JP2022521375A - Structured aqueous composition with dispersed liquid beneficial agent droplets - Google Patents

Abstract

Provided are an aqueous composition, a sprayable composition containing the aqueous composition, and a method for producing the aqueous composition. The aqueous composition comprises an aqueous phase and liquid beneficial agent droplets disperse discontinuously throughout the aqueous phase. The aqueous phase has a structuring agent system containing a first polysaccharide and a second polysaccharide different from the first polysaccharide. The aqueous phase contains less than 10,000 ppm of surfactant. The aqueous composition exhibits the yield stress as measured by the rheology test method.

Description

The present disclosure relates to phase-stable aqueous compositions with suspended liquid beneficial agent droplets and products for spraying phase-stable aqueous compositions.

There is a consumer demand for sprayable products containing various liquid beneficial agents (eg, fragrances, conditioning oils) to treat a wide variety of surfaces. Consumers may also be interested in sprayable products that are easily portable for use outside the home or office. Consumers have a phase-stable aqueous composition to prevent bulk separation of liquid beneficial agents so that the first and last sprays are certainly the same and eliminate the need to shake the product before use. I'm looking for it. Also, for some uses, it may be necessary to minimize the residue left on the surface, especially when unsightly stains or unpleasant properties can occur. Consumers may also prefer specific spray characteristics with respect to parameters such as spray droplet size, cone angle, and flow rate.

Liquid beneficial agents can be water insoluble. Emulsification may be used to stabilize the water-insoluble liquid beneficial agent in the aqueous composition. Emulsification is a method of dispersing a liquid beneficial agent from a bulk raw material into separate droplets in an aqueous composition, generally using a surfactant and / or an emulsifier. However, surfactants do not always succeed in emulsifying liquid beneficial agents, and high concentrations of surfactant may be required to emulsify certain liquid beneficial agents. Consumers are also clamoring for products with natural ingredients. There is a general consumer tendency towards natural materials away from the use of chemicals in search of safety and sustainability (etc.). Many surfactants and / or emulsifiers may not be classified or considered as natural ingredients.

Therefore, there is a need for a sprayable, phase-stable aqueous composition with suspended liquid beneficial agent droplets and a method for producing a phase-stable aqueous composition. In addition, there is a need for sprayable, phase-stable, natural aqueous compositions with suspended liquid beneficial agents, as well as methods for producing phase-stable aqueous compositions.

Aqueous compositions are provided. The aqueous composition comprises an aqueous phase and liquid beneficial agent droplets that are homogeneously and discontinuously dispersed throughout the aqueous phase. The aqueous phase comprises a structuring agent system comprising a first polysaccharide and a second polysaccharide different from the first polysaccharide. The aqueous phase contains less than 10,000 ppm of surfactant. The aqueous composition exhibits the yield stress as measured by the rheology test method.

A method of prescribing an aqueous composition is provided. The method is a step of dispersing the structuring agent system in water to form a concentrate, in which the structuring agent system is a first polysaccharide and a second polysaccharide different from the first polysaccharide. And; the liquid beneficial agent is mixed with the concentrate to form liquid beneficial agent droplets dispersed throughout the concentrate; and; the concentrate is diluted with additional water to form an aqueous composition. The concentration of the structuring agent system in the concentrate is higher than the concentration of the structuring agent system in the aqueous composition.

It is a schematic diagram of the composition of this invention, and the composition and the manufacturing method. In the direct emulsification route (left), the raw materials are combined and mixed to prepare a composition. The emulsification route (right) of the present invention requires two steps, (1) emulsification step and 2) dilution step. In the emulsification step, the concentrate is utilized to promote the emulsification of the liquid beneficial agent; in the dilution step, the concentrate is further diluted to reach the composition.

The present invention can be more easily understood by reference to the following detailed description of exemplary and preferred compositions. The claims are not limited to the particular product, method, condition, device, or parameter described herein, and the terms used herein limit the claimed invention. Please understand that is not intended. Also, as used herein, including the appended claims, the singular "a," "an," and "the" include the plural, and references to specific numbers are content. Includes at least that particular value unless explicitly stated otherwise. When a range of values is represented, another embodiment includes from one particular value and / or to the other. Similarly, when a value is expressed as an approximation by the use of the antecedent "about", it is understood that the particular value constitutes another embodiment. All ranges include endpoints and can be combined. All percentages and ratios used herein are by weight of the entire product and all measurements were made at 25 ° C. unless otherwise specified.

The following definitions may be helpful in understanding this disclosure.

The "aqueous phase" includes water, polysaccharides, and trace components.

The "trace component" includes a water-soluble component in the aqueous phase. These include salts, organics such as glycerin and propylene diols, solvents, and / or low concentrations of surfactant.

"Liquid beneficial agent" or "LBA" means a water-insoluble material that is liquid at 25 ° C. and has an effect on surfaces such as fabrics, hair, and skin.

By "liquid beneficial agent droplet" is meant a liquid beneficial agent droplet completely surrounded by an aqueous phase. The liquid beneficial agent droplets floating on the surface of the aqueous phase are not "liquid beneficial agent droplets".

The "concentrate" contains a portion of the aqueous phase containing trace components, liquid beneficial agents, and polysaccharides, has a higher solid content than the final product composition, and emulsifies the liquid beneficial agent into stable droplets. Facilitate.

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

"Essential oil" means a concentrated hydrophobic liquid containing a volatile aroma compound from a plant (defined as "the substance tends to evaporate"). Essential oils are also known as volatile oils, ether oils, etherolea, or simply extracted vegetable oils such as clove oil, peppermint oil and the like.

"Natural oil" is derived from renewable plant resources.

"Solid particles" means particles.

"Ppm" means 1 mg / L = 1 ppm.

The aqueous composition of the present disclosure comprises a plurality of liquid beneficial agent droplets and a structuring agent system for suspending the liquid beneficial agent droplets. Since the liquid beneficial agent droplets can be suspended by the structuring agent system, the aqueous composition may or may not contain a surfactant. The aqueous composition may be sprayable. The aqueous composition can be phase stable. This means that the liquid beneficial agent droplets remain suspended in the aqueous composition for extended periods of time, eliminating the need to shake the product prior to use. The aqueous composition is used in the air or on the surface by application from a spray dispenser and / or removes or reduces the amount of malodor in the air or on the surface and / or the beneficial agent in the air. Alternatively, it may be delivered on the surface. The product may include a spray dispenser containing an aqueous composition.

By incorporating a structuring agent system to suspend liquid beneficial agent droplets in the aqueous composition, the aqueous composition exhibits yield stress. The yield stress of the aqueous composition prevents the liquid beneficial agent droplets from phase-separating.

It has been found that the method of combining the structuring agent system with the liquid beneficial agent affects the phase stability of the composition. In a typical emulsification method using a surfactant as an emulsifier, all raw materials are combined and mixed at once to prepare an emulsified composition. However, by preparing an aqueous phase concentrate containing water at a concentration lower than the concentration of the final aqueous composition, a stable aqueous composition of liquid beneficial agent droplets dispersed discontinuously across the aqueous phase can be obtained. Was found.

Without being bound by theory, increasing the viscosity of the concentrate as well or substantially as the viscosity of the liquid beneficial agent, at least during the emulsification step, is a liquid of a droplet size small enough for the aqueous composition. It is believed that the beneficial agent droplets maintain phase stability. As the viscosities of the aqueous phase concentrate and the liquid beneficial agent differ from each other, the resulting liquid beneficial agent droplets become larger and the aqueous composition is less likely to be phase stable. As the viscosities of the aqueous phase concentrate and the liquid beneficial agent approach each other, the aqueous composition becomes phase stable and even when further diluted with water to form an more easily sprayable aqueous composition. Maintain stability.

Spray dispenser A sprayable product may include an aqueous composition container within a spray dispenser. The spray dispenser may include a bottle and a spray engine for accommodating the aqueous composition.

The spray engine can be configured by various methods such as a direct compression trigger sprayer, a preload trigger sprayer, or an aerosol spray dispenser. One suitable spray dispenser is the TS800 Trigger Atomizer (ExxonMobil PP1063, material fractionation 100003913, manufacturer: Calmar).

Another suitable atomizing engine may be a continuously operating atomizer, such as a FLAIROSOL ™ dispenser manufactured by Afa Dispensing Group. FLAIRSOL ™ dispensers include preload spray engines and aerosol-like pressurizers for aqueous compositions using a pressure or buffer chamber.

A wide range of trigger atomizers or finger pump atomizers are suitable for use in the aqueous compositions of the present invention. These are from Calmar, Inc. (City of Industry, Calif.); CSI (Continental Sprayers, Inc.), St. Peters, Mo. Berry Globals Corp. , Evansville, Ind. Easily available from sources such as Guala® Atomizer Distributors; or SeaQuest Dispensing, 30 Cary, Ill. A preferred trigger atomizer is Berry Globals Corp. Blue Insert Guala® Atomizer available from, or Calmar Inc. Calmar TS800-1A®, TS1300®, and TS-800-2®, available from, because of the 35 properties of fine and uniform spray, spray volume, and more. And pattern size. A nebulizer with a preload function, finer atomizing characteristics, and a uniform distribution, such as a Japanese Yshino atomizer, is more preferred. Any suitable bottle or container can be used with the trigger sprayer. The recommended bottle is a 1740 fl oz bottle (about 500 ml), a good ergonomic one that is similar in shape to a 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 forms a bottle. It is preferably made of 45 high density polyethylene or clear polyethylene terephthalate.

If the size of the fluid ounce is smaller (such as 1-8 ounces for illustration purposes only), a finger pump can be used with the canister or cylindrical bottle. A preferred pump for this application is the Cylindrical Euromist II® from SeaQuest Dispensing. More preferably, it has a preload function.

The bottle can be configured as a container with a base and sidewalls terminated at the opening. The bottle may include a bag-in-bag or a bag-in-can container.

The bottle may be large to enclose hundreds of grams of aqueous composition as a current fabric treatment spray. Alternatively, the bottle may be small to enclose tens of grams of the aqueous composition and can be carried in a purse or pocket to apply the aqueous composition on the move or in between. The bottle may have a longest dimension of less than 20 cm, preferably less than 10 cm, most preferably less than 5 cm. The bottle may contain 0.1 ml (“mL”) to 50 mL, more preferably 1 mL to 30 mL, and most preferably 1 mL to 20 mL.

If the spray dispenser is configured as an aerosol, the spray dispenser can be pressurized with a propellant. Any suitable propellant can be used.

Aqueous Composition The aqueous composition of the present invention comprises an aqueous phase and a plurality of liquid beneficial agent droplets disperse discontinuously throughout the aqueous phase. The aqueous phase contains an aqueous carrier, a structuring agent system, and trace components. Aqueous compositions can be formulated initially by forming a concentrate containing at least one aqueous phase and a structuring agent system. The concentrate can also contain trace components. The liquid beneficial agent is then mixed with the concentrate to form discontinuously dispersed liquid beneficial agent droplets throughout the concentrate. The concentrate with the liquid beneficial agent droplets can then be diluted with an additional aqueous phase while maintaining the phase stability of the aqueous composition. The additional aqueous phase may contain water, a structuring agent system, and / or trace components.

Structuring agent system In particular, the structuring agent system can be in the form of a polysaccharide system. Preferred polysaccharides include xanthan gum, glucomannan gum, galactomannan gum, and combinations thereof. Glucomannan can be derived from natural gums such as konjac gum. Galactomannan can be derived from natural gums such as locust bean gum or tara gum. The polysaccharide may also contain carrageenan. One or more polysaccharides may be denatured by deacetylation or the like. Xanthan gum may be acetylated.

The aqueous composition may include a polysaccharide system comprising at least two polysaccharides, such as a first polysaccharide and a second polysaccharide. The first polysaccharide can 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.

Although not bound by theory, two or more polysaccharides exhibit synergistic bonds, so that the binding of sites between different polysaccharides is stronger than the binding between sites of the same polysaccharide and is liquid. It is believed to produce a structuring agent system capable of suspending beneficial agent droplets.

The first polysaccharide may make up 10% to 80% by weight of the polysaccharide system; the second polysaccharide may make up 20% to 90% by weight of the polysaccharide system, but the composition. More than the case.

The first polysaccharide may be present in a concentration of more than 10% by weight and less than 90% by weight of the polysaccharide system, or about 20% by weight to about 80% by weight, or about 40% by weight to about 60% by weight. ..

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

The total concentration of polysaccharides present in the aqueous composition is greater than about 0.1% by weight, preferably greater than about 0.2% by weight, or preferably greater than about 0.3% by weight, more preferably 0.4% by weight. It can be greater than% by weight, most preferably greater than 0.5% by weight. Without being bound by theory, the higher the overall concentration of polysaccharides in the aqueous composition, the higher the viscosity, the better the emulsification of the liquid beneficial agent, and then the higher the yield stress. It is believed to prevent coalescence of liquid beneficial agents and bulk separation.

