain the peak areas of all required peaks from the chromatogram, and calculate the absolute values of each target peak. The relative percentage of each methyl abietate present may be measured by dividing the peak area of the measured methyl abietate by the sum of the peak areas of all methyl abietates.
[0171] Method for treating fabric When treating fabric with the compositions described in the present disclosure in the following experiments, unless otherwise indicated, follow the following method. For each treatment, load the washing machine (e.g., Miele) with a fabric load of approximately 3 kg. The fabric load includes approximately 1065 g of cotton jersey fabric and approximately 1065 g of polyester - cotton fabric (50 / 50). Additionally, the fabric load includes 20 terry towel tracers weighing approximately 870 g in total. Conduct the washing cycle at 95°C.
[0172] Before the test treatment, pre - condition the load twice using 79 g of an odorless IEC A - type detergent (ex WFK, Testgewebe GmbH) with a short cotton cycle at 95°C each time, followed by two additional 95°C washes without detergent.
[0173] For the test treatment, wash the load using a short cotton cycle at 40°C and a spin speed of 1200 rpm with 79 g of IEC A - type detergent, which is added to the appropriate dispenser at the start of the washing cycle. Add a 40 mL dose of the test fabric treatment composition to the appropriate dispenser.
[0174] Method for determining the headspace concentration above the treated fabric At least two specific touch points: - WFO (Wet Fabric Odor or WET): Analyze the wet fabric after the fabric treatment method is completed. -DFO (Dry Fabric Odor or DRY): The fabric tracer by the above-described fabric treatment method was analyzed by headspace analysis in which the dried fabric was analyzed after line drying the fabric in a sealed room for approximately 24 hours.
[0175] Use the SPME headspace GC / MS (Gas Chromatography-Mass Spectrometry) method to analyze the headspace on the terry cotton tracer. Transfer a 4 cm × 4 cm aliquot of the cotton tracer to a 25 mL headspace vial. Equilibrate the fabric sample at 65 °C for 10 minutes. Sample the headspace above the fabric with SPME (50 / 30 μm DVB / Carboxen / PDMS) for 5 minutes. Subsequently, thermally desorb the SPME fiber online into the GC. Analyze the analytes by GC / MS in full scan mode. The HS response of the total fragrance and the fragrance headspace composition at the top of the test leg can be measured.
[0176] Viscosity method Use a Brookfield DV-E viscometer to measure the viscosity of the liquid composition. Automatically rotate the spindle at a speed of 60 rpm until a stable value in centipoise (cP) is obtained.
[0177] Measure the viscosity of the premix containing the vegetable rosin, the delivery agent, and the potential emulsifier using a Thermo Scientific HAAKE MARS with a 60 mm, 1-degree cone and a gap size of 52 micrometers. The shear viscosity at 20 s -1 is obtained from a logarithmic shear rate sweep from 0.01 s -1 to 1200 s -1 at 21 °C. The viscosity may be expressed in centipoise (cP).
[0178] Particle size measurement Depending on the relative diameter of the particles, use one of two methods: image analysis if the volume-weighted median particle diameter of the population is approximately 10 μm or greater, or microscopic analysis if the volume-weighted median particle diameter of the population is less than 10 μm. These methods are described in more detail below.
[0179] A. Image analysis The volume-weighted median particle diameter is calculated from images obtained from samples flowing through flow cells of various sizes. This instrument is specifically designed for image analysis devices for liquid applications (Occhio FC200S). The sample is pumped through a syringe pump that flows through the flow cell very slowly, and an image is acquired at a set time point while the sample passes through the flow cell. The speed matches the frame rate of the camera and depends on the behavior of the sample and the particles it contains. The flow cell sizes used were 250 μm and 500 μm and depended on the size of the capsules. Detection of the capsules is performed via a grayscale threshold. Pixels are read using Callisto version 2013.13 software, and size and shape parameters are calculated. The size descriptor used is the ISO area diameter.
[0180] The illumination is a red LED light source, and the illumination was adjusted manually until appropriate grayscale detection of the particles was possible. The hardware magnification depends on the size of the particles and is 6x or 9x.
[0181] B. Microscopy The volume-weighted median particle diameter of the particles is calculated from the values obtained by observing and measuring the diameters of approximately 900 capsules obtained from randomly sampled aliquots using a microscope. The microscope used is a Leica DM6000B. The magnification of the microscope is set to 200x. The output obtained after analysis by microscopy is (1) a list of the detected diameters and (2) the count for each detected diameter size.
[0182] Therefore, the volume (V) of each particle is given by the following equation:
[0183]
Equation
Example
[0184] The examples provided below are intended to be illustrative in nature and not limiting.
[0185] Example 1. Exemplary Vegetable Rosin Materials Table 1 shows various commercially available vegetable rosin materials. Additional information is provided where available.
