Structured aqueous compositions having dispersed liquid benefit agent droplets

Abstract

Aqueous compositions, sprayable compositions containing the aqueous compositions, and methods for making the aqueous compositions are provided. The aqueous compositions include an aqueous phase and liquid benefit agent droplets dispersed discontinuously throughout the aqueous phase. The aqueous phase has a structurant system including a first polysaccharide and a second polysaccharide different from the first polysaccharide. The aqueous phase includes less than 10,000 ppm of surfactant. The aqueous compositions exhibit a yield stress as measured by a rheological test method.

Description

[Technical Field]

[0001] SUMMARY The present disclosure relates to phase-stable aqueous compositions having suspended liquid benefit agent droplets and products for spraying the phase-stable aqueous compositions. [Background technology]

[0002] There is consumer demand for sprayable products containing various liquid benefit agents (e.g., fragrances, conditioning oils) to treat a wide variety of surfaces. Consumers may also be interested in easily portable sprayable products for use outside the home or business. Consumers seek phase-stable aqueous compositions to prevent bulk separation of the liquid benefit agents, ensuring the first and last sprays are identical and eliminating the need to shake the product before use. Additionally, some uses may require minimal residue left on surfaces, especially where unsightly stains or unpleasant properties may result. Consumers may also prefer specific spray characteristics with respect to parameters such as spray droplet size, cone angle, and flow rate.

[0003] Liquid benefit agents can be water-insoluble. Emulsification may be used to stabilize water-insoluble liquid benefit agents in aqueous compositions. Emulsification is generally a method of dispersing a liquid benefit agent from bulk raw materials into discrete droplets in an aqueous composition using surfactants and / or emulsifiers. However, surfactants are not always successful in emulsifying liquid benefit agents, and high concentrations of surfactants may be required to emulsify certain liquid benefit agents. Additionally, consumers are increasingly seeking products made from natural ingredients. There is an overall consumer trend away from the use of chemicals and toward natural materials for safety, sustainability (etc.). Many surfactants and / or emulsifiers may not be classified or considered as natural ingredients. Summary of the Invention [Problem to be solved by the invention]

[0004] Therefore, there is a need for sprayable, phase-stable aqueous compositions having suspended liquid benefit agent droplets, and methods for making the phase-stable aqueous compositions. Further, there is a need for sprayable, phase-stable natural aqueous compositions having suspended liquid benefit agents, and methods for making the phase-stable aqueous compositions. [Means for solving the problem]

[0005] An aqueous composition is provided. The aqueous composition comprises an aqueous phase and liquid benefit agent droplets dispersed uniformly and discontinuously throughout the aqueous phase. The aqueous phase comprises a structurant system comprising a first polysaccharide and a second polysaccharide different from the first polysaccharide. The aqueous phase comprises less than 10,000 ppm of surfactant. The aqueous composition exhibits a yield stress as measured by a rheological test method.

[0006] A method of formulating an aqueous composition is provided, comprising the steps of dispersing a structurant system in water to form a concentrate, the structurant system comprising a first polysaccharide and a second polysaccharide different from the first polysaccharide; mixing a liquid benefit agent with the concentrate to form liquid benefit agent droplets dispersed throughout the concentrate; and diluting the concentrate with additional water to form an aqueous composition, wherein the concentration of the structurant system in the concentrate is greater than the concentration of the structurant system in the aqueous composition. [Brief explanation of the drawings]

[0007] [Figure 1]

[0023] Figure 1 is a schematic diagram of the compositions of the present invention, as well as the composition and method of manufacture. In the direct emulsification route (left), raw materials are combined and mixed to create the composition. The emulsification route of the present invention (right) requires two steps: (1) an emulsification step and 2) a dilution step. The emulsification step utilizes a concentrate to facilitate emulsification of a liquid benefit agent; the dilution step further dilutes the concentrate to arrive at the composition. DETAILED DESCRIPTION OF THE INVENTION

[0008] The present invention may be more readily understood by reference to the following detailed description of exemplary and preferred compositions. It is understood that the claims are not limited to the specific products, methods, conditions, devices, or parameters described herein, and that the terms used herein are not intended to limit the claimed invention. Also, as used in this specification, including the appended claims, the singular forms "a," "an," and "the" include the plural, and reference to a particular numerical value includes at least that particular value unless the content clearly dictates otherwise. When a range of values ​​is expressed, another embodiment includes from the one particular value and / or to the other particular value. Similarly, when a value is expressed as an approximation, by use of the antecedent "about," it is understood that the particular value constitutes another embodiment. All ranges are inclusive and combinable. All percentages and ratios used herein are by weight of total product, and all measurements were made at 25°C unless otherwise specified.

[0009] The following definitions may be useful in understanding this disclosure.

[0010] The "aqueous phase" comprises water, polysaccharides, and minor ingredients.

[0011] "Minor components" include water-soluble components in the aqueous phase. These include salts, organics such as glycerin and propylene diol, solvents, and / or low levels of surfactants.

[0012] "Liquid benefit agent" or "LBA" means a water-insoluble material that is liquid at 25°C and provides benefit to surfaces such as fabric, hair, and skin.

[0013] "Liquid benefit agent droplets" means droplets of liquid benefit agent that are completely surrounded by an aqueous phase. Droplets of liquid benefit agent that float on the surface of an aqueous phase are not "liquid benefit agent droplets."

[0014] A "concentrate" comprises a portion of the aqueous phase containing minor ingredients, liquid benefit agents, and polysaccharides, and has a higher solids content than the final product composition, facilitating emulsification of the liquid benefit agents into stable droplets.

[0015] By "substantially free," it is meant that the component is not intentionally incorporated into the composition, but may be included in the composition as a by-product or contaminant of another component.

[0016] "Essential oil" means a concentrated hydrophobic liquid containing volatile (defined as "a substance that tends to evaporate") aromatic compounds from a plant. Essential oils are also known as volatile oils, ethereal oils, aetherolea, or simply extracted plant oils, e.g., clove oil, peppermint oil, etc.

[0017] "Natural oils" are derived from renewable plant resources.

[0018] "Solid particles" means particles.

[0019] "ppm" means 1 mg / L = 1 ppm.

[0020] The aqueous composition of the present disclosure comprises a plurality of liquid benefit agent droplets and a structurant system for suspending the liquid benefit agent droplets. Because the structurant system can suspend the liquid benefit agent droplets, the aqueous composition may be free of, or substantially free of, surfactants. The aqueous composition may be sprayable. The aqueous composition may be phase stable, meaning that the liquid benefit agent droplets remain suspended in the aqueous composition for extended periods of time, eliminating the need to shake the product before use. The aqueous composition may be used in the air or on a surface by application from a spray dispenser, and / or to remove or reduce the amount of malodor in the air or on a surface, and / or to deliver a benefit agent into the air or on a surface. The product may comprise a spray dispenser containing the aqueous composition.

[0021] By incorporating a structurant system to suspend the liquid benefit agent droplets in the aqueous composition, the aqueous composition exhibits a yield stress. The yield stress of the aqueous composition prevents the liquid benefit agent droplets from phase separating.

[0022] It has been found that the method of combining structurant system with liquid benefit agent affects the phase stability of composition.In the typical emulsification method using surfactant as emulsifier, all raw materials are combined and mixed at once to make emulsified composition.However, it has been found that by preparing a concentrate of aqueous phase that contains water at a concentration lower than that of the final aqueous composition, a stable aqueous composition of liquid benefit agent droplets that are discontinuously dispersed throughout the aqueous phase can be obtained.

[0023] Without being bound by theory, it is believed that increasing the viscosity of the concentrate to a similar or substantially similar level to the viscosity of the liquid benefit agent, at least during the emulsification process, allows for liquid benefit agent droplets of a small enough droplet size for the aqueous composition to maintain phase stability. As the viscosities of the aqueous phase concentrate and liquid benefit agent differ from one another, the resulting liquid benefit agent droplets become larger and the aqueous composition becomes less phase stable. As the viscosities of the aqueous phase concentrate and liquid benefit agent approach one another, the aqueous composition becomes phase stable and maintains phase stability even when further diluted with water to form a more easily sprayable aqueous composition.

[0024] spray dispenser The sprayable product may include a container of the aqueous composition within a spray dispenser. The spray dispenser may include a bottle for containing the aqueous composition and a spray engine.

[0025] The spray engine can be configured in various ways, such as a direct compression trigger sprayer, a pre-pressure trigger sprayer, or an aerosol spray dispenser. One suitable spray dispenser is the TS800 trigger sprayer (Exxon Mobil PP1063, material classification 10003913, manufacturer: Calmar).

[0026] Another suitable spray engine is a continuous action sprayer such as the FLAIROSOL™ dispenser manufactured by Afa Dispensing Group, which includes a pre-pressurized spray engine and aerosol-like pressurizer for aqueous compositions using a pressure or buffer chamber.

[0027] A wide variety of trigger or finger pump sprayers are suitable for use with the aqueous compositions of the present invention. These are readily available from suppliers such as Calmar, Inc. (City of Industry, Calif.); CSI (Continental Sprayers, Inc.), St. Peters, Mo.; Berry Plastics Corp., Evansville, Ind., and Guala® sprayer dispensers; or Seaquest Dispensing, 30 Cary, Ill. Preferred trigger sprayers are the blue insert Guala® sprayer available from Berry Plastics Corp., or the Calmar TS800-1A®, TS1300®, and TS-800-2® available from Calmar Inc., due to their fine, uniform spray characteristics, spray volume, and pattern size. Sprayers with pre-pressure capabilities and finer spray characteristics and uniform distribution, such as the Japanese Yshino sprayer, are more preferred. Any suitable bottle or container can be used with the trigger sprayer. A recommended bottle is a 1740 fluid ounce bottle (approximately 500 ml) with good ergonomics, similar in shape to the Cinch® bottle. It can be made of any material, such as high-density polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyethylene terephthalate, glass, or any other material that can be used to form a bottle. Preferably, it is made of 45 high-density polyethylene or clear polyethylene terephthalate.

[0028] For smaller fluid ounce sizes (such as 1-8 ounces for illustrative purposes only), a finger pump can be used with a canister or cylindrical bottle. A preferred pump for this application is the cylindrical Euromist II® pump manufactured by Seaquest Dispensing. More preferred are those with a pre-load feature.

[0029] The bottle may be configured as a container having a base and a sidewall terminating in an opening. The bottle may comprise a bag-in-bag or bag-in-can container.

[0030] The bottle may be large to contain hundreds of grams of aqueous composition as a current fabric treatment spray. Alternatively, the bottle may be small to contain tens of grams of aqueous composition and can be carried in a purse or pocket for application of the aqueous composition while traveling or in between trips. The bottle may have a longest dimension of less than 20 cm, preferably less than 10 cm, and most preferably less than 5 cm. The bottle may hold from 0.1 milliliters ("mL") to 50 mL, more preferably from 1 mL to 30 mL, and most preferably from 1 mL to 20 mL.

[0031] When the spray dispenser is configured as an aerosol, the spray dispenser can be pressurized with a propellant. Any suitable propellant can be used.

[0032] aqueous composition The aqueous compositions of the present invention comprise an aqueous phase and a plurality of liquid benefit agent droplets dispersed discontinuously throughout the aqueous phase. The aqueous phase comprises an aqueous carrier, a structurant system, and minor ingredients. The aqueous compositions can be formulated by first forming a concentrate comprising at least one aqueous phase and a structurant system. The concentrate can also comprise minor ingredients. A liquid benefit agent is then mixed with the concentrate to form liquid benefit agent droplets dispersed discontinuously throughout the concentrate. The concentrate with the liquid benefit agent droplets can then be diluted with additional aqueous phase while maintaining the phase stability of the aqueous composition. The additional aqueous phase can comprise water, a structurant system, and / or minor ingredients.

[0033] structurant system In particular, the structurant system may be in the form of a polysaccharide system. Preferred polysaccharides include xanthan gum, glucomannan gum, galactomannan gum, and combinations thereof. Glucomannan may be derived from natural gums such as konjac gum. Galactomannan may be derived from natural gums such as locust bean gum or tara gum. Polysaccharides may also include carrageenan. One or more polysaccharides may be modified, such as by deacetylation. Xanthan gum may be acetylated.

[0034] The aqueous composition may include a polysaccharide system including at least two polysaccharides, such as a first polysaccharide and a second polysaccharide. The first polysaccharide may be xanthan gum. The second polysaccharide may be selected from the group consisting of glucomannan, galactomannan, and combinations thereof. The second polysaccharide may be selected from the group consisting of konjac gum, locust bean gum, tara gum, and combinations thereof.

[0035] Without being bound by theory, it is believed that two or more polysaccharides exhibit synergistic bonding, such that bonding between sites on different polysaccharides is stronger than bonding between sites on the same polysaccharide, producing a structurant system capable of suspending liquid benefit agent droplets.

[0036] The first polysaccharide may comprise 10% to 80% by weight of the polysaccharide system; the second polysaccharide may comprise 20% to 90% by weight of the polysaccharide system, but more in the case of the composition.

[0037] The first polysaccharide may be present at a concentration of greater than 10% and less than 90% by weight of the polysaccharide system, alternatively from about 20% to about 80% by weight, alternatively from about 40% to about 60% by weight.

[0038] The second polysaccharide may be present at a concentration of from about 15% to about 85% by weight of the polysaccharide system, alternatively from about 20% to about 80% by weight, alternatively from about 40% to about 60% by weight.

[0039] The total concentration of polysaccharides present in the aqueous composition can be greater than about 0.1 wt%, or preferably greater than about 0.2 wt%, or preferably greater than about 0.3 wt%, more preferably greater than 0.4 wt%, and most preferably greater than 0.5 wt%. Without being bound by theory, it is believed that the higher the overall concentration of polysaccharides in the aqueous composition, the higher the viscosity and the better the emulsification of the liquid benefit agent, which in turn provides a higher yield stress, preventing coalescence and bulk separation of the liquid benefit agent.