Polysaccharides are from about 10,000 daltons to about 15,000,000 daltons, preferably from about 200,000 daltons to about 10,000,000 daltons, more preferably from about 500,000 daltons to about 9,000,000 daltons. 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. It may have a weight average molecular weight in the range of 6,000,000 daltons, more preferably about 3.5 million daltons to about 6,000,000 daltons.

Polysaccharides may be characterized by the rate of acetylation. The acetylation rate of one or more of the polysaccharides in the structuring agent system ranges from about 5.0 to about 0.2, preferably from about 3.5 to about 0.3, preferably about 2. It may range from 0.0 to about 0.35, preferably from about 1.5 to about 0.37, preferably from about 1.0 to about 0.39.

The aqueous composition may have a total protein concentration of less than about 100 million percent (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 in order to minimize surface fading to which the aqueous composition is applied.

Liquid Beneficial Agent Droplets The aqueous composition may contain multiple liquid beneficial agent droplets suspended in the aqueous phase. On the surface of air or products, the liquid beneficial agent can be a fragrance that provides the surface of furniture, carpets, curtains, etc. with freshness such as reduced malodor and improved scent. In hair products, the liquid beneficial agent can be a silicone oil that provides effects such as feel, deodorization, and antistatic. In fabric treated products, the liquid beneficial agent can be a liquid that provides an anti-wrinkle effect and / or a fresh effect. Liquid beneficial agents consist of raw fragrances; waxes such as silicone oil, polyethylene wax; essential oils such as fish oil, jasmine, camphor, lavender; skin coolants such as menthol, methyl lactate; glycerin, etc.; and mixtures thereof. It may include materials selected from the group.

Suitable beneficial agents are Givaudan Corp. (Mount Olive, New Jersey, USA), International Flavors & Fragrances Corp. It can be obtained from (South Brunswick, New Jersey, USA) or Firmenich Company (Geneva, Switzerland).

Liquid beneficial agents may include materials used to impart a particular conditioning effect to hair and / or skin. In hair compositions, suitable liquid beneficial agents have effects related to gloss, flexibility, compatibility, antistatic properties, wet handling, damage, manageability, volume, and greasiness. Includes one or more bring.

Suitable liquid beneficial agents include conditioning agents such as hair conditioners, skin conditioners, or fabric conditioners such as silicones, petrolatum, hydrocarbon oils (eg mineral oils), natural and synthetic waxes (eg microcrystalline waxes), paraffin. , Ozokerite, polyethylene, polybutene, polydecene, pentahydrosqualene, vegetable oils, triglycerides, fats and oils, and combinations thereof. Further, the liquid beneficial agent may be a perfume oil or may contain a perfume oil. Some liquid beneficial agents suitable for use herein are described below.

The liquid beneficial agent droplets may be small enough to form a stable suspension. For example, liquid beneficial agent droplets are 300 μm (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 when measured by the droplet size test method described below. It may have a diameter of less than or equal to 20 μm or less. The liquid beneficial agent droplet may contain one liquid beneficial agent or may contain a combination of two or more different liquid beneficial agents.

The concentration of the liquid beneficial agent in the concentrate and final composition should be sufficient to produce the desired effect. Such concentrations may vary depending on the liquid beneficial agent, the desired performance, the type and concentration of other components, and other similar factors. However, increasing the concentration of the liquid beneficial agent affects the concentration of the structuring agent system required to suspend the liquid beneficial agent. Therefore, it may be desirable to limit the concentration of the liquid beneficial agent in the concentrate and final aqueous composition to some extent.

The concentration of liquid beneficial agent droplets in the concentrate is 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. It can be less than or equal to 2% by weight.

The concentration of liquid beneficial agent droplets in the final aqueous composition is 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. It can be less than or equal to 0.2% by weight or less.

The liquid beneficial agent droplets are 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, as measured by the viscosity of the LBA test method. , More preferably less than 100 mPa · s, more preferably less than 10 mPa · s.

Silicone The liquid beneficial agent of the aqueous composition of the present invention can be a water-insoluble silicone. Silicones may include volatile silicones, non-volatile silicones, or combinations thereof. Non-volatile silicone conditioning agents are preferred. The presence of volatile silicones typically accompanies use as a solvent or carrier for commercially available forms of non-volatile silicone material components such as silicone gums and resins. The silicone may contain a silicone fluid conditioning agent and may also contain other components such as silicone resin to improve the adhesion efficiency of the silicone fluid or enhance the surface gloss.

Suitable silicones are selected from the group consisting of siloxanes, silicone gums, aminosilicones, terminal aminosilicones, alkylsiloxane polymers, cationic organopolysiloxanes, and mixtures thereof.

The liquid beneficial agent may include one or more silicones, including high molecular weight polyalkyl or polyarylsiloxanes and silicone gums, low molecular weight polydimethylsiloxane fluids and aminosilicones.

High molecular weight polyalkyl or polyarylsiloxanes and silicone gums are at 25 ° C. from about 100,000 mPa · s to about 30,000,000 mPa · s, or from about 200,000 mPa · s to about 30,000,000 mPa · s. It has a viscosity 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.

Preferred higher molecular weight silicone compounds useful herein include polyalkylsiloxanes or polyarylsiloxanes having the following structures:

式中、Ｒ^９３はアルキル又はアリールであり、ｐは、約１，３００～約１５，０００、より好ましくは約１，６００～約１５，０００の整数である。Ｚ^８は、シリコーン鎖の末端を封鎖する基を表す。シロキサン鎖において置換されるアルキル若しくはアリール基（Ｒ^９３）又はシロキサン鎖の末端において置換されるアルキル若しくはアリール基Ｚ^８は、得られるシリコーンが室温で流体のままであり、分散性であり、表面に適用されたときに刺激性がなく、毒性もなく、その他の点で有害でもなく、水性組成物の他の成分と相溶性であり、通常の使用及び保管条件下で化学的に安定であり、毛髪に付着することができ、かつ表面の状態を整える限り、任意の構造を有してよい。好適なＺ^８基としては、ヒドロキシ、メチル、メトキシ、エトキシ、プロポキシ、及びアリールオキシが挙げられる。ケイ素原子上の２つのＲ^９３基は、同一の基又は異なる基を表してもよい。好ましくは、２つのＲ^９３基は、同一の基を表す。好適なＲ^９３基としては、メチル、エチル、プロピル、フェニル、メチルフェニル及びフェニルメチルが挙げられる。好ましいシリコーン化合物は、ポリジメチルシロキサン、ポリジエチルシロキサン、及びポリメチルフェニルシロキサンである。ジメチコンとしても知られるポリジメチルシロキサンが、特に好ましい。本明細書で有用な市販のシリコーン化合物としては、例えば、Ｇｅｎｅｒａｌ Ｅｌｅｃｔｒｉｃ ＣｏｍｐａｎｙからＴＳＦ４５１シリーズで入手可能なもの、及びＤｏｗ ＣｏｒｎｉｎｇからＤｏｗ Ｃｏｒｎｉｎｇ ＳＨ２００シリーズで入手可能なものが挙げられる。

In the formula, R ⁹³ is an 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. Z ⁸ represents a group that blocks the end of the silicone chain. The alkyl or aryl group (R ⁹³ ) substituted at the end of the siloxane chain or the alkyl or aryl group Z8 substituted at the end of the siloxane chain allows the resulting silicone to remain fluid at room temperature, dispersible and ^on the surface. It is non-irritating, non-toxic, non-harmful in other respects when applied, compatible with other components of the aqueous composition, and chemically stable under normal use and storage conditions. It may have any structure as long as it can adhere to the hair and the surface condition is adjusted. Suitable ^Z8 groups include hydroxy, methyl, methoxy, ethoxy, propoxy, and aryloxy. The two ^R93 groups on a silicon atom may represent the same group or different groups. Preferably, the two ^R93 groups represent the same group. Suitable ^R93 groups include methyl, ethyl, propyl, phenyl, methylphenyl and phenylmethyl. Preferred silicone compounds are polydimethylsiloxane, polydiethylsiloxane, and polymethylphenylsiloxane. Polydimethylsiloxane, also known as dimethicone, is particularly preferred. Commercially available silicone compounds useful herein include, for example, those available in the TSF451 series from General Electric Company and those available in the Dow Corning SH200 series from Dow Corning.

Silicone gums can also be mentioned as the silicone compounds that can be used herein. As used herein, the term "silicone gum" means a polyorganosiloxane material having a viscosity of 1,000,000 mPa · s or higher at 25 ° C. It is recognized that the silicone gums described herein may have some overlap with the silicone compounds disclosed above. This duplication is not intended to be limiting in any of these materials. A "silicone gum" typically has a mass molecular weight of more than about 165,000, generally 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.

Low molecular weight silicones have viscosities of about 1 mPa · s to about 10,000 mPa · s, or about 5 mPa · s to about 5,000 mPa · s at 25 ° C., and about 400 to about 65,000, or about 800 to. It has a molecular weight of about 50,000.

Preferred lower molecular weight silicone compounds useful herein include polyalkylsiloxanes or polyarylsiloxanes having the following structures:

式中、Ｒ^９３はアルキル基又はアリール基であり、ｐは、約７～約８５０、より好ましくは約７～約６６５の整数である。Ｚ^８は、シリコーン鎖の末端を封鎖する基を表す。シロキサン鎖において置換されるアルキル若しくはアリール基（Ｒ^９３）又はシロキサン鎖の末端において置換されるアルキル若しくはアリール基Ｚ^８は、得られるシリコーンが室温で流体のままであり、分散性であり、表面に適用されたときに刺激性がなく、毒性もなく、その他の点で有害でもなく、水性組成物の他の成分と相溶性であり、通常の使用及び保管条件下で化学的に安定であり、毛髪に付着することができ、かつ表面の状態を整える限り、任意の構造を有してよい。好適なＺ^８基としては、ヒドロキシ、メチル、メトキシ、エトキシ、プロポキシ、及びアリールオキシが挙げられる。ケイ素原子上の２つのＲ^９３基は、同一の基又は異なる基を表してもよい。好ましくは、２つのＲ^９３基は、同一の基を表す。好適なＲ^９３基としては、メチル、エチル、プロピル、フェニル、メチルフェニル及びフェニルメチルが挙げられる。好ましいシリコーン化合物は、ポリジメチルシロキサン、ポリジエチルシロキサン、及びポリメチルフェニルシロキサンである。ジメチコンとしても知られるポリジメチルシロキサンが、特に好ましい。本明細書で有用な市販のこれらのシリコーン化合物としては、例えば、Ｇｅｎｅｒａｌ Ｅｌｅｃｔｒｉｃ ＣｏｍｐａｎｙからＴＳＦ４５１シリーズで入手可能なもの、及びＤｏｗ ＣｏｒｎｉｎｇからＤｏｗ Ｃｏｒｎｉｎｇ ＳＨ２００シリーズで入手可能なものが挙げられる。

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. Z ⁸ represents a group that blocks the end of the silicone chain. The alkyl or aryl group (R ⁹³ ) substituted at the end of the siloxane chain or the alkyl or aryl group Z8 substituted at the end of the siloxane chain allows the resulting silicone to remain fluid at room temperature, dispersible and ^on the surface. It is non-irritating, non-toxic, non-harmful in other respects when applied, compatible with other components of the aqueous composition, and chemically stable under normal use and storage conditions. It may have any structure as long as it can adhere to the hair and the surface condition is adjusted. Suitable ^Z8 groups include hydroxy, methyl, methoxy, ethoxy, propoxy, and aryloxy. The two ^R93 groups on a silicon atom may represent the same group or different groups. Preferably, the two ^R93 groups represent the same group. Suitable ^R93 groups include methyl, ethyl, propyl, phenyl, methylphenyl and phenylmethyl. Preferred silicone compounds are polydimethylsiloxane, polydiethylsiloxane, and polymethylphenylsiloxane. Polydimethylsiloxane, also known as dimethicone, is particularly preferred. Examples of these commercially available silicone compounds useful herein include those available in the TSF451 series from General Electric Company and those available in the Dow Corning SH200 series from Dow Corning.

The liquid beneficial agent of the present invention may contain one or more aminosilicones. The aminosilicone provided herein is a silicone 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, more preferably less than about 0.2% by weight, more preferably less than about 0.1% by weight nitrogen. The higher the concentration of nitrogen (amine functional group) in the aminosilicone, the less likely it is that friction reduction will occur, and as a result, the conditioning effect from the aminosilicone tends to decrease. It should be understood that in some product forms higher concentrations of nitrogen are also acceptable according to the present invention.