[0186]
Table 2
[0187] Example 2. Exemplary Liquid Fabric Conditioning Products Containing Particles The LFE formulation in Table 2A below is an example of a liquid fabric softener product containing particles. An exemplary liquid fabric conditioning product is prepared by adding a fragrance and a vegetable rosin material to the base composition with a premix containing the fragrance and glycerol ester resin in a 50:50 weight ratio.
[0188]
Table 3
[0189] a. Microscopy A micrograph of the liquid product composition is taken with a confocal laser scanning microscope (CLSM) at a magnification of 63x. Figure 1 shows a representative micrograph, and particles with a diameter of approximately 5 - 14 microns are visible.
[0190] For at least the following reasons, it is considered that the vegetable rosin material and the fragrance are arranged in the same location in the particles. First, the particles are visible under an optical / confocal microscope. The fragrance can be stained with coumarin, and it is observed that the fragrance is arranged in the same location as the particles by using different filters and detectors on the microscope. Furthermore, the presence of the rosin material in the particles is confirmed by squeezing the particles on a microslide. When sufficient pressure is applied to collapse the particles, the rosin (observed to be a viscous / sticky material) can be identified at the same position as the fragrance.
[0191] b. Product headspace Furthermore, the fragrance concentration in the headspace of the product composition can be analyzed. It has been found that there is less fragrance in the headspace of the formulation containing the rosin / fragrance premix compared to the formulation without rosin. This indicates that the rosin interacts with the fragrance and prevents it from evaporating from the formulation into the headspace.
[0192] c. Particle size Additionally, the presence of capsules in the final liquid fabric softener product (e.g., generally following the formula in Table 2A, the amount varies as shown below) can be evaluated by the particle size characterization method described in the test methods section. Depending on the size range of the particles, one of two methods: image analysis or microscopy, is used.
[0193] Legs 1, 2, and 3 differ in terms of the amounts of resin, fragrance, and emulsifier, and the amounts in the percentages provided below are based on the weight of the final product ("FP"). For Legs 1 and 2, the presence of large particles required an image analysis method, but for Leg 3, since the particles were relatively small, microscopy was preferred. Table 2B presents the particle diameters at various points of the weight-weighted particle size distribution (PSD). For each of the three legs, the median particle diameter (50% weight-weighted distribution) is reported in Table 2B.
[0194] [Table 4]
[0195] As shown in Table 3, a relatively large number of vegetable rosin materials tend to produce relatively large particles; for example, see Leg 1 versus Leg 2. Additionally, the presence of an emulsifier such as Surfadone™ is thought to promote the formation of relatively small particles.
[0196] Example 3. Ratio of Vegetable Rosin to Beneficial Agent As shown in Table 3, prepare the following rosin / fragrance premixes. The weight percentages are based on the weight of the premix composition.
[0197] Provide the premixes at levels that provide the same total amount of fragrance to the liquid fabric softener (LFE) base composition, and the total amount of fragrance present in the resulting liquid fabric (LFE) composition is 0.6 wt%. Use the resulting liquid conditioning product to treat the fabric according to the method provided above.
[0198] Use headspace analysis to evaluate the dry fabric odor (DFO), and present the results in Table 3.
[0199] [Table 5]
[0200] As shown in Table 3, the amount of fragrance (nM / L) in the DFO headspace increases as the amount of vegetable rosin material in the premix increases.
[0201] Additionally, polarized transmitted light is used at a magnification of 10 times to obtain micrographs of the final liquid conditioning products prepared with premixes 1, 2, 3, and 4. As shown in Figure 2A, no particles are visible in the liquid composition prepared with premix 1 that does not contain vegetable rosin material. As shown in Figures 2B - 2D, the particles are present in a visible state in the liquid compositions prepared with premixes 2 (Figure 2B), 3 (Figure 2C), and 4 (Figure 2D). Furthermore, the particles are considered to be relatively large in the compositions containing premixes with a relatively large amount of vegetable rosin material. For example, please check the micrographs of the products prepared with premix 3 (Figure 2C) and premix 4 (Figure 2D).
[0202] Example 4. Effect of refreshingness Hereinafter, a liquid fabric (LFE) - based composition described in Table 4A is provided.
[0203] [Table 6] 1 Diester quaternary ammonium compound (Ci - DEEDMAC = ditallow oil ethoxy ester dimethyl ammonium chloride [MDEA - based, methyl diethanolamine - based quaternary ammonium salt, available from Evonik]). 2 FLOSOFT (trademark) FS 222 (former SNF Floerger (registered trademark))
[0204] As shown in Table 4B, the following rosin / fragrance premixes are prepared, and some contain emulsifiers. The weight percentages are based on the weight of the premix composition.
[0205] [Table 7]
[0206] Prepare various liquid fabric conditioning products with the premix of Table 4B and add them to the composition of Table 4A. For each leg, prepare a similar product with only fragrance added (no premix, no vegetable rosin material), and use this as a reference product. Add the premix of Table 4B in an amount that delivers the same amount of fragrance as the reference product (no premix, no vegetable rosin material). The premix can be added to the composition of Table 4A during Ultraturrax® overhead mixing or during mixing with Ultraturrax®.