[0040] The polysaccharide may have a weight average molecular weight in the range of about 10,000 daltons to about 15,000,000 daltons, preferably about 200,000 daltons to about 10,000,000 daltons, more preferably about 500,000 daltons to about 9,000,000 daltons, more preferably about 750,000 daltons to about 8,000,000 daltons, more preferably about 1,000,000 daltons to about 7,000,000 daltons, more preferably about 2,000,000 daltons to about 6,000,000 daltons, and more preferably about 3,500,000 daltons to about 6,000,000 daltons.

[0041] The polysaccharides may be characterized by their acetylation rate. The acetylation rate of one or more of the polysaccharides in the structurant system may be in the range of about 5.0 to about 0.2, preferably in the range of about 3.5 to about 0.3, preferably in the range of about 2.0 to about 0.35, preferably in the range of about 1.5 to about 0.37, preferably in the range of about 1.0 to about 0.39.

[0042] The aqueous composition may have a total protein concentration of less than about 100 parts per million (ppm), preferably less than 50 ppm, preferably less than 25 ppm, more preferably less than 10 ppm. It may be desirable to limit the total protein concentration in the aqueous composition to minimize discoloration of the surface to which the aqueous composition is applied.

[0043] Liquid Benefit Agent Droplets The aqueous composition may comprise a plurality of droplets of liquid benefit agent suspended in an aqueous phase. In the air or on product surfaces, the liquid benefit agent may be a fragrance that provides freshness, such as reduced malodors or improved fragrance, to surfaces such as furniture, carpets, and curtains. In hair products, the liquid benefit agent may be a silicone oil that provides benefits such as feel, deodorization, and anti-static. In fabric treatment products, the liquid benefit agent may be a liquid that provides anti-wrinkle benefits and / or freshness. The liquid benefit agent may comprise a material selected from the group consisting of unprocessed fragrances; waxes such as silicone oils and polyethylene waxes; essential oils such as fish oil, jasmine, camphor, and lavender; skin cooling agents such as menthol, methyl lactate; glycerin, and the like; and mixtures thereof.

[0044] Suitable benefit agents are available from Givaudan Corp. (Mount Olive, New Jersey, USA), International Flavors & Fragrances Corp. (South Brunswick, New Jersey, USA), or Firmenich Company (Geneva, Switzerland).

[0045] Liquid benefit agents may include materials used to provide specific conditioning benefits to hair and / or skin. In hair compositions, suitable liquid benefit agents include those that provide one or more benefits related to shine, softness, combability, anti-static properties, wet manageability, damage, manageability, volume, and greasiness.

[0046] Suitable liquid benefit agents include conditioning agents, such as hair conditioners, skin conditioners, or fabric conditioners, such as silicones, petrolatum, hydrocarbon oils (e.g., mineral oil), natural and synthetic waxes (e.g., microcrystalline wax), paraffin, ozokerite, polyethylene, polybutene, polydecene, pentahydrosqualene, vegetable oils, triglycerides, fats and oils, and combinations thereof. Furthermore, the liquid benefit agent may be or include a perfume oil. Some liquid benefit agents suitable for use herein are described below.

[0047] The liquid benefit agent droplets may be small enough to form a stable suspension. For example, the liquid benefit agent droplets may have a diameter of 300 micrometers (μm) or less, or 200 μm or less, or 100 μm or less, or 75 μm or less, or 40 μm or less, or 30 μm or less, or 20 μm or less, as measured by the Droplet Size Test Method described below. The liquid benefit agent droplets may comprise one type of liquid benefit agent or may comprise a combination of two or more different liquid benefit agents.

[0048] The concentration of the liquid benefit agent in the concentrate and final composition must be sufficient to produce the desired effect. Such concentration can vary depending on the liquid benefit agent, the desired performance, the type and concentration of other ingredients, and other similar factors. However, increasing the concentration of the liquid benefit agent will affect the concentration of the structuring agent system required to suspend the liquid benefit agent. Therefore, it may be desirable to limit the concentration of the liquid benefit agent in the concentrate and final aqueous composition to some extent.

[0049] The concentration of the liquid benefit agent droplets in the concentrate may be 20% by weight or less, or 10% by weight or less, or 6% by weight or less, or 4% by weight or less, or 2% by weight or less, or 1% by weight or less, or 0.2% by weight or less.

[0050] The concentration of the liquid benefit agent droplets in the final aqueous composition may be 5% by weight or less, or 4% by weight or less, or 3% by weight or less, or 2% by weight or less, or 1% by weight or less, or 0.4% by weight or less, or 0.2% by weight or less.

[0051] The liquid benefit agent droplets may have a viscosity in the range of 0.001 mPa·s to 5000 mPa·s, more preferably less than 2500 mPa·s, more preferably less than 1000 mPa·s, more preferably less than 500 mPa·s, more preferably less than 100 mPa·s, more preferably less than 10 mPa·s, as measured by the LBA test method viscosity.

[0052] silicone The liquid benefit agent of the aqueous composition of the present invention can be a water-insoluble silicone.The silicone can include volatile silicone, non-volatile silicone, or a combination thereof.A non-volatile silicone conditioning agent is preferred.When volatile silicone is present, it is typically used as a solvent or carrier for commercially available non-volatile silicone material components such as silicone gums and resins.The silicone can include a silicone fluid conditioning agent, and can also include other components, such as silicone resins, to improve the deposition efficiency of silicone fluids or enhance the gloss of surfaces.

[0053] Suitable silicones are selected from the group consisting of siloxanes, silicone gums, aminosilicones, amino-terminated silicones, alkylsiloxane polymers, cationic organopolysiloxanes, and mixtures thereof.

[0054] Liquid benefit agents may include one or more silicones, including high molecular weight polyalkyl or polyaryl siloxanes and silicone gums, low molecular weight polydimethylsiloxane fluids, and aminosilicones.

[0055] The high molecular weight polyalkyl or polyaryl siloxanes and silicone gums have a viscosity at 25°C of about 100,000 mPa·s to about 30,000,000 mPa·s, or about 200,000 mPa·s to about 30,000,000 mPa·s, and a molecular weight of about 100,000 Daltons to about 1,000,000 Daltons, or about 120,000 Daltons to about 1,000,000 Daltons.

[0056] Preferred higher molecular weight silicone compounds useful herein include polyalkylsiloxanes or polyarylsiloxanes having the following structure:

[0057] [ka] In the formula, R 93 is alkyl or aryl, and p is an integer of about 1,300 to about 15,000, more preferably about 1,600 to about 15,000. 8 represents a group that caps the end of the silicone chain. The alkyl or aryl group (R 93 ) or an alkyl or aryl group Z substituted at the end of the siloxane chain 8 The Z may have any structure so long as the resulting silicone remains fluid at room temperature, is dispersible, is non-irritating, non-toxic or otherwise harmful when applied to a surface, is compatible with the other ingredients of the aqueous composition, is chemically stable under normal conditions of use and storage, is capable of adhering to hair, and conditions the surface. 8 Groups include hydroxy, methyl, methoxy, ethoxy, propoxy, and aryloxy. Two R on the silicon atom 93 The groups may represent the same or different groups. Preferably, two R 93 The groups represent the same group. 93Groups include methyl, ethyl, propyl, phenyl, methylphenyl and phenylmethyl.Preferred silicone compounds are polydimethylsiloxane, polydiethylsiloxane and polymethylphenylsiloxane.Particularly preferred is polydimethylsiloxane, also known as dimethicone.Commercially available silicone compounds useful herein include, for example, those available from General Electric Company under TSF451 series and those available from Dow Corning under Dow Corning SH200 series.

[0058] Silicone compounds that can be used herein can also include silicone gums. As used herein, the term "silicone gum" refers to polyorganosiloxane materials having a viscosity of 1,000,000 mPa·s or greater at 25°C. It is recognized that the silicone gums described herein may have some overlap with the silicone compounds disclosed above. This overlap is not intended to limit any of these materials. "Silicone gums" typically have a mass molecular weight greater than about 165,000, generally from about 165,000 to about 1,000,000. Specific examples include polydimethylsiloxane, poly(dimethylsiloxane-methylvinylsiloxane) copolymer, poly(dimethylsiloxane-diphenylsiloxane-methylvinylsiloxane) copolymer, and mixtures thereof. Commercially available silicone gums useful herein include, for example, TSE200A and CF330M, available from General Electric Company.

[0059] Lower molecular weight silicones have a viscosity at 25° C. of about 1 mPa·s to about 10,000 mPa·s, or about 5 mPa·s to about 5,000 mPa·s, and a molecular weight of about 400 to about 65,000, or about 800 to about 50,000.

[0060] Preferred lower molecular weight silicone compounds useful herein include polyalkylsiloxanes or polyarylsiloxanes having the following structure:

[0061] [ka] In the formula, R 93 is an alkyl group or an aryl group, and p is an integer of about 7 to about 850, more preferably about 7 to about 665. 8 represents a group that caps the end of the silicone chain. The alkyl or aryl group (R 93 ) or an alkyl or aryl group Z substituted at the end of the siloxane chain 8 The Z may have any structure so long as the resulting silicone remains fluid at room temperature, is dispersible, is non-irritating, non-toxic or otherwise harmful when applied to a surface, is compatible with the other ingredients of the aqueous composition, is chemically stable under normal conditions of use and storage, is capable of adhering to hair, and conditions the surface. 8 Groups include hydroxy, methyl, methoxy, ethoxy, propoxy, and aryloxy. Two R on the silicon atom 93 The groups may represent the same or different groups. Preferably, two R 93 The groups represent the same group. 93 Groups include methyl, ethyl, propyl, phenyl, methylphenyl and phenylmethyl.Preferred silicone compounds are polydimethylsiloxane, polydiethylsiloxane and polymethylphenylsiloxane.Particularly preferred is polydimethylsiloxane, also known as dimethicone.Commercially available silicone compounds useful herein include, for example, those available from General Electric Company under TSF451 series and those available from Dow Corning under Dow Corning SH200 series.

[0062] The liquid benefit agent of the present invention may contain one or more aminosilicones. The aminosilicones provided herein are silicones containing at least one primary amine, secondary amine, tertiary amine, or quaternary ammonium group. Preferred aminosilicones may have less than about 0.5% by weight of the aminosilicone, more preferably less than about 0.2% by weight, more preferably less than about 0.1% by weight of nitrogen. The higher the concentration of nitrogen (amine functional group) in the aminosilicone, the less friction reduction occurs, and as a result, the conditioning effect from the aminosilicone tends to be reduced. It should be understood that in some product forms, higher concentrations of nitrogen are also acceptable according to the present invention.

[0063] The aminosilicones can have a viscosity of from about 1,000 centipoise ("cP") to about 100,000 cP, or from about 2,000 cP to about 50,000 cP, or from about 4,000 cP to about 40,000 cP, or from about 6,000 cP to about 30,000 cP. The viscosity of the aminosilicones described herein is measured at 25°C.

[0064] The aminosilicone may be included in the aqueous composition of the present invention at a concentration of from about 0.5% to about 30% by weight, or from about 1.0% to about 24% by weight, or from about 2.0% to about 16% by weight, or from about 3.0% to about 8% by weight.

[0065] Examples of preferred aminosilicones for use in the present invention include, but are not limited to, those conforming to the general formula (I): (R 1 ) a G 3-a -Si-(-OSiG2) n -(-OSiG b (R 1 ) 2-b ) m -O-SiG 3-a (R 1 ) a (I) In the formula, G is hydrogen, phenyl, hydroxy, or C1-C8 alkyl, preferably methyl; a is 0 or an integer having a value of 1 to 3, preferably 1; b is 0, 1, or 2, preferably 1; a is 0 and b is not 2; n is a number from 0 to 1,999; m is an integer from 0 to 1,999; the sum of n and m is a number from 1 to 2,000; neither a nor m is 0; 1 is the general formula CqH 2q L, where q is an integer having a value of 2 to 8, and L is -N(R 2 )CH2-CH2-N(R 2 )2, -N(R 2 )2, -N(R 2 ) + 3A - , -N(R 2 )CH2-CH2-NR 2 H2A - , wherein R 2 is hydrogen, phenyl, benzyl, or a saturated hydrocarbon group, preferably from about C1 to about C 20 is an alkyl group of the formula A - is a halide ion.

[0066] As used herein, some silicones may include aminosilicones corresponding to formula (I) where m=0, a=1, q=3, G=methyl, n is preferably about 1500 to about 1700, more preferably about 1600, and L is -N(CH3)2 or -NH2, more preferably -NH2. Other aminosilicones may include those corresponding to formula (I) where m=0, a=1, q=3, G=methyl, n is preferably about 400 to about 600, more preferably about 500, and L is -N(CH3)2 or -NH2, more preferably -NH2. Because one or both ends of the silicone chain are terminated with a nitrogen-containing group, these aminosilicones are sometimes referred to as terminal aminosilicones.

[0067] An exemplary aminosilicone corresponding to formula (I) is the polymer known as "trimethylsilylamodimethicone," shown below in formula (II):

[0068] [ka] In the formula, n is a number from 1 to 1,999, and m is a number from 1 to 1,999.

[0069] The silicone may also be an amino-terminated silicone. As defined herein, "amino-terminated silicone" refers to a silicone polymer containing one or more amino groups at one or both ends of the silicone backbone. The hydrophobic coating may be substantially free of any silicone compounds other than the amino-terminated silicone.

[0070] The amino group at at least one end of the silicone backbone of the amino-terminated silicone may be selected from the group consisting of primary amines, secondary amines, and tertiary amines. The amino-terminated silicone may conform to Formula III: (R1) a G 3-a -Si-(-OSiG2) n -O-SiG 3-a (R1) a (III) wherein G is hydrogen, phenyl, hydroxy, or C1-C8 alkyl, preferably methyl; a is an integer having a value of 1 to 3 or is 1; b is 0, 1, or 2 or is 1; n is a number from 0 to 1,999; and R1 is a group of the general formula CqH 2q L is a monovalent radical according to the formula: where q is an integer having a value of 2 to 8, and L is -N(R2)CH2-CH2-N(R2)2, -N(R2)2, -N(R2)3A - , -N(R2)CH2-CH2-NR2H2A - wherein R2 is hydrogen, phenyl, benzyl, or a saturated hydrocarbon group; -is a halide ion. R2 can be an alkyl group having 1 to 20 carbon atoms, or 2 to 18 carbon atoms, or 4 to 12 carbon atoms.