Aminosilicone is about 1,000 centipores (“cP”) to about 100,000 cP, or about 2,000 cP to about 50,000 cP, or about 4,000 cP to about 40,000 cP, or about 6,000 cP to about 30. It can have a viscosity of 000 cP. The viscosities of the aminosilicones described herein are measured at 25 ° C.

Aminosilicone is about 0.5% by weight to about 30% by weight, or about 1.0% by weight to about 24% by weight, or about 2.0% by weight to about 16% by weight, or about 3.0% by weight. It can be included in the aqueous composition of the present invention at a concentration of about 8% by weight.

Examples of preferred aminosilicones for use in the present invention include, but are not limited to, those according to general formula (I):
(R ¹ ) _a G _3-a -Si- (-OSiG ₂ ) _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 C ₁ to C ₈ alkyl, preferably methyl, a is an integer having a value of 0, or 1 to 3, preferably 1. 0, 1, or 2, preferably 1, a is 0, b is not 2, n is a number from 0 to 1,999, and m is an integer from 0 to 1,999. , N and m are numbers from 1 to 2,000, a and m are neither 0, R ¹ is a monovalent group according to the general formula CqH _2q L, and q is in the formula. An integer having a value of 2 to 8, where L is -N (R ² ) CH ₂ -CH ₂ -N (R ² ) ₂ , -N (R ² ) ₂ , -N (R ² ) ⁺ ₃ . Selected from the groups A- ^, -N (R ² ) CH ₂ -CH ₂ ^- NR ² H ₂ A-, in the formula, R ² is a hydrogen, phenyl, benzyl or saturated hydrocarbon group, preferably a saturated hydrocarbon group. It is an alkyl group of about C ₁ to about C ₂₀ , and A ⁻ is a halide ion.

Some silicones used herein are of formula (I) [in formula, m = 0, a = 1, q = 3, G = methyl, where n is preferably from about 1500 to about 1700, more. It is preferably about 1600, where L may comprise aminosilicone corresponding to -N (CH ₃ ) ₂ or -NH ₂ , more preferably -NH ₂ . For other aminosilicones, the formula (I) [in the formula, m = 0, a = 1, q = 3, G = methyl, n is preferably about 400 to about 600, more preferably about 500, L. May include -N (CH ₃ ) ₂ or -NH ₂ , more preferably -NH ₂ ]. These aminosilicones are sometimes referred to as terminal aminosilicones because one or both ends of the silicone chain are terminally treated with nitrogen-containing groups.

An exemplary aminosilicone corresponding to formula (I) is a polymer known as "trimethylsilyl amodimethicone" and is represented by formula (II) below:

式中、ｎは１～１，９９９の数であり、ｍは１～１，９９９の数である。

In the formula, n is a number from 1 to 1,999 and m is a number from 1 to 1,999.

The silicone may also be terminal aminosilicone. As defined herein, "terminal aminosilicone" means a silicone polymer containing one or more amino groups at one end or both ends of a silicone backbone. The hydrophobic coating may be substantially free of any silicone compound other than the terminal aminosilicone.

The amino group at least one terminal of the silicone backbone of the terminal aminosilicone can be selected from the group consisting of primary amines, secondary amines and tertiary amines. The terminal aminosilicone may follow Formula III:
(R ₁ ) _a G _3-a -Si- (-OSiG ₂ ) _n -O-SiG _3-a (R ₁ ) _a (III)
In the formula, G is hydrogen, phenyl, hydroxy, or C ₁ to C ₈ alkyl, preferably methyl, a is an integer having a value of 1 to 3, or b is 0, 1 or 2 or 1, where n is a number from 0 to 1,999, R ₁ is a monovalent group according to the general formula CqH _2q L, where q is 2 to 8 in the formula. L is an integer having the value of -N (R ₂ ) CH ₂ -CH ₂ -N (R ₂ ) ₂ , -N (R ₂ ) ₂ , -N (R ₂ ) ₃ A- ^, -N. (R ₂ ) Selected from the groups CH ₂ ^- CH ₂ -NR ₂ H ₂ A-, where R ₂ is a hydrogen, phenyl, benzyl or saturated hydrocarbon group ^and A- is a halide. It is an 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.

Suitable terminal aminosilicones corresponding to formula III are a = 1, q = 3, G = methyl, n is about 1000 to about 2500, or about 1500 to about 1700, and L is -N (CH ₃ ). ) ₂ . Suitable terminal aminosilicones corresponding to formula III are a = 0, G = methyl, n is about 100 to about 1500, or about 200 to about, and L is the following group: -N (R ₂ ). ) CH ₂ -CH ₂ -N (R ₂ ) ₂ , -N (R ₂ ) ₂ , -N (R ₂ ) ₃ A- ^, -N (R ₂ ) CH ₂ -CH ₂ ^- NR ₂ H ₂ A- In the formula, R ₂ is a hydrogen, phenyl, benzyl, or saturated hydrocarbon group, A ^- is a halide ion, or L is -NH ₂ . _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 aminosilicone can be selected from the group consisting of bis-aminomethyldimethicone, bis-aminoethyldimethicone, bis-aminopropyldimethicone, bis-aminobutyldimethicone, and mixtures thereof.

Suitable terminal aminosilicones include aminopropyl-terminal polydimethylsiloxanes (eg, having a viscosity of 4,000-6,000 cSt (4-6 Pa · s)); Gelest, Inc. (Available under the trade name DMS-A35), polydimethylsiloxane, trimethylsiloxy-terminated (eg, having a viscosity of 5,000 cSt (5 Pa · s)); Gelest, Inc. (Available under the trade name DMS-T35), polydimethylsiloxane, trimethylsiloxy-terminated (eg, with a viscosity of 1,000 cSt (1 Pa · s)); Gelest, Inc. (Available under the trade name DMS-T31), aminopropyl-terminated polydimethylsiloxane (eg, having a viscosity of 900 to 1,100 cSt (0.9 to 1.1 Pa · s)); Gelest, Inc. (Available under the trade name DMS-A31), polydimethylsiloxane, trimethylsiloxy-terminated (eg, having a viscosity of 50 cSt (0.05 Pa · s)); Gelest, Inc. (Available under trade name DMS-T15), aminopropyl-terminated polydimethylsiloxane (eg, 50-60 cSt (having a viscosity of 0.05-0.06 Pa · s); from Gelest, Inc. under trade name DMS-A15. (Available), bis-aminopropyldimethicone (eg, having a viscosity of 10,220 cSt (10.2 Pa · s)); Momentive Performance Materials Inc. (Available from), and mixtures thereof.

Suitable conditioning agents as beneficial agents for alkylsiloxane polymers hydrophobic coatings include US Patent Application Publication Nos. 2011/0243874 (A1), 2011/0243875 (A1), 2011/0240065 (A1). , 2011/0243788 (A1), 2011/0243871 (A1), and 2011/0243876 (A1), further include alkylsiloxane polymers.

Suitable conditioning agents as beneficial agents for cationic organopolysiloxane hydrophobic coatings include US Patent Application Publication Nos. 2014/0030206 (A1), International Publication Nos. 2014/018985 (A1), 2014/018986 (A1). Further, as described in detail in A1), 2014/018987 (A1), 2014/018988 (A1), 2014/018989 (A1), cationic organopolysiloxanes are further added. included.

Organic Oils The liquid beneficial agents of the present invention may include at least one organic conditioning oil as a conditioning agent, alone or in combination with other conditioning agents such as silicone.

Hydrocarbon-based beneficial materials include 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.

Hydrocarbon oils Suitable organic oils for use as liquid beneficial agents in the aqueous compositions of the present invention include hydrocarbon oils having at least about 10 carbon atoms, such as cyclic hydrocarbons, linear aliphatic hydrocarbons. Examples include, but are not limited to, hydrogen (saturated or unsaturated) and branched chain aliphatic hydrocarbons (saturated or unsaturated) (including, but not limited to, polymers thereof and mixtures thereof). The linear hydrocarbon oil is preferably about C ₁₂ to about C ₁₉ . Branched-chain hydrocarbon oils (including hydrocarbon polymers) typically contain more than 19 carbon atoms.

Specific non-limiting examples of these hydrocarbon oils include paraffin oils, mineral oils, saturated and unsaturated dodecanes, saturated and unsaturated tridecanes, saturated and unsaturated tetradecanes, saturated and unsaturated pentadecanes, saturated and unsaturated hexadecanes. , Polybutene, polyisobutylene, polydecane, and mixtures thereof. Branched chain isomers as well as long chain hydrocarbons of these compounds can also be used, eg, highly branched, saturated or unsaturated alkanes such as permethyl substituted isomers, 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) and other permethyl-substituted isomers of hexadecane and icosane. Can be mentioned. Hydrocarbon polymers such as polybutene and polydecene. Preferred hydrocarbon polymers are polybutene, such as copolymers 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 is from about 0.05% to about 20% by weight, or from about 0.08% to about 1.5% by weight, or from about 0.1% by weight. It can be in the range of about 1% by weight.

Polyolefins Examples of the organic oil for use as a liquid beneficial agent include liquid polyolefins, more preferably liquid poly-α-olefins, and more preferably hydrogenated liquid poly-α-olefins. Polyolefins for use herein are prepared by polymerizing an olefinic monomer of C ₄ to about C ₁₄ , preferably about C ₆ to about C ₁₂ .

Non-limiting examples of olefinic monomers used to prepare the polyolefin liquids herein are ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-octene, 1-decene. , 1-dodecene, 1-tetradecene, 4-methyl-1-pentene and other branched chain isomers, and mixtures thereof. Olefin-containing purified raw materials or eluates are also suitable for preparing polyolefin solutions. Preferred hydrogenated α-olefin monomers include, but are not limited to, 1-hexene to 1-hexadecene, 1-octene to 1-tetradecene, and mixtures thereof.

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. Examples of these fatty acid esters include esters with hydrocarbyl chains derived from fatty acids or alcohols (eg, monoesters, polyhydric alcohol esters, and di- and tri-carboxylic acid esters). The hydrocarbyl group of the fatty acid ester herein may contain other compatible functional groups such as amides and alkoxy moieties (eg, ethoxy or ether bonds) or may be covalently attached to it.

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, and adipine. Examples include, but are not limited to, dihexyl decyl acid acid, lauryl lactate, myristyl lactate, cetyl lactate, oleyl stearate, oleyl oleate, oleyl myristate, lauryl acetate, cetyl propionate, and oleyl adipate.

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

Still other fatty acid esters suitable for use in the aqueous compositions of the present invention are esters of _C4 to _C8 dicarboxylic acids ₍ eg, C1 to _C22 of succinic acid, glutaric acid, and adipic acid, preferably C. Di- and tri-alkyl and alkenyl esters of carboxylic acids such as _{1 -} C6 esters). Specific non-limiting examples of di- and tri-alkyl and alkenyl esters of carboxylic acids include isosetylstearoylstearate, diisopropyladipate, and tristearylcitrate.

Other fatty acid esters suitable for use in the aqueous compositions of the present invention are known as polyhydric alcohol esters. Examples of such polyvalent alcohol esters include ethylene glycol mono and difatty acid ester, diethylene glycol mono and difatty acid ester, polyethylene glycol mono and difatty acid ester, propylene glycol mono and difatty acid ester, polypropylene glycol monooleate, and polypropylene glycol 2000 monosteer. Rate, ethoxylated propylene glycol monostearate, glyceryl mono and difatty acid ester, polyglycerol polyfatty acid ester, ethoxylated monostearate glyceryl, 1,3-butylene glycol monostearate, 1,3-butylene glycol distearate, Examples thereof include alkylene glycol esters such as polyoxyethylene polyol fatty acid ester, sorbitan fatty acid ester, and polyoxyethylene sorbitan fatty acid ester.

Still other fatty acid esters suitable for use in the aqueous compositions of the present invention are glycerides, examples of which are mono-, di-, and tri-glycerides, more preferably di- and tri-glycerides. Examples include, but are not limited to, triglycerides. When used in the aqueous compositions described herein, the glycerides are preferably mono-, di- and try esters of glycerol and long chain carboxylic acids such as C ₁₀ -C ₂₂ carboxylic acids. Various these types of materials are obtained from plant 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. be able to. Examples of synthetic oils include, but are not limited to, triolein and tristeering lyceryl dilaurate.