[0207]
Table 8
[0208] Use the products to treat the fabric according to the method provided above, and measure the dry fabric odor (DFO) for each. Report the formulation of the LFE composition in Table 4B.
[0209] The results are presented in Table 4D below. Additionally, Table 4D shows "Delta DFO". This indicates the difference between the DFO scores of the product containing the premix of Table 4B and the product containing only fragrance. Further, the "DFO ratio" is the ratio of the two DFO scores for that leg. Relatively high Delta DFO scores and DFO ratios indicate that the formulation containing the premix provides a refreshing effect compared to the fragrance-only formulation.
[0210] Additionally, notes regarding dispersibility are provided for the premix based on observations made while attempting to disperse the premix in the LFE-based composition. Premix 16 was not tested.
[0211]
Table 9
[0212] Additionally, some micrographs of the liquid fabric conditioning product are presented in FIGS. 3A, 3B, and 3C. The micrographs are taken with a confocal laser scanning microscope (CLSM) at a magnification of 63x. The figures show 63x micrographs of samples of the premix-containing product from leg A (FIG. 3A), leg D (FIG. 3B), and leg G (FIG. 3C). Particles can be identified in each of the products.
[0213] The dimensions and values disclosed herein should not be understood to be strictly limited to the exact numerical values recited. Instead, unless otherwise indicated, each such dimension is intended to mean both the recited value and the functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".
[0214] All documents cited herein, including any patents or patent applications that are cross-referenced or related, and any patent application or patent for which this application claims priority or the benefit thereof, are hereby incorporated by reference in their entirety, unless expressly excluded or limited. The citation of any document is not to be construed as an admission that it is prior art to any invention disclosed or claimed herein, nor that it alone or in combination with any other reference(s) teaches, suggests, or discloses any such invention. Further, in the event of any conflict between the meaning or definition of any term in this document and the same term in any document incorporated by reference, the meaning or definition given to the term in this document shall apply.
[0215] Although 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 present invention. Accordingly, it is intended that all such changes and modifications within the scope of the present invention be covered by the appended claims.
Claims
1. A liquid fabric care composition comprising particles and auxiliary components, wherein the particles contain a vegetable rosin material and one or more beneficial agents, wherein the one or more beneficial agents contain an aromatic material, and the vegetable rosin material is present in an amount of 60% by weight or more of the total amount of the vegetable rosin material and the beneficial agent, the liquid fabric care composition.
2. The liquid fabric care composition according to claim 1, wherein the particles have a volume-weighted median particle diameter of 10 microns to 400 microns.
3. The liquid fabric care composition according to claim 1 or 2, wherein the vegetable rosin material and the one or more beneficial agents are present in the particles in a weight ratio of 5:95 to 95:
5.
4. The liquid fabric care composition according to any one of claims 1 to 3, wherein the vegetable rosin material contains a material selected from the group consisting of gum rosin, wood rosin, tall oil rosin, derivatives thereof, and mixtures thereof.
5. The liquid fabric care composition according to any one of claims 1 to 4, wherein the vegetable rosin material contains at least 50% by weight of abietic acid type acids, derivatives of abietic acid type acids, or mixtures thereof.
6. The liquid fabric care composition according to claim 1, wherein the aromatic material contains 1% to 40% by weight of the aromatic material, a fragrance raw material in the first quadrant having a boiling point lower than 250°C and a logP lower than 3, and / or 60% to 99% by weight of the aromatic material that is not a fragrance raw material in the first quadrant.
7. The liquid fabric care composition according to any one of claims 1 to 6, wherein the one or more beneficial agents are encapsulated in and / or partially embedded in the vegetable rosin material.
8. The liquid fabric care composition is formed by a process comprising adding a premix to a base composition, wherein the premix contains the vegetable rosin material and the one or more beneficial agents, the liquid fabric care composition according to any one of claims 1 to 7.
9. The liquid fabric care composition according to any one of claims 1 to 8, wherein the auxiliary component contains a surfactant system, a fabric softener, or a combination thereof.
10. The liquid fabric care composition according to any one of claims 1 to 9, wherein the liquid fabric care composition contains at least 8% by weight of water.
11. The liquid fabric care composition has a viscosity of 20 s -1 and 1 to 1500 centipoises (1 to 1500 mPa * s) at 21°C, and relates to the liquid fabric care composition according to any one of claims 1 to 10.
12. The liquid fabric care composition according to any one of claims 1 to 11, further comprising a structuring agent.
13. The liquid fabric care composition according to any one of claims 1 to 12, wherein the liquid fabric care composition is a fabric detergent composition, a fabric conditioning composition, or a mixture thereof.
14. A method of treating a fabric, the method comprising contacting the fabric with the liquid fabric care composition according to any one of claims 1 to 13, optionally in the presence of water.
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