[0071] Suitable terminal amino silicones corresponding to Formula III have a = 1, q = 3, G = methyl, n is about 1000 to about 2500, or about 1500 to about 1700, and L is -N(CH3)2. Suitable terminal amino silicones corresponding to Formula III have a = 0, G = methyl, n is about 100 to about 1500, or about 200, and L is one of the following groups: -N(R2)CH2-CH2-N(R2)2, -N(R2)2, -N(R2)3A. - , -N(R2)CH2-CH2-NR2H2A - wherein R2 is hydrogen, phenyl, benzyl, or a saturated hydrocarbon group; - is a halide ion, or L is -NH2. R2 can be an alkyl group having 1 to 20 carbon atoms, or 2 to 18 carbon atoms, or 4 to 12 carbon atoms. The terminal amino silicone can be selected from the group consisting of bis-aminomethyl dimethicone, bis-aminoethyl dimethicone, bis-aminopropyl dimethicone, bis-aminobutyl dimethicone, and mixtures thereof.

[0072] Suitable amino-terminated silicones include aminopropyl-terminated polydimethylsiloxane (e.g., having a viscosity of 4,000-6,000 cSt (4-6 Pa·s); available from Gelest, Inc. under the trade name DMS-A35), polydimethylsiloxane, trimethylsiloxy-terminated (e.g., having a viscosity of 5,000 cSt (5 Pa·s); available from Gelest, Inc. under the trade name DMS-T35), polydimethylsiloxane, trimethylsiloxy-terminated (e.g., having a viscosity of 1,000 cSt (1 Pa·s); available from Gelest, Inc. under the trade name DMS-T31), aminopropyl-terminated polydimethylsiloxane (e.g., having a viscosity of 1,000 cSt (1 Pa·s); available from Gelest, Inc. under the trade name DMS-T31), Examples of suitable siloxanes include polydimethylsiloxanes, trimethylsiloxy-terminated (e.g., having a viscosity of 50 cSt (0.05 Pa·s); available from Gelest, Inc. under the trade name DMS-T15), aminopropyl-terminated polydimethylsiloxanes (e.g., having a viscosity of 50 cSt (0.05 Pa·s); available from Gelest, Inc. under the trade name DMS-A15), bis-aminopropyl dimethicone (e.g., having a viscosity of 10,220 cSt (10.2 Pa·s); available from Momentive Performance Materials Inc.), and mixtures thereof.

[0073] Alkylsiloxane Polymer Suitable conditioning agents as benefit agents in the hydrophobic coating further include alkylsiloxane polymers, as described in detail in U.S. Patent Application Publication Nos. 2011 / 0243874(A1), 2011 / 0243875(A1), 2011 / 0240065(A1), 2011 / 0243878(A1), 2011 / 0243871(A1), and 2011 / 0243876(A1).

[0074] Cationic organopolysiloxane Suitable conditioning agents as benefit agents in the hydrophobic coating further include cationic organopolysiloxanes, as described in detail in U.S. Patent Application Publication No. 2014 / 0030206(A1), WO 2014 / 018985(A1), WO 2014 / 018986(A1), WO 2014 / 018987(A1), WO 2014 / 018988(A1), WO 2014 / 018989(A1).

[0075] organic oil The liquid benefit agents of the present invention may include at least one organic conditioning oil as the conditioning agent, either alone or in combination with other conditioning agents such as silicones.

[0076] The hydrocarbon-based benefit material comprises an average carbon chain length of greater than 20, or an average carbon chain length of greater than 30, or an average carbon chain length of greater than 40.

[0077] hydrocarbon oil Organic oils suitable for use as liquid benefit agents in the aqueous compositions of the present invention include, but are not limited to, hydrocarbon oils having at least about 10 carbon atoms, such as cyclic hydrocarbons, straight chain aliphatic hydrocarbons (saturated or unsaturated), and branched chain aliphatic hydrocarbons (saturated or unsaturated), including polymers thereof and mixtures thereof. Straight chain hydrocarbon oils preferably have at least about C 12 ~About C 19 Branched chain hydrocarbon oils (including hydrocarbon polymers) typically contain more than 19 carbon atoms.

[0078] Specific, non-limiting examples of these hydrocarbon oils include paraffin oil, mineral oil, saturated and unsaturated dodecane, saturated and unsaturated tridecane, saturated and unsaturated tetradecane, saturated and unsaturated pentadecane, saturated and unsaturated hexadecane, polybutene, polyisobutylene, polydecene, and mixtures thereof. Branched-chain isomers of these compounds and long-chain hydrocarbons can also be used, including highly branched, saturated or unsaturated alkanes, such as permethyl-substituted isomers of hexadecane and eicosane, such as 2,2,4,4,6,6,8,8-dimethyl-10-methylundecane and 2,2,4,4,6,6-dimethyl-8-methylnonane (available from Permethyl Corporation). Hydrocarbon polymers, such as polybutene and polydecene. A preferred hydrocarbon polymer is polybutene, such as a copolymer of isobutylene and butene. A commercially available material of this type is L-14 polybutene from Amoco Chemical Corporation. The concentration of such hydrocarbon oils in the aqueous composition may range from about 0.05% to about 20% by weight, alternatively from about 0.08% to about 1.5% by weight, alternatively from about 0.1% to about 1% by weight.

[0079] Polyolefin Organic oils for use as liquid benefit agents can include liquid polyolefins, more preferably liquid poly-α-olefins, more preferably hydrogenated liquid poly-α-olefins. Polyolefins for use herein range from C4 to about C 14 Preferably about C6 to about C 12 It is prepared by polymerizing olefinic monomers.

[0080] Non-limiting examples of olefinic monomers for use in preparing the polyolefin liquids herein include ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-octene, 1-decene, 1-dodecene, 1-tetradecene, branched chain isomers of 4-methyl-1-pentene, and mixtures thereof. Olefin-containing refinery feedstocks or effluents are also suitable for preparing polyolefin liquids. Preferred hydrogenated α-olefin monomers include, but are not limited to, 1-hexene to 1-hexadecene, 1-octene to 1-tetradecene, and mixtures thereof.

[0081] fatty acid esters Other suitable organic oils for use as conditioning agents in the aqueous compositions of the present invention include, but are not limited to, fatty acid esters having at least 10 carbon atoms. These fatty acid esters include esters with hydrocarbyl chains derived from fatty acids or alcohols (e.g., monoesters, polyhydric alcohol esters, and di- and tri-carboxylic acid esters). The hydrocarbyl groups of the fatty acid esters herein may contain or be covalently bonded to other compatible functional groups, such as amide and alkoxy moieties (e.g., ethoxy or ether linkages).

[0082] Specific examples of preferred fatty acid esters include isopropyl isostearate, hexyl laurate, isohexyl laurate, isohexyl palmitate, isopropyl palmitate, decyl oleate, isodecyl oleate, hexadecyl stearate, decyl stearate, isopropyl isostearate, dihexyldecyl adipate, lauryl lactate, myristyl lactate, cetyl lactate, oleyl stearate, oleyl oleate, oleyl myristate, lauryl acetate, cetyl propionate, and oleyl adipate, but are not limited to these.

[0083] Other fatty acid esters suitable for use in the aqueous compositions of the present invention are monocarboxylic acid esters of the general formula R'COOR, where R' and R are alkyl or alkenyl groups, and the total number of carbon atoms in R' and R is at least 10, preferably at least 22.

[0084] Still other fatty acid esters suitable for use in the aqueous compositions of the present invention are esters of C4 to C8 dicarboxylic acids (e.g., C1 to C8 dicarboxylic acids of succinic acid, glutaric acid, and adipic acid). 22 and preferably C1-C6 esters). Specific non-limiting examples of di- and tri-alkyl and alkenyl esters of carboxylic acids include isocetyl stearoyl stearate, diisopropyl adipate, and tristearyl citrate.

[0085] Other fatty acid esters suitable for use in the aqueous compositions of the present invention are known as polyhydric alcohol esters, including alkylene glycol esters such as ethylene glycol mono- and di-fatty acid esters, diethylene glycol mono- and di-fatty acid esters, polyethylene glycol mono- and di-fatty acid esters, propylene glycol mono- and di-fatty acid esters, polypropylene glycol monooleate, polypropylene glycol 2000 monostearate, ethoxylated propylene glycol monostearate, glyceryl mono- and di-fatty acid esters, polyglycerol polyfatty acid esters, ethoxylated glyceryl monostearate, 1,3-butylene glycol monostearate, 1,3-butylene glycol distearate, polyoxyethylene polyol fatty acid esters, sorbitan fatty acid esters, and polyoxyethylene sorbitan fatty acid esters.

[0086] Still other fatty acid esters suitable for use in the aqueous compositions of the present invention are glycerides, including, but not limited to, mono-, di-, and triglycerides, preferably di- and tri-glycerides, and more preferably triglycerides. When used in the aqueous compositions described herein, glycerides are preferably a mixture of glycerol and C 10 ~C 22 These are mono-, di-, and tri-esters of long-chain carboxylic acids such as carboxylic acids. A variety of these types of materials can be derived from vegetable and animal fats and oils such as castor oil, safflower oil, cottonseed oil, corn oil, olive oil, cod liver oil, almond oil, avocado oil, palm oil, sesame oil, lanolin, and soybean oil. Synthetic oils include, but are not limited to, triolein and tristearin glyceryl dilaurate.

[0087] Other fatty acid esters suitable for use in the aqueous compositions of the present invention are water-insoluble synthetic fatty acid esters. Some preferred synthetic esters conform to the general formula (IX):

[0088] [ka] In the formula, R 1 is a C7-C9 alkyl, alkenyl, hydroxyalkyl, or hydroxyalkenyl group, preferably a saturated alkyl group, more preferably a saturated straight chain alkyl group; n is a positive integer having a value of 2 to 4, preferably 3; and Y is an alkyl, alkenyl, hydroxy- or carboxy-substituted alkyl or alkenyl having from about 2 to about 20 carbon atoms, preferably from about 3 to about 14 carbon atoms. Other preferred synthetic esters conform to the general formula (X):

[0089] [ka] In the formula, R 2 is C8~C 10It is an alkyl, alkenyl, hydroxyalkyl, or hydroxyalkenyl group, preferably a saturated alkyl group, more preferably a saturated straight chain alkyl group, and n and Y are as defined above in formula (X).

[0090] Specific non-limiting examples of synthetic fatty acid esters suitable for use in the aqueous compositions of the present invention include P-43 (C8-C6 fatty acid esters of trimethylolpropane) and P-43 (C8-C6 fatty acid esters of trimethylolpropane). 10 triester), MCP-684 (tetraester of 3,3-diethanol-1,5-pentanediol), MCP121 (C8-C adipic acid 10 diesters), all of which are available from Mobil Chemical Company.

[0091] Metathesized Unsaturated Polyol Ester Other suitable organic oils as benefit agents include metathesized unsaturated polyol esters. Exemplary metathesized unsaturated polyol esters and their starting materials are described in U.S. Patent Application Publication No. 2009 / 0220443(A1). Metathesized unsaturated polyol esters refer to products obtained when one or more unsaturated polyol ester components are subjected to a metathesis reaction. Metathesis is a catalytic reaction involving the exchange of alkylidene units between compounds containing one or more double bonds (i.e., olefinic compounds) through the formation and cleavage of carbon-carbon double bonds. Metathesis can occur between two identical molecules (often referred to as self-metathesis) and / or between two different molecules (often referred to as cross-metathesis).

[0092] Silane-modified oil Other suitable organic oils as liquid beneficial agent include silane-modified oil.Generally, suitable silane-modified oil comprises a hydrocarbon chain selected from the group consisting of saturated oil, unsaturated oil and their mixture, and a hydrolyzable silyl group covalently bonded to the hydrocarbon chain.Suitable silane-modified oil is described in detail in U.S. Patent Application No. 61 / 821,818 filed on May 10, 2013.

[0093] Other liquid benefit agents Also suitable for use in the aqueous compositions herein are the liquid benefit agents described in U.S. Patent Nos. 5,674,478 and 5,750,122 by Procter & Gamble Company.Also suitable for use herein are the liquid benefit agents described in U.S. Patent Nos. 4,529,586 (Clairol), 4,507,280 (Clairol), 4,663,158 (Clairol), 4,197,865 (L'Oreal), 4,217,914 (L'Oreal), 4,381,919 (L'Oreal), and 4,422,853 (L'Oreal).

[0094] fragrance The hydrophobic benefit agents of the present invention may also include one or more fragrances. The one or more fragrances may be selected from any fragrance or fragrance chemical suitable for topical application to the particular surface being treated. The concentration of fragrance in the personal care composition should be effective to provide a desired fragrance, including but not limited to unscented. Generally, the concentration of the primary fragrance is from about 0.5% to about 30%, or from about 1% to about 20%, or from about 2% to about 10%, or from about 3% to about 8% of the solid article.

[0095] The fragrance may be selected from the group consisting of perfumes, highly volatile fragrance materials having a boiling point below about 250° C., and mixtures thereof. The fragrance may be selected from fragrance ingredients having a high impact accord, having a ClogP greater than about 2 and an odor detection threshold of 50 parts per billion (ppb) or less.

[0096] Water-based carrier The aqueous composition may include an aqueous carrier. The aqueous carrier used may be distilled water, deionized water, or tap water. Water may be present in any amount in the aqueous composition. The water may be present in an amount of about 85% to 99.5% by weight of the composition, preferably about 90% to about 99.5% by weight, more preferably about 92% to about 99.5% by weight, more preferably about 95% by weight. Water containing small amounts of low molecular weight monohydric alcohols, such as ethanol, methanol, and isopropanol, or polyols such as ethylene glycol and propylene glycol, may also be useful.

[0097] Trace ingredients The composition may include one or more minor ingredients in the aqueous phase selected from the group consisting of buffers, solubilizers, antimicrobial compounds, preservatives, malodor counteractants, fragrance delivery technologies, diluents, antioxidants, water-soluble metal salts including zinc salts, copper salts, antistatic agents; pest repellents; colorants, and combinations thereof.