Another fatty acid ester suitable for use in the aqueous composition of the present invention is a water-insoluble synthetic fatty acid ester. Some preferred synthetic esters are consistent with the general formula (IX):

式中、Ｒ^１は、Ｃ_７～Ｃ_９アルキル、アルケニル、ヒドロキシアルキル、又はヒドロキシアルケニル基であり、好ましくは飽和アルキル基、より好ましくは飽和直鎖アルキル基であり、ｎは２～４、好ましくは３の値を有する正の整数であり、Ｙは約２～約２０個の炭素原子、好ましくは約３～約１４個の炭素原子を有する、アルキル、アルケニル、ヒドロキシ又はカルボキシ置換アルキル又はアルケニルである。他の好ましい合成エステルは、一般式（Ｘ）に一致する：

In the formula, R ¹ is a C ₇ to C ₉ alkyl, alkenyl, hydroxyalkyl, or hydroxyalkenyl group, preferably a saturated alkyl group, more preferably a saturated linear alkyl group, and n is 2 to 4, preferably. Is a positive integer having a value of 3 and Y is an alkyl, alkenyl, hydroxy or carboxy-substituted alkyl or alkenyl having about 2 to about 20 carbon atoms, preferably about 3 to about 14 carbon atoms. be. Other preferred synthetic esters correspond to the general formula (X):

式中、Ｒ^２は、Ｃ_８～Ｃ_１０アルキル、アルケニル、ヒドロキシアルキル、又はヒドロキシアルケニル基であり、好ましくは飽和アルキル基、より好ましくは飽和直鎖アルキル基であり、ｎ及びＹは、式（Ｘ）において上に定義したとおりである。

In the formula, R ² is a C ₈ to C ₁₀ alkyl, alkenyl, hydroxyalkyl, or hydroxyalkenyl group, preferably a saturated alkyl group, more preferably a saturated linear alkyl group, and n and Y are formulas (n and Y. As defined above in X).

Specific non-limiting examples of synthetic fatty acid esters suitable for use in the aqueous compositions of the invention are P-43 (C _{- 8} to C10 triesters of trimethylolpropane), MCP-684 (3, 3). 3 Diethanol-1,5 _- pentanediol tetraester), _MCP121 (C8 to C10 diester of adipic acid), all of which are available from the Mobile Chemical Company.

Metathesis Unsaturated Polyol Esters Other suitable organic oils as beneficial agents include metathesis Unsaturated polyol esters. Exemplary metathesisted unsaturated polyol esters and their starting materials are described in US Patent Application Publication No. 2009/0220443 (A1). Metathesis-ized unsaturated polyol ester refers to the product obtained when one or more unsaturated polyol ester components are subjected to a metathesis reaction. Metathesis is a catalytic reaction involving the exchange of alkylene units between compounds containing one or more double bonds (ie, 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).

Silane-modified oil Other suitable organic oils as liquid beneficial agents include silane-modified oil. Generally, suitable silane-modified oils include a hydrocarbon chain selected from the group consisting of saturated oils, unsaturated oils, and mixtures thereof, and hydrolyzable silyl groups covalently bonded to the hydrocarbon chains. Suitable silane-modified oils are described in detail in US Patent Application No. 61 / 821,818, filed May 10, 2013.

Other Liquid Beneficial Agents The liquid beneficial agents described in US Pat. Nos. 5,674,478 and 5,750,122 by Procter & Gamble Company are also used in the aqueous compositions herein. Suitable for. In addition, US Pat. Nos. 4,529,586 (Clairol), 4,507,280 (Clairol), 4,663,158 (Clairol), 4,197,865 (L'). Oral), No. 4,217,914 (L'Oreal), No. 4,381,919 (L'Oreal), and No. 4,422,853 (L'Oreal). Beneficial agents are also suitable for use herein.

Fragrances The hydrophobic beneficial agents of the present invention may also contain one or more perfumes. One or more fragrances can be selected from any fragrance or fragrance chemical suitable for topical application to the particular surface to be treated. The concentration of the fragrance in the personal care composition needs to be an effective concentration to provide the desired fragrance, such as, but not limited to, unscented ones. Generally, the concentration of the fragrant main fragrance is about 0.5% to about 30%, or about 1% to about 20%, or about 2% to about 10%, or about 3% to about 8% of the solid article. be.

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

Aqueous Carriers Aqueous compositions may include aqueous carriers. The aqueous carrier used can be distilled water, deionized water or tap water. Water may be present in any amount of the composition, which is an aqueous solution. Water is about 85% by weight to 99.5% by weight, preferably about 90% by weight to about 99.5% by weight, more preferably about 92% by weight to about 99.5% by weight, more preferably about. It may be present in an amount of 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.

Trace component The composition may contain one or more trace components in the aqueous phase. Trace components are water-soluble metal salts including buffers, solubilizers, antibacterial compounds, preservatives, malodor neutralizers, fragrance delivery technologies, diluents, antioxidants, zinc salts, copper salts, antistatic agents; Pest repellent; colorant, selected from the group consisting of combinations thereof.

Aqueous compositions may be added to any excess hydrophobic organic material, in particular certain malodor reducing materials, fragrance materials, as well as aqueous compositions for producing clear translucent solutions. Substantially low concentrations of solubilizing aids may be included to solubilize optional components that are not readily soluble in the composition (eg, 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, amphoteric ionic surfactants, and mixtures thereof. If present, the solubilizing aid is preferably a nonionic surfactant.

Aqueous compositions 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 an aqueous composition is sold as Basophor ™ (available from BASF).

When the aqueous composition comprises a surfactant, the total amount of the surfactant present in the aqueous composition is less than 10,000 ppm, preferably less than 1,000 ppm, 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, "effective amount of surfactant" is the amount of surfactant in the aqueous composition in which the surfactant acts as an emulsifier between the liquid beneficial agent droplets and the aqueous carrier. ..

The buffering agent can include a carboxylic acid, a dicarboxylic acid such as maleic acid, a polybasic acid such as citric acid, or a polyacrylic acid.

Non-limiting examples of this type of surface tension reducing agent are described in US Pat. No. 5,714,137 and the Silket® interface available from Momentive Performance Chemical, Aliquid benefit agent, New York. Activators can be mentioned. Exemplary Silvert surfactants are:

Examples of the water-soluble antibacterial compound 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.

A quaternary compound may be used. Examples of commercially available quaternary compounds suitable for use in aqueous compositions are Barquat available from Lonza Corporation; and quaternary didecyldimethyl available from Lonza Corporation under the trade name Bardac® 2250. There is ammonium chloride.

Fragrance delivery technologies include professional fragrances, polymer particles, soluble silicones, polymer-assisted delivery, molecule-assisted delivery, fiber-assisted delivery, amine-assisted delivery, cyclodextrins, starch-encapsulated accords, zeolites, and inorganic carriers, as well as these. It can be selected from the group consisting of mixtures.

Solid Particles Aqueous compositions may contain multiple solid particles. Solid particles can be in the form of mesoporous particles, activated carbon, zeolites, beneficial agent delivery particles, waxes, hydrogels, ground nut shells, and / or combinations thereof.

The solid particles can be in the form of beneficial agent delivery particles. Beneficial agent delivery particles may include a wall material that encloses the beneficial agent. Beneficial agents may be referred to herein as "beneficial agents" or "encapsulated beneficial agents." Beneficial agents may be selected from the group consisting of fragrance mixtures, insect repellents, stink neutralizers, and combinations thereof. Beneficial agents include 3- (4-t-butylphenyl) -2-methylpropanol, 3- (4-t-butylphenyl) -propanal, 3- (4-isopropylphenyl) -2-methylpropanol. , 3- (3,4-Methylenedioxyphenyl) -2-methylpropanol, and 2,6-dimethyl-5-heptenal, α-damascorn, β-damascorn, γ-damascorn, β-damasenone, 6,7 -Dihydro-1,1,2,3,3-pentamethyl-4 (5H) -Indanone, Methyl-7,3-dihydro-2H-1,5-benzodioxepin-3-one, 2- [2- [2- (4-Methyl-3-cyclohexenyl-1-yl) propyl] cyclopentane-2-one, 2-sec-butylcyclohexanone, and β-dihydroionone, linalol, ethyllinalol, tetrahydrolinalol, and dihydromilsenol. Fragrance raw materials such as; silicone oil, wax such as polyethylene wax; essential oils such as fish oil, jasmine, phenyl, lavender; skin cooling agents such as menthol, methyl lactate; vitamins such as vitamins A and E; sunscreens; glycerin; Catalysts such as manganese catalysts or bleaching agent catalysts; bleaching agent particles such as perborate; silicon dioxide particles; antiperspirant active substances; cationic polymers, and materials selected from the group consisting of mixtures thereof. obtain. Suitable beneficial agents are Givaudan Corp. (Mount Olive, New Jersey, USA), International Flavors & Fragrances Corp. It can be obtained from (South Brunswick, New Jersey, USA) or Firmenich Company (Geneva, Switzerland).

Beneficial agents can include materials that are liquid beneficial agents, as described in the present invention. In such an example, the aqueous composition may include liquid beneficial agent droplets dispersed discontinuously throughout the aqueous phase, in addition to the encapsulated liquid beneficial agent dispersed throughout the aqueous phase.

In one aspect, the perfume delivery technique may include beneficial agent delivery particles made by at least partially wrapping with a beneficial agent having a wall material.

The wall material of the beneficial agent delivery particles is melamine, polyacrylamide, silicone, silica, polystyrene, polyurea, polyurethane, polyacrylate-based material, polyacrylic acid ester-based material, gelatin, styrene-apple acid anhydride, polyamide, aromatic alcohol. , Polyvinyl alcohol, and mixtures thereof. Melamine wall materials can include formaldehyde-crosslinked melamine, formaldehyde-crosslinked melamine-dimethoxyethanol, and mixtures thereof. Polystyrene wall materials may include polystyrene crosslinked with divinylbenzene. Polyurea wall materials can include formaldehyde-crosslinked urea, glutaraldehyde-crosslinked urea, polyamide-reacted polyisocyanates, aldehyde-reacted polyamines, and mixtures thereof. Polyacrylate-based wall materials include polyacrylates formed from methyl methacrylate / dimethylaminomethyl methacrylate, amine acrylates and / or methacrylates, and polyacrylates formed from strong acids, carboxylic acid acrylates and / or methacrylate monomers, and strong bases. Polyacrylates, amine acrylates and / or methacrylate monomers and polyacrylates formed from carboxylic acid acrylates and / or carboxylic acid methacrylate monomers, and mixtures thereof may be included.

Polyacrylic acid ester-based wall materials include polyacrylic acid esters formed by alkyl and / or glycidyl esters of acrylic acid and / or methacrylic acid, acrylic acid esters having hydroxy and / or carboxy groups and allylgluconamides and /. Alternatively, it may contain a polyacrylic acid ester formed by a methacrylic acid ester, and a mixture thereof.

The aqueous composition may contain any amount of particles. With respect to the beneficial agent delivery particles, the aqueous composition may contain from about 0.001% by weight to about 2.0% by weight of the beneficial agent, including the wall material of the beneficial agent delivery particles. Alternatively, the aqueous composition is a wall of beneficial agent delivery particles of from about 0.01% to about 1.0% by weight, or most preferably from about 0.05% to about 0.5% by weight of the aqueous composition. It may contain a beneficial agent containing the material.

The aqueous composition of the present invention can be a hair conditioner composition. The hair conditioner composition may include one or more liquid beneficial agents that are water-insoluble hydrophobic conditioning agents such as silicones, organic oils, or other water-insoluble conditioning agents.

The hair conditioner composition may also include a gel matrix containing a combination of a cationic surfactant and a refractory aliphatic alcohol (melting point above 25 ° C.).

Non-limiting examples of refractory aliphatic alcohols include ethyl alcohol, stearyl alcohol, behenyl alcohol, and mixtures thereof. An exemplary hair conditioning composition of the present invention is shown in Example 1.

Production Method As described above, a phase-stable aqueous composition containing a structuring agent system and an aqueous phase containing liquid beneficial agent droplets disperse discontinuously throughout the aqueous phase by the method for producing an aqueous composition of the present invention. Was found to be obtained. The formation of a phase-stable discontinuous phase of the liquid beneficial agent droplets in the final aqueous composition requires at least two steps, an emulsification step and a dilution step.

In the emulsification step, the liquid beneficial agent is emulsified into a concentrate. The concentrate contains some or all structuring agent systems, some water, and optionally some or all trace components. First, a concentrate is formed by mixing a structuring agent system, water, and any trace components. The liquid beneficial agent is then emulsified into a concentrate using a strong mixture. Without being bound by theory, the concentrate is a relatively high concentration, the viscosity of which is set to substantially match the viscosity of the liquid beneficial agent in order to effectively disperse the liquid beneficial agent. It has a structuring agent system. In addition, the ratio and concentration of polysaccharides are selected to ensure the presence of yield stress, which eliminates drainage between droplets in the concentrate and provides stability to droplet creaming and coalescence. Be thorough. Both studies are needed to surprisingly enable the formation of stable emulsions of liquid beneficial agent droplets without the need for detergents or at very low concentrations of detergents.

The dilution step is then diluted with additional water to form the final aqueous composition. Along with additional water, additional structuring agent systems and / or trace components 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 liquid beneficial agent droplets formed in the aqueous phase concentrate.

Various mixers can be used to mix the liquid beneficial agent into the concentrated aqueous phase. The mixer can be a high speed mixer, a static mixer, an overhead mixer, or any other mixer. Preferably, a fast mixer can be used to form liquid beneficial agent droplets. However, any mixer is suitable as long as sufficient mixing is applied to disperse the liquid beneficial agent into the liquid beneficial agent droplets.

In order to emulsify the liquid beneficial agent in the concentrate, the viscosity of the concentrate is 10 Pa · s to 0.00 Pa · s, more preferably 1 Pa · s to 0.01 Pa · s, as measured by the rheology test method. It can be more preferably 1 Pa · s to 0.1 Pa · s, and most preferably 1 Pa · s to 0.3 Pa · s. The concentrate has a yield stress of more than 2 Pa to 0 Pa, more preferably 1.5 Pa to 0.02 Pa, more preferably 1.0 Pa to 0.05 Pa, and most preferably 1 Pa to 0.3 Pa when measured by a rheology test method. Must be shown.

The aqueous composition comprises 0.1% by weight to 20% by weight, more preferably 10% by weight to 0.2% by weight, more preferably 5% by weight to 0.5% by weight, and most preferably 5% by weight to 0% by weight. Contains 5% by weight liquid beneficial agent droplets.

Achievements in the emulsification step are defined by the droplet size of the liquid beneficial agent, the liquid beneficial agent on the surface of the preparation, and the stability. The most preferred aqueous composition has a liquid beneficial agent droplet diameter of less than about 500 μm, most preferably less than about 250 μm, most preferably less than about 100 μm, as evidenced by the turbidity in the preparation; 24 hours. Only very small amounts of the liquid beneficial agent are essentially present on the surface of the preparation in the production of; there is no instability in the preparation, as indicated by the bulk separation of the liquid beneficial agent. Preferred aqueous compositions have a liquid beneficial agent droplet diameter of less than about 500 μm, most preferably less than about 250 μm, most preferably less than about 100 μm, as evidenced by the turbidity in the preparation; for 24 hours. Very small amounts of liquid beneficial agent are present on the surface of the preparation in production (estimated to be less than 5% by weight of the total mixture); no instability in the preparation as indicated by bulk separation of the liquid beneficial agent. .. Comparative embodiments have a diameter of liquid beneficial agent droplets greater than about 500 μm or show incomplete dispersion, as evidenced by the relative clarity in the preparation; the surface of the preparation in 24 hours of production. There is a significant liquid beneficial agent (estimated to be greater than 5% by weight of the total mixture); there is significant instability in the preparation as indicated by the bulk separation of the liquid beneficial agent. Achievements in the dilution step bring liquid beneficial agent droplets of comparable droplet size to the most preferred or preferred aqueous composition.

Test Method Rheology Test Method To measure the yield stress and / or viscosity of a sample (eg, concentrate or aqueous composition, but not LBA), TA Discovery HR-2 Hybrid Rheometer (TA Instruments (New Castle, Delaware, U). Measurements are made using S.A.)) and the accompanying TRIOS software version 4.2.1.36612, or equivalent. This device includes concentric cylinders Double Gap Cup (eg, TA Instrument, catalog number 546050.901), Double Gap Rotor (eg, TA Instruments, catalog number 546049.901), and Split Coverer (eg, TA Instruments, catalog number). 545626.001) is equipped. Calibrate according to the manufacturer's recommendations. A cooling circulation water bath set at 25 ° C. is attached to the concentric cylinder. Set the concentric cylinder temperature to 25 ° C. The temperature may be monitored in the control panel until the instrument reaches the set temperature, at which time the sample material may be loaded into the Double Gap Cup after an additional 5 minutes to ensure equilibrium.

The parameters for Double Gap Cup are as follows. The inner cup diameter is 30.2 mm, the inner bob diameter is 32 mm, the outer bob diameter is 35 mm, the outer cup diameter is 37 mm, the inner cylinder height is 55 mm, and the immersion height. Is 53 mm, the operating gap is 2,000.0 μm, the loading gap is 900.0 μm, the environmental system is Pelche, and the sample volume is 12 ml to 15 ml (preferably 12 ml). ..

To load the sample, use a syringe to add at least 12 ml of the sample to the Double Gap Cup, then allow the sample to stand for 15 minutes to ensure that any air bubbles trapped on the surface emerge. The Double Gap Rotor is then lowered to the appropriate gap and data is collected according to the following settings and procedures.

Data is collected in a series of steps that are performed exactly in the following order. Perform the sample adjustment process using the following device settings. Set environmental control at a temperature of 25 ° C; select Inherit Set Point as Off; set Sok Time to 0.0s; select Wait for Temperature as On; select Wait for axial force as Off; Select Performance Pressear as Off to set the Pressear Options; select Performance Equilibration as On, set the Equilibrium, and set the Duration to 600.0s.

The flow peak holding step is performed using the following equipment settings. Set the Environmental Control at a temperature of 25 ° C; select the Inherit Set Point as Off; set the Sok Time to 0.0s; select the Wait for Torque as Off; set the Test Parameters to 600.0s. Select Shear Rate and set it to 0.01s-1; select Inherit internal value as Off; select Sampleting interval and set it to 3.0s / pt; select Motor mode as Auto and Control Set Rate Advanced; Select End of step as Zero torque to set Data accuracy; Set Fast Sample as Off; Select Save image as Off; Set Limit Switching selected as On Yes; select Strine (%), select>, set to 500% and set the Temperature step when; select Equilibrium Enabled as Off; select Step Repeat Enabled as Off.

The sample preparation process is performed using the following equipment settings. Set the Environmental Control at 25 ° C. Temperature; select the Inherit Set Point as Off; set the Sok Time to 10.0s; select Wait for Temperature as Off; select Wait for Force; Select Presear as Off to set the Presear Options; select Performance Equilibration as On, set the Equilibrium, and set the Duration to 600.0s.

The flow sweep process is performed using the following device settings. Set the Environmental Control at a temperature of 25 ° C; select the Inherit Set Point as Off; set the Soak Time to 0.0s; select the Wait For Temperture as Off; select the Logarithmic Swep and select Data Select Shear Rate and set it to 1.0e-3s-1 to 1000.0s-1; Set Points Per Decade to 5; Select Steady State Sensing as On; Max Equilibration Time to 45.0s Set; Set Single Period to 5.0s; Set% Temperature to 5.0; Set Consecutive Within to 3; Select Scaled Time Average as Off; Select Motor Mode as Auto and Control Set Rate Advanced; Select Save Point Display as Off to set Data Acquisition; Select Save image as Off; Select Limit Checking Enable as Off; Select Step Ember as Off; Set Steady State Select; Step Repeat Allow as Off.

The adjustment process at the end of the test is performed using the following device settings. Select Set Temperature as Off; select Set Temperature System Idle (only if axial force management is active) as On.

The yield stress is calculated from the data collected during the flow peak holding process by the following method. Data points are plotted as stress (mPa) on the y-axis with respect to the step time (s) on the x-axis. Yield stress is determined by selecting the "Analysis" tab, then selecting "Signal max" from the Function drop-down list, and finally selecting "Analysis" within the Commands category. For continuous datasets (including a single stress value greater than zero for each time value), if a "maximum Y" value occurs in the first 250 seconds, the yield stress will be a "maximum Y" value. Equal, if the value of "maximum Y" occurs after 250 seconds, the yield stress is equal to zero. If the measured sample is a concentrate, the value is defined as the yield stress of the concentrate (“YS _cone. ”); If the measured sample is an aqueous composition, the value is the yield stress of the aqueous composition. Defined as ("YS _aku. "); If no yield stress was measured, the yield stress of the concentrate and / or aqueous composition is assigned a value of "NM".

Viscosity is determined as the viscosity measured when the shear rate is 10s-1, or as the viscosity measured at the nearest data point within 1% of the shear rate of 10s-1, expressed in mPa · s. If the measured sample is a concentrate, the value is defined as the viscosity of the concentrate ("h _cone. "); If the measured sample is an aqueous composition, the value is the viscosity of the aqueous composition ("h cone."). Defined as " _{ha qua.} "); If no yield stress was measured, the viscosity of the concentrate and / or the aqueous composition is assigned a value of "NM".

LBA Test Method Viscosity Measurements of the viscosity of liquid beneficial agents include TA Discovery HR-2 Hybrid Rheometer (TA Instruments, New Castle, Delaware, USA), and the accompanying TRIOS software version 4.2.1. This is done using 36612, or equivalent. The instrument is equipped with a 60 mm stainless steel cone with a two degree angle (eg, TA Instruments, catalog number 511606.095), a Pelce plate (TA Instruments, catalog number 533230.901). Calibrate according to the manufacturer's recommendations. A cooling circulation water bath set at 25 ° C. is attached to the Pelche plate. Set the temperature of the Pelche plate to 25 ° C. Monitor the temperature in the control panel until the device reaches the set temperature.

To load the Liquid Beneficial Agent (LBA), transfer 2 ml of LBA onto the central surface of the Pelche plate using a 5 ml slip tip syringe or the like. If the loaded sample liquid contains visible bubbles, wait 10 minutes and wait for the bubbles to move through the sample and burst, or the bubbles can be removed using a transfer pipette. If visible air bubbles still remain, remove the sample from the plate, clean the plate with an isopropanol wipe and evaporate the solvent. The sample loading procedure is then retried and repeated until the sample is successfully loaded without visible air bubbles.

The 60mm cone is lowered to the "trim gap". This is unique to the cone for this attachment and has been shown to be 66 micrometers. The cone is then locked and a flexible rubber spatula, such as a rubber policeman, is used to remove excess sample material from around the cone. It is important to ensure that the sample is evenly distributed around the edge of the cone and that there is no sample 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.

Data is collected in a series of steps that are performed exactly in the following order. Perform the sample adjustment process using the following device settings. Set environmental control to a temperature of 25 ° C; select Inherit Set Point as Off; set Sok Time to 0.0s; select Wait for Temperture as On; select Wait For Axial Force as Off; Perform Select Pressear as On and set Pressear Options; set the shear rate to 100.0 1 / s; set the duration to 20.0 seconds; after pre-shear is selected for Leave, at zero velocity Set advanced options; set zero velocity threshold as 0.1 rad / s; select Motor mode as Auto; select Performance Equilibration as On, set Equilibrium, and set Duration to 600.0s.

The flow sweep process is performed using the following device settings. Set the Environmental Control at a temperature of 25 ° C; select the Inherit Set Point as Off; set the Soak Time to 0.0s; select the Wait For Temperture as Off; select the Logarithmic Swep and select Data Select Shear Rate and set it to 1.0e-3s-1 to 1000.0s-1; Set Points Per Decade to 15; Select Steady State Sensing as On; Max Equilibration Time to 45.0s Set; Set Single Period to 5.0s; Set% Temperature to 5.0; Set Consecutive Within to 3; Select Scaled Time Average as Off; Select Motor Mode as Auto and Control Set Rate Advanced; Select Save Point Display as Off to set Data Acquisition; Select Save image as Off; Select Limit Checking Enable as Off; Select Step Ember as Off; Set Steady State Select; Step Repeat Allow as Off.

The adjustment process at the end of the test is performed using the following device settings. Select Set Temperature as On; set the temperature to 25 ° C. Select Set Temperature System Idle (only when axial force management is active) as Off.

The LBA viscosity is determined as the viscosity measured when the shear rate is 100s-1, or the viscosity measured at the nearest data point within 1% of the shear rate of 100s-1. The reported LBA viscosity values (“h _LBA ”) are the average of the viscosity values obtained from three independent viscosity measurements (ie, three repeated sample preparations) and are expressed in units of mPa · s. Will be done. If the viscosity of the sample was not measured, the viscosity value reported for LBA (“h _LBA ”) is given a value of “NM”.

Drop size test method A light microscope is used to measure the drop size, which is the number-weighted average diameter of the liquid beneficial agent droplets in the test sample of the composition. It should be noted that the drop size values claimed herein refer to the average diameter and the values are number weighted rather than volume weighted. Droplets are imaged using a transmitted light composite microscope equipped with a digital camera and an array of flatfield objectives at 10x to 100x magnification. The microscope is tuned for Kohler illumination and calibrated for linear measurements in the xy image plane using a stage micrometer. Suitable microscopes include a Zeiss AxioCam digital camera (Carl Zeiss AG (Oberkochen, Germany)) or an equivalent Zeiss Axio Imager (Carl Zeiss AG) that employs Normarski differential interference contrast contrast (DIC). ). One of ordinary skill in the art will use image analysis software (such as AxioVision, Carl Zeiss Microscopy GmbH, Germany, or ImagePro Premier, Media Cybernetics, Rockville Maryland USA, or equivalent) to measure the diameter of the image. You can choose that. Measurements in the image can also be made using a precisely calibrated physical device such as a ruler, caliper, reticle, reticle.