[0098] The aqueous composition may contain a substantially low concentration of a solubilizing aid to solubilize any excess hydrophobic organic materials, particularly certain malodor-reducing materials, fragrance materials, as well as optional ingredients that may be added to the aqueous composition to produce a clear, translucent solution and that are not readily soluble in the aqueous composition (e.g., pest repellents, antioxidants, etc.). Suitable solubilizing aids are surfactants, such as non-foaming or low-foaming surfactants. Suitable surfactants are nonionic surfactants, cationic surfactants, amphoteric surfactants, zwitterionic surfactants, and mixtures thereof. When present, the solubilizing aid is preferably a nonionic surfactant.

[0099] The aqueous composition can contain nonionic surfactants, cationic surfactants, and mixtures thereof. The aqueous composition can contain ethoxylated hydrogenated castor oil. One suitable hydrogenated castor oil that can be used in the aqueous composition is sold under the trademark Basophor (available from BASF).

[0100] If the aqueous composition contains a surfactant, the total amount of surfactant present in the aqueous composition is less than 10,000 ppm, preferably less than 1,000 ppm, and most preferably less than 100 ppm. The aqueous composition may be substantially free of surfactant. Alternatively, the aqueous composition may not contain an effective amount of surfactant. As used herein, an "effective amount of surfactant" is the amount of surfactant in the aqueous composition such that the surfactant acts as an emulsifier between the liquid benefit agent droplets and the aqueous carrier.

[0101] The buffering agent may include a carboxylic acid, a dicarboxylic acid such as maleic acid, or a polybasic acid such as citric acid, or a polyacrylic acid.

[0102] Non-limiting examples of surface tension reducing agents of this type are described in U.S. Patent No. 5,714,137 and include Silwet® surfactants available from Momentive Performance Chemical, Aliquid benefit agent, New York. Exemplary Silwet surfactants are as follows:

[0103] [Table 1]

[0104] Water-soluble antimicrobial compounds include organic sulfur compounds, halogenated compounds, cyclic organic nitrogen compounds, low molecular weight aldehydes, quaternary compounds, dehydroacetic acid, phenyl and phenoxy compounds, or mixtures thereof.

[0105] Quaternary compounds may also be used. Examples of commercially available quaternary compounds suitable for use in the aqueous compositions include Barquat, available from Lonza Corporation; and quaternary didecyldimethylammonium chloride, available from Lonza Corporation under the trade name Bardac® 2250.

[0106] The perfume delivery technology may be selected from the group consisting of pro-perfumes, polymer particles, soluble silicones, polymer-assisted delivery, molecule-assisted delivery, fiber-assisted delivery, amine-assisted delivery, cyclodextrins, starch-encapsulated accords, zeolites, and inorganic carriers, and mixtures thereof.

[0107] solid particles The aqueous composition may include a plurality of solid particles, which may be in the form of mesoporous particles, activated carbon, zeolites, benefit agent delivery particles, waxes, hydrogels, crushed nutshells, and / or combinations thereof.

[0108] The solid particles may be in the form of benefit agent delivery particles. The benefit agent delivery particles may include a wall material that encapsulates the benefit agent. The benefit agent may be referred to herein as a "benefit agent" or an "encapsulated benefit agent." The benefit agent may be selected from the group consisting of a perfume blend, an insect repellent, a malodor counteractant, and combinations thereof. Benefit agents include 3-(4-t-butylphenyl)-2-methylpropanal, 3-(4-t-butylphenyl)-propanal, 3-(4-isopropylphenyl)-2-methylpropanal, 3-(3,4-methylenedioxyphenyl)-2-methylpropanal, and 2,6-dimethyl-5-heptenal, α-damascone, β-damascone, γ-damascone, β-damascenone, 6,7-dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanone, methyl-7,3-dihydro-2H-1,5-benzodioxepin-3-one, 2-[2-(4-methyl-3-cyclohexenyl-1-yl)propyl]cyclohexyl The material may be selected from the group consisting of: perfume raw materials such as pentan-2-one, 2-sec-butylcyclohexanone, and β-dihydroionone, linalool, ethyl linalool, tetrahydrolinalool, and dihydromyrcenol; waxes such as silicone oil and polyethylene wax; essential oils such as fish oil, jasmine, camphor, and lavender; skin coolants such as menthol, methyl lactate; vitamins such as vitamin A and E; sunscreen; glycerin; catalysts such as manganese catalyst or bleach catalyst; bleach particles such as perborate; silicon dioxide particles; antiperspirant active substances; cationic polymers, and mixtures thereof.Suitable benefit agents can be obtained from Givaudan Corp. (Mount Olive, New Jersey, USA), International Flavors & Fragrances Corp. (South Brunswick, New Jersey, USA), or Firmenich Company (Geneva, Switzerland).

[0109] The benefit agent, as described herein, can include materials that are liquid benefit agents. In such instances, the aqueous composition may include liquid benefit agent droplets dispersed discontinuously throughout the aqueous phase, in addition to encapsulated liquid benefit agents dispersed throughout the aqueous phase.

[0110] In one aspect, the perfume delivery technology may include benefit agent delivery particles made by at least partially encasing a benefit agent with a wall material.

[0111] The wall material of the benefit agent delivery particle may include melamine, polyacrylamide, silicone, silica, polystyrene, polyurea, polyurethane, polyacrylate-based materials, polyacrylic ester-based materials, gelatin, styrene-malic anhydride, polyamide, aromatic alcohol, polyvinyl alcohol, and mixtures thereof. Melamine wall materials may include melamine cross-linked with formaldehyde, melamine-dimethoxyethanol cross-linked with formaldehyde, and mixtures thereof. Polystyrene wall materials may include polystyrene cross-linked with divinylbenzene. Polyurea wall materials may include urea cross-linked with formaldehyde, urea cross-linked with glutaraldehyde, polyisocyanate reacted with polyamide, polyamine reacted with aldehyde, and mixtures thereof. Polyacrylate-based wall materials may include polyacrylates formed from methyl methacrylate / dimethylaminomethyl methacrylate, polyacrylates formed from amine acrylate and / or methacrylate and strong acids, polyacrylates formed from carboxylic acid acrylate and / or methacrylate monomers and strong bases, polyacrylates formed from amine acrylate and / or methacrylate monomers and carboxylic acid acrylate and / or carboxylic acid methacrylate monomers, and mixtures thereof.

[0112] Polyacrylate-based wall materials may include polyacrylates formed with alkyl and / or glycidyl esters of acrylic and / or methacrylic acid, polyacrylates formed with acrylic and / or methacrylic acid esters having hydroxy and / or carboxy groups and allyl gluconamide, and mixtures thereof.

[0113] The aqueous composition may contain any amount of particles. With respect to benefit agent delivery particles, the aqueous composition may contain from about 0.001% to about 2.0% by weight of the aqueous composition of the benefit agent comprising the wall material of the benefit agent delivery particle. Alternatively, the aqueous composition may contain from about 0.01% to about 1.0% by weight of the aqueous composition, or most preferably from about 0.05% to about 0.5% by weight of the aqueous composition of the benefit agent comprising the wall material of the benefit agent delivery particle.

[0114] The aqueous compositions of the present invention may be hair conditioner compositions, which may include one or more liquid benefit agents that are water-insoluble hydrophobic conditioning agents, such as silicones, organic oils, or other water-insoluble conditioning agents.

[0115] The hair conditioner composition may also include a gel matrix that includes a combination of a cationic surfactant and a high melting point fatty alcohol (above 25°C).

[0116] Non-limiting examples of high melting point fatty alcohols include ethyl alcohol, stearyl alcohol, behenyl alcohol, and mixtures thereof. An exemplary hair conditioning composition of the present invention is provided in Example 1.

[0117] [Table 2]

[0118] Manufacturing method As noted above, it has been discovered that the method of making the aqueous composition of the present invention results in a phase-stable aqueous composition comprising a structurant system and an aqueous phase comprising liquid benefit agent droplets dispersed discontinuously throughout the aqueous phase. Formation of a phase-stable discontinuous phase of liquid benefit agent droplets in the final aqueous composition requires at least two steps: an emulsification step and a dilution step.

[0119] In the emulsification process, the liquid benefit agent is emulsified into a concentrate. The concentrate includes some or all of the structurant system, some water, and optionally some or all minor ingredients. The concentrate is first formed by mixing the structurant system, water, and any minor ingredients. The liquid benefit agent is then emulsified into the concentrate using vigorous mixing. Without being bound by theory, the concentrate has a relatively high concentration of the structurant system, with a viscosity set to substantially match that of the liquid benefit agent to effectively disperse the liquid benefit agent. Furthermore, the ratio and concentration of polysaccharides are selected to ensure a yield stress exists, which eliminates drainage between droplets in the concentrate and ensures stability against creaming and coalescence of the droplets. Both considerations are necessary to surprisingly enable the formation of a stable emulsion of liquid benefit agent droplets without the need for surfactants or with very low concentrations of surfactants.

[0120] In a dilution step, the concentrate containing the liquid benefit agent droplets is then diluted with additional water to form the final aqueous composition. Along with the additional water, additional structurant systems and / or minor ingredients may also be added to the concentrated aqueous phase. Subsequent dilution of the concentrate has been found to have no effect on the stable suspension of the liquid benefit agent droplets formed in the concentrate in the aqueous phase.

[0121] A variety of mixers can be used to mix the liquid benefit agent into the concentrated aqueous phase. The mixer can be a high-speed mixer, a static mixer, an overhead mixer, or other mixers. Preferably, a high-speed mixer can be used to form the liquid benefit agent droplets. However, any mixer is suitable as long as it applies sufficient mixing to disperse the liquid benefit agent into liquid benefit agent droplets.

[0122] To emulsify the liquid benefit agent in the concentrate, the viscosity of the concentrate, as measured by rheological test methods, can be from 10 Pa·s to 0.00 Pa·s, more preferably from 1 Pa·s to 0.01 Pa·s, more preferably from 1 Pa·s to 0.1 Pa·s, and most preferably from 1 Pa·s to 0.3 Pa·s. The concentrate should exhibit a yield stress of greater than 2 Pa to 0 Pa, more preferably from 1.5 Pa to 0.02 Pa, more preferably from 1.0 Pa to 0.05 Pa, and most preferably from 1 Pa to 0.3 Pa, as measured by rheological test methods.

[0123] The aqueous composition comprises from 0.1% to 20% by weight of the liquid benefit agent droplets, more preferably from 10% to 0.2%, more preferably from 5% to 0.5%, most preferably from 5% to 0.5% by weight.

[0124] The achievement of emulsification process is determined by droplet size of liquid benefit agent, liquid benefit agent on the surface of preparation, and stability.Most preferred aqueous composition has a diameter of liquid benefit agent droplets of less than about 500 μ m, most preferably less than about 250 μ m, most preferably less than about 100 μ m, as evidenced by the turbidity in the preparation; there is essentially only a small amount of liquid benefit agent on the surface of the preparation after 24 hours of preparation; there is no instability in the preparation, as evidenced by the bulk separation of liquid benefit agent.Preferred aqueous composition has a diameter of liquid benefit agent droplets of less than about 500 μ m, most preferably less than about 250 μ m, most preferably less than about 100 μ m, as evidenced by the turbidity in the preparation; there is essentially only a small amount of liquid benefit agent on the surface of the preparation after 24 hours of preparation (estimated to be less than 5% by weight of the total mixture); there is no instability in the preparation, as evidenced by the bulk separation of liquid benefit agent. Comparative embodiments have liquid benefit agent droplet diameters greater than about 500 μm or exhibit incomplete dispersion as evidenced by the relative transparency of the formulation; there is significant liquid benefit agent present at the surface of the formulation at 24 hours of manufacture (estimated to be greater than 5% by weight of the total mixture); and there is significant instability in the formulation as evidenced by bulk segregation of the liquid benefit agent. The dilution step achieves delivery of liquid benefit agent droplets having comparable droplet sizes to the most preferred or preferred aqueous compositions.

[0125] Test Method Rheological Testing Methods To measure the yield stress and / or viscosity of a sample (e.g., a concentrate or aqueous composition, but not an LBA), measurements are performed using a TA Discovery HR-2 Hybrid Rheometer (TA Instruments, New Castle, Delaware, USA) and accompanying TRIOS software version 4.2.1.36612, or equivalent. The instrument is equipped with a concentric cylinder Double Gap Cup (e.g., TA Instruments, catalog number 546050.901), a Double Gap Rotor (e.g., TA Instruments, catalog number 546049.901), and a Split Cover (e.g., TA Instruments, catalog number 545626.001). Calibration is performed according to the manufacturer's recommendations. A cooled circulating water bath set to 25°C is attached to the concentric cylinder. The concentric cylinder temperature is set to 25°C. The temperature is monitored in the control panel until the instrument reaches the set temperature, at which time, after an additional 5 minutes to ensure equilibration, the sample material may be loaded into the Double Gap Cup.

[0126] The parameters for the Double Gap Cup are as follows: inner cup diameter is 30.2 mm, inner bob diameter is 32 mm, outer bob diameter is 35 mm, outer cup diameter is 37 mm, inner cylinder height is 55 mm, immersion height is 53 mm, operating gap is 2,000.0 μm, loading gap is 90,000.0 μm, environmental system is Peltier, and sample volume is 12 ml to 15 ml (preferably 12 ml).

[0127] To load the sample, use a syringe to add a minimum of 12 ml of sample to the Double Gap Cup, then allow the sample to sit for 15 minutes, ensuring any trapped air bubbles rise to the surface. The Double Gap Rotor is then lowered to the appropriate gap and data is collected according to the following settings and procedure:

[0128] Data is collected through a series of steps performed in exactly the following order: The sample conditioning step is performed using the following instrument settings: Set environmental control at a temperature of 25°C; Select Inherit Set Point as Off; Set Soak Time to 0.0 s; Select Wait for Temperature as On; Select Wait for axial force as Off; Set Preshear Options by selecting Perform Preshear as Off; Set Equilibrium by selecting Perform Equilibration as On and set Duration to 600.0 s.