Before measuring their average drop size, it is necessary to visually inspect the samples to make sure they are well emulsified, including a homogeneous dispersion of LBA. A poorly emulsified sample may exhibit one of two characteristics: 1) The sample looks almost transparent (ie, almost turbid) because it contains a few very large LBA drops. No) or 2) Containing a visually enriched or increased LBA concentrate near the surface of the preparation, the LBA is not evenly dispersed throughout the volume. If the sample appears visually well emulsified, measure the average drop size as described below. If the sample does not appear to be fully emulsified, the average drop size is not measured and instead the diameter value of the final average drop size is assigned the "IE" value of "Infective Emulsion".

A sample of the fully emulsified composition is used to make a wet mount slide preparation. Now drop a few drops of the composition on a standard or concave glass microscope slide and gently cover with a standard glass coverslip. Make the wet mount slide preparation three times. Observe the preparation under a microscope without delay and be careful not to apply as much pressure or shear as possible to the coverslip.

The prepared sample is observed under a microscope under several different magnifications to assess the range of typical and numerically highest droplet sizes in the sample. This evaluation is used to select the objective lens that provides the image. Here, the diameters of the most representative droplets are perfectly adjusted within the captured image and also magnified sufficiently to allow accurate measurements of their diameters. Such images are captured from each duplicate sample preparation until at least 10 representative droplets are imaged.

Within the captured image, the diameter of all particles that look like nearly circular (spherical) droplets is measured. Measurements of non-droplet objects such as bubbles or solid microcapsules are excluded from the recorded values. The average diameter value is calculated from all droplets measured in each duplicate wet mount slide preparation. Final average diameter value

は、全ての複製にわたって計算された平均値であり、液体有益剤滴サイズの直径としてマイクロメートル単位で報告される。サンプル上で平均滴サイズが測定されなかった場合、最終的な平均直径値

Is the average value calculated over all replicas and is reported in micrometer increments as the diameter of the liquid beneficial droplet size. If the average drop size was not measured on the sample, the final average diameter value

には「ＮＭ」の値が与えられる。

Is given a value of "NM".

Sprayability Test Method The sprayability of the composition is determined by measuring the angle of the spray cone produced during the attempted spraying and comparing this value with the value obtained from the specified negative control reference solution. Compositions are classified as either "sprayable" or "non-sprayable". The composition typically forms a visible cone-shaped plume of droplets exiting the nozzle. Here, the cone is narrowest when it is closest to the nozzle, widens as it is further away from the nozzle, and then the plume of the droplets is finally dispersed. The angle of the spray cone is measured by attempting to spray the composition vertically over the display area of the recording video camera under conditions of sufficient lighting and no ventilation. The image captured by the video camera is analyzed to measure the angle of the cone in the visible plume of the sprayed material within a region extending 10 cm outside the nozzle in the direction of the plume trajectory. The angle of the spray cone is defined as the angle measured between the two specified straight lines. One designated straight line is the central axis of the locus of the plume away from the nozzle, and the other designated straight line is the visual average of the plume at the first 10 cm distance away from the nozzle. Possible upper outer margin.

The camcorder should be firmly mounted to prevent movement and vibration, positioned, zoomed and focused so that the plume area at least 10 cm from the nozzle is in focus. One of the suitable video cameras is Phantom V310 (Vision Research). Select lighting and background conditions to allow the plume of droplets to be easily observed in high contrast in the captured image. The composition, bottle, and environment are at laboratory ambient air temperature of 18 ° C-25 ° C. The air conditions surrounding the nozzle and spray plume area are as steady as possible.

During the analysis, each composition is dispensed from the bottle as a spray plume. The composition is loaded into a small handheld spray spray bottle with a pump actuation mechanism for the top push button. Such bottles include refillable bottles with a capacity of 10 mL, commonly used by travelers to distribute fragrances or other sprayable cosmetic fluids. Suitable bottles include a dropper stop, 10 ml aluminum silver color travel spray. Test spray the sample several times just before imaging with the camera to ensure that the bottle tube is primed and the nozzles are not clogged. During the test, manually press the spray actuation button with the index finger at a constant force and speed to advance the duration of the fully actuated stroke as fast as possible, with a length of less than 1 second. Suitable interval speeds include synchronous compression with a 90 second ^-1 metronome with full compression at the beat.

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

Polysaccharide Weight Average Molecular Weight Test Method The weight average molecular weight (Mw) of xanthan gum is measured using gel permeation chromatography by multi-angle light scattering detection (GPC-MALS). A suitable device is a Waters 2695 Separation Module (Waters Associate) device in which a DAWN EOS 18-angle LS detector and an Optilab REX differential RI detector (Wyatt Technology) are connected in series.

About 10 mg of gum material was dispersed in 5 mL of purified HPLC grade water to prepare a gum solution. The sample solution was mixed and inflated overnight. Prior to GPC-MALS analysis, each sample was diluted with 0.1 M NaNO3 buffer to a concentration of 0.2 mg / mL. Samples were filtered directly into HPLC vials through a 0.45 μm Nylon 66 filter (Thermo Fisher Scientific) to remove any microgels or particulate matter.

Separation is performed on two GPC columns, such as the series-connected Waters 7.8 x 300 mm Ultrahydrogel 2000 and 7.8 x 300 mm Ultrahydrogel 250 or equivalent columns maintained at 40 ° C. The components are eluted with a mobile phase of 0.1 M NaNO3 at a uniform concentration flow rate of 1.00 mL / min. A 50 μL sample is injected for analysis.

Data from the two detectors is digitally collected using suitable software (eg, Wyatt Astra software). The weight average molecular weight (Mw) is calculated using the Zimm equation. The index index increment (dn / dc) typical of xanthan gum in aqueous solution was used in the calculation.

Polymer Acetylation Test Method Flow Injection Electrospray Ionized Quadrupole Time-of-Flight Mass Spectrometry (FI-QTOF-MS) is used to measure the ratio of acetylated to non-acetylated fragments and tested as a result. Determines the relative degree of acetylation modification in polysaccharide polymer materials. In this tandem mass spectrometry, the first quadrupole mass spectrometer is set in RF-only (broadband) mode, and as a result, all ions generated by electrospray ionization do not select a specific precursor ion. Passes through the mass filter of 1. All ions after passing through the first quadrupole are then fragmented at the second quadrupole. All fragment ions are finally mass separated and detected by a TOF mass spectrometer according to their mass-to-charge ratio (m / z). For polymer or gum materials, the polysaccharide is 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, and the higher ratio indicates the higher degree of acetylation.

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

Perform flow injection-QTOF-MS analysis using a suitable tandem quadrupole mass spectrometer system with electrospray ionization (such as Q-Tof 2 equipment from Waters Corporation (Milford, Massachusetts, USA) or equivalent). .. The equipment is controlled and analyzed using ancillary software supplied by the equipment manufacturer (MassLynx NT version 4.1 data acquisition and processing software from Waters Corporation, or equivalent). The instrument system is constructed with a delivery solvent of 5 mM ammonium acetate / 10% acetonitrile in water at a rate of 40 μL / min. No column is used in this equipment configuration. Set the electrospray capillary voltage to 3.5 kV. The first quadrupole mass spectrometer is set up in RF-only (broadband) mode. A second quadrupole with collision cell energy is set at 70 V so that both signature fragment ions, ie: m / z 205, and m / z 163, are produced to fragment the polymer material. .. The TOF mass spectrometer scans 50 Da to 3000 Da with a data acquisition time of 5 minutes for each flow injection run. The peak intensity of the m / z 205 fragment (ie, acetylated sugar) and the peak intensity of the m / z 163 fragment (ie, non-acetylated sugar) 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 A)
A sample of the invention demonstrating the preparation of a fabric treatment composition with a very low viscosity perfume liquid beneficial agent (Example A). Emulsify perfume oil and stabilize in product concentrate. The product concentrate is then diluted with water to form a sprayable aqueous composition.

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 Biochemical SA) diluted to 30% Coralone 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%;
Carda Mom Ginger Lemongrass Natural Fragrance (Procter & Gamble Company)
Water (Millipore, 18 MW)

Preparation 1 wt% 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. 5.0 grams of xanthan gum was quickly added to the beaker while mixing at 5000 RPM using a Ross Mill mixer equipped with mixing blades (4 blade stainless steel, 2.5 inches in diameter). As the solution thickened, the stirring speed was increased to 8000 RPM and mixing was continued at 8000 rpm for an additional 300 seconds.

1 wt% 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. 5.0 grams of konjac gum was quickly added to the container while mixing at 5000 RPM using a Ross Mill mixer equipped with mixing blades (4 blade stainless steel, 2.5 inches in diameter). The stirring speed was increased to 8000 RPM as the solution thickened, and the mixture was continuously mixed at 8000 RPM for another 300 seconds.

Concentrate containing liquid beneficial agent (Table 1)
The mixing vessel (1 liter glass beaker, VWR) was completely cleaned and a magnetic stir bar was added. LBA (Cardamom Ginger Lemongrass Natural Fragrance) is added to the mixing vessel. A 1 wt% xanthan gum stock solution was added to the container. 1 wt% konjac gum stock solution was added to the container. The container was placed on a magnetic stirring plate and stirred at a rate sufficient to generate a vortex in the mixture. The mixture was stirred until completely homogeneous.

Dilution to aqueous composition (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 inches in diameter). The agitation rate was set to be sufficient to generate vortices in the mixture without excessive foaming. The following materials were added to the mixing vessel in sequence and the mixture was thoroughly homogenized 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 container. The resulting mixture was trimmed with sodium hydroxide until pH 7.4 was reached (Orion, Thermo Scientific, Catalog No. 2115000). The mixture was stirred for the last 10 minutes.

Parameter measurement The aqueous composition was tested according to the following method:
Judgment of sprayability by spray test method;
The viscosity of LBA was measured by the viscosity of the liquid beneficial agent test method.

(Example B)
A sample of the invention (Example B) demonstrating the preparation of a fabric treatment composition with a very low viscosity perfume liquid beneficial agent. Emulsify perfume oil and stabilize in product concentrate. The product concentrate is then diluted with water to form a stable, sprayable aqueous composition with an acceptable average drop size distribution.

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)
Korean 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, deionization (Millipore, 18 MW)

Preparation 1 wt% 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. 5.0 grams of xanthan gum was quickly added to the beaker while mixing at 5000 RPM using a Ross Mill mixer equipped with mixing blades (4 blade stainless steel, 2.5 inches in diameter). The stirring speed was increased to 8000 RPM as the solution thickened, and the mixture was continuously mixed at 8000 RPM for another 300 seconds.

1 wt% 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. 5.0 grams of konjac gum was quickly added to the container while mixing at 5000 RPM using a Ross Mill mixer equipped with mixing blades (4 blade stainless steel, 2.5 inches in diameter). The stirring speed was increased to 8000 RPM as the solution thickened, and the mixture was continuously mixed at 8000 RPM for another 300 seconds.

Concentrate containing liquid beneficial agent (Table 3)
The mixing vessel (100 ml glass beaker, VWR) was thoroughly washed and a magnetic stir bar was added. LBA (cardamom ginger lemongrass natural fragrance) was added to the mixing vessel. A 1 wt% xanthan gum stock solution was added to the container. A 1 wt% konjac gum stock solution was added to the container. The container was placed on a magnetic stirring plate and stirred at a rate sufficient to generate a vortex in the mixture. The mixture was stirred until completely homogeneous.

Dilution to aqueous composition (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 mixing blades (4 blade stainless steel, 2.5 inches in diameter). The agitation rate was set to generate vortices in the mixture without excessive foaming. The following ingredients were added in sequence to the mixing vessel and after each addition the mixture was thoroughly homogenized: water, ethanol, Koralone B-119, and citric acid. After 10 minutes of mixing, hydroxypropyl beta CD was added to the vessel and further mixed for 600 seconds. The pH of the resulting mixture was 6.4 (measured by Orion, Thermo Scientific, Catalog No. 2115000).

Parameter measurement The aqueous composition was tested according to the following method:
Judgment of sprayability by spray test method;
Yield stress was measured by a rheological test method;
The diameter of the LBA droplet is measured by the droplet size test method;
The viscosity of LBA was measured by the viscosity of the liquid beneficial agent test method.

(Examples C to E)
Demonstrated the preparation of hair and surface treatment compositions with viscosities ranging from 58 mPa · s (Example D) to 288 mPa · s (Example C) to 4,545 mPa · s (Example E). A sample of the present invention. The LBA is emulsified and stabilized in the concentrate. The concentrate is diluted with water to form a stable, sprayable aqueous composition with an acceptable average drop size distribution.

Material Konjac gum (Nutricol® XP 3464, FMC Corp, lot 11926051)
Water (Millipore, 18 MW)
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 131481), Xanthan gum (Jungbunzlauer Inc., CAS number 11138-66-2, lot 2532585), a mixture of 0.3 wt% Symdir 68 (Syrise, Symdil® 68 preservative lot 10300058).
PDMS (Gelest, DMS-T35, Lot 4H-23386)
Argan oil (BASF, Lipofructyl® Argan LS 9779 Argania spinosa kernel oil, lot 001552044)
Liquid Beneficial 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 a speed mixer cup (FlashTek, item code 501222t) with a capacity of 60 grams or 100 grams and mixed with a BlackTek DAC 150.1 FVZ K speed mixer.

Concentrate containing liquid beneficial agent (Table 5)
Konjac gum was added to a speed mixer cup containing a pre-weighed amount of water, preservatives and flavors. Samples were mixed at 3500 RPM for 300 seconds. Xanthan gum was added to the speed mixer cup and mixed at 3500 RPM for an additional 300 seconds. The resulting mixture was allowed to stand for 24 hours. A liquid beneficial agent was added to the speed mixer cup. The sample was mixed again at 3500 RPM for an additional 300 seconds.

Dilution to aqueous composition (Table 6)
Add the amount of concentrate to the beaker (VWR Heavy Duty Low Foam Beaker, Catalog No. 10536-390) and stand mixer (VWR VOS) with propeller blades (3 blades, 1 inch radius) set at 500 RPM, 300 seconds. Diluted with water using power control, catalog number 03.306886) to give the final aqueous composition.

Parameter measurement The aqueous composition was tested according to the following method:
Judgment of sprayability by spray test method;
Yield stress is measured by rheology test method;
The diameter of the LBA droplet is measured by the droplet size test method;
The viscosity of LBA was measured by the viscosity of the liquid beneficial agent test method.

(Examples FG)
A sample of the invention demonstrating the preparation of two hair treatments or surface-treated aqueous compositions containing a blend of a liquid beneficial agent and solid fragrance particles by different mixing routes. For the first aqueous composition (Example F), perfume capsules are dispersed in the concentrate, the liquid beneficial agent (silicone blend) is emulsified and stabilized in the second concentrate. The two concentrates are mixed with water to make the final aqueous composition. For the second aqueous composition (Example G), the perfume capsule concentrate was diluted with water to prepare a preliminary aqueous composition 1, and the liquid beneficial agent (silicone blend) was diluted with water to prepare a preliminary aqueous composition. 2 is produced. These two preliminary aqueous compositions were blended to make the final aqueous composition.

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 (Syrise, lot 131481)
Fragrance Capsules (Encapsys, Lot 2018-6479)
Liquid Beneficial Agent: Silicone Blend with Y-14945 01P (Momentive, Lot 18FWFA462)
Cyclopentasiloxane (Momentive, Lot 17CWFA324)
Max 20 Speed Mixer Cup (Flacktek, Max 20 Translucent, 501 224t), Max 60 Speed Mixer Cup (Flacktek, Max 60 Cup Translucent, 501 222t), or Max 100 Speed Mixer Cup (Flacktek, Max12t) All preparations were made with a speed mixer (Flashtek DAC 150.1 FVZ-K) using any of the above.

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, 49.156 grams of water were added to the Max 60 speed mixer cup. 0.505 grams of xanthan gum was added to the cup. The cup was placed in a speed mixer at 3500 RPM for 300 seconds.

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, 49.151 grams of water were added to the Max 60 Speed Mixer Cup. 0.504 grams of konjac gum was added to the cup. The cup was placed in a speed mixer at 3500 RPM for 300 seconds.

Preparation of Silicone Blend Stock 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 a speed mixer at 3500 RPM for 300 seconds.

Concentrates containing liquid beneficial agents (Table 7)
Preparation of Concentrates Containing Perfume Microcapsules Benzyl alcohol, Euxyl PE 9010, SymDiol 68, and water were added to the Max 100 Speed Mixer Cup. Xanthan gum stock solution and konjac gum stock solution were added to the cup and mixed at 2500 RPM for 300 seconds. Finally, 1.803 grams of perfume capsules were added to the cup. The cup was placed in a speed mixer at 2500 RPM for 300 seconds.

Preparation of Concentrates Containing Silicone Blends Benzyl alcohol, Euxyl PE 9010, SymDiol 68, and water were added to the Max 100 Speed Mixer Cup. 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 a speed mixer at 2500 RPM for 300 seconds.

Dilution to aqueous composition (Table 8)
Preparation Aqueous Composition 1
Water, a concentrate containing perfume microcapsules, a concentrate containing a silicone blend, benzyl alcohol, Exyl PE 9010, and SymDiol 68 were added to a Max 100 speed mixer cup. The cup was placed in a speed mixer at 2500 RPM for 300 seconds.

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

Preliminary aqueous composition 2 was prepared by adding water, a concentrate containing a silicone blend, benzyl alcohol, Exyl PE 9010, and SymDiol 68 to a speed mixer cup. The cup was placed in a speed mixer at 2500 RPM for 300 seconds.

Prepared aqueous composition 2
The pre-aqueous composition 1 and the pre-aqueous composition 2 were added to the speed mixer cup. The cup was placed in a speed mixer at 2500 RPM for 300 seconds.

Parameter measurement The aqueous composition was tested according to the following method:
Judgment of sprayability by spray test method;
Yield stress is measured by rheology test method;
The diameter of the LBA droplet is measured by the droplet size test method;
The viscosity of LBA was measured by the viscosity of the liquid beneficial agent test method.

(Examples H to AJ)
The combination of Examples and Comparative Examples of the present invention demonstrates the importance of preparing concentrates. The sample of the present invention has good yield stress and good drop size as Example H (peppermint oil) and Example AC (argan oil). Like Example N (peppermint oil), one of the comparative examples has no yield stress. Although other comparative examples have yield stresses, the viscosity of the concentrate preparation is such that it emulsifies a liquid beneficial agent that yields very large drops similar to Example AH (T31 oil) and Example M (peppermint oil). Is inadequate.

Material Xanthan gum (CPK Keltrol 1000, 7C5936K)
Konjac gum (Nutricol® XP 3464, FMC Corp. 11926051)
Water (Millipore Corporations, 18 MW)
Acticide MBS preservatives (Thor GmbH, Acticide® MBS biocides, lots RP-332371-1710)
Koralone (Koralone ™ B-119 Preservative, Dow Chemical Company, Lot YY00G46902)
Liquid Beneficial Agent: Peppermint Oil (MFR Underher Bethlehem USA, Lot 50725K);
Argan oil (manufacturer, lot PL-A128787)
T31 Silicone Oil (Gelest Corporation)
All preparations were made with a speed mixer (Flashtek DAC 150.1 FVZ K, model) using a 60 ml speed mixer cup (model).

1 wt% xanthan gum stock solution 0.08 grams of Koralone and 99.0 grams of water were added to the speed mixer cup. 1.0 gram of xanthan gum powder was added to the speed mixer cup. The samples were mixed in a speed mixer at 3500 RPM for 300 seconds. The resulting sample was left on a shaker table (VWR Standard 3500 Orbital Shaker, Catalog No. 89032-094) set at a moderate rate for 12 hours to ensure complete hydration of xanthan gum.

1 wt% konjac gum stock solution 0.08 grams of Koralone and 99.0 grams of water were added to the speed mixer cup. 1.0 g of konjac gum powder was added to the speed mixer cup. The samples were mixed in a speed mixer at 3500 RPM for 300 seconds. The resulting sample was left on a shaker table (VWR Standard 3500 Orbital Shaker, Catalog No. 89032-094) set at a moderate rate for 12 hours to ensure complete hydration of konjac gum.

Concentrates containing liquid beneficial agents (Tables 9-14)
A 1 wt% xanthan gum stock solution and a 1 wt% 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.

Parameter measurement The obtained preparation was measured by the following method:
The viscosity of LBA is measured by the viscosity of the liquid beneficial agent test method;
The viscosity of the concentrate is measured by the rheology method;
Yield stress of concentrate is measured by rheology test method;
The diameter of the LBA droplet was measured by the droplet size test method.

(Examples AK to AL)
In the examples of the invention demonstrating the preparation of concentrated compositions of products, it may be suggested that both cod gum and heat are utilized to enhance the binding of the gum. First, peppermint oil was emulsified into a concentrated composition containing a blend of xanthan gum and tara gum maintained at room temperature (Example AK). Next, peppermint oil was emulsified into a concentrated composition containing a blend of xanthan gum and tara gum maintained at a temperature of 60 ° C. (Example AL).

Material Water (Millipore Corporations, 18MW)
Xanthan gum (CPK Keltrol 1000, lot 7C5936K)
Tara Gum (Ingredion TIC Pretested Tara Gum 100, Lot 33809)
Preservatives (Koralone B19, Dow Chemical Company, Lot YY00G41902)
Liquid Beneficial Agent: Peppermint Oil (MFR Underher Bethlehem USA, Lot 50725 K)
All preparations were made with a speed mixer (Flashtek DAC 150.1 FVZ K).

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 a speed mixer at 3500 RPM for 300 seconds.

Preparation of 1 wt% Tara Gum Stock Solution Add 0.049 grams of preservative and 49.467 grams of deionized water to a Speed Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t). Add 0.502 grams of tara gum powder to the cup and place the cup in a speed mixer at 3500 RPM for 300 seconds.

Concentrates containing liquid beneficial agents (Table 15)
Preparation of concentrate at room temperature Using a Speed Mixer Max 60 cups, add the mass of preservatives, add the mass of water, add the mass of 1% by weight xanthan gum stock, and add 1% by weight of tara gum stock. Add mass and add the specified mass of LBA. Speed Mixer Max 60 cups and all contents were mixed at a specified speed for a specified time. The composition was maintained at room temperature for 12 hours.

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 1% by weight of cod. Add the mass of gum stock and add the specified mass of LBA. Speed Mixer Max 60 cups and all contents were mixed at a specified speed for a specified time. The composition was maintained at a temperature of 60 ° C. for 1 hour.

Parameter measurement The obtained preparation was measured by the following method:
Viscosity of LBA as measured by the viscosity of the liquid beneficial agent test method;
Viscosity of concentrate measured by rheological method;
Yield stress of concentrate measured by rheology test method;
The diameter of the LBA droplet is measured by the droplet size test method.

(Example AM-AR)
The examples and comparative examples of the present invention show the importance of comparing the viscosity of the liquid beneficial agent with the concentrated composition in producing good droplets. Examples AM to AQ have a reduced concentration in the concentrated composition and have a corresponding viscosity. As shown in the top 5% of the distribution, the drop size increases with decreasing viscosity until Example AQ is unable to produce acceptable drops. However, replacement with a highly viscous liquid beneficial agent (Example AR) allows for the formation of acceptable drops.

Materials 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 (Guest Corporation)
Preservatives (Thor GmbH, Actide® MBS Biocide, Lot RP-332371-1710)

A concentrate containing a liquid beneficial agent 200 grams of water and 0.6 g of Actide were added to a 100 ml beaker. Xanthan gum and konjac gum were added slowly 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 gum. A portion of this composition was placed in a 100 mL speed mixer cup (FlashTek, item code 501 222t). A liquid beneficial agent was added to the cup. The cup was tightly covered and placed in a speed mixer (FlashTek DAC 150.1 FVZ K speed mixer) and mixed at 3500 RPM for 300 seconds.

Dilution to Aqueous Composition The resulting aqueous mixture was diluted with water to a total gum concentration of 0.05% by weight.

Parameter measurement The obtained preparation was measured by the following method:
The viscosity of LBA is measured by the viscosity of the liquid beneficial agent;
The viscosity of the concentrate was measured by a rheology test method;
The diameter of the drop size of LBA in an aqueous composition is measured by the drop size test method;
The yield stress of the aqueous composition was measured by the rheology test method.

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

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 (Syrise, lot 131481)
Peppermint oil (MFR Underher Bethlehem USA, lot 50725 K)
All preparations were made with a speed mixer (Flashtek DAC 150.1 FVZ K).

Preparation of 1 wt% xanthan gum stock solution In a Speed Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t), 0.102 grams of benzyl alcohol, 0.104 grams of Exyl PE 9010, 0.151 grams of SymDiol 68. , And 49.156 grams of deionized water are added. Add 0.502 grams of xanthan gum powder to the cup and place the cup in a speed mixer at 3500 RPM for 300 seconds.