[0129] The flow peak hold step is performed using the following instrument settings: set Environmental Control with a temperature of 25°C; select Inherit Set Point as Off; set Soak Time as 0.0 s; select Wait for Temperature as Off; set Test Parameters with a Duration of 600.0 s; select Shear Rate and set it to 0.01 s-1; select Inherit initial value as Off; select Sampling interval and set it to 3.0 s / pt; set Controlled Rate Advanced with Motor mode selected as Auto; set Data acquisition with End of step selected as Zero torque; set Fast Sampling as Off; select Save image as Off; set Step Termination with Limit checking Enabled selected as On; set Terminate step when by selecting Strain (%), selecting >, and setting to 500%; select Equilibrium Enabled as Off; and select Step Repeat Enabled as Off.

[0130] The sample conditioning step is performed using the following instrument settings: Environmental Control set at 25°C Temperature; Inherit Set Point selected as Off; Soak Time set at 10.0 s; Wait for Temperature selected as Off; Wait for axial force selected as Off; Set Preshear Options by selecting Perform Preshear as Off; Set Equilibrium by selecting Perform Equilibration as On and Duration set to 600.0 s.

[0131] The flow sweep process is performed using the following instrument settings: Set Environmental Control with a temperature of 25°C; select Inherit Set Point as Off; set Soak Time as 0.0s; select Wait For Temperature as Off; select Logarithmic Sweep and set Test Parameters; select Shear Rate and set it to 1.0e-3s-1~1000.0s-1; set Points Per Decade as 5; select Steady State Sensing as On; set Max Equilibration Time as 45.0s; set Sample Period as 5.0s; set %Tolerance as 5.0; set Consecutive Within as 3; select Scaled Time Average as Off; select Motor Mode as Auto and set Controlled Rate Advanced; select Save Point Display as Off and set Data Acquisition; select Save image as Off; select Limit Checking Enabled as Off and set Step Termination; select Equilibrium Enabled as Off; select Step Repeat Enabled as Off.

[0132] The end-of-test adjustment process is performed using the following equipment settings: Set Temperature selected as Off; Set Temperature System Idle (only if axial force management is active) selected as On.

[0133] The yield stress is calculated from the data collected during the flow peak hold step in the following manner: Plot the data points as stress (mPa) on the y-axis against step time (s) on the x-axis. The yield stress is determined by selecting the "Analysis" tab, then selecting "Signal max" from the Function drop-down list, and finally selecting "Analyze" in the Commands category. For continuous data sets (containing a single stress value greater than zero for each time value), if the "Max Y" value occurs within the first 250 seconds, the yield stress is equal to the "Max Y" value; if the "Max Y" value occurs after 250 seconds, the yield stress is equal to zero. If the measured sample is a concentrate, the value is the yield stress of the concentrate ("YS"). conc. "); if the sample being measured is an aqueous composition, the value is the yield stress ("YS aqu. "); if the yield stress was not measured, the yield stress of the concentrate and / or aqueous composition is assigned a value of "NM."

[0134] Viscosity is determined as the viscosity measured at a shear rate of 10 s-1 or at the nearest data point within 1% of a shear rate of 10 s-1 and is expressed in mPa·s. If the measured sample is a concentrate, the value is the viscosity of the concentrate ("h conc. "); if the measured sample is an aqueous composition, the value is the viscosity of the aqueous composition ("h aqu. "); if the yield stress was not measured, the viscosity of the concentrate and / or aqueous composition is assigned a value of "NM."

[0135] Viscosity according to the LBA test method Viscosity measurements of liquid benefit agents are performed using a TA Discovery HR-2 Hybrid Rheometer (TA Instruments, New Castle, Delaware, USA) and accompanying TRIOS software version 4.2.1.36612, or equivalent. The instrument is equipped with a 60 mm stainless steel cone with a 2-degree angle (e.g., TA Instruments, catalog number 511606.905), a Peltier plate (TA Instruments, catalog number 533230.901). Calibration is performed according to the manufacturer's recommendations. A cooled circulating water bath set at 25°C is attached to the Peltier plate. The Peltier plate temperature is set to 25°C. The temperature is monitored in the control panel until the instrument reaches the set temperature.

[0136] To load the liquid beneficial agent (LBA), use a 5 ml slip-tip syringe or similar to transfer 2 ml of LBA onto the central surface of the Peltier plate. If the loaded sample liquid contains visible bubbles, wait 10 minutes for the bubbles to move through the sample and burst, or use a transfer pipette to extract the bubbles. If visible bubbles still remain, remove the sample from the plate, clean the plate with an isopropanol wipe, and allow the solvent to evaporate. Then, try the sample loading procedure again and repeat until the sample is successfully loaded without any visible bubbles.

[0137] The 60 mm cone is lowered to the "trim gap," which is specific to the cone for this attachment and is shown to be 66 micrometers. The cone is then locked and excess sample material is removed from around the cone using a flexible rubber spatula, such as a rubber policeman. It is important to ensure that the sample is evenly distributed around the edge of the cone and that no sample is present on the sides or top of the plate. If sample material is present on the sides or top of the cone, gently remove this excess material. If sample material is present on the sides or top of the plate, gently remove this excess material. Carefully apply the Solvent Trap Cover over the cone and lower the cone to its final position by setting the gap distance to 55 micrometers.

[0138] Data is collected through a series of steps performed in exactly the following order. The following instrument settings are used to perform the sample conditioning step: Set Environmental Control to a temperature of 25°C; Select Inherit Set Point as Off; Set Soak Time to 0.0 s; Select Wait for Temperature as On; Select Wait For Axial Force as Off; Set Preshear Options by selecting Perform Preshear as On; Set Shear Rate to 100.0 1 / s; Set Duration to 20.0 s; Set Advanced Options with Zero Speed ​​After Preshear selected to Leave; Set Zero Speed ​​Threshold as 0.1 rad / s; Select Motor mode as Auto; Set Equilibrium by selecting Perform Equilibration as On and setting Duration to 600.0 s.

[0139] The flow sweep process is performed using the following instrument settings: Set Environmental Control with a temperature of 25°C; select Inherit Set Point as Off; set Soak Time as 0.0s; select Wait For Temperature as Off; select Logarithmic Sweep and set Test Parameters; select Shear Rate and set it to 1.0e-3s-1~1000.0s-1; set Points Per Decade as 15; select Steady State Sensing as On; set Max Equilibration Time as 45.0s; set Sample Period as 5.0s; set %Tolerance as 5.0; set Consecutive Within as 3; select Scaled Time Average as Off; select Motor Mode as Auto and set Controlled Rate Advanced; select Save Point Display as Off and set Data Acquisition; select Save image as Off; select Limit Checking Enabled as Off and set Step Termination; select Equilibrium Enabled as Off; select Step Repeat Enabled as Off.

[0140] The end of test adjustment process is performed using the following equipment settings: Select Set Temperature as On; set temperature to 25°C. Select Set Temperature System Idle (only if axial force management is active) as Off.

[0141] The LBA viscosity is determined as the viscosity measured at a shear rate of 100 s-1 or at the nearest data point within 1% of a shear rate of 100 s-1. Reported LBA viscosity values ​​("h LBA") is the average of viscosity values ​​obtained from three independent viscosity measurements (i.e., three replicate sample preparations) and is expressed in units of mPa·s. If the viscosity of the sample was not measured, the LBA ("h LBA Viscosity values ​​reported for the acrylic copolymer are given a value of "NM."

[0142] Drop Size Test Method An optical microscope is used to measure the droplet size, which is the number-weighted average diameter of the liquid benefit agent droplets in the test sample of the composition. Note that the droplet size values ​​claimed herein refer to the average diameter, and the values ​​are number-weighted, not volume-weighted. A transmitted light compound microscope equipped with a digital camera and an array of flat-field objectives with 10x to 100x magnification is used to image the droplets. The microscope is adjusted for Kohler illumination and calibrated for linear measurements in the xy image plane using a stage micrometer. Suitable microscopes include a Zeiss Axio Imager (Carl Zeiss AG, Oberkochen, Germany) employing Normarski differential interference contrast (DIC) and equipped with a Zeiss AxioCam digital camera (Carl Zeiss AG, Oberkochen, Germany) or equivalent. One skilled in the art may choose to measure the diameter of the imaged droplets using image analysis software (such as AxioVision, Carl Zeiss Microscopy GmbH, Germany, or ImagePro Premier, Media Cybernetics, Rockville, Maryland, USA, or equivalent). Measurements within the image can also be made using precisely calibrated physical devices such as rulers, calipers, reticles, graticules, etc.

[0143] Before measuring their average drop size, samples should be visually inspected to ensure they are adequately emulsified, including a homogeneous distribution of the LBA. A poorly emulsified sample may exhibit one of two characteristics: 1) contain a few very large LBA droplets, causing the sample to appear nearly transparent (i.e., little turbidity), or 2) contain a visually concentrated or increased concentration of LBA near the surface of the preparation, with the LBA not being uniformly dispersed throughout the volume. If the sample appears visually adequately emulsified, measure the average drop size as described below. If the sample appears inadequately emulsified, the average drop size is not measured; instead, the final average drop size diameter value is assigned a value of "IE," for "Ineffective Emulsion."

[0144] A sample of the fully emulsified composition is used to prepare a wet-mount slide. Here, a few drops of the composition are placed on a standard or concave glass microscope slide and gently covered with a standard glass cover slip. Three wet-mount slide preparations are made. The preparations are observed under a microscope without delay, taking care to avoid applying pressure and shear forces to the cover slip as much as possible.

[0145] The prepared samples are observed under a microscope at several different magnifications to assess the range of typical and numerically most abundant droplet sizes in the sample. This assessment is used to select an objective lens that will provide an image where the diameters of the most abundant representative droplets are perfectly aligned within the captured image, as well as sufficiently magnified to allow accurate measurement of their diameters. Such images are captured until at least 10 representative droplets from each replicate sample preparation have been imaged.

[0146] The diameter of all particles that appear to be approximately round (spherical) droplets in the captured image is measured. Measurements of non-droplet objects such as air bubbles or solid microcapsules are excluded from the recorded value. An average diameter value is calculated from all droplets measured in each replicate wet mount slide preparation. Final average diameter value

[0147]

number

[0148]

number

[0149] Sprayability Test Method The sprayability of a composition is determined by measuring the angle of the spray cone produced during attempted spraying and comparing this value with that obtained from a designated negative control reference solution. Compositions are classified as either "sprayable" or "non-sprayable." Compositions typically form a visible cone-shaped plume of droplets exiting the nozzle, where the cone is narrowest closest to the nozzle and widens as the distance from the nozzle increases, before the plume of droplets finally disperses. Spray cone angle is measured by attempting to spray the composition vertically across the viewing area of ​​a recording video camera under conditions of sufficient lighting and no drafts. Images captured by the video camera are analyzed to measure the cone angle of the visible plume of sprayed material within an area extending 10 cm outward from the nozzle in the direction of the plume's trajectory. The spray cone angle is defined as the angle measured between two designated lines. One designated line is the central axis of the plume's trajectory away from the nozzle, and the other designated line is the visible upper outer margin of the plume, represented by a linear average of the first 10 cm of distance away from the nozzle.

[0150] The video camera is securely mounted to prevent movement or vibration, and is positioned, zoomed, and focused to capture a plume area extending at least 10 cm from the nozzle. One suitable video camera is the Phantom V310 (Vision Research). Lighting and background conditions are selected so that the droplet plume is easily observed with high contrast in the captured image. The composition, bottle, and environment are at ambient laboratory air temperatures of 18°C ​​to 25°C. The air conditions surrounding the nozzle and spray plume area are as constant as possible.

[0151] During analysis, each composition is dispensed from the bottle as a spray plume. The compositions are loaded into a small, handheld atomizing spray bottle with a top-push button pump activation mechanism. Such bottles include 10 mL refillable bottles commonly used by travelers to dispense fragrances or other sprayable cosmetic fluids. A suitable bottle is a dropper-stop, 10 mL aluminum silver color travel spray. To ensure the bottle tubing is primed and the nozzle is not clogged, the sample is test sprayed several times immediately before imaging with the camera. During the test, the spray activation button is manually pressed with the index finger with consistent force and speed, with the duration of the fully activated stroke progressing as quickly as possible, less than 1 second in length. A suitable interval speed is 90 seconds, with full compression in the beat. -1 Examples include synchronized compression using a metronome.

[0152] During analysis, each test composition is dispensed from the bottle as a spray plume. Two standard control solutions are also dispensed, and their spray cone angles are measured. These serve as reference values ​​for sprayable and non-sprayable performance. The negative control reference solution is a 0.1 wt% aqueous solution of a 1,000,000 dalton PEO polymer (e.g., Aldrich 372781-250G) and demonstrates unacceptable / non-sprayable performance. The positive control reference solution is deionized water and demonstrates acceptable / sprayable performance. If the spray angle is significantly greater than the negative control, the composition is given a spray grade of "sprayable." Therefore, [(spray angle composition - spray angle negative control) / (spray angle positive control - spray angle negative control)] is greater than 0.10. Otherwise, the composition is given a spray grade of "non-sprayable." In the example data provided herein, if a spray angle measurement was not performed on the sample, the composition would be given a spray grade of "NM."

[0153] Polysaccharide weight-average molecular weight test method The weight average molecular weight (Mw) of xanthan gum is measured using gel permeation chromatography with multi-angle light scattering detection (GPC-MALS). A suitable instrument is a Waters 2695 Separation Module (Waters Associates) or equivalent device, which is connected in series with a DAWN EOS 18-angle LS detector and an Optilab REX differential RI detector (Wyatt Technology).

[0154] Gum solutions were prepared by dispersing approximately 10 mg of gum material in 5 mL of purified HPLC-grade water. The sample solutions were mixed and allowed to swell overnight. Prior to GPC-MALS analysis, each sample was diluted to a concentration of 0.2 mg / mL with 0.1 M NaNO3 buffer. Samples were filtered directly into HPLC vials through 0.45 μm Nylon 66 filters (Thermo Fisher Scientific) to remove any microgels or particulate matter.