Preparation of 1 wt% konjak gum stock solution In a Speed Mixer Max 60 cup (Flacktek, Max 60 Cup Translucent, 501 222t), 0.106 grams of benzyl alcohol, 0.108 grams of Exyl PE 9010, 0.154 grams of SymDiol. 68 and 49.157 grams of deionized water are added. Add 0.501 grams of konjac gum powder to the cup and place the cup in a speed mixer at 3500 RPM for 300 seconds.

Concentrates containing liquid beneficial agents (Table 18)
Preparation of 30:70 Concentrate Using a Speed Mixer Max 60 cups, 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. Was added to a Speed Mixer Max 60 cup (Flashtek, Max 60 Cup Translucent, 501 222t). 4.506 grams of xanthan gum stock was added, 10.508 grams of konjac gum stock was added, and the cup was placed in a speed mixer at 2500 RPM for 300 seconds. 1.057 grams of peppermint oil was added and the cup was placed in a speed mixer at 2500 RPM for an additional 300 seconds.

Preparation of 60:40 Concentrate Using a Speed Mixer Max 60 cups, 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. Was added to a Speed Mixer Max 60 cup (Flashtek, Max 60 Cup Translucent, 501 222t). 9.002 grams of xanthan gum stock was added, 6.006 grams of konjac gum stock was added, and the cup was placed in a speed mixer at 2500 RPM for 300 seconds. 1.355 grams of peppermint oil was added to the cup and the cup was placed in a speed mixer at 2500 RPM for an additional 300 seconds.

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

Preparation of aqueous composition, option 2
In one example, using a Speed Mixer Max 60 cups, deionized water, 60:40 concentrate, benzyl alcohol, Euxyl PE 9010, and SymDiol 68 were added and treated at 2500 RPM for 300 seconds. In the second embodiment, deionized water, 60:40 concentrate, benzyl alcohol, Euxyl PE 9010, SymDiol 68, and konjac gum stock were added using a speed mixer Max 60 cup and treated at 2500 RPM for 300 seconds. ..

Parameter measurement:
The viscosity of LBA is measured by the viscosity of the liquid beneficial agent;
The viscosities of the aqueous composition and the concentrated composition were measured by a rheological test method;
The diameter of the drop size of LBA in an aqueous composition is measured by the drop size test method;
The yield stress of the aqueous composition and the concentrated composition was measured by a rheology test method.

(Examples AW to BL)
Examples and comparative examples of the present invention demonstrate important parameters in the preparation of product concentrates. These include samples of the invention having yield stress and good drop size, such as Examples AW-BE. Since these include comparative examples having no yield stress as in Examples BG to BL, the amounts and ratios of xanthan gum and konjac gum are different. Most importantly, these examples are capable of emulsifying up to 20% by weight of the liquid beneficial agent (Example AZ), but 60% by weight despite the presence of relative viscosity and yield stress. It has been demonstrated that the liquid beneficial agent (Example BF) cannot be effectively emulsified.

Material Konjac gum (konjac gum, FMC, Nutricol XP 3464, lot 11926051)
Water, deionization (Millipore, 18 MW)
Preservatives Actidide 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 a speed mixer cup (FlashTek, item code 501222t) with a capacity of 60 grams or 100 grams and mixed with a BlackTek DAC 150.1 FVZ K speed mixer.

Concentrate containing liquid beneficial agent Konjac gum was added to a speed mixer cup containing water, preservatives, and fragrances. The samples were mixed at 3500 rpm for 5 minutes. Xanthan gum was weighed, carefully and slowly added to the speed mixer cup and mixed again at 3500 rpm for an additional 5 minutes. If any significant undissolved gum chunks are found, the sample is further mixed at 3500 rpm for an additional 5 minutes until the gum is completely dissolved. The resulting mixture was allowed to stand for 24 hours. A liquid beneficial agent was added to the speed mixer cup. The sample was mixed again at 3500 rpm for an additional 5 minutes.

Dilution to Aqueous Compositions A portion of the concentrate was removed, added to a plastic jar and diluted with water. The mixture was stirred at 500 rpm for 300 seconds in a Ross mill mixer equipped with a mixing blade (4-blade stainless steel, 2.5 inches in diameter) (or equivalent) to give an aqueous composition.

Parameter measurement The obtained preparation was measured by the following method:
The viscosity of LBA was measured by the viscosity of the liquid beneficial agent test method. The viscosity of the concentrate was measured by the rheology test method. The diameter of the drop size of LBA in the aqueous composition was measured by the drop size test method. The yield stress of an object was measured

(Examples BM to BP)
A single concentrate each containing a beneficial agent (Example BM and Example BN), a blend of two concentrates with a beneficial agent (Example BO), and a single concentrate prepared with both beneficial agents. Examples of the present invention demonstrating the preparation of an aqueous composition from a product (BP).

Material Xanthan gum (xanthan gum, CPK Keltrol 1000, 7C5936K)
Konjac gum (Konjac gum (Nutricol (registered trademark) 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 (Syrise, lot 131481)
All preparations were made with a speed mixer (Flashtek DAC 150.1 FVZ K, model).

1 wt% xanthan gum stock solution 0.106 grams of benzyl alcohol, 0.106 grams of Exyl alcohol, 0.151 grams of SymDiol 68 were added to 49.154 grams of water in a 60 ml speed mixer cup (part). .. 0.505 grams of xanthan gum was carefully added to the cup. The mixture was treated with a speed mixer at 3500 RPM for 300 seconds.

1 wt% konjac gum stock solution 0.101 grams of benzyl alcohol, 0.100 grams of Exyl alcohol, 0.157 grams of SymDiol 68 are added to 49.153 grams of water in a 60 ml speed mixer cup (part). bottom. 0.502 grams of konjac gum was carefully added to the cup. The mixture was treated in a speed mixer at 3500 RPM for 300 seconds.

Silicone Blend Stock Solution 3.308 grams of Y14945 silicone oil and 6.708 grams of cyclopentasiloxane silicone oil are blended. The mixture was treated with a speed mixer at 3500 RPM for 300 seconds.

Gum Concentrate with Liquid Beneficial Agent Concentrate with Beneficial Agent Concentrate with Perfume Capsule Water, preservatives, xanthan gum stock solution, and konjac gum stock solution were added to a 50 ml speed mixer cup with the perfume capsule. The mixture was mixed at 2500 rpm for 300 seconds.

Concentrate water containing a silicone blend, preservatives, xanthan gum stock solution, and konjac gum stock solution were added to a 50 ml speed mixer cup with the silicone blend. The mixture was mixed at 2500 rpm for 300 seconds.

Concentrate water containing perfume capsules and silicone blends, preservatives, xanthan gum stock solution, and konjac gum stock solution were added to a 60 mL speed mixer cup with perfume capsules and silicone blends. The mixture was mixed at 2500 rpm for 300 seconds.

Dilution to Aqueous Composition Completion of Preparation Add water to a 100 ml speed mixer cup. Then, a suitable amount of benzyl alcohol, Exyl PE 9010, and SymDiol 68 are added. Finally, different concentrates are added. The mixture was mixed at 2500 rpm for 300 seconds.

The dimensions and values disclosed herein should not be understood as being strictly limited to the exact numbers listed. Instead, unless otherwise indicated, each such dimension is intended to mean both the listed values and the functionally equivalent range surrounding the values. For example, the dimension disclosed as "40 mm" is intended to mean "about 40 mm".

It should be understood that all maximum numerical limits given throughout the specification include all lower numerical limits as if such lower numerical limits were explicitly stated herein. be. All minimum numerical limits given throughout the specification include all higher numerical limits as if such higher numerical limits were expressly described herein. All numerical ranges given throughout the specification are all narrower numerical ranges contained within such a wider numerical range, and are all such narrower numerical ranges explicitly stated herein. Including like.

All documents cited herein, including any cross-referenced or related patents or patent applications, and any patent applications or patents for which this application claims priority or interest thereof, are excluded or limited. Unless expressly stated, the whole is incorporated herein by reference. Citation of any document is not considered prior art to any invention disclosed or claimed herein, or it may be used alone or in combination with any other reference (s). At times, no such invention is considered to teach, suggest or disclose. In addition, if any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in the document incorporated by reference, the meaning or definition given to that term in this document applies. It shall be.

Having exemplified and described specific embodiments of the invention, it will be apparent to those skilled in the art that various other modifications and modifications can be made without departing from the spirit and scope of the invention. Accordingly, it is intended that all such changes and modifications within the scope of the invention are covered by the appended claims.

Claims (15)

It ’s a sprayable product,
With a spray dispenser,
A water phase comprising an aqueous composition placed in the spray dispenser, the aqueous composition comprising a liquid phase and liquid beneficial agent droplets in which the aqueous composition is uniformly and discontinuously dispersed throughout the aqueous phase. Contains a structuring agent system comprising a first polysaccharide and a second polysaccharide different from the first polysaccharide, the aqueous phase containing less than 10,000 ppm of a surfactant and said aqueous composition. Is a sprayable product that exhibits yield stress as measured by the rheology test method. The sprayable product according to 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. The sprayable product according to claim 2, wherein the second polysaccharide is selected from the group consisting of konjac gum, tara gum, locust bean gum, or a combination thereof. The sprayable product according to any one of claims 1 to 3, wherein the structuring agent system is present in a concentration of 0.5% by weight or less based on the total weight of the aqueous composition. The sprayable according to any one of claims 1 to 4, wherein the first polysaccharide is present in a concentration of more than 10% by weight and less than 90% by weight based on the total weight of the structuring agent system. Product. The sprayable product according to any one of claims 1 to 5, wherein the aqueous phase contains less than 100 ppm of a surfactant, preferably the aqueous composition does not contain an effective amount of the surfactant. .. The sprayable product according to any one of claims 1 to 6, wherein the aqueous composition contains more than 90% by weight of water. The one according to any one of claims 1 to 7, wherein the liquid beneficial agent is selected from the group consisting of silicone, aminosilicone, D5, PDMS, essential oils, natural oils, perfume oils, polyoils, and combinations thereof. A product that can be sprayed. The sprayable product according to any one of claims 1 to 8, wherein the liquid beneficial agent droplet has a diameter of less than 300 μm measured by a droplet size test method. The sprayable product according to any one of claims 1 to 9, wherein the liquid beneficial agent droplet constitutes less than 20% by weight of the aqueous composition. An aqueous composition comprising an aqueous phase and liquid beneficial agent droplets disperse discontinuously throughout the aqueous phase, wherein the aqueous composition comprises.
A step of mixing the first polysaccharide and the second polysaccharide in water to form a concentrated aqueous phase, wherein the first polysaccharide is different from the second polysaccharide. ;
A step of emulsifying a liquid beneficial agent in the concentrated aqueous phase to form discontinuously dispersed liquid beneficial agent droplets across the concentrated aqueous phase;
It is produced by a method comprising diluting the concentrated aqueous phase with additional water to form the aqueous composition, and the concentration of the structuring agent system in the concentrated aqueous phase is said to be aqueous. An aqueous composition that is higher than the concentration of the structuring agent system in the composition. 11. The aqueous composition of claim 11, further comprising a plurality of solid particles. The aqueous composition according to claim 11 or 12, wherein the liquid beneficial agent droplet contains two or more different liquid beneficial agents. A method of prescribing an aqueous composition, wherein the method is:
A step of dispersing the structuring agent system in water to form a concentrate, wherein the structuring agent system contains a first polysaccharide and a second polysaccharide different from the first polysaccharide. , Process and;
With the step of mixing the liquid beneficial agent with the concentrate to form liquid beneficial agent droplets dispersed throughout the concentrate;
Including the step of diluting the concentrate with additional water to form the aqueous composition, the concentration of the structuring agent system in the concentrate is the structuring agent system in the aqueous composition. Higher than the concentration of, the method. The method according to claim 14, wherein the concentrate is a first concentrate and the liquid beneficial agent is a first liquid beneficial agent.
A step of dispersing the structuring agent system in water to form a second concentrate, wherein the structuring agent system is a second polysaccharide different from the first polysaccharide and the first polysaccharide. Including processes and;
A step of mixing the second liquid beneficial agent with the second concentrate to form a second liquid beneficial agent droplet disperse discontinuously throughout the concentrated aqueous phase, wherein the first and second liquid beneficial agents are formed. The second liquid beneficial agent has different viscosities, with the process;
With the step of mixing the first and second concentrates;
Further comprising diluting the first and second concentrates with additional water, the concentration of the structuring agent system in the second concentrate is the structuring agent system in the aqueous composition. Higher than the concentration of, the method.

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