[0155] Separation is performed on two GPC columns, such as a Waters 7.8 x 300 mm Ultrahydrogel 2000 and a 7.8 x 300 mm Ultrahydrogel 250 or equivalent column connected in series, maintained at 40 °C. Components are eluted with a mobile phase of 0.1 M NaNO3 at an isocratic flow rate of 1.00 mL / min. A 50 μL sample is injected for analysis.

[0156] Data from the two detectors is collected digitally using suitable software (e.g., Wyatt Astra software). The weight average molecular weight (Mw) is calculated using the Zimm equation. A refractive index increment (dn / dc) of 0.145 mL / g, typical for xanthan gum in aqueous solution, was used for the calculation.

[0157] Polymer Acetylation Test Method Flow injection electrospray ionization quadrupole time-of-flight mass spectrometry (FI-QTOF-MS) was used to measure the ratio of acetylated to non-acetylated sugar fragments, thereby determining the relative degree of acetylation modification in the polysaccharide polymer material being tested. In this tandem mass analysis, the first quadrupole mass analyzer was set in RF-only (broadband) mode, so that all ions generated by electrospray ionization passed through this first mass filter without selecting specific precursor ions. All ions passing through the first quadrupole were then fragmented in the second quadrupole. All fragment ions were finally mass-separated and detected by the TOF mass analyzer according to their mass-to-charge ratio (m / z). For polymer or gum materials, polysaccharides were fragmented to give the structural signature ion m / z 205 (acetylated sugar) and the structural signature ion m / z 163 (non-acetylated sugar). The ratio of the peak intensity values ​​from these two mass fragments indicates the degree of acetylation present in the material being tested, with a higher ratio indicating a higher degree of acetylation.

[0158] A sample of any individual polymer raw material to be tested (e.g., konjac flour or xanthan gum) is dissolved in 1 mL of water at a concentration of 0.5 mg of polymer. The aqueous polymer sample solution is mixed and allowed to hydrate overnight. After overnight hydration, the solution is filtered through a 0.8 μm pore size filter (e.g., a Versapor acrylic copolymer membrane disc filter from Pall Corporation (Port Washington, New York, USA), or equivalent). The filtered solution is placed in an HPLC sample vial for analysis.

[0159] Flow injection-QTOF-MS analysis is performed using a suitable tandem quadrupole mass spectrometer system with electrospray ionization (such as a Q-Tof 2 instrument from Waters Corporation (Milford, Massachusetts, USA) or equivalent). The accompanying software provided by the instrument manufacturer (Mass Lynx NT version 4.1 data acquisition and processing software from Waters Corporation, or equivalent) is used to control the instrument and perform the analysis. The instrument system is configured with a delivery solvent of 5 mM ammonium acetate / 10% acetonitrile in water at a rate of 40 μL / min. No column is used with this instrument configuration. The electrospray capillary voltage is set to 3.5 kV. The first quadrupole mass analyzer is configured in RF-only (broadband) mode. To fragment the polymeric material, the second quadrupole is set at 70 V with a collision cell energy such that both signature fragment ions, namely, m / z 205 and m / z 163, are generated. The TOF mass analyzer is scanned from 50 Da to 3000 Da with a 5 minute data collection time for each flow injection run. The peak intensities of the m / z 205 fragment (i.e., acetylated sugars) and the m / z 163 fragment (i.e., non-acetylated sugars) are obtained. The ratio of these two peak intensity values ​​is calculated to represent the acetylated to non-acetylated sugar fragment ratio. This ratio indicates the relative degree of acetylation in the gum or polysaccharide polymer material being tested. [Example]

[0160] Example A

[0039] Example A of the present invention demonstrates the preparation of a fabric treatment composition having a very low viscosity perfume oil liquid benefit agent. The perfume oil is emulsified and stabilized in a product concentrate. The product concentrate is then diluted with water to form a sprayable aqueous composition.

[0161] material Ethanol (94.3%, Equistar Chemicals) Alpha Cyclodextrin (Sigma Aldrich product code C4642) Diethylene glycol (99.6%, Indorama Ventures LLC) Lactic acid, 30% active (Purac PF 90, Purac Bioquímica SA) diluted to 30% Koralone B119 (Dow Chemical Company) Konjac gum (Nutricol® XP 3464, FMC Corp) Xanthan gum (Jungbunzlauer Inc.) Hydroxypropyl beta-cyclodextrin (Cavasol W7 HP TL, 40%, Wacker Biosolution) Sodium hydroxide (50% Membrane Grade Brenntag Mid-South, Inc.), diluted to 5%; Cardamom Ginger Lemongrass Natural Fragrance (Procter & Gamble Company) Water (Millipore, 18 MW)

[0162] preparation 1% by weight xanthan gum stock solution 494.61 grams of water was added to a clean mixing vessel (1 liter glass beaker, VWR). 0.39 grams of Koralone B-119 was added to the beaker and stirred until homogeneously mixed. Using a Ross Mill mixer equipped with a mixing blade (4-blade stainless steel, 2.5 inch diameter), 5.0 grams of xanthan gum was quickly added to the beaker while mixing at 5000 RPM. As the solution thickened, the stirring speed was increased to 8000 RPM, and mixing was continued at 8000 RPM for an additional 300 seconds.

[0163] 1% by weight konjac gum stock solution 494.61 grams of water was added to a clean mixing vessel (1 liter glass beaker, VWR). 0.39 grams of Koralone B-119 was added to the vessel and stirred until homogeneously mixed. Using a Ross Mill mixer equipped with a mixing blade (4-blade stainless steel, 2.5 inch diameter), 5.0 grams of konjac gum was quickly added to the vessel while mixing at 5000 RPM. As the solution thickened, the stirring speed was increased to 8000 RPM and mixing continued at 8000 RPM for an additional 300 seconds.

[0164] Concentrates containing liquid benefit agents (Table 1) A mixing vessel (1 liter glass beaker, VWR) was thoroughly cleaned and a magnetic stir bar was added. LBA (Cardamom Ginger Lemongrass Natural Fragrance) was added to the mixing vessel. 1 wt% xanthan gum stock solution was added to the vessel. 1 wt% konjac gum stock solution was added to the vessel. The vessel was placed on a magnetic stir plate and stirred at a speed sufficient to create a vortex in the mixture. The mixture was stirred until completely homogenous.

[0165] Dilution into aqueous compositions (Table 2) Water was added to a clean mixing vessel (1-liter glass beaker, VWR). The mixture was stirred with a Ross Mill mixer equipped with a mixing blade (4-blade stainless steel, 2.5-inch diameter). The stirring speed was set high enough to create a vortex in the mixture without excessive foaming. The following materials were added to the mixing vessel in order, ensuring the mixture was homogenous after each addition: water, ethanol, Alpha CD, lactic acid, Koralone B-119, and citric acid. After 10 minutes, hydroxypropyl Beta CD was added to the vessel. The resulting mixture was trimmed with sodium hydroxide (Orion, Thermo Scientific, catalog number 2115000) until a pH of 7.4 was reached. The mixture was stirred for the final 10 minutes.

[0166] Parameter Measurement The aqueous compositions were tested according to the following methods: Determine sprayability by spray test method; The viscosity of the LBA was measured by the Viscosity of Liquid Benefit Agents Test Method.

[0167] [Table 3]

[0168] [Table 4]

[0169] Example B

[0043] Example B of the present invention demonstrates the preparation of a fabric treatment composition with a very low viscosity perfume oil liquid benefit agent. The perfume oil is emulsified and stabilized in a product concentrate. The product concentrate is then diluted with water to form a sprayable, stable aqueous composition with an acceptable average droplet size distribution.

[0170] material Ethanol (94.3%, Equistar Chemicals) Alpha Cyclodextrin (Sigma Aldrich product code C4642) Diethylene glycol (99.6%, Indorama Ventures LLC) Citric acid, 50% active (Univar) Koralone B119 (Dow Chemical Company) Konjac gum (Nutricol® XP 3464, FMC Corp) Xanthan gum (Jungbunzlauer Inc.) Hydroxypropyl beta-cyclodextrin (Cavasol W7 HP TL, 40%, Wacker Biosolution) Sodium hydroxide (50% Membrane Grade Brenntag Mid-South, Inc.) diluted to 5%; Cardamom Ginger Lemongrass Natural Fragrance (Procter & Gamble Company) Water, deionized (Millipore, 18 MW)

[0171] preparation 1% by weight xanthan gum stock solution 494.61 grams of water was added to a clean mixing vessel (1 liter glass beaker, VWR). 0.39 grams of Koralone B-119 was added to the beaker and stirred until homogeneously mixed. Using a Ross Mill mixer equipped with a 4-blade stainless steel mixing blade (2.5 inch diameter), 5.0 grams of xanthan gum was quickly added to the beaker while mixing at 5000 RPM. As the solution thickened, the stirring speed was increased to 8000 RPM and mixing continued at 8000 RPM for an additional 300 seconds.

[0172] 1% by weight konjac gum stock solution 494.61 grams of water was added to a clean main mixing vessel (1 liter glass beaker, VWR). 0.39 grams of Koralone B-119 was added to the vessel and stirred until homogeneously mixed. Using a Ross Mill mixer equipped with a mixing blade (4-blade stainless steel, 2.5 inch diameter), 5.0 grams of konjac gum was quickly added to the vessel while mixing at 5000 RPM. As the solution thickened, the stirring speed was increased to 8000 RPM and mixing continued at 8000 RPM for an additional 300 seconds.

[0173] Concentrates containing liquid benefit agents (Table 3) A mixing vessel (100 ml glass beaker, VWR) was thoroughly cleaned and a magnetic stir bar was added. LBA (Cardamom Ginger Lemongrass Natural Fragrance) was added to the mixing vessel. 1 wt% xanthan gum stock solution was added to the vessel. 1 wt% konjac gum stock solution was added to the vessel. The vessel was placed on a magnetic stir plate and stirred at a speed sufficient to create a vortex in the mixture. The mixture was stirred until completely homogenous.

[0174] Dilution into aqueous compositions (Table 4) Water was added to a clean main mixing vessel (1-liter glass beaker, VWR). The mixture was stirred with an overhead propeller mixer, IKA Model RW20DZM, equipped with a mixing blade (4-blade stainless steel, 2.5-inch diameter). The stirring speed was set to create a vortex in the mixture without excessive foaming. The following materials were added to the mixing vessel in order, ensuring a homogeneous mixture after each addition: water, ethanol, Koralone B-119, and citric acid. After 10 minutes of mixing, Hydroxypropyl Beta CD was added to the vessel and mixed for an additional 600 seconds. The pH of the resulting mixture was 6.4 (measured by Orion, Thermo Scientific, catalog number 2115000).

[0175] Parameter Measurement The aqueous compositions were tested according to the following methods: Determine sprayability by spray test method; The yield stress was measured by rheological testing method; Measure the diameter of the LBA droplets by the droplet size test method; The viscosity of the LBA was measured by the Viscosity of Liquid Benefit Agents Test Method.

[0176] [Table 5]

[0177] [Table 6]

[0178] (Examples C to E) These samples demonstrate the preparation of hair and surface treatment compositions with a very wide range of viscosities, from 58 mPa·s (Example D) to 288 mPa·s (Example C) to 4,545 mPa·s (Example E). LBA is emulsified and stabilized in a concentrate. The concentrate is diluted with water to form a sprayable, stable aqueous composition with an acceptable average droplet size distribution.

[0179] material Konjac gum (Nutricol® XP 3464, FMC Corp, lot 11926051) Water (Millipore, 18 MW) A mixture of preservatives, 0.2 wt. % benzyl alcohol (Ineos Maastricht BV, benzyl alcohol NF lot 6M07AE1), 0.2 wt. % Euxyl PE 9010 (Schuelke & Mayr GmbH, Euxyl® PE 9010 preservative lot 1310481), and 0.3 wt. % Symdiol 68 (Symrise, Symdiol® 68 preservative lot 10300058). Xanthan gum (Jungbunzlauer Inc., CAS number 11138-66-2, lot 2532585) PDMS (Gelest, DMS-T35, lot 4H-23386) Argan oil (BASF, Lipofructyl® Argan LS 9779 Argania Spinosa Kernel Oil, Lot 001552044) Liquid benefit agent: 0.1 wt% 10,000 mPa·s amodimethicone (Momentive, Y14945, lot 14NWFA182) 0.2 wt% cyclopentasiloxane (Sigma Aldrich, lot MKCC9214) All samples were prepared in 60 gram or 100 gram capacity speed mixer cups (FlackTek, item code 501 222t) and mixing was carried out in a FlackTek DAC 150.1 FVZ K speed mixer.

[0180] Concentrates containing liquid benefit agents (Table 5) Konjac gum was added to a Speed ​​Mixer cup containing pre-weighed amounts of water, preservatives, and flavorings. The sample was mixed for 300 seconds at 3500 RPM. Xanthan gum was added to the Speed ​​Mixer cup and mixed for an additional 300 seconds at 3500 RPM. The resulting mixture was allowed to rest for 24 hours. Liquid benefit agent was added to the Speed ​​Mixer cup. The sample was mixed again for an additional 300 seconds at 3500 RPM.

[0181] Dilution into aqueous compositions (Table 6) A quantity of the concentrate was added to a beaker (VWR Heavy Duty Low Foam Beaker, Catalog No. 10536-390) and diluted with water using a stand mixer (VWR VOS Power Control, Catalog No. 03.306886) equipped with a propeller blade (3 blades, 1 inch radius) set at 500 RPM for 300 seconds to obtain the final aqueous composition.

[0182] Parameter Measurement The aqueous compositions were tested according to the following methods: Determine sprayability by spray test method; Measure the yield stress by rheological testing method; Measure the diameter of the LBA droplets by the droplet size test method; The viscosity of the LBA was measured by the Viscosity of Liquid Benefit Agents Test Method.

[0183] [Table 7]

[0184] [Table 8]

[0185] (Examples F to G)

[0039] Examples of the present invention demonstrate the preparation of two hair treatment or surface treatment aqueous compositions containing a blend of liquid benefit agent and solid perfume particles by different mixing routes. For the first aqueous composition (Example F), perfume capsules are dispersed in a concentrate, and the liquid benefit agent (silicone blend) is emulsified and stabilized in the second concentrate. The two concentrates are mixed with water to form the final aqueous composition. For the second aqueous composition (Example G), the perfume capsule concentrate is diluted with water to form Preliminary Aqueous Composition 1, and the liquid benefit agent (silicone blend) is diluted with water to form Preliminary Aqueous Composition 2. These two preliminary aqueous compositions were blended to form the final aqueous composition.

[0186] material Water (Millipore Corporations, 18MW) Xanthan gum (CPK Keltrol 1000, lot 6J3749K) Konjac gum (Nutricol® XP 3464, FMC, lot 11926051) Benzyl alcohol (Spectrum, lot 7F14AN1) Euxyl PE 9010 (Schulke, lot 7M20AN1) SymDiol 68 (Symrise, lot 1310481) Fragrance capsules (Encapsys, lot 2018-6479) Liquid benefit agent: Silicone blend with Y-14945 01P (Momentive, lot 18FWFA462) Cyclopentasiloxane (Momentive, lot 17CWFA324) All preparations were carried out in a speed mixer (Flacktek DAC 150.1 FVZ-K) using either a Max 20 speed mixer cup (Flacktek, Max 20 Translucent, 501 224t), a Max 60 speed mixer cup (Flacktek, Max 60 Cup Translucent, 501 222t), or a Max 100 speed mixer cup (Flacktek, Max 100 Translucent, 501 221 Mt).

[0187] Preparation of 1 wt% xanthan gum stock solution 0.106 grams of benzyl alcohol, 0.104 grams of Euxyl PE 9010, 0.158 grams of SymDiol 68, and 49.156 grams of water were added to a Max 60 Speed ​​Mixer cup. 0.505 grams of xanthan gum was added to the cup. The cup was placed in the Speed ​​Mixer at 3500 RPM for 300 seconds.

[0188] Preparation of 1 wt% konjac gum stock solution 0.100 grams of benzyl alcohol, 0.105 grams of Euxyl PE 9010, 0.152 grams of SymDiol 68, and 49.151 grams of water were added to a Max 60 Speed ​​Mixer cup. 0.504 grams of konjac gum was added to the cup. The cup was placed in the Speed ​​Mixer at 3500 RPM for 300 seconds.

[0189] Preparation of Silicone Blendstock 6.704 grams of cyclopentasiloxane and 3.302 grams of Y-14945 were added to a Max 20 speed mixer cup. The cup was placed in the speed mixer at 3500 RPM for 300 seconds.

[0190] Concentrates containing liquid benefit agents (Table 7) Preparation of concentrates containing fragrance microcapsules Benzyl alcohol, Euxyl PE 9010, SymDiol 68, and water were added to a Max 100 speed mixer cup. The xanthan gum stock solution and konjac gum stock solution were added to the cup and mixed for 300 seconds at 2500 RPM. Finally, 1.803 grams of a flavor capsule was added to the cup. The cup was placed in the speed mixer for 300 seconds at 2500 RPM.

[0191] Preparation of Concentrates Containing Silicone Blends Benzyl alcohol, Euxyl PE 9010, SymDiol 68, and water were added to a Max 100 Speed ​​Mixer cup. The xanthan gum stock solution and konjac gum stock solution were added to the cup and mixed at 2500 RPM for 300 seconds. Finally, the silicone blend stock was added to the cup. The cup was placed in the Speed ​​Mixer at 2500 RPM for 300 seconds.

[0192] Dilution into aqueous compositions (Table 8) Prepared aqueous composition 1 The water, concentrate containing fragrance microcapsules, concentrate containing silicone blend, benzyl alcohol, Euxyl PE 9010, and SymDiol 68 were added to a Max 100 Speed ​​Mixer cup. The cup was placed in the Speed ​​Mixer at 2500 RPM for 300 seconds.

[0193] Prepared aqueous composition 1 Preliminary aqueous composition 1 was prepared by adding water, the concentrate containing the perfume microcapsules, benzyl alcohol, Euxyl PE 9010, and SymDiol 68 to a Max 100 speed mixer cup. The cup was placed in the speed mixer at 2500 RPM for 300 seconds.

[0194] Preliminary aqueous composition 2 was prepared by adding water, the concentrate containing the silicone blend, benzyl alcohol, Euxyl PE 9010, and SymDiol 68 to a Speedmixer cup. The cup was placed in the Speedmixer at 2500 RPM for 300 seconds.

[0195] Prepared aqueous composition 2 Preliminary Aqueous Composition 1 and Preliminary Aqueous Composition 2 were added to a Speedmixer cup. The cup was placed in the Speedmixer at 2500 RPM for 300 seconds.

[0196] Parameter Measurement The aqueous compositions were tested according to the following methods: Determine sprayability by spray test method; Measure the yield stress by rheological testing method; Measure the diameter of the LBA droplets by the droplet size test method; The viscosity of the LBA was measured by the Viscosity of Liquid Benefit Agents Test Method.

[0197] [Table 9]

[0198] [Table 10]

[0199] (Examples H to AJ) The combination of the inventive examples and comparative examples demonstrates the importance of concentrate preparation. The inventive samples have good yield stress and good droplet size, such as Example H (peppermint oil) and Example AC (argan oil). One of the comparative examples does not have yield stress, such as Example N (peppermint oil). The other comparative examples have yield stress, but the viscosity of the concentrate preparation is insufficient to emulsify the liquid benefit agent, resulting in very large droplets, as with Example AH (T31 oil) and Example M (peppermint oil).

[0200] material Xanthan gum (CPK Keltrol 1000, 7C5936K) Konjac gum (Nutricol® XP 3464, FMC corp. 11926051) Water (Millipore Corporations, 18 MW) Acticide MBS preservative (Thor GmbH, Acticide® MBS biocide, lot RP-332371-1710) Koralone (Koralone™ B-119 preservative, Dow Chemical Company, lot YY00G46902) Liquid Benefit Agent: Peppermint Oil (MFR Ungerer Bethlehem USA, Lot 50725K); Argan oil (manufacturer, lot PL-A128787) T31 Silicone Oil (Gelest Corporation) All preparations were carried out in a speedmixer (Flacktek DAC 150.1 FVZ K, model) using a 60 ml speedmixer cup (model).

[0201] 1% by weight xanthan gum stock solution 0.08 grams of Koralone and 99.0 grams of water were added to a Speed ​​Mixer cup. 1.0 gram of xanthan gum powder was added to the Speed ​​Mixer cup. The sample was mixed in the Speed ​​Mixer at 3500 RPM for 300 seconds. The resulting sample was placed on a shaker table (VWR Standard 3500 Orbital Shaker, catalog number 89032-094) set at a moderate speed for 12 hours to ensure complete hydration of the xanthan gum.

[0202] 1% by weight konjac gum stock solution 0.08 grams of Koralone and 99.0 grams of water were added to a Speed ​​Mixer cup. 1.0 gram of konjac gum powder was added to the Speed ​​Mixer cup. The sample was mixed in the Speed ​​Mixer at 3500 RPM for 300 seconds. The resulting sample was left on a shaker table (VWR Standard 3500 Orbital Shaker, catalog number 89032-094) set at a moderate speed for 12 hours to ensure complete hydration of the konjac gum.

[0203] Concentrates containing liquid benefit agents (Tables 9-14) 1% by weight xanthan gum stock solution and 1% by weight konjac gum stock solution were added to the Speed ​​Mixer cup. Water was added to the Speed ​​Mixer cup. Finally, LBA (peppermint oil, argan oil, or T31 silicone oil) was added to the Speed ​​Mixer cup. The mixture was mixed at 3500 RPM for 300 seconds.

[0204] Parameter Measurement The resulting preparations were measured in the following manner: Measure the viscosity of the LBA according to the Viscosity of Liquid Benefit Agents Test Method; Measuring the viscosity of the concentrate by rheological methods; Measuring the yield stress of the concentrate by rheological test method; The diameter of the LBA droplets was measured by the droplet size test method.

[0205] [Table 11]

[0206] [Table 12]

[0207] [Table 13]

[0208] [Table 14]

[0209] [Table 15]

[0210] [Table 16]

[0211] (Examples AK to AL) In the examples of the present invention demonstrating the preparation of product concentrate compositions, it may be suggested that both tara gum and heat be used to enhance gum binding. First, peppermint oil was emulsified in a concentrate composition containing a blend of xanthan gum and tara gum maintained at room temperature (Example AK). Next, peppermint oil was emulsified in a concentrate composition containing a blend of xanthan gum and tara gum maintained at a temperature of 60°C (Example AL).

[0212] material Water (Millipore Corporations, 18MW) Xanthan gum (CPK Keltrol 1000, lot 7C5936K) Tara Gum (Ingredion TIC Pre-Tested Tara Gum 100, Lot 33809) Preservative (Koralone B19, Dow Chemical Company, Lot YY00G41902) Liquid Benefit Agent: Peppermint Oil (MFR Ungerer Bethlehem USA, Lot 50725 K) All preparations were carried out in a speed mixer (Flacktek DAC 150.1 FVZ K).

[0213] Preparation of 1 wt% xanthan gum stock solution Add 0.047 grams of preservative and 49.462 grams of deionized water to a Speed ​​Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t). Add 0.503 grams of xanthan gum powder to the cup and place the cup in the Speed ​​Mixer at 3500 RPM for 300 seconds.

[0214] Preparation of 1 wt% tara gum stock solution To a Speed ​​Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t) add 0.049 grams of preservative and 49.467 grams of deionized water. Add 0.502 grams of tara gum powder to the cup and place the cup in the Speed ​​Mixer at 3500 RPM for 300 seconds.

[0215] Concentrates containing liquid benefit agents (Table 15) Preparation of concentrate at room temperature Using a Speed ​​Mixer Max 60 cup, add the mass of preservative, add the mass of water, add 1% by weight of xanthan gum stock, add 1% by weight of tara gum stock, and add the specified mass of LBA. The Speed ​​Mixer Max 60 cup and all contents were mixed at the specified speed for the specified time. The composition was kept at room temperature for 12 hours.

[0216] Preparation of concentrate at 60°C Using a Speed ​​Mixer Max 60 cup, add the mass of preservative, add the mass of deionized water, add the mass of 1% by weight xanthan gum stock, add the mass of 1% by weight tara gum stock, and add the specified mass of LBA. The Speed ​​Mixer Max 60 cup and all contents were mixed at the specified speed for the specified time. The composition was maintained at a temperature of 60°C for 1 hour.

[0217] Parameter Measurement The resulting preparations were measured in the following manner: The viscosity of the LBA as measured by the Viscosity of Liquid Benefit Agents Test Method; viscosity of the concentrate measured by rheological methods; Yield stress of concentrate measured by rheological test method; The diameter of the LBA droplets is measured by the Drop Size Test Method.

[0218] [Table 17]

[0219] (Examples AM to AR) The present and comparative examples demonstrate the importance of the viscosity of a liquid benefit agent compared to a concentrated composition in producing good droplets. Examples AM-AQ have decreasing concentrations in the concentrated composition and corresponding viscosities. As shown in the top 5% of the distribution, droplet size increases with decreasing viscosity until Example AQ is unable to produce acceptable droplets. However, substituting a higher viscosity liquid benefit agent (Example AR) allows for the formation of acceptable droplets.

[0220] material Xanthan Gum (Xanthan Gum, Novaxan, Dispersible, Lot 140521) Konjac Gum (Konjac Gum, FMC, Nutricol XP 3464, Lot 11926051) Water (Millipore Corporations, 18 MW) Flash AS (Momentive Corporation, XX-8766, Lot PE12152016) A15 (Gelest Corporation) Preservative (Thor GmbH, Acticide® MBS Biocide, Lot RP-332371-1710)

[0221] Concentrates containing liquid benefit agents 200 grams of water and 0.6 g of Acticide were added to a 100 ml beaker. The xanthan gum and konjac gum were slowly added with overhead stirring until a visually homogeneous concentrated composition was obtained. These preparations were further shaken for at least 48 hours to ensure complete hydration of the gums. A portion of this composition was placed in a 100 ml speed mixer cup (FlackTek, item code 501 222t). The liquid benefit agent was added to the cup. The cup was tightly covered and placed in a speed mixer (FlackTek DAC 150.1 FVZ K speed mixer) and mixed at 3500 RPM for 300 seconds.

[0222] Dilution into aqueous compositions The resulting aqueous mixture was diluted with water to a total gum concentration of 0.05% by weight.

[0223] Parameter Measurement The resulting preparations were measured in the following manner: Measure the viscosity of the LBA according to the viscosity of the liquid benefit agent; Measure the viscosity of the concentrate by rheological test method; measuring the diameter of the droplet size of the LBA in the aqueous composition by the Droplet Size Test Method; The yield stress of the aqueous composition was measured by a rheological test method.

[0224] [Table 18]

[0225] [Table 19]

[0226] (Examples AS to AV) Examples of the present invention demonstrate the preparation of aqueous compositions by diluting a concentrate with water and by diluting a concentrate with water combined with other ingredients in an aqueous composition. A first concentrate was prepared by emulsifying and stabilizing peppermint oil in a concentrate containing a 30:70 mixture of xanthan gum and konjac gum; a second concentrate was prepared by emulsifying and stabilizing peppermint oil in a concentrate containing a 60:40 mixture of xanthan gum and konjac gum. These concentrates were diluted with water (Examples AS and U), xanthan gum stock solution (Example AT), and / or konjac gum stock solution (Example AV) to prepare final aqueous compositions.

[0227] material Water (Millipore Corporations, 18 MW) Xanthan gum (CPK Keltrol 1000, lot 6J3749K) Konjac gum (Nutricol® XP 3464, FMC corp., lot 11926051) Benzyl alcohol (Spectrum, lot 7F14AN1) Euxyl PE 9010 (Schulke, lot 7M20AN1) SymDiol 68 (Symrise, lot 1310481) Peppermint oil (MFR Ungerer Bethlehem USA, Lot 50725 K) All preparations were carried out in a speed mixer (Flacktek DAC 150.1 FVZ K).

[0228] Preparation of 1 wt% xanthan gum stock solution To a Speed ​​Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t) is added 0.102 grams of benzyl alcohol, 0.104 grams of Euxyl PE 9010, 0.151 grams of SymDiol 68, and 49.156 grams of deionized water. 0.502 grams of xanthan gum powder is added to the cup, and the cup is placed in the Speed ​​Mixer at 3500 RPM for 300 seconds.

[0229] Preparation of 1 wt% konjac gum stock solution To a Speed ​​Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t) is added 0.106 grams of benzyl alcohol, 0.108 grams of Euxyl PE 9010, 0.154 grams of SymDiol 68, and 49.157 grams of deionized water. 0.501 grams of konjac gum powder is added to the cup, and the cup is placed in the Speed ​​Mixer at 3500 RPM for 300 seconds.

[0230] Concentrates containing liquid benefit agents (Table 18) Preparation of 30:70 concentrate Using a Speedmixer Max 60 cup, 0.104 grams of benzyl alcohol, 0.105 grams of Euxyl PE 9010, 0.152 grams of SymDiol 68, and 33.608 grams of deionized water were added to a Speedmixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t). 4.506 grams of xanthan gum stock was added, followed by 10.508 grams of konjac gum stock, and the cup was placed in the Speedmixer at 2500 RPM for 300 seconds. 1.057 grams of peppermint oil was added, and the cup was placed in the Speedmixer at 2500 RPM for an additional 300 seconds.

[0231] Preparation of 60:40 concentrate Using a Speedmixer Max 60 cup, 0.102 grams of benzyl alcohol, 0.107 grams of Euxyl PE 9010, 0.152 grams of SymDiol 68, and 33.308 grams of deionized water were added to a Speedmixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t). 9.002 grams of xanthan gum stock was added, followed by 6.006 grams of konjac gum stock, and the cup was placed in the Speedmixer at 2500 RPM for 300 seconds. 1.355 grams of peppermint oil was added to the cup, and the cup was placed in the Speedmixer at 2500 RPM for an additional 300 seconds.

[0232] Dilution into aqueous compositions (Table 19) Preparation of the aqueous composition, option 1 Using a Speed ​​Mixer Max 60 cup, deionized water, 30:70 concentrate, benzyl alcohol, Euxyl PE 9010, and SymDiol 68 were added and processed for 300 seconds at 2500 RPM. In a second example, using a Speed ​​Mixer Max 60 cup, deionized water, 30:70 concentrate, benzyl alcohol, Euxyl PE 9010, SymDiol 68, and xanthan gum stock were added and processed for 300 seconds at 2500 RPM.

[0233] Preparation of the aqueous composition, option 2 In one example, a Speed ​​Mixer Max 60 cup was used to mix deionized water, 60:40 concentrate, benzyl alcohol, Euxyl PE 9010, and SymDiol 68 and process for 300 seconds at 2500 RPM. In a second example, a Speed ​​Mixer Max 60 cup was used to mix deionized water, 60:40 concentrate, benzyl alcohol, Euxyl PE 9010, SymDiol 68, and konjac gum stock and process for 300 seconds at 2500 RPM.

[0234] Parameter measurement: Measure the viscosity of the LBA according to the viscosity of the liquid benefit agent; measuring the viscosity of the aqueous composition and the concentrated composition by a rheological test method; measuring the diameter of the droplet size of the LBA in the aqueous composition by the Droplet Size Test Method; The yield stress of the aqueous and concentrated compositions was measured by a rheological test method.

[0235] [Table 20]

[0236] [Table 21]

[0237] (Examples AW to BL) The inventive and comparative examples demonstrate important parameters in preparing product concentrates. These include inventive samples with yield stress and good droplet size, such as Examples AW-BE. They also include comparative examples with no yield stress, such as Examples BG-BL, which vary in the amount and ratio of xanthan gum and konjac gum. Most importantly, these examples demonstrate that it is possible to emulsify up to 20% by weight of liquid benefit agent (Example AZ), but not effectively emulsify 60% by weight of liquid benefit agent (Example BF), despite the relative viscosity and the presence of yield stress.

[0238] material Konjac Gum (Konjac Gum, FMC, Nutricol XP 3464, Lot 11926051) Water, deionized (Millipore, 18 MW) Preservative Acticide MBS (Thor GmbH, Acticide® MBS Biocide Lot RP-332371-1710) Xanthan gum (Xanthan gum, Jungbunzlauer, FG, lot 2532585) 0.050 Pa·s PDMS (Gelest, DMS-T15, lot 8F-13015) 5 Pa·s PDMS (Gelest, DMS-T35, lot 4H-23386) All samples were prepared in 60 gram or 100 gram capacity speed mixer cups (FlackTek, item code 501 222t) and mixing was carried out in a FlackTek DAC 150.1 FVZ K speed mixer.

[0239] Concentrates containing liquid benefit agents Konjac gum was added to the Speed ​​Mixer cup containing water, preservatives, and flavor. The sample was mixed for 5 minutes at 3500 rpm. Xanthan gum was weighed and carefully and slowly added to the Speed ​​Mixer cup and mixed again for an additional 5 minutes at 3500 rpm. If any significant undissolved gum chunks are observed, the sample is further mixed for an additional 5 minutes at 3500 rpm until the gum is completely dissolved. The resulting mixture is allowed to stand for 24 hours. Liquid benefit agent was added to the Speed ​​Mixer cup. The sample was mixed again for an additional 5 minutes at 3500 rpm.

[0240] Dilution into aqueous compositions A portion of the concentrate was removed, added to a plastic jar, and diluted with water. The mixture was mixed in a Ross mill mixer equipped with a mixing blade (four-blade stainless steel, 2.5 inch diameter) (or equivalent) at 500 rpm for 300 seconds to obtain an aqueous composition.

[0241] Parameter Measurement The resulting preparations were measured in the following manner: The viscosity of the LBA was measured using the Viscosity of Liquid Benefit Agents Test Method. The viscosity of the concentrate was measured by a rheological test method. The droplet size diameter of LBA in aqueous compositions was measured by the droplet size test method. The yield stress of the aqueous composition was measured using a rheological test method.

[0242] [Table 22]

[0243] Table 23

[0244] Table 24

[0245] Table 25

[0246] Table 26

[0247] Table 27

[0248] Table 28

[0249] Table 29

[0250] Table 30

[0251] Table 31

[0252] Table 32

[0253] [Table 33]

[0254] (Examples BM to BP) Examples of the present invention demonstrating the preparation of aqueous compositions from single concentrates each containing a benefit agent (Examples BM and BN), a blend of two concentrates with a benefit agent (Example BO), and a single concentrate prepared with both benefit agents (BP).

[0255] material Xanthan gum (Xanthan gum, CPK Keltrol 1000, 7C5936K) Konjac Gum (Nutricol® XP 3464, FMC Corp. 11926051) Water (Millipore Corporations, 18 MW) Silicone oil, Y14945 (Momentive, Y14945, Lot 14NWFA 182) Silicone oil, cyclopentasiloxane (Sigma Aldrich, 444278 Decamethylcyclopentasiloxane, lot MKCC9214) Fragrance capsules (Encapsys, lot 2018-6479) Benzyl alcohol (Spectrum, lot 7F14AN1) Euxyl PE 9010 (Schulke, lot 7M20AN1) SymDiol 68 (Symrise, lot 1310481) All preparations were carried out in a speed mixer (Flacktek DAC 150.1 FVZ K, model).

[0256] 1% by weight xanthan gum stock solution 0.106 grams of benzyl alcohol, 0.106 grams of Euxyl alcohol, and 0.151 grams of SymDiol 68 were added to 49.154 grams of water in a 60 ml Speedmixer cup (portion). 0.505 grams of xanthan gum was carefully added to the cup. The mixture was processed in the Speedmixer at 3500 RPM for 300 seconds.

[0257] 1% by weight konjac gum stock solution 0.101 grams of benzyl alcohol, 0.100 grams of Euxyl alcohol, and 0.157 grams of SymDiol 68 were added to 49.153 grams of water in a 60 ml Speedmixer cup (portion). 0.502 grams of konjac gum was carefully added to the cup. The mixture was processed in the Speedmixer at 3500 RPM for 300 seconds.

[0258] Silicone Blend Stock Solution 3.308 grams of Y14945 silicone oil and 6.708 grams of cyclopentasiloxane silicone oil were blended together. The mixture was processed in a Speedmixer at 3500 RPM for 300 seconds.

[0259] Gum concentrate with liquid benefit agents Concentrates containing benefit agents Concentrates containing fragrance capsules The water, preservatives, xanthan gum stock solution, and konjac gum stock solution were added to a 50 ml speed mixer cup along with the flavor capsules. The mixture was mixed at 2500 rpm for 300 seconds.

[0260] Concentrates containing silicone blends The water, preservatives, xanthan gum stock solution, and konjac gum stock solution were added to a 50 ml Speed ​​Mixer cup along with the silicone blend. The mixture was mixed at 2500 rpm for 300 seconds.

[0261] Concentrate containing fragrance capsules and silicone blend The water, preservatives, xanthan gum stock solution, and konjac gum stock solution were added to a 60 mL speed mixer cup along with the flavor capsules and silicone blend. The mixture was mixed at 2500 rpm for 300 seconds.

[0262] Dilution into aqueous compositions Completion of the preparation Add water to a 100 ml Speed ​​Mixer cup. Then add the appropriate amounts of benzyl alcohol, Euxyl PE 9010, and Add SymDiol 68. Finally, add the different concentrates. The mixture is mixed at 2500 rpm for 300 seconds.

[0263] [Table 34]

[0264] [Table 35]

[0265] Dimensions and values ​​disclosed herein should not be understood as being strictly limited to the exact numerical values ​​recited. Instead, unless otherwise indicated, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm."

[0266] It should be understood that every maximum numerical limitation given throughout this specification includes every lower numerical limitation, as if such lower numerical limitations were expressly written herein. Every minimum numerical limitation given throughout this specification includes every higher numerical limitation, as if such higher numerical limitations were expressly written herein. Every numerical range given throughout this specification includes every narrower numerical range that falls within such broader numerical range, as if such narrower numerical ranges were all expressly written herein.

[0267] All documents cited herein, including any cross-referenced or related patents or patent applications, and any patent applications or patents to which this application claims priority or benefit, are incorporated herein by reference in their entirety, unless expressly stated to the contrary. The citation of any document shall not be deemed to be prior art to any invention disclosed or claimed herein, or to teach, suggest, or disclose such invention, either alone or in combination with any other reference(s). Furthermore, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.

[0268] While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims

1. A sprayable product comprising: A spray dispenser, an aqueous composition contained within said spray dispenser, said aqueous composition comprising an aqueous phase and liquid benefit agent emulsified droplets uniformly and discontinuously dispersed throughout said aqueous phase, said aqueous phase comprising a structurant system comprising a first polysaccharide and a second polysaccharide different from said first polysaccharide, said aqueous phase comprising less than 100 ppm of a surfactant, said aqueous composition exhibiting a yield stress as measured by a rheology test method, and said liquid benefit agent emulsified droplets having a diameter of less than 300 μm as measured by a droplet size test method; A sprayable product to which at least one of (a) and (b) is applied. (a) the first polysaccharide comprises xanthan gum, and the second polysaccharide is selected from the group consisting of glucomannan, galactomannan, or a combination thereof; (b) the structurant system is present at a concentration of 0.5 wt.% or less, based on the total weight of the aqueous composition;

2. 10. The sprayable product of claim 1, wherein the first polysaccharide comprises xanthan gum and the second polysaccharide is selected from the group consisting of glucomannan, galactomannan, or a combination thereof.

3. 3. The sprayable product of claim 2, wherein the second polysaccharide is selected from the group consisting of konjac gum, tara gum, locust bean gum, or combinations thereof.

4. A sprayable product according to any one of claims 1 to 3, wherein the structurant system is present at a concentration of 0.5% by weight or less, based on the total weight of the aqueous composition.

5. 5. The sprayable product of any one of claims 1 to 4, wherein the first polysaccharide is present at a concentration of greater than 10% and less than 90% by weight, based on the total weight of the structurant system.

6. The sprayable product of any one of claims 1 to 5, wherein the aqueous composition is surfactant-free.

7. A sprayable product according to any one of claims 1 to 6, wherein the aqueous composition comprises more than 90% by weight of water.

8. 8. The sprayable product of any one of claims 1 to 7, wherein the liquid benefit agent is selected from the group consisting of silicones, aminosilicones, PDMS, essential oils, natural oils, perfume oils, and combinations thereof.

9. The sprayable product of any one of claims 1 to 8, wherein the liquid benefit agent emulsified droplets comprise less than 20% by weight of the aqueous composition.

10. 1. A method of formulating an aqueous composition, said method comprising: dispersing a structurant system in water to form a concentrate, said structurant system comprising a first polysaccharide and a second polysaccharide different from said first polysaccharide; mixing a liquid benefit agent into said concentrate to form emulsified droplets of the liquid benefit agent dispersed throughout said concentrate; diluting said concentrate with additional water to form said aqueous composition, wherein the concentration of said structurant system in said concentrate is greater than the concentration of said structurant system in said aqueous composition, and wherein said liquid benefit agent emulsion droplets in said aqueous composition have a diameter of less than 300 μm as measured by a Droplet Size Test Method.

11. A method of formulating an aqueous composition, said method comprising: dispersing a structurant system in water to form a first concentrate and a second concentrate, respectively, wherein the structurant system comprises a first polysaccharide and a second polysaccharide different from the first polysaccharide; mixing a first liquid benefit agent into said first concentrate to form emulsified liquid benefit agent droplets dispersed throughout said first concentrate, and mixing a second liquid benefit agent into said second concentrate to form emulsified second liquid benefit agent droplets dispersed throughout said second concentrate, said first and second liquid benefit agents having different viscosities; mixing the first and second concentrates; diluting said first and second concentrates with additional water, wherein the concentration of said structurant system in said first and second concentrates is greater than the concentration of said structurant system in said aqueous composition, and wherein said liquid benefit agent emulsion droplets in said aqueous composition have a diameter of less than 300 μm as measured by a Droplet Size Test Method.